CN110639432B - Square flaky diamond large single crystal and preparation equipment and preparation method thereof - Google Patents
Square flaky diamond large single crystal and preparation equipment and preparation method thereof Download PDFInfo
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- CN110639432B CN110639432B CN201910869215.XA CN201910869215A CN110639432B CN 110639432 B CN110639432 B CN 110639432B CN 201910869215 A CN201910869215 A CN 201910869215A CN 110639432 B CN110639432 B CN 110639432B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/065—Presses for the formation of diamonds or boronitrides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
Abstract
The invention discloses a square sheet diamond large single crystal and a preparation device and a preparation method thereof, wherein the preparation device is a large-cavity press, a heat insulation pipe, a heating pipe and an insulation pipe are sleeved in a growth cavity of the large-cavity press from outside to inside, a carbon source, a catalyst and a crystal bed containing crystal seeds are stacked in the cavity of the insulation pipe from top to bottom, the growth cavity is a cavity with a square cross section, the heat insulation pipe, the heating pipe and the insulation pipe are all square pipes, the carbon source, the catalyst and the crystal bed are all square sheets, and the crystal seeds are square diamond crystal sheets. The preparation method adopts the preparation equipment for the square flaky diamond large single crystal to prepare the square flaky diamond large single crystal, and the pressure range and the temperature range in the growth cavity are controlled to be 5-10 GPa and 1200-2000 ℃. The square sheet diamond large single crystal is prepared by the preparation method of the square sheet diamond large single crystal. When the square seed crystal is used, a high-quality large single crystal of square plate-like diamond can be obtained.
Description
Technical Field
The invention belongs to the field of high-temperature and high-pressure technology and superhard materials, and particularly relates to a square flaky diamond large single crystal and preparation equipment and a preparation method thereof.
Background
The growth of the large diamond single crystal at high temperature and high pressure generally adopts a temperature difference method (seed crystal method), the core structure of the method comprises diamond single crystal seed crystals, a catalyst and a carbon source, the growth pressure and temperature are generally above 5GPa and 1200 ℃, the catalyst metal or alloy is in a molten state, the temperature of the carbon source position is slightly higher than that of the seed crystal position through the structural design of a cavity, and the temperature difference between the carbon source and the seed crystals becomes the driving force for the continuous growth of the seed crystals.
The shape of a diamond single crystal grown under high temperature and high pressure is generally a 6-8 plane body composed of a (100) plane and a (111) plane. When the (100) plane is used as the seed surface, the grown crystal generally takes a sheet-like square shape if grown at a lower temperature; the grown crystals generally exhibit a tower shape if grown at higher temperatures. Therefore, it is generally necessary to use (100) seed crystals when growing plate-like square crystals, and it is necessary to control the growth temperature in a lower range.
A large-cavity press is generally used for preparing large diamond single crystals, wherein a pressure transmission medium commonly used on a cubic block of pyrophyllite is arranged on a cubic block of cubic block, the central part of the cubic block of pyrophyllite contains a circular through hole, and the internal space of the circular through hole is generally called as a growth cavity. The pressure transmission medium commonly used on the two-sided jacking machine is cylindrical, the central part of the pressure transmission medium contains a circular through hole, and the inner space of the circular through hole is also generally called as a growth cavity.
The growth cavity generally contains a heat insulation pipe, a heating pipe, an insulation pipe, a crystal bed, a catalyst and a carbon source, and the shape of the material in the growth cavity is matched with the shape of a circular inner hole of a pressure transmission medium, and is generally in a circular pipe or a circular disc shape. The temperature field distribution inside the cylindrical growth cavity has an axisymmetric characteristic, namely, the inside isotherms are concentric when observed from the upper and lower axial directions. If the square seed crystal is used in the cylindrical growth cavity, especially the larger size seed crystal, because the temperature of the seed crystal is different at different positions, for example, the temperature of the four corners of the seed crystal is greatly different from the temperature of the central point of the four sides, certain parts of the seed crystal preferentially grow and certain parts do not grow, as a result, the uniform growth of the whole seed crystal surface is difficult to realize, catalyst inclusions are easily generated in the grown single crystal, and a large amount of polycrystalline can be grown under more serious conditions.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a large square sheet diamond monocrystal capable of avoiding generation of catalyst inclusion and a large amount of polycrystals when a square seed crystal is used, and a preparation device and a preparation method thereof.
The invention provides equipment for preparing a square sheet-shaped diamond large single crystal, which is a large-cavity press, wherein a heat insulation pipe, a heating pipe and an insulation pipe are sleeved in a growth cavity of the large-cavity press from outside to inside, and a carbon source, a catalyst and a crystal bed containing crystal seeds are stacked in a cavity of the insulation pipe from top to bottom, wherein the growth cavity is a cavity with a square cross section, the heat insulation pipe, the heating pipe and the insulation pipe are all square pipes, the carbon source, the catalyst and the crystal bed are all square sheets, and the crystal seeds are square diamond crystal sheets.
According to one embodiment of the apparatus for producing a large single crystal of square plate-shaped diamond of the present invention, the large-chamber press is a double-side press, a cubic press or a divided ball press.
According to one embodiment of the manufacturing equipment of the square sheet diamond large single crystal, the material of the heating pipe is one or more of graphite material, mixed material of graphite and sodium chloride, mixed material of graphite and ceramic material, metal material and lanthanum chromate material, wherein the ceramic material is magnesium oxide, zirconium oxide or aluminum oxide.
According to one embodiment of the apparatus for producing a large single crystal of diamond in a square plate shape of the present invention, the material of the heat insulating tube is one or more of magnesia, zirconia, alumina, pyrophyllite and dolomite.
According to one embodiment of the apparatus for producing a large single crystal of square plate-shaped diamond according to the present invention, the material of the insulating tube is one or more of magnesium oxide, zirconium oxide, aluminum oxide, and sodium chloride.
According to one embodiment of the apparatus for producing a large single crystal of square plate-shaped diamond of the present invention, the catalyst is made of metallic iron, metallic nickel, metallic cobalt, and a binary or ternary alloy containing two or three of iron, cobalt, and nickel.
According to one embodiment of the apparatus for producing a large single crystal of square plate-shaped diamond of the present invention, the carbon source is one or more of graphite, diamond, and graphene.
According to one embodiment of the apparatus for producing a large single crystal of square plate-shaped diamond of the present invention, the material of the seed bed is one or more of magnesium oxide, zirconium oxide, aluminum oxide and sodium chloride, the seed crystal is a diamond single crystal grown by a high temperature and high pressure method or a CVD method, the side length of the seed crystal is 0.1 mm to 10 cm, and the number of seed crystals to be set is 1 or more.
The invention also provides a preparation method of the square sheet diamond large single crystal, which is characterized in that the preparation equipment of the square sheet diamond large single crystal is adopted to prepare the square sheet diamond large single crystal, wherein the pressure range in the growth cavity is controlled to be 5-10 GPa, and the temperature range is controlled to be 1200-2000 ℃.
In another aspect, the invention provides a large square sheet diamond monocrystal, which is prepared by the preparation method of the large square sheet diamond monocrystal, wherein the size of the large square sheet diamond monocrystal is 1 mm-10 cm, most of the surface of the large square sheet diamond monocrystal is a (100) crystal face, and the small part of the surface of the large square sheet diamond monocrystal is a (111) crystal face.
When the apparatus and method of the present invention are used, since the isotherm inside the square cross-section growth chamber is square, when the square seed crystal is used, the temperature of the growth front edge of the seed crystal is substantially the same, for example, the temperature of the four corners of the seed crystal is substantially the same as the temperature of the central point of the four sides, and thus it is easier to grow a single crystal and it is not easy to generate a catalyst inclusion inside the grown crystal, and a high quality square plate-shaped diamond large single crystal can be obtained.
Drawings
Fig. 1 shows a schematic structural diagram of a pressure transfer medium in a large-cavity press in the prior art, wherein a cylindrical growth cavity is arranged in the middle of the press.
Fig. 2 a to c are schematic views showing the structures of a cylindrical adiabatic tube, a cylindrical heating tube and a cylindrical adiabatic tube, respectively, in the related art.
Fig. 3 a to c respectively show the structure of a circular carbon source, a circular catalyst and a circular crystal bed in the prior art, wherein the circular crystal bed contains square crystal pieces.
Figure 4a shows an isotherm profile of the interior of a prior art cylindrical growth chamber and figure 4b shows a schematic of crystal growth within a prior art cylindrical growth chamber.
Fig. 5 is a schematic view showing the structure of a pressure medium in a large-chamber press in the apparatus for producing a large single crystal of square plate-like diamond according to the exemplary embodiment of the present invention, in which a growth chamber having a square cross section is formed in the middle.
Fig. 6 a to c are schematic structural views showing a square heat insulating tube, a square heating tube, and a square insulating tube in a square diamond large single crystal according to an exemplary embodiment of the present invention, respectively.
Fig. 7 a to c are schematic structural diagrams illustrating a square carbon source, a square catalyst and a square seed bed in a large single crystal of square plate-shaped diamond according to an exemplary embodiment of the present invention, respectively, wherein the square seed bed contains square plate-shaped diamond.
Fig. 8a shows an isotherm distribution diagram inside a square cross-section growth cavity in a large single crystal of a square plate diamond according to an exemplary embodiment of the present invention, and fig. 8b shows a crystal growth diagram inside a square cross-section growth cavity in a large single crystal of a square plate diamond according to an exemplary embodiment of the present invention.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
Fig. 1 shows a schematic structural diagram of a pressure transfer medium in a large-cavity press in the prior art, wherein a cylindrical growth cavity is arranged in the middle of the pressure transfer medium, fig. 2 shows schematic structural diagrams of a cylindrical heat insulation pipe, a cylindrical heating pipe and a cylindrical insulation pipe in the prior art respectively, and fig. 3 shows schematic structural diagrams of a circular carbon source, a circular catalyst and a circular crystal bed in the prior art respectively, wherein the circular crystal bed contains square crystal pieces. Figure 4a shows an isotherm profile of the interior of a prior art cylindrical growth chamber and figure 4b shows a schematic of crystal growth within a prior art cylindrical growth chamber.
As shown in fig. 1 to 4b, the isotherms (dotted lines) inside the cylindrical growth chamber are concentric, and when a square seed crystal sheet, especially a large-sized seed crystal sheet, is used in the cylindrical growth chamber, the temperatures at different positions of the seed crystal sheet are different, for example, the temperatures (Ta) at the four corners of the seed crystal sheet and the temperature (Tb) at the central points of the four sides are greatly different. Because the temperature of the surface of the seed crystal is not uniform, certain parts of the seed crystal preferentially grow and certain parts of the seed crystal may not grow, and as a result, the whole seed crystal surface is difficult to realize uniform growth, catalyst inclusion is more easily generated in the growing single crystal, and a large amount of polycrystal is generated in a serious case.
Based on the above, the invention provides equipment and a method for manufacturing the square sheet diamond large single crystal. The following description will first be made with reference to the drawings.
Fig. 5 is a schematic view showing the structure of a pressure medium in a large-chamber press in the apparatus for producing a large single crystal of square plate-like diamond according to the exemplary embodiment of the present invention, in which a growth chamber having a square cross section is formed in the middle. Fig. 6 a to c are schematic structural views showing a square heat insulating tube, a square heating tube, and a square insulating tube in a square diamond large single crystal according to an exemplary embodiment of the present invention, respectively. Fig. 7 a to c are schematic structural diagrams illustrating a square carbon source, a square catalyst and a square seed bed in a large single crystal of square plate-shaped diamond according to an exemplary embodiment of the present invention, respectively, wherein the square seed bed contains square plate-shaped diamond.
As shown in fig. 5 to 7, according to an exemplary embodiment of the present invention, the preparation apparatus is a large-chamber press, and a heat insulating pipe, a heating pipe and an insulating pipe are sleeved inside a growth chamber of the large-chamber press from outside to inside and a carbon source, a catalyst and a crystal bed containing a seed crystal are stacked inside a cavity of the insulating pipe from top to bottom. The growth cavity is a cavity with a square cross section, the heat insulation pipe, the heating pipe and the insulation pipe are square pipes, the carbon source, the catalyst and the crystal bed are square pieces, and the seed crystal is a square diamond crystal piece.
Specifically, the large-cavity press adopted by the invention can be a double-faced press, a cubic press or a split ball press, and the growth cavity is positioned in the central part of the pressure transmission medium.
The material of the heating tube in the invention can be one or more of graphite material, mixed material of graphite and sodium chloride, mixed material of graphite and ceramic material, metal material and lanthanum chromate material, wherein the ceramic material is magnesia, zirconia or alumina. That is, the heating tube may be made of a conventionally used conductive material.
The material of the heat insulation pipe can be one or more of common heat insulation materials such as magnesia, zirconia, alumina, pyrophyllite and dolomite, the material of the heat insulation pipe can be one or more of common heat insulation materials such as magnesia, zirconia, alumina and sodium chloride, and the material of the catalyst can be metallic iron, metallic nickel, metallic cobalt and binary or ternary alloy containing two or three of iron, cobalt and nickel. In addition, the catalyst is added with nitrogen removing agent such as aluminum, titanium and the like to grow IIa type diamond single crystal.
The carbon source in the invention can be one or more of pure carbon materials such as graphite, diamond, graphene and the like, and the material of the crystal bed can be one or more of common insulating materials such as magnesium oxide, zirconium oxide, aluminum oxide, sodium chloride and the like. The seed crystal is preferably a diamond single crystal grown by a high-temperature high-pressure method or a CVD method, the side length of the seed crystal is 0.1 millimeter-10 centimeters, and the set number of the seed crystals is more than or equal to 1.
The shape of the diamond single crystal grown under high temperature and high pressure is generally 6 to 8 hedrons consisting of a (100) plane and a (111) plane. Using the (100) plane as a seed plane, the grown crystal generally takes the form of a sheet square if grown at a lower temperature; the grown crystals generally exhibit a tower shape if grown at higher temperatures. Therefore, the present invention grows the flaky square crystal, generally requires the use of (100) seed crystals, and requires the control of the growth temperature in a lower range.
Fig. 8a shows an isotherm distribution diagram inside a square cross-section growth cavity in a large single crystal of a square plate diamond according to an exemplary embodiment of the present invention, and fig. 8b shows a crystal growth diagram inside a square cross-section growth cavity in a large single crystal of a square plate diamond according to an exemplary embodiment of the present invention.
As shown in fig. 8a and 8b, the isotherm inside the square growth chamber is square, and when the square seed crystal is used, the temperature of the growth front of the seed crystal piece is substantially the same, for example, the temperature (Ta) of the four corners of the seed crystal piece is substantially the same as the temperature (Tb) of the center point of the four sides. Therefore, the temperature field in the growth cavity with the square cross section is more suitable for the growth of the square flaky crystal, the catalyst inclusion is not easy to generate in the grown crystal, and the purity of the grown diamond single crystal is better and the practical value is higher.
The invention also provides a preparation method of the square sheet diamond large single crystal, which is characterized in that the preparation equipment of the square sheet diamond large single crystal is adopted to prepare the square sheet diamond large single crystal, wherein the pressure range in the growth cavity is controlled to be 5-10 GPa, and the temperature range is controlled to be 1200-2000 ℃. Therefore, the square sheet diamond large single crystal which meets the requirement can be prepared.
The large square sheet diamond single crystal is prepared by the preparation method of the large square sheet diamond single crystal, the size of the large square sheet diamond single crystal is 1 mm-10 cm, most of the surface of the large square sheet diamond single crystal is a (100) crystal face, and the small part of the surface of the large square sheet diamond single crystal is a (111) crystal face.
The present invention will be further described with reference to the following specific examples.
TABLE 1 Experimental parameters and preparation results for examples 1-3 and comparative examples 4-5
| Examples | Shape of cavity | Catalyst for the preparation of a catalyst | Temperature (C) | Seed crystal (mm) | Time (hr) | Growing crystal (mm) |
| 1 | Square shape | Iron-nickel alloy (50:50) | 1250 | 0.5x0.5 | 20 | Single crystal 2x1.5 |
| 2 | Square shape | Iron-nickel alloy (80:20) | 1300 | 3x3 | 50 | Single crystal 6x6x2 |
| 3 | Square shape | Iron-cobalt-nickel alloy (60:20:20) | 1300 | 5x5 | 120 | Single crystal 10x10x2 |
| Comparative example | Shape of cavity | Catalyst for the preparation of a catalyst | Temperature (C) | Seed crystal (mm) | Time (hr) | Growing crystal (mm) |
| 4 | Circular shape | Iron-nickel alloy (50:50) | 1250 | 0.5x0.5 | 20 | Single crystal (with inclusion) |
| 5 | Circular shape | Iron-nickel alloy (80:20) | 1300 | 3x3 | 50 | Polycrystalline |
| 6 | Circular shape | Iron-cobalt-nickel alloy (60:20:20) | 1300 | 5x5 | 120 | Polycrystalline |
Table 1 shows experimental parameters and preparation results of examples 1 to 3 and comparative examples 4 to 6. The examples of the present invention all grew high quality square plate-like single crystals, but the round cavity grown crystals of the comparative examples were mostly polycrystalline (examples 5, 6), and although the grown crystals of example 4 were single crystals, the inside thereof contained a large amount of metal inclusions, and the performance was poor.
The invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
Claims (10)
1. The preparation equipment of the square sheet diamond large single crystal is characterized by being a large-cavity press, wherein a heat insulation pipe, a heating pipe and an insulation pipe are sleeved in a growth cavity of the large-cavity press from outside to inside, and a carbon source, a catalyst and a crystal bed containing crystal seeds are stacked in a cavity of the insulation pipe from top to bottom, wherein the growth cavity is a cavity with a square cross section, the heat insulation pipe, the heating pipe and the insulation pipe are all square pipes, the carbon source, the catalyst and the crystal bed are all square pieces, the crystal seeds are square diamond crystal pieces, and a (100) surface is used as a crystal seed surface;
the temperature range in the growth cavity is controlled to be 1200-1300 ℃, the isothermal line in the square growth cavity is square, and the temperature of the growth front edge of the square diamond wafer is the same.
2. The apparatus for producing a square plate-like diamond large single crystal according to claim 1, wherein the large cavity press is a double-side press, a cubic press or a split ball press.
3. The apparatus for preparing a large single crystal of square diamond plate according to claim 1, wherein the material of the heating tube is one or more of graphite material, mixed material of graphite and sodium chloride, mixed material of graphite and ceramic material, metal material and lanthanum chromate material, wherein the ceramic material is magnesia, zirconia or alumina.
4. The apparatus for producing a square plate-like large diamond single crystal according to claim 1, wherein the material of the heat insulating pipe is one or more of magnesia, zirconia, alumina, pyrophyllite, and dolomite.
5. The apparatus for producing a large single crystal of square plate-shaped diamond according to claim 1, wherein the material of the insulating tube is one or more of magnesium oxide, zirconium oxide, aluminum oxide, and sodium chloride.
6. The apparatus for producing a square plate-like diamond large single crystal according to claim 1, wherein the catalyst is selected from the group consisting of metallic iron, metallic nickel, metallic cobalt, and a binary or ternary alloy containing two or three of iron, cobalt, and nickel.
7. The apparatus for producing a large single crystal of square plate-shaped diamond according to claim 1, wherein the carbon source is one or more of graphite, diamond, and graphene.
8. The apparatus for preparing a large square plate-shaped diamond single crystal according to claim 1, wherein the material of the seed bed is one or more of magnesia, zirconia, alumina and sodium chloride, the seed crystal is a diamond single crystal grown by a high temperature and high pressure method or a CVD method, the side length of the seed crystal is 0.1 mm-10 cm, and the number of the seed crystal is 1 or more.
9. A method for producing a large square plate-like diamond single crystal, characterized by producing a large square plate-like diamond single crystal by using the apparatus for producing a large square plate-like diamond single crystal according to any one of claims 1 to 8, wherein the pressure inside the growth chamber is controlled within a range of 5 to 10GPa and the temperature is controlled within a range of 1200 to 1300 ℃.
10. A large square plate-shaped diamond single crystal, which is prepared by the method for preparing a large square plate-shaped diamond single crystal according to claim 9, wherein the size of the large square plate-shaped diamond single crystal is 1 mm-10 cm, most of the surface of the large square plate-shaped diamond single crystal is a (100) crystal face, and the small part of the surface of the large square plate-shaped diamond single crystal is a (111) crystal face.
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| CN2571478Y (en) * | 2002-04-19 | 2003-09-10 | 张书达 | Pressure transmitted synthesis block for making ultrahard material |
| US7128547B2 (en) * | 2004-01-13 | 2006-10-31 | Chien-Min Sung | High pressure split die and associated methods |
| CN201454497U (en) * | 2009-04-27 | 2010-05-12 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Cubic diamond compact synthesis cavity |
| CN203874752U (en) * | 2014-03-14 | 2014-10-15 | 李强 | Square synthesis cavity with fillets for improving safety |
| CN207478528U (en) * | 2017-10-31 | 2018-06-12 | 江苏西玉钻石科技有限公司 | A kind of double carbon source synthesis of artificial diamond preparation facilities |
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