CN103602942B - The method of high-temperaure coating coating crucible surface protection precious metal crucible - Google Patents
The method of high-temperaure coating coating crucible surface protection precious metal crucible Download PDFInfo
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- CN103602942B CN103602942B CN201310578308.XA CN201310578308A CN103602942B CN 103602942 B CN103602942 B CN 103602942B CN 201310578308 A CN201310578308 A CN 201310578308A CN 103602942 B CN103602942 B CN 103602942B
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Abstract
The present invention relates to the method for a kind of high-temperaure coating coating crucible surface protection precious metal crucible, described method comprises: the surface preparation of precious metal crucible: in closed cabinet, adopt alumina particle to spray at a high speed hit precious metal crucible outside surface, make precious metal crucible outside surface form superfine hole to increase the external surface area of crucible; And high-temperature plasma spraying: thin oxidation zircon sand, through high-temperature plasma spray coating precious metal crucible outside surface after the pre-treatment, forms compact zirconia protective layer.The present invention forms superfine hole to increase the external surface area of crucible by carrying out spray at a high speed to hit fine particle to the outside surface of precious metal crucible; thus the adsorptive power added between protective layer and crucible outside surface; and form compact zirconia protective layer by plasma spraying; thus reduce the volatilization of precious metal crucible; reduce service wear, save crystal growth cost.
Description
Technical field
The present invention relates to the guard method of precious metal crucible, belong to field of crystal growth, more specifically belong to precious metal crucible and use guard method field.
Background technology
Crystalline material is the basis of the new high-tech industries such as information, electronics, communication, laser, as semiconductor crystal in microelectronics, piezoquartz in mechanics of communication, laser crystals in photoelectron technology, scintillation crystal in medical imaging technology and high energy physics.Along with the continuous exploration of field of crystals, the artificial lens of more and more excellent property is developed successfully.In the artificial lens of these excellent propertys, the fusing point of most crystal is all higher, scintillation crystal as: mix cerium silicic acid lutetium Lu
2siO
5: Ce(LSO:Ce) fusing point about 2200 DEG C, yttrium luetcium silicate (Lu
(1-x)y
(x))
2siO
5: the fusing point about 2150 DEG C of Ce (LYSO:Ce), mix cerium Luetcium aluminum garnet Lu
3al
5o
12: Ce(LuAG:Ce) fusing point about 2050 DEG C, bismuth germanium oxide Bi
4ge
3o
12(BGO) fusing point about 1050 DEG C; Laser crystals is as neodymium-doped yttrium-aluminum garnet Y
3al
5o
12: Nd(YAG:Nd) fusing point about 1970 DEG C, yttrium aluminate YAlO
3(YAP) fusing point about 1850 DEG C, yttrium vanadate crystal YVO
4fusing point about 2150 DEG C, gadolinium gallium garnet Gd
3ga
5o
12(GGG) fusing point about 1720 DEG C, terbium gallium garnet Tb
3ga
5o
12(TGG) fusing point about 1725 DEG C, these high temperature crystal growths require very high to the use temperature of crucible.
The process of growth of artificial lens needs first the raw material prepared to be contained in vessels crucible to be heated to more than crystalline melting point by various method, raw materials melt is made to be solution status, then slow cooling adopt seed crystal or spontaneous nucleation etc. to make the generation tuberculosis crystallization of zone melt be solid crystals.The fusing point of this process entails vessels crucible is greater than the fusing point of crystal, the material of crucible can not react with high-temperature fusant, and this outer crucible also needs to have high thermal conductivity with the temperature field structure of thermal conduction and melt not affecting high-temperature fusant or the natural convection of melt.This is main with regard to limiting crucible for crystal growth mainly with the material that thermal conductivity is high.
The crucible for crystal growth material adopted in the world at present mainly contains: platinum, iridium, rhodium, tungsten, molybdenum, graphite, quartz etc.The wherein fusing point of graphite about 3500 DEG C, but under high temperature carbon can with many metal reactions, generate metallic carbide etc., and graphite will react with the oxygen in air 350 DEG C-400 DEG C time, this will ask the oxygen level in growth furnace will keep extremely low, and these all limit the use of plumbago crucible.Quartz fusing point about 1750 DEG C, but will softening transform more than about 1200 DEG C, and the thermal conductivity of quartz low (about 0.88w/mk), be mainly used in some fusing points lower than the crystal growth of 1600 DEG C.The fusing point of tungsten about 3400 DEG C, but its easy volatilization in oxidizing atmosphere pollutes crystal, therefore tungsten crucible general requirement uses under high vacuum or reducing atmosphere, working temperature is at about 2450 DEG C.The fusing point of platinum about 1770 DEG C, physical and chemical stability is good, does not at high temperature also react with oxygen, long-time stable can use, be widely used in the growth of fusing point lower than 1150 DEG C of crystal below 1150 DEG C.The fusing point of iridium about 2440 DEG C, specifically comparatively stablizes physical and chemical performance, and working temperature can reach about 2200 DEG C, can use under weak oxide atmosphere, reducing atmosphere, vacuum.
In real crystal process of growth, very multicrystal fusing point close to the fusing point of crucible, as LSO, the fusing point of LYSO crystal is all close to the limit of working temperature of iridium crucible, easily make metal distil, the volatilization phenomenon of crucible is comparatively serious, and precious metal loss is that one of crystal growth cost is paid greatly.In order to reduce the usage quantity of crucible material and crucible heat conductivility to the impact of crystal growth temperature field, the thickness of crucible for crystal growth is all thinner, particularly precious metal crucible is as platinum crucible, Iridium Crucible, and crucible thickness is generally in 1 ~ 5mm scope, and what have even only has about 0.3mm.Crucible in use, the precious metal on surface has the volatilization of different depth, volatilization causes the direct loss of precious metal on the one hand, increase growth cost, on the other hand, the volatilization of precious metal makes natively very thin sidewall of crucible become thinner, the uneven different sites thickness of crucible that makes of volatilization differs, environment of crystal growth becomes and is difficult to control, and affects the stability of crystal growth, reduces the yield rate of crystal growth; The ununiformity of precious metal volatilization also reduces the access times of crucible, adds the number of times of precious metal crucible from new production, improves total use cost of precious metal crucible.Therefore, protect to prevent precious metal from volatilizing thus reduce service wear to become important research direction to precious metal crucible.Such as Chinese patent CN108033A discloses a kind of method protecting iridium crucible growth of tetravalent chromium doping high-temp oxide crystal, wherein sprays zirconium white protective layer with plasma spraying technology at iridium crucible outer wall; Chinese patent CN1122730C is openly mixed with the protective layer of iridium powder and zirconia powder further in the spraying of iridium crucible outside surface with plasma spraying technology, with the stability of this heavy seal coat.But these methods are all directly spray at iridium crucible outside surface, there is coating and the more weak problem of crucible outside surface adsorptive power.
Summary of the invention
In the face of prior art Problems existing, a kind of dense refractory coating is the object of the present invention is to provide firmly to be coated on crucible surface thus the method for protection precious metal crucible.The method of using plasma spraying of the present invention; be formed with the zirconium white protective layer of crucible outer surface one deck densification in superfine hole; with the contact of isolated crucible outside surface and atmosphere; reduce precious metal as the volatilization of iridium in crystal growing process; thus reduce the service wear of precious metal crucible, save crystal growth cost.
At this, the invention provides the method for a kind of high-temperaure coating coating crucible surface protection precious metal crucible, comprise: the surface preparation of precious metal crucible: in closed cabinet, adopt alumina particle to spray at a high speed hit precious metal crucible outside surface, make precious metal crucible outside surface form superfine hole to increase the external surface area of crucible; And high-temperature plasma spraying: thin oxidation zircon sand, through high-temperature plasma spray coating precious metal crucible outside surface after the pre-treatment, forms compact zirconia protective layer.
The present invention forms superfine hole to increase the external surface area of crucible by carrying out spray at a high speed to hit fine particle to the outside surface of precious metal crucible; thus the adsorptive power added between protective layer and crucible outside surface; and form compact zirconia protective layer by plasma spraying; thus reduce the volatilization of precious metal crucible; reduce service wear, save crystal growth cost.
Preferably, the particle diameter of described alumina particle is 800 μm.
Preferably, the speed that described spray is hit is the speed that spray is hit is 15 ~ 20m/s, and the spray time of hitting is directly proportional to crucible outside surface size, is generally 15 ~ 60 minutes.
Preferably, the particle diameter of described thin oxidation zircon sand is 18 ~ 45 μm.
Preferably, the working gas of described high-temperature plasma spraying is argon gas, and working temperature is 5000 ~ 6000 DEG C.
Preferably, the thickness of described zirconium white protective layer is 0.3 ~ 1.2mm.
In the present invention, described precious metal crucible comprises iridium crucible, platinum crucible and rhodium crucible.
Method of the present invention is simple, and remarkable to the protected effect of precious metal, in the use of precious metal, the loss of precious metal is only less than 1/3 of the loss of unprotected crucible.
The directly armor coated crucible without pre-treatment of the present invention, in use there will be local securing layer and peels off the shortcomings such as uneven and work-ing life is short that cause precious metal crucible to volatilize in advance.And the present invention can make protective layer be incorporated into crucible outside surface securely and can not peel off in advance, therefore, it is possible to protect precious metal crucible better.
Accompanying drawing explanation
Fig. 1 be unprotect layer and through the inventive method protection crucible outside surface and heat insulation material surface situation comparison diagram.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.
In order to reduce the usage quantity of crucible material and crucible heat conductivility to the impact of crystal growth temperature field, the thickness of crucible for crystal growth is all thinner, particularly precious metal crucible is as platinum crucible, Iridium Crucible, and crucible thickness is generally in 1 ~ 5mm scope, and what have even only has about 0.3mm.Crucible in use, the precious metal on surface has volatilization, because crucible is thinner, volatilization causes the direct loss of precious metal on the one hand, increases growth cost, on the other hand, the volatilization of precious metal makes natively very thin sidewall of crucible become thinner, and the uneven different sites thickness of crucible that makes of volatilization differs, and environment of crystal growth becomes uncontrollable, affect the stability of crystal growth, reduce the yield rate of crystal growth; The ununiformity of precious metal volatilization also reduces the access times of crucible, adds the number of times of precious metal crucible from new production, improves total use cost of precious metal crucible.
The method that the present invention sprays at precious metal surface using plasma; be formed with the zirconium white protective layer of crucible outer surface one deck densification in superfine hole; with the contact of isolated crucible outside surface and atmosphere; reduce precious metal as the volatilization of iridium in crystal growing process; thus reduce the service wear of precious metal crucible, save crystal growth cost.The embodiment of an example is as described below.
1. the surface preparation of precious metal crucible
As precious metal crucible to be protected, include but not limited to iridium crucible, platinum crucible and rhodium crucible.First precious metal crucible surface can be carried out clean, such as, be placed in ethanol ultrasonic cleaning; Then, in airtight glove box, alumina particle spray is adopted to hit Iridium Crucible outside surface.The particle diameter hitting the alumina particle of particle as spray can be 800 μm.The spray speed of hitting can be 15 ~ 20m/s, and the spray time of hitting can be 15 ~ 60 minutes.By carrying out this pre-treatment, superfine hole can be formed to increase the external surface area of crucible at precious metal crucible surface, thus increase the adsorptive power between coating and crucible outside surface.
2. high-temperature plasma spraying
Precious metal crucible outside surface after the pre-treatment carries thin zirconium white sand blasting through plasma body (such as high temperature argon plasma body) and is coated with, and forms compact zirconia protective layer.The particle diameter of thin oxidation zircon sand can be 18 ~ 45 μm.The processing parameter of spraying can be: working gas is argon gas, and working temperature is 5000 ~ 6000 DEG C.The thickness of the protective layer formed can be 0.3 ~ 1.2mm, if too thin, cannot play a protective role, if too thick, protective layer easily comes off.
3. the use contrast of protective layer
In order to verify the validity of protective layer of the present invention, can also by through above-mentioned pre-treatment and have the precious metal crucible of zirconium white protective layer through use after contrast with unprotected crucible and the crucible directly armor coated without pre-treatment.Namely to using the different crucible quality of front and back to contrast, the loss situation of somewhat expensive metallic crucible.In one example; adopt unprotected Iridium Crucible respectively, the Iridium Crucible directly armor coated without pre-treatment and through the Iridium Crucible of aforesaid method process as the growth crucible of LYSO:Ce crystal, carry out the contrast of crucible service condition after growth.See Fig. 1, it illustrates unprotect layer (figure left) and through the crucible outside surface (figure is right) of the inventive method protection and heat insulation material surface situation comparison diagram, be can be observed unshielded crucible surface roughen by figure and had with peripheral refractory insulating layer to cohere phenomenon, the precious metal adsorption on peripheral refractory insulating layer is many; Crucible protective layer through the inventive method protection is unchanged, and namely loss is few less for the precious metal adsorption on peripheral refractory insulating layer.Unprotect layer Iridium Crucible average loss about 30 grams is learnt through weighing; the Iridium Crucible average loss directly armor coated without pre-treatment about 16 grams; through the inventive method protection Iridium Crucible average loss lower than 10 grams; as can be seen here; the present invention can play the effect reducing the loss of precious metal crucible, and is better than the scheme directly armor coated without pre-treatment to the protected effect of precious metal crucible.
Exemplify embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter etc. that following example is concrete is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1
The fusing point of 1.LYSO:Ce crystal is about 2150 DEG C, many employing Iridium Crucible are the growth crucible of this crystal at present, the maximum operation temperature of iridium is 2200 DEG C, in the process of growth of LYSO:Ce crystal, the cost loss that the volatilization of iraurite causes is a sport of this crystal growth cost, in order to reduce the service wear of iraurite, first we carry out surface treatment to the Iridium Crucible of new production, namely Iridium Crucible surface is after clean, in airtight glove box, employing particle diameter is that the alumina particle of 800 μm hits Iridium Crucible outside surface 25 minutes with the spray of 15 ~ 20m/s speed, iridium crucible outside surface is made to form superfine hole to increase the external surface area of crucible, thus the adsorptive power increased between coating and crucible outside surface.
2. the Iridium Crucible that surface is treated; it is that 18 ~ 45 μm thin zirconium white sand blastings are coated with that outside surface carries particle diameter through high temperature argon plasma body; the processing parameter of spraying: working gas is argon gas, working temperature is 5000 ~ 6000 DEG C, forms the compact zirconia protective layer that thickness is 0.7mm.Iridium Crucible through protection is used for LYSO:Ce crystal growth.
Comparative example 1
Direct employing, without the Iridium Crucible of protection, carries out the LYSO:Ce crystal growth identical with embodiment 1.
Comparative example 2
Do not carry out the pre-treatment step of embodiment 1 and directly adopt the technique identical with embodiment 1 to carry out the plasma spraying of zirconium white protective layer; namely the outside surface of Iridium Crucible carries particle diameter for being coated with for 18 ~ 45 μm thin zirconium white sand blastings through high temperature argon plasma body; the processing parameter of spraying: working gas is argon gas, working temperature is 5000 ~ 6000 DEG C, forms the compact zirconia protective layer that thickness is 0.7mm.Iridium Crucible through protection is used for carrying out the LYSO:Ce crystal growth identical with embodiment 1.
The crucible service condition of embodiment 1 with comparative example 1 contrasted, see Fig. 1, can be observed unshielded crucible surface roughen and have with peripheral refractory insulating layer to cohere phenomenon, the precious metal adsorption on peripheral refractory insulating layer is many; Crucible protective layer through the inventive method protection is unchanged, and namely loss is few less for the precious metal adsorption on peripheral refractory insulating layer.In addition; weigh to measure its quality loss to the crucible before and after using; result shows the unprotect layer Iridium Crucible average loss about 30 grams of comparative example 1; the Iridium Crucible average loss directly armor coated without pre-treatment about 16 grams of comparative example 2, the Iridium Crucible average loss of embodiment 1 is lower than 10 grams.
Industrial applicability: the present invention can be used for the protection of precious metal crucible, reduces precious metal loss, saves crystal growth cost, is applicable to field of crystal growth.
Claims (3)
1. a method for high-temperaure coating coating crucible surface protection precious metal crucible, is characterized in that, comprising:
The surface preparation of precious metal crucible: adopt alumina particle to spray at a high speed in closed cabinet and hit precious metal crucible outside surface, precious metal crucible outside surface is made to form superfine hole to increase the external surface area of crucible, the particle diameter of described alumina particle is 800 μm, the speed that described spray is hit is 15 ~ 20m/s, and the spray time of hitting is 15 ~ 60 minutes; And
High-temperature plasma sprays: thin oxidation zircon sand is through high-temperature plasma spray coating precious metal crucible outside surface after the pre-treatment; form compact zirconia protective layer; the particle diameter of described thin oxidation zircon sand is 18 ~ 45 μm; the working gas of described high-temperature plasma spraying is argon gas, and working temperature is 5000 ~ 6000 DEG C.
2. method according to claim 1, is characterized in that, the thickness of described zirconium white protective layer is 0.3 ~ 1.2mm.
3. method according to claim 1 and 2, is characterized in that, described precious metal crucible comprises iridium crucible, platinum crucible and rhodium crucible.
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| CN107245698B (en) * | 2017-06-30 | 2019-03-12 | 福州大学 | A kind of internal heat type integration evaporating basket with aluminum oxide porous textured buffer layers |
| CN107653487A (en) * | 2017-10-23 | 2018-02-02 | 安徽中晶光技术股份有限公司 | A kind of recycling bin for being used in crystal growing process reclaim iridium powder |
| CN114455964B (en) * | 2021-12-30 | 2023-09-05 | 西安超码科技有限公司 | C/SiC composite material crucible containing alumina coating |
| CN115478320A (en) * | 2022-09-22 | 2022-12-16 | 安徽光智科技有限公司 | Crucible, manufacturing method and method for growing tellurium dioxide crystal by using crucible |
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| CN101955314A (en) * | 2009-07-15 | 2011-01-26 | 肖特公开股份有限公司 | The continuous smelting or the purified method and apparatus that are used for melt |
| CN102744404A (en) * | 2012-07-26 | 2012-10-24 | 江西稀有稀土金属钨业集团有限公司 | Surface bonding-proof method for hard alloy parison sintering boat |
| CN102797042A (en) * | 2012-09-06 | 2012-11-28 | 张礼强 | Crucible for melting crystalline silicon, method for producing crucible and spray coating liquid |
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2013
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|---|---|---|---|---|
| CN1080334A (en) * | 1992-06-17 | 1994-01-05 | 中国科学院上海光学精密机械研究所 | The method of protection iridium crucible growth of tetravalent chromium doping high-temp oxide crystal using |
| CN201534815U (en) * | 2009-06-23 | 2010-07-28 | 珠海彩珠实业有限公司 | Platinum crucible |
| CN101955314A (en) * | 2009-07-15 | 2011-01-26 | 肖特公开股份有限公司 | The continuous smelting or the purified method and apparatus that are used for melt |
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| CN102797042A (en) * | 2012-09-06 | 2012-11-28 | 张礼强 | Crucible for melting crystalline silicon, method for producing crucible and spray coating liquid |
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