CN101328065B - Preparation of vitrified Ta2O5-TiO2 composite metal oxide vapor deposition material - Google Patents
Preparation of vitrified Ta2O5-TiO2 composite metal oxide vapor deposition material Download PDFInfo
- Publication number
- CN101328065B CN101328065B CN2008101224432A CN200810122443A CN101328065B CN 101328065 B CN101328065 B CN 101328065B CN 2008101224432 A CN2008101224432 A CN 2008101224432A CN 200810122443 A CN200810122443 A CN 200810122443A CN 101328065 B CN101328065 B CN 101328065B
- Authority
- CN
- China
- Prior art keywords
- tio
- crucible
- preparation
- metal oxide
- composite metal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a method for preparing a crystalloid Ta2O5-TiO2 composite metal oxide vapor plating material comprising preparing mixed oxide powders of 70%-90% of tantalum pentaoxide and 10%-30% of titanium dioxide by weight percentage in a high vacuum high frequency furnace crucible, heating the mixed powders till 1800 DEG C by means of high frequency source under a vacuum less than or equal to 1*10<-2>Pa, forming Ta2O5-TiO2 composite oxide molten mass, slowly sedimenting and cooling the molten mass with a certain sedimentation rate to form pre-molten crystalloid Ta2O5-TiO2 composite oxide vapor plating material. The vapour and residual gas arisen during the preparation process are trapped by a cold trapper at a deep cold temperature less than or equal to -120 DEG C. The invention prepares pre-molten crystalloid Ta2O5-TiO2 composite oxide using slow sedimentation crystal growth method in a high vacuum high frequency furnace crucible. The product of the invention is the high pure and density original evaporating material used in the vapor plating advanced optical film with a low cost and reliable quality.
Description
Technical field
The present invention relates to a kind of structural evaporation coating film material preparation method, relate in particular to a kind of crystal qualitative Ta
2O
5-TiO
2The preparation method of composite metal oxide vapor deposition.
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, do not have evolving 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.But by the optical thin film of simple oxide compound evaporation, often internal stress is bigger, and anti-environmental stability is relatively poor, makes moist easily, also is difficult to satisfy the needed specific refractory power size of different application.Therefore, those composite oxides deposition materials are subjected to very big attention, such as Si-Al, La-Ti, La-Al and Al-Zr system etc.Because, people are according to the pre-provisioning request of 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 infusibility high-temperature material mostly, adopt conventional ceramic sintering process to be difficult to reach the fine and close requirement of homogeneous, often to 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, be ceramic sintered bodies, 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 someone adopts the oxide ceramics that will sinter, be put into again in the great-power electronic bundle stove and heat, become the pre-fusion material.This two-step approach is made the technology of deposition material, complex operation production cost height.
Ta
2O
5And TiO
2It all is high-index material.Ta
2O
5After repeatedly evaporating, the evaporator crucible bottom can produce the hole, makes the evaporation process instability; Ta
2O
5Usually need post processing just can obtain transparent film.TiO
2Be good deposition material, but easily form the heterogeneous body thin-film material.So often need to use Ti
3O
5Make the evaporation parent material.Ta
2O
5-TiO
2Composite oxide film still keeps high refractive index, and it not only has the stable properties of materials that homogenizes, and its internal stress is more much lower than titanium deoxid film.Ta
2O
5-TiO
2Composite oxides are Ta
2O
5And TiO
2A kind of deposition material of making according to a certain ratio, about 1800 ℃ of fusing point.Traditional composite oxides deposition material, employing generation solid state reaction under the high temperature high vacuum forms sintered compact usually, but is not the crystalloid formed material of pre-fusion.Therefore, as the evaporation parent material time, must be earlier before the evaporation in the indoor elder generation of vacuum plating with electron beam by its long-time fully fusion, the entrap bubble that splashes and eliminate in the material to be contained of molecule when avoiding evaporating, can make complex operation like this, prolong the plated film cycle, increased production cost.
Summary of the invention
In order to overcome defects, the invention provides a kind of crystal qualitative Ta
2O
5-TiO
2The preparation method of composite metal oxide vapor deposition.This preparation method can prepare the crystal qualitative Ta of pre-fusion easily
2O
5-TiO
2Composite metal oxide vapor deposition, the initial evaporating materials of high purity high dense degree 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 Ta
2O
5-TiO
2The preparation method of composite metal oxide vapor deposition, successively according to the following steps:
Step (1), configuration Ta
2O
5And TiO
2Composite metal oxide powder is by weight percentage by Ta
2O
5: 70%-90% and TiO
2: 10%-30% forms;
Step (2) is with this Ta
2O
5-TiO
2Mixed powder places crucible, and crucible places the vacuum high-frequency stove, vacuum pressure≤1 * 10
-2Pa utilizes the high-frequency power supply of coreless induction furnace directly to heat Ta
2O
5-TiO
2Mixed oxide powder to 1750 ℃-1800 ℃ forms Ta
2O
5-TiO
2The composite oxides molten mass;
Step (3) makes described Ta
2O
5-TiO
2The composite oxides molten mass leaves the thermal treatment zone and slowly sedimentation cooling gradually, and the sinking speed (this speed is current techique) during sedimentation just can make described Ta
2O
5-TiO
2The composite oxides molten mass forms pre-fusion crystal qualitative Ta
2O
5-TiO
2The composite oxides deposition material.
The settling velocity of crucible is 5-10mm/h in the described step (3).
Further technical scheme of the present invention is:
Crucible in the described step (2) directly adopts this Ta
2O
5-TiO
2The mixed oxide powder makes Ta with high-frequency power supply as the crucible material in vacuum drying oven
2O
5-TiO
2Mixed oxide powder fusing is equipped with water-circulating cooling device in the coil of coreless induction furnace, the top layer material powder is not melted and forms the housing that is made up of material powder, becomes crucible.
The high-frequency power supply frequency of described step (2) medium-high frequency stove is 1MHz-5MHz, with Ta
2O
5-TiO
2The mixed oxide powder is heated to 1750 ℃-1800 ℃.
The steam that occurs in described step (2) and (3) preparation process and entrap bubble adopt the cold trap trapping device to capture, and the cold trap trapping device captures cryogenic temperature≤-120 of adopting ℃.
Described crystalloid Ta
2O
5-TiO
2When the composite oxides deposition material was used as optical coating, the light refractive index at 500 nano wave length places was 2.2-2.25, optical extinction coefficient≤2 * 10
-4
Useful technique effect of the present invention is: the present invention adopts the long brilliant method of high frequency high vacuum furnace crucible, and a direct step is realized pre-fusion crystalloid Ta2O
5-TiO
2The preparation of composite oxides deposition material need not to use other Technology with its fritting again, and method is simple, and cost is lower, existing shortcoming when having overcome in the past the composite oxide material evaporation;
The crystal qualitative Ta of the present invention's preparation
2O
5-TiO
2Composite oxides 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, and can improve Ta
2O
5Repeatedly crucible bottom produces the defective in hole after the evaporation, thereby can prepare the optical thin film of homogeneous, more stable N, K optical parametric is arranged, 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 growth cost.
Description of drawings
Fig. 1 is preparation method's schema of the present invention.
Embodiment
With the Ta for preparing by weight proportion
2O
5(70%-90%) and TiO
2(10%-30%) the mixed oxide powder is put into vacuum oven (crucible) ,≤1 * 10
-2By high frequency source this mixed oxide powder is heated to 1800 ℃ under the Pa vacuum, the profound hypothermia cold trap trapping device of fusion and being aided with in vacuum oven (crucible)≤-120 ℃ captures aqueous vapor and other entrap bubbles in this powder, by the slow sedimentation cooling of crucible (lowering speed 5-10mm/h), obtain the crystalloid Ta of pre-fusion at last simultaneously
2O
5-TiO
2The composite oxides product.
Because described composite oxides are infusibility high-temperature materials, can't in the crucible that is formed by high melting point metal materials, allow their meltings long brilliant.Therefore, the present invention directly uses described Ta
2O
5And TiO
2Mixed oxidization raw material itself is as crucible material, in vacuum drying oven, make its inner fully fusing with high frequency power source, the crucible outside is then because being equipped with water-circulating cooling device, its top layer raw material is not melted, thereby form one deck by the not fusion crust body that raw material own forms, played the effect that is equivalent to crucible.The inner described Ta that has melted
2O
5-TiO
2Composite oxides rely on the slow sedimentation of crucible, break away from the thermal treatment zone, and the temperature of melt also reduces thereupon gradually, form crystalloid oxide pre-fusion body.For guaranteeing the high-purity of pre-melt, in whole preparation process, reach negative 120 cold-trap devices of spending Celsius by temperature, the absorption such as the residual gas in the stove and hydrone are fallen, reduce the pollution to melt, also effectively improve the vacuum in the stove simultaneously.
Because the molten mass that generates is not directly to contact crucible, but the material of contact and melt powder of the same race, so there is not pollution problem in molten mass, thereby can obtain the fritting crystal qualitative Ta of high-purity, high-compactness
2O
5-TiO
2Compound deposition material.This material appearance is pitch black bright crystalloid particle, and purity 99.99%, density are 8.1g/cm
3
As embodiments of the invention, with pre-fusion crystal qualitative Ta
2O
5-TiO
2Composite oxides during electron gun evaporation, do not need fritting as deposition material, almost do not have the gentle body of aqueous vapor and discharge, molecule can not take place yet spatter, the optical coating of deposition, transparency range: 0.4-7 μ, in 500 nanometer wave strong points, refractive index is: 2.1-2.25, extinction coefficient≤2 * 10
-4The rete wet fastness: 50 ℃ of relative humidity 95% time, theca interna was intact in 72 hours.
Claims (5)
1. crystal qualitative Ta
2O
5-TiO
2The preparation method of composite metal oxide vapor deposition is characterized in that: successively according to the following steps:
Step (1), configuration Ta
2O
5And TiO
2Composite metal oxide powder is by weight percentage by Ta
2O
5: 70%-90% and TiO
2: 10%-30% forms;
Step (2) is with this Ta
2O
5-TiO
2Mixed powder places crucible, and crucible places the vacuum high-frequency stove, vacuum pressure≤1 * 10
-2Pa utilizes the high-frequency power supply of coreless induction furnace directly to heat Ta
2O
5-TiO
2Mixed oxide powder to 1750 ℃-1800 ℃ forms Ta
2O
5-TiO
2The composite oxides molten mass;
Step (3) makes described Ta
2O
5-TiO
2The composite oxides molten mass leaves the thermal treatment zone and slowly sedimentation cooling gradually, and the sinking speed during sedimentation just can make described Ta
2O
5-TiO
2The composite oxides molten mass forms pre-fusion crystal qualitative Ta
2O
5-TiO
2The composite oxides deposition material;
The settling velocity of crucible is 5-10mm/h in the described step (3).
2. crystal qualitative Ta as claimed in claim 1
2O
5-TiO
2The preparation method of composite metal oxide vapor deposition is characterized in that: the crucible in the described step (2) directly adopts this Ta
2O
5-TiO
2The mixed oxide powder makes Ta with high-frequency power supply as the crucible material in vacuum drying oven
2O
5-TiO
2Mixed oxide powder fusing is equipped with water-circulating cooling device in the coil of coreless induction furnace, the top layer material powder is not melted and forms the housing that is made up of material powder, becomes crucible.
3. crystal qualitative Ta as claimed in claim 1
2O
5-TiO
2The preparation method of composite metal oxide vapor deposition is characterized in that: the high-frequency power supply frequency of described step (2) medium-high frequency stove is 1MHz-5MHz, with Ta
2O
5-TiO
2The mixed oxide powder is heated to 1750 ℃-1800 ℃.
4. crystal qualitative Ta as claimed in claim 1
2O
5-TiO
2The preparation method of composite metal oxide vapor deposition is characterized in that: the steam that occurs in described step (2) and (3) preparation process and residual gas adopt the cold trap trapping device to capture, the cryogenic temperature that the capture of cold trap trapping device is adopted≤-120 ℃.
5. crystal qualitative Ta as claimed in claim 1
2O
5-TiO
2The preparation method of composite metal oxide vapor deposition is characterized in that: crystal qualitative Ta
2O
5-TiO
2The composite oxides deposition material is 2.2-2.25 at the light refractive index of 500 nanometer wave strong points when the optical coating, extinction coefficient≤2 * 10
-4
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101224432A CN101328065B (en) | 2008-05-28 | 2008-05-28 | Preparation of vitrified Ta2O5-TiO2 composite metal oxide vapor deposition material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101224432A CN101328065B (en) | 2008-05-28 | 2008-05-28 | Preparation of vitrified Ta2O5-TiO2 composite metal oxide vapor deposition material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101328065A CN101328065A (en) | 2008-12-24 |
| CN101328065B true CN101328065B (en) | 2011-08-24 |
Family
ID=40204115
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008101224432A Expired - Fee Related CN101328065B (en) | 2008-05-28 | 2008-05-28 | Preparation of vitrified Ta2O5-TiO2 composite metal oxide vapor deposition material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101328065B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101439968B (en) * | 2008-12-26 | 2011-07-20 | 北京工业大学 | Method for realizing (Ta2O5)1-x(TiO2)x based ceramic dielectric temperature coefficient thermal compensation |
| CN103046134A (en) * | 2012-12-20 | 2013-04-17 | 上海晶炼新材料有限公司 | Crystalline optical coating material tantalum oxide with high refractive index and preparation method thereof |
| JP7044328B2 (en) * | 2018-06-01 | 2022-03-30 | 株式会社荏原製作所 | A method for producing a Ni—Fe-based alloy powder and an alloy film using the Ni—Fe-based alloy powder. |
| CN112522674B (en) * | 2021-02-18 | 2021-05-04 | 中南大学湘雅医院 | Titanium alloy surface composite coating and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076527A (en) * | 1992-03-19 | 1993-09-22 | 默克专利股份有限公司 | The vapour-deposition material that is used for production high index of refraction optical coating |
-
2008
- 2008-05-28 CN CN2008101224432A patent/CN101328065B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076527A (en) * | 1992-03-19 | 1993-09-22 | 默克专利股份有限公司 | The vapour-deposition material that is used for production high index of refraction optical coating |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101328065A (en) | 2008-12-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhou et al. | Surface plasmon resonance induced excellent solar control for VO 2@ SiO 2 nanorods-based thermochromic foils | |
| CN101328065B (en) | Preparation of vitrified Ta2O5-TiO2 composite metal oxide vapor deposition material | |
| KR101514443B1 (en) | Transparent phosphor and process for producing the transparent phosphor | |
| CN102560665B (en) | Method for growing cerium-doped alumina-yttrium aluminum garnet eutectic fluorescent material | |
| CN103803804A (en) | Nano glass ceramic up-conversion luminescent material and preparation method thereof | |
| CN100549216C (en) | Crystal qualitative SiO 2-Al 2O 3The preparation method of mixed oxide deposition material | |
| CN109400123A (en) | A kind of fine-grained alumina ceramics and its preparation method and application | |
| CN106536449A (en) | Transparent metal fluoride ceramic | |
| CN100532629C (en) | Method for preparing premelting lanthanum titanate crystalloid steam plating material | |
| CN104386723A (en) | Preparation method of high-purity aluminum oxide | |
| CN109053157A (en) | A kind of Ga2O3Base co-doped material target and preparation method thereof | |
| US7449238B1 (en) | LiF-coated doped and undoped yttrium oxide | |
| CN107555800A (en) | Transparent Sr3Al2O6‑SrAl2O4Glass-ceramic and method for producing the same | |
| Zong et al. | Preparation and characterization of VO2/Cu-Zr NPs/VO2 composite films with enhanced thermochromic properties | |
| CN101013614A (en) | Transparent conducting Composite material, film, board and method of manufacturing the same | |
| CN108409148B (en) | Infrared incoherent LED excited upconversion NaLuF4Glass-ceramic and method for producing the same | |
| CN110204200A (en) | A kind of preparation method of doped silica glass evaporation material | |
| CN105887182A (en) | Preparation technology of trititanium pentoxide crystal | |
| CN111252799B (en) | Preparation of YAG Ce by containerless solidification3+Method for mixing amorphous material with aluminum nitride | |
| EP2639343B1 (en) | A method of manufacturing thin layers of eutectic composites | |
| Suleimanov et al. | Effective antireflection coating based on TiO 2-SiO 2 mixture for solar cells | |
| CN110983270B (en) | Oxide-metal composite nano glass material | |
| US7300617B2 (en) | Method of making fusion cast articles | |
| CN113184893B (en) | Praseodymium aluminate optical film melting material and preparation method and application thereof | |
| CN115417602A (en) | Vanadium pentoxide thin film material for intelligent window and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20081224 Assignee: Jing Bang optical products (Changshu) Co., Ltd. Assignor: Kunshan Guangming Optoelectronics Element Co., Ltd. Contract record no.: 2013320000084 Denomination of invention: Method for preparing crystalline Ta2O5-TiO2 composite metal oxide evaporation material Granted publication date: 20110824 License type: Exclusive License Record date: 20130312 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110824 Termination date: 20160528 |