CN102062881B - High refractive index evaporation material lanthanum titanate mixture and preparation method thereof - Google Patents
High refractive index evaporation material lanthanum titanate mixture and preparation method thereof Download PDFInfo
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- CN102062881B CN102062881B CN2010105589457A CN201010558945A CN102062881B CN 102062881 B CN102062881 B CN 102062881B CN 2010105589457 A CN2010105589457 A CN 2010105589457A CN 201010558945 A CN201010558945 A CN 201010558945A CN 102062881 B CN102062881 B CN 102062881B
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Abstract
The invention relates to a high refractive index evaporation material lanthanum titanate mixture and a preparation method thereof. The mixture is composed of La2Ti2O7 and La4Ti9O24 in a chemical formula. The preparation method thereof comprises the following steps: taking TiO2 and La(OH)3 as raw materials, and mixing to be uniform; carrying out an initial catalytic reaction at normal temperature,and obtaining the required shape by cold pressing or hot pressing; transferring a crucible filled with the obtained semi-finished product into a normal-pressure high-temperature furnace, and heating the furnace to 700-1300 DEG C for processing, thus the product is initially sized; and placing the semi-finished product into a vacuum sintering furnace, heating the whole system to 1400-1600 DEG C and vacuumizing, insulating for 2-4 hours, and cooling to obtain the lanthanum titanate mixture material. The preparation method has high production efficiency, manufacturing cost is low, and lanthanum titanate mixture in arbitrary shape can be prepared, the melting point of the prepared lanthanum titanate mixture is low, and the prepared lanthanum titanate mixture is easy to be melted and evaporated to form a stable optical coating.
Description
[technical field]
The present invention relates to a kind of high index of refraction evaporating materials lanthanium titanate preparation process of mixture.
[background technology]
High index of refraction optical thin film material is widely used in the design of various optical films; They mainly are used for being used the various antireflective films of preparation with low-index material or with middle refraction materials, and these films mainly are used in the lens, prism, reflective mirror of optical instrument etc.Present widely used high-index material mainly contains the oxide of various titaniums, zirconium, hafnium, tantalum, niobium and their composite material.
Now along with constantly more new development of field of optical applications, and the improving constantly of performance requirement, impel the thin evaporated film material also must be along with synchronized development.And oxide film material as in the membraneous material must a ring, various element different proportions are combined into compound or potpourri, can be better particularly strong support be provided the image field for the photoelectric field that now constantly advances.
Existing oxide film material preparation method is being broken into particle for powder through direct vacuum-sintering of moulding or the direct vacuum-sintering of powder, and sintering time is long, and broken behind the sintering, and initial powder is more, and yield rate is low.
[summary of the invention]
Technical matters to be solved by this invention is to provide a kind of high index of refraction evaporating materials lanthanium titanate preparation process of mixture; This preparation method's production efficiency is high, low cost of manufacture and can be made into the lanthanium titanate potpourri of arbitrary shape; Prepared lanthanium titanate potpourri fusing point is low, and the fusing evaporation forms stable optical coating easily.
The present invention adopts following technical scheme to solve the problems of the technologies described above:
A kind of high index of refraction evaporating materials lanthanium titanate preparation process of mixture comprises the steps:
Step 1: get TiO
2And La (OH)
3Be raw material, press mole molecular proportion example La a: Ti=1: 1～2 this potpourri of configuration, and mix;
Step 2: under room temperature, carry out preliminary catalytic reaction,, process required shape through mode of colding pressing or hot pressing mode through water with as the alcohols of organic catalyst;
Step 3: the crucible that the semi-manufacture of step 2 gained are placed moves in the constant-pressure and high-temperature stove, furnace temperature is risen to 700～1300 ℃ carry out pre-service, and product is tentatively finalized the design;
Step 4: the semi-manufacture with the step 3 gained are positioned in the vacuum sintering furnace again, total system is warming up to 1400～1600 ℃, and vacuumizes, and keep beginning to cool down after 2～4 hours, prepare the lanthanium titanate mixture material.
The invention has the advantages that: this method is passed through moulding and pre-service in advance, has effectively solved the problem of shape size, and has reduced the vacuum-sintering sintering time, effectively raises production efficiency, saves production cost.This mixture melt temperature is 1770 ℃, and is lower than the lanthanium titanate fusing point of one-component, and easy fusing evaporation forms stable optical coating, reduces service condition, for the production optical coating reduces cost strong support is provided.
[embodiment]
Embodiment one:
With raw material TiO
2And La (OH)
3La: Ti=1 in molar ratio: 1 configuration; Under room temperature, carry out preliminary catalytic reaction through water with as the ethanol of organic catalyst, with press the complex that above-mentioned catalytic reaction produces is processed into the certain specification shape again, the crucible that the semi-manufacture of gained are placed moves in the constant-pressure and high-temperature stove; Furnace temperature is risen to 1300 ℃ carry out pre-service; Product is tentatively finalized the design, and the semi-manufacture with gained are positioned in the vacuum sintering furnace again, are evacuated to 10
-3Pa keeps beginning to cool down after 4 hours, prepares lanthanium titanate mixture material (La
2Ti
2O
7And La
4Ti
9O
24).In concrete practice, can add a spot of Ti in the raw material.
Embodiment two
With raw material TiO2, Ti and La (OH) 3 La: Ti=1 in molar ratio: 2 configurations; Under room temperature, carry out preliminary catalytic reaction through water with as the glycerine of organic catalyst, with press the complex that above-mentioned catalytic reaction produces is processed into the certain specification shape again, the crucible that the semi-manufacture of gained are placed moves in the constant-pressure and high-temperature stove; Furnace temperature is risen to 700 ℃ carry out pre-service; Product is tentatively finalized the design, and the semi-manufacture with gained are positioned in the vacuum sintering furnace again, are evacuated to 10
-3Pa keeps beginning to cool down after 2 hours, prepares lanthanium titanate mixture material (La
2Ti
2O
7And La
4Ti
9O
24).In concrete practice, can add a spot of Ti in the raw material.
Preparation method of the present invention passes through moulding and pre-service in advance, has effectively solved the problem of shape size, and has reduced the vacuum-sintering sintering time, effectively raises production efficiency, saves production cost.This mixture melt temperature is 1770 ℃, and is lower than the lanthanium titanate fusing point of one-component, and easy fusing evaporation forms stable optical coating, reduces service condition, for the production optical coating reduces cost strong support is provided.
Claims (1)
1. a high index of refraction evaporating materials lanthanium titanate preparation process of mixture is characterized in that: comprise the steps:
Step 1: get TiO
2And La (OH)
3Be raw material, press mole molecular proportion example La a: Ti=1: 1～2 this potpourri of configuration, and mix;
Step 2: under room temperature, carry out preliminary catalytic reaction,, process required shape through mode of colding pressing or hot pressing mode through water with as the alcohols of organic catalyst;
Step 3: the crucible that the semi-manufacture of step 2 gained are placed moves in the constant-pressure and high-temperature stove, furnace temperature is risen to 700～1300 ℃ carry out pre-service, and product is tentatively finalized the design;
Step 4: the semi-manufacture with the step 3 gained are positioned in the vacuum sintering furnace again, total system is warming up to 1400～1600 ℃, and vacuumizes, and keep beginning to cool down after 2～4 hours, prepare the lanthanium titanate mixture material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105589457A CN102062881B (en) | 2010-11-25 | 2010-11-25 | High refractive index evaporation material lanthanum titanate mixture and preparation method thereof |
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|---|---|---|---|
| CN2010105589457A CN102062881B (en) | 2010-11-25 | 2010-11-25 | High refractive index evaporation material lanthanum titanate mixture and preparation method thereof |
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|---|---|
| CN102062881A CN102062881A (en) | 2011-05-18 |
| CN102062881B true CN102062881B (en) | 2012-07-04 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107226481B (en) * | 2017-06-26 | 2019-04-23 | 河北工业大学 | A kind of preparation method of the spherical lanthanium titanate of particle |
| CN109879308B (en) * | 2019-02-25 | 2022-10-11 | 江西师范大学 | Method for preparing lanthanum titanate |
Citations (6)
| 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 |
| CN1365956A (en) * | 2000-12-29 | 2002-08-28 | 默克专利股份有限公司 | Gaseous phase sedimentary material for producing high refractive index optical coating layer and production method of said gaseous phase sedimentary material |
| JP2002365590A (en) * | 2001-06-06 | 2002-12-18 | Tochigi Nikon Corp | Optical element, method of manufacturing optical element and optical isolator |
| DE10201492A1 (en) * | 2002-01-16 | 2003-07-31 | Fraunhofer Ges Forschung | Optical coating system for radiation-sensitive plastic substrates comprises a protective oxide layer with high absorbance at short wavelengths and optically-functional outer layers |
| CN101178440A (en) * | 2006-11-07 | 2008-05-14 | 北京有色金属研究总院 | LaTiO3 evaporation material for high refractivity optical film, method of producing the same and use |
| CN101200794A (en) * | 2007-07-09 | 2008-06-18 | 昆山光铭光电子元件有限公司 | Method for preparing premelting lanthanum titanate crystalloid steam plating material |
-
2010
- 2010-11-25 CN CN2010105589457A patent/CN102062881B/en active Active
Patent Citations (6)
| 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 |
| CN1365956A (en) * | 2000-12-29 | 2002-08-28 | 默克专利股份有限公司 | Gaseous phase sedimentary material for producing high refractive index optical coating layer and production method of said gaseous phase sedimentary material |
| JP2002365590A (en) * | 2001-06-06 | 2002-12-18 | Tochigi Nikon Corp | Optical element, method of manufacturing optical element and optical isolator |
| DE10201492A1 (en) * | 2002-01-16 | 2003-07-31 | Fraunhofer Ges Forschung | Optical coating system for radiation-sensitive plastic substrates comprises a protective oxide layer with high absorbance at short wavelengths and optically-functional outer layers |
| CN101178440A (en) * | 2006-11-07 | 2008-05-14 | 北京有色金属研究总院 | LaTiO3 evaporation material for high refractivity optical film, method of producing the same and use |
| CN101200794A (en) * | 2007-07-09 | 2008-06-18 | 昆山光铭光电子元件有限公司 | Method for preparing premelting lanthanum titanate crystalloid steam plating material |
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| CN102062881A (en) | 2011-05-18 |
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Address after: 350299 No. 169 Taiping lane, Lane Village, Changle City, Fujian Patentee after: FUZHOU ACETRON PHOTOELECTRIC MATERIALS CO., LTD. Address before: 350000, Taiping lane, Changle City, Fujian province Fuzhou City air city streets Qin Village No. 168 Patentee before: Fuzhou ACETRON Optoelectronic Materials Co., Ltd. |