CN102600766B - Method for synthesizing gem grade diamond by using cubic press - Google Patents
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Abstract
The invention discloses a method for synthesizing a gem grade diamond by using a cubic press. The method comprises the steps of using high-quality diamond micro powder with grain size being less than 50 micrometers as raw materials, loading catalysts and the diamond micro powder into a metal cup in a stacking way, densifying under pressure being 200-400MPa, forming an indirect heating-type diamond synthesis assembly, and synthesizing for 20-240h at high temperature being 1450-2000 DEG C and under high pressure being 50000-60000 atmospheric pressure in the cubic press to obtain the gem grade diamond. The diamond synthesis assembly uses metal niobium, tantalum, molybdenum or tungsten to make the metal cup which is also used as a heating element, and aluminum oxide ceramic materials are additionally used for making a high-temperature protection pipe. By forming the indirect heating-type diamond synthesis assembly according to the method disclosed by the invention, the requirements of higher synthesizing temperature and longer heating time can be satisfied, the stability of diamond synthesis technology and equipment by using the cubic press is improved and the synthesis of the gem grade diamond under high pressure and at high temperature is realized.
Description
Technical field
The present invention relates to a kind of synthetic method of diamond, particularly relate to a kind of method of hexahedron synthetic diamond press synthetic gem grade diamond.
Background technology
Artificial diamond industrial produces, and generally take high purity graphite as raw material, adds catalytic alloy (for example Fe, Ni, Mn, the alloy that Co etc. form), under HTHP, graphite part is converted into diamond.According to existing industrial diamond synthesizing technology, under the high temperature and high pressure environment of 30 minutes, utilize about 100 microns of the synthetic diamond particle diameter of iron nickel by powder catalyst.If inferred according to crystal constant speed growth theory, by extending generated time, carry out the diamond of growth diameter 3mm, the generated time needing is 30 hours.But in fact because crystal growth is not constant speed, with the increase of crystal particle diameter, the area of each flat surface also increases rapidly, and theoretical according to layer growth, its speed of growth is also more and more slower; Diamond single crystal more than growth diameter 3mm need to surpass 6 day time.Therefore, the synthetic assembling of existing diamond and technique are difficult to meet the demands.
The problem that the synthetic assembling of producing for abrasive-grade diamond at present exists is: during (1) long-time heating, pyrophyllite powder briquetting temperature raises, easy quick-fried hammer.The temperature of synthetic chamber and heater element surpasses 1450 ℃, and long-time heating raises pyrophyllite powder briquetting temperature, and temperature causes that material generation volume changes suddenly during higher than phase transition temperature, thereby causes quick-fried hammer; (2) heater element poor stability when long-time heating.Its heater element of indirect mode generally using is at present cool molded graphite pipe or electrothermal alloy.Under high pressure deformation quantity is larger for the former, and poor stability, the process repeatability of resistance value are poor.The latter is irony alloy (the mixture 0.5-2 % of one or more in iron content 65-80%, chromium 13-27%, aluminium 4-7%, niobium, tantalum, molybdenum three), and fusing point is relatively low, is difficult to bear higher heating-up temperature.In addition, the reproducibility of iron, aluminium is strong, at high temperature easily oxidized, react, and then resistance value changes with acidic oxide or the oxide that contains dithizone.(3) the rear and front end temperature difference of top hammer becomes large during long-time heating, and swelling stress easily causes quick-fried hammer.
Aspect equipment, technology innovation along with China's diamond synthesis device, most enterprises has been eliminated old-fashioned supercharger systems, and adopts more efficiently high-pressure pump to carry out supercharging, has broken the generated time restriction that supercharger systems causes because oil cylinder piston stroke is limited.With high-pressure pump, carrying out supercharging can be without time limit pressurize.This is just the synthetic advantage that provides of gem grade diamond.
How to improve the stability of diamond synthesizing process and equipment, meet the desired higher synthesis temperature of synthesis technique, extend the heat time, reduce top hammer loss, on hexahedron synthetic diamond press, realizing the synthetic of gem grade diamond is problem to be solved by this invention.
Summary of the invention
The present invention is directed to the synthetic middle problem existing of existing diamond, aim to provide a kind of method of cubic hinge press synthetic gem grade diamond, by improving the synthetic assembling of indirect diamond, take diadust as raw material, at the downward warm generated time that grows tall of higher synthesis temperature, realize the synthetic of gem grade diamond on cubic hinge press.
In brief; the present invention makes metal cup and doubles as heating with refractory metal; additional alumina ceramic material is made high temperature protection pipe; be assembled into the synthetic assembling of indirect diamond (piece); in metal cup, fill diadust; by improving synthesis temperature and extending the heat time, adopt synthetic gem grade diamond under hexahedron synthetic diamond press high pressure-temperature condition.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method of cubic hinge press synthetic gem grade diamond, it is characterized in that, take diadust as raw material, with overlapped way, catalyst and diadust are seated in metal cup, densified under 200-400MPa pressure, form the synthetic assembling of indirect heating type diamond; Described synthetic assembling is made metal cup with metal niobium, tantalum, molybdenum or tungsten, metal cup is placed in the cylindrical synthetic chamber of pyrophyllite powder briquetting of liner dolomite sleeve pipe, metal cup outer wrapping aluminium oxide ceramics high temperature protection pipe, high temperature protection pipe external diameter and dolomite casing inner diameter match; Metal cup both sides arrange respectively metallic conduction sheet; Dolomite sleeve pipe two ends are sealed by the composite conducting plug of filling aluminium oxide ceramics heat Insulation film respectively, and metal cup, metallic conduction sheet and composite conducting plug conduction are connected; To synthesize assembling and be placed in cubic hinge press, under temperature 1450-2000 ℃, pressure 5-6 ten thousand atmospheric pressure, 20-240h condition, the synthetic gem grade diamond that makes of HTHP.
Described method specifically comprises the following steps:
(1) with metal niobium, tantalum, molybdenum or tungsten, be made into metal cup (heater element of holding concurrently).
(2) take a-aluminium oxide and the talcum of mass percent 75～90%:10～25% is aggregate, and through 850-1200 ℃ of sintering, making wall thickness is 3-8mm, and internal diameter and described metal cup external diameter match, highly identical high temperature protection pipe.
(3) adopt mild steel to make the external conductive casing of composite conducting plug; thickness >=3mm; external diameter is identical with high temperature protection pipe external diameter; in external conductive casing, fill heat Insulation film (energising end protection pad) and form cylindric composite conducting plug; heat Insulation film at least comprises that a slice is the a-aluminium oxide of mass percent 75～90%:10～25% and the aluminium oxide ceramics disk that talcum is made through 850-1200 ℃ of sintering; thickness is 3-8mm, diameter >=metal cup external diameter.
(4) take diadust as raw material, with overlapped way, chip catalyst and diadust are loaded in metal cup, densified under 200-400MPa pressure.
(5) the synthetic assembling of assembling: metal cup is placed in the cylindrical synthetic chamber of pyrophyllite powder briquetting of liner dolomite sleeve pipe, metal cup outer wrapping high temperature protection pipe, high temperature protection pipe external diameter and dolomite casing inner diameter match; Metal cup both sides arrange respectively metallic conduction sheet and are connected with metal cup; Dolomite sleeve pipe two ends are sealed by composite conducting plug respectively, and aluminium oxide ceramics disk contacts with metallic conduction sheet, and external conductive casing is connected with metallic conduction sheet.
(6) by the synthetic assembling after assembling, be positioned in cubic apparatus synthesis press, the synthesis condition in cubic hinge press is: temperature 1450-2000 ℃; Pressure 5-6 ten thousand atmospheric pressure (5-6x10
3mPa); Time 20-240 hour; Gained synthetic rod obtains diamond single crystal through electrolysis, fragmentation, screening.
Described metal cup is by refractory metal, as niobium, tantalum, molybdenum, tungsten sheet metal are made by Sheet Metal Forming Technology or welding procedure.Metal cup can adopt the cup of one end sealing to add the form of metal bowl cover, or the form that the cup openend of two single-ended sealings fastens forms, its size can be determined according to the synthetic chamber of cubic hinge press size, be generally wall thickness 0.1-0.3mm, diameter 10-50mm, height 10-50mm.In the inventive method, diamond synthesis material is filled in metal cup, and while metal cup also doubles as heating, and the high temperature protection pipe of cup outer wrapping can be effectively by heating and the isolation of pyrophyllite powder briquetting.
Described high temperature protection pipe adopts following methods preparation: according to mass percent a-aluminium oxide: talcum=75～90%:10～25% preparation aggregate, the binding agent polyvinyl alcohol that adds aggregate quality 1～4%, by wet ball grinding technique, make slurry, slurry mist projection granulating makes ceramic powder; Again that ceramic powder is compressing, 850-1200 ℃ of sintering, makes described high temperature protection pipe.
In described composite conducting plug, fill the heat Insulation film of two stacks in external conductive casing, a slice is aluminium oxide ceramics disk, and another sheet is dolomite disk.
Described metallic conduction sheet is the disk that diameter is identical with high temperature protection pipe external diameter, adopts refractory metal to make, and comprises metal niobium, tantalum, molybdenum or tungsten.
Described diadust particle diameter is less than 50 microns.
Described catalyst can adopt the catalyst of existing diamond in synthetic, and for example mass percent is the teleoseal catalyst of iron 65-75%, nickel 22-35%, cobalt 0-8%.
The inventive method is made metal cup and doubles as heating with refractory metal (niobium, tantalum, molybdenum, tungsten), and additional alumina ceramic material is made high temperature protection pipe, and higher heating-up temperature can be provided, and extends the heat time; Take diadust as raw material, the synthetic Tabular gem-grade diamond that obtains under suitable process conditions.
Advantage of the present invention and beneficial effect comprise:
(1) fusing point of the metal such as niobium, tantalum, molybdenum, tungsten is high, and the metal cup made from refractory metal doubles as heater element, and the heating-up temperature that can bear significantly improves; And the good stability of long-time heating.
(2) metal cup doubles as heater element, and the high temperature protection pipe of cup outer wrapping can prevent from the phase transformation of pyrophyllite powder briquetting from reducing quick-fried hammer risk.
(3) high-temperature insulating quality of the ceramic high temperature protection tube made from a-aluminium oxide and talcum and heat Insulation film (energising end pad) is good, does not at high temperature undergo phase transition, and cubical expansivity changes little, the pressurize good stability of cavity.In addition, this pottery has during higher than 1450 ℃ a small amount of liquid phase to produce in temperature, be conducive to pressure transmission, and the pressure uniformity in cavity is good, thereby can improve distributing homogeneity and the concentration degree of diamond particles.
(4) take particle diameter is less than the gem grade diamond micro mist of 50 microns as raw material growth gem grade diamond, has avoided graphite to change into volume contraction (the graphite density 1.9g/cm of diamond process
3, diamond density 2.3g/cm
3).Reduced the variable quantity of cumulative volume in diamond film process, the volume stability of system is good.
Therefore (5) the filling mode of synthesis material adopts stackedly, and under high temperature, adamantine electrical conductivity, well below metal electric heating element, does not need complicated indirect assembling, and simple in structure, stability improves.
(6) structure of the synthetic assembling of indirect of the present invention is compacter, and the transport performance of synthetic assembled product improves, and has reduced breakage rate.
Below in conjunction with specific embodiment, describe the present invention.Protection scope of the present invention is not limited with the specific embodiment, but is limited by claim.
Accompanying drawing explanation
The structural representation of the synthetic assembling of diamond in Fig. 1 the inventive method.
1, pyrophyllite powder briquetting, 2, dolomite sleeve pipe, 3, aluminium oxide ceramics high-temperature pipe, 4, composite conducting plug, 5, metallic conduction sheet, 6, synthetic stem stem, 7, metal cup (heater element of holding concurrently).
Fig. 2 diadust and chip catalyst filling mode schematic diagram.
7, metal cup, 8, chip catalyst, 9, diadust.
The specific embodiment
A method for cubic hinge press synthetic gem grade diamond, specifically comprises the following steps:
(1) the refractory metal cup heating of holding concurrently is made
By metallic plate punchings such as niobium, tantalum, molybdenum, tungsten or to be welded into thickness be 0.1-0.3mm, the cup-shaped heater element of diameter 10-50mm, height 10-50mm.
(2) high temperature protection pipe preparation
By a-aluminium oxide and the talcum powder preferred 85%:15% of 75～90%:10～25%(by mass percentage) mix, be loaded in ball grinder, take water as medium, with corundum ball, be ground into particle diameter and be less than 200 object slurries, again by aluminium oxide and talcum powder quality 1～4%(preferably 3%) add polyvinyl alcohol (PVA molecular weight >=10000, polyvinyl alcohol water solution concentration is 5-10%), with atomizing granulating technology, be prepared into the powder ball of particle diameter 0.3-0.7mm.
(3) high temperature protection pipe is made
It is 3-8mm that the repressed moulding of ceramic powder, the high temperature sintering of preparation in step (2) are made to wall thickness, the protective casing of internal diameter and length and above-mentioned cup-shaped heater element external diameter and matched.Ceramic powder is pressed into required tubular blank with wolfram steel mould, is embedded in coarse granule alumina powder, in 850-1200 ℃ of sintering 1-3 hour, (preferably 3.5 ℃/min was warmed up to 550 ℃ of insulations and comes unstuck for 1 hour; With 5 ℃/min, be warmed up to 1000 ℃ again sintering 1 hour) become high temperature protection earthenware.The shrinkage factor of pottery in sintering process is 5-8%, and therefore, the design of mould should be done corresponding size by actual shrinkage factor and amplify.
By tubular blank landfill sintering in alumina powder, buried powder has limited earthenware in sintering process and, along diametric contraction deformation, has guaranteed diameter uniformity and the caliber size of pipe on the one hand; On the other hand, high temperature sintering has been removed volatile material (as the hydroxyl in raw material, moisture and binding agent), has avoided prepared high-temperature pipe to produce gas under the high pressure-temperature condition of diamond synthesis; The 3rd, by sintering process, the density of earthenware is larger, and intensity is high, is difficult for broken.
(4) composite conducting plug is made
The external conductive casing of composite conducting plug is low-carbon steel material punch forming, and thickness is for being at least 3mm, and the cavity diameter of external profile diameter and briquetting matches.In external conductive casing, fill two heat Insulation films, one is powder aluminium oxide ceramics disk dry-pressing formed and that form in 850-1200 ℃ of (preferably 1000 ℃) sintering 1-3 hour in above-mentioned steps (2).Another piece is dolomite disk.Dolomite disk manufacture craft is: the mass percent of dolomite powder (particle diameter 100-300 order), waterglass (modulus 2.3) and polyvinyl alcohol (molecular weight is greater than 10000) is 84%:13%:3% (it is 5% aqueous solution that polyvinyl alcohol is mixed with concentration in use), above-mentioned material is stirred in agitator, with dry pressuring forming process, be pressed into disk, then in 450 ℃ of heating 1-2 hour.Dolomite heat Insulation film and aluminium oxide ceramics heat Insulation film are filled in external conductive casing successively, make composite conducting plug.
(5) the interior material of metal cup (heating of holding concurrently) is filled
The diadust and the chip catalyst that particle diameter are less than to 50 microns are filled in (as Fig. 2) in metal cup with overlapped way, distance between chip catalyst (diadust layer thickness) is wished the diamond single crystal size synthesizing for 2-5 mm(depends on), densified under 200-400MPa pressure.
(6) the synthetic assembling of assembling
The metal cup of briquetting, high temperature protection pipe, fill material, metallic conduction sheet, composite conducting plug etc. are assembled into synthetic assembling (as Fig. 1).
(7) gem grade diamond is synthetic
Synthetic assembling after assembling is positioned in cubic apparatus synthesis press, and follow procedure is raised to desirable value by pressure and temperature, temperature 1450-2000 ℃; Pressure 5-6 ten thousand atmospheric pressure (5-6x10
3mPa); Keep 20-240 hour; Gained synthetic rod gets final product to obtain product through electrolysis, fragmentation, screening.
Embodiment 1
Synthetic gem grade diamond in the hexahedron synthetic diamond press of cavity diameter 23mm, synthetic assembling comprises:
Briquetting size: 38mm
3
High temperature protection pipe: wall thickness 5mm, outer through 23mm, interior through 13mm, height 11.6 mm
Metal cup: metal molybdenum, wall thickness 0.2mm, outer through 13mm, height 11.6mm
Refractory metal conducting strip: metal molybdenum, thickness 0.2mm, diameter 23mm
Composite conducting plug: box hat: thickness 3mm, outer through 23mm, height 13mm
Aluminium oxide ceramics disk: diameter 17mm, thickness 5mm
Dolomite disk: diameter 17mm, thickness 5mm.
Synthesis condition: 1450 ℃ of temperature (with bismuth silk phase transformation estimation); Pressure 52000 atmospheric pressure; Generated time: 55 hours.
Use raw material: W14 diadust 2.8g, 4 of iron-nickel accelerant sheets.
Products obtained therefrom: 1.61 grams of the above diamond single crystals of diameter 1mm, the largest particles diameter 2.8mm.
Embodiment 2
Synthetic gem grade diamond in the hexahedron synthetic diamond press of cavity diameter 23mm, synthetic assembling comprises:
Briquetting size: 38mm
3
High temperature protection pipe: wall thickness 5mm, outer through 23mm, interior through 13mm, height 11.6 mm
Metal cup: metal molybdenum, wall thickness 0.2mm, outer through 13mm, height 11.6mm
Refractory metal conducting strip: metal molybdenum, thickness 0.2mm, diameter 23mm
Composite conducting plug: box hat: thickness 3mm, outer through 23mm, height 13mm
Aluminium oxide ceramics disk: diameter 17mm, thickness 5mm
Dolomite disk: diameter 17mm, thickness 5mm.
Synthesis condition: 1450 ℃ of temperature (with bismuth silk phase transformation estimation); Pressure 52000 atmospheric pressure; Generated time: 76 hours.
Use raw material: W14 diadust 2.8g, 4 of iron-nickel accelerant sheets.
Products obtained therefrom: 1.79 grams of the above diamond single crystals of diameter 1mm, the largest particles diameter 3.0mm.
Embodiment 3
Synthetic gem grade diamond in the hexahedron synthetic diamond press of cavity diameter 23mm, synthetic assembling comprises:
Briquetting size: 38mm
3
High temperature protection pipe: wall thickness 5mm, outer through 23mm, interior through 13mm, height 11.6 mm
Metal cup: metal molybdenum, wall thickness 0.2mm, outer through 13mm, height 11.6mm
Refractory metal conducting strip: metal molybdenum, thickness 0.2mm, diameter 23mm
Composite conducting plug: box hat: thickness 3mm, outer through 23mm, height 13mm
Aluminium oxide ceramics disk: diameter 17mm, thickness 5mm
Dolomite disk: diameter 17mm, thickness 5mm.
Synthesis condition: 1450 ℃ of temperature (with bismuth silk phase transformation estimation); Pressure 52000 atmospheric pressure; Generated time: 96 hours.
Use raw material: W14 diadust 2.8g, 4 of iron-nickel accelerant sheets.
Products obtained therefrom: 1.91 grams of the above diamond single crystals of diameter 1mm, the largest particles diameter 3.2mm.
Embodiment 4
Synthetic assembling is substantially the same manner as Example 3, and metal cup and metallic conduction sheet adopt tungsten.Because tungsten hardness is large, metal cup can not be used punch forming.Adopt argon arc welding technique to make metal cup.
In synthesis condition, except temperature is 1700 ℃, other condition is identical with embodiment 1, products obtained therefrom: 1.80 grams of the above diamond single crystals of diameter 1mm, the largest particles diameter 3.0 mm.Metal tube present situation remains intact, and deformation is even, the electrolytic treatments speed of synthetic piece, and electrolyte is favourable to improving electrolytic speed containing organic acid.
Claims (6)
1. the method for a cubic hinge press synthetic gem grade diamond, it is characterized in that, take diadust as raw material, with overlapped way, catalyst and diadust are seated in metal cup, densified under 200-400MPa pressure, form the synthetic assembling of indirect heating type diamond; Described synthetic assembling is made metal cup with metal niobium, tantalum, molybdenum or tungsten, metal cup is placed in the cylindrical synthetic chamber of pyrophyllite powder briquetting of liner dolomite sleeve pipe, metal cup outer wrapping aluminium oxide ceramics high temperature protection pipe, high temperature protection pipe external diameter and dolomite casing inner diameter match; Metal cup both sides arrange respectively metallic conduction sheet; Dolomite sleeve pipe two ends are sealed by the composite conducting plug of filling aluminium oxide ceramics heat Insulation film respectively, and metal cup, metallic conduction sheet and composite conducting plug conduction are connected; To synthesize assembling and be placed in cubic hinge press, at temperature 1450-2000 ℃, pressure 5-6x10
3under MPa, 20-240h condition, the synthetic gem grade diamond that makes of HTHP.
2. the method for cubic hinge press synthetic gem grade diamond according to claim 1, is characterized in that, described method comprises the following steps:
(1) with metal niobium, tantalum, molybdenum or tungsten, be made into metal cup;
(2) take a-aluminium oxide and the talcum of mass percent 75～90%:10～25% is aggregate, and through 850-1200 ℃ of sintering, making wall thickness is 3-8mm, and internal diameter and described metal cup external diameter match, highly identical high temperature protection pipe;
(3) adopt mild steel to make the external conductive casing of composite conducting plug, thickness >=3mm, external diameter is identical with high temperature protection pipe external diameter, in external conductive casing, fill heat Insulation film and form cylindric composite conducting plug, heat Insulation film at least comprises that a slice is the a-aluminium oxide of mass percent 75～90%:10～25% and the aluminium oxide ceramics disk that talcum is made through 850-1200 ℃ of sintering, thick is 3-8mm, diameter >=metal cup external diameter;
(4) take diadust as raw material, with overlapped way, chip catalyst and diadust are loaded in metal cup, densified under 200-400MPa pressure;
(5) the synthetic assembling of assembling: metal cup is placed in the cylindrical synthetic chamber of pyrophyllite powder briquetting of liner dolomite sleeve pipe, metal cup outer wrapping high temperature protection pipe, high temperature protection pipe external diameter and dolomite casing inner diameter match; Metal cup both sides arrange respectively metallic conduction sheet and are connected with metal cup; Dolomite sleeve pipe two ends are sealed by composite conducting plug respectively, and aluminium oxide ceramics disk contacts with metallic conduction sheet, and external conductive casing is connected with metallic conduction sheet;
(6) by the synthetic assembling after assembling, be positioned in cubic hinge press, the synthesis condition in cubic hinge press is: temperature 1450-2000 ℃; Pressure 5-6x10
3mPa; Time 20-240 hour; Gained synthetic rod obtains diamond single crystal through electrolysis, fragmentation, screening.
3. the method for cubic hinge press synthetic gem grade diamond according to claim 1 and 2, it is characterized in that, described high temperature protection pipe adopts following methods preparation: according to mass percent a-aluminium oxide: talcum=75～90%:10～25% preparation aggregate, the binding agent polyvinyl alcohol that adds aggregate quality 1～4%, by wet ball grinding technique, make slurry, slurry mist projection granulating makes ceramic powder; Again that ceramic powder is compressing, 850-1200 ℃ of sintering, makes described high temperature protection pipe.
4. the method for cubic hinge press synthetic gem grade diamond according to claim 2, is characterized in that, in described composite conducting plug, fills the heat Insulation film of two stacks in external conductive casing, and a slice is aluminium oxide ceramics disk, and another sheet is dolomite disk.
5. the method for cubic hinge press synthetic gem grade diamond according to claim 1 and 2, is characterized in that, described metallic conduction sheet is the disk that diameter is identical with high temperature protection pipe external diameter, adopts metal niobium, tantalum, molybdenum or tungsten to make.
6. the method for cubic hinge press synthetic gem grade diamond according to claim 1 and 2, is characterized in that, described diadust particle diameter is less than 50 microns.
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| CN104226198B (en) * | 2014-09-11 | 2016-02-10 | 河南省力量新材料有限公司 | For the preparation method of the heater element of ultra-fine diamond synthesis |
| CN106215808B (en) * | 2016-08-18 | 2019-01-11 | 中南钻石有限公司 | A kind of Synthetic block and its synthetic method of artificial synthesized jewellery colorless diamond |
| CN111203153B (en) * | 2020-01-20 | 2022-11-01 | 常州大学 | Operation and sealing method of large cubic press based on double-face top mode |
| CN112495303B (en) * | 2020-11-25 | 2022-08-05 | 内蒙古唐合科技有限公司 | Self-sharpening diamond and preparation method thereof |
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| ES2258919B2 (en) * | 2005-02-21 | 2007-04-01 | Instituto De Monocristales, S.L. | CAPSULE AND ELEMENTS FOR THE PRODUCTION OF DIAMOND SYNTHESIS. |
| CN101007251A (en) * | 2006-01-23 | 2007-08-01 | 郑州人造金刚石及制品工程技术研究中心 | Outer indirect heating diamond synthesis block |
| CN101279223B (en) * | 2008-05-05 | 2010-11-17 | 江苏工业学院 | Use of electrothermal alloy in six-side top high-temperature high-pressure synthetic cavity |
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