Device and method for forming diamonds

FIELD: production of synthetic diamonds, which may be used as windows in high power lasers or as anvils in high pressure devices.

SUBSTANCE: device for forming a diamond in precipitation chamber contains heat-draining holder for holding a diamond and ensuring thermal contact with side surface of diamond, adjacent to the side of growth surface of diamond, non-contact temperature measurement device, positioned with possible measurement of diamond temperature from edge to edge of growth surface of diamond, and main device for controlling technological process for producing temperature measurement from non-contact device for measuring temperature and controlling temperature of growth surface in such a way, that all temperature gradients from edge to edge of growth surface are less than 20°C. A structure of sample holder for forming a diamond is also included. Method for forming a diamond includes placing a diamond in the holder in such a way, that thermal contact is realized with side surface of diamond, adjacent to growth surface side of diamond, measurement of temperature of growth surface of diamond, with the goal of realization of temperature measurements, control of growth surface temperature on basis of temperature measurements and growth of monocrystalline diamond by means of microwave plasma chemical precipitation from steam phase on growth surface, under which the speed of diamond growth exceeds 1 micrometer per hour.

EFFECT: possible production of sufficiently large high quality monocrystalline diamond with high growth speed.

7 cl, 1 tbl, 7 dwg

 

This invention confirms the preferential right of the provisional application No. 60/331073, filed November 7, 2001, which is incorporated in this description by reference in full.

Confirmation of state law

This invention was made with government support under grants No. EAR-8929239 and DMR-9972750, awarded by the national science Foundation. The government has certain rights to this invention.

The premise of the inventions

The scope of the invention

This invention relates to a device and method for producing a diamond, and more specifically the growing diamond by using a method of microwave plasma chemical vapour deposition (MPCVD) in the chamber for deposition.

Description related field

Large-scale production of synthetic diamonds has long been the object of both scientific research and industrial production. Diamond in addition to its qualities of precious stone is the hardest known material and has the highest known thermoprotection, and transparent to a wide spectrum of electromagnetic radiation. Therefore, it is highly valued because of the wide range of applications in several industries, along with its value as a precious stone.

For at least the last twenty years was to the accessible way to obtain a small amount of diamonds by means of chemical vapour deposition (CVD). As reported B.V.Spitsyn et al. in "Vapor Growth of Diamond on Diamond and Other Surfaces", Journal of Crystal Growth, vol.52, pp.219-226, the method consists in the formation of diamond by CVD method on the substrate using a combination of methane or other simple hydrocarbon gas and hydrogen gas at low pressures and temperatures of 800-1200°C. Inclusion of hydrogen prevents the formation of graphite, while the formation of centers of crystallization and growth of diamond., In the case of use of this method have been reported growth rates of up to 1 μm/hour.

In subsequent work, for example, the work of Kato et al., reported in "Diamond Synthesis from Gas Phase in Microwave Plasma", Journal of Crystal Growth, vol.62, pp.642-644, shows the use of microwave plasma chemical vapour deposition (MPCVD) to get the diamond at pressures 1-8 kPa within temperatures of 800-1000°when the power of the microwaves 300-700 W and frequency of 2.45 GHz. In the way Kamo et al. used the concentration of methane gas 1-3%. In the case of using MPCVD method reported maximum growth rates of 3 μm/hour.

In the above-described methods and in a number of recently described how the growth rate is limited to only a few micrometers per hour. Known high-speed ways to get growth or grow only polycrystalline shape of a diamond. As a rule, attempts to get monokristallicheskij the diamond at speeds growth over approximately one micrometer per hour lead largely to the twinning of single-crystal diamond, polycrystalline diamond or even to the absence of diamond. In addition, the known processes for the production of a diamond usually require low pressures less than 100 Torr.

The invention

Thus, the invention is directed to a device and method for producing diamond, which substantially obviates one or more problems due to limitations and disadvantages inherent to this technology.

The object of this invention is a device and method for producing diamond in the system of microwave plasma chemical vapour deposition with a high growth rate and at moderate pressures.

Additional features and advantages of the invention will be disclosed in the description that follows, and will be partially understood from the description and can be explored in the practical implementation of the invention. The objects and other advantages of the invention will be specified and achieved through detailed patterns of presentation of the description and claims, and accompanying drawings.

To ensure these and other advantages and in accordance with the purpose of the present invention, which is implemented and broadly described, a device for obtaining a diamond in the chamber for deposition includes a heat sink holder for holding a diamond and for realized what I thermal contact with a side surface of the diamond, adjacent to the brink of a growth surface of the diamond, the contactless device for temperature measurement in order to measure the temperature of diamond growth surface of the diamond, and the control unit of the main technological process for obtaining temperature measurements with non-contact device for measuring temperature and temperature control the growth surface, so that all temperature gradients from the edge to the edge of the growth surface were less than 20°C.

In another embodiment of the invention provides for the design of the sample holder to obtain a diamond, which includes the diamond holder with heat-conducting thermal contact with a side surface of the diamond adjacent to the brink of a growth surface of the diamond, where the diamond is set in a heat sink holder so that it can vdvinut'sâ platform, receiving thermal energy from the heat sink holder and the first element of the actuator, which can move along an axis essentially perpendicular to the growth surface, to change the location of the diamond heat sink holder.

In another embodiment of the invention provides for the design of the sample holder to obtain a diamond, which includes a diamond heat sink holder engaged in thermal contact with the side surface is of lasa, adjacent to the brink of a growth surface of the diamond, thermal mass, receiving thermal energy from the heat of the holder, where the diamond is held in a heat sink holder under the pressure exerted by thermal mass, and a platform for receiving thermal energy from the heat of the holder through thermal mass.

According to another variant of the present invention is a method of obtaining diamond involves placing the diamond in the holder with the possibility of thermal contact with the side surface of the diamond adjacent to the edge of the growth surface of the diamond, measuring the temperature of the growth surface of the diamond, to obtain temperature measurements, temperature control growth surface-based temperature measurements and growing single-crystal diamond by the method of microwave plasma chemical vapour deposition, where the growth rate of the diamond is more than 1 micrometer per hour.

According to another variant of the present invention is a method of obtaining diamond involves placing the diamond in the holder, measuring the temperature of the growth surface of the diamond to obtain temperature measurements, temperature control growth surface using device management the main technological process using the measurement temperature t is to ensure that all temperature gradients from the edge to the edge of the growth surface were less than 20° With the growing diamond on the growth surface and changing the position of the diamond in the holder.

According to another variant of the present invention is a method of obtaining diamond includes regulating the temperature of the growth surface of the diamond such that all temperature gradients from the edge to the edge of the growth surface were less 20°and growing a single crystal diamond by the method of microwave plasma chemical vapour deposition on the growth surface at a temperature in the growth chamber for the deposition, the pressure of the atmosphere, which is at least 130 Torr.

According to another variant of the present invention is a method of obtaining diamond includes regulating the temperature of the growth surface of the diamond so that all temperature gradients from the edge to the edge of the growth surface were less than 20°and growing a single crystal diamond by the method of microwave plasma chemical vapour deposition on the growth surface at a temperature of 900-1400°C.

It should be understood that the foregoing General description and the following detailed description are exemplary and explanatory and are intended for further explanation of the claimed invention.

Brief description of drawings

Accompanying drawings, which are included to generate the, to provide further understanding of the invention, and are included in this description and form part of this specification, illustrate variants of the invention and together with the description serve to explain the principles of the invention.

Figure 1 illustrates the diagram of a device for obtaining diamond according to a variant implementation of the present invention, which shows a cross section of a device for deposition with the design of the sample holder for fixed retention of the diamond during the growth of diamond.

Figa depicts a perspective view of the device for deposition, shown in figure 1.

Fig.2b illustrates a perspective view of the diamond and the casing shown in figure 1.

Figure 3 represents a diagram of a device for obtaining a diamond according to the variant of the present invention, which shows a cross section of a device for deposition with the design of the sample holder to move the diamond growth process of diamond.

On figa-4C depict views in cross section of holders or thermal mass, which can be used according to this invention.

Figure 5 is a diagram of a device for obtaining diamond according to another variant of the present invention, which shows a cross section of a device for deposition with the design of the sample holder to move the diamond in processesof diamond.

6 illustrates a graph of a process flow illustrating a method 600 according to variants of the present invention, which can be used with the design of the sample holder shown in figure 1.

7 illustrates a graph of a process flow illustrating a method 700 according to variants of the present invention, which can be used in the case of the design of the sample holder shown in figure 5.

A detailed description of the preferred options

Now will refer to the preferred options for the implementation of the present invention, examples of which are illustrated by the accompanying drawings. Figure 1 is a diagram of a system for obtaining diamond 100 according to a variant of the present invention, in which the device 102 for deposition is depicted in cross section. The system of obtaining diamond 100 includes a system of microwave plasma chemical vapour deposition 104 (MPCVD), which contains the device 102 for deposition, and the blocks adjust reagents and plasma 106. For example, the system 104 MPCVD can be WAVEMAT MPDR 330 313 ENR, production Wavemat, Inc. This MPCVD system is capable of producing output power 6 kW with a frequency of 2.45 GHz and has a chamber volume of approximately 5000 cubic centimeters. However, the specifications with the MPCVD system can vary depending on the scale of the deposition process on the size of the area of deposition and/or deposition rate.

The system 104 MPCVD includes a camera device 102 for deposition, which is at least partially limited by a glass cover 108, which is used to seal the chamber. Before operations MPCVD the air from the chamber removed. For example, use the first vacuum pump mechanical type, for pumping the camera, and then the second vacuum pump deep-vacuum type, such as a turbo pump or a cryogenic pump, additional pumps out the air from the chamber. The plasma in the chamber generate with the help of a set of plasma electrodes placed in the chamber separately. No pumps, no plasma electrodes are not shown in figure 1.

Device for deposition 102 also includes the design of the sample holder 120 that is installed in the camera system 104 MPCVD. Usually the design of the sample holder is located in the centre of the base of the camera 122 for the deposition device 102 for deposition, as shown in figure 1. The design of the sample holder 120, as shown in figure 1, shown in cross section. The design of the sample holder 120 can have a platform 124, mounted in the base of the device 102 for deposition.

As shown in figure 1, the platform 124 may be connected to the base of the chamber for deposition 122 using bolts a and 126 C. the Platform 124 may be made of molybdenum or material of any other the CSO type, having a high thermoprotect. In addition, the platform 124 can be cooled during the growth of diamond cooling agent can flow through the pipe 128 to the cooling agent in the platform 124. The cooling agent may be water, coolant or other liquid type with sufficient capacity to serve as a coolant for cooling the platform. Although it is shown that the tube for the cooling agent has a U-shaped passage through the platform 124 in figure 1, the tube 128 to the cooling agent may have a spiral passage or other types of openings in the platform 124 for more efficient cooling of the platform 124.

On the platform 124 design of the sample holder 120, as shown in figure 1, is the set ring 130 having set screws, such as screws a and 131 for fixing elements 132A and 132b around the casing 134, which holds the diamond 136. The casing 134 is a holder, which provides thermal contact with a side surface of the diamond 136 adjacent to the upper face surface of the diamond 136. As collets 132A and 132b are screwed on the casing 134 by screws 131, the cover 134 holds the diamond 136 in a stationary position and acts as a heat sink to prevent the formation of twins or polycrystalline diamond along the edges, the growth surface of the diamond 136.

The diamond 136 may contain seed cha is th 138 diamond and cultivated part of the diamond 140. The bare part 138 of the diamond can be an artificial diamond or natural diamond. As shown in figure 1, the upper side of the growth surface of the diamond 136 is located in the area of plasma 141 having energy resonance at a height H above the base of the chamber for deposition 122. The energy of the resonance may be the maximum energy of the resonance in the plasma 141 or some fraction of the maximum energy. The upper side of the growth surface of the diamond 136 first is the bare portion 138 of the diamond, and then grown portion 140 of the diamond as the diamond grows.

As shown in figure 1, the upper face of the housing 134 is located at a distance D below the top surface or upper faces of the diamond 136. The distance D should be quite large enough to impact on the verge of a growth surface of the diamond 136 plasma 141. However, the distance D should not be so large as to prevent the cooling action of the casing 134, which prevents the formation of twins or polycrystalline diamond along the edges, the growth surface of the diamond 136. Thus, D must be in a specific range, namely 0-1,5 mm, Distance D and height H, as shown in figure 1, are set manually using screws 131 adjusting ring 130 by placing the diamond 136 in the casing, placing the casing in the collet 132 is and 132b and then tighten the screws 131.

Figure 2 is a perspective view of the device for deposition, shown in figure 1. In the centre of the base of the camera 122 for deposition figure 2 is an annular platform 124 with a Central recess 125. As shown in figure 2, the platform 124 is held in position by bolts 126a-126d. The platform 124 may be made of molybdenum or other materials having high thermal conductivity. Ring 130 with four screws a-131b is located in the recess 125 of the platform 124 together with collets 132A-132b. Alternative ring 130 may be bolted to the platform 124 to increase the conduction of heat between the platform and mounting ring.

As shown in figa, rectangular casing 134, which can be either rectangular tube, or plate, rolled into a rectangle, located in the Tsang 132A and 132b with diamond 136 inside. The cover 124 may be made of molybdenum or any other material having a high thermoprotection. The screws 131a-131d tighten the collets 132A-132b so as to tighten the cover 134 on the diamond 136 to the housing 134 acted as a heat sink with four side surfaces of the diamond 136. As shown in figure 1, the housing 134 also provides thermal contact with the platform 124. Collets 132A-132b provide thermal contact with the platform 124 and serve as the heat is x mass to transfer heat from the casing 134 to the platform 124. The tightening of the cover 134 on the diamond 136 improves the quality of thermal contact between the diamond and the casing. As shown in figure 1, the cover 134 may also make thermal contact with the platform 124. Although figa shown a rectangular shape as in the case of the shroud, and in the case of diamond, the cover and the diamond can have any geometric shape, such as elliptical, circular or polygonal. The shape of the casing or holder essentially should be the same as the shape of the diamond.

In an exemplary embodiment of the invention shown in figures 1 and 2A, the platform 124 may have a diameter of about 10.1 cm, and the cover 134 may have a width of about 2.5 see Regardless of the size chosen for the platform and shroud 134, it is possible to adjust thermal mass of the platform 122, molybdenum casing 124 and Tsang 132 for optimum heat transfer for the diamond 136. In addition, the passage and the length of the tubes 128 for the cooling agent can be modified for greater cooling effect, in particular if you want to get a particularly large diamond. In addition, as a cooling agent can be used coolant or other low-temperature liquid.

Molybdenum is the only one of the possible materials used for the platform 124, the mounting ring 130, Tsang 132, casing 134 and other components. Molib the Yong is appropriate for these components, because it has a high melting point, which is equal 2617°and high thermoprotect. Additionally, there is no tendency for the formation of large fusion graphite to molybdenum. Alternative instead of molybdenum is possible to use other materials such as alloys of molybdenum-tungsten or engineered ceramics having a high melting point above the process temperature and thermoprotect comparable with thermoprotect molybdenum.

Returning to figure 1, another component of the system receiving the diamond 100 is a contactless measuring device such as an infrared pyrometer 142, which is used for monitoring the temperature of the crystal seed 138 diamond and then grown diamond 140 during the growth process without contact with the diamond 136. An infrared pyrometer 142, for example, can be a two-color infrared pyrometer MMRON M77/78 production Mikron Instruments, Inc. of Oakland, New Jersey. An infrared pyrometer 142 focus on the crystal, the seed crystal diamond 138 or then grown on the diamond 140 by measuring the area of the target 2 mm Using an infrared pyrometer 142 measures the temperature of the growth surface of the diamond 136 with an accuracy of 1°C.

The system of obtaining diamond 100 figure 1 also includes a device 144 management MPCVD process. The device 144 management process MPCD is normally supplied as a component of the system 104 MPCVD. As is well known in the art, the device management process 144 MPCVD regulates on the basis of feedback of a number of parameters MPCVD, including, but not limited to the above the process temperature, the mass flow rate of gas, the plasma parameters and the flow rate of the reagents, using blocks 106 adjusting reagents and plasma. The device 144 management MPCVD process operates in cooperation with the main unit 146 process control. Main unit 146 of the control process receives the input signal from the device 144 MPCVD process control, infrared pyrometer 142 and from other measurement devices and other components in the system 100 receiving the diamond and performs control of the entire process. For example, the host device 146 process control can measure and control the temperature of the cooling agent and/or the flow speed of the cooling agent in the platform, using the controller 148 of the cooling agent.

The main device of the process control 146 may be a universal computer, a computer system for special purposes, such as ASIC or other known type of computer system for process control MPCVD. Depending on the type of the primary device 146 process control in trojstvo 144 process control MPCVD can be integrated into the basic device control process to combine the functions of two components. For example, the main device 146 process control may be a generic computer equipped with LabVIEW programming language from National Instruments, Inc. of Austin, Texas and the LabVIEW program so versatile computer was equipped to provide regulation, registration and notification of all process parameters.

Main unit 146 process control figure 1 regulates the temperature of the growth surface so that all temperature gradients from the edge to the edge of the growth surface were less than or equal to 20°C. the Exact temperature growth surface in General, and temperature gradients growth surface prevents the formation of polycrystalline diamond or doubles, so you can grow a large single crystal diamond. The ability to regulate the temperature gradients from the edge to the edge of the growth surface of the diamond 136 may be affected by several factors, including the ability to sink the platform 124, the position of the upper surface of the diamond in plasma 141, homogeneity of 141, the impact of which is exposed to the growth surface of the diamond, the quality of heat transfer from the edges of the diamond through the holder or casing 134 to the platform 124, the ability to adjust the power of the microwaves, the flow velocity of the cooling agent, the temperature of the cooling agent, the MSE of the spine of the gas stream, the flow rate of reagents and characteristics of reception of the infrared pyrometer 142. On the basis of the temperature measurements received from the pyrometer 142, the host device 146 process control monitors the temperature of the growth surface so that the temperature gradients from the edge to the edge of the growth surface were less than 20°C by adjusting at least one of the parameters: power microwave plasma 141, the flow speed of the cooling agent, the temperature of the cooling agent, the velocities of the gas streams and the flow rate of the reactants.

Fig.2b represents a perspective view of the diamond 136, shown in figure 1, which shows the sample points P1, P2, P3 and P4 along the growth surface 137 of the diamond 136. On fig.2b also shows the distance D between the growth surface 137 and the upper edges 139 of the diamond 136 and edge 135 of the casing 134. Usually there are large temperature changes from the point of view of differences of temperatures from edge to edge of the growth surface between the edges and the middle of the growth surface of the diamond. For example, the temperature gradients that occur between the points P1 and P2, is greater than between points P1 and P3. In another example, the temperature gradients occurring between points P4 and P2, is greater than between points P4 and P3. Thus, when regulating the temperature of the growth surface Alma is for that all temperature gradients from the edge to the edge of the growth surface were less than 20°you must at least take into account the temperature measurement between middle and edge 139 growth surface 137. For example, the host device 146 process control can regulate the temperature of the growth surface so that the temperature gradient between the points P1 and P2 was less than 20°C.

The spot size of the infrared pyrometer may affect the ability to control the temperature gradients from the edge to the edge of the top surface of the diamond and therefore the rate of growth of diamond. For example, if the size of the diamond is large compared to the spot size of the infrared pyrometer, the temperature of each of the faces of the growth surface of the diamond may be outside the field of view of an infrared pyrometer. Therefore, in the case of a diamond with a large surface growth, it is necessary to use a variety of thermometers. Each of the many thermometers should be focused on the different facets around the of the diamond surface and preferably near the corners, if any. Therefore, the host device 146 process control, which is shown in figure 1, must be programmed to integrate the overlapping fields of view from a variety of thermometers to obtain continuous "to the mouths" of temperatures from edge to edge of the diamond surface, or interpolating non-overlapping fields of view to obtain the interpreted maps of temperatures from edge to edge of the growth surface of the diamond. Alternative temperature gradient between the individual face or corner point towards the middle of the growth surface can be controlled in the form of a measure of the maximum temperature gradient that exists from edge to edge of the growth surface of the diamond.

In addition to the infrared pyrometer 142 for controlling the temperature in the system 100 receiving the diamond may be included other instrumentation. Additional instrumentation may include equipment to determine the type and quality of the diamond 136 during the growth process. Examples of such equipment include spectrometers in the visible, infrared spectrum and Raman scattering, that the nature of work are spectral and can be focused on the same point, and an infrared pyrometer 142 to obtain data on the structure and quality of the diamond during the growth process. If you have the optional equipment you can connect with the main unit 146 process control to the main unit 146 process control controlled test equipment and pre what was the results analytical methods, along with other information about the state. Additional instrumentation may be particularly useful in experimental settings, when "a proportional increase of the process to get a bigger diamond and attempts to control the quality in case of the existing system 100 receiving diamond and related processes.

As the growth process of the diamond 136 distance D and the height H increases. As the distance D increases the ability of the heat sink casing 134 faces 139 growth surface of the diamond 136 decreases. In addition, plasma characteristics, such as temperature and/or texture change as the growth surface of the diamond 136 extends into the plasma 141. In the system of obtaining diamond 100 the growth process periodically stops to the position of the diamond 136 can be adjusted down relative to the casing 134 to reduce the distance D, and the diamond 136 and the cover 134 can be adjusted down relative to the base of the camera 122 for deposition, to reduce the height H. This change of position allows you to place the growth of diamond growth surface of the diamond 136 in the desired energy resonance in the plasma 141, allows infrared pyrometer 142 and an additional when the oram to stay focused on the growth surface of the diamond 136 and provides the effect of maintaining an efficient thermal contact for heat dissipation from the faces of the growth surface of the diamond 136. However, multiple stop the growth process can be inconvenient for large-scale production and increase the chance of introducing contamination into the process, if not carried out carefully.

Figure 3 represents a diagram of a device 300 for receiving the diamond according to a variant implementation of the present invention, which shows a cross-section of the device 304 for deposition with the design 320 of the sample holder to move the diamond 136 during the growth of diamond. Some of the components of the device 300 to obtain diamonds are essentially the same. As components of the system 100 receiving diamonds, and, consequently, the discussion above with respect to figure 1, it will be sufficient to describe the components which are similarly designated, figure 3. For example, a pyrometer 142, the base of the chamber 122 for deposition, the tube 128 for the cooling agent and the glass cap 108 figure 3 is essentially the same as described in figure 1.

As shown in figure 3, the diamond 136 mounted on the element 360 drive diamond in the casing 134 structure 320 of the sample holder. The diamond 136 is installed in the casing 134 slidable on the drive element of the diamond 360, which moves along an axis essentially perpendicular to the growth surface. Item 360 drive diamond extends through the platform 324 and is regulated by the bottom platform is RMI 324 unit adjustment of the diamond shown as part of blocks 329 adjustment of the cooling agent and diamond/holder figure 3. Item 360 drive is used for installation height H between the growth surface of the diamond 136 and the base of the chamber 122 for deposition. Even though the 360 drive figure 3 shows in the form of a threaded rod, an element of the actuator may have any geometric shape, which allows you to set the diamond 136 at a certain height and position above the base of the chamber for deposition. Specialists in this field will understand that the components are placed in a glass cap, such as the element 360 drive diamond must be compatible with the conditions of vacuum, to eliminate the problems associated with maintaining the desired atmosphere.

The actuator (not shown) for element 360 drive diamond represents a motor (not shown). However, the actuator may be any of several known types of actuators depending on the size of the diamond that you want to grow, the growth rate and the desired level of precision of the movement. For example, if the diamond 136 has a small size, you can use the piezoelectric actuator. If the diamond 136 relatively large or maybe grown relatively large, the preferred motorized computer-controlled actuator. Regardless of the particular used drive main unit 346 management technology is a logical process controls the moving element 360 drive so to the diamond 136 can automatically move down in the growth process.

In addition, the drive element of the holder 362 extends through the platform 324 and is controlled by the bottom platform 324 unit adjustment of the holder, which is shown as part of blocks 329 adjustment of the cooling agent and diamond/holder figure 3.

Element 362 of the drive holder is moved along an axis essentially perpendicular to the growth surface, and serves to maintain the distance D between the face of the growth surface of the diamond 136 and the top face of the holder or casing 134. The receiving system of the diamond can have the drive element of the diamond, the drive element of the holder, or a combination of both.

Element 362 of the drive of the holder 3 can be screwed into the platform element 324 and 360 drive diamond is screwed into the element 362 of the drive holder. As a result of such arrangement, the adjustment blocks of diamond and holder comprising blocks 329 adjustment of the cooling agent and diamond/holder, shown in figure 3, can move the diamond 136, the cover 134 and or casing 134 and the diamond 136. Although the drive element of the holder 362 figure 3 shows in the form of a threaded cylinder with threads on the inner side of the element 360 drive diamond and threaded on the outside for screwing into the platform 324, the drive element of the holder may have any geometric shape, which allows oderjivat limit the distance between the face of the growth surface of the diamond 136 and the top face of the holder or casing 134. Specialists in this field will understand that the components are placed in a glass cap, such as 362 the drive element of the holder or the combination of the drive holder and the drive element of the diamond must be compatible with the vacuum conditions, in order to avoid problems associated with maintaining the desired atmosphere.

As shown in figure 3, thermal mass 364 is located in a recess in the platform 324. The holder or casing 134 is in thermal mass 364 so that he can vdvinut'sâ, to transfer heat energy from the casing 134 to the platform 324. The upper surface of thermal mass 364 may fit snugly to prevent heat transfer from the casing 134, while minimizing the electrical effect of thermal mass 364 on plasma 341. Thermal mass a, 466b and s on figa-4C, respectively, are examples of other tight thermal masses with different cross-sectional shape that alternative can be used instead of thermal mass 364, shown in figure 3. Thermal mass can be made of molybdenum. Other materials, such as alloys of molybdenum-tungsten or engineered ceramics having a high melting point above the process temperature and thermoprotect comparable with thermoprotect molybdenum, can be used as the heat treatment of the Russian mass to transfer heat away from the face of the diamond to the platform. While minimizing the electrical effect of thermal mass 364 on plasma 341, a region in the plasma 341, in which the grown diamond will be more homogeneous. In addition, during the growth of diamond, you can use a higher pressure, which will increase the rate of growth of monocrystalline diamond. For example, the pressure may range from 130 to 400 Torr and the growth rate of the single crystal can be more than 1 μm, from 1 to 150, or from 50 to 150 microns per hour. You can use a higher pressure, such as 400 Torr, so as uniformity, shape and/or position of the plasma 341 is not easily subjected to tight thermal mass 364 so as to remove heat from the faces of the growth surface of the diamond, and minimizes the electrical effect of thermal mass 364 on plasma 341. In addition, lower power microwaves, such as 1-2 kW required to maintain plasma 341. Otherwise, it would be necessary to use a lower pressure and/or increased power of the microwaves, in order to maintain uniformity, shape and/or position of the plasma 341.

As the diamond 136 increases, and the distance D and the height H increases. As the distance D increases, the ability to heat sink casing 134 faces 139 growth surface of the diamond 136 decreases. In addition, plasma characteristics, such as temperature is RA, change as the growth surface of the diamond 136 extends into the plasma 341. In the system of obtaining diamond 300 the growth process periodically stops when the diamond 136 reaches a predetermined thickness, as the distance D and the height can be adjusted primary device 346 process control through blocks 329 adjustment of the cooling agent and diamond/holder using element 362 of the drive holder and element 360 drive diamond during growth of diamond. This change of position, either manually or automatically under the control devices 144 management provides the ability to place the growth of diamond growth surface of the diamond 136 in the desired energy resonance in the plasma 341. In addition, the change of position allows infrared pyrometer 142 and any additional devices to stay focused on the growth surface of the diamond 136 and can maintain effective heat removal from the faces of the growth surface of the diamond 136.

Figure 5 is a diagram of a device for obtaining diamond 500 according to a variant of the present invention, which shows a cross-section of the device 504 for deposition with the design of the holder 520 sample to move the diamond 136 during the growth of diamond. Some components of the device 500 according to the teachings of the diamond is essentially the same as in the system 100, and 300 receiving diamond and therefore, the above discussion in relation to figures 1 and 3 will be sufficient to describe these components, similarly marked on figure 5. For example, a pyrometer 142, the base of the chamber for deposition 122, the tube 128 with a cooling agent, and a glass cap 108 figure 5 is essentially the same as described in figure 1. In another example, block 329, the adjustment of the cooling agent and diamond/holder, and the element 360 drive diamond figure 5 are essentially the same as in figure 3.

As shown in figure 5, the diamond 136 mounted on the element 360 drive diamond and tight thermal mass 566, which acts as a holder. When the location of the diamond 136 directly in skintight thermal mass 566, thermal efficiency of heat removal from the diamond 136 increases. However, the plasma 541 easier to influence, because in General skintight thermal mass to move with the actuator 562 holder platform 524 using block adjustment diamond, which is shown as part of blocks 329 adjustment of the cooling agent and diamond/holder figure 3.

Therefore, the host device 546 managing technological process should take into account such factors as the appropriate control plasma and/or other parameters of the growth process. Alternative convex thermal mass 364, showing the percent figure 3, thermal mass 466b with inclined faces on fig.4b, thermal mass with inclined faces/cylindrical top s on figs or other geometric configurations can be used instead of the concave thermal mass 566, shown in figure 5.

6 is a diagram of the sequence of processes, illustrating a method 600 according to variants of the present invention, which can be used in the case of the design of the sample holder shown in figure 1. The process 600 starts by stage S670, where appropriate seed crystal of a diamond or diamond growth process is placed in the holder. For example, in the construction of 120 sample holder figure 1, the operator places the bare portion 138 of the diamond in the casing 134 and tighten screws 131a-131d. You can use other mechanisms to hold as diamond and casing in a certain position, such as spring collets, hydraulic, or you can use other mechanisms for the application of force to the holder or casing.

As stated at the stage S672 measure the temperature of the growth surface of the diamond, or the seed diamond or cultivated diamond. For example, a pyrometer 142 figure 1 provides measurements of the growth surface, which is the upper side of a growing diamond 140, and transmits the measurement to the host device 146 control technology and the policy process. Measurements do so that the main unit of the process control can determine the temperature gradient from edge to edge of the growth surface of the diamond 136 or in the main unit of the process control enter at least the temperature verge of a growth surface of the diamond.

Main unit process control, such as the main unit 146 process control, shown in figure 1, is used to measure the temperature of the growth surface of the diamond, as indicated at stage S674 figure 6. The main unit of the process control regulates the temperature, maintaining the temperature gradients less than 20°from edge to edge of the growth surface. While regulating the temperature of the growth surface, hold the determining whether to change the position of the diamond in the holder, as shown at the stage S675 figure 6. If the main control device can regulate the temperature of the growth surface of the diamond so that all temperature gradients from the edge to the edge of the growth surface were less than 20°by adjusting the plasma gas flows and the flows of the cooling agent, the growth process is halted, so that you can change the location of the diamond in the holder, as on Asino on stage S678 figure 6, to ensure the best heat sink from the diamond and/or the best location of the diamond in the plasma. If the main device of the process control can support all temperature gradients from the edge to the edge of the growth surface of the diamond are less than 20°s, then there is the growth of diamond growth surface, as shown in stage S676 figure 6.

Measuring the temperature of the growth surface of the diamond, to regulate the temperature of the growth surface and growth of diamond growth surface occur until, until you determine that you want to change the position of the diamond, as shown in Fig.6. Although the measurement, control, cultivation and actions to determine the condition shown and described in the form of stages, they are not necessarily sequential and may coincide with each other. For example, stage of growth of diamond growth surface can occur while there is measurement of the temperature of the growth surface of the diamond and regulate the temperature of the growth surface.

Changing the position of the diamond, as indicated at stage S678, can be done manually or with a robotic mechanism. In addition, you can define reached if a diamond is predetermined or desired thickness, as shown at the stage S673 figure 6. The determination may be based on actual measurement of the mechanical or optical devices. In another example, the determination may be based on the length of processing time, taking into account the known growth rate during the process. If the diamond has reached a predetermined thickness, the growth process is terminated, as indicated at the stage of 680 figure 6. If the diamond has not reached a predetermined thickness, the growth process starts again and continues to measure the temperature of the growth surface of the diamond, temperature regulation and growth of diamond growth surface before determine that it is necessary to change the position of the diamond as shown in Fig.6.

Fig.7 is a diagram of the sequence of processes, illustrating a method 700 according to variants of the present invention, which can be used in the case of the design of the sample holder shown in figure 3 and 5. The process 700 starts by stage S770, where appropriate seed diamond, which can be a grown diamond, synthetic diamond, natural diamond, or a combination, is placed in the holder. For example, in the construction of the holder 320 sample figure 3 bare portion 138 of the diamond is placed inside the casing 134 of element 360 drive diamond, as shown in figure 3. In another example, the design of the sample holder of the bare portion 138 of the diamond is placed in a close fitting thermal mass is 566 actuator 360 diamond as shown in figure 5.

As stated at the stage S772 measure the temperature of the growth surface of the diamond, or the seed diamond, or re-grown diamond. For example, a pyrometer 142 figure 3 provides measurements of the growth surface, which is the upper side of a growing diamond 140, and transmits the measurement to the host device 346 process control. In another example, the pyrometer 142 figure 5 performs measurements on the growth surface, which is the upper surface of the bare part of the diamond 138, and transmits the measurement to the host device 546 process control. Measurements do so that the main unit of the process control can determine the temperature gradient from edge to edge of the growth surface of the diamond or in the main unit of the process control enter at least the temperature of the edge and the middle of the growth surface.

Main unit process control, such as the main unit 346 or 546, process control is used to regulate the temperature of the growth surface, as indicated at stage S774 7. The main unit of the process control regulates the temperature of the growth surface of the diamond so that the temperature and g is adiante from edge to edge of the growth surface was less than 20° C. while regulating the temperature of the growth surface, shall determine whether to change the position of the diamond in the holder, as shown at the stage S775 figure 1. If the main control unit cannot maintain the temperature of the growth surface of the diamond so that all temperature gradients from the edge to the edge of the growth surface were less than 20°by adjusting the plasma gas flows and the flows of the cooling agent, the diamond is moved in the growth process of diamond, as shown in Fig.7, with the path "YES" means the path from the stage S775 to both stages S776 and S778. Changing the location of the diamond in the holder heat from the faces of the growth surface is improved. In addition, the growth surface can be placed in the optimal region of the plasma having the consistency to maintain all thermal gradients from the edge to the edge of the growth surface of the diamond are less than 20°C. If the primary device management process can support all temperature gradients from the edge to the edge of the growth surface of the diamond are less than 20°s, then there is the growth of diamond growth surface without changing position, as shown as path "NO" from the stage S775 to step S776 7.

Measuring the temperature of the growth surface of the diamond, to regulate the temperature of the growth surface and growth of diamond on rostovgiproshat and changing the position of the diamond in the holder to happen as long until you determine that the diamond has reached a predetermined thickness. As stated at the stage S773 7, determine, do I have the diamond predetermined or desired thickness. The determination may be based on the actual measurement using mechanical or optical devices. For example, the activity monitoring software that records the depth or quantitatively determines the distance that the diamond you want to move during the growth process. In another example, the determination may be based on the length of processing time, taking into account the known growth rate during the growth process. If the diamond has reached a predetermined thickness, the growth process is terminated, as indicated at stage 780 7. If the diamond has not reached a predetermined thickness, the process of growth continues, by measuring the temperature of the growth surface of the diamond, temperature regulation, growth of diamond growth surface and by changing the position of the diamond in the holder before determine that it is necessary to change the position of the diamond, as shown as path "NO" from S773 to S774 7.

In the implementation of the methods 600 and 700 growth of diamond usually lasts as long as it can support the terms "growth stage". In General, the condition "stages of growth" refers to growth, in which a diamond is expressed is more on the growth surface of the diamond 136 so, to the diamond 136 was smooth by nature without separate protrusions on the surface or doubles. The "growth stage" can be monitored visually. Alternative you can use a laser to scan the growth surface of the diamond 136. Changing the laser reflection will testify about the education of protrusions on the surface or doubles. This laser reflection can be programmed in the main device of the process control as a condition to stop the growth process. For example, in addition to determine as to whether the diamond pre-set thickness, it is also possible to determine if the laser reflection.

In General, methods according to exemplary variants of implementation of the present invention are designed to create a large diamond high quality with high speed growth [100]. The process temperature can be selected in the range of approximately 900-1400°depending on the specific type single-crystal diamond that you want, or whether oxygen. At higher temperatures can be obtained polycrystalline diamond, and at lower temperatures can be obtained diamond like carbon. During the growth process using a pressure of approximately 130-400 Torr at a concentration of methane in the range 6-12% methane. The concentration of hydrocarbons of you who e 15% can cause excessive precipitation of graphite in the chamber MPCVD. 1-5% N2/CH4added to the reaction mixture, creating more available space growth, increase the growth rate and stimulate end the growth of {100}. Other aspects of the invention can be understood in more detail from the following examples.

Example 1

The growth process of diamond was carried out in the above-described MPCVD chamber, shown in figure 1. First commercial crystal is a seed crystal of diamond type Ib, synthesized at high pressure and high temperature (NRNT), 3.5×to 3.5×1.6 mm3was placed in the chamber for deposition. Crystal is a seed crystal of diamond had a shiny smooth surface, which was cleaned by ultrasound in acetone. Surface deposition corresponded to the surface of the {100} crystal, the seed crystal diamond with an accuracy of two degrees.

Then the chamber for deposition was evacuated to a main pressure 10-3Torr. An infrared pyrometer 142 focused through a quartz window at an angle of incidence of 65 degrees to the growth surface of the diamond and he had the minimum spot size 2 mm2. The growth of diamond was carried out at a pressure of 160 Torr using a gas concentration 3% N2/CH4and 12% of CH4/N2. The process temperature was 1220°and flow rate of gases was 500 cm3in min H2, 60 cm3min CH4and 1.8 cm3min N2. The deposition was given the opportunity to continue Atsa within 12 hours.

The resulting diamond was a dull diamond size 4,2×4,2×2.3 mm3and represented approximately 0.7 mm knot on the crystal on the seed crystal, which was grown at the growth rate of 58 microns per hour. The structure of growth showed that the rate of growth of the face <100> was higher than the growth rate of angular faces <111>. Option growth αequal to 2.5-3.0.

Obtained by the deposition of diamond characterized. Using x-ray diffraction (XRD), Raman spectroscopy Raman scattering, photoluminescence (PL) spectroscopy and electron paramagnetic resonance (EPR). The study of x-ray diffraction of the resulting diamond confirmed that it was a single crystal with a low degree of polycrystalline, localized on the upper faces of the diamond. Visible/near infrared transmittance spectrum grown using MPCVD diamond and seed diamonds confirms that nitrogen is effectively embedded in the crystal structure. Raman spectroscopy shows that the top face is grown using MPCVD diamond has different optical characteristics than the bare diamond, but has the same internal stress.

Received a number of MPCVD-diamonds according to the instructions of example 1, varying the temperature of the described process is. These experiments show the limits of the temperature of the process for obtaining different types of diamond growth process according to variants of the present invention. Table 1 presents the results of these additional experiments.

Table 1
The process temperature for different types of diamond
Temperature limitsThe type of the obtained diamond
<1000°Spherical, dark diamond-like carbon (DLC)
1000-1100°Smooth dark brown
1100-1200°Brown
1200-1220°Smooth growth of yellow tint
1220-1400°Step-drop-down type up a pyramid-like the octahedron yellow
>1300°Twin or polycrystalline diamond

Example 2

Net received by way of the CVD single crystal diamond high quality thickness of more than 0.6 mm was formed essentially in accordance with the method of example 1 described above, adding a small amount (1-3%) of oxygen and lowering the growth temperature to 900 degrees Celsius. Added oxygen makes possible more or what kind of growth temperature, that fixes related to nitrogen impurities and reduces the level of impurities of silicon and hydrogen. The growth rate using this method is approximately 10 μm/hour, less than the rate in example 1, but still higher than with conventional methods.

The color of the diamond formed discussed above ways, changed by annealing. For example, yellow brown diamond by using annealing to change to green. For more information on diamond obtained in the examples described above, is a publication of the inventors, entitled "Very High Growth Rate Chemical Vapor Deposition of Single-Crystal Diamond" Proceedings of the National Academy of the Sciences, October 1, 2002, volume 99, No. 20, pages 12523-12525, which is incorporated in this description by reference in full. Diamond obtained by the above described methods and devices will be fairly large, not containing defects and translucent, so that it was applicable as Windows when it is used in high power lasers or as anvils in the device is high-pressure.

As this invention may be implemented in several forms without departing from the essence or its main characteristics, it should also be understood that the above described implementations of the invention are not limited by any details of the above description, unless otherwise stated, and which should be interpreted broadly within the entity, and volume defined in the attached claims, and therefore mean that all changes and modifications that fall within the boundaries and scope of the claims or the equivalent of the boundaries and the scope of the claims, therefore, included in the accompanying claims.

1. Apparatus for forming a diamond in the chamber for deposition containing a heat holder for holding a diamond and for making thermal contact with a side surface of the diamond adjacent to the edge of the growth surface of the diamond, the contactless device temperature measurement located with the possibility of measuring the temperature of the diamond from edge to edge of the growth surface of the diamond and the main device control process for receiving temperature measurements from the proximity device for measuring temperature and temperature control the growth surface so that all temperature gradients from the edge to the edge of the growth surface were less than 20°C.

2. The device according to claim 1, in which the heat sink holder comprises a tubular part made of molybdenum.

3. The device according to claim 1, in which the heat sink holder is located in the platform and provides the transfer of thermal energy to the platform, installed in the chamber for deposition.

4. The device according to claim 3, in which the heat-removing the sample holder provides thermal contact with thermal mass, which transfers thermal energy to the platform.

5. The device according to claim 4, in which the diamond is held in heat the sample holder with screws, tightening thermal mass before contact with the holder.

6. The device according to claim 1, in which the diamond is set in a heat sink holder slidable.

7. The device according to claim 1, in which the diamond is set in a heat sink holder slidable and installed on the element of the actuator, which moves along an axis essentially perpendicular to the growth surface.

8. The device according to claim 7, in which the heat sink holder is placed on the element of the actuator, which moves along an axis essentially perpendicular to the growth surface to maintain the distance between the face of the growth surface of the diamond and the top face of the heat sink holder.

9. The device according to claim 1, in which the heat sink holder is placed on the element of the actuator slidable in thermal mass for receiving heat from the diamond.

10. The device according to claim 9, in which the diamond is set in a heat sink holder slidable, and is installed on the element of the actuator, which moves along an axis essentially perpendicular to the growth surface.

11. The device according to claim 9, in which thermal mass is installed on the platform in Cham is e for deposition.

12. The device according to claim 9, in which the element of the actuator moves along an axis essentially perpendicular to the growth surface to keep the distance between the face of the growth surface of the diamond and the top face of the heat sink holder.

13. The device according to claim 1, wherein the contactless device temperature measurement is an infrared pyrometer.

14. The device according to claim 1, in which the diamond is, basically, a single-crystal diamond.

15. The design of the sample holder for the formation of diamond containing a diamond heat sink holder engaged in thermal contact with a side surface of the diamond adjacent to the edge of the growth surface of the diamond, the diamond is mounted for sliding in a heat sink holder, a platform for receiving thermal energy from the heat sink holder and the element of the actuator is arranged to move along an axis essentially perpendicular to the growth surface, to change the location of the diamond heat sink holder.

16. The design indicated in paragraph 15, in which the heat sink holder made of molybdenum.

17. The design indicated in paragraph 15, in which the cooling of the sample holder provides thermal contact with thermal mass, which transfers thermal energy to the platform.

18. The design indicated in paragraph 15, in which warm the outlet holder is placed on the element of the actuator, which moves along an axis essentially perpendicular to the growth surface, to maintain the distance between the face of the growth surface of the diamond and the top face of the heat sink holder.

19. The design of the sample holder for the formation of diamond containing a diamond heat sink holder engaged in thermal contact with a side surface of the diamond adjacent to the edge of the growth surface of the diamond thermal mass for receiving thermal energy from the heat sink holder, while the diamond is held in a heat sink holder under pressure, supplied through thermal mass, and a platform for receiving thermal energy from the heat of the holder through thermal mass.

20. Design according to claim 19, in which the pressure put by means of a screw.

21. Design according to claim 19, in which thermal mass is a collet.

22. Method of forming a diamond, comprising the following steps: placing the diamond in the holder so that was performed thermal contact with a side surface of the diamond adjacent to the growth surface of the diamond, measuring the temperature of the growth surface of the diamond to form the results of the temperature measurements, the temperature control growth surface-based temperature measurements and the growing single crystal and the MAZ using microwave plasma chemical vapour deposition on the growth surface, when the growth rate of the diamond is greater than 1 μm/h

23. The method according to item 22, in which the atmosphere contains hydrogen, 1-5% of nitrogen per unit of hydrogen and 6-12% of methane per unit of hydrogen.

24. The method according to item 23, in which the atmosphere also contains 1-3% oxygen per unit of hydrogen.

25. The method according to paragraph 24, in which the growth temperature is 900-1400°C.

26. The method according to item 22, in which the atmosphere contains 3% of nitrogen per unit of hydrogen and 12% of methane per unit of hydrogen.

27. The method according to item 22, in which the pressure is 130-400 Torr.

28. The method according to item 22, in which the growth temperature is 1000 to 1400°C.

29. The method according to item 22, which further includes the steps: changing the position of the diamond in the holder after the stage of growth of diamond and again the growth of diamond by microwave plasma chemical vapour deposition on the growth surface.

30. The method according to item 22, which further includes the step of changing the position of the diamond in the holder during the growth of diamond.

31. The method according to item 22, which further includes the step of determining whether to change the position of the diamond in the holder.

32. The method according to item 22, which further includes the steps of determining whether a diamond is a preset thickness, and stop the growth of the diamond if the diamond has a preset thickness.

33. The method of forming the diamond shall include the placement of the diamond in the holder, measuring the temperature of the growth surface of the diamond to form a measurement of temperature, temperature regulation of the growth surface using the main unit process control using temperature measurements so that all temperature gradients from the edge to the edge of the growth surface were less than 20°With the growing diamond on the growth surface and changing the position of the diamond in the holder, the pressure is 130-400 Torr.

34. The method according to p which further includes the step of determining whether to change the position of the diamond in the holder.

35. The method according to p which further includes the steps of determining whether a diamond is a preset thickness and stopping of the growth of the diamond if the diamond has a preset thickness.

36. The method according to p, in which the atmosphere contains hydrogen, 1-5% of nitrogen per unit of hydrogen and 6-12% of methane per unit of hydrogen.

37. The method according to p, in which the diamond is, basically, a single-crystal diamond.

38. The method according to p, in which the growth temperature is 900-1400°C.

39. The method according to p, in which the atmosphere contains 3% of nitrogen per unit of hydrogen and 12% of methane per unit of hydrogen.

40. The method according to p, in which the temperature growth of diamond is 1000-1400°C.

41. The method according to p, in which the phase exp is farming diamond is repeated after changing the position of the diamond in the holder.

42. The method according to p in which the change of position of the diamond in the holder occurs during the stage of growth of the diamond.

43. The method according to p, in which the growth rate of diamond is higher than 1 μm/h and the diamond is a single crystal diamond.

44. Method of forming a diamond that includes the following steps: regulate the temperature of the growth surface of the diamond so that all temperature gradients from the edge to the edge of the growth surface was less than 20°and growing the single-crystal diamond by microwave plasma chemical vapour deposition on the growth surface at a growth temperature in the chamber for deposition having an atmosphere with a pressure of at least 130 Torr.

45. The method according to item 44, in which the atmosphere contains hydrogen, 1-5% of nitrogen per unit of hydrogen and 6-12% of methane per unit of hydrogen.

46. The method according to item 45, in which the atmosphere also contains 1-3% oxygen per unit of hydrogen.

47. The method according to item 46, in which the growth temperature is 900-1400°C.

48. The method according to item 45, in which the atmosphere contains 3% of nitrogen per unit of hydrogen and 12% of methane per unit of hydrogen.

49. The method according to item 44, in which the pressure is 130-400 Torr.

50. The method according to item 44, in which the growth temperature is 1000 to 1400°C.

51. The method according to item 44, which further includes the step of placing the seed diamond in erately.

52. The method according to § 51, which further includes the steps of changing the position of the diamond in the holder after the step of growing a single crystal diamond and repeating the step of growing single-crystal diamond.

53. The method according to § 51, which further includes the step of changing the position of monocrystalline diamond in the holder during the growing single-crystal diamond.

54. The method according to item 44, in which the rate of growth of monocrystalline diamond is from 1 to 150 μm/h

55. Method of forming a diamond comprising the following steps:

regulate the temperature of the growth surface of the diamond so that all temperature gradients from the edge to the edge of the growth surface was less than 20°and growing the single-crystal diamond by microwave plasma chemical vapor phase deposition on the growth surface at a temperature of 900-1400°C.

56. The method according to § 55, in which the atmosphere contains hydrogen, 1-5% of nitrogen per unit of hydrogen and 6-12% of methane per unit of hydrogen.

57. The method according to § 55, in which the atmosphere also contains 1-3% oxygen per unit of hydrogen.

58. The method according to p, in which the atmosphere contains 3% of nitrogen per unit of hydrogen and 12% of methane per unit of hydrogen.

59. The method according to § 55, in which the pressure of the atmosphere in which the growth of diamond is 130-car.

60. The method according to § 55, which further includes the step of placing the seed diamond in the holder.

61. The method according to p which further includes the steps of changing the position of the diamond in the holder after the step of growing a single crystal diamond and repeating the step of growing single-crystal diamond.

62. The method according to p which further includes the step of changing the position of monocrystalline diamond in the holder during the growing single-crystal diamond.

63. The method according to § 55, in which the rate of growth of monocrystalline diamond is from 1 to 150 μm/h



 

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FIELD: chemical industry; cutting tool industry; mechanical engineering; methods of the production of the artificial highly rigid materials.

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EFFECT: the invention ensures the improved quality and the increased sizes of the produced monocrystals, the decreased labor input of the production process.

2 cl, 2 ex

FIELD: treatment of diamonds.

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46 cl, 4 dwg, 1 ex

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31 cl, 4 dwg, 2 ex

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30 cl, 4 dwg, 1 ex

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32 cl, 8 dwg, 1 tbl, 4 ex

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36 cl, 10 dwg, 1 tbl, 4 ex

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32 cl, 8 dwg, 1 tbl, 4 ex

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36 cl, 10 dwg, 1 tbl, 4 ex

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36 cl, 10 dwg, 1 tbl, 4 ex

FIELD: semiconductor technology; production of microelectronic devices on the basis of substrates manufactured out of III-V groups chemical element nitride boules.

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FIELD: semiconductor technology; production of microelectronic devices on the basis of substrates manufactured out of III-V groups chemical element nitride boules.

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102 cl, 9 dwg

FIELD: semiconductor technology; production of microelectronic devices on the basis of substrates manufactured out of III-V groups chemical element nitride boules.

SUBSTANCE: the invention is pertaining to production of microelectronic devices on the basis of substrates manufactured out of III-V groups chemical element nitride boules and may be used in semiconductor engineering. Substance of the invention: the boule of III-V groups chemical element nitride may be manufactured by growing of the material of III-V groups the chemical element nitride on the corresponding crystal seed out of the same material of nitride of the chemical element of III-V of group by epitaxy from the vapor phase at the speed of the growth exceeding 20 micrometers per hour. The boule has the quality suitable for manufacture of microelectronic devices, its diameter makes more than 1 centimeter, the length exceeds 1 millimeter, defects density on the boule upper surface is less than 107 defects·cm-2.

EFFECT: the invention ensures manufacture of the microelectronic devices of good quality and above indicated parameters.

102 cl, 9 dwg

FIELD: manufacture of mono-crystalline materials and films, possibly used for making semiconductor materials suitable for solar cells, integrated circuit boards, solid-state SHF-devices.

SUBSTANCE: method comprises steps of using as material of substrates for growing films of GaAs (100) mono-crystals of intermetallic compounds made of one of binary alloys such as NiAl, CoAl, AlTi, NiGa.

EFFECT: possibility for growing mirror epitaxial films of GaAs in wider temperature range of deposition and over-saturation, simplified process for making devices of reduced cost.

3 cl

FIELD: infra-red optics; production of zinc selenide specimens more than 20 mm in thickness used as passive optic elements of high-power CO2 lasers and other equipment working in infra-red range of long waves.

SUBSTANCE: proposed method includes delivery of hydrogen selenide and zinc vapor by argon flow to substrates heated to temperature of 650-750 C and sedimentation of zinc selenide on them at total pressure of 0.5-1.3 kPa, equimolar flow rates of zinc and hydrogen selenide is equal to 0.4-0.47 l/min and that of argon of 3-4 l/min; temperature of substrates is increased at rate of 0.1-0.15 deg./h throughout the entire period of selenide sedimentation. Zinc selenide obtained by this method has size of grains of 30-80 mcm and possesses the property of absorption at wave length of CO2 not above 5.10-4 cm-1.

EFFECT: enhanced efficiency.

2 cl, 1 ex

The invention relates to the production of semiconductor materials and can be used for the production of the original polycrystalline silicon deposition on heated basics in the process of hydrogen restoration of CHLOROSILANES or from the gas phase monosilane

The invention relates to the production of semiconductor materials and can be used for the production of the original polycrystalline silicon deposition on a heated substrate (base) in the process of hydrogen restoration of CHLOROSILANES or from the gas phase monosilane

FIELD: infra-red optics; production of zinc selenide specimens more than 20 mm in thickness used as passive optic elements of high-power CO2 lasers and other equipment working in infra-red range of long waves.

SUBSTANCE: proposed method includes delivery of hydrogen selenide and zinc vapor by argon flow to substrates heated to temperature of 650-750 C and sedimentation of zinc selenide on them at total pressure of 0.5-1.3 kPa, equimolar flow rates of zinc and hydrogen selenide is equal to 0.4-0.47 l/min and that of argon of 3-4 l/min; temperature of substrates is increased at rate of 0.1-0.15 deg./h throughout the entire period of selenide sedimentation. Zinc selenide obtained by this method has size of grains of 30-80 mcm and possesses the property of absorption at wave length of CO2 not above 5.10-4 cm-1.

EFFECT: enhanced efficiency.

2 cl, 1 ex

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