Method for binding of diamond single crystal with metal

FIELD: technological processes.

SUBSTANCE: invention may be used for creation of different single crystal processing tools, medical tools, for creation of electric contacts with metal on the surface of semiconductor and other diamonds. Preliminarily surface of diamond single crystal is polished to 5th class of roughness (according to state standard GOST 2789-73) and degreased. Degreased surface of diamond single crystal is coated with intermediate layer with thickness of 0.05÷0.4 mm from mixture of nanodispersed powders of ferric oxides with size of particles of 20÷40 nm and fullerene C60. Ratio of ferrous oxides content to fullerene C60 makes 10-50:90-50 wt %. Then place of contact is exposed to pressure of 2.0÷5.0 GPa and simultaneously to shift effect by rotation at the angle of 100÷1000 degrees.

EFFECT: higher strength and quality of diamond single crystal binding to metal.

3 cl, 3 ex

 

The invention relates to the field connection of dissimilar materials, in particular to the connection of the single crystal diamond with metals, and can be used to create a different kind of chip machining tool, for example incisors; medical instrument, such as dental, surgical; to create on the surface of the semiconductor diamonds and other electrical contacts.

Currently, to create a diamond-based composites metal-diamond widely used method of connection of a diamond with metal using an intermediate layer or solder exposure to high temperatures and high pressures; and there are ways to create ohmic contacts to diamond-metal, in which the surface of the diamond is subjected to special processing to create the intermediate layer.

A method of obtaining a layered product for cutting tools (ed. the certificate of the USSR No. 814987, class SW 35/71, WV 15/00, SS 29/00, publ. 23.03.81), according to which the coated article includes a substrate made from a powder of transition metals and transition metal diborides IV-VII groups, with a particle size of 0.1-10 μm in the ratio of 7:3-3:7 and superhard layer made from a powder of at least one superhard material group: diamond, cubic boron nitride is coy or wurtzite modifications and superhard layer additionally contains a mixture with the following ratio of components,% by weight:

the mixture of transition metal diborides IV-VII groups0,5-50
superhard material50-95,5

Ingredients pre-crushed in a ball mill or vibrating mill with carbide balls for one or more hours to the desired grain size and pressed products in layers, thoroughly dried at a temperature of 60-200°and placed into a high pressure chamber, where it is exposed to high pressure 35-100 kbar and temperature 1200-2600°C for 0.5 to 5 minutes. The result is high-quality polycrystalline single-layer, bilayer, and multilayer products. The disadvantage of this method is the need to use heavy forging equipment. He is energy and resource intensive. This method cannot be applied for point contacts.

Known solid solder and a soldering method of diamond on a metal substrate using this solder (U.S. Pat. U.S. No. 6889890, class VC 31/02, publication 18.06.06, priority 10.02.02). The main components of the solder used gold or silver and copper. The solder further contains 0.001 to 5% vanadium, preferably not more than 2%. In the process p is s is directed solidification of the solder side of the diamond on the surface of the connection of the diamond to the substrate, to form a carbide of vanadium, which improves the connection soldered connection. The solder can improve the bonding strength of the diamond to the substrate, prevents corrosion of solder joints and improves the appearance of the brazed product. However, the use as components solder gold and silver considerably increases the cost of this method.

A known method of manufacturing electrical contacts on the diamond (U.S. Pat. USA 4511783, class U.S. 219/121 .85; 219/121 .8; publication 16.04.1985, priority 03.02.1983), in which the surface layer of the diamond with a laser beam is transformed into graphite with surface resistance 5-100 Ohms. This laser operates at this frequency and duration of pulses, and the laser beam is focused and moving across the diamond so that the formed recesses merge or overlap. After the graphitization wire or conductor of electricity is fixed on the graphite layer, forming, thus, the electrical contact. The disadvantage of this method is the use of rather expensive laser equipment, the need to specifically focus and adjust the laser.

A known method of creating electrical contacts on diamond substrates (U.S. Pat. USA 5002899, class U.S. 438/105; 117/3; 257/77; 437/173, 175, 180, 187, publishing 26.03.1991, priority 22.03.1990), which includes radiation treatment of the diamond substrate by radiation with long ox is s in the range of 193 nm, when this area with improved electrical conductivity can be formed without subsequent heating of the substrate surface. Then, the metal film can be attached to the place treated with radiation with the formation of an ohmic contact or a contact type of Schottky. The field with anisotropic conductivity can be used for polarizing optical devices. The disadvantage of this method is the use of the radiation source.

A method of obtaining ohmic contacts on semiconducting diamond (U.S. patent 5055424, class U.S. 438/105; 437/192-195, 188, publication 08.10.1991. priority 29.06.1989), including deposition carbidopa metal and then corrosion-resistant metal to the surface by precipitation from the gas phase, and subsequent heating in an inert atmosphere to a temperature of 350-1200°C. And carbidopazapomnit metal chosen from the group of tungsten, molybdenum, chromium, vanadium, niobium, tantalum, titanium, Nickel, cobalt, iron, manganese, aluminum, silicon, boron, zirconium and hafnium, and the corrosion resistant metal is chosen from the group of gold, platinum, palladium, iridium, silver, copper, Nickel and chromium. In some applications, the intermediate metal precipitated on the surface carbidopa metal, this metal is chosen from the group of tungsten, molybdenum, chromium, vanadium, niobium, tantalum, titanium, nick is l, cobalt, iron, manganese, aluminum, silicon, boron, zirconium, and hafnium, gold, platinum, palladium, iridium, silver, and copper. The disadvantage of this method is the use for the deposition of metals by the method of deposition from the gas phase, involving special training machined surfaces, vacuuming, use special masks for the formation of the contact area.

A method of obtaining metal-boride ohmic contact on the surface of the semiconductor diamond (U.S. patent 5382808, class U.S. 257/77; 257/607; 257/742; 257/77, 607, 734, 741, 748, 763, 764, 770, publication 17.01.1995, priority 14.05.1993). Bored metal consists of boron and a transition metal, preferably of refractory. The heating layer boride metal and diamond leads to diffusion of boron and education vysokoduhovnoy boron surface of the semiconductor diamond. An alternative method of obtaining vysokoduhovnoy area can be selective ion implantation, annealing for formation of graphitized surface area and the removal of the graphitized surface area by etching. Vysokopetrovsky surface area reduces the electrical contact resistance. Additionally, by heating can be created intermediate surface layer of carbide. Intermediate carbide region increases the adhesion of boride m is metal, and also reduces the electrical resistance of the contact. The disadvantages of this method include the necessity of applying boride metal on the surface of the diamond one of the following methods: sputtering, evaporation, chemical vapor deposition or molecular beam epitaxy.

Known way to create ohmic contacts on diamond n-type conductivity, or the introduction of contact to the diamond with p-type conductivity (US patent 6140148, class U.S. 438/105; 257/22; 257/77; 427/523; 438/931, publication 31.10.2000, priority 18.12.1997). The method includes the implantation of the diamond surface alloying of n-type atoms at doses slightly lower than the rate of amorphization of the diamond, with the aim of creating implanted region below the surface and extending inward from the surface, subsequent annealing to create opportunities as electrons in the diamond case, diamond n-type and create opportunities injection box electrons in the diamond case, diamond p-type, and metallization, at least part of the surface through which the injection of electrons. Moreover, alloying elements taken from a number of: phosphorus, arsenic, antimony, oxygen, fluorine and nitrogen. The disadvantages of this method include the need to stage implantation.

The closest technical solution to the claimed is solder for connection of single crystals is of Laza with metal (U.S. Pat of the Russian Federation No. 2270743, class VC 35/28, UK 35/30, priority 14.02.02, publ. 27.08.03), according to which the solder contains silver, copper, tin, titanium, titanium carbide and silicon carbide, in the following ratio, wt.%:

copper14.4V-18,4
tin14.4V-18,4
titanium14.4V-18,4
the titanium carbideof 4.5 to 15.6
silicon carbide0,3-0,7
silver38,0-43,0

when the ratio of silver, copper, tin and titanium 3,1:1,2:1,2:1,2.

For the communication of diamond single crystals with metal was preparing a mixture of powders of silver, copper, tin and titanium, with subsequent addition of carbides of titanium and silicon. Source powders of metals and carbides used 99.5%purity. Soldering was carried out in vacuum conditions (10-3mm Hg) or inert atmosphere (argon) at a temperature of 1050-1150°C. the Solder used for the manufacture of chip tool in the form of drills of steel grade P6. The properties of the solder and the bonding strength of the single crystal diamond material of the drill was determined by operating characteristics, namely the total length drilled holes in crystalline quartz for drills with a diameter of 0.4-0.5 mm, in particular at high work is her temperature (700° C). Used solder provides greater mechanical strength of the single-crystal diamond faction 500/400 with steel material and high performance made drills. The disadvantage of this technical solution is the need to conduct brazing under vacuum and apply a sufficiently high temperature that may adversely when soldering on the diamonds with special properties (e.g., semiconductor).

The objective of the proposed technical solution is to eliminate the above shortcomings and enhancing the technical capacity due to the formation on the surface of the diamond intermediate transition layer, which has high mechanical properties and forms a durable and high-quality connection of the single crystal diamond with metal.

This technical result is achieved in the following way. On the surface of the diamond monocrystal in addition put intermediate layer of a mixture of nano-dispersed powders of oxides selected from the range: Fe3O4, Fe2O3, FeO, or a mixture thereof with a particle size of 20-40 nm and fullerene C60. The content ratio of iron oxide to the fullerene C60is, wt.% 10-50:90-50. The surface of the diamond monocrystal pre-polished to a 5-grade roughness (according to GOST 2789-73) and degreased, for example, is using serial processing in acetone and alcohol. On the fat surface, apply an intermediate layer of a thickness of 0.05-0.4 mm, and then the contact of the diamond single crystal intermediate layer is exposed to pressure of 2.0 to 5.0 GPA and at the same time the shear deformation of the rotation angle 100-1000 degrees. A feature of this method is the lack of thermal treatment at the site of contact of the diamond single crystal and an intermediate layer that allows you to save properties of single crystal diamond, for example, doped or semiconductor.

An intermediate layer of specified composition, applied as described, has a high mechanical strength, and promotes a strong connection to diamond due to the fact that during the pressure and shear strain is the interaction of fullerene and nanodispersed oxides of iron with diamond on the surface roughness of the diamond that make it a pre-polished to a 5-grade roughness (according to GOST 2789-73). Degreasing and grinding the surface of the diamond monocrystal provide better passage of the mechano-chemical reaction (nano-particles) remaining after the grinding surface irregularities.

Diamond coated with an intermediate layer connected to the metal by soldering with the corresponding solder or welding, for example laser or ultraslo the updates.

Fullerene is used as a component of the transition layer, because it is part of the proposed composition when exposed to high pressure and shear deformation becomes Almazny carbon, forming the desired intermediate layer having high mechanical properties, and is firmly connected with diamond. It is known that fullerene under the influence of high pressures and temperatures is polymerized with the formation of the highly rigid, and other superhard phases, for example, as in the following example and the links. Known for superhard materials obtained in the following way (RF patent 2078033, class SW 31/00, SW 31/06, priority 16.11.1994, publ. 27.04.1997): in the high pressure chamber of the type Bridgman anvil" or "toroid" put a portion of the fullerene C60. Impact pressure 5-12 GPA at t=200-350°C. Receive a polymorphic compound of carbon with interplanar distances, Å: 7,760±10; 6,00±30; 4,790±05; 4,580±05; 4,130±05; 3,710±10; 3,240±10; 2,900±10; 2,490±10; 2,490±10; 2,200±10 that leaves scratches on the surface of boron nitride and diamond.

A mixture of iron oxides and fullerene, and the use of shear deformation, reduces the parameters to obtain the highly rigid phases, which form the intermediate layer, in particular a pressure up to values of 2.0 to 5.0 GPA and temperatures up to on the th (about 20° C). The iron oxides are taking in the form of nanosized powder with a particle size in the range of 20-40 nm, which also reduces the exposure parameters (the magnitude of pressure and the degree of shear deformation).

The composition of the intermediate layer, in which the ratio of iron oxide content to the fullerene C60is the mass percent of 10-50:90-50, determined experimentally and ensures the creation of the intermediate layer with the desired properties. When the content of the fullerene less than 50 wt.% not the formation of solid intermediate layer. When the content of the fullerene more than 90 wt.% the reaction of formation of non-diamond carbon is not fully and, in addition, reduced iron content impairs the ability of the intermediate layer to form a soldered connection.

The thickness of the intermediate layer is 0.05-0.4 mm was determined experimentally. When the layer thickness of more than 0.4 mm when exposed to high pressure and shear deformation occurs "leakage" component of the intermediate layer from the contact areas. Reduce the layer to a thickness less than 0.05 mm complicates the process of applying the intermediate layer.

We offer pressure and angles of shear deformation (pressure of 2.0 to 5.0 GPA, the rotation angle of 100-1000 degrees) determined experimentally for selected compositions of the intermediate layer, and the lower the pressure, the more to the wives to be applied angle shear strain.

Diamond is the so-called wide-gap semiconductor with a band gap of 5.4 eV, is higher than silicon, germanium, gallium arsenide and other semiconductors, the breakdown voltage, the cutoff frequency (cutoff frequency), the maximum operating voltage. Unlike the most common semiconductor diamond is resistant to temperatures up to 600°and radiation. Its thermal conductivity is the highest of all known substances. All this makes the diamond are promising for the development of electronic devices of new generation.

Example 1.

Prepare a mix of original powders of fullerene C60and iron oxide Fe3About4with a particle size of 20-40 nm in the ratio of iron oxide to the fullerene 10:90 wt.%, carry out the mixing in a planetary mill for 10 minutes. The mixture is applied with a layer of 0.05 mm on the pre-polished to a 5-grade roughness (according to GOST-2789-73), peeled and fat sequential treatment with acetone and alcohol to the surface of the diamond, then applied pressure of 2.0 GPA core made of hard alloy and at the same time spend shear deformation by the rotation of the rod at an angle 1000°. The contact area of the intermediate layer on the single crystal diamond is about 1 mm2further, the connection of the single crystal diamond with metal (metal case and is the instrument) is carried out by soldering the solder SGP-25. Such a single crystal diamond is used for the manufacture of the diamond scalpel.

Example 2.

Prepare a mix of original powders of fullerene C60and iron oxide FeO with a particle size of 20-40 nm in the ratio of iron oxide to the fullerene 50:50 wt.%, carry out the mixing in a planetary mill for 10 minutes. The mixture is applied with a layer of 0.4 mm on the pre-polished to a 5-grade roughness (according to GOST-2789-73), peeled and fat sequential processing in acetone and alcohol, the surface of the diamond single crystal, then applied a pressure of 5.0 GPA rod made of hard alloy and at the same time spend shear deformation by the rotation of the rod at an angle 100°. The contact area of the intermediate layer and the single crystal diamond is about 0.1 mm2. In a similar way to create the same intermediate layer on the other surface of the same single crystal diamond. Further connection of the received contact with current-carrying copper conductors with a diameter of ≤0.1 mm by ultrasonic welding using an ultrasonic welding machine USSM 1-1,0/22. The obtained single crystal diamond with attached copper conductors is used as a thermistor.

Example 3.

Prepare a mix of original powders of fullerene C60and a mixture of iron oxide and 10 wt.% FeO+90 wt.% Fe2O3with size h is IC 20÷ 40 nm in the ratio of the oxides to the fullerene 25:75 wt.%, carry out the mixing in a planetary mill for 10 minutes, put it with a layer of 0.3 mm on a previously polished to a 5-grade roughness (according to GOST-2789-73), peeled and fat sequential processing in acetone and alcohol the surface of the diamond, then applied pressure of 3.5 GPA rod made of hard alloy and at the same time spend shear deformation by the rotation of the rod at an angle 500°. Further connection of the single crystal diamond with metal carried out as follows. Applied on the formed intermediate layer the next layer with thickness of 0.1 mm of copper powder with particle sizes in the range of 1-10 μm, the applied pressure of 0.5 GPA rod made of hard alloy and at the same time spend shear deformation by the rotation of the rod at an angle 500°. The obtained single crystal diamond with the intermediate layer and the second copper layer is used as a heat sink substrate for semiconductor devices. Connection heat the substrate to conduct heat sink by soldering the solder alloys with high conductivity, such as POS-10, POS 30, POS 61M.

The proposed method of connection of the single-crystal diamond with metal can be used to create a different kind of chip machining tool, for example, cutters; medical instrument is, for example, dental and surgical; to create on the surface of the semiconductor and other diamond electrical contact with the metal.

1. The connection method of the single crystal diamond with metal, characterized in that on the surface of the diamond put intermediate layer with a thickness of 0.05-0.4 mm, which is prepared from a mixture of nanosized iron oxide powder with a particle size of 20-40 nm and fullerene C60when the ratio of iron oxide and fullerene C60(10-50):(90-50) wt.%, the surface of the diamond monocrystal pre-polished and degreased, the contact of the single crystal diamond coated intermediate layer is exposed to pressure of 2.0 to 5.0 GPA and simultaneous shear effects rotation angle 100-1000°and the connection of the single crystal diamond with the surface of the metal is carried out by soldering or ultrasonic welding.

2. The method according to claim 1, characterized in that the iron oxide take Fe3O4and/or Fe2About3and/or FeO.

3. The method according to claim 1, characterized in that the surface of the diamond is polished to a 5-grade roughness (according to GOST-2789-73), and the degreasing is carried out in acetone and alcohol.



 

Same patents:

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EFFECT: lowered metal consumption due to using one frame of apparatus and simplified system for pressure transfer.

3 cl, 2 dwg

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