CN101200794A - Method for preparing premelting lanthanum titanate crystalloid steam plating material - Google Patents
Method for preparing premelting lanthanum titanate crystalloid steam plating material Download PDFInfo
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- CN101200794A CN101200794A CNA2007100237623A CN200710023762A CN101200794A CN 101200794 A CN101200794 A CN 101200794A CN A2007100237623 A CNA2007100237623 A CN A2007100237623A CN 200710023762 A CN200710023762 A CN 200710023762A CN 101200794 A CN101200794 A CN 101200794A
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Abstract
A pre-melted lanthanum titanate vapor plating material preparation method is provided. Firstly, lanthanum titanate mixed oxide powder is configured, which consists of 8 to 70 percent of La2O3 and 30 to 92 percent of TiO2 according to the weight percentage. The mixed oxide powder is arranged in a vacuum furnace cold crucible. Under the high vacuum (less than or equal to 1*10<-2>Pa), high frequency source is heated to 1800-2500 DEG C to form lanthanum titanate molten mass. The lanthanum titanate molten mass is cooled through slow settlement to form the pre-melted lanthanum titanate sparry vapor plating material. Water vapor and residue gas during the preparation process are trapped through a cold trap. The deep cold temperature is less than or equal to 100 DEG C below zero. The invention uses a high vacuum high frequency cold crucible slow settlement crystal growth method to prepare the pre-melted mixed oxide to be used as initial material with high purity and density used for vapor plating advanced optical films.
Description
Technical field
The invention belongs to evaporation coating material preparation technology and scientific domain, particularly a kind of method for preparing fritting lanthanium titanate crystalloid deposition material.
Background technology
Optical coating Application Areas fast-developing day by day and thereupon propose more high performance demand impels deposition material and film thereof must keep synchronized development.For example in emerging photoelectronic industry, digital display screen, imaging and optical projection system, communication are with products such as accurate optical filterings, more and more be tending towards high brightness, high definition, overlarge area and hyperfine structure direction and develop, require optical thin film that stable specific refractory power, high light transmittance, high-compactness and high purity or the like are arranged.Except strictness control coating process, evaporation parent material and technology of preparing thereof become a very crucial problem, for example require deposition material not have particle in evaporate process and splash, can evolving gas, and can stablize the use good reproducibility.For this reason, the homogeneous 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
2O
3-TiO
2System, La
2O
3-Al
2O
3System, Al
2O
3-ZrO
2System or the like according to the pre-provisioning request of specific refractory power size, can reach by the proportioning that designs mixture easily, adopts certain Technology, makes the deposition material of high-bulk-density, high stability, realizes stablizing film forming purpose.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 hot pressing or HIP sintering, Medium frequency induction sintering, microwave sintering or high temperature high vacuum sintering or the like.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 increased the plated film cycle undoubtedly, increases production cost.Therefore, optimal deposition material should be a fused material in advance, so there is the people to adopt the method that is heated into pre-melt behind the ceramic post sintering again in great-power electronic bundle stove.
Lanthanium titanate is the mixed oxide of rare earth lanthanum oxide and titanium oxide.Before five more than ten years, made the low-temperature coefficient electrical condenser with this material, people have done a lot of researchs to its phasor thereafter, might be the candidate materials of high temperature piezoelectric device and electro-optical device.In recent years, German Merck company and U.S. Phelly Materials Co., Ltd etc. were with La
2O
3-TiO
2Be used for deposition material.Merck company adopts high temperature (1500 ℃-1600 ℃) high vacuum 10
-4Mbar) go through and sintered black lanthanium titanate block in 5.5-6.5 hour into, but be not a kind of crystallization lanthanium titanate of fritting as deposition material.
Summary of the invention
The present invention is to provide a kind of method for preparing premelting lanthanum titanate crystalloid steam plating material, be equipped with the mixed oxide of pre-fusion, the high purity high dense degree parent material of using as evaporation high optics film with the long brilliant legal system of the slow sedimentation of a kind of high vacuum high frequency cold crucible.
Technical scheme of the present invention is achieved in that a kind of fritting lanthanum titanate evaporation material preparation method, may further comprise the steps successively:
(1) configuration lanthanium titanate mixed oxide powder is by weight percentage by La
2O
3(8-70%) and TiO
2(30-92%) form;
(2) this mixed oxide powder is placed the melted and cooled in vacuum crucible, vacuum pressure≤1 * 10
-2Pa utilizes high frequency source to be heated to 1800 ℃-2500 ℃, forms the lanthanium titanate molten mass;
(3) this lanthanium titanate molten mass is cooled off by slow sedimentation, form fritting lanthanium titanate crystalloid deposition material.
As a further improvement on the present invention, this cold crucible directly adopts this lanthanium titanate mixed oxide powder as the crucible material, makes its material inside fusing at the indoor high frequency electric source of vacuum, and water cooling plant is equipped with in the outside, the top layer raw material is not melted, thereby forms this melted and cooled in vacuum crucible.
As a further improvement on the present invention, this high frequency source frequency is 1MHZ-5MHZ.
As a further improvement on the present invention, this sedimentation speed of cooling is 5-10mm/hr.
As a further improvement on the present invention, adopt the cold trap trapping device to capture to steam and entrap bubble in the preparation process, cryogenic temperature≤-100 ℃.
Useful technique effect of the present invention is: the fritting lanthanium titanate crystalloid deposition material of the present invention's preparation, in the vacuum film coating chamber crucible, do not need long-time fusion in advance, do not splash, can evolving gas, thereby can prepare the high refractive index film of homogeneous, good reproducibility; Owing to do not need long-time fritting, compare in addition, shorten the fritting time greatly, thereby shorten (plated film) cycle of production, save the growth cost with other non-pre-fusion deposition material.
Description of drawings
Fig. 1 is preparation method's schema of the present invention.
Embodiment
With the La for preparing
2O
3(8-70%) and TiO
2(30-92%) the mixed oxide powder is put into vacuum oven (containing cold crucible) ,≤1*10
-2By high frequency source this mixed oxide powder is heated to 1800 ℃-2500 ℃ under the Pa vacuum, the profound hypothermia cold trap trapping device of fusion and being aided with in the melted and cooled in vacuum crucible≤-100 ℃, capture aqueous vapor and other entrap bubbles in this powder, by slow sedimentation cooling (lowering speed 5-10mm/hr), obtain the crystalloid lanthanium titanate product of fritting at last simultaneously.
Because described lanthanium titanate mixed oxide all is refractory high-temperature material, can't in the earthenware Crucible that forms by high melting point metal materials, allow their fusions long brilliant.Therefore, the present invention directly with described lanthanium titanate mixed oxidization raw material itself as earthenware Crucible material, make its inner fully fusing at the indoor high frequency electric source of vacuum, the outside is then because of being equipped with water cooling plant, its top layer raw material is not melted, thereby form the not fusion crust body that one deck is made up of raw material own, played earthenware Crucible effect.The inner described lanthanium titanate mixed oxide that has melted relies on the slow sedimentation of earthenware Crucible, breaks away from the heating zone, and the temperature of melt also reduces thereupon gradually, forms crystalloid oxide compound pre-fusion body.For guaranteeing the high purity of pre-melt, in whole process of preparation, reach the negative 100 cold-trap devices of spending Celsius by temperature, absorption such as entrap bubble in the stove and water molecules are fallen, reduce pollution to melt, also improve the vacuum tightness in the stove simultaneously effectively.
Because the molten mass that generates is not directly to contact the crucible material, but contact and melt powder of the same race, so there is not pollution problem in molten mass, thereby can obtain high-compactness, highly purified fritting lanthanium titanate crystalloid deposition material.
Be applicable to the deposition of all kinds of optical thin films with the deposition material of long crystal method preparation of the present invention.With the sedimentary optical coating of this fritting lanthanum titanate evaporation material, at 500 nano wave length places, specific refractory power is as embodiment: 2.10～2.28, and optical extinction coefficient≤2*10
-4
Claims (5)
1. a method for preparing premelting lanthanum titanate crystalloid steam plating material is characterized in that, may further comprise the steps successively:
(1) configuration lanthanium titanate mixed oxide powder is by weight percentage by La
2O
3(8-70%) and TiO
2(30-92%) form;
(2) this mixed oxide powder is placed the melted and cooled in vacuum crucible, vacuum pressure≤1 * 10
-2Pa utilizes high frequency source to be heated to 1800 ℃-2500 ℃, forms the lanthanium titanate molten mass;
(3) this lanthanium titanate molten mass is cooled off by slow sedimentation, form fritting lanthanium titanate crystalloid deposition material.
2. a kind of method for preparing premelting lanthanum titanate crystalloid steam plating material as claimed in claim 1, it is characterized in that, cold crucible in the step (2) directly adopts this lanthanium titanate mixed oxide powder as the crucible material, make its material inside fusing at the indoor high frequency electric source of vacuum, water cooling plant is equipped with in the outside, the top layer raw material is not melted, thereby forms this melted and cooled in vacuum crucible.
3. a kind of method for preparing premelting lanthanum titanate crystalloid steam plating material as claimed in claim 1 is characterized in that, the high frequency source frequency in the step (2) is 1MHZ-5MHZ.
4. a kind of method for preparing premelting lanthanum titanate crystalloid steam plating material as claimed in claim 1 is characterized in that, the settling velocity in the step (3) is 5-10mm/hr.
5. a kind of method for preparing premelting lanthanum titanate crystalloid steam plating material as claimed in claim 1 is characterized in that, adopts the cold trap trapping device to capture to steam and entrap bubble in the preparation process, cryogenic temperature≤-100 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100237623A CN100532629C (en) | 2007-07-09 | 2007-07-09 | Method for preparing premelting lanthanum titanate crystalloid steam plating material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100237623A CN100532629C (en) | 2007-07-09 | 2007-07-09 | Method for preparing premelting lanthanum titanate crystalloid steam plating material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101200794A true CN101200794A (en) | 2008-06-18 |
| CN100532629C CN100532629C (en) | 2009-08-26 |
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ID=39516144
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|---|---|---|---|
| CNB2007100237623A Expired - Fee Related CN100532629C (en) | 2007-07-09 | 2007-07-09 | Method for preparing premelting lanthanum titanate crystalloid steam plating material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102062881A (en) * | 2010-11-25 | 2011-05-18 | 福州阿石创光电子材料有限公司 | High refractive index evaporation material lanthanum titanate mixture and preparation method thereof |
| CN102864410A (en) * | 2012-08-31 | 2013-01-09 | 西北工业大学 | Preparation method of high dielectric constant gate dielectric lanthanum titanium oxide amorphous film |
| 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 |
| CN114133226A (en) * | 2021-12-30 | 2022-03-04 | 苏州晶生新材料有限公司 | Optical coating substrate and using method thereof |
-
2007
- 2007-07-09 CN CNB2007100237623A patent/CN100532629C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102062881A (en) * | 2010-11-25 | 2011-05-18 | 福州阿石创光电子材料有限公司 | High refractive index evaporation material lanthanum titanate mixture and preparation method thereof |
| CN102062881B (en) * | 2010-11-25 | 2012-07-04 | 福州阿石创光电子材料有限公司 | High refractive index evaporation material lanthanum titanate mixture and preparation method thereof |
| CN102864410A (en) * | 2012-08-31 | 2013-01-09 | 西北工业大学 | Preparation method of high dielectric constant gate dielectric lanthanum titanium oxide amorphous film |
| 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 |
| CN114133226A (en) * | 2021-12-30 | 2022-03-04 | 苏州晶生新材料有限公司 | Optical coating substrate and using method thereof |
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| Publication number | Publication date |
|---|---|
| CN100532629C (en) | 2009-08-26 |
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