CN102600768A - Indirect heating-type synthesis assembly for high-temperature and high-pressure artificial single crystal synthesis by using cubic press - Google Patents
Indirect heating-type synthesis assembly for high-temperature and high-pressure artificial single crystal synthesis by using cubic press Download PDFInfo
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Abstract
The invention relates to an indirect heating-type synthesis assembly for single crystal synthesis by using a cubic press. The indirect heating-type synthesis assembly comprises pyrophyllite powder pressing block which is internally lined with a dolomite casing. The indirect heating-type synthesis assembly is characterized in that a cylindrical metal cup made of metal niobium, tantalum, molybdenum or tungsten is arranged in the dolomite casing, an aluminum oxide ceramic high-temperature pipe is wrapped outside the cylindrical metal cup and the aluminum oxide ceramic high-temperature pipe is made of alpha-aluminum oxide and talc through high-temperature sintering; metal conducting strips are respectively arranged on the two sides of the metal cup and are connected with the metal cup; and the two ends of the dolomite casing are respectively sealed by composite conducting plugs and the composite conducting plugs are connected with the metal conducting strips. The indirect heating-type synthesis assembly uses high-melting-point metals to make the metal cup which is also used as an electric heating element, aluminum oxide ceramic materials are additionally used for making the high-temperature protection pipe, the indirect heating-type synthesis assembly is suitable for synthesizing artificial single crystals such as diamonds by using the cubic press, the requirements of higher temperature and longer heating time are satisfied, the stability of single crystal synthesis technology and equipment is improved, the losses of anvils are reduced and favorable conditions are provided for the synthesis of gem grade diamonds.
Description
Technical field
The invention belongs to the artificial synthesis technical field of diamond or other monocrystalline; Relate to the synthetic assembling of a kind of monocrystalline; Particularly relate to the indirect heating type synthetic assembling (synthetic piece) of the artificial monocrystalline of a kind of cubic hinge press HTHP in synthetic; Hexahedron top press high-pressure high temperature diamond synthesis be can be used for, cubic boron nitride, single-crystal silicon carbide and gallium nitride single crystal growth also can be applied to.
Background technology
The artificial diamond industrial produces, and generally is raw material with the high purity graphite, adds catalytic alloy (for example Fe, Ni, Mn, the alloy that Co etc. form), under HTHP, graphite part is converted into diamond.The adamantine synthetic cubic hinge press that adopts usually provides crystal growth required HTHP, and present most cubic hinge press diamond synthesis all adopt the indirect mode.The heating of synthetic cavity is to form connect form circuit through tungsten carbide top hammer with the cavity heater element with low-voltage and high-current.With graphite matter tubing or electrothermal alloy is heating element heater indirect graphite synthetic rod.The graphite synthetic rod is wrapped among the ferrous metal shell (metal cup), to reduce nonhomogeneous deformation.Install insulation tube additional between heating element heater and the shell, avoid electric current to pass through graphite synthetic rod and ferrous metal shell leakage conductance.The used briquetting of diamond synthesis is the pyrophillite powder with the waterglass bonding, is cylindrical synthetic chamber in the middle of the cube briquetting, the dolomite insulating tube that liner 3-4mm is thick.Pyrophyllite powder briquetting, insulating tube, heating element heater and conduction plug, insulation tube, metal cup (including synthetic rod) etc. are combined into the synthetic assembling of diamond (or synthetic piece); Place the cubic apparatus synthesis press; By synthetic technological condition pressure and temperature is raised to desirable value, obtains artificially synthesizing diamond behind the crystal growth certain hour.
For example, ZL201020686676 discloses that a kind of diamond is synthetic uses indirect heating apparatus, comprises the pyrophyllite composite block; The pyrophyllite composite block is installed the conduction plug respectively in two ends up and down; Stem stem is installed in the centre of pyrophyllite composite block, and the stem stem periphery is installed metal cup, and the metal cup upper and lower surfaces are installed insulating trip respectively; The metal cup two sides are installed insulation tube respectively; Insulation tube outer wall two sides are installed metal electric heating tube respectively, and insulating trip is connected with sheet metal respectively, and sheet metal is connected with the termination heating plate.CN200610017366.5 discloses a kind of outer indirect heating diamond synthesis block; Comprise diamond synthesizing column; Synthetic post two ends are provided with the composite conducting heat-proof device; The synthetic post and the composite conducting heat-proof device outside are arranged with hermetical and pressure madium, inwardly are disposed with heater element, heat transfer element and isolated component between hermetical and pressure madium and composite conducting heat-proof device and the synthetic post certainly outward.The composite conducting heat-proof device comprises conducting metal disk and the metallic cylinder that an end joins with it and diameter is less, closely embeds prefabricated insulation material cylinder in the cylinder, and the cylinder periphery closely is arranged with prefabricated thermal insulation material cylinder.
In the synthetic assembling that at present diamond is produced, metal cup (isolated component) is provided with respectively with heating element heater, between install insulation tube additional; High-temperature insulation and insulation material adopt dolomite to make.The problem that exists is: during (1) long-time heating, pyrophyllite powder briquetting (hermetical and pressure madium) temperature raises, easy quick-fried hammer.The temperature of synthetic chamber and heater element surpasses 1450 ℃, and adiabatic poor between pyrophyllite powder briquetting and the heater element, long-time heating raises pyrophyllite powder briquetting temperature, causes when temperature is higher than phase transition temperature that material generation volume changes suddenly, thereby causes quick-fried hammer.(2) gas that produces when the high-temperature insulation made of dolomite and insulation material high temperature is drained easy quick-fried hammer.The water glass of binder that dolomite insulation and insulating tube add when making forms silica dioxide gel and does not fully react with dolomite, and at high temperature both react and produce water and carbon dioxide.Though pyrophillite is sheet crystal structure (being different from metal), allow the part micro-molecular gas to overflow along inter-level diffusion, the top hammer can safety relief.But the thickness of used insulating tube and insulation tube and oversized, the gas flow that produces during heating increases, and has improved the risk of quick-fried hammer.(3) heater element poor stability when long-time heating: the indirect heater element that generally uses at present is cool molded graphite pipe or electrothermal alloy.Under high pressure deformation quantity is bigger 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 among iron content 65-80%, chromium 13-27%, aluminium 4-7%, niobium, tantalum, the 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, and is at high temperature oxidized easily, reacts with acidic oxide or the oxide that contains the oxidisability ion.And then resistance value changes.(4) the rear and front end temperature difference of long-time heating time top hammer becomes big, and swelling stress is prone to cause quick-fried hammer.
Aspect equipment, along with the technology innovation of China's diamond synthesis device, most of enterprises have eliminated old-fashioned supercharger systems, and adopt more efficiently high-pressure pump to carry out supercharging.Broken supercharger systems because the limited generated time restriction that causes of oil cylinder piston stroke is carried out supercharging with high-pressure pump and can not had the time limit pressurize.Therefore; The stability of synthesis techniques such as the indirect heating type that improves in the cubic hinge press synthesizes assembling, the raising diamond and equipment satisfies the desired higher synthesis temperature of technology; Prolong heat time heating time; Reduce top hammer loss, for the synthetic advantage that provides of gem grade diamond, significant for the diamond industrial upgrading.
Summary of the invention
The present invention aims to provide the indirect heating type synthetic assembling of the artificial monocrystalline of a kind of cubic hinge press HTHP in synthetic; Can overcome existing above-mentioned defective in the prior art; Improve the stability of synthesis technique such as diamond and equipment, satisfy higher synthesis temperature and prolong heat time heating time, reduce the top to hammer loss into shape; Improve the quality of diamond synthesis, and then realize the synthetic of gem grade diamond.
In brief; The present invention makes metal cup and double as heating with refractory metal (niobium, tantalum, molybdenum, tungsten); Add alumina ceramic material and make the high temperature protection pipe; Be assembled into the synthetic assembling of indirect stone (piece) with it, be applicable to cubic apparatus diamond press high pressure-temperature synthetic gem grade diamond.This assembling also can be applied to cubic boron nitride, single-crystal silicon carbide and gallium nitride single crystal growth.
For realizing the foregoing invention purpose, the present invention adopts following technical scheme:
The synthetic assembling of indirect heating type during the artificial monocrystalline of a kind of cubic hinge press HTHP is synthetic; Comprise pyrophyllite powder briquetting (1); In the liner dolomite sleeve pipe (2), dolomite sleeve pipe (2) is cylindrical synthetic chamber, it is characterized in that; Comprise the cylindric metal cup of processing with metal niobium, tantalum, molybdenum or tungsten (7) in the dolomite sleeve pipe (2); Cylinder outerwrap aluminium oxide ceramics high temperature pipe (3), described aluminium oxide ceramics high temperature pipe (3) is an aggregate with the а-aluminium oxide and the talcum of mass percent 75～90%:10～25%, makes through 850-1200 ℃ of sintering; Described metal cup (7) both sides are provided with metallic conduction sheet (5) respectively and are connected with metal cup (7); By composite conducting plug (4) sealing, composite conducting plug (4) is connected with metallic conduction sheet (5) respectively at dolomite sleeve pipe (2) two ends.
Described metal cup is made through Sheet Metal Forming Technology or welding procedure like niobium, tantalum, molybdenum, tungsten sheet metal by refractory metal.Metal cup can adopt the cup of end sealing to add the form of metal bowl cover; Or the form that the cup openend of two single-ended sealings fastens is formed; Its size can be confirmed according to the synthetic chamber of cubic hinge press size, be generally wall thickness 0.1-0.3mm, diameter 10-50mm, height 10-50mm.Synthetic assembling of the present invention, the synthetic stem stem of diamond (or other monocrystalline) is filled in the metal cup, while metal cup and double as heating, the aluminium oxide ceramics high temperature pipe of cup outerwrap can be isolated heating and pyrophyllite powder briquetting effectively.
Described aluminium oxide ceramics high temperature thickness of pipe wall is 3-8mm, and internal diameter and metal cup external diameter are complementary, and height is identical with metal cup; External diameter and synthetic chamber diameter (dolomite casing inner diameter) are complementary.
Described aluminium oxide ceramics high temperature pipe adopts the preparation of following method: according to mass percent а-aluminium oxide: talcum=75～90%:10～25% preparation aggregate; The binding agent polyvinyl alcohol that adds aggregate quality 1～4%; Make slurry through wet ball grinding technology, the slurry mist projection granulating makes ceramic powder; With ceramic powder compression moulding, 850-1200 ℃ of sintering makes described ceramic high temperature pipe again.
Described metallic conduction sheet is diameter and the identical disk of aluminium oxide ceramics high temperature external diameter of pipe, adopts refractory metal, comprises metal niobium, tantalum, molybdenum or tungsten.
Described composite conducting plug comprises the cylindrical conductive shell, or adopts the low-carbon steel material punch forming, and thickness is >=3mm external diameter identical with aluminium oxide ceramics high temperature external diameter of pipe (being complementary with the synthetic cavity diameter of briquetting).Described external conductive casing is connected with metallic conduction sheet conduction.Fill heat Insulation film (energising end protection pad) in the external conductive casing; Preferred heat Insulation film of filling two stacks; One piece material is identical with aluminium oxide ceramics high temperature pipe, promptly adopts the ceramic powder in the above-mentioned aluminium oxide ceramics high temperature control fully, through compression moulding; The 850-1200 ℃ of aluminium oxide ceramics disk that sintering forms, another sheet is the dolomite disk.Described aluminium oxide ceramics disk is thick to be 3-8mm, diameter >=metal cup external diameter, and contact with the metallic conduction sheet.
The synthetic assembling of indirect heating type of the present invention can prepare by following method:
(1) is made into the metal cup (heater element) of wall thickness 0.1-0.3mm, diameter 10-50mm, height 10-50mm through Sheet Metal Forming Technology or welding procedure with niobium, tantalum, molybdenum, tungsten sheet metal.
(2) be aggregate with aluminium oxide and talcum (mass percent is 75～90%:10～25%); Making wall thickness through high temperature 850-1200 ℃ of sintering is 3-8mm; Internal diameter and metal cup external diameter coupling, length identical with metal cup aluminium oxide ceramics high temperature pipe (protective casing).
(3) with aluminium oxide and talcum (mass percent is 75～90%:10～25%), to make thick be 3-8mm to (2) identical method set by step, the aluminium oxide ceramics heat Insulation film (energising is held and protected pad) of diameter and composite conducting plug coupling.
(4) adopt the low-carbon steel material punch forming to make the external conductive casing of composite conducting plug, thickness is >=3mm that the cavity diameter of external profile diameter and briquetting is complementary.Fill dolomite heat Insulation film and aluminium oxide ceramics heat Insulation film in the external conductive casing successively.
(5) in metal cup, fill synthetic stem stem, assembling becomes synthetic assembling.
Above-mentioned synthetic assembling promptly can be used for artificial monocrystalline such as diamond in the cubic hinge press HTHP is synthetic.
Beneficial effect of the present invention: the present invention makes metal cup and double as heating with refractory metal (niobium, tantalum, molybdenum, tungsten); Add alumina ceramic material and make the high temperature protection pipe; Be assembled into the synthetic assembling of indirect (piece) with it, be applicable to artificial monocrystalline such as hexahedron top press high-pressure high temperature diamond synthesis.The stability that synthetic assembling of the present invention can improve synthesis technique and equipment in the cubic hinge press such as diamond satisfies desired higher temperature of technology and longer heat time heating time, reduces top hammer loss, is the synthetic advantage that provides of gem grade diamond.Beneficial effect of the present invention comprises:
(1) fusing point of metals such as niobium, tantalum, molybdenum, tungsten is high, and with the metal cup double as heater element that refractory metal is made, the heating-up temperature that can bear significantly improves; And the good stability of long-time heating.
(2) metal cup double as heater element can reduce the use of high temperature insulating material, and the aluminium oxide ceramics high temperature pipe of cup outerwrap can be isolated heating (metal cup) and pyrophyllite powder briquetting effectively, reduces quick-fried hammer risk.
(3) adopt the corundum of high temperatures to process earthenware, and it is carried out high annealing, avoided the gas of material in the monocrystalline building-up process to discharge.Alumina ceramic tube so that а-aluminium oxide and talcum are made is good with the high-temperature insulating quality of aluminium oxide ceramics heat Insulation film (energising end pad), does not at high temperature undergo phase transition, and the cubical expansivity variation is little, the pressurize good stability of cavity.In addition, this ceramic material has a spot of liquid-phase generating when temperature is higher than 1450 ℃, help the pressure transmission, the pressure good uniformity in the cavity, thus can improve the distributing homogeneity of single crystal grain in the synthetic stem stem and the concentration degree of a footpath distribution.
(4) the alumina ceramic material density that makes through sintering is bigger, and intensity is high, is difficult for fragmentation, helps the assembling of synthetic assembling; Metal cup and heating element heater unite two into one, and make that the synthetic assembled construction of indirect of the present invention is compact more, and the transport performance of assembled product improves, and has reduced breakage rate.
Describe the present invention below in conjunction with specific embodiment.Protection scope of the present invention is not exceeded with the specific embodiment, but is limited claim.
Description of drawings
Fig. 1 indirect heating type of the present invention synthesizes the assembled construction sketch map.
1, pyrophyllite powder briquetting, 2, the dolomite sleeve pipe, 3, aluminium oxide ceramics high temperature pipe, 4, the composite conducting plug, 5, the metallic conduction sheet, 6, synthetic stem stem, 7, metal cup (heater element of holding concurrently).
The specific embodiment
Describe the present invention below in conjunction with specific embodiment.Protection scope of the present invention is not exceeded with the specific embodiment, but is limited claim.
The synthetic assembling of indirect heating type during the artificial monocrystalline of cubic hinge press HTHP of the present invention is synthetic; Equally applicable to synthetic other the artificial monocrystalline of cubic hinge press HTHP; Like cubic boron nitride, single-crystal silicon carbide and gallium nitride single crystal etc.; Below in conjunction with accompanying drawing, be assembled into example and be described in detail so that diamond is synthetic.
According to the synthetic assembling of cubic hinge press indirect heating type diamond of the present invention,, comprise pyrophyllite powder briquetting 1, dolomite sleeve pipe 2, aluminium oxide ceramics high temperature pipe 3, composite conducting plug 4, metallic conduction sheet 5, metal cup (heater element of holding concurrently) 7 referring to Fig. 1.Pyrophyllite powder briquetting 1 liner dolomite sleeve pipe 2; In the dolomite sleeve pipe 2 is cylindrical synthetic chamber; The synthetic stem stem 6 of diamond places synthetic chamber; Synthetic stem stem 6 is filled in the metal cup 7, and synthetic certainly stem stem 6 is respectively metal cup 7, aluminium oxide ceramics high temperature pipe 3, dolomite sleeve pipe 2 and pyrophyllite powder briquetting 1 from inside to outside.
Metal cup 7 is by aluminium oxide ceramics high temperature pipe 3 parcels, and height is identical with metal cup 7; Both sides are provided with metallic conduction sheet 5 respectively.Metallic conduction sheet 5 one sides are connected with metal cup 7, and opposite side is connected with composite conducting plug 4.Aluminium oxide ceramics high temperature pipe 3 external diameters, metallic conduction sheet 5 diameters are identical with composite conducting plug 4 external diameters, and are complementary with dolomite sleeve pipe 2 internal diameters, and dolomite sleeve pipe 2 both sides are respectively by 4 sealings of composite conducting plug.
Metal cup 7 is processed with metal niobium, tantalum, molybdenum or tungsten, and aluminium oxide ceramics high temperature pipe 3 is an aggregate with the а-aluminium oxide and the talcum of mass percent 75～90%:10～25%, processes through 850-1200 ℃ of sintering.Metallic conduction sheet 5 adopts metal niobium, tantalum, molybdenum or tungsten material, and composite conducting plug 4 comprises hollow cylindrical mild steel external conductive casing, and external conductive casing is filled dolomite heat Insulation film and aluminium oxide ceramics heat Insulation film from inside to outside successively.
Above-mentioned its manufacturing process of synthetic assembling comprises the steps:
(1) refractory metal cup 7 (heating of holding concurrently) is made
With metallic plate punching 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) aluminium oxide ceramics dry powder preparation
With а-aluminium oxide and talcum powder 75～90%:10～25% (preferred 85%:15%) mixing by mass percentage; Be loaded in the ball grinder; With water is medium, is ground into particle diameter less than 200 purpose slurries with the corundum ball, presses aluminium oxide and talcum powder quality 1～4% (preferred 3%) again and adds polyvinyl alcohol (PVA molecular weight >=10000; Polyvinyl alcohol water solution concentration is 5-10%), with atomizing granulating technology it is prepared into the powder ball of particle diameter 0.3-0.7mm.
(3) aluminium oxide ceramics high temperature pipe 3 is made
It is 3-8mm that the ceramic powder of preparation in the step (2) is processed wall thickness through compression moulding, high temperature sintering, 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 the wolfram steel mould, tubular blank is embedded in the coarse granule alumina powder, (preferred 3.5 ℃/min was warmed up to 550 ℃ of insulations and came unstuck in 1 hour in 850-1200 ℃ of sintering 1-3 hour; Be warmed up to 1000 ℃ sintering 1 hour again with 5 ℃/min) become aluminium oxide ceramics high temperature pipe.The shrinkage factor of pottery in sintering process is 5-8%, and therefore, Mould design should be done corresponding size by actual shrinkage factor and amplify.With tubular blank landfill sintering in alumina powder, bury powder on the one hand and limited the earthenware diametric contraction deformation in edge in the sintering process, guaranteed the diameter uniformity and the caliber size of pipe; On the other hand, high temperature sintering has been removed volatile material (like the hydroxyl in the raw material, moisture and binding agent), has avoided prepared high temperature pipe under the high pressure-temperature condition of diamond synthesis, to produce gas; The 3rd, through sintering process, the density of earthenware is bigger, and intensity is high, is difficult for broken.
(4) composite conducting plug 4 is made
The external conductive casing of composite conducting plug plug is the low-carbon steel material punch forming, and thickness is at least 3mm, and the cavity diameter of external profile diameter and briquetting is complementary.Fill two heat Insulation films in the external conductive casing, one for the powder that makes in the above-mentioned steps (2) aluminium oxide ceramics disk dry-pressing formed and that formed in sintering 1-3 hour in 850-1200 ℃ (preferred 1000 ℃).Another piece is the dolomite disk.Its common manufacture craft of dolomite disk 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; Be pressed into disk with dry pressuring forming process, again in 450 ℃ of heating 1-2 hour.Dolomite heat Insulation film and aluminium oxide ceramics heat Insulation film are filled in the external conductive casing successively, process the composite conducting plug.
(5) pyrophyllite powder briquetting 1, dolomite sleeve pipe 2, aluminium oxide ceramics high temperature pipe 3, metal cup 7 (including synthetic stem stem 6), metallic conduction sheet 5, composite conducting plug 4 are assembled into synthetic assembling, press said structure assembling (like Fig. 1) and become the synthetic assembling of indirect heating type.
When described synthetic assembling is used for the synthetic of gem grade diamond; The interior material filling mode of metal cup (heating of holding concurrently) is: particle diameter is loaded in metal cup with overlapped way less than 50 microns gem grade diamond micro mist and chip catalyst; Densified under 200-400MPa pressure, assembling becomes synthetic assembling then.
Synthetic assembling after the assembling can be used for the synthetic of gem grade diamond: the synthetic assembling after will assembling, be positioned in the cubic apparatus synthesis press, and follow procedure is raised to desirable value with pressure and temperature, keeps 10-240 hour.The gained synthetic rod through electrolysis, fragmentation, screening get final product product.
Embodiment 1
Synthetic assembling in the cubic apparatus diamond press of cavity diameter 23mm comprises:
The pyrophyllite powder briquetting, size 38mm
3Liner dolomite sleeve pipe, centre are the cylindrical synthetic chamber of diameter 23mm
Aluminium oxide ceramics high temperature protection pipe: wall thickness 5mm, interior outward through 23mm through 13mm, height 11.6 mm
Metal cup: metal molybdenum, wall thickness 0.2mm, outward through 13mm, height 11.6mm
Refractory metal conducting strip: metal molybdenum, thickness 0.2mm, diameter 23mm
Composite conducting plug: box hat: thickness 3mm, outward through 23mm, height 13mm
Fill in the box hat: aluminium oxide ceramics disk, diameter 17mm, thickness 5mm
Dolomite disk: diameter 17mm, thickness 5mm
Be assembled into synthetic assembling, fill synthetic stem stem in the metal cup.
Synthetic assembling is positioned in the cubic hinge press, and follow procedure is raised to pressure and temperature desirable value and is retained to generated time.The gained synthetic rod through electrolysis, fragmentation, screening get final product product.
Synthesis condition: 1450 ℃ of temperature; Pressure 52000 atmospheric pressure (with bismuth silk phase transformation estimation); Generated time 55 hours.
Synthetic stem stem: use raw material to be W14 diadust 2.8g, 4 of iron-nickel accelerant sheet; Load in metal cup by overlapped way, densified under 200-400MPa pressure.
Products obtained therefrom: above diamond single crystal 1.61 grams of diameter 1mm, the largest particles diameter 2.8mm.
Embodiment 2
Synthetic assembling in the cubic apparatus diamond press of cavity diameter 23mm comprises:
The pyrophyllite powder briquetting, size 38mm
3Liner dolomite sleeve pipe, centre are the cylindrical synthetic chamber of diameter 23mm
Aluminium oxide ceramics high temperature protection pipe: wall thickness 5mm, interior outward through 23mm through 13mm, height 11.6 mm
Metal cup: metal molybdenum, wall thickness 0.2mm, outward through 13mm, height 11.6mm
Refractory metal conducting strip: metal molybdenum, thickness 0.2mm, diameter 23mm
Composite conducting plug: box hat: thickness 3mm, outward through 23mm, height 13mm
Fill in the box hat: aluminium oxide ceramics disk: diameter 17mm, thickness 5mm
Dolomite disk: diameter 17mm, thickness 5mm
Be assembled into synthetic assembling, fill synthetic stem stem in the metal cup.
Synthetic assembling is positioned in the cubic hinge press, and follow procedure is raised to pressure and temperature desirable value and is retained to generated time.The gained synthetic rod through electrolysis, fragmentation, screening get final product product.
Synthesis condition: 1450 ℃ of temperature; Pressure 52000 atmospheric pressure (with bismuth silk phase transformation estimation); Generated time 76 hours.
Synthetic stem stem: use raw material to be W14 diadust 2.8g, 4 of iron-nickel accelerant sheet; Load in metal cup by overlapped way, densified under 200-400MPa pressure.
Products obtained therefrom: above diamond single crystal 1.79 grams of diameter 1mm, the largest particles diameter 3.0mm.
Embodiment 3
Synthetic assembling is identical with embodiment 1, prolongation generated time to 96 hour.
Synthesis condition: 1450 ℃ of temperature; Pressure 52000 atmospheric pressure (with bismuth silk phase transformation estimation); Generated time 96 hours.
Synthetic stem stem: use raw material to be W14 diadust 2.8g, 4 of iron-nickel accelerant sheet; Load in metal cup by overlapped way, densified under 200-400MPa pressure.
Products obtained therefrom: the above diamond single crystal of diameter 1mm: 1.91 grams, the largest particles diameter 3.2mm.
Embodiment 4
Synthetic assembling in the cubic apparatus diamond press of cavity diameter 23mm comprises:
Briquetting size: 38mm
3Liner dolomite sleeve pipe, centre are the cylindrical synthetic chamber of diameter 23mm
Aluminium oxide ceramics high temperature protection pipe: wall thickness 5mm, interior outward through 23mm through 13mm, height 11.6 mm
Metal cup: metal tantalum, wall thickness 0.2mm, outward through 13mm, height 11.6mm
Refractory metal conducting strip: metal tantalum, thickness 0.2mm, diameter 23mm
Composite conducting plug: box hat: thickness 3mm, outward through 23mm, height 13mm
Fill in the box hat: aluminium oxide ceramics disk, diameter 17mm, thickness 5mm
Dolomite disk: diameter 17mm, thickness 5mm.
Synthesis condition is identical with embodiment 1, products obtained therefrom: above diamond single crystal 1.62 grams of diameter 1mm, the largest particles diameter 2.8mm.The electrolytic treatments speed of synthetic piece is very slow, needs electrolysis of fluorides matter to do electrolyte.
Embodiment 5
Basic identical with embodiment 4, metal cup and metallic conduction sheet adopt niobium.Because metal niobium is softer relatively, the easy moulding of metal cup.
Synthesis condition is identical with embodiment 1, products obtained therefrom: above diamond single crystal 1.60 grams of diameter 1mm, the largest particles diameter 2.8mm.The metal tube present situation remains intact, and deformation is even, the electrolytic treatments rapid speed of synthetic piece.
Embodiment 6
Basic identical with embodiment 4, metal cup and metallic conduction sheet adopt tungsten.Because tungsten hardness is big, metal cup can not be used punch forming.Adopt the argon arc welding procedure to make metal cup.
Removing temperature in the synthesis condition is 1700 ℃, and other condition is identical with embodiment 1, products obtained therefrom: above diamond single crystal 1.80 grams of diameter 1mm, the largest particles diameter 3.0 mm.The metal tube present situation remains intact, and deformation is even, the electrolytic treatments rapid speed of synthetic piece.It is favourable to improving electrolytic speed that electrolyte contains organic acid.
Claims (6)
1. the synthetic assembling of indirect heating type during the artificial monocrystalline of cubic hinge press HTHP synthesizes; Comprise pyrophyllite powder briquetting (1); In the liner dolomite sleeve pipe (2), dolomite sleeve pipe (2) is cylindrical synthetic chamber, it is characterized in that; Comprise the cylindric metal cup of processing with metal niobium, tantalum, molybdenum or tungsten (7) in the dolomite sleeve pipe (2); Cylinder outerwrap aluminium oxide ceramics high temperature pipe (3), described aluminium oxide ceramics high temperature pipe (3) is an aggregate with the а-aluminium oxide and the talcum of mass percent 75～90%:10～25%, makes through 850-1200 ℃ of sintering; Described metal cup (7) both sides are provided with metallic conduction sheet (5) respectively and are connected with metal cup (7); By composite conducting plug (4) sealing, composite conducting plug (4) is connected with metallic conduction sheet (5) respectively at dolomite sleeve pipe (2) two ends.
2. the synthetic assembling of indirect heating type according to claim 1 is characterized in that described aluminium oxide ceramics high temperature pipe (3) wall thickness is 3-8mm, and internal diameter and metal cup (7) external diameter is complementary, and height is identical with metal cup (7); External diameter and dolomite sleeve pipe (2) internal diameter are complementary.
3. the synthetic assembling of indirect heating type according to claim 1; It is characterized in that; Described aluminium oxide ceramics high temperature pipe (3) adopts following method preparation: according to mass percent а-aluminium oxide: talcum=75～90%:10～25% preparation aggregate; Add the binding agent polyvinyl alcohol of aggregate quality 1～4%, make slurry through wet ball grinding technology, the slurry mist projection granulating makes ceramic powder; With ceramic powder compression moulding, 850-1200 ℃ of sintering makes described ceramic high temperature pipe again.
4. the synthetic assembling of indirect heating type according to claim 1 is characterized in that described metallic conduction sheet (5) adopts metal niobium, tantalum, molybdenum or tungsten, is diameter and the identical disk of aluminium oxide ceramics high temperature pipe (3) external diameter.
5. the synthetic assembling of indirect heating type according to claim 1; It is characterized in that described composite conducting plug (4) comprises cylindrical conductive shell, thickness >=3mm; External diameter is identical with aluminium oxide ceramics high temperature pipe (3) external diameter, fills heat Insulation film in the external conductive casing; External conductive casing is connected with metallic conduction sheet (5) conduction.
6. the synthetic assembling of indirect heating type according to claim 5 is characterized in that described heat Insulation film is the heat Insulation film of two stacks; A slice is an aggregate for а-aluminium oxide and the talcum with mass percent 75～90%:10～25%; The 850-1200 ℃ of aluminium oxide ceramics disk that sintering forms, another sheet is the dolomite disk, wherein the aluminium oxide ceramics disk is thick is 3-8mm; Diameter >=metal cup (7) external diameter, and contact with metallic conduction sheet (5).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210087887.3A CN102600768B (en) | 2012-03-30 | 2012-03-30 | Indirect heating-type synthesis assembly for high-temperature and high-pressure artificial single crystal synthesis by using cubic press |
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| CN201210087887.3A CN102600768B (en) | 2012-03-30 | 2012-03-30 | Indirect heating-type synthesis assembly for high-temperature and high-pressure artificial single crystal synthesis by using cubic press |
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| CN102600768A true CN102600768A (en) | 2012-07-25 |
| CN102600768B CN102600768B (en) | 2014-03-05 |
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| CN201210087887.3A Expired - Fee Related CN102600768B (en) | 2012-03-30 | 2012-03-30 | Indirect heating-type synthesis assembly for high-temperature and high-pressure artificial single crystal synthesis by using cubic press |
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| CN108940125A (en) * | 2018-06-13 | 2018-12-07 | 燕山大学 | It is a kind of to prepare Al13Fe3The method of single crystal grain |
| CN111659318A (en) * | 2020-06-15 | 2020-09-15 | 山东聊城君锐超硬材料有限公司 | Assembly block for high-temperature and high-pressure modification of diamond cultivated by CVD and modification method |
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| CN111659318B (en) * | 2020-06-15 | 2023-10-27 | 山东聊城君锐超硬材料有限公司 | Assembled block for high-temperature high-pressure modification of CVD cultivated diamond and modification method |
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| CN102600768B (en) | 2014-03-05 |
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