CN102776509B - 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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- CN102776509B CN102776509B CN201210287522.5A CN201210287522A CN102776509B CN 102776509 B CN102776509 B CN 102776509B CN 201210287522 A CN201210287522 A CN 201210287522A CN 102776509 B CN102776509 B CN 102776509B
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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 the surface repairing method of the rear pyrolytic boron nitride crucible of a kind of use, belong to semiconductor single-crystal growth equipment technical field.
Background technology
Artificial crystal growth is as a kind of technique, people are long-standing for its research, the crystal that nature is produced almost can be grown by artificial means, and artificial-synthetic crystal's experimental technique develops rapidly in recent years, and its principle is mainly to prepare by the heterogeneous transformation of homogeneity.The growth method of crystal also has a variety of, and actual process of growth depends on the feature of physics and chemistry character, phasor and the method for material itself.For example Slow cooling method is that the material preparing is added to crucible, then makes its fusing, is incubated the regular hour so that material fully reacts homogenizing, then with the cooling crystal that obtains of certain rate of cooling; Top-seeded solution growth is that melt growth is lifted to a kind of growing technology that technology combines with flux growth method, seed crystal is fixed on to seed rod lower end, drop to slowly with the saturated solution liquid level in crucible and contact, and then by liquation Slow cooling, also can upwards promote slowly seed crystal simultaneously.But the gentle cold process of top-seeded solution growth is the same, all need to use high-quality crucible to load melt, this crucible need to meet the grow requirement of required high thermal resistance and the required mechanical property of carrying melt of crystal, also needs to meet the requirement of purity aspect.
Crucible material about growing single-crystal requires have good heat conductance and high thermal resistance, and in applied at elevated temperature process, thermal expansivity is little, and anxious heat, chilling are had to certain anti-strain property.To acid, the erosion resistance of basic solution is stronger, and general normal is platinum (Pt), iridium (Ir), molybdenum (Mo), graphite, boron nitride (BN) or other refractory oxide.The crucible of preparing with respect to metallic substance such as platinum, iridium, molybdenums, cost is high, technique relative complex, and under graphite high temperature, volatilization seriously adds in the process of graphite material preparation process and inevitably can introduce impurity, can contaminated feedstock as the crucible of growing single-crystal with graphite.Limited plumbago crucible in the application of preparing high quality single crystal Material Field.
Pyrolitic boron nitride (PBN) has high purity, and the resistance to elevated temperatures having had can keep good lubricity and thermostability under high temperature, is again hot good conductor and tool insulativity simultaneously, and many advantages become one of appropriate materials of spare-crucible.Pyrolitic boron nitride (PBN), by chemical vapour deposition principle, adopts the disclosed method of US Patent No. 3152006 to form, and this patent disclosure is incorporated herein by reference.The method comprises the ammonia of proper ratio and gaseous state halogenation boron boron trichloride (BC1 for example
3), boron trichloride (BF
3) etc. steam introduce in the reactor heated, produce scission reaction, make BN be deposited on suitable substrate as on the surface of graphite.BN is with the form deposition of layer, cooling after, it is separated from base material, form PBN crucible.
But pyrolytic boron nitride crucible is prepared by chemical Vapor deposition process, the production cycle is long, and temperature of reaction is high, and cost is higher.PBN crucible is after crystal growth use, insulating covering agent (environment for use for PBN crucible is mainly boron oxide) used during crystal growth can infiltrate its top layer, when the monocrystalline of separation growth, may cause the damage of PBN crucible, be mainly internal surface damage, this damage mainly comprises: insulating covering agent sticks, surface irregularity, internal surface layering peel off, through check and the fragmentation of crucible local perforations etc.Wherein through check and the fragmentation of crucible local perforations can directly cause PBN crucible to lose efficacy and can not continue to use; Internal surface layering is peeled off and is looked the thickness difference of exfoliation layer and different treatment, when exfoliation layer is thicker, PBN crucible is directly discarded does not re-use, to avoid crucible inefficacy in single crystal growth process to result in greater loss, when exfoliation layer is thinner, PBN crucible can continue to use, but reuse also can cause peeling off again, occurs, damage accumulation, exfoliation layer thickens, and repeatedly makes afterwards the blocked up or crucible local perforations of exfoliation layer, causes crucible to lose efficacy; Insulating covering agent sticks with the minor injury such as surface irregularity does not generally affect PBN crucible, but damage accumulation after repeatedly using can cause the generation that the layering of PBN inner surface of crucible is peeled off.
Generally speaking, PBN crucible is the damage accumulation of internal surface in use, is to cause PBN crucible to lose efficacy the major cause that cannot reuse.Cause be thus generally the work-ing life of the PBN crucible that growth compound semiconductor monocrystal uses 6-10 time, therefore if to repairing the work-ing life that can extend PBN crucible with rear PBN inner surface of crucible, reduce costs.
Problem and defect in view of above-mentioned prior art existence, the inventor relies on practical experience for many years and abundant expertise are actively studied and innovate, the final surface repairing method that proposes a kind of rear pyrolytic boron nitride crucible of use of lower cost, can make PBN crucible after repair on surface again for the growth of compound semiconductor single crystal.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the invention provides the surface repairing method of the rear pyrolytic boron nitride crucible of a kind of use, can make pyrolytic boron nitride crucible after repair on surface again for the growth of compound semiconductor single crystal, reduced cost.
In order to solve the problems of the technologies described above, the present invention has adopted following technical scheme:
A surface repairing method for the rear pyrolytic boron nitride crucible of use, comprises the steps: first boron oxide powder and resol to be mixed with to slip; Again the slip preparing be evenly coated on to the use rear pyrolytic boron nitride crucible surface of the needs reparation cleaning up and be dried; Then above-mentioned dried pyrolytic boron nitride crucible is placed in to high-temperature atmosphere furnace heating, under certain atmospheric condition, reacts, original position generates boron nitride coating; Finally by the pyrolytic boron nitride crucible after being repaired after surface finish polishing.
Further, the surface repairing method of the rear pyrolytic boron nitride crucible of use as above, wherein, boron oxide powder purity is higher than 99.9%, and granularity is less than 0.074 millimeter.
Further, the surface repairing method of the rear pyrolytic boron nitride crucible of use as above, wherein, the quality of boron oxide powder and resol than scope at 1～5:1.
Further, the surface repairing method of the rear pyrolytic boron nitride crucible of use as above, wherein, adopt spread coating, spraying method, spin-coating method or crystal pulling method to be evenly coated on the rear pyrolytic boron nitride crucible of the use cleaning up surface the slip preparing, coating thickness need to make coating cover injured surface completely.
Further, the surface repairing method of the rear pyrolytic boron nitride crucible of use as above, wherein, the rear pyrolytic boron nitride crucible of the use that is coated with slip is placed in to the condition that high-temperature atmosphere furnace heats is, with 1-10 ℃/min, be warming up to 300-500 ℃, insulation 3-24 hour, continues to be warming up to 1100-1600 ℃ of insulation 1-24 hour with 1-10 ℃/min, and original position generates BN coating.
Further, the surface repairing method of the rear pyrolytic boron nitride crucible of use as above, when wherein the rear pyrolytic boron nitride crucible of the use that is coated with slip being placed in to high-temperature atmosphere furnace and heating, need to pass into gas, and described gas is nitrogen, ammonia or both gas mixtures.
Further, the surface repairing method of the rear pyrolytic boron nitride crucible of use as above, wherein, needs the rear pyrolytic boron nitride crucible of the use surface of repairing to adopt water, dehydrated alcohol, methyl alcohol or acetone as cleaning medium, or adopts ultrasonic cleaning.
Further, the surface repairing method of the rear pyrolytic boron nitride crucible of use as above, 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 with rear PBN crucible, extend the work-ing life of PBN crucible;
2, the raw materials cost that this method adopts 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, after PBN crucible growing semiconductor compound monocrystal 3-5 time, by present method, carrying out surface repairs, thereafter every use is carried out one-time surface reparation 2-4 time, can make extend to the work-ing life of PBN crucible 15 to 20 times, the interval number of times that specifically carries out repairing on surface is depending on PBN inner surface of crucible degree of impairment.Because repair layer is combined with PBN crucible surface and is weaker than PBN crucible itself, when the PBN crucible generation layering after therefore repairing is peeled off, peel off and preferentially betide in repair layer and the interface of repair layer and PBN crucible, also have small part situation can occur in PBN crucible.The inventive method is for significant by the recycling of rear PBN crucible.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but not as a limitation of the invention.
Embodiment 1:
The pyrolytic boron nitride crucible of 4 inches of diameters, wall thickness 1.5mm, for VGF (VGF) growth GaAs monocrystalline.
PBN crucible finds that inner surface of crucible exists the layering of 2 places to peel off after using 4 times continuously, 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 to the 1st subsurface reparation.
1, the surface of this PBN crucible is used successively acetone, methyl alcohol and deionized water ultrasonic cleaning clean, removed surperficial chip and greasy dirt, then dry;
2, by 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, boron oxide-resol slip of preparation is coated on to the rear PBN crucible surface of the use cleaning up with crystal pulling method, and dry, with crystal pulling method, repeat after 2 times, the about 0.1mm of coat-thickness, and fill up the exfoliation layer pit of 2 places damage completely;
4, the rear PBN crucible of use that applies boron oxide-resol slip is placed in to high-temperature atmosphere furnace, passes into nitrogen, with 2 ℃/min, be warming up to 400 ℃, be incubated 4 hours, continue to be warming up to 1200 ℃ of insulations 3 hours with 8 ℃/min, original position generates BN coating.Then naturally cool to room temperature, by the PBN crucible preparing after internal surface sanding and polishing after 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 after 4 times, and discovery repair layer major part is peeled off, but former PBN crucible part internal surface peels off without newfound, carries out the 2nd subsurface reparation.
1, the surface of this PBN crucible is used successively acetone, methyl alcohol and deionized water ultrasonic cleaning clean, removed surperficial chip and greasy dirt, then dry;
2, by 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, boron oxide-resol slip of preparation is coated on to the rear PBN crucible surface of the use cleaning up with crystal pulling method, and dry, with crystal pulling method, repeat after 3 times, the about 0.15mm of coat-thickness, and fill up the exfoliation layer pit of damage completely;
4, the rear PBN crucible of use that applies boron oxide-resol slip is placed in to high-temperature atmosphere furnace, passes into nitrogen, with 2 ℃/min, be warming up to 400 ℃, insulation 4h, continues to be warming up to 1200 ℃ of insulations 3 hours with 8 ℃/min, and original position generates BN coating.Then naturally cool to room temperature, by the PBN crucible preparing after internal surface sanding and polishing after 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, use after 3 times, discovery repair layer major part is peeled off, and peel off at former PBN crucible part internal surface new discovery 1 place, area is about 20mm * 40mm, carries out the 3rd subsurface reparation.
1, the surface of this PBN crucible is used successively acetone, methyl alcohol and deionized water ultrasonic cleaning clean, removed surperficial chip and greasy dirt, then dry;
2, by 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, boron oxide-resol slip of preparation is coated on to the rear PBN crucible surface of the use cleaning up with crystal pulling method, and dry, with crystal pulling method, repeat after 3 times, the about 0.15mm of coat-thickness, and fill up the exfoliation layer pit of damage completely;
4, the rear PBN crucible of use that applies boron oxide-resol slip is placed in to high-temperature atmosphere furnace, passes into nitrogen, with 2 ℃/min, be warming up to 400 ℃, insulation 4h, continues to be warming up to 1200 ℃ of insulations 3 hours with 8 ℃/min, and original position generates BN coating.Then naturally cool to room temperature, by the PBN crucible preparing after internal surface sanding and polishing after 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 after 3 times, finds that repair layer major part peels off, but former PBN crucible part internal surface peels off without newfound, carries out the reparation of the 4th surface.
1, the surface of this PBN crucible is used successively acetone, methyl alcohol and deionized water ultrasonic cleaning clean, removed surperficial chip and greasy dirt, then dry;
2, by 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, boron oxide-resol slip of preparation is coated on to the rear PBN crucible surface of the use cleaning up with crystal pulling method, and dry, with crystal pulling method, repeat after 3 times, the about 0.15mm of coat-thickness, and fill up the exfoliation layer pit of damage completely;
4, the rear PBN crucible of use that applies boron oxide-resol slip is placed in to high-temperature atmosphere furnace, passes into nitrogen, with 2 ℃/min, be warming up to 400 ℃, insulation 4h, continues to be warming up to 1200 ℃ of insulations 3 hours with 8 ℃/min, and original position generates BN coating.Then naturally cool to room temperature, by the PBN crucible preparing after internal surface sanding and polishing after 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, use after 2 times, discovery repair layer major part is peeled off, former PBN crucible part internal surface new discovery 2 place's larger areas are peeled off, area is about 30mm * 30mm and 40mm * 50mm, carries out the 5th surface and repairs.
1, the surface of this PBN crucible is used successively acetone, methyl alcohol and deionized water ultrasonic cleaning clean, removed surperficial chip and greasy dirt, then dry;
2, by 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, boron oxide-resol slip of preparation is coated on to the rear PBN crucible surface of the use cleaning up with crystal pulling method, and dry, with crystal pulling method, repeat after 3 times, the about 0.15mm of coat-thickness, and fill up the exfoliation layer pit of damage completely;
4, the rear PBN crucible of use that applies boron oxide-resol slip is placed in to high-temperature atmosphere furnace, passes into nitrogen, with 2 ℃/min, be warming up to 400 ℃, insulation 4h, continues to be warming up to 1200 ℃ of insulations 3 hours with 8 ℃/min, and original position generates BN coating.Then naturally cool to room temperature, by the PBN crucible preparing after internal surface sanding and polishing after 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, use after 3 times, discovery repair layer major part is peeled off, thicker the peeling off in former PBN crucible part internal surface exfoliation new discovery 1 place, area is about 10mm * 10mm, thickness is about 0.7mm, for guaranteeing the safety of GaAs single crystal growth process, this PBN crucible is discarded.
Adopt after the rear PBN crucible surface of this use 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, than the access times of the PBN crucible that does not adopt surface to repair originally, has increased.
Embodiment 2:
The PBN crucible of 6 inches of diameters, wall thickness 1.5mm, for VGF (VGF) growth GaAs monocrystalline.
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 after using 4 times continuously.It is carried out to the 1st subsurface reparation.
1, the surface of this PBN crucible is used successively acetone, methyl alcohol and deionized water ultrasonic cleaning clean, removed surperficial chip and greasy dirt, then dry;
2, by 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, boron oxide-resol slip of preparation is coated on to the internal surface of the rear PBN crucible of the use cleaning up with spin-coating method, and dry, with spin-coating method, repeat after 1 time, the about 0.1mm of coat-thickness, and fill up the exfoliation layer pit of 1 place damage completely;
4, the rear PBN crucible of use that applies boron oxide-resol slip is placed in to high-temperature atmosphere furnace, passes into nitrogen, with 3 ℃/min, be warming up to 350 ℃, insulation 5h, continues to be warming up to 1250 ℃ of insulations 2 hours with 10 ℃/min, and original position generates BN coating.Then naturally cool to room temperature, by the PBN crucible preparing after internal surface sanding and polishing after 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, use after 4 times, find that repair layer partly peels off, peel off at former PBN crucible part internal surface new discovery 1 place, area is about 20mm * 30mm, carries out the 2nd subsurface reparation.
1, the surface of this PBN crucible is used successively acetone, methyl alcohol and deionized water ultrasonic cleaning clean, removed surperficial chip and greasy dirt, then dry;
2, by 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, boron oxide-resol slip of preparation is coated on to the internal surface of the rear PBN crucible of the use cleaning up with spin-coating method, and dry, with spin-coating method, repeat after 1 time, the about 0.1mm of coat-thickness, and fill up the exfoliation layer pit of damage completely;
4, the rear PBN crucible of use that applies boron oxide-resol slip is placed in to high-temperature atmosphere furnace, passes into nitrogen, with 3 ℃/min, be warming up to 350 ℃, insulation 5h, continues to be warming up to 1250 ℃ of insulations 2 hours with 10 ℃/min, and original position generates BN coating.Then naturally cool to room temperature, by the PBN crucible preparing after internal surface sanding and polishing after 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, use after 3 times, find that repair layer partly peels off, peel off at former PBN crucible part internal surface new discovery 1 place, area is about 30mm * 30mm, carries out the 3rd subsurface reparation.
1, the surface of this PBN crucible is used successively acetone, methyl alcohol and deionized water ultrasonic cleaning clean, removed surperficial chip and greasy dirt, then dry;
2, by 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, boron oxide-resol slip of preparation is coated on to the internal surface of the rear PBN crucible of the use cleaning up with spin-coating method, and dry, with spin-coating method, repeat after 1 time, the about 0.1mm of coat-thickness, and fill up the exfoliation layer pit of damage completely;
4, the rear PBN crucible of use that applies boron oxide-resol slip is placed in to high-temperature atmosphere furnace, passes into nitrogen, with 3 ℃/min, be warming up to 350 ℃, insulation 5h, continues to be warming up to 1250 ℃ of insulations 2 hours with 10 ℃/min, and original position generates BN coating.Then naturally cool to room temperature, by the PBN crucible preparing after internal surface sanding and polishing after 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, use after 2 times, find that repair layer partly peels off, former PBN crucible is found 1 place's through check, and length is about 20mm, and crucible lost efficacy, and this PBN crucible is discarded.
Adopt after the rear PBN crucible surface of this use 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, than the access times of the PBN crucible that does not adopt surface to repair originally, has increased.
Above embodiment is only 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 considered as dropping in protection scope of the present invention.
Claims (5)
1. with a surface repairing method for rear pyrolytic boron nitride crucible, it is characterized in that, comprise the steps: first boron oxide powder and resol to be mixed with to slip; Again the slip preparing be evenly coated on to the use rear pyrolytic boron nitride crucible surface of the needs reparation cleaning up and be dried; Then above-mentioned dried pyrolytic boron nitride crucible is placed in to high-temperature atmosphere furnace heating, under certain atmospheric condition, reacts, original position generates boron nitride coating; Finally by the pyrolytic boron nitride crucible after being repaired after surface finish polishing, wherein
Boron oxide powder purity is higher than 99.9%, and granularity is less than 0.074 millimeter, the quality of boron oxide powder and resol than scope at 1～5:1;
The rear pyrolytic boron nitride crucible of the use that is coated with slip is placed in to the condition that high-temperature atmosphere furnace heats is, with 1-10 ℃/min, be warming up to 300-500 ℃, insulation 3-24 hour, continues to be warming up to 1100-1600 ℃ of insulation 1-24 hour with 1-10 ℃/min, and original position generates BN coating.
2. the surface repairing method of the rear pyrolytic boron nitride crucible of use according to claim 1, it is characterized in that, adopt spread coating, spraying method, spin-coating method or crystal pulling method to be evenly coated on the rear pyrolytic boron nitride crucible of the use cleaning up surface the slip preparing, coating thickness need to make coating cover injured surface completely.
3. the surface repairing method of the rear pyrolytic boron nitride crucible of use according to claim 1, it is characterized in that, when the rear pyrolytic boron nitride crucible of the use that is coated with slip is placed in to high-temperature atmosphere furnace and heats, need to pass into gas, described gas is nitrogen, ammonia or both gas mixtures.
4. the surface repairing method of the rear pyrolytic boron nitride crucible of use according to claim 1, is characterized in that, needs the rear pyrolytic boron nitride crucible of the use surface of repairing to adopt water, dehydrated alcohol, methyl alcohol or acetone as cleaning medium, or adopts ultrasonic cleaning.
5. the surface repairing method of the rear pyrolytic boron nitride crucible of use 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 |
| 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 |
| 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 |
| CN112247678B (en) * | 2020-09-01 | 2022-04-22 | 威科赛乐微电子股份有限公司 | PBN crucible seed crystal cavity repairing method |
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| CN101318636A (en) * | 2008-05-12 | 2008-12-10 | 中国科学院上海硅酸盐研究所 | Method for preparing hexagonal boron nitride containing composite material with nitridation in situ |
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| CN101092735A (en) * | 2006-06-20 | 2007-12-26 | 通用电气公司 | Multi-piece ceramic crucible and method for making thereof |
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Effective date of registration: 20190529 Address after: 101101 No. 108 Binhe Road, Tongzhou District, Beijing Co-patentee after: Bo Yu (Chaoyang) semiconductor technology Co., Ltd. Patentee after: Beijing Boyu Semiconductor Process Containers Technology Co., Ltd. Co-patentee after: Bo Yu (Tianjin) semiconductor materials Co., Ltd. Address before: 101101 No. 108 Binhe Road, Tongzhou District, Beijing Patentee before: Beijing Boyu Semiconductor Process Containers Technology Co., Ltd. |
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