Diamond tool, synthetic monocrystallic diamond, method of monocrystallic diamond synthesis, and diamond jewelry

FIELD: technological processes.

SUBSTANCE: invention claims diamond tool manufactured with monocrystallic diamond, synthesised under high pressure by temperature gradient method, so that the claimed diamond crystal contains not more than 3 parts per million of nitrogen. The tool features a blade with its edge oriented in plane (110), so that Knoop scale hardness at the plane (100) in direction <110> is higher than in direction <100>. Such synthetic monocrystallic diamond is synthesised by temperature gradient method under superhigh pressure and high temperature, and its crystals contain nickel atoms introduced by atomic substitution or boron and nickel atoms introduced by atomic substitution.

EFFECT: obtaining cheap synthetic monocrystallic diamonds with reduced flaw number.

24 cl, 4 ex, 2 tbl, 7 dwg

 

The technical field to which the invention relates.

The present invention in General relates to diamond tools, synthetic monocrystalline diamond, methods of synthesis of single-crystal diamonds and diamond jewelry, and in particular to the diamond tools with superior performance, such as manufactured using diamond cutting tools, knives, etc. having a sharp cutting edge, excellent resistance to abrasion, fracture, etc. and stable quality, diamond dies, diamond tools for grinding, diamond cutters and the like, excellent resistance to abrasion, synthetic single-crystal diamond having a crystal containing Nickel in the result of atomic substitution, and to methods of synthesis of such monocrystalline diamond, synthetic single-crystal diamond having a crystal containing boron and Nickel in the atomic substitution, and to methods of synthesis of such monocrystalline diamonds and diamond jewelry with bright color.

The level of technology

Conventional instruments on the basis of single-crystal diamond previously made with natural diamonds, appropriately selected from unprocessed raw diamonds in Addition, some basic tools on the basis of single-crystal diamond was produced with the use of artificial, synthetic monocrystalline diamond (type Ib), containing nitrogen as an impurity.

Diamond is widely used for various purposes in industry, for the manufacture of jewelry and the like, because the diamond has an extremely high hardness and relatively large thermal conductivity and has a high refractive index and therefore has glitter ("play of light"). However, natural diamond is very expensive. Accordingly manufactured diamonds are widely used mainly in various industries. Such manufactured diamonds are usually synthesized by the method of temperature gradient or a similar method of growing crystals under high pressure at high temperature (as described in patent documents 1-6).

In addition, according to a recent industrial improvements were also created synthetic diamond single crystals, homogeneous, etc. and excellent resistance to abrasion and therefore superior mechanical and physical properties of natural diamond (as described in patent documents 7 to 9).

In addition, was also created synthetic monocrystalline diamond, which is the first is a semi-conducting or electrically conductive or similarly has the property that which is not inherent in the diamond (as described in patent document 10).

Patent document 1: laid Japan patent No. 60-12747

Patent document 2: lined the Japan patent No. 5-137999

Patent document 3: lined the Japan patent No. 5-138000

Patent document 4: lined the Japan patent No. 5-329356

Patent document 5: lined the Japan patent No. 6-182182

Patent document 6: lined the Japan patent No. 6-182184

Patent document 7: lined the Japan patent No. 3-131407

Patent document 8: lined the Japan patent No. 3-228504

Patent document 9: lined the Japan patent No. 7-116494

Patent document 10: lined the Japan patent No. 5-200271

Non-patent document 1: Sumiya et al., Diamond and Related Materials, 5, 1359 (1996).

Disclosure of inventions

The problem addressed by the invention

Since natural diamond contains a large amount of nitrogen as an impurity, and, in addition, reflects the complex history of its growth in the bowels of the Earth, its crystals have a large number of stress and crystal defects, and there are also large differences between them. Essentially cannot always be obtained from high-quality natural diamond crystal that does not contain impurities, crystal defects and the like. Such crystal defects natural diamond, impurities and the like are place in to the torus, it is possible triggering its destruction. As such, conventional tools are manufactured using natural diamond, are unreliable in quality, and vary considerably in their performance, service life, etc.

On the contrary, the single crystals of synthetic diamond grown under high pressure at high temperature, allowing the diamond to be in a thermodynamically stable state, surpass natural diamond crystallinity and also more stable as compared to natural diamond. However, a typical synthetic diamond contains from a few dozen to several hundred parts per million (ppm) of nitrogen in the form of isolated impurities of substitution (that is, type Ib), affecting a number of characteristics. In particular, in the ultraviolet and infrared spectral regions admixture of nitrogen causes significant absorption. In addition, the admixture of nitrogen in the crystal are not evenly distributed. As such, inside the crystal is more or less tensioned.

In addition, among the artificial synthetic diamonds, the ones that are of type Ib and contain admixtures of nitrogen as an isolated impurity substitution is used for the manufacture of cutting tools, knives and the like. Although artificial synthetic diamond is superior in stability of quality is as natural diamond, still he was still insufficient for sharpness and resistance to abrasive wear, which determines the characteristics of the instruments.

When for the synthesis of diamond applied temperature gradient method without the use of metal solvent containing added special getpagetitle nitrogen, the nitrogen contained in the solvent, can be captured in the crystal, which leads to the yellow color of the diamond, which is also described in patent documents 2 to 6.

This is atomic nitrogen substitutional impurity, and, in addition, the nitrogen atom has a larger size than the carbon atom. This causes a partial distortion of the cubic crystal structure of diamond. As a result, diamond decrease the hardness and conductivity.

In particular, when the diamond is used for industrial purposes as a cutting edge tool, such deterioration in the properties, as described above, not only directly affect the sustainability of a product for grinding (polishing), abrasion and the like, but also cause problems in the production process of the product and, therefore, indirectly affect product specifications.

More precisely, for forming from it a cutting edge diamond grind. This causes friction and therefore heat output, and less than thermal conductivity of al is Aza, the slower given that warmth, and therefore the cutting edge of the blade excessively heated and oxidized. This leads to the appearance on the cutting edge in its active steps approximately 0.04 mm, usually called a sector. This reduces the sharpness of the active part of the blade as the tool and the surface of the product after grinding polished with poor precision.

In addition, to provide a synthetic diamond having improved mechanical properties, semiconductor conductivity and electrical conductivity, which is not inherent in the diamond, crystal diamond are also introducing boron (B), which was also described in patent documents 9 and 10. However, to implement this as a source of carbon requires a special type of diamond powder, and the modern level of development of the technology for this is still insufficient.

In addition, the diamond with yellow coating, in particular a dark yellow color, instead of to be transparent or to have such color, such as blue and red, has a smaller value as jewelry. In addition, it is also difficult to use as optical components, laser Windows, etc.

In order to prevent the occurrence of nitrogen in the diamond crystal, has developed a number of ways by adding aluminum (Al), titanium (Ti), t is rcone (Zr) or similar getpagetitle nitrogen in the metal solvent in the production of diamond. These methods can provide diamond with reduced nitrogen content and also colorless and transparent. However, in order to prevent capture by crystal diamond carbides formed by getpagetitle nitrogen in the solvent, the crystal must be grown with a reduced speed. It has also been implemented using a variety of methods, which are described in patent documents 2 to 6. Currently, crystal is grown at a rate of 2 mg/h up to 2.5 mg/h max. This affects the increase in the cost of its production.

In addition, semiconductor conductivity and electrical conductivity are properties that are not inherent to diamond, and these properties are achieved in the present time, is still insufficient.

Thus, there is still a need for synthetic single-crystal diamond having a small content of impurities or nitrogen and produce low-cost way for industrial purposes, in particular for use as a tool. In addition, there is also a need for synthetic monocrystalline diamond with improved resistance to abrasive wear or similar mechanical and physical properties. Similarly, there is a need for synthetic single-crystal diamond semiconductor Prov is a need, an appropriate level of electrical conductivity. In addition, there is also a need for synthetic single-crystal diamond has a beautiful color and produce low-cost way for jewelry. Additionally, there is also a need for tools, jewelry, etc. obtained from such a synthetic monocrystalline diamond.

Besides the above, there is also a need for a method designed to facilitate the solder diamonds to the shank or something similar, the main part (body) of the tool when using diamond as the blade of the tool.

Accordingly, one of the objectives of the present invention is to provide a diamond tool, which surpasses conventional diamond tools for sharpness, resistance to abrasive wear and stability.

Another objective of the present invention is to obtain a synthetic monocrystalline diamond, which may have reduced impurity content or nitrogen and inexpensive way to be used for industrial purposes and is excellent in resistance to abrasion and similar mechanical and physical properties, can have a beautiful color and can be easily soldered to the body of the instrument, as well as in the creation of a method of manufacture is as such a synthetic monocrystalline diamond.

Another objective of the present invention is the creation of diamond jewelry using beautifully colored and inexpensive synthetic monocrystalline diamond.

Resolving problems

The proposed diamond tools manufactured using a single crystal diamond, artificially synthesized under high pressure using temperature gradient and having a crystal containing an impurity in amounts of at most 3 ppm, preferably at most 0.1 h/million

Artificial, synthetic diamond can have an admixture of nitrogen removed in the synthesis of diamond under high pressure by adding to the solvent component, which serves as getpagetitle (getter) nitrogen. This, however, has an adverse effect on the diamond because of the appearance of inclusions, resulting in deterioration of the quality of the crystal. The authors of the present invention proposed a method, which can provide crystal of good quality despite the fact that add getpagetitle nitrogen (non-patent document 1). Thus, high-purity crystal synthetic diamond (type IIa)with an admixture of nitrogen, controlled at the level of at most 3 ppm, may not contain crystal defects, stresses and the like, obukov is the R of this admixture. This will lead to increased hardness and strength and other improved mechanical properties, and reduced variation in quality. In addition to this, except that there is the admixture of nitrogen weak absorption in the ultraviolet region at 270 nm, absent any other acquisition, the admixture. When the nitrogen content of at most 0,1 ppm not observed no absorption at 270 nm. Thus can be obtained a transparent crystal in the spectral region from ultraviolet to infrared.

The authors of the present invention have studied the mechanical properties of high-purity synthetic diamond more detail and found that there is a feature that is not observed neither in the natural diamond, or in conventional synthetic diamonds.

Table 1 shows the results of measurement of Knoop hardness of synthetic diamond crystals with different concentrations of nitrogen in the plane (100) in the direction <100> and <110>. As shown in figure 1, in the plane (100) in the direction <100> Knoop hardness is improved as reduced nitrogen content. Synthetic diamond crystal with a nitrogen content of at most 1 ppm provides high hardness, comprising at least 10,000 kg/mm2. Synthetic diamond crystal with included the eating of nitrogen at most 3 ppm, according to measurements in the plane (100) in the direction <110>, does not give the usual imprint Copa that actually proves its extreme hardness. Figure 2 shows the results of measurement of Knoop hardness on the plane (100) for each orientation in this plane synthetic diamond crystal IIa with a nitrogen content of 0.1 ppm, Ib diamond crystal with nitrogen 60-240 ppm and natural crystal diamond Ia (containing about 1000 ppm of the total nitrogen as an impurity).

Table 1
No. sampleThe nitrogen concentration (ppm)Knoop hardness (kg/mm2)
(100) <100>(100) <110>
IIa-01011779*
IIa-02012898*
IIa-030,0410554*
IIa-040,0411396*
IIa-050,0411950*
IIa-060,059867*
IIa-070,3610027*
IIa-080,5 10401*
IIa-091,78474*
IIa-102,69428*
Ib-016086078475
Ib-028896697401
Ib-0323594798075
* Not measurable due to the lack of the generated fingerprint

While natural diamond and a typical synthetic diamond on the face (100) had a greater hardness in the direction <100>than in the direction <110>, a diamond with an impurity content of at most 3 ppm reveals the opposite trend. In particular, in the direction <110> it is impossible to create a print using the indenter Krupa, thereby showing that the diamond is extremely hard. This is probably due to the fact that synthetic diamond crystal IIa has significantly fewer impurities and defects, which give the opportunity to initiate deformation, when the indenter is pushed into the crystal. It should be noted that in the case of impurity contents in excess of 3 ppm, this trend was not observed, and instead, there was a trend similar to the trend for natural diamond crystal and manufactured the mini-crystal diamond Ib.

The proposed diamond tool can be made in the form of high-precision cutting tools. The above diamond with low nitrogen content, high hardness, can provide substantially resistant to abrasion high-precision cutting tools.

In addition, the proposed diamond tool can be made in the form of a microtome knife, surgical knife or the like of the diamond knife. The above diamond with low nitrogen content, high hardness and low number of defects, can provide an excellent sharp diamond knife.

Similarly, the proposed diamond tool can be made in the form of tools for drawing lines, diamond cutters (diamond needle) or the like. The above diamond with low nitrogen content, high hardness and low number of defects, can provide a tool for drawing lines, excellent resistance to abrasion and has a limited number of defects.

In addition, the proposed diamond tool can be designed as a tool for sharpening (correct tool). The above diamond with low nitrogen content, high hardness and low number of defects, can provide a sharp tool for satoc and with excellent resistance to abrasive wear.

Based on the above experimental data, the synthetic diamond with an impurity content of at most 3 ppm, preferably at most of 0.1 ppm, and with a reduced number of defects used for making tools. The content of impurities can be reduced by using a source of high-purity carbon and solvent-based Fe-Co and added to this solvent getpagetitle nitrogen, such as Ti. In addition, line defects or dislocations can be removed when used as a seed crystal, carved from a diamond crystal with low defect density.

Proposed synthetic single crystal diamond according to one aspect of the invention synthesized under high pressure at high temperature using temperature gradient, and thus it differs in that it has a crystal containing Nickel, introduced by atomic substitution.

The present invention uses a solvent having a high content of Nickel. Accordingly, this leads to a pale green color synthetic monocrystalline diamond. In addition, because the synthetic monocrystalline diamond contains a reduced amount of the replacement of the nitrogen atoms, it may have reduced stress in the crystal is, that increases hardness and resistance to abrasive wear.

Reducing the amount of nitrogen allows the diamond to be resistant to degradation due to oxidation caused by excessive heating of the diamond when it is processed in the blade tool or the like, Thus, may be provided with a raised edge.

Preferably the Nickel is contained in an amount of from 0.01 ppm to 10 h/million Nickel Content of at most 10 ppm has no adverse effect on the synthetic monocrystalline diamond in terms of hardness, resistance to abrasion and severity and, in addition, allows the diamond to show a beautiful pale green color. The Nickel content in excess of 10 ppm, causes excessive voltage, and the function and effect according to the present invention hardly show, and, in addition, the diamond becomes dark in color. The Nickel content less than 0.01 ppm is preferred for synthetic monocrystalline diamond with respect to strength and other mechanical and physical characteristics. However, the production of such a diamond is expensive and requires a large investment of time. This is due to the fact that the use of Nickel-containing solvent makes it possible to grow a crystal with a much larger IC is the rate. In addition, to achieve a pale green color in the diamond preferred way contains at least 1 ppm of Nickel.

The nitrogen is preferably contained in an amount of from 0.01 ppm to 3 h/million Specified range can effectively increase the hardness, resistance to abrasion and the like and, in addition, provides a lower cost of production.

The present invention, which is applied to the synthetic single-crystal diamond is used for a tool that can greatly show the same effect as increased hardness.

If the proposed synthetic single crystal diamond is used as the blade of the tool, and to prepaymania this diamond to the shank (or the main body of the instrument) using solder, it is preferable to use titanium-containing activated solid solder, as it allows you to solder the diamond at a relatively low temperature.

Proposed synthetic monocrystalline diamond containing Nickel and having an extremely low content of nitrogen, demonstrates not dark yellow, and pale green color. In this regard, it is preferable to use such a proposed diamond as jewelry.

When a proposed synthetic monocrystalline and the MAZ use for the tool, this tool can be very hard and resistant to abrasion tool, and thus ensures a long service life, etc. This tool may be a cutting tool, the tool for sharpening and the like. In addition, when the proposed synthetic single crystal diamond is used in jewelry, pale green coloring greatly increases the cost of diamond jewelry.

In the proposed method of synthesis of single-crystal diamond it is synthesized under high pressure at high temperature using temperature gradient, and thus the method is distinguished by the use of a solvent containing at least one of iron and cobalt, at least 36 wt.% Nickel, 1-2 wt.% titanium and 3-5,5 wt.% graphite.

In the present invention, the solvent contains about 1-2 wt.%, preferably about 1.5 wt.%, titanium, which reacts with nitrogen as an impurity, and thus prevents adverse occurrence of nitrogen in the diamond crystal. In addition, although not to add copper or a similar element, which prevents impurities, titanium will not penetrate into the diamond crystal in the form of inclusion. This is presumably due to the fact that will dissolve the al contains approximately 36 wt.%, preferably about 40 wt.%, Nickel, which is in the Periodic table, the situation is quite near the copper. Nickel is included in the diamond crystal as a substitute of atomic impurities in amounts of at most 10 h/million

The bare face of the crystal, the seed crystal preferably is a plane (100), because this allows the preferred crystal growth. In addition, synthetic single crystal diamond synthesized preferably at a temperature of 1380±25°C because this temperature can contribute to the introduction of the Nickel crystal diamond appropriately as a substitute atomic impurities.

Synthetic single crystal diamond synthesized preferably at a velocity of 3.9 to 4.7 mg/h (hour), because this speed can help increase the effectiveness from the point of view of cost and also to facilitate the introduction of the Nickel crystal diamond appropriately as a substitute atomic impurities.

Offered in another aspect of the invention a synthetic single crystal diamond synthesized at high pressure at high temperature using temperature gradient and has a crystal containing boron and Nickel, introduced by atomic substitution.

The present invention provides opportunities for the use of a solvent, containing high concentration of Nickel, and, in addition, it is added to the titanium or similar getpagetitle nitrogen and boron. This allows the synthetic single-crystal diamond to contain a reduced number of replacement of the nitrogen atoms, instead of them contain substitutional boron atoms and Nickel.

Mainly can be obtained synthetic monocrystalline diamond, which has a reduced voltage in the crystal due to the reduced nitrogen content and has considerable strength and high resistance to abrasive wear due to the contained boron. Reduced nitrogen content allows the diamond to be resistant to degradation due to oxidation caused by excessive heating of the diamond when it is processed in the blade tool or the like, Thus, may be provided with a raised edge. Moreover, synthetic monocrystalline diamond containing boron is also electrically conductive. In addition, synthetic monocrystalline diamond, which contains boron and Nickel, has a pale blue-green color.

Preferably, boron is contained in an amount of 1-300 h/million boron Content of 300 ppm or less allows you to capture the metal from the solvent in the diamond crystal as impurities in small quantities, which contributes to excellent condition is ascioti to abrasive wear. The boron content greater than 300 ppm, makes the fragile crystal, and dark in color and, therefore, unsuitable for practical use. The boron content in one h/m or more, in particular more than 5 ppm, allows the diamond to possess relevant pale blue-green color, as well as to have an appropriate level of electrical conductivity.

The Nickel is preferably contained in an amount of 0.01-10 h/million Nickel contained in an amount of 10 ppm or less, allows the diamond to have a pale blue-green color and, together with the effect of titanium or similar getpagetitle nitrogen, is a relative decrease in the amount of nitrogen included in the diamond crystal in the atomic substitution, and thus provides a single-crystal diamond, acceptable hardness, resistance to abrasion and sharp. The Nickel contained in excess of 10 ppm, is the cause of great stress and, in addition, gives the diamond a dark color. The Nickel is contained in an amount of less than 0.01 ppm, increases the time and cost of production of the diamond. In addition, Nickel is preferably contained in an amount of at least 1 ppm, because he can act together with at the same time the presence of boron to give a pale blue-green color.

Pre is respectfully nitrogen is contained in an amount of 3 ppm or less. This number allows the diamond crystal to have a reduced voltage, ensuring an acceptable level of hardness, resistance to abrasion and sharp.

The present invention, when applied to synthetic single-crystal diamond is used as a tool, can find excellent resistance to abrasive wear or significant this effect.

If the proposed synthetic single crystal diamond is used as the blade of the tool and to prepaymania diamonds to the shank (or the main part of the tool) using solder, it is preferable to use titanium-containing activated solder, because it allows you to solder the diamond at a relatively low temperature.

Because of the composition of the proposed synthetic monocrystalline diamond is essentially eliminated nitrogen, and it contains boron and Nickel, this diamond has a pale blue-green color. Preferably such diamond is used as jewelry.

When a proposed synthetic single crystal diamond is used for tool, this tool can be very hard and resistant to abrasion tool, and, thus, ensures a longer service life, etc. This tool may predstavljaetsja cutting tool, tool for sharpening and the like. In addition, when the proposed synthetic single crystal diamond is used in jewelry, pale green coloring greatly increases the cost of diamond jewelry.

As proposed in another aspect of the invention the method for the synthesis of single-crystal diamond it is synthesized under high pressure at high temperature using temperature gradient, and thus the method is distinguished by the use of a solvent containing at least one of iron and cobalt, at least 36 wt.% Nickel, 1-2 wt.% titanium, 0.1 to 0.2 wt.% boron and 3-5,5 wt.% graphite.

In the present invention, the solvent contains about 1-2 wt.%, preferably approximately 1.5 (±10) wt.%, getpagetitle nitrogen (as an example, titanium), which reacts with nitrogen as an impurity, and thus prevents adverse occurrence of nitrogen in the diamond crystal. In addition, although not to add copper or a similar element, which prevents inclusion, titanium or similar getpagetitle nitrogen will not be included in the diamond crystal as inclusions. This is presumably due to the fact that the solvent contains about 36 wt.%, preferably about 40 wt.%, Nickel, which is a Periodic eskay table position very close to the copper. Nickel is included in the diamond crystal as a substitute of atomic impurities in amounts of at most 10 h/million additionally, boron, which is contained in the solvent in a quantity of approximately 0.1-0.2 wt.%, preferably about 0.15 wt.%, also included in the diamond crystal as a substitute of atomic impurities in amounts of at most 300 h/million

In addition, the bare face of the crystal, the seed crystal preferably is a plane (100) crystal diamond, as it allows the Bor to be evenly distributed, and the diamond crystal to be grown preferred.

In addition, synthetic single crystal diamond synthesized preferably at a temperature of 1350±30°C because this temperature allows the replacement of atomic impurities, i.e. Nickel and boron, to enter into the diamond crystal accordingly.

In addition, synthetic single crystal diamond synthesized preferably with a speed of 3.1-3.8 mg/h (hour), as such rate may contribute to the increased efficiency from a cost perspective, but also allows the replacement of atomic impurities, i.e. Nickel and boron, to enter into the diamond crystal accordingly.

The proposed diamond jewelry is made of the above-described synthetic monocrystalline diamond.

The result of the inventions

When single-crystal diamond is used for making tool used synthetic diamond having a small content of nitrogen as an impurity, allows this tool to be a diamond tool having a high hardness and a low number of defects, and, therefore, more to surpass conventional diamond tools for sharpness, resistance to abrasive wear and stability.

Proposed synthetic single-crystal diamond can be characterized by the presence of a limited number of alternative nitrogen atoms. This may contribute to the reduction of stresses in the crystal and to increase the hardness and resistance to abrasive wear, allowing you to make your preferred tool.

In addition, the solvent containing Nickel, allows to synthesize diamond with increased growth rate and, thus, to obtain a diamond with a reduced cost. In addition, because the proposed synthetic monocrystalline diamond may have a pale green color, it gives it a much higher price in jewelry.

In addition, the proposed synthetic monocrystalline diamond has a low content of nitrogen contained in the crystal as a substitute atomic impurities, and contains suitable the number of boron. As such, the proposed diamond can have excellent resistance to abrasive wear. In addition, the proposed diamond can also provide synthetic monocrystalline diamond, superior, for example, resistance to abrasion and, therefore, suitable for use as a blade tool. In addition, the proposed diamond can provide a sufficiently conductive synthetic monocrystalline diamond. In addition, the proposed synthetic monocrystalline diamond may contain in the crystal of Nickel and boron as a substitute atomic impurities and, thus, have a pale blue-green color having a high value as jewelry. In addition, the above-described synthetic single crystal diamond can be obtained in an inexpensive manner.

Brief description of drawings

Figure 1 shows the Knoop hardness of synthetic diamond in the plane (100) along the direction of <100>.

Figure 2 presents the Knoop hardness of different types of diamond in the plane (100) for each orientation in this plane.

Figure 3 is a General view of the setup for the synthesis of synthetic single crystal diamond according to the third example of the present invention.

Figa is a side view of the blade of the tool, ispolzuya the synthetic single crystal diamond according to the third example of the present invention.

FIGU is a top view of the blade of the tool shown in figa.

Figure 5 is a perspective view of the tool for sharpening, use a synthetic single crystal diamond according to the third example of the present invention.

6 is a General view of the setup for the synthesis of synthetic single crystal diamond according to the fourth example of the present invention.

Figa is a side view of the blade of the tool, using a synthetic single crystal diamond according to the fourth example of the present invention.

FIGU is a top view of the blade of the tool shown in figa.

Description reference positions

11 is a source of carbon; 12 - metal solvent; 13 - crystal seed; 14 - insulating material; 15 graphite heater; 16 - working under pressure; 21 - blade of synthetic monocrystalline diamond; 22 - a layer of solder; 23 - end part of the shank; 31 - a tool for sharpening of synthetic monocrystalline diamond; 32 - sintered part.

The best ways of carrying out the invention

Hereinafter the present invention will be described using examples.

Example 1

For the synthesis of diamond crystal used method of temperature gradient at high pressure. More to ncrete, as a material of the carbon source used high-purity graphite, and the solvent used solvent from Fe-Co with the addition of 1.5 wt.% Ti as getpagetitle nitrogen. As crystal, the seed used crystal with low defect density, and as a bare face was a plane (001), and applied pressure of 5.5 GPA at a temperature of 1350°C for 70 hours for the synthesis of IIa diamond single crystal of high purity, weight about 0.8 carats.

Received the diamond crystal was colorless (achromatic and transparent, and it basically was not observed absorption in the ultraviolet, visible and infrared spectral regions with nitrogen or similar admixture, and the crystal is represented by a crystal IIa high purity with impurity content of 0.1 ppm or less. In addition, as determined using a polarizing microscope, crystal diamond essentially had no internal stresses, and, as determined by x-ray topography, crystal diamond essentially had no crystal defects.

Crystal diamond obtained as described above, used for the manufacture of cutting tools as follows: crystal diamond was processed so that it had a length of 3 mm, a width of 1 mm and a thickness of 1 mm was soldered to the tail of the vetch cutting tool preferably with the use of titanium-containing, activated solder, because it allows the welded diamond crystal at a relatively low temperature and thus provides the possibility that the surface of the single crystal diamond was less thermally damaged. Furthermore, the material of the diamond you solder to the shank with a layer of solder, preferably having a thickness of 100 μm or more. This allows the obtained cutting tool to have in the end portion reduced residual stress caused by the solder bead to the shank. In addition, to provide a surface for prepaymania material monocrystalline diamond, as the upper and lower faces of the selected plane (100). In the future made a cutting tool with a diamond blade with a cutting edge having a radius R of 10 mm and an angle of 45°.

If the plane orientation of the cutting edge corresponds to the plane (110), it facilitates the grinding of the material and, thus, allows the tool to be cutting edge with high durability and sharpness. In addition, in the manufacture of cutting tools used scalp with free abrasive grains of diamond cast iron cast parts rotating at high speed. Thus obtained cutting tool had a blade with a cutting edge, which according nablyudeniya did not contain small cracks with a size of several microns or less. This cutting tool (cutter) was mounted on a precision lathe, rotating the workpiece with a speed of 800 revolutions per minute (rpm), and the tool promoted with a speed of 0.3 μm/about to ensure slice 1 μm in metallic Ni the second part covering the surface of the mold for injection molding. Traces generated as the tool feeding was not observed, and the result has been mirror-polished surface with high precision.

Example 2

Except that getpagetitle nitrogen or Ti was added in the amount of 1.5 wt.%, for the synthesis of IIa diamond single crystal of high purity by weight is about 0.8 carats used a method similar to that described in example 1. The obtained crystal diamond was slightly yellow in varying degrees, were absorbed in the ultraviolet and visible regions of the spectrum due to the isolated substitutional nitrogen impurities contained in the amount of approximately 2.8 h/million When observed through a polarizing microscope, it was confirmed that crystal diamond essentially had no internal stresses, as in the study by x-ray topography was confirmed that he essentially had no crystal defects.

Thus obtained crystal diamond used for the manufacture of the cutting tool in a manner similar to described in the example 1. The cutting tool had a blade with a cutting edge, which according to the observations did not contain small cracks with a size of several microns or less. This cutting tool (cutter) was mounted on a precision lathe and was selected conditions similar to those described in example 1, for cutting metal Ni the second part covering the surface of the mold for injection molding. Traces generated when applying the tool was not observed, and the result has been mirror-polished surface with high precision.

Comparative example 1

Except that you didn't use getpagetitle nitrogen for the synthesis of diamond was used the method similar to that described in example 1. Received the diamond was a crystal Ib weight of one carat, containing nitrogen as an impurity and having a yellow color. According to an estimate made by means of infrared absorption spectrum, the nitrogen was present in the amount of approximately 60 h/million This synthetic Ib diamond crystal used for the manufacture of servicecatalog cutting tool in a manner similar to described in example 1. The obtained cutting tool was worse than the tool according to example 1, in relation to the severity and resistance to abrasive wear.

Comparative example 2

Natural diamond Ia used formanufacture of the cutting tool by the way similar to that described in example 1. Probably due to the fact that the cutting tool had a blade with a defect, it was not sharp and also gave considerable abrasive wear when cutting the workpiece.

Example 3

The present invention will be described hereinafter in example 3.

Synthesis

First will be described the synthesis of diamond.

Figure 3 shows the setup for the synthesis of diamond in this example. Figure 3 reference position 11, 12, 13, 14, 15 and 16 represent respectively the source of carbon, a metal solvent, the crystal is a seed crystal, an insulating material, a graphite heater and a working medium under pressure.

Source 11 carbon was graphite. Metal solvent 12 contained 42 wt.% Nickel as a main component and 1.5 wt.% titanium as getpagetitle nitrogen.

The rest was 53 wt.% iron, 5 wt.% cobalt and 4.5 wt.% graphite, with all of the above were in the form of high-purity powders having a grain size of 50-100 microns. It should be noted that iron and cobalt were mixed in the ratio, allowing for a wide variation. In addition, in the case of a crystal, the seed crystal plane (100) of the abrasive grains synthetic diamond served as a bare face.

For the synthesis of 10 pieces monocrystalline diamond weight of 1.5 carats applied pressure of 5.5 GPA at 1380 C and used the carbon source and the crystal is a seed crystal having the difference (gradient) temperatures in the 30°C for 70 hours. It should be recalled that one carat is equal to 200 mg of the Obtained monocrystalline diamond had a large plane (100). Was measured absorption in the ultraviolet, visible and infrared spectral regions, and it was confirmed that it contained 3 ppm or less of nitrogen, and 10 ppm or less of Nickel. It should be noted that since the diamond had a pale green color, the Nickel content was estimated to be at least 1 ppm, which corresponds to the concentration at which the diamond takes a pale green color. It is established that the diamond contains at least 1.5 to 2 ppm Nickel.

In addition, as determined using a polarizing microscope, diamond essentially had no internal stresses. In addition, as determined by x-ray topography, diamond essentially had no crystal defects.

Manufacturer blade tool

Synthetic diamond in this example, used for the manufacture of blades of the tool as described below.

The above synthetic diamond was processed to obtain material from a synthetic monocrystalline diamond, having a length of 5 mm, a width of 1 mm and a thickness of 1 mm and designed to climb the Oia. This material was soldered to the shank using a titanium-containing activated solder, because it allows the solder material at a relatively low temperature and therefore allows single-crystal diamond to be less thermally damaged surface.

In addition, to prevent the cutting tool from the presence of the end portion remaining there to thermal stresses solder applied layer, preferably having a thickness of 100 μm or more. In addition, to provide a surface for prepaymania this material to the shank, as the upper and lower surfaces asked the plane (100).

Then used a rapidly rotating grinding apparatus for forming the blade of the cutting tool (cutter)having a cutting edge with a radius R 100 μm, the angle of taper 30° and the slope angle of 20°. It was confirmed that the cutting edge had no cracks size of 1 μm or more and, thus, was sharp.

The cutter shown in figa and 4B. In these figures the reference position 21 denotes a blade of synthetic monocrystalline diamond; R denotes the radius of the cutting edges; α refers to the angle that is 20°; and β refers to the angle edge angle of taper), which is 30°. The reference position 22 denotes a titanium-containing layer is about solder. Reference 23 denotes the end part of the shank.

This cutter is attached to a high precision lathe. Cut the piece had a diameter of 5 mm and was rotated with a speed of 3000 rpm, the tool was applied with a rate of 0.3 μm/about to perform the cutoff of 0.1 μm in the Nickel coating covering the surface of a metal mold for injection molding, to obtain a mirror-polished surface with high precision.

When the manufacturing tool used conventional synthetic monocrystalline diamond and instruments used in the cutting mode, these tools withstood 58 treatments, whereas in the case of the present invention for the manufacture of tools and use these tools in the same mode of cutting tools withstood 93 processing. In the result, it was confirmed that in this example, the received synthetic monocrystalline diamond, suitable as a material for the blade of the tool.

Manufacturer of tool grinding

Synthetic single crystal diamond according to this example were used for making tool for sharpening as described next.

Rough diamond synthesized by using the above setup described above, rusk is lively along the plane (111) to its thickness was 0.8 mm, and cut by laser so as to obtain a material in the form of a plate having a length of 3 mm, a width of 0.8 mm and a thickness of 0.8 mm. Three such plates were placed in a sintering powder containing Nickel as a main component, and specaly.

It should be noted that the plate was obtained having an elongated portion of the surface corresponding to the plane (111) of the split plane (110) of laser cutting and sharpening surface corresponding to the plane (211). Accordingly, the end surface of the test specimen formed from this album will be a sharpening surface and thus be parallel to the direction <110> grinding.

This tool for sharpening shown in figure 5. In this figure the reference position 31 denotes a material of synthetic monocrystalline diamond plate, and the reference position 32 denotes obtained by sintering the part around it.

Tool for sharpening did reciprocating motion using a grinding stone SN80N8V51S (manufactured by Noritake, 405×50×127 mm)having a circular speed of 1500 rpm, to perform a cutoff value of 0.1 mm in each iteration, while it was applied at 0.5 mm/reverse in terms of the way with liquid (lubricant-coolant for grinding: Noritake cool NK8) for 20 minutes in the direction parallel to the axis of rotation of the grinding stone for sharpening the processed product, and measured the degree of abrasive wear.

In addition, in the same conditions also measured the degree of abrasive wear of the tool for sharpening using conventional synthetic monocrystalline diamond. The results, shown in table 2, indicate that in this example was obtained synthetic monocrystalline diamond, providing significantly less abrasive wear compared to conventional synthetic monocrystalline diamond, and, therefore, it is suitable as a material for tool sharpening.

Table 2
Orientation in the planeThe direction of the grindingThe degree of abrasive wear (10-3mm3)
Conventional product(211)<110>13,5
The present invention(211)<110>9,8

Use for jewelry

In the end there will be described a synthetic single crystal diamond according to this example, used for jewelry.

Diamond weight of 1.55 carats, sintesio the p using the above setup as described above, handled saifam so that he has acquired a rounded, diamond cut.

Received for jewelry diamond weight of 0.45 carats did not contain chips and cracks and was a green diamond.

Example 4

The present invention will be described further in the fourth example.

Synthesis

First, in this example, the diamond was synthesized as described below.

Figure 6 shows the setup for the synthesis of diamond used in this example. In this figure the reference position 11, 12, 13, 14, 15 and 16 represent respectively the source of carbon, a metal solvent, the crystal is a seed crystal, an insulating material, a graphite heater and a working medium under pressure.

Source 11 carbon was graphite. Metal solvent 12 contained 42 wt.% Nickel and 0.15 wt.% boron as main components, and 1.5 wt.% titanium as getpagetitle nitrogen. The rest was 46,85 wt.% iron, 5 wt.% cobalt and 4.5 wt.% graphite, with all of the above were in the form of high-purity powders having a grain size of 50-100 microns. You should pay attention to the fact that iron and cobalt were mixed in the ratio, allowing for a wide variation. In addition, in the case of a crystal, the seed crystal plane (100) of the abrasive grains synthetic diamond served as the seed Gras is I.

For the synthesis of 10 pieces monocrystalline diamond weight of 1.2 carats applied pressure of 5.5 GPA at 1350°C and used the carbon source and the crystal is a seed crystal having a temperature difference of 30°C for 70 hours.

The obtained monocrystalline diamond had a large plane (100). Was measured absorption in the ultraviolet, visible and infrared spectral regions, and it was confirmed that it contained 3 ppm or less of nitrogen, 50 ppm boron and 10 ppm or less of Nickel. Diamond estimates had a Nickel content of at least 1 ppm, because crystal diamond had pale blue-green color, a mixture of blue, which was attributed to Bohr, and green, which was attributed to Nickel.

In addition, as determined using a polarizing microscope, diamond essentially had no internal stresses. In addition, as determined by x-ray topography, diamond essentially had no crystal defects. In addition, single-crystal diamond was also measured in terms of electrical resistance. Crystal had a specific resistance of 10-100 Ohm·cm, showing that he had sufficient conductivity.

Manufacturer blade tool

Synthetic diamond in this example, used for the manufacture of blades of the tool according to the op the sled next.

The above synthetic monocrystalline diamond was processed to obtain material from a synthetic monocrystalline diamond, having a length of 5 mm, a width of 1 mm and a thickness of 1 mm and intended for the blade (insert) diamond end mills. This material was soldered to the shank with the activated titanium-containing solder, because it allows the solder material at a relatively low temperature and therefore allows single-crystal diamond to be less thermally damaged surface.

In addition, to prevent the cutting tool from the presence of the end portion remaining there to thermal stresses solder applied layer, preferably having a thickness of 100 μm or more. In addition, to provide a surface for prepaymania this material to the shank, as the upper and lower surfaces asked the plane (100).

Then used a rapidly rotating grinding apparatus for forming the blade of the cutting tool having a cutting edge with a radius R 100 μm, the angle of taper 30° and the slope angle of 20°. It was confirmed that the cutting edge had no cracks size of 1 μm or more and, thus, was sharp.

This blade is shown in figa and 7B. In these figures the reference position 21 l denotes swie of synthetic single crystal diamond; R denotes the radius of the cutting edges; α refers to the angle that is 20°; and β refers to the angle edge angle of taper), which is 30°. The reference position 22 denotes a layer of titanium-containing solder. Reference 23 denotes the end part of the shank.

This cutting tool attached to a high precision lathe. Cut the billet had a diameter of 5 mm and was rotated with a speed of 3000 rpm, the tool was applied with a rate of 0.3 μm/about to perform the cutoff of 0.1 μm in the Nickel coating covering the surface of a metal mold for injection molding, to obtain the mirror-polished surface with high precision.

When the manufacturing tool used conventional synthetic monocrystalline diamond and instruments used in the cutting mode, tools withstood 58 treatments, whereas in the case of the present invention for the manufacture of tools and use these tools in the same mode of cutting tools withstood 85 treatments. In the result, it was confirmed that in this example, the received synthetic monocrystalline diamond, suitable for use as a material for the blade of the tool.

According to this example of the obtained synthetic is the cue diamond single crystal, having sufficient electrical conductivity. In this regard, if the crystal is attached to the equipment that can automatically replace the tool, the tool can be measured electrical resistance to determine whether it is in contact with the cut object or the like due to this can be simplified management tools, as well as the quality management of production.

Use for jewelry

In the end there will be described a synthetic single crystal diamond is used in this example for jewelry.

Synthetic monocrystalline diamond weight of 1.2 carats, synthesized using the above setup as described above, were treated with saifam so that he has acquired a rounded, diamond cut.

Received for jewelry diamond weight of 0.36 carats did not contain chips and cracks and was a green diamond.

Each of the above described variant of implementation of the present invention may be appropriately combined with any other. In addition, although the present invention has been described and illustrated in detail here, it should be clearly understood that this is done only as an illustration and example and should not be construed as limiting the nature and scope this is the first invention, limited only by the terms of the attached claims.

Industrial applicability

The present invention is effectively applicable to diamond tools, synthetic monocrystalline diamond, methods of synthesis of single-crystal diamonds and diamond jewelry.

1. Diamond tools are manufactured using a single crystal diamond, artificially synthesized under high pressure using temperature gradient, characterized in that the said diamond has a crystal containing nitrogen in an amount of not more than 3 hours/million, and the tool has a blade, the end of which has an orientation in the plane which is the plane (110), and a Knoop hardness in the plane (100) in the direction <110> is higher than in the direction <100>.

2. The diamond tool according to claim 1, in which said crystal mentioned contains nitrogen in an amount of not more than 0.1 hours/million

3. The diamond tool according to claim 1, which is one of servicecatalog cutting tool, microtome knife, a diamond knife, diamond cutter, tool for drawing lines and tool sharpening.

4. The diamond tool according to claim 1, in which for attaching said diamond to the main body of the tool used titanium-containing activated solder (22).

5. Diamond inst the side, fabricated using single-crystal diamond, artificially synthesized under high pressure using temperature gradient, characterized in that the said diamond has a crystal containing nitrogen in an amount of not more than 3 hours/million, and the tool has a blade, the end of which has an orientation in the plane which is the plane (110)and said crystal also contains Nickel, and Knoop hardness in the plane (100) in the direction <110> is higher than in the direction <100>.

6. The diamond tool according to claim 5 in which the said Nickel is contained in an amount of at least 0,01 h/m and not more than 10 hours/million

7. The diamond tool according to claim 5, in which for attaching said diamond to the main body of the tool used titanium-containing activated solder (22).

8. Diamond tools are manufactured using a single crystal diamond, artificially synthesized under high pressure using temperature gradient, characterized in that the said diamond has a crystal containing nitrogen in an amount of not more than 3 hours/million, and the tool has a blade, the end of which has an orientation in the plane which is the plane (110)and said crystal also contains boron and Nickel, and a Knoop hardness in the plane (100) in the direction of <10> is higher than in the direction <100>.

9. The diamond tool of claim 8, in which the aforementioned boron is contained in an amount of at least 0,01 h/m and not more than 300 hours/million

10. The diamond tool of claim 8 in which the said Nickel is contained in an amount of at least 0,01 h/m and not more than 10 hours/million

11. The diamond tool of claim 8, in which to attach the aforementioned diamond to the main body of the tool used titanium-containing activated solder (22).

12. Diamond jewelry made using monocrystalline diamond, artificially synthesized at high pressure using temperature gradient, characterized in that the said diamond has a crystal containing nitrogen in an amount of not more than 3 hours/million and Nickel as a substitute of the atom, and the Knoop hardness mentioned diamond in the plane (100) in the direction <110> is higher than in the direction <100>.

13. Diamond jewelry indicated in paragraph 12, in which the said Nickel is contained in an amount of at least 0,01 h/m and not more than 10 hours/million

14. Diamond jewelry at para.12 containing nitrogen in amounts of at least 0,01 h/m and not more than 3 hours/million

15. Diamond jewelry at para.12, also containing boron as a substitute of the atom.

16. Diamond jewelry product is s indicated in paragraph 15 in which mentioned boron is contained in an amount of at least 0,01 h/m and not more than 300 hours/million

17. The method of synthesis of single-crystal diamond under high pressure at high temperature using temperature gradient, characterized by the use of a solvent consisting of at least one of iron and cobalt, at least 36 wt.% Nickel, at least 1 wt.% and not more than 2 wt.% titanium and at least 3 wt.% and not more than 5.5 wt.% graphite.

18. The method according to 17, in which use crystal is a seed crystal and the seed crystal verge-priming (13) is a plane (100) crystal diamond.

19. The method according to 17, in which the mentioned single crystal diamond synthesized at 1380±25°C.

20. The method according to 17, in which the mentioned single crystal diamond synthesized at a speed of at least 3.9 mg/h and not more than 4.7 mg/h

21. The method of synthesis of single-crystal diamond under high pressure at high temperature using temperature gradient, characterized by the use of a solvent consisting of at least one of iron and cobalt, at least 36 wt.% Nickel, at least 1 wt.% and not more than 2 wt.% titanium, at least 0.1 wt.% and not more than 0.2 wt.% boron and at least 3 wt.% and not more than 5.5 wt.% graphite.

22. The method according to item 21, which use the crystal seed, is rich seed crystal verge-priming (13) is a plane (100) crystal diamond.

23. The method according to item 21, in which the mentioned single crystal diamond synthesized at 1350±ZO°C.

24. The method according to item 21, in which the mentioned single crystal diamond synthesized with a speed of at least 3.1 mg/h and not more than 3.8 mg/h

Priority items:

10.10.2003 according to claims 1 to 4;

28.09.2004 on pp.5-24.



 

Same patents:

FIELD: technological process.

SUBSTANCE: invention pertains to the technology of obtaining plates made from monocrystalline diamond, grown using a chemical vapour deposition method (CVDM) on a substrate. The grown diamond is divided across the surface of the substrate and the plate is obtained. Its main surfaces are located across the surface of the substrate.

EFFECT: obtaining plates with large area, which do not have natural defects.

41 cl, 4 ex, 6 dwg

FIELD: technological process.

SUBSTANCE: invention pertains to the technology of obtaining monocrystalline diamond material and can be used in optics for making optical and laser windows, optical reflectors and refractors, diffraction grating and calibration devices. The diamond material is obtained using chemical vapour deposition method (CVDM) in the presence of a controlled nitrogen level, which allows for controlling development of crystal defects and therefore obtain diamond material with basic characteristics, necessary for use in optics.

EFFECT: material with basic characteristics, necessary for use in optics.

75 cl, 8 tbl, 15 ex, 9 dwg

Coloured diamonds // 2328563

FIELD: technological process.

SUBSTANCE: invention is related to the field of coloured diamonds preparation, which are used, for instance, in decorative purposes. Method of coloured single crystal diamond transformation into different colour includes stages, at which coloured single crystal diamond is prepared by method of chemical depositing from steam phase (CDSP) and prepared diamond is thermally treated at temperature from 1200 to 2500°C and pressure that stabilises diamond, or in inert or stabilising atmosphere. Prepared single crystal may be shaped as thick layer or fragment of layer, which is cut as precious stone.

EFFECT: allows to prepare diamonds with wide range of colour gamma.

61 cl, 8 ex, 5 dwg

FIELD: chemistry.

SUBSTANCE: process of hard monocrystalline diamond preparation compises fixing of inoculating diamond in the holder and its growing by the way of chemical deposition from gaseous phase induced by microwave plasma. The process is implemented at temperature ca 1000°C - 1100°C in medium N2/CH4=0.2-5.0 and CH4/H2=12-20% at total pressure 120-220 torr. Derived monocrystalline diamond has the hardness in the range 50-90GPa and fracture strength 11-20MPa m1/2.

EFFECT: increasing of diamond hardness.

7 cl, 4 dwg

FIELD: carbon materials.

SUBSTANCE: monocrystalline diamond grown via chemical precipitation from gas phase induced by microwave plasma is subjected to annealing at pressures above 4.0 GPa and heating to temperature above 1500°C. Thus obtained diamonds exhibit hardness higher than 120 GPa and crack growth resistance 6-10 Mpa n1/2.

EFFECT: increased hardness of diamond product.

12 cl, 3 dwg, 5 ex

FIELD: crystal growth.

SUBSTANCE: method comprises separating the inoculation from the source of carbon by a metal-dissolver made of an alloy of ferrous, aluminum, and carbon when a 20-30°C temperature gradient is produced between the carbon source and inoculation. The growth zone is heated up to a temperature higher than the melting temperature of the alloy by 10-20°C, and the melt is allowed to stand at this temperature for 20 hours. The temperature then suddenly increases above the initial temperature by 10-25°C and decreases down to the initial value with a rate of 0.2-3 degree per minute.

EFFECT: improved quality of crystal.

1 tbl, 2 ex

FIELD: inorganic chemistry; mining industry; electronics; other industries; methods of the synthesis of the needle-shaped and lengthened diamonds.

SUBSTANCE: the invention is pertaining to the field of the inorganic chemistry, in particular, to the method of production of the needle shape synthetic diamonds and may be used in the industrial production of the special-purpose diamonds, for example, for manufacture of the boring crown bits and the dressers, and also in the capacity of the blocks details of the audio-video playback equipment, for manufacture of the feeler probes, in the micro-mechanical devices etc. The method provides for commixing of the fusion charge composed of the alloy of Mn-Ni-Fe in the mass ratio of 60±5÷30±5÷10±5 and the powder of the carbon-containing substance and treatment of the mixture at the pressure exceeding 40 kbar and the temperature over 950°С at heating rate less than 100°C/minutes. In the capacity of the carbon-containing substance use the needle-shaped coke or graphite on the coke basis with the single-component anisotropic structure with the degree of graphitization of no less than 0.55 relative units. The invention allows to simplify the production process of the synthesis of the needle-shaped and lengthened diamonds and to increase the percentage of their output within one cycle of the production process.

EFFECT: the invention ensures simplification of the production process of the synthesis of the needle-shaped and lengthened diamonds, the increased percentage of their output within one cycle of the production process.

2 ex, 2 dwg

FIELD: carbon materials.

SUBSTANCE: invention relates to preparation of boron-alloyed monocrystalline diamond layers via gas phase chemical precipitation, which can be used in electronics and as jewelry stone. The subject matter is uniformity of summary boron concentration in above-mentioned layer. The latter is formed in one growth sector and characterized by thickness above 100 μm and/or volume exceeding 1 mm3. Boron-alloyed monocrystalline diamond preparation involves diamond substrate provision step, said substrate having surface containing substantially no crystal lattice defects, initial boron source-containing gas preparation step, initial gas decomposition step, and the step comprising homoepitaxial growth of diamond on indicated surface containing substantially no crystal lattice defects.

EFFECT: enabled preparation of thick high-purity monocrystalline diamond layers exhibiting uniform and useful electronic properties.

44 cl, 5 tbl, 7 ex

FIELD: producing artificial diamonds.

SUBSTANCE: method comprises preparing diamond substrate virtually having no defects, preparing the initial gas, decomposing initial gas to produce the atmosphere for synthesis that nitrogen concentration of which ranges from 0.5 to 500 particles per million, and homogeneous epitaxy growth of diamond on the surface.

EFFECT: increased thickness of diamond.

40 cl, 9 dwg, 5 ex

FIELD: carbon particles.

SUBSTANCE: invention relates to technology of preparing particles having monocrystalline diamond structure via growing from vapor phase under plasma conditions. Method comprises step ensuring functioning of plasma chamber containing chemically active gas and at least one carbon compound and formation of reactive plasma, which initiate appearance of seed particles in the plasma chamber. These particles ensure multidirectional growing of diamond-structured carbon thereon so that particles containing growing diamond are formed. Functioning of plasma chamber proceeds under imponderability conditions but can also proceed under gravitation conditions. In latter case, seed particles and/or diamond-containing particles in reactive plasma are supported under effect of external gravitation-compensating forces, in particular by thermophoretic and/or optic forces. Temperature of electrons in the plasma are lowered by effecting control within the range from 0.09 to 3 ev. Chamber incorporates plasma generator to generate plasma with reduced electron temperature and device for controlling forces to compensate gravitation and to allow particles to levitate in the plasma with reduced electron temperature. This device comprises at least one levitation electrode for thermophoretic levitation of particles in plasma with reduced electron temperature or an optical forceps device.

EFFECT: enabled efficient growing of high-purity duly shaped particles with monocrystalline diamond structure having sizes from 50 μm to cm range (for instance, 3 cm).

19 cl, 5 dwg

FIELD: technological processes.

SUBSTANCE: invention may be used for production of parts and cutting tools for processing of wear resistant materials, in particular, silicon-containing aluminium alloys. Layers of diamond powder and material of impregnation that are in contact are placed layer by layer on charge. Layer of diamond powder is divided into two layers. In one of the layers, which contacts with impregnation material, diamond powder is used with size of particles from 20/14 to 2/1 mcm. Additionally detonating diamond powder is introduced with size of particles in the range from 1 to 100 nanometers in the amount from 1 to 30 percents from the volume of diamond powder of this layer. In the second layer, which contacts the first one, diamond powder is used with size of particles in the range from 40/28 to 28/20 mcm, at that height of this layer in respect to the first one amounts from 2:1 to 3:1. As impregnation material silicon or silicon-containing materials are used, for example, mixture of silicon powders, flaked graphite and detonating diamond. Stock prepared by this method is affected with high pressure - from 3 to 8 GPa and temperature of 1200 - 2000°C, for 40 - 120 sec. Prior to effect of high pressure and temperature stock may be shaped in round, square, rhombic, triangular, hexagonal and other forms. Ultrahard compact is prepared with high cutting ability and output of serviceable products.

EFFECT: permits to provide high purity of processed materials surface.

2 cl, 2 dwg, 1 tbl, 6 ex

FIELD: blasting.

SUBSTANCE: blasting chamber comprises a vertically mounted cylindrical shell with bottoms, an access door and means for securing an explosive charge inside the chamber. The chamber is made of steel-plated reinforced concrete, the chamber walls contain pipes being evenly distributed over the chamber inner surface. The centrelines of said pipes are directed to the centre of the chamber, wherein the pipes are connected with air-tight water tanks that are connected with a compressed air receiver through solenoid valves, wherein the chamber bottoms have a conical shape and in the centre of each bottom there is an expander having the shape of a cylinder or a polygon, on the side face of which there is a door for loading a charge into the chamber and discharging explosion solid products. Said means for securing the explosive charge have the form of a steel wire rope extending along the chamber centerline and capable of moving, lifting and holding the charge by means of an electric hoist mounted on the top expander bottom and of a section wire, one end of which is attached to the wire rope, and another - to the charge.

EFFECT: improving the efficiency of the chamber; safety and ease of its use requiring no personnel entry inside the chamber.

2 cl, 1 dwg

FIELD: chemistry.

SUBSTANCE: process of hard monocrystalline diamond preparation compises fixing of inoculating diamond in the holder and its growing by the way of chemical deposition from gaseous phase induced by microwave plasma. The process is implemented at temperature ca 1000°C - 1100°C in medium N2/CH4=0.2-5.0 and CH4/H2=12-20% at total pressure 120-220 torr. Derived monocrystalline diamond has the hardness in the range 50-90GPa and fracture strength 11-20MPa m1/2.

EFFECT: increasing of diamond hardness.

7 cl, 4 dwg

FIELD: blasting operations.

SUBSTANCE: explosion chamber contains cylindrical hull, plain bottom, cover and fastening tools for charge of explosive substance inside the chamber, installed in cooling casing. The vertical hull and the chamber bottom is faced by steel of reinforced concrete, and as cooling casing it is used the water, partly filling the internal chamber volume, on the chamber bottom it is fixed the perforated tubes, connected with gas system or with water pump, on the inside hull surface it is fixed the vertical splitter of the air-blast wave with rectangular section, connected by several steel rings, the hull is provided with hatch, which is opened inside the chamber, nipples for gas and water excluding from the chamber and nipples for gas feeding to perforated tubes, the hatch is steel hermetical cistern filled with the water, which has nipples for water and water feeding, and also nipples for water feeding from cistern to the chamber, which are made as curved tubes, that the curve is situated higher then the water level in the cistern.

EFFECT: it is exceeded the productivity of the chamber as well as the convenience of using without stuff entering inside.

4 cl, 2 dwg

FIELD: inorganic chemistry, possible use in bio-medical research and during manufacture of non-magnetic materials, sorbents.

SUBSTANCE: in accordance to the method, industrial mixture of diamond with graphite and metals is processed by mixture of acids and oxidizing compounds. The suspension is additionally processed by cleaned concentrated hydrochloric acid with concentration of nano-diamonds in the hydrochloric acid not exceeding two percents with simultaneous ultrasound processing. Temperature of suspension is measured. Then temperature increases by at least ten degrees, irradiation is stopped. Suspension is settled. Aforementioned operations are repeated at least three times. Then suspension is washed by cleaned concentrated hydrochloric acid until coloration disappears and thiocyanate sample reaction becomes positive. Final washing is performed by deionized water until suspension stops settling.

EFFECT: resulting nano-diamonds do not contain admixtures of iron.

4 ex

FIELD: crystal growth.

SUBSTANCE: method comprises separating the inoculation from the source of carbon by a metal-dissolver made of an alloy of ferrous, aluminum, and carbon when a 20-30°C temperature gradient is produced between the carbon source and inoculation. The growth zone is heated up to a temperature higher than the melting temperature of the alloy by 10-20°C, and the melt is allowed to stand at this temperature for 20 hours. The temperature then suddenly increases above the initial temperature by 10-25°C and decreases down to the initial value with a rate of 0.2-3 degree per minute.

EFFECT: improved quality of crystal.

1 tbl, 2 ex

FIELD: inorganic chemistry; mining industry; electronics; other industries; methods of the synthesis of the needle-shaped and lengthened diamonds.

SUBSTANCE: the invention is pertaining to the field of the inorganic chemistry, in particular, to the method of production of the needle shape synthetic diamonds and may be used in the industrial production of the special-purpose diamonds, for example, for manufacture of the boring crown bits and the dressers, and also in the capacity of the blocks details of the audio-video playback equipment, for manufacture of the feeler probes, in the micro-mechanical devices etc. The method provides for commixing of the fusion charge composed of the alloy of Mn-Ni-Fe in the mass ratio of 60±5÷30±5÷10±5 and the powder of the carbon-containing substance and treatment of the mixture at the pressure exceeding 40 kbar and the temperature over 950°С at heating rate less than 100°C/minutes. In the capacity of the carbon-containing substance use the needle-shaped coke or graphite on the coke basis with the single-component anisotropic structure with the degree of graphitization of no less than 0.55 relative units. The invention allows to simplify the production process of the synthesis of the needle-shaped and lengthened diamonds and to increase the percentage of their output within one cycle of the production process.

EFFECT: the invention ensures simplification of the production process of the synthesis of the needle-shaped and lengthened diamonds, the increased percentage of their output within one cycle of the production process.

2 ex, 2 dwg

FIELD: chemical industry; methods of processing of the diamond-containing concentrates.

SUBSTANCE: the invention is pertaining to separation of the diamonds from the diamonds-containing rock and the marks of technological processes concentration and may be used in the production shops of the final treatment of the diamond- -containing concentrates in the mining-and-processing integrated works of the diamond-mining firms. For creation of the self-contained ecologically safe cycle of production of pure diamonds the processing of the diamond-containing concentrates is conducted in the autoclave at the temperatures of 200-400° С using the saturated solution of the sodium carbonate with addition of 3-5 % of the weight % of sodium hydroxide in the field of the ultrasonic radiation, then the autoclave is cooled and in the reaction mass, which contains the non-reacted water solution of the sodium carbonate, they route oppositely to the gravitational force the stream of the concentrated hydrochloric and nitrogen acids for formation of the conditions of the flotation-gravitational division and separation of the diamonds from the products of the production process. At that for creation of the closed cycle of the production process at flotation-gravitational separation of the diamonds from the products of the production process use the concentrated acids, which have remained after the final cleaning of the diamonds. The invention ensures the high quality of the cleaning of the diamonds at the minimal usage of the toxic mediums, which allows the considerable reduction of the cost of the production process.

EFFECT: the invention ensures the high quality of the diamonds cleaning, the minimal usage of the toxic mediums in the production process, the considerable reduction of its cost.

2 cl, 2 ex

FIELD: chemical industry; mining industry; other industries; methods of production of the heat-resistant composite diamond sintered articles.

SUBSTANCE: the invention is pertaining to the heat-resistant composite diamond sintered articles used in the capacity of the cutting tools, the tool used for the high-precision machining and to the jewelry branch. The diamond composite sintered article contains in the capacity of the article the diamond crystal and the very small amount of the non-diamond carbon and has the hardness according to Vickers of 85 GPa or more. The article is produced by the method providing for inclusion of the synthetic diamond powder having the average size of the grains of 200 nanometers or less, in the tantalum or molybdenum capsule, both heating and application of the pressure at usage of the apparatus for the synthesis under the super-high pressure in the thermodynamically stable conditions including the temperature of 2100°С or more and the pressure of 7.7 GPa or more. The technical result of the invention is production of the articles having the electric conductivity, the high thermal stability and having the brilliance and the glaze.

EFFECT: the invention ensures production of the articles having the electric conductivity, the high thermal stability and having the brilliance and the glaze.

6 cl, 4 ex, 3 dwg

FIELD: chemical industry; other industries; production of the superfine-grained diamond sintered articles of the high purity and high hardness.

SUBSTANCE: the invention is pertaining to the production of the superfine-grained diamond sintered articles of the high purity and high hardness, which is intended for usage in the capacity of the wear-resistant material capable to let the light go through it, and may be used in production of jewels. The article has the size of the grain equal to 100 nanometers or less. For its manufacture the superfine-grained natural diamond powder having the granulometric spread of values from null up to 0.1 microns is subjected to desiliconization, to sublimation drying in the solution, inclusion into the tantalum or molybdenum capsule without the sintering additive, heating and application of the excessive pressure to the capsule using the device for the synthesis at the super-high pressure at the temperature of 1700°С or more and under pressure of 8.5 GPa or more, which meet the conditions of the thermodynamic stability of the diamond. The technical result of the invention is realization of the synthesis of the diamond sintered article at the more low pressure, than in the standard method and without usage of any sintering additive. The article has hardness according to Vickers - 80 GPa and more and is excellent concerning resistance to the tear and wear and the thermal resistance.

EFFECT: the invention ensures realization of the synthesis of the diamond sintered article at the more low pressure, than in the standard method, and without usage of any sintering additive, ensures its hardness of 80 GPa and more according to Vickers and the excellent properties concerning resistance to the tear and wear and the thermal resistance.

4 cl, 5 ex, 3 dwg

Cutting plate // 2201846
The invention relates to the processing of materials by cutting, fine grinding
Up!