CN101178440A - LaTiO3 evaporation material for high refractivity optical film, method of producing the same and use - Google Patents

LaTiO3 evaporation material for high refractivity optical film, method of producing the same and use Download PDF

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Publication number
CN101178440A
CN101178440A CNA2006101143510A CN200610114351A CN101178440A CN 101178440 A CN101178440 A CN 101178440A CN A2006101143510 A CNA2006101143510 A CN A2006101143510A CN 200610114351 A CN200610114351 A CN 200610114351A CN 101178440 A CN101178440 A CN 101178440A
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China
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evaporating materials
film
latio
high index
refraction optical
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CNA2006101143510A
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Inventor
张碧田
潘德明
王星明
段华英
储茂友
邓世斌
孙静
张明贤
龚述荣
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Beijing General Research Institute for Non Ferrous Metals
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Beijing General Research Institute for Non Ferrous Metals
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Abstract

The invention relates to a vaporizing material for a high refraction optics film, namely a compound with the chemical reaction of LaTiO3. The material is formed by single structure with no other doping. The density of the material is 5.2 to 5.9g/cm<3 > with good filling performance, taking Ti2O3 and La2O3, or TiO2, La2O3 and Ti as the material to be reacted under high temperature and vacuum state to produce TiO3. The LaTiO3 vaporizing material is used for producing the high refraction optics film which is a rigid medium film with good performance. The high refraction optics film is an antireflection coating of filming of a resin lens, a dichroic prism or a broad band. In the method of producing the high refraction optics film, the vaporizing material LaTiO3 is not changed in the vaporizing process and the vaporizing material LaTiO3 in crucible needs no update to keep stable refraction rate of the film. Multi high-refraction optics films are produced through once fusion and multi times of vaporization.

Description

High index of refraction optical thin film LaTiO 3Evaporating materials and its production and use
Technical field
The invention belongs to a kind of high index of refraction optical thin film LaTiO 3Evaporating materials and its production and use.
Background technology
High index of refraction optical thin film material is widely used in the design of various optical films, they are mainly used to be used the various antireflective films of preparation with low-index material or with middle refractive index, low-index material, 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.
In order further to widen the range of choice of material, satisfy the optical film designing requirement, various mixing coating materials are developed and are widely used in during optical thin film is coated with.Mix the application of coating materials in film and not only can obtain required refractive index, but also can improve the characteristic of rete and the evaporation characteristic of material.As the refractive index ratio zirconia height of zirconia tantalum mixing coating materials, overcome the zirconia refractive index along with thicknesses of layers increases and the deficiency of decline, its rete is compact and firm more.In zirconia, add the heterogeneity that yttria also can suppress film refractive index, improve the density of rete and the smooth finish of face, but in titanium dioxide, add the oxidation of compound accelerating oxidation titaniums such as zirconia, tantalum oxide, niobium oxide when evaporation, reduce rete and absorb.At TiO 2The middle La that adds 2O 3, Pr 6O 11Deng the mixing coating materials of making, this material can carry out evaporation when substrate is not heated, be applicable to the plated film of resin lens.
In recent years, resin lens was because it was in light weight, intensity is high, light transmission good, be used widely in the production of optical element and eyeglass, but substrate is thermo-labile, and being heated easily produces distortion.Common membraneous material needs just can be coated with the firm rete of compact structure under the condition that substrate is heated.By improving coating process and filming equipment, can obtain firmly fine and close rete and minimizing harmful effect, but will increase technology difficulty and equipment investment substrate.Therefore, the high-index material that can be used for resin substrate of seeking a kind of stable performance is one of content of developing material.
Summary of the invention
The object of the present invention is to provide a kind of high index of refraction optical thin film LaTiO 3Evaporating materials.This evaporating materials structure is single, and stable performance has higher transmittance near ultraviolet near infrared.
Another object of the present invention is to provide a kind of preparation high index of refraction optical thin film LaTiO 3The method of evaporating materials.
A further object of the present invention is to provide a kind of high index of refraction optical thin film LaTiO 3The purposes of evaporating materials.Made rete densification, firm, stable is fit to the design that various films are.
Also purpose of the present invention is to provide a kind of high index of refraction optical thin film LaTiO 3The method for preparing the high index of refraction optical thin film of evaporating materials.
For achieving the above object, the present invention takes following technical scheme: a kind of high index of refraction optical thin film evaporating materials, this material are that a kind of chemical formula is LaTiO 3Compound; Show that with XRD analysis this material is that single phase structure is formed, do not have other dephasign, it is stable that being formed with of single phase is beneficial to the material evaporation, and evaporate process is easy to control, and keeps thin-film refractive index stable; This density of material is 5.2~5.9g/cm 3, density is higher, and the material filling is good.This material can make things convenient for the coating process operation and improve the filming equipment production capacity.
Preparation high index of refraction optical thin film LaTiO 3The method of evaporating materials is with Ti 2O 3And La 2O 3Perhaps TiO 2, La 2O 3With Ti be raw material, under high temperature and vacuum state, carry out solid phase reaction, generate LaTiO 3
High index of refraction optical thin film LaTiO 3The purposes of evaporating materials, this evaporating materials is used to prepare the high index of refraction optical film, and this rete is the hard media coating of excellent performance.
High index of refraction optical thin film LaTiO of the present invention 3Evaporating materials can be widely used in the design of various optical films, they are mainly used to be used the various antireflective films of preparation with low-index material or with middle refractive index, low-index material, and these films mainly are used in the lens, prism, reflective mirror of optical instrument etc.In the design of optical film, high index of refraction optical thin film LaTiO of the present invention 3Refractive index was 1.95-2.15 when evaporating materials was 550nm at wavelength, can with in, low-index material be used the preparation various optical thin films.LaTiO of the present invention 3The prepared high index of refraction optical film of evaporating materials is the hard media coating of excellent performance, and said here hard media coating is for soft-medium (ZnS etc.) optical thin film.
Described high index of refraction optical film is the plated film of resin lens.
Described high index of refraction optical film is the anti-reflection film in colour splitting prism or broadband.
Use high index of refraction optical thin film LaTiO 3Evaporating materials prepares the method for high index of refraction optical thin film, with described LaTiO 3The crucible that evaporating materials is put into electron beam evaporation equipment carries out evaporation, preparation high index of refraction optical thin film, wherein, LaTiO in evaporation process 3The evaporating materials composition remains unchanged LaTiO in the crucible of electron beam evaporation equipment 3Evaporating materials need not upgrade and keep the refractive index of prepared film stable.
Use high index of refraction optical thin film LaTiO 3Evaporating materials prepares the method for high index of refraction optical thin film, with described LaTiO 3Evaporating materials is put into the crucible of electron beam evaporation equipment, carries out fritting earlier, is molten condition substantially after the fritting, after this once melts, can repeatedly evaporate, and prepares a plurality of high index of refraction optical thin films.
Advantage of the present invention is:
LaTiO 3Be a kind of high index of refraction evaporating materials of excellent performance, near infrared higher transmittance arranged near ultraviolet, fusing before this material evaporation, evaporation technology is controlled easily, can carry out evaporation when substrate is not heated, and is specially adapted to the plated film of resin lens.Its structure is single LaTiO 3Phase structure.About 1800 ℃ of this material melting point, not splash during fritting is a molten condition substantially after the fritting, it is stable that being formed with of single phase helps the material evaporation, evaporate process is easy to control, and material is formed and to be remained unchanged in evaporation process, and material can upgrade and keeps thin-film refractive index stable in the crucible.Density of material is determined as 5.2~5.9g/cm with drainage 3, density is higher, and the material filling is good, and once fusing can repeatedly be evaporated, and helps making things convenient for coating operation and improves the filming equipment production capacity.Rete roughness and firmness add at substrate does not have obvious difference when gentleness is not heated, rete is all fine and close, firm.LaTiO 3Can be applicable to the suitability for industrialized production of colour splitting prism and broad-band transparence-increased film as stable high-index material.
The preparation high index of refraction optical thin film LaTiO that the present invention developed 3Evaporating materials, structure is single, and stable performance has higher transmittance near ultraviolet near infrared, and rete densification, firm, stable is fit to the design that various films are.
Description of drawings
Fig. 1 is high index of refraction optical thin film LaTiO of the present invention 3The XRD figure of evaporating materials.
Embodiment
Embodiment 1: material preparation
With Ti 2O 3Fine powder and La 2O 3Fully mix by weight (3: 7), and with the abundant ground and mixed 4-6 of potpourri hour, and suppress granulation in a suitable manner, and at 1700 ℃, vacuum tightness: 2 * 10 -1Pa-8 * 10 -2Pa is incubated cooling after 3-8 hour.Prepare the Dark grey material, this density of material is about 5.3g/cm 3, about 1800 ℃ of fusing point.Made high index of refraction optical thin film LaTiO 3The XRD figure of evaporating materials shows that with XRD analysis this material is that single phase structure is formed, and does not exist other dephasign as shown in Figure 1.
Embodiment 2: material preparation
With TiO 2Fine powder, Ti powder and La 2O 3Fully mix by weight (70.3: 6.7: 23.0), and with the abundant ground and mixed 4-6 of potpourri hour, and suppress granulation in a suitable manner, and at 1700 ℃, vacuum tightness: 2 * 10 -1Pa-8 * 10 -2Pa is incubated cooling after 3-8 hour.Prepare the Dark grey material, this density of material is about 5.5g/cm 3, about 1800 ℃ of fusing point.
Embodiment 3: material is used
The plated film substrate is a quartz substrate, and deposited by electron beam evaporation equipment carries out evaporation, and vacuum tightness is 1.5 * 10 -4Torr, substrate temperature are 200 ℃, and evaporating temperature is about 2200 ℃, and evaporation rate is , made coatings is 2.11 in the refractive index of 550nm, rete is firm, at visible region light is not absorbed.
Embodiment 4: material is used
During experiment at first to the abundant fritting of material, the fritting of in the oxygen-free copper crucible of diameter of phi 30 * 15mm, feeding, prefusing temperature is about 2200-2400 ℃, not splash during fritting is a molten condition substantially after the fritting.Substrate is a quartz substrate, does not heat or substrate is heated and carried out evaporation under 150 ℃ of conditions, and vacuum tightness is 5~6 * 10 -3Pa.Made coatings is 2.10 in the refractive index of 550nm, and rete is firm.By test transmitted spectrum and reflectance spectrum, analyze and learn LaTiO 3The rete of material absorbs very little.

Claims (7)

1. high index of refraction optical thin film evaporating materials is characterized in that, this material is that a kind of chemical formula is LaTiO 3Compound, this material is that single phase structure is formed, and does not have other dephasign, this density of material is 5.2~5.9g/cm 3, the material filling is good.
2. prepare the method for the described evaporating materials of claim 1, it is characterized in that, with Ti 2O 3And La 2O 3Perhaps TiO 2, La 2O 3With Ti be raw material, under high temperature and vacuum state, carry out solid phase reaction, generate LaTiO 3
3. the purposes of the described evaporating materials of claim 1 is characterized in that, this LaTiO 3Evaporating materials is used to prepare the high index of refraction optical film, and this rete is the hard media coating of excellent performance.
4. the purposes of evaporating materials according to claim 3 is characterized in that, described high index of refraction optical film is the plated film of resin lens.
5. the purposes of evaporating materials according to claim 3 is characterized in that, described high index of refraction optical film is the anti-reflection film in colour splitting prism or broadband.
6. use the described evaporating materials of claim 1 to prepare the method for high index of refraction optical thin film, it is characterized in that, described LaTiO 3The crucible that evaporating materials is put into electron beam evaporation equipment carries out evaporation, preparation high index of refraction optical thin film, wherein, LaTiO in evaporation process 3The evaporating materials composition remains unchanged LaTiO in the crucible of electron beam evaporation equipment 3Evaporating materials need not upgrade and keep the refractive index of prepared film stable.
7. use the described evaporating materials of claim 1 to prepare the method for high index of refraction optical thin film, it is characterized in that, described LaTiO 3Evaporating materials is put into the crucible of electron beam evaporation equipment, carries out fritting earlier, is molten condition substantially after the fritting, after this once melts, can repeatedly evaporate, and prepares a plurality of high index of refraction optical thin films.
CNA2006101143510A 2006-11-07 2006-11-07 LaTiO3 evaporation material for high refractivity optical film, method of producing the same and use Pending CN101178440A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
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
CN107664781A (en) * 2017-08-30 2018-02-06 中国科学院上海技术物理研究所 A kind of controllable polarization-maintaining color separation film of face shape based on ion beam sputter depositing film
CN115142015A (en) * 2021-12-14 2022-10-04 常州瞻驰光电科技股份有限公司 High-absorption optical coating material and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
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
CN107664781A (en) * 2017-08-30 2018-02-06 中国科学院上海技术物理研究所 A kind of controllable polarization-maintaining color separation film of face shape based on ion beam sputter depositing film
CN115142015A (en) * 2021-12-14 2022-10-04 常州瞻驰光电科技股份有限公司 High-absorption optical coating material and preparation method thereof
CN115142015B (en) * 2021-12-14 2024-04-30 常州瞻驰光电科技股份有限公司 High-absorption optical coating material and preparation method thereof

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