CN102776509A - Method for repairing surface of used pyrolytic boron nitride crucible - Google Patents
Method for repairing surface of used pyrolytic boron nitride crucible Download PDFInfo
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Abstract
The invention discloses a method for repairing the surface of a used pyrolytic boron nitride crucible, which comprises the following steps: preparing boron oxide powder and phenolic resin into slurry; uniformly spreading the prepared slurry the surface of the used pyrolytic boron nitride crucible which is cleaned and needs to be repaired, and drying; then, putting the dried pyrolytic boron nitride crucible into a high-temperature furnace to be heated, reacting at a certain condition, and in situ producing a boron nitride coating; and finally, grinding and polishing the surface, and thus obtaining the repaired pyrolytic boron nitride crucible. The method can enable the pyrolytic boron nitride crucible which is subjected to surface repair to be used for growing compound semiconductor single crystals, so the cost is lowered.
Description
Technical field
The present invention relates to a kind of surface repairing method, belong to the semiconductor single-crystal growth equipment technical field with back pyrolysis boron nitride crucible.
Background technology
Artificial crystal growth is as a kind of technology; People are of long duration for its research; Almost can both choose construction method growth of the crystal that nature is produced, artificial-synthetic crystal's experimental technique develops rapidly in recent years, and its principle mainly is to change through the homogeneity heterogenetic to prepare.The crystalline growth method also has a variety of, and actual process of growth depends on the physics of material and the characteristics of chemical property, phasor and method itself.For example slowly method of cooling is that prepared materials is added crucible, makes its fusing then, is incubated the regular hour so that material fully reacts homogenizing, cools off with certain rate of cooling to obtain crystal again; Top-seeded solution growth is a kind of growing technology that combines the melt growth technology of lifting with flux growth method; Be fixed on the seed rod lower end to seed crystal; Drop to slowly with crucible in the saturated solution liquid level contact, and then liquation is slowly cooled off, also can upwards promote seed crystal slowly simultaneously.But the gentle cold process of top-seeded solution growth is the same, all need use high-quality crucible to load melt, and this crucible need satisfy the requirement of the required high thermal resistance of the crystal growth mechanical property required with carrying melt, also need satisfy the requirement of purity aspect.
Crucible material about growing single-crystal requires that good heat conductance and high thermal resistance are arranged, and thermal expansivity is little in the high temperature use, and anxious heat, chilling are had certain anti-strain property.To acid, the erosion resistance of basic soln is stronger, and general normal is platinum (Pt), iridium (Ir), molybdenum (Mo), graphite, SP 1 (BN) or other refractory oxide.Crucible with respect to the preparation of metallic substance such as platinum, iridium, molybdenum; Cost is high; The technology relative complex, and volatilization adds seriously that graphite material prepares and inevitably can introduce impurity in the process of process under the graphite high temperature, can contaminated feedstock with graphite as the crucible of growing single-crystal.Limited the application of plumbago crucible in preparation high quality single crystal field of materials.
Pyrolitic boron nitride (PBN) has high purity, and good resistance to elevated temperatures is arranged, and can keep good lubricating property and thermostability under the high temperature, is again simultaneously the good conductor and the tool insulativity of heat, and many advantages make it become one of appropriate materials of spare-crucible.Pyrolitic boron nitride (PBN) adopts U.S. Pat 3152006 disclosed methods to form through the chemical vapour deposition principle, and this patent disclosure is introduced this paper as a reference.This method comprises the ammonia of proper ratio and gaseous state halogenation boron boron trichloride (BC1 for example
3), boron trichloride (BF
3) steam that waits introduces in the reactor drum that has heated, produces scission reaction, makes BN be deposited on the surface of suitable substrate such as graphite.BN, separates it after the cooling with the form deposition of layer from base material, form the PBN crucible.
But the pyrolitic boron nitride crucible is by the chemical Vapor deposition process preparation, and the production cycle is long, and temperature of reaction is high, and cost is higher.After the PBN crucible uses through crystal growth; Insulating covering agent (environment for use for the PBN crucible mainly is a boron oxide) used during crystal growth can soak into its top layer; When separating the monocrystalline of growth; May cause PBN crucible damage, mainly be the internal surface damage, and this damage mainly comprises: insulating covering agent sticks, surface irregularity, internal surface exfoliated, through check and the fragmentation of crucible local perforations etc.Wherein through check and the fragmentation of crucible local perforations can directly cause the PBN crucible to lose efficacy and can not continue to use; The internal surface exfoliated is looked thickness difference and the different treatment of exfoliation layer, and the PBN crucible was directly discarded when exfoliation layer was thicker does not re-use, and results in greater loss to avoid in the single crystal growth process crucible to lose efficacy; When exfoliation layer was thin, the PBN crucible can continue to use, and took place but reuse also can cause peeling off once more; Damage accumulation; Exfoliation layer thickens, and makes the blocked up or crucible local perforations of exfoliation layer after repeatedly, causes crucible to lose efficacy; Insulating covering agent sticks with minor injury such as surface irregularity does not generally influence the PBN crucible, but repeatedly uses the back damage accumulation, can cause the generation of PBN inner surface of crucible exfoliated.
Generally speaking, the PBN crucible is the damage accumulation of internal surface in use, is to cause the PBN crucible to lose efficacy the major cause that can't reuse.Cause be generally 6-10 time the work-ing life of the PBN crucible that the growth compound semiconductor monocrystal uses thus, therefore if can reduce cost repairing the work-ing life that can prolong the PBN crucible with back PBN inner surface of crucible.
Problem and defective in view of above-mentioned prior art existence; Inventor's dependence practical experience is for many years actively studied with abundant expertise and is innovated; The final surface repairing method with back pyrolysis boron nitride crucible that proposes a kind of lower cost can make PBN crucible after repair on the surface be used for the growth of compound semiconductor single crystal once more.
Summary of the invention
In order to solve the problems referred to above that exist in the prior art, the invention provides a kind of surface repairing method with back pyrolysis boron nitride crucible, can make pyrolitic boron nitride crucible after repair on the surface be used for the growth of compound semiconductor single crystal once more, reduced cost.
In order to solve the problems of the technologies described above, the present invention has adopted following technical scheme:
A kind of surface repairing method with back pyrolysis boron nitride crucible comprises the steps: earlier boron oxide powder and resol to be mixed with slip; Again the slip for preparing evenly is coated on the surperficial and drying with back pyrolysis boron nitride crucible of the needs reparation that cleans up; Then above-mentioned dried pyrolitic boron nitride crucible is placed the high-temperature atmosphere furnace heating, reaction under certain atmospheric condition, original position generates boron nitride coating; At last with the pyrolitic boron nitride crucible after promptly obtaining repairing after the surface finish polishing.
Further, aforesaid surface repairing method with back pyrolysis boron nitride crucible, wherein, boron oxide powder purity is higher than 99.9%, and granularity is less than 0.074 millimeter.
Further, aforesaid surface repairing method with back pyrolysis boron nitride crucible, wherein, the quality of boron oxide powder and resol than scope at 1～5:1.
Further; Aforesaid surface repairing method with back pyrolysis boron nitride crucible; Wherein, The slip employing spread coating, spraying method, spin-coating method or the crystal pulling method that prepare evenly are coated on clean up surperficial with back pyrolysis boron nitride crucible, and coating thickness need make coating cover injured surface fully.
Further; Aforesaid surface repairing method with back pyrolysis boron nitride crucible, wherein, the condition that places high-temperature atmosphere furnace to heat pyrolysis boron nitride crucible after the use that is coated with slip does; Be warming up to 300-500 ℃ with 1-10 ℃/minute; Be incubated 3-24 hour, continue to be warming up to 1100-1600 ℃ of insulation 1-24 hour with 1-10 ℃/minute, original position generates the BN coating.
Further, aforesaid surface repairing method with back pyrolysis boron nitride crucible, wherein will be coated with slip place high-temperature atmosphere furnace to heat with back pyrolysis boron nitride crucible the time, need feeding gas, said gas is nitrogen, ammonia or both gas mixtures.
Further, aforesaid surface repairing method with back pyrolysis boron nitride crucible, wherein, the back pyrolysis boron nitride crucible surface of using that needs to repair adopts water, absolute ethyl alcohol, methyl alcohol or acetone as cleaning medium, or adopts ultrasonic cleaning.
Further, aforesaid surface repairing method with back pyrolysis boron nitride crucible wherein, mixes high-purity boron oxide powder with the ethanolic soln of resol, be configured to boron oxide-resol slurry.
Compared with prior art, beneficial effect of the present invention is:
1, can repair the surface of using back PBN crucible, prolong the work-ing life of PBN crucible;
2, the raw materials cost of this method employing is lower, and preparation temperature is low, and preparation cycle is short, has embodied the characteristic of low-cost and energy-conserving and environment-protective.
Generally speaking; 3-5 back of PBN crucible growing semiconductor compound monocrystal carried out the surface with present method and repaired; Thereafter every use is carried out the one-time surface reparation 2-4 time; Extended to 15 to 20 the work-ing life of PBN crucible, and the interval number of times that specifically carries out repairing on the surface is looked PBN inner surface of crucible degree of impairment and is decided.Because repair layer combines to be weaker than PBN crucible itself with the PBN crucible surface; During PBN crucible generation exfoliated after therefore repairing; Peel off preferentially betide in the repair layer and repair layer and PBN crucible at the interface, also have few part situation can occur in the PBN crucible.The inventive method is for significant with utilizing again of back PBN crucible.
Embodiment
Below in conjunction with specific embodiment the present invention is described in further detail, but not as to qualification of the present invention.
Embodiment 1:
The pyrolitic boron nitride crucible of 4 inches of diameters, wall thickness 1.5mm is used for VGF (VGF) growth GaAs monocrystalline.
After using 4 times continuously, the PBN crucible finds that inner surface of crucible exists the layering of 2 places to peel off, the about 10mm * 10mm of place's area, the about 0.1mm of thickness, the about 15mm * 20mm of another place's area, the about 0.2mm of thickness.It is carried out the 1st subsurface reparation.
1, use acetone, methyl alcohol and deionized water ultrasonic cleaning clean successively on the surface of this PBN crucible, remove the chip and the greasy dirt on surface, dry then;
2, with high-purity oxidation boron powder levigate to 200 orders (0.074 millimeter) with carefully, adding massfraction is the ethanolic soln of 20% resol, is configured to boron oxide-resol slurry, wherein the mass ratio of boron oxide and resol is 4:1;
3, with the boron oxide-resol slip of preparation with crystal pulling method be coated on clean up with back PBN crucible surface, and dry, repeat 2 times with crystal pulling method after, the about 0.1mm of coat-thickness, and fill up the exfoliation layer pit that 2 places are damaged fully;
What 4, will apply boron oxide-resol slip places high-temperature atmosphere furnace with back PBN crucible, feeds nitrogen, with 2 ℃/min, is warming up to 400 ℃, be incubated 4 hours, continues to be warming up to 1200 ℃ of insulations 3 hours with 8 ℃/min original position generation BN coating.Naturally cool to room temperature then, with the PBN crucible for preparing behind the internal surface sanding and polishing after the reparation.The newly-generated about 0.05mm of repair layer thickness.
PBN crucible after continue to use repairing carries out VGF (VGF) GaAs single crystal growing, uses 4 times after, discovery repair layer major part is peeled off, but former PBN crucible part internal surface does not have newfound peeling off, and carries out the 2nd subsurface reparation.
1, use acetone, methyl alcohol and deionized water ultrasonic cleaning clean successively on the surface of this PBN crucible, remove the chip and the greasy dirt on surface, dry then;
2, with high-purity oxidation boron powder levigate to 200 orders with carefully, adding massfraction is the ethanolic soln of 20% resol, is configured to boron oxide-resol slurry, wherein the mass ratio of boron oxide and resol is 5:1;
3, with the boron oxide-resol slip of preparation with crystal pulling method be coated on clean up with back PBN crucible surface, and dry, repeat 3 times with crystal pulling method after, the about 0.15mm of coat-thickness, and fill up the exfoliation layer pit of damage fully;
What 4, will apply boron oxide-resol slip places high-temperature atmosphere furnace with back PBN crucible, feeds nitrogen, with 2 ℃/min, is warming up to 400 ℃, and insulation 4h continues to be warming up to 1200 ℃ of insulations 3 hours with 8 ℃/min, and original position generates the BN coating.Naturally cool to room temperature then, with the PBN crucible for preparing behind the internal surface sanding and polishing after the reparation.The newly-generated about 0.05mm of repair layer thickness.
Continue to use the PBN crucible after repairing to carry out VGF (VGF) GaAs single crystal growing; After using 3 times, discovery repair layer major part is peeled off, and peel off at former PBN crucible part internal surface newly discovered 1 place; Area is about 20mm * 40mm, carries out the 3rd subsurface reparation.
1, use acetone, methyl alcohol and deionized water ultrasonic cleaning clean successively on the surface of this PBN crucible, remove the chip and the greasy dirt on surface, dry then;
2, with high-purity oxidation boron powder levigate to 200 orders with carefully, adding massfraction is the ethanolic soln of 20% resol, is configured to boron oxide-resol slurry, wherein the quality of boron oxide and resol than scope at 3:1;
3, with the boron oxide-resol slip of preparation with crystal pulling method be coated on clean up with back PBN crucible surface, and dry, repeat 3 times with crystal pulling method after, the about 0.15mm of coat-thickness, and fill up the exfoliation layer pit of damage fully;
What 4, will apply boron oxide-resol slip places high-temperature atmosphere furnace with back PBN crucible, feeds nitrogen, with 2 ℃/min, is warming up to 400 ℃, and insulation 4h continues to be warming up to 1200 ℃ of insulations 3 hours with 8 ℃/min, and original position generates the BN coating.Naturally cool to room temperature then, with the PBN crucible for preparing behind the internal surface sanding and polishing after the reparation.The newly-generated about 0.05mm of repair layer thickness.
PBN crucible after continue to use repairing carries out VGF (VGF) GaAs single crystal growing, uses 3 times after, find that the repair layer major part peels off, but former PBN crucible part internal surface does not have newfound peeling off, and carries out the reparation of the 4th surface.
1, use acetone, methyl alcohol and deionized water ultrasonic cleaning clean successively on the surface of this PBN crucible, remove the chip and the greasy dirt on surface, dry then;
2, with high-purity oxidation boron powder levigate to 200 orders with carefully, adding massfraction is the ethanolic soln of 20% resol, is configured to boron oxide-resol slurry, wherein the quality of boron oxide and resol than scope at 1:1;
3, with the boron oxide-resol slip of preparation with crystal pulling method be coated on clean up with back PBN crucible surface, and dry, repeat 3 times with crystal pulling method after, the about 0.15mm of coat-thickness, and fill up the exfoliation layer pit of damage fully;
What 4, will apply boron oxide-resol slip places high-temperature atmosphere furnace with back PBN crucible, feeds nitrogen, with 2 ℃/min, is warming up to 400 ℃, and insulation 4h continues to be warming up to 1200 ℃ of insulations 3 hours with 8 ℃/min, and original position generates the BN coating.Naturally cool to room temperature then, with the PBN crucible for preparing behind the internal surface sanding and polishing after the reparation.The newly-generated about 0.05mm of repair layer thickness.
Continue to use the PBN crucible after repairing to carry out VGF (VGF) GaAs single crystal growing; After using 2 times; Discovery repair layer major part is peeled off; Peel off than big area at former PBN crucible part internal surface newly discovered 2 places, and area is about 30mm * 30mm and 40mm * 50mm, carries out the 5th surface and repair.
1, use acetone, methyl alcohol and deionized water ultrasonic cleaning clean successively on the surface of this PBN crucible, remove the chip and the greasy dirt on surface, dry then;
2, with high-purity oxidation boron powder levigate to 200 orders with carefully, adding massfraction is the ethanolic soln of 20% resol, is configured to boron oxide-resol slurry, wherein the quality of boron oxide and resol than scope at 4:1;
3, with the boron oxide-resol slip of preparation with crystal pulling method be coated on clean up with back PBN crucible surface, and dry, repeat 3 times with crystal pulling method after, the about 0.15mm of coat-thickness, and fill up the exfoliation layer pit of damage fully;
What 4, will apply boron oxide-resol slip places high-temperature atmosphere furnace with back PBN crucible, feeds nitrogen, with 2 ℃/min, is warming up to 400 ℃, and insulation 4h continues to be warming up to 1200 ℃ of insulations 3 hours with 8 ℃/min, and original position generates the BN coating.Naturally cool to room temperature then, with the PBN crucible for preparing behind the internal surface sanding and polishing after the reparation.The newly-generated about 0.05mm of repair layer thickness.
Continue to use the PBN crucible after repairing to carry out VGF (VGF) GaAs single crystal growing; After using 3 times, discovery repair layer major part is peeled off thicker the peeling off in former PBN crucible part internal surface exfoliation newly discovered 1 place; Area is about 10mm * 10mm; Thickness is about 0.7mm, and is for guaranteeing the safety of GaAs single crystal growth process, that this PBN crucible is discarded.
After adopting this usefulness back PBN crucible surface restorative procedure, this PBN crucible has used 5 subsurface reparations altogether, and accumulative total is used this PBN crucible 4+4+3+3+2+3=19 time, has increased than the access times that originally do not adopt the surperficial PBN crucible of repairing.
Embodiment 2:
The PBN crucible of 6 inches of diameters, wall thickness 1.5mm is used for VGF (VGF) growth GaAs monocrystalline.
After using 4 times continuously, the PBN crucible finds that inner surface of crucible exists the layering of 1 place to peel off, the about 15mm * 20mm of area, the about 0.1mm of thickness.It is carried out the 1st subsurface reparation.
1, use acetone, methyl alcohol and deionized water ultrasonic cleaning clean successively on the surface of this PBN crucible, remove the chip and the greasy dirt on surface, dry then;
2, with high-purity oxidation boron powder levigate to 200 orders with carefully, adding massfraction is the ethanolic soln of 10% resol, is configured to boron oxide-resol slurry, wherein the quality of boron oxide and resol than scope at 5:1;
3, the boron oxide-resol slip with preparation is coated on the internal surface with back PBN crucible that cleans up with spin-coating method, and dry, after spin-coating method repetition 1 time, and the about 0.1mm of coat-thickness, and fill up the exfoliation layer pit of 1 place damage fully;
What 4, will apply boron oxide-resol slip places high-temperature atmosphere furnace with back PBN crucible, feeds nitrogen, with 3 ℃/min, is warming up to 350 ℃, and insulation 5h continues to be warming up to 1250 ℃ of insulations 2 hours with 10 ℃/min, and original position generates the BN coating.Naturally cool to room temperature then, with the PBN crucible for preparing behind the internal surface sanding and polishing after the reparation.The newly-generated about 0.05mm of repair layer thickness.
Continue to use the PBN crucible after repairing to carry out VGF (VGF) GaAs single crystal growing; After using 4 times, find that repair layer partly peels off, peel off at former PBN crucible part internal surface newly discovered 1 place; Area is about 20mm * 30mm, carries out the 2nd subsurface reparation.
1, use acetone, methyl alcohol and deionized water ultrasonic cleaning clean successively on the surface of this PBN crucible, remove the chip and the greasy dirt on surface, dry then;
2, with high-purity oxidation boron powder levigate to 200 orders with carefully, adding massfraction is the ethanolic soln of 10% resol, is configured to boron oxide-resol slurry, wherein the quality of boron oxide and resol than scope at 2:1;
3, the boron oxide-resol slip with preparation is coated on the internal surface with back PBN crucible that cleans up with spin-coating method, and dry, after spin-coating method repetition 1 time, and the about 0.1mm of coat-thickness, and fill up the exfoliation layer pit of damage fully;
What 4, will apply boron oxide-resol slip places high-temperature atmosphere furnace with back PBN crucible, feeds nitrogen, with 3 ℃/min, is warming up to 350 ℃, and insulation 5h continues to be warming up to 1250 ℃ of insulations 2 hours with 10 ℃/min, and original position generates the BN coating.Naturally cool to room temperature then, with the PBN crucible for preparing behind the internal surface sanding and polishing after the reparation.The newly-generated about 0.05mm of repair layer thickness.
Continue to use the PBN crucible after repairing to carry out VGF (VGF) GaAs single crystal growing; After using 3 times, find that repair layer partly peels off, peel off at former PBN crucible part internal surface newly discovered 1 place; Area is about 30mm * 30mm, carries out the 3rd subsurface reparation.
1, use acetone, methyl alcohol and deionized water ultrasonic cleaning clean successively on the surface of this PBN crucible, remove the chip and the greasy dirt on surface, dry then;
2, with high-purity oxidation boron powder levigate to 200 orders with carefully, adding massfraction is the ethanolic soln of 10% resol, is configured to boron oxide-resol slurry, wherein the quality of boron oxide and resol than scope at 3:1;
3, the boron oxide-resol slip with preparation is coated on the internal surface with back PBN crucible that cleans up with spin-coating method, and dry, after spin-coating method repetition 1 time, and the about 0.1mm of coat-thickness, and fill up the exfoliation layer pit of damage fully;
What 4, will apply boron oxide-resol slip places high-temperature atmosphere furnace with back PBN crucible, feeds nitrogen, with 3 ℃/min, is warming up to 350 ℃, and insulation 5h continues to be warming up to 1250 ℃ of insulations 2 hours with 10 ℃/min, and original position generates the BN coating.Naturally cool to room temperature then, with the PBN crucible for preparing behind the internal surface sanding and polishing after the reparation.The newly-generated about 0.05mm of repair layer thickness.
PBN crucible after continue to use repairing carries out VGF (VGF) GaAs single crystal growing, uses 2 times after, find that repair layer partly peels off, former PBN crucible is found 1 place's through check, length is about 20mm, crucible lost efficacy, and this PBN crucible is discarded.
After adopting this usefulness back PBN crucible surface restorative procedure, this PBN crucible has used 3 subsurface reparations altogether, and accumulative total is used this PBN crucible 4+4+3+2=13 time, has increased than the access times that originally do not adopt the surperficial PBN crucible of repairing.
Above embodiment is merely exemplary embodiment of the present invention, is not used in restriction the present invention, and protection scope of the present invention is defined by the claims.Those skilled in the art can make various modifications or be equal to replacement the present invention in essence of the present invention and protection domain, this modification or be equal to replacement and also should be regarded as dropping in protection scope of the present invention.
Claims (8)
1. the surface repairing method with back pyrolysis boron nitride crucible is characterized in that, comprises the steps: earlier boron oxide powder and resol to be mixed with slip; Again the slip for preparing evenly is coated on the surperficial and drying with back pyrolysis boron nitride crucible of the needs reparation that cleans up; Then above-mentioned dried pyrolitic boron nitride crucible is placed the high-temperature atmosphere furnace heating, reaction under certain atmospheric condition, original position generates boron nitride coating; At last with the pyrolitic boron nitride crucible after promptly obtaining repairing after the surface finish polishing.
2. the surface repairing method with back pyrolysis boron nitride crucible according to claim 1 is characterized in that wherein, boron oxide powder purity is higher than 99.9%, and granularity is less than 0.074 millimeter.
3. the surface repairing method with back pyrolysis boron nitride crucible according to claim 1 is characterized in that, the quality of boron oxide powder and resol than scope at 1～5:1.
4. the surface repairing method with back pyrolysis boron nitride crucible according to claim 1; It is characterized in that; The slip employing spread coating, spraying method, spin-coating method or the crystal pulling method that prepare evenly are coated on clean up surperficial with back pyrolysis boron nitride crucible, and coating thickness need make coating cover injured surface fully.
5. the surface repairing method with back pyrolysis boron nitride crucible according to claim 1; It is characterized in that; The condition that places high-temperature atmosphere furnace to heat pyrolysis boron nitride crucible after the use that is coated with slip does, is warming up to 300-500 ℃ with 1-10 ℃/minute, is incubated 3-24 hour; Continuation is warming up to 1100-1600 ℃ of insulation 1-24 hour with 1-10 ℃/minute, and original position generates the BN coating.
6. the surface repairing method with back pyrolysis boron nitride crucible according to claim 1; It is characterized in that; Be coated with slip place high-temperature atmosphere furnace to heat with back pyrolysis boron nitride crucible the time, need to feed gas, said gas is nitrogen, ammonia or both gas mixtures.
7. the surface repairing method with back pyrolysis boron nitride crucible according to claim 1 is characterized in that, the back pyrolysis boron nitride crucible surface of using that needs to repair adopts water, absolute ethyl alcohol, methyl alcohol or acetone as cleaning medium, or adopts ultrasonic cleaning.
8. the surface repairing method with back pyrolysis boron nitride crucible according to claim 1 is characterized in that, high-purity boron oxide powder is mixed with the ethanolic soln of resol, is configured to boron oxide-resol slurry.
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| CN104120406B (en) * | 2014-07-02 | 2016-06-15 | 厦门润晶光电集团有限公司 | The tungsten crucible trimming device of long crystal furnace use and method |
| CN105779976A (en) * | 2016-05-10 | 2016-07-20 | 中国环境科学研究院 | Boron oxide film-plating method for combustion reactor under condition of laboratory |
| CN105779976B (en) * | 2016-05-10 | 2018-03-16 | 中国环境科学研究院 | The boron oxide film plating process of combustion reactor under laboratory condition |
| CN108911749A (en) * | 2018-08-31 | 2018-11-30 | 青岛中冶坩埚有限公司 | A kind of preparation method of graphite-silicon carbide crucible |
| CN110219051A (en) * | 2019-06-12 | 2019-09-10 | 有研光电新材料有限责任公司 | The separation method and separator of arsenide gallium monocrystal are separated from pyrolytic boron nitride crucible |
| CN110730607A (en) * | 2019-10-16 | 2020-01-24 | 深圳市飞鸿达科技有限公司 | Heat-conducting wave-absorbing insulating sheet with high heat-conducting performance and preparation method thereof |
| CN110730607B (en) * | 2019-10-16 | 2021-08-03 | 湖南飞鸿达新材料有限公司 | Heat-conducting wave-absorbing insulating sheet with high heat-conducting performance and preparation method thereof |
| CN112247678A (en) * | 2020-09-01 | 2021-01-22 | 威科赛乐微电子股份有限公司 | PBN crucible seed crystal cavity repairing method |
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| CN102776509B (en) | 2014-04-16 |
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