CN101205628A - Sapphire crystal growth method - Google Patents
Sapphire crystal growth method Download PDFInfo
- Publication number
- CN101205628A CN101205628A CNA2006101677734A CN200610167773A CN101205628A CN 101205628 A CN101205628 A CN 101205628A CN A2006101677734 A CNA2006101677734 A CN A2006101677734A CN 200610167773 A CN200610167773 A CN 200610167773A CN 101205628 A CN101205628 A CN 101205628A
- Authority
- CN
- China
- Prior art keywords
- alumina
- crystal
- sapphire
- particle
- aluminum oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention discloses a growing method of sapphire crystal, which includes the steps that: alumina powder is crushed and grinded to ultra-micro powder particles; alumina particles are purified until the purity over 99.999 percent; the grinded and purified alumina with solvent is churned into pulpous state, pressed with a high pressure pump, delivered to a prilling nozzle, and sprayed into a high temperature drying tower, the pulpous state alumina which is sprayed from the prilling nozzle is dried into alumina particles and collected, and added with organic binder. The pure alumina powder particles are arranged in a mould, and added with the organic binder, and forms a body on a forcing press; the body is fired into an alumina block in half-done state in advance, arranged in a vacuum super-high-temperature furnace for preburning, thereby exhausting impure gas; the furnace is vacuumized and introduced with inert gas, and the alumina in half-done state is heated into liquid state, until the crystal growth is completed, and is solidified, cooled and contracted into monocrystal sapphire. The invention saves time for crystal growing, has low cost, is not limited in quality and size of the crystal, and fulfills the requirement of optic components, semiconductor components, communication components and other components.
Description
Technical field
The present invention relates to a kind of sapphire crystal growth method, belong to monocrystalline sapphire (alumina single crystal) crystal growing technology field,
Background technology
At present, single crystal sapphire substrate is very important in the utilization of modern science and technology product, photodiode (LED) with opto-electronics is an example, the investigation of materials of gan (GaN) is above 20 years, but always because the substrate (Substrate) that does not have lattice parameter to cooperate, so crystal is long bad, and p type gan is difficult for making, so make slow progress, these problems are until nineteen eighty-three, the loyal doctor's Shi human aluminium nitride (AlN) such as (S.Yoshida) in the field of Japan is grown up with high temperature earlier on sapphire (Sapphire) substrate and is done buffer layer, again thereon during growing gallium nitride, crystallization is better, red rugged brave professor people such as (I.Akasaki) discovery of Nagoya University afterwards uniformly at the thin aluminium nitride of the long one deck of low temperature (about 600 ℃), can obtain the material of picture minute surface with organo-metallic vapour deposition process (MOCVD or OMVPE) thereon again with high temperature (about about 1000 ℃) gallium nitride growth.1991 Nian Riya companies (Nichia Co.) researcher's Shuji Nakamuras (S.Nakamura) are used noncrystal gan instead and are grown into buffer layer (Buffer Layer) earlier with low temperature, during again with the high temperature gallium nitride growth, also obtain smooth film as the minute surface.Another problem of how being p-GaN also obtains to break through, people such as red rugged brave professor at first were entrained in magnesium (Mg) and make its growth in the gan in 1989, carry out the electron beam irradiation after growing up to and obtain p type gan, the back future, the Shuji Nakamura of inferior company was found electron beam, but be that the temperature of gan is raise, hydrogen among the Ma-H is separated and the magnesium acceptor is produced low-impedance gan by sensitization, if he finds also hydrogen to be driven away with about 700 ℃ thermal annealing, make the magnesium sensitization and finish the work of p type.Utilize above two discoveries, Ri Ya company announced successfully to develop the GaN blue light-emitting diode (LED) of luminosity one candle light (Cd) in 1993, and the life-span reaches tens thousand of hours.After this message is delivered, cause global attention at once, the existing a lot of groups in all parts of the world are in manufacturing, character and the application of this type of material of research at present.With the TaiWan, China patent is example, invents the I245440 name and is called photodiode patent (with reference to patent announcement on December 11st, 2005), and it includes: a substrate; One nucleating layer is arranged on this substrate, and is formed by AlxGa1-xN, to solve the unmatched phenomenon of lattice, wherein 0≤x≤1; One buffer layer is arranged on this nucleating layer; One n type contact layer is arranged on this buffer layer, and is electrically connected at a n type electrode, and this n type contact layer is formed by n-AlxGa1-xN, wherein 0≤x≤0.3; One n type coating is arranged on this n type contact layer, and is formed by n-AlxGa1-xN, wherein 0≤x≤0.3; One luminescent layer is arranged on this n type coating layer; One p type barrier layer is formed on this luminescent layer, prevents the carrier overflow, and this p type barrier layer is formed by p-AlxGa1-xN, wherein 0≤x≤0.4; One p type coating is formed on this p type barrier layer, and with the limitation carrier, this p type coating is formed by p-AlxGa1-xN, wherein 0≤x≤0.3; And a p type contact layer, be to be positioned on this p type coating, and be electrically connected at a p type electrode that this p type contact layer is formed by p-AlxGa1-xN, wherein 0≤x≤0.15; Wherein, when applying a suitable forward bias voltage drop in this n type electrode and this p type electrode, can excite this luminescent layer to produce wavelength is the how light output of rice of 300-380.And wherein this substrate is to be selected from by sapphire substrate, silicon substrate, silicon carbide substrate, gallium nitride base board, aluminium nitride substrate, aluminium gallium nitride alloy substrate and zinc oxide substrate institute to become one of combination.And, be fit closely baseplate material, so also important with regard to especially of the technology that grows up to of sapphire substrate because lattice and the gan of sapphire substrate (alumina single crystal) is very approaching.
In addition, produces the main gordian technique of sapphire substrate and be in 2050 ℃ of high temperature alumina powder to be melted and growing crystal, and the long crystal method of sapphire includes following several substantially usually:
Flame melting method (Flame Fusion): the flame melting method is to utilize hydrogen, oxygen combustion pyritous torch, the aluminum oxide powder that drops is from top to down melted, liquid melts and drops on the crystal seed that lower wall accepts and solidify, and the change as growing up just like the stalagmite in the stalactite grotto is big.This kind alumina single crystal maximum can reach 3 centimetres of diameters, but bubble may be contained in its inside, and flaws such as aluminum oxide powder that does not melt and residual stress, so only be applicable to the purposes such as sapphire glass, sapphire gear (Gear) and ornament on wrist-watch surface.The sapphire factory of this kind of world production gains fame and fortune in Europe, and for example Fa Guo Bircon is well-known.
The method of fluxing (Flux Growth): the rule of fluxing is to utilize fusing assistant, as plumbous oxide, aluminum fluoride and Sodium Fluoride etc., aluminum oxide is being lower than 2050 ℃ of dissolvings, slowly cools off via liquid again, and supersaturation is separated out.This kind method is the method that novel material is cultivated in the traditional experiment chamber, is not suitable for the volume production of industry member.Be the company that produces ornaments such as jewel with this at present, as U.S. JO Crystal and Chatham.
Czochralski method (Czochralski method): Czochralski method is to utilize graphite resistance or the heating of induced method, the aluminum oxide powder that is contained in crucible is melted under passivity gas or in the vacuum, again the sapphire crystal seed is fallen at leisure from top to bottom, contact liquid level slightly, the rotation slowly of crystal seed this moment, and upwards drawing goes out sapphire crystal seed.The size of its diameter and quality then decide according to the speed and the liquid level temperature controlling that draw high, and this method is fit to industrial production, and there are companies such as the Union Carbide of the U.S. and Canadian Crystar in well-known in the world production firm.
Thermal gradient method (Thermal Gradient Technique): thermal gradient is to be formed in research and development in 1978 by U.S. Crystal systems company, and has applied for patented technology.It is with directional crystal inductive melt single crystal method, comprise the crucible, heating element and the shielding unit that are placed in the simple bell-jar vacuum resistance furnace, still, there is molybdenum polution in this law crystal growing process, other impurity is mainly introduced by raw material, the essential high-purity raw that adopts.
Guided mode method (Edge-defined Film-fed Growth EFG): the brilliant equipment unit of length of EFG guided mode method, be similar to Czochralski method, but its crystal does not rotate in growth, and diameter of upwards drawing and shape, is controlled by a metal pattern (Die) that is suspended in the aluminum oxide liquid level.It has great pulling rate, can produce the circle crystal column or the flat chip of hollow.Good in economic efficiency, but crystal contains highdensity residual stress and difference row (dislocation), is suitable for optical applications but not semiconductor substrate.The Kyocera that main in the world production company is a Japan.
The Kyropoulos:Kyropoulos method utmost point is similar to Czochralski method, but its crystal does not utilize rotation, unfavorable using to regard it as the control diameter in growth, and solidifies cooling and contraction in crucible.The crystalline size that grows up at last is slightly less than crucible, so must be through numerous and diverse post-treatment to reach final diameter.
The monocrystalline sapphire that the above long crystal method of sapphire is grown, have contaminating impurity or its crystal mass and size and all be restricted, be difficult to satisfy the long long disappearance of brilliant needs time of high performance requirements, cost height and high temperature of assemblies such as optics, semi-conductor, communication.More than be the disappearance of existing technology maximum, in fact the technical barrier of demanding urgently overcoming for industry.
Summary of the invention
In view of this, main purpose of the present invention is to provide lower, crystal mass of long brilliant time of a kind of saving monocrystalline sapphire, cost and size unrestricted, and the monocrystalline sapphire quality can satisfy the high performance requirements of assemblies such as optics, semi-conductor, communication.
For achieving the above object, technical scheme of the present invention is achieved in that a kind of sapphire crystal growth method, the steps include: alumina powder is ground to the ultrafine powder particle through pulverizing, chemical assistant; The above purity of alumina purifying particle to 99.999%; Add an amount of solvent and stir the group Pu with brute force and stir into pulpous state being ground to ultrafine powder particle and aluminum oxide through purifying to 99.999% above purity, again the pulpous state aluminum oxide is pressurizeed with high pressure group Pu, send into the granulation nozzle, be ejected in the high temperature drying tower, utilize the pulpous state aluminum oxide of the warm air of high speed hot-fluid in the tower with the ejection of granulation nozzle, wink-dry becomes aluminium oxide particles of uniform size and collection; Add organic binder again; Described pure alumina powder is placed mould, add a small amount of organic binder again after, pressurization forms the base substrate of predetermined shape on pressing machine; To be scheduled to profile aluminum oxide base substrate earlier and burn till the alumina block of some semi-ripe condition in advance, insert pre-burning in the special High Temperature Furnaces Heating Apparatus of a vacuum, eliminate small organic matter, impurity, bubble etc., form closely knit proportion, described vacuum extra-high-speed temperature stove and accessory has gas discharge outlet, and impure gas is discharged; Then with described vacuum extra-high-speed temperature stove evacuation and import rare gas element, and improve temperature, the alumina block of some semi-ripe condition is heated to molten soup state, finish and solidify, cool off, be shrunk to monocrystalline sapphire until long crystalline substance.
Above-mentioned alumina lap becomes tens of how ultrafine powder particles of rice, to save the long brilliant time of follow-up high temperature and to improve crystal mass.
Above-mentioned how ground rice body secondary is at low temperatures assembled particle for tens of microns, and has original how ground rice body size, and filters thus and remove impurity, purifying alumina particle.
The technique effect that the present invention produces is as follows:
1. utilization the inventive method, thermograde is opposite with gravity direction during crystal growth, and crucible, crystal and heating element do not move the melt-flow that this can be avoided thermal convection and mechanical movement to produce.
2. utilization the inventive method after the crystal growth, is surrounded by melt, still is in the hot-zone, so just can control its rate of cooling, reduce thermal stresses, and thermal stresses is the principal element that produces crystal crackle and dislocation.
3. utilization the inventive method, during crystal growth, solid-liquid interface is among the melt encirclement, and the thermal perturbation of bath surface and mechanical disturbance can be reduced by melt even eliminate before arriving solid-liquid interface like this, so effect very important to the crystal tool of growing high-quality.
4. utilization the inventive method, crystal mass and size are unrestricted, and quality can satisfy the high performance requirements of assemblies such as optics, semi-conductor, communication, and cost is comparatively cheap, saves the long brilliant time of monocrystalline sapphire.
Description of drawings
Fig. 1 is the sapphire growth sintering oven structural representation of present embodiment.
Embodiment
The step that sapphire crystal growth method of the present invention is implemented is as follows:
Grind: with aluminum oxide (Al
2O
3) powder through pulverize, chemical assistant is ground to the ultrafine powder particle, the ultrafine powder particle of for example tens of how rice.Pulverize and a small step of grinding to not lacking on the powder making processes, pulverizing is normal to be working in advance of grinding, or claims to roughly grind, and grinds then general term and obtains the step that particle diameter is lower than millimeter.To pulverizing speech, the pulverizer kind is more; Concerning grinding, then generally many is means with the ball milling.For the traditional ceramics powder, pulverizing with grinding operation is the only effective means of this powder of acquisition.But for ceramic powder of new generation, pulverize with grinding operation and may contain many-sided purpose, comprising: break up aggregate, reduce aggregate, or make the powder that constitutes powder become terminal particle (Ultimate Particles); Reduce diameter of particle, eliminate too coarse particles, and make size-grade distribution in certain scope, meet suitable granularity and size-grade distribution and require specification.A large amount of finess obviously can increase the specific surface area and the reactive behavior of powder.Can uniform mixing between powder, between powder and solvent, from physical angle, pulverizing is a kind of switching process of energy.Be the kinetic energy of size reduction machinery or the mechanical work of being done, by and powder between bump, roll, rub, powder smashed, break or grind corner angle etc., the powder specific surface is increased, thereby the surface free energy increase, pulverizing thus is the energy conversion process that a kind of mechanical energy changes surface energy into.Whether every physicals that the Chemical Composition of powder is related to alumina-ceramic can be guaranteed, and the impure situation in the material also has influence in various degree to the sintering process of back.Granularity and structure major decision the density and the formability thereof of base substrate.Granularity is thinner, structure is more imperfect, and then it is active bigger, more helps agglomerating and carries out.And because the contact of particle is counted and square being inversely proportional to of particle radii in the unit volume, thereby particle radii reduce, and the speed of diffusion mass transfer process obviously increases.On the other hand, finer particles, surface-area is big more, thereby just increase of the influence of surface diffusion, and surface diffusion is more faster than bulk diffusion.Moreover sintering rate is determined by motivating force, rate of mass transfer and this three of contact area, and they are all closely related with the particle diameter of powder.Therefore, can effectively save the long brilliant time of high temperature and the raising crystal mass of back.
Purify: no matter the above purity of alumina purifying particle to 99.999% of gettinging rid of the weed and keep the flower of the leek, pottery adopt natural still synthesis material, and its purity is generally all on the low side.So homogeneity, stability and the reliability of its quality are all poor than metal and macromolecular material, therefore the above purity of alumina purifying particle to 99.999% of the present invention improve homogeneity, stability and the reliability of material, prepares against required.
Mist projection granulating: will be ground to ultrafine powder particle and aluminum oxide and add an amount of solvent and stir the group Pu with brute force and stir into pulpous state through purifying to 99.999% above purity, again the pulpous state aluminum oxide is pressurizeed with high pressure group Pu, send into the granulation nozzle, be ejected in the high temperature drying tower, utilize the pulpous state aluminum oxide of the warm air of high speed hot-fluid in the tower with the ejection of granulation nozzle, wink-dry becomes aluminium oxide particles of uniform size and collects, how the commercialization of ground rice body is used, it is gordian technique that powder is collected, how ground rice is known from experience in air suspends and the suction human body, cause the problem of Health hazard, and high temperature mode commonly used, assemble collection and how can to make the ground rice body assemble and become big, thereby how to lose meter ruler cun.In the method for the invention, utilization low temperature is made and how to be collected the ground rice body, can be effectively at low temperatures secondary assemble particle for tens of microns, can possess original how ground rice body size simultaneously, and filter removal impurity with this, purifying aluminum oxide powder, according to the high-purity mangesium oxide aluminium powder form that this law is made, its foreign matter content is very low, and diameter of particle is also little, have superior physics and chemical property, use in order to crystal raw material.
Add organic binder: add organic binder.
Moulded section: be pressed into predetermined profile, the characteristics of moulded section are that cakingagent content is lower, have only ten thousand/several, not directly pre-burning of drying, and base substrate shrinks little, but and automatic production.The pure aluminum oxide powder that aforementioned mist projection granulating is finished places mould, add a small amount of organic binder as described above, pressurization forms the base substrate of predetermined shape on pressing machine, the essence of moulded section is under the effect of external force, and particle is close mutually in mould, and borrows internal friction securely each particle to be connected, keep certain shape, the technology of moulded section is simple, and is easy to operate, and the cycle is short, the efficient height, be convenient to realize automatic production, in addition, blank density is big, size is accurate, shrink little, physical strength height, the advantage of good electrical property.
Crystal grows up to: the alumina block (cake) of earlier the predetermined profile aluminum oxide base substrate of preceding processing procedure being burnt till in advance some semi-ripe condition, this material is inserted pre-burning in the special High Temperature Furnaces Heating Apparatus of a vacuum, calcined temperature can be set in more than 1600 ℃, and the small organic matter of the elimination of mat, impurity, bubble etc., and produce closely knit proportion, owing to organic matter, impurity etc. all are lighter weight and easily flotation usually, so can in high temperature, remove, this vacuum extra-high-speed temperature stove and accessory has gas discharge outlet, so that impure gas is smoked discharge; Then with vacuum extra-high-speed temperature stove evacuation and import rare gas element, and improve temperature, the alumina block of some semi-ripe condition is heated to molten soup state, finish and solidify, cool off, be shrunk to monocrystalline sapphire until long crystalline substance.
Include crucible, heating element and shielding unit, the refrigerating unit made from materials such as molybdenum, zirconium, platinums in the special High Temperature Furnaces Heating Apparatus of vacuum of the present invention, design temperature is about 2040～2100 ℃, required time apparent volume and deciding, time that can be more about one times than the saving of prior art, relatively also saved one times energy consumption, and cost is lower, crystal mass and size are unrestricted, and quality can satisfy the high performance requirements of assemblies such as optical module, semi-conductor, communication.
Sapphire growth sintering oven of the present invention is as follows: as shown in Figure 1, it comprises outer stove 1, should outer stove 1 have between the thermal capacitance of adding 10 and be installed with interior stove 2, add between thermal capacitance 10 inner edge and be provided with heating unit 11, the top is provided with the secondary combustion chamber 13 of tool heating unit 12, this secondary combustion chamber 13 connects the cooling particle collector 3 with air exhausting device 30, will be through the gas cooling after secondary combustion chamber 13 perfect combustions, and having reached emission standard and can be discharged from after the impurity filtering.
As shown in Figure 1, sapphire growth sintering oven also comprises interior stove 2, should include a siege 20 by interior stove 2, siege 20 bottoms are provided with thermofin 21 and cooling-cycle device 22, and siege 20 upper ends are provided with heating unit 23, siege 20 and thermofin 21 outer rims are provided with inner furnace body 24, but inner furnace body 24 is these tightness system 25 sealings in use, and inner furnace body 24 is detachable with siege 20, and by tightness system 25 sealings, tightness system is blocking the internal atmosphere gas leak, generally adopts the silicone rubber kinds material to make.This inner furnace body 24 also can be provided with coupling apparatus 26 in addition with tightness system 25, present embodiment connects (also available bolt connects) with rapid-acting coupling, but sharp separation inner furnace body 24 and siege 20, should be provided with inlet pipe 27 by interior stove 20, outer rim is provided with vapor pipe 28 with one heart in the top of this inlet pipe 27, the external diameter of this vapor pipe 28 is greater than inlet pipe 27, and its length is less than inlet pipe 27, and by the inlet pipe inlet mouth 270 introduction atmosphere gas of being located at central authorities, and the back atmosphere gas is used in the discharge of vapor pipe venting port 280, make the atmosphere gas circulation in the inner furnace body 24 good, and then reach the effect of soaking, with production high quality oxide artificial lens.
Sapphire growth sintering oven is applied to sapphire crystal, and to grow up to process as follows: monocrystalline sapphire is that the oxide compound artificial lens is a kind of, to be scheduled to profile aluminum oxide base substrate earlier and insert pre-burning on the siege 20, calcined temperature can be set in more than 1600 ℃, can burn till the alumina block (cake) of some semi-ripe condition in advance, can eliminate small organism, impurity, bubble etc., and produce closely knit proportion, because organism, impurity etc. all are lighter weight and easily floating usually, so can in high temperature, remove, and pass through air exhausting device 30 with impure air importing secondary combustion chamber 13, under the high temperature with impurity perfect combustion, again through the cooling particle collector 3 will be through the gas cooling after secondary combustion chamber 13 perfect combustions, reach emission standard after the impurity filtering and be discharged from.To be somebody's turn to do the alumina block of finishing through pre-burning again and insert a crucible (not shown), in order to obtain the sapphire crystal growth correct orientation, bottom surface at this crucible is provided with seed crystal, and this crucible placed on the siege 20, and inner furnace body 24 combined by coupling apparatus 26 with siege 20, at present embodiment, coupling apparatus 26 is rapid-acting coupling, then inner furnace body 24 is vacuumized and imports rare gas element, improve temperature simultaneously, the alumina block of some semi-ripe condition is heated to dissolved state, finish and solidify until long crystalline substance, cooling, be shrunk to monocrystalline sapphire, thermofin 21 that siege 20 bottoms are provided with and cooling-cycle device 22 then are used for cooling, avoid seed crystal and tightness system 25 to burn.
The above is preferred embodiment of the present invention only, is not to be used to limit protection scope of the present invention.
Claims (3)
1. a sapphire crystal growth method is characterized in that, step is: alumina powder is ground to the ultrafine powder particle through pulverizing, chemical assistant; The above purity of alumina purifying particle to 99.999%; Add an amount of solvent and stir the group Pu with brute force and stir into pulpous state being ground to ultrafine powder particle and aluminum oxide through purifying to 99.999% above purity, again the pulpous state aluminum oxide is pressurizeed with high pressure group Pu, send into the granulation nozzle, be ejected in the high temperature drying tower, utilize the pulpous state aluminum oxide of the warm air of high speed hot-fluid in the tower with the ejection of granulation nozzle, wink-dry becomes aluminium oxide particles of uniform size and collection; Add organic binder again; Described pure alumina powder is placed mould, add a small amount of organic binder again after, pressurization forms the base substrate of predetermined shape on pressing machine; To be scheduled to profile aluminum oxide base substrate earlier and burn till the alumina block of some semi-ripe condition in advance, insert pre-burning in the special High Temperature Furnaces Heating Apparatus of a vacuum, eliminate small organic matter, impurity, bubble etc., form closely knit proportion, described vacuum extra-high-speed temperature stove and accessory has gas discharge outlet, and impure gas is discharged; Then with described vacuum extra-high-speed temperature stove evacuation and import rare gas element, and improve temperature, the alumina block of some semi-ripe condition is heated to molten soup state, finish and solidify, cool off, be shrunk to monocrystalline sapphire until long crystalline substance.
2. sapphire crystal growth method as claimed in claim 1 is characterized in that, described alumina lap becomes tens of how ultrafine powder particles of rice, to save the long brilliant time of follow-up high temperature and to improve crystal mass.
3. sapphire crystal growth method as claimed in claim 2 is characterized in that, described how ground rice body secondary is at low temperatures assembled particle for tens of microns, and has original how ground rice body size, and filters thus and remove impurity, purifying alumina particle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101677734A CN101205628A (en) | 2006-12-18 | 2006-12-18 | Sapphire crystal growth method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101677734A CN101205628A (en) | 2006-12-18 | 2006-12-18 | Sapphire crystal growth method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101205628A true CN101205628A (en) | 2008-06-25 |
Family
ID=39566102
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006101677734A Pending CN101205628A (en) | 2006-12-18 | 2006-12-18 | Sapphire crystal growth method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101205628A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011184A (en) * | 2010-12-29 | 2011-04-13 | 四川鑫通新材料有限责任公司 | Production method of alpha-aluminum oxide single crystal |
| CN102011185A (en) * | 2010-12-29 | 2011-04-13 | 四川鑫通新材料有限责任公司 | Method for artificially synthesizing sapphire |
| CN102168886A (en) * | 2010-12-30 | 2011-08-31 | 河南农业大学 | Combustion furnace for flue-cured bulk curing barn |
| CN102233606A (en) * | 2011-06-30 | 2011-11-09 | 张君芳 | Method for manufacturing alumina single crystal blocky raw material |
| CN102603273A (en) * | 2012-03-10 | 2012-07-25 | 锦州晶城新能源材料制造有限公司 | Preparation method of high-purity sintered alumina for monocrystal sapphire growth |
| CN102634845A (en) * | 2012-02-07 | 2012-08-15 | 徐州协鑫光电科技有限公司 | Method for heating and melting materials in growth of sapphire single crystals by Kyropoulos method and application thereof |
| CN102674418A (en) * | 2012-05-24 | 2012-09-19 | 大连海蓝光电材料有限公司 | Method for preparing high-purity alumina particles |
| CN107829132A (en) * | 2017-10-10 | 2018-03-23 | 上海应用技术大学 | A kind of method for preparing alumina single crystal |
| CN114408954A (en) * | 2022-01-26 | 2022-04-29 | 株洲科能新材料股份有限公司 | Preparation method of single crystal alumina micro powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1102680A (en) * | 1994-01-23 | 1995-05-17 | 易育宁 | Stone slab building |
| CN1103679A (en) * | 1993-09-24 | 1995-06-14 | 通用电气公司 | Solid state thermal conversion of polycrystalline alumina to sapphire |
| CN1727303A (en) * | 2005-06-29 | 2006-02-01 | 上海大学 | Method for fabricating Mg, Ti adulterated Al2O3 crystalline material, and transparent laser ceramics |
-
2006
- 2006-12-18 CN CNA2006101677734A patent/CN101205628A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1103679A (en) * | 1993-09-24 | 1995-06-14 | 通用电气公司 | Solid state thermal conversion of polycrystalline alumina to sapphire |
| CN1102680A (en) * | 1994-01-23 | 1995-05-17 | 易育宁 | Stone slab building |
| CN1727303A (en) * | 2005-06-29 | 2006-02-01 | 上海大学 | Method for fabricating Mg, Ti adulterated Al2O3 crystalline material, and transparent laser ceramics |
Non-Patent Citations (2)
| Title |
|---|
| 张立德: "《超微粉体制备与应用技术》", 30 April 2001 * |
| 王崇鲁: "《白宝石单晶》", 31 March 1983 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011184A (en) * | 2010-12-29 | 2011-04-13 | 四川鑫通新材料有限责任公司 | Production method of alpha-aluminum oxide single crystal |
| CN102011185A (en) * | 2010-12-29 | 2011-04-13 | 四川鑫通新材料有限责任公司 | Method for artificially synthesizing sapphire |
| CN102011185B (en) * | 2010-12-29 | 2013-03-20 | 四川鑫通新材料有限责任公司 | Method for artificially synthesizing sapphire |
| CN102011184B (en) * | 2010-12-29 | 2013-04-10 | 四川鑫通新材料有限责任公司 | Production method of alpha-aluminum oxide single crystal |
| CN102168886A (en) * | 2010-12-30 | 2011-08-31 | 河南农业大学 | Combustion furnace for flue-cured bulk curing barn |
| CN102233606A (en) * | 2011-06-30 | 2011-11-09 | 张君芳 | Method for manufacturing alumina single crystal blocky raw material |
| CN102634845A (en) * | 2012-02-07 | 2012-08-15 | 徐州协鑫光电科技有限公司 | Method for heating and melting materials in growth of sapphire single crystals by Kyropoulos method and application thereof |
| CN102603273A (en) * | 2012-03-10 | 2012-07-25 | 锦州晶城新能源材料制造有限公司 | Preparation method of high-purity sintered alumina for monocrystal sapphire growth |
| CN102603273B (en) * | 2012-03-10 | 2013-12-18 | 锦州晶城新能源材料制造有限公司 | Preparation method of high-purity sintered alumina for monocrystal sapphire growth |
| CN102674418A (en) * | 2012-05-24 | 2012-09-19 | 大连海蓝光电材料有限公司 | Method for preparing high-purity alumina particles |
| CN107829132A (en) * | 2017-10-10 | 2018-03-23 | 上海应用技术大学 | A kind of method for preparing alumina single crystal |
| CN114408954A (en) * | 2022-01-26 | 2022-04-29 | 株洲科能新材料股份有限公司 | Preparation method of single crystal alumina micro powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101205628A (en) | Sapphire crystal growth method | |
| JP5896627B2 (en) | Method for producing crystalline silicon ingot | |
| CN101061065B (en) | Process for producing polycrystalline silicon bar | |
| CN104736746B (en) | The manufacture of improved crystalline silicon | |
| KR101594474B1 (en) | Poly-crystalline silicon ingot, silicon wafer therefrom and method of fabricating poly-crystalline silicon ingot | |
| CN102534756B (en) | Composite crucible and method of manufacturing the same | |
| CN102471926A (en) | Composite crucible, method for producing same, and method for producing silicon crystal | |
| CN103510157A (en) | Induced crystal growth technology for efficient ingot casting | |
| CN101591807A (en) | Directionally solidified casting monocrystalline silicon of nitrating and preparation method thereof | |
| US20190078231A1 (en) | Hybrid crucible assembly for czochralski crystal growth | |
| CN102312291A (en) | Doped casting monocrystalline silicon and preparation method | |
| CN102719881A (en) | Graphite crucible for single crystal furnace | |
| CN101220507A (en) | Method for manufacturing silicon crystal plate for solar battery | |
| JP2008156184A (en) | Method for growing sapphire crystal | |
| CN104499049B (en) | Method for removing polysilicon hard inclusion in ingot casting process | |
| CN100590235C (en) | Method for preparing solar grade silicon | |
| CN102212871A (en) | Growth method for sapphire crystals and crystal growth furnace structure for growing sapphire crystals | |
| CN106987903B (en) | A kind of improved large scale synthetic sapphire production technology | |
| JP2008239438A (en) | Manufacturing process and manufacturing apparatus for spherical crystal | |
| CN202099407U (en) | Crystal growth furnace structure for sapphire crystal growth | |
| CN202688508U (en) | Graphite crucible used for single crystal furnace | |
| JP2007194513A (en) | Manufacturing method for crystal semiconductor particle, and photovoltaic conversion device | |
| JP2009292652A (en) | Production method of crystalline silicon grain | |
| JP4025608B2 (en) | Method for producing granular silicon crystal | |
| CN214458446U (en) | Nested crucible for growing large-size calcium fluoride crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| AD01 | Patent right deemed abandoned |
Effective date of abandoning: 20160720 |
|
| C20 | Patent right or utility model deemed to be abandoned or is abandoned |