CN101294269A - Process for producing vitrification SiO2-Al2O3 mix oxide deposition material - Google Patents
Process for producing vitrification SiO2-Al2O3 mix oxide deposition material Download PDFInfo
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- CN101294269A CN101294269A CNA2008101224447A CN200810122444A CN101294269A CN 101294269 A CN101294269 A CN 101294269A CN A2008101224447 A CNA2008101224447 A CN A2008101224447A CN 200810122444 A CN200810122444 A CN 200810122444A CN 101294269 A CN101294269 A CN 101294269A
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Abstract
The invention relates to a preparation method of crystalloid SiO2-Al2O3 mixed oxide vapor deposition material. SiO2-Al2O3 mixed oxide powders which comprise SiO2 (that is 50 percent to 90 percent by weight percentage) and Al2O3 (that is 10 percent to 50 percent by weight percentage) are deployed; the mixed powders are put in a plumbago pot of a vacuum medium frequency induction furnace; under the vacuum degree that is less than or equals to 1*10<-2>Pa, a medium frequency source is utilized to induce that the plumbago pot is heated until the temperature reaches 1650 to 1750 DEG C to form a SiO2-Al2O3 mixed oxide molten mass; the molten mass is cooled through slow settlement to form pre-fusion crystalloid SiO2-Al2O3 mixed oxide vapor deposition material. Water vapor and residual gas which are generated during the preparation process are gathered by adopting a cold trap drip catcher, and the cryogenic temperature is less than or equals to minus 120 DEG C. The preparation method utilizes a microvacuum medium frequency induction furnace to induce the heating of the plumbago pot, and adopts the slow settlement crystal increasing method to prepare pre-fusion crystalloid SiO2-Al2O3 mixed oxide which is used as starting materials with high purity and high relative density for vapor-plating an advanced optical thin film. The preparation method can shorten the production period and save the manufacturing cost.
Description
Technical field
The present invention relates to a kind of preparation method of structural evaporation coating film material, particularly a kind of crystal qualitative SiO
2-Al
2O
3The preparation method of mixed oxide deposition material.
Background technology
Optical coating Application Areas fast-developing day by day and thereupon optical thin film is proposed more high performance demand, except strictness control coating process, evaporation parent material and technology of preparing thereof become a very crucial problem.For example require deposition material in evaporate process, not have particle and splash, can emergent gas, and can stablize and use good reproducibility.For this reason, the homogeneous deposition material of high purity, high-compactness, specific refractive index is continually developed application, and those mixed oxide deposition materials are subjected to very big attention especially, as La-Ti, La-Al, Al-Zr system or the like.Because, pre-provisioning request according to the specific refractory power size, and to the stressed condition of film and good environmental stability requirement, can reach by the kind of selecting mixed oxide and the proportioning that designs mixture, adopt certain Technology, make the deposition material of high-bulk-density, high stability, realize stablizing the purpose of film forming and application requiring.Those mixed oxides belong to the refractory material mostly, adopt conventional ceramic sintering process to be difficult to reach the fine and close requirement of homogeneous, often adopt technology such as hot pressing or HIP sintering, Medium frequency induction sintering, microwave sintering or high temperature high vacuum sintering, be prepared into suitable evaporation parent material.With the deposition material of these technology preparation, in use, must be before the beginning evaporation, allow its abundant fusion in that vacuum plating is indoor, to prevent the entrap bubble that splashes and eliminate in the material to be contained of molecule.This has prolonged the plated film cycle undoubtedly, has increased production cost.Therefore, optimal deposition material should be a fused crystalloid formed material in advance.So after someone adopts ceramic post sintering, the technology that in great-power electronic bundle stove, heats again in addition, production pre-fusion crystal qualitative deposition material.This two-step approach is made technology, has increased the production cost of deposition material.
Silicon-aluminium-mixed oxide is silica (SiO
2) and aluminium oxide (Al
2O
3) a kind of deposition material of making according to a certain ratio, about 1730 ℃ of fusing point.SiO
2-Al
2O
3The refractive index of mixed oxide film and silica membrane approach, but its internal stress is more much lower than silica membrane, is particularly suitable for plated film on the glass lens, and its environmental stability is good.Traditional silicon-aluminium-mixed oxide, sintering forms under the high temperature high vacuum in employing usually, is a kind of ceramic sintered bodies, is not the crystalloid formed material of pre-fusion.Therefore, must be earlier before evaporation in the vacuum chamber crucible with electron beam by its abundant melting, to prevent the residual gas that splashes and eliminate in the material to be contained of molecule, complex operation has prolonged the plated film cycle, has increased production cost.
Summary of the invention
In order to overcome defects, the invention provides a kind of crystal qualitative SiO
2-Al
2O
3The preparation method of mixed oxide deposition material.This preparation method can prepare the crystal qualitative SiO of pre-fusion easily
2-Al
2O
3Mixed oxide, the high purity high dense degree parent material of using as evaporation high optics film, and cost is low and product quality is higher.
The present invention for the technical scheme that solves its technical problem and adopt is: a kind of crystal qualitative SiO
2-Al
2O
3The preparation method of mixed oxide deposition material, successively according to the following steps:
Step (1), configuration SiO
2-Al
2O
3The mixed oxide powder is by weight percentage by SiO
2(50%-90%) and Al
2O
3(10%-50%) form;
Step (2) is with described SiO
2-Al
2O
3The mixed oxide powder places black-fead crucible, and black-fead crucible places vacuum medium frequency induction furnace, vacuum pressure≤1 * 10
-2Pa with intermediate frequency furnace eddy-current heating black-fead crucible, makes graphite crucible induction heating to 1650 ℃-1750 ℃, and heat radiation and heat conduct to SiO
2-Al
2O
3The mixed oxide powder forms SiO
2-Al
2O
3The mixed oxide molten mass;
Step (3) is to this SiO
2-Al
2O
3The mixed oxide molten mass is by the slow sedimentation cooling in the relative thermal treatment zone of black-fead crucible, and sinking speed just can form pre-fusion SiO
2-Al
2O
3Oxide crystal qualitative deposition material.
Further technical scheme of the present invention is:
Graphite crucible in the described step (2) adopts this SiO
2-Al
2O
3The mixed oxide powder is directly as the crucible material, and the heating power of vacuum medium frequency induction furnace is heated the graphite induction, and heat radiation and heat conduct to SiO
2-Al
2O
3Mixed powder inside makes it fusing, forms molten mass; The coil of intermediate frequency furnace is provided with circulating water, makes the SiO near sidewall of crucible
2-Al
2O
3The mixed oxide powder is not melted, and forms by SiO
2-Al
2O
3The crucible housing that raw material forms.
The intermediate frequency power power-supply frequency that medium-frequency induction furnace in the described step (2) is used is 20KHz-30KHz, and the plumbago crucible induction is generated heat to 1650 ℃-1750 ℃.
The crucible settling velocity that breaks away from the heating zone in the described step (3) is 5-10mm/h.
The steam and the entrap bubble that are occurred in described step (2) and (3) adopt the cold trap trapping device to be captured, the cryogenic temperature of cold trap trapping device≤-120 ℃.
This pre-fusion crystal qualitative SiO
2-Al
2O
3The mixed oxide deposition material is 1.46-1.48 at the light refractive index of 500 nanometer wave strong points when the optical coating, extinction coefficient≤1 * 10
-4
The invention has the beneficial effects as follows: the present invention adopts intermediate frequency furnace eddy-current heating graphite crucible, makes the mixed oxide melting and adopts the crucible sedimentation, realizes crystal qualitative SiO
2-Al
2O
3The preparation of mixed oxide deposition material.Method is simple, and cost is lower, has overcome the SiO with in the past technology of preparing production
2-Al
2O
3Existing shortcoming during the mixed oxide material evaporation;
The crystal qualitative SiO of the present invention's preparation
2-Al
2O
3Mixed oxide fritting deposition material does not need long-time melting in advance in the vacuum film coating chamber crucible, almost do not have the gentle body of aqueous vapor during evaporation and discharge, and do not produce particle in the evaporate process and splash, thereby can prepare the optical thin film of homogeneous, good reproducibility; Owing to do not need long-time fritting, compare with other non-pre-fusion deposition material in addition, greatly shorten the fritting time, thereby shorten (plated film) cycle of production, save production cost.
Description of drawings
Fig. 1 is preparation method's schema of the present invention.
Embodiment
Embodiment: the SiO that will prepare by weight proportion
2(50%-90%) and Al
2O
3(10%-50%) mixed powder is put into the vacuum medium frequency induction furnace plumbago crucible, in vacuum pressure≤1 * 10
-2Under the Pa, medium-frequency induction furnace is heated the plumbago crucible induction, because thermal radiation and conduction make the mixed oxide powder be warming up to 1650-1750 ℃ and fusion, rely on the slow sedimentation of plumbago crucible, break away from the heating zone, the temperature of melt also reduces thereupon gradually, and control settling velocity (this speed is current techique) forms crystalloid oxide compound pre-fusion body.For guaranteeing the high-purity of pre-fusion body, in whole preparation process, reach negative 120 degrees centigrade cold trap trapping device (device) by temperature, the absorption such as the residual gas in the intermediate frequency furnace and aqueous vapor are fallen, minimizing is to the pollution of melt, also effectively improve simultaneously the vacuum in the intermediate frequency furnace, thereby obtain high-compactness, highly purified pre-fusion SiO
2-Al
2O
3The crystal qualitative deposition material.This material appearance is white or shallow dark brown crystalline particle, purity 99.99%, density 2.22g/cm
3
Be applicable to the deposition of all kinds of optical thin films with the deposition material of the present invention preparation, with the sedimentary optical coating of this pre-fusion crystalloid deposition material, at 500 nano wave length places, specific refractory power is: 1.46-1.48, optical extinction coefficient≤1 * 10
-4This material has " elasticity " characteristic, and especially film forming has high-durability and adherence on glass lens, can not chap.
Claims (6)
1. crystal qualitative SiO
2-Al
2O
3The preparation method of mixed oxide deposition material is characterized in that: successively according to the following steps:
Step (1), configuration SiO
2-Al
2O
3The mixed oxide powder is by weight percentage by SiO
2: 50%-90% and Al
2O
3: 10%-50% forms;
Step (2) is with described SiO
2-Al
2O
3The mixed oxide powder places black-fead crucible, and black-fead crucible places vacuum medium frequency induction furnace, vacuum pressure≤1 * 10
-2Pa with intermediate frequency furnace eddy-current heating black-fead crucible, makes graphite crucible induction heating to 1650 ℃-1750 ℃, and heat radiation and heat conduct to SiO
2-Al
2O
3The mixed oxide powder forms SiO
2-Al
2O
3The mixed oxide molten mass;
Step (3) is to this SiO
2-Al
2O
3The mixed oxide molten mass is by the slow sedimentation cooling in the relative thermal treatment zone of black-fead crucible, and sinking speed just can form pre-fusion SiO
2-Al
2O
3Oxide crystal qualitative deposition material.
2. crystal qualitative SiO as claimed in claim 1
2-Al
2O
3The preparation method of mixed oxide deposition material is characterized in that: the graphite crucible in the described step (2) adopts this SiO
2-Al
2O
3The mixed oxide powder is directly as the crucible material, and the heating power of vacuum medium frequency induction furnace is heated the graphite induction, and heat radiation and heat conduct to SiO
2-Al
2O
3Mixed powder inside makes it fusing, forms molten mass; The coil of intermediate frequency furnace is provided with circulating water, makes the SiO near sidewall of crucible
2-Al
2O
3The mixed oxide powder is not melted, and forms by SiO
2-Al
2O
3The crucible housing that raw material forms.
3. crystal qualitative SiO as claimed in claim 1
2-Al
2O
3The preparation method of mixed oxide deposition material is characterized in that: the intermediate frequency power power-supply frequency that the intermediate frequency furnace in the described step (2) is used is 20KHz-30KHz, makes black-fead crucible induction heating to 1650 ℃-1750 ℃.
4. crystal qualitative SiO as claimed in claim 1
2-Al
2O
3The preparation method of mixed oxide deposition material is characterized in that: the crucible sinking speed that breaks away from the thermal treatment zone in the described step (3) is 5-10mm/h.
5. crystal qualitative SiO as claimed in claim 1
2-Al
2O
3The preparation method of mixed oxide deposition material is characterized in that: the steam and the residual gas that occur in described step (2) and (3), adopt the cold trap trapping device to be captured, the cryogenic temperature of cold trap trapping device≤-120 ℃.
6. crystal qualitative SiO as claimed in claim 1
2-Al
2O
3The preparation method of mixed oxide deposition material is characterized in that: this pre-fusion crystal qualitative SiO
2-Al
2O
3The mixed oxide deposition material is 1.46-1.48 at the light refractive index of 500 nanometer wave strong points when the optical coating, extinction coefficient≤1 * 10
-4
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|---|---|---|---|
| CNB2008101224447A CN100549216C (en) | 2008-05-28 | 2008-05-28 | Crystal qualitative SiO 2-Al 2O 3The preparation method of mixed oxide deposition material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2008101224447A CN100549216C (en) | 2008-05-28 | 2008-05-28 | Crystal qualitative SiO 2-Al 2O 3The preparation method of mixed oxide deposition material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101294269A true CN101294269A (en) | 2008-10-29 |
| CN100549216C CN100549216C (en) | 2009-10-14 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557039A (en) * | 2014-12-24 | 2015-04-29 | 福州阿石创光电子材料有限公司 | Intermediate-refraction index evaporation coating material, as well as preparation technique and application thereof |
| CN105405986A (en) * | 2015-12-16 | 2016-03-16 | 张家港康得新光电材料有限公司 | Moisture barrier film, preparation method thereof and display containing the same |
| CN106019417A (en) * | 2016-08-08 | 2016-10-12 | 北京富兴凯永兴光电技术有限公司 | Low-refractive-index optical coating material |
| CN109207934A (en) * | 2017-06-29 | 2019-01-15 | 中国科学院上海硅酸盐研究所 | A method of high-reflecting film microdefect is improved using quartz ring optical filming material |
-
2008
- 2008-05-28 CN CNB2008101224447A patent/CN100549216C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557039A (en) * | 2014-12-24 | 2015-04-29 | 福州阿石创光电子材料有限公司 | Intermediate-refraction index evaporation coating material, as well as preparation technique and application thereof |
| CN105405986A (en) * | 2015-12-16 | 2016-03-16 | 张家港康得新光电材料有限公司 | Moisture barrier film, preparation method thereof and display containing the same |
| CN106019417A (en) * | 2016-08-08 | 2016-10-12 | 北京富兴凯永兴光电技术有限公司 | Low-refractive-index optical coating material |
| CN109207934A (en) * | 2017-06-29 | 2019-01-15 | 中国科学院上海硅酸盐研究所 | A method of high-reflecting film microdefect is improved using quartz ring optical filming material |
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| Publication number | Publication date |
|---|---|
| CN100549216C (en) | 2009-10-14 |
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Granted publication date: 20091014 Termination date: 20160528 |