CN113200566A - Pre-melted high-refractive-index optical coating material and preparation method and application thereof - Google Patents
Pre-melted high-refractive-index optical coating material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a pre-melted high-refractive-index optical coating material and a preparation method and application thereof, belonging to the field of optical thin film materials. The high-refractive-index optical coating material is praseodymium titanate with a chemical formula of Pr5Ti5O17(ii) a And the praseodymium titanate is TiO2、Pr6O11And Ti powder as raw material through solid phase synthesis reaction. The praseodymium titanate prepared by the preparation method provided by the invention keeps stable chemical composition in the evaporation process, can form a very flat evaporation surface in premelting, and is beneficial to process control in the film coating process. In addition, the optical film layer plated by the praseodymium titanate has higher transmittance in the near ultraviolet to near infrared bands, and meanwhile, the film layer is compact, firm and chemicalThe product has stable quality, and can be used as a high-quality high-refractive-index material for optical film system design and batch coating production.
Description
Technical Field
The invention relates to the technical field of optical thin film materials, and mainly relates to a pre-melted high-refractive-index optical coating material, and a preparation method and application thereof.
Background
In the optical coating material, the choice of high refractive index materials available for electron beam evaporation is very limited, and most of the high refractive index materials are oxides of titanium, zirconium, hafnium, tantalum and niobium, and their mixtures or mixtures with other metal oxides. In the technical field, the mixture coating can change the refractive index of a single oxide optical film layer, expand the selection range of materials for optical film system design, and improve the characteristics of the film such as stress and the like.
However, since the melting points and vapor pressures of the components in the materials of these mixtures are different, if the components are selected or the ratio is not proper, the ratio of the components may change during the evaporation process, which may affect the stability of the properties of the optical film and the consistency of the production lot.
Therefore, in order to solve the problems of unstable performance and poor consistency of production batches of the prepared optical thin film of the high refractive index material in the prior art, a new high refractive index material is urgently needed in the technical field.
Disclosure of Invention
The invention provides a novel high-refractive-index optical coating and a preparation method thereof, aiming at the problems of unstable performance, poor consistency of production batches and the like of the prepared optical film of the existing high-refractive-index material. The specific contents are as follows:
in a first aspect, the present invention provides a pre-melted high refractive index optical coating material, wherein the high refractive index optical coating material is praseodymium titanate with a chemical formula of Pr5Ti5O17；
Wherein the praseodymium titanate is TiO2、Pr6O11And Ti powder as raw material through solid phase synthesis reaction.
Preferably, the density of the high-refractive-index optical coating material is 5.3-5.5g/cm3The melting point of the material is 1900 ℃, and the refractive index at 500nm is 2.10.
In a second aspect, the present invention provides a method for preparing praseodymium titanate according to the first aspect, including:
with TiO2、Pr6O11And Ti powder as raw materials, and mechanically mixing the raw materials and the Ti powder according to a certain proportion to obtain uniformly mixed powder;
briquetting or granulating the powder to obtain blocks or granules;
carrying out solid-phase synthesis reaction on the block or the particle under high-temperature vacuum and melting to obtain a melting system;
cooling the molten system to room temperature and crushing under vacuum to obtain praseodymium titanate, wherein the chemical formula of the praseodymium titanate is Pr5Ti5O17。
Optionally, the ratio of each component in the raw materials is as follows: TiO 22Content 23-27 wt.%, Pr6O11The content is 68-72 wt.%, and the content of Ti powder is 2-6 wt.%. .
Preferably, the raw materials comprise the following components in proportion: TiO 22The content is 25-26 wt.%, Pr6O11The content is 70-72 wt.%, and the content of Ti powder is 2-5 wt.%.
Optionally, the time for mechanical mixing is 4-10 h; the pressure adopted by the briquetting or the granulation is 300-800N/cm2。
Preferably, the mechanical mixing time is 6-8 h; the pressure adopted by the briquetting or the granulation is 500-600N/cm2。
Optionally, the vacuum degree of the solid phase synthesis reaction is 10-1 × 10-3Pa; the reaction temperature of the solid-phase synthesis reaction is 1500-2200 ℃, and the reaction is carried outThe time is 3-20 h, and the temperature rising speed is 5-15 ℃/min.
Preferably, the vacuum degree of the solid phase synthesis reaction is 2X 10-1Pa～5×10-2Pa; the reaction temperature of the solid-phase synthesis reaction is 1700-2000 ℃, the reaction time is 8-12 h, and the heating rate is 7-12 ℃/min.
In a third aspect, the present invention provides an application of a pre-melted high refractive index optical coating material, wherein the high refractive index optical coating material of the first aspect is applied to the preparation of an optical coating.
The invention provides a pre-melted high-refractive-index optical coating material and a preparation method and application thereof. Wherein the high refractive index optical coating material is praseodymium titanate with a chemical formula of Pr5Ti5O17. Compared with the prior art, the high-refractive-index optical coating material provided by the invention is composed of a single compound, so that the problems of poor performance stability, poor production batch consistency and the like of an optical film in a mixture optical coating material are solved, and the problem of low refractive index of the optical film in the existing single-component compound is improved.
In addition, the optical coating material provided by the invention is a single compound, so that the stable chemical composition can be kept in the evaporation process, and a very flat evaporation surface can be formed in the pre-melting process, thereby being beneficial to the process control of the coating process. Meanwhile, the optical film coated by the praseodymium titanate has high transmittance in the near ultraviolet to near infrared bands, is compact and firm, has stable chemical properties, and can be used as a high-quality high-refractive-index material to be applied to optical film system design and batch coating production.
Compared with the prior art, the optical coating material provided by the invention at least has the following advantages:
1. the optical coating material provided by the invention is a single compound, avoids the problem of difficult control of the proportion of each component in the mixture, and is beneficial to keeping the stability of the components of the material in the evaporation process. In addition, in actual operation, when the material is charged for multiple times for evaporation, the stability of the evaporation process of the material and the consistent performance of the optical film can be kept.
2. Praseodymium titanate Pr5Ti5O17Is TiO2、Pr6O11And Ti powder as raw material, and preparing the pre-melting material through solid-phase synthesis reaction. Based on the characteristics of pre-melting, the gas release of the material during pre-melting is reduced, the pre-melting time of the material is shortened, and the use efficiency of the coating equipment is improved.
3. The material can form a very flat evaporation surface during premelting, which is beneficial to the process control of the material evaporation process and the homogeneous optical film layer is obtained.
4. The preparation method of the praseodymium titanate comprises the following steps: the praseodymium titanate is obtained by performing solid-phase synthesis and melting at high temperature under vacuum, crystallizing at vacuum state, and cooling to room temperature. The method has the characteristics of simple process flow, short period, low cost, environmental friendliness and the like, and is suitable for industrial production.
Drawings
FIG. 1 is a flow chart of a method for preparing a praseodymium titanate optical thin film molten material according to an embodiment of the present invention;
FIG. 2 is a view showing an appearance of a praseodymium titanate molten particle material prepared in example 1 of the present invention;
fig. 3 shows an XRD pattern of a praseodymium titanate molten particle material prepared in example 1 of the present invention;
FIG. 4 is a graph showing a transmittance spectrum of a film layer obtained by vapor deposition of a praseodymium titanate molten particle material prepared in example 1 of the present invention;
fig. 5 shows XRD patterns of praseodymium titanate molten particle material prepared in example 1 of the present invention, tested before and after evaporation;
fig. 6 shows an appearance of a praseodymium titanate melt prepared in example 2 of the present invention.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The specific experimental procedures or conditions not specified in the examples can be performed according to the procedures or conditions of the conventional experimental procedures described in the prior art in this field. The reagents and other instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
The invention is based on TiO2、Pr6O11And Ti powder is used as a raw material, and a new compound is formed by reaction through a solid-phase synthesis reaction by controlling the raw material proportion and the solid-phase reaction conditions, so that the defect of component change of a material in the evaporation process of a pure mixed material is overcome, and the stability of the material in the evaporation process and the consistency of the performance of a film are maintained.
The embodiment of the invention provides a pre-melted high-refractive-index optical coating material and a preparation method thereof. The method mainly comprises the following steps: by using TiO2、Pr6O11And Ti powder as raw material, mechanically mixing them uniformly according to a certain mixing ratio, briquetting, high-temp. vacuum solid-phase synthesizing and melting, vacuum crystallizing, cooling to room temp. to obtain new compound Pr5Ti5O17. The compound keeps stable chemical composition in the evaporation process, can form a very flat evaporation surface in premelting, and is beneficial to process control in the film coating process. The optical film coated by the material has higher transmittance in the near ultraviolet to near infrared wave bands, is compact and firm, has stable chemical properties, and can be used as a high-quality high-refractive-index material to be applied to optical film system design and batch coating production.
The embodiment of the invention specifically comprises the following contents:
in a first aspect, embodiments of the present invention provide a pre-melted high refractive index optical coating material, where the high refractive index optical coating material is praseodymium titanate with a chemical formula of Pr5Ti5O17. Wherein the praseodymium titanate is TiO2、Pr6O11And Ti powder as raw material through solid phase synthesis reaction.
In addition, the density of the high refractive index optical coating material provided by the embodiment is 5.3-5.5g/cm3The melting point of the material is 1900 ℃, and the refractive index at 500nm is 2.10.
Compared with the prior art, the high-refractive-index optical coating material provided by the invention is composed of a single compound, so that the problems of poor performance stability, poor production batch consistency and the like of an optical film in a mixture optical coating material are solved, and the problem of low refractive index of the optical film in the existing single-component compound is improved.
In addition, the optical coating material provided by the invention is a single compound, so that the stable chemical composition can be kept in the evaporation process, and a very flat evaporation surface can be formed in the pre-melting process, thereby being beneficial to the process control of the coating process. Meanwhile, the optical film coated by the praseodymium titanate has high transmittance in the near ultraviolet to near infrared bands, is compact and firm, has stable chemical properties, and can be used as a high-quality high-refractive-index material to be applied to optical film system design and batch coating production.
Compared with the prior art, the optical coating material provided by the invention at least has the following advantages:
1. the optical coating material provided by the invention is a single compound, avoids the problem of difficult control of the proportion of each component in the mixture, and is beneficial to keeping the stability of the components of the material in the evaporation process. In addition, in actual operation, when the material is charged for multiple times for evaporation, the stability of the evaporation process of the material and the consistent performance of the optical film can be kept.
2. Praseodymium titanate Pr5Ti5O17Is TiO2、Pr6O11And Ti powder as raw material, and preparing the pre-melting material through solid-phase synthesis reaction. Based on the characteristics of pre-melting, the gas release of the material during pre-melting is reduced, the pre-melting time of the material is shortened, and the use efficiency of the coating equipment is improved.
3. The material can form a very flat evaporation surface during premelting, which is beneficial to the process control of the material evaporation process and the homogeneous optical film layer is obtained.
In a second aspect, an embodiment of the present invention provides a method for preparing praseodymium titanate according to the first aspect, as shown in fig. 1, the method including:
s1-1, in TiO2、Pr6O11And Ti powder as raw materials, and mechanically mixing the raw materials and the Ti powder according to a certain proportion to obtain uniformly mixed powder.
In the present embodiment, the raw material ratio of the solid phase synthesis reaction is TiO2 23％～27％(wt.)，Pr6O1168-72% (wt.), and the balance Ti powder such as TiO2 26％(wt.)，Pr6O1170% (wt.), Ti 4% (wt.), preferably TiO225-26% (wt.) of Pr6O11The content is 70-72% (wt.), and the balance is Ti powder.
In specific implementation, the mechanical mixing mode can be a mixing mode such as stirring mixing, ball milling mixing and the like, the mixing time is 4-12 hours, and in order to ensure the mixing uniformity of the powder and improve the production efficiency, the preferable time is 6-10 hours.
S1-2, briquetting or granulating the powder to obtain blocks or granules.
In specific implementation, the mixed powder is at 300-800N/cm2The briquetting or the granulation can be carried out on an oil press, an isostatic press, a granulator and other equipment, the briquetting can increase the contact area between different component powders and is beneficial to the solid-phase reaction, and the preferable pressure is 400-600N/cm2。
In the implementation step, the powdery mixture is pressed into a blocky mixed material by an oil press, so that the problem that the powdery material is pumped away and blown away due to vacuumizing in the subsequent vacuum sintering process is avoided.
S1-3, carrying out solid phase synthesis reaction on the block or the particle under high temperature vacuum and melting to obtain a melting system.
In specific implementation, the obtained block or particle is subjected to high-temperature solid-phase synthesis reaction in a vacuum state, and the high-temperature solid-phase synthesis equipment can adopt high-temperature vacuum equipment such as an intermediate frequency furnace, a carbon tube furnace, a hot pressing furnace and the like, and adopts a hot pressing furnaceThe pressing and the solid phase synthesis can be carried out simultaneously without briquetting or pelleting; the solid phase synthesis vacuum degree is 10 Pa-1 × 10-3Pa; the preferred degree of vacuum is 2X 10-1Pa～5×10-2Pa. The solid-phase synthesis time is 3-20 h, and in order to ensure complete reaction and improve production efficiency, the synthesis time is preferably 8-12 h. The temperature rise speed of the solid-phase synthesis material is 5-15 ℃/min, and the temperature rise speed is preferably 5-12 ℃/min. The phase composition and the material density obtained at different synthesis temperatures have certain difference, the solid phase synthesis temperature is 1500-2200 ℃, and the preferable synthesis temperature is 1700-2100 ℃. When the temperature is lower than 1900 ℃, the synthesized material is a sintered material, and the synthesized material can form a molten state when the temperature exceeds 1900 ℃.
In the actual operation process, segmented heating can be carried out, and Pr is prepared at 1700-1900 ℃ firstly5Ti5O17Sintering the material and then raising the temperature to Pr5Ti5O17Melting the sintered material to obtain Pr5Ti5O17The material is melted.
Here, it should be noted that the method can be comprehensively considered according to actual needs and industrial factors, and then the method for preparing Pr is determined5Ti5O17Then, is made into Pr5Ti5O17Sintering the material to prepare Pr5Ti5O17The material is melted. In the present embodiment, this is not limited. The main purpose of the embodiment is to provide a single-component high-refractive-index optical coating material Pr5Ti5O17(ii) a Secondly, in order to ensure the optical stability of the film made of the material and reduce the problems of splashing and the like in the film-making process, Pr is prepared5Ti5O17In the process of (2), it is directly made into a molten material.
S1-4, cooling the molten system to room temperature and crushing under vacuum to obtain praseodymium titanate Pr5Ti5O17。
In specific implementation, after the reaction in the step S1-3 is finished, the generated material is cooled to room temperature in a vacuum state, and the praseodymium titanate Pr is obtained5Ti5O17And crushing the product into particles with preset particle size according to the requirement for later use in preparing the film.
The preparation method of the praseodymium titanate provided by the embodiment of the invention has the characteristics of simple process flow, short period, low cost, environmental friendliness and the like, and is suitable for industrial production.
Praseodymium titanate Pr prepared by the method provided by the invention5Ti5O17The material is a pre-melted material, i.e., a melting process has been performed prior to evaporation to produce the optical film. Therefore, the material has the characteristics of high density, small closed porosity, single phase and the like after condensation. Based on the characteristics, the material has the advantages of small gas emission, stable evaporation process, easy control, no change of material composition in the evaporation process, capability of keeping the refractive index of a film layer stable without updating the material in a coating crucible and the like when the material is used for preparing the optical film by evaporation.
In addition, because the melted material has high density and good filling property, the praseodymium titanate provided by the embodiment of the invention can be evaporated for many times after being melted once, and the efficiency of the coating equipment is improved.
In addition, since the material is deposited on the substrate in a high-temperature environment when the deposition is performed by the electron beam evaporation apparatus, the material ejected from the electron beam evaporation apparatus is in a molten state. The existing optical coating material is granular sintering material, and for the sintering material, because the sintering granules are not molten material obtained after melting, on one hand, when the sintering granules are converted into a molten state in electron beam evaporation equipment, the problems of incomplete reaction, material spraying, unstable physicochemical properties and the like exist, and on the other hand, after the optical film is prepared, because the sintering material is not single-phase material and has impurity phase, the prepared optical film has the problems of unstable refractive index, incompactness and insecurity of the film layer, unstable chemical properties and the like. The praseodymium titanate provided by the embodiment of the invention is a molten material, so that the process of converting sintered particles into a molten state does not exist in evaporation equipment, and the problems of incomplete reaction, material spraying, unstable physical and chemical properties and the like of the existing optical coating material are solved. In addition, the praseodymium titanate provided by the embodiment of the invention is a single-phase material and has no impurity phase, so that the praseodymium titanate provided by the embodiment of the invention can avoid the problems of the existing optical coating material, such as the phenomena of slip, vapor deposition and splashing, unstable chemical performance of the obtained film, insecure film layer and the like.
In the preparation method provided by the embodiment of the invention, the selected TiO2、Pr6O11And the Ti powder has the characteristic of stable material performance, so that the praseodymium titanate is not easy to change in quality in the process of preparing the praseodymium titanate, and the physical and chemical properties of the praseodymium titanate are stable while the praseodymium titanate is smoothly generated.
In addition, in the preparation method provided by the embodiment of the invention, the praseodymium titanate molten material is prepared by utilizing a solid-phase melting reaction, and the preparation method has the advantages of simple process flow, short period, relatively low cost and easiness in industrial batch production. Meanwhile, the selected reaction raw material TiO2、Pr6O11And Ti powder, in the process of preparing the praseodymium titanate molten material, carbon dioxide and moisture in the air can not be absorbed, therefore, the preparation method provided by the invention, on one hand, avoids the generation of impurities or impure phases in the praseodymium titanate molten material, and ensures the chemical stability of the optical film prepared from the praseodymium titanate molten material, and on the other hand, the preparation method is easy for industrialized mass production and has wide industrialized application prospect.
In a third aspect, the present invention provides an application of a pre-melted optical coating material with a high refractive index, wherein the optical coating material with a high refractive index according to the first aspect is applied to the preparation of optical coatings in optical elements, mobile phone shells or touch screens. The specific implementation content is as follows:
firstly, fully premelting praseodymium titanate molten material, wherein the specific premelting method comprises the following steps: the praseodymium titanate molten material is placed in an oxygen-free copper crucible with the diameter of 30 multiplied by 15mm for pre-melting, the pre-melting temperature is 2200 ℃, and the praseodymium titanate in a molten state is obtained.
Then, coating was performed based on the premelted praseodymium titanate. The substrate used for coating isThe quartz substrate is evaporated by electron beam evaporation equipment with vacuum degree of 1.5 × 10-4torr, substrate temperature of 100 deg.C, evaporation temperature of about 2200 deg.C, evaporation rate of 3A/s. Coating is performed based on these evaporation conditions to obtain a praseodymium titanate thin film layer.
In the embodiment of the invention, the praseodymium titanate molten material prepared by the preparation method provided by the embodiment of the invention is a single-phase material, and no other impurity phase and/or impurity exists, so that the optical film prepared by the material has the advantages of compact and firm film layer, good chemical stability and the like, and the refractive index is stable.
In order to make the technical personnel in the field understand the invention better, the pre-melted high refractive index optical coating material provided by the invention and the preparation method and application thereof are illustrated by specific examples.
Example 1:
TiO is proportioned according to raw materials2 26％(wt.)，Pr6O1171% (wt.) and 2.5% (wt.) of Ti are accurately weighed, a stirring mixer is adopted for mechanical mixing for 8 hours, and the mixed powder is processed at 400N/cm by an oil press2Briquetting and charging under the pressure of (1), heating the hearth at a speed of 5 ℃/min under a vacuum state, at a temperature of 2000 ℃ and a vacuum degree of 2 x 10-1The solid phase synthesis reaction is carried out for 8h under the condition of Pa, and the reaction product is cooled to room temperature under the vacuum state. The material prepared by this method was a black molten material (appearance pattern is shown in FIG. 2, density of the material was 5.4g/cm as measured by the drainage method3。
Fig. 3 shows an XRD pattern of a praseodymium titanate molten particle material prepared in example 1 of the present invention. As can be seen from FIG. 3, the praseodymium titanate obtained by the method has a single-phase structure, and the structure is similar to that of Pr5Ti5O17The structures of the two are consistent.
When in use, the material is fully pre-melted firstly, the material is filled in a water-cooling oxygen-free copper crucible for pre-melting, the pre-melting temperature is 2200 ℃, the material is not splashed in the pre-melting process, and the surface of the material is in a molten state after pre-melting. The substrate for coating is quartz substrate, and the evaporation of material is carried out by electron beam evaporation coating equipment with vacuum degree of 1.6 × 10-2Pa, the substrate temperature is 80 ℃, the evaporation temperature is about 2400 ℃,evaporation rate of
Fig. 4 is a transmittance spectrum of a film layer infrared absorption spectrum obtained after evaporation of a praseodymium titanate molten particle material prepared in example 1 of the present invention. As can be seen from FIG. 4, the refractive index of the film layer is 2.10 at 500nm, the film layer is firm and compact, and the absorption in the near ultraviolet to near infrared band is small.
Fig. 5 shows XRD patterns of the praseodymium titanate molten particle material prepared in example 1 of the present invention, which were measured before and after evaporation. As can be seen from fig. 5, the phase structures of the praseodymium titanate molten particle material before and after evaporation are consistent, which indicates that the structure of the material is not changed during the evaporation process, and the chemical properties of the material are stable.
The adhesion of the film was rated 0 using a 3M tape using a cross-hatch test.
Example 2:
TiO is proportioned according to raw materials2 25％(wt.)，Pr6O11Weighing 72% (wt.) and 3% (wt.) Ti accurately, mechanically mixing for 8h by using a stirring mixer, and mixing the powder at 400N/cm by using an oil press2Briquetting and charging under vacuum condition, heating furnace hearth at 5 deg.C/min, 1900 deg.C and 2 × 10 vacuum degree-1The solid phase synthesis reaction is carried out for 8h under the condition of Pa, and the reaction product is cooled to room temperature under the vacuum state. The material prepared by this method was a black molten material (appearance pattern is shown in FIG. 6), and the density of the material was measured by the drainage method to be 5.4g/cm3。
When in use, the material is fully pre-melted firstly, the material is filled in a water-cooling oxygen-free copper crucible for pre-melting, the pre-melting temperature is 2200 ℃, the material is not splashed in the pre-melting process, and the surface of the material is in a molten state after pre-melting. The substrate for coating is quartz substrate, and the evaporation of material is carried out by electron beam evaporation coating equipment with vacuum degree of 1.6 × 10-2Pa, substrate temperature of 80 deg.C, evaporation temperature of 2400 deg.C, and evaporation rate of
The refractive index of the film coating film layer at 500nm is 2.10, the film layer is firm and compactThe absorption in the near ultraviolet to near infrared band was small (the infrared absorption spectrum was the same as that of the film layer obtained in example 1 and is not repeated in this example). The adhesion of the film was still rated 0 using a 3M tape with a cross-hatch test.
Example 3:
TiO is proportioned according to raw materials2 25％(wt.)，Pr6O11Weighing 72% (wt.) and 3% (wt.) Ti accurately, mechanically mixing for 6h by using a stirring mixer, and mixing the powder at 400N/cm by using an oil press2Briquetting and charging under the pressure of (1), heating the hearth at a speed of 5 ℃/min under a vacuum state, at a temperature of 1800 ℃ and a vacuum degree of 2 x 10-1The solid phase synthesis reaction is carried out for 6h under the condition of Pa, and the reaction product is cooled to room temperature under the vacuum state. The material prepared by the method is dark gray material, and the density of the material is 5.1g/cm by a drainage method3。
When in use, the material is fully pre-melted firstly, the material is filled in a water-cooling oxygen-free copper crucible for pre-melting, the pre-melting temperature is 2200 ℃, the material is not splashed in the pre-melting process, and the surface of the material is in a molten state after pre-melting. The substrate for coating is quartz substrate, and the evaporation of material is carried out by electron beam evaporation coating equipment with vacuum degree of 1.6 × 10-2Pa, substrate temperature of 80 deg.C, evaporation temperature of 2400 deg.C, and evaporation rate of
The refractive index of the film coating film layer at 500nm is 2.10, the film layer is firm and compact, and the absorption in the near ultraviolet to near infrared wave band is small. (the infrared absorption spectrum is the same as that of the film layer obtained in example 1 and is not repeated in this example). The adhesion of the film was still rated 0 using a 3M tape with a cross-hatch test.
It should be noted that the steps and methods in the embodiments of the present application are not limited to the corresponding embodiments, and the details of the operations and the cautions of the embodiments are all corresponding to each other.
The applicant states that the present invention is illustrated by the detailed process flow of the present invention through the above examples, but the present invention is not limited to the above detailed process flow, that is, it does not mean that the present invention must rely on the above detailed process flow to be implemented. It will be understood by those skilled in the art that any simple modification, equivalent substitution of each raw material and addition of auxiliary components, selection of specific modes and the like, of the product of the present invention falls within the scope and disclosure of the present invention.
For simplicity of explanation, the method embodiments are described as a series of acts or combinations, but those skilled in the art will appreciate that the present invention is not limited by the order of acts, as some steps may occur in other orders or concurrently in accordance with the invention. Further, those skilled in the art will appreciate that the embodiments described in the specification are preferred embodiments and that the acts and elements referred to are not necessarily required to practice the invention.
The pre-melted high refractive index optical coating material provided by the invention, the preparation method and the application thereof are described in detail, the principle and the implementation mode of the invention are explained by applying specific examples, and the description of the examples is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. A pre-melted high-refractive-index optical coating material is characterized in that the high-refractive-index optical coating material is praseodymium titanate with a chemical formula of Pr5Ti5O17；
Wherein the praseodymium titanate is TiO2、Pr6O11And Ti powder as raw material through solid phase synthesis reaction.
2. The high refractive index optical coating material of claim 1, wherein the density of the high refractive index optical coating material is 5.3-5.5g/cm3Material melting point of 190The refractive index at 0 ℃ at 500nm is 2.10.
3. A method for preparing the praseodymium titanate of claim 1 or 2, characterized in that the method comprises:
with TiO2、Pr6O11And Ti powder as raw materials, and mechanically mixing the raw materials and the Ti powder according to a certain proportion to obtain uniformly mixed powder;
briquetting or granulating the powder to obtain blocks or granules;
carrying out solid-phase synthesis reaction on the block or the particle under high-temperature vacuum and melting to obtain a melting system;
cooling the molten system to room temperature and crushing under vacuum to obtain praseodymium titanate, wherein the chemical formula of the praseodymium titanate is Pr5Ti5O17。
4. The method according to claim 3, wherein the raw materials comprise the following components in parts by weight: TiO 22Content 23-27 wt.%, Pr6O11The content is 68-72 wt.%, and the content of Ti powder is 2-6 wt.%.
5. The method according to claim 3, wherein the raw materials comprise the following components in parts by weight: TiO 22The content is 25-26 wt.%, Pr6O11The content is 70-72 wt.%, and the content of Ti powder is 2-5 wt.%.
6. The method according to claim 3, wherein the time for mechanical mixing is 4-10 hours; the pressure adopted by the briquetting or the granulation is 300-800N/cm2。
7. The method according to claim 3, wherein the time for mechanical mixing is 6-8 h; the pressure adopted by the briquetting or the granulation is 500-600N/cm2。
8. The method of claim 3, wherein the step of removing the metal oxide layer is performed by a chemical vapor deposition methodThe vacuum degree of the solid phase synthesis reaction is 10-1 × 10- 3Pa; the reaction temperature of the solid-phase synthesis reaction is 1500-2200 ℃, the reaction time is 3-20 h, and the temperature rise speed is 5-15 ℃/min.
9. The method of claim 3, wherein the degree of vacuum of the solid phase synthesis reaction is 2X 10-1Pa～5×10-2Pa; the reaction temperature of the solid-phase synthesis reaction is 1700-2000 ℃, the reaction time is 8-12 h, and the heating rate is 7-12 ℃/min.
10. Use of a pre-melted optical coating material with a high refractive index, wherein the optical coating material with a high refractive index according to claim 1 or 2 is used for preparing an optical coating.
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