CN100497721C - Preprocessed method of optical coating materials - Google Patents
Preprocessed method of optical coating materials Download PDFInfo
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- CN100497721C CN100497721C CNB2005101092694A CN200510109269A CN100497721C CN 100497721 C CN100497721 C CN 100497721C CN B2005101092694 A CNB2005101092694 A CN B2005101092694A CN 200510109269 A CN200510109269 A CN 200510109269A CN 100497721 C CN100497721 C CN 100497721C
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Abstract
The invention discloses a pretreated optical coating material and its pretreated methods. The methods includes: (1) selecting the optical coating powder, (2) preparing simple blank at a temperature of 700-1400DEG C, pressure of 10-40Mpa, (3) sintering in a high-temperature sintering furnace at 900-1800DEG C for 2-4h for the preparation bodyware; (4)processing and forming the bodyware strictly in accordance with coater crucible size, (5) degassing in the reduction furnace, at a temperature of 1000-1700DEG C, for 2-6hours to obtain the pretreated optical coating materials. The TiO2 pretreated optical coating materials has a relative density of 99%, oxygen content of 39.8%, oxygen loss rate of 6%, by fitting its stoichiometric formula, its molecular formula is TiO1.979. Pretreated optical coating material has the following characteristics: 1) high pyknosis with relative density over 90%, close to the theoretical density; 2) losing some lattice oxygen according to high refractive index optical oxide coating materials.
Description
Technical field
The present invention relates to a kind of pretreated optical filming material and pretreatment process thereof.
Background technology
When adopting electron gun evaporation technology plated film, Coating Materials is carried out the premelt of certain hour under certain power with electron beam gun before plated film begins, material is through fusing wholly or in part behind the beam bombardment.The result that premelt is handled makes the material densification on the one hand, and discharges the gas that is mingled with, and material outgassing produces splash when avoiding plated film; On the other hand, concerning the oxide compound high-index material, also lose a small amount of lattice oxygen.Concerning most of oxide optical Coating Materials, the oxygen loss in advance of material makes the easier control of coating process process.
Ordinary electronic rifle evaporation coating all will carry out abundant fritting to material before the evaporation beginning.But several problems are arranged generally in the operation: during 1) with particle or small pieces Coating Materials, the whole crucible of filling fully begins plated film after the pre-treatment earlier, intermittently repeatedly feeds in raw material, repeats plated film according to service condition then; 2) particle or patch material loadings are limited.Like this because all repeat to vacuumize before the plated film of each reinforced back, preprocessing process, expended the plenty of time; In addition particularly for accurate film system is big produce for because each periodical operation all needs to readjust coating process, so film is repeated bad.
In the last few years, for improving the performance of film, increasing electron gun evaporation equipment configuration ion source, in coating process, sedimentary film is carried out ion beam bombardment, make the compactness of film be improved, the bonding force of rete strengthens, as use the oxonium ion source, can also be to film delivery of supplemental oxygen ion.The Assisted by Ion Beam electron gun evaporation obtains commercial application in the production that some extensive accurate films are.The plated film of the multi-coated interference membrane filtration mating plate of using as DWDM is exactly to produce in this way.
Summary of the invention
The pretreated optical filming material that the purpose of this invention is to provide a kind of high compactionization.
Another object of the present invention provides a kind of pretreatment process of pretreated optical filming material, can carry out particular procedure so that this material loses the part lattice oxygen to the high refractive index oxide optical filming material.
Originally for achieving the above object, the present invention takes following technical scheme:
A kind of pretreated optical filming material is characterized in that: this pretreated optical filming material is any one in the following material:
TiO
2Pretreated optical filming material, its relative density reaches 99%, and oxygen level is 39.8%, and oxygen loss rate is 6%, is TiO by its molecular formula of stoichiometry match
1.979
Ta
2O
5Pretreated optical filming material, its relative density reaches 96%, oxygen level 17.84%, oxygen loss rate 1.5% is Ta by its molecular formula of stoichiometry match
2O
4.91
The pretreated optical filming material of ZnO, its relative density reaches 98%;
Ti
2O
3Pretreated optical filming material, its relative density reaches 99%, oxygen level 33.24%, oxygen loss rate 4.51% is Ti by its molecular formula of stoichiometry match
2O
2.988
Ti
3O
5Pretreated optical filming material, its relative density reaches 99%, oxygen level 35.53%, oxygen loss rate 6.8% is Ti by its molecular formula of stoichiometry match
3O
4.950
The pretreatment process of above-mentioned optical filming material has following three kinds:
The pretreatment process of first kind of optical filming material, this method comprises the steps:
(1), selects the material powder of optical filming material for use;
(2), be 700～1400 ℃ with the above-mentioned raw materials powder in temperature, pressure is that vacuum hot pressing formation prepares biscuit under 10～40Mpa condition;
(3) with biscuit sintering in high temperature sintering furnace of above-mentioned preparation, the constant temperature sintering is 2～4 hours under 900～1800 ℃ of conditions of sintering temperature, the preparation base substrate;
(4), with the dimensioned moulding of base substrate in strict accordance with the coating equipment crucible;
(5), in the reducing atmosphere stove, be under 1000～1700 ℃ of conditions in temperature, above-mentioned base substrate is outgased handled 2～6 hours, be pretreated optical filming material through resulting material after the above-mentioned processing.
The pretreatment process of first kind of optical filming material can prepare titanium dioxide (TiO
2) pretreated optical filming material, tantalum pentoxide (Ta
2O
5) pretreated optical filming material.
In the pretreatment process of first kind of above-mentioned optical filming material, in described step (1), the purity of described material powder is 99.9%～99.99%; Its granularity D
50Be 1-50 μ m.
In the pretreatment process of first kind of above-mentioned optical filming material, in the pretreatment process of first kind of above-mentioned optical filming material, in described step (1), the granularity D of described material powder
50Be 1-10 μ m.
In the pretreatment process of first kind of above-mentioned optical filming material, in described step (2), the biscuit relative density is controlled at 80%～99%.
In the pretreatment process of first kind of above-mentioned optical filming material, in described step (4), with the dimensioned moulding of base substrate in strict accordance with the coating equipment crucible, base substrate is as follows according to the detailed process of the dimensioned moulding of crucible: the base substrate that high temperature sintering is handled utilizes the dimensioned moulding in strict accordance with crucible of surface grinding machine, cylindrical grinder, and dimensional precision is controlled at below the 0.1mm.
In the pretreatment process of first kind of above-mentioned optical filming material, in described step (5), the reducing atmosphere in the described reducing atmosphere stove is H
2, or H
2And N
2Gas mixture, perhaps use other reducing atmosphere source, the processing that outgases of reducing atmosphere stove promptly, after the dimensioned moulding of base substrate according to crucible, is cleaned, is put into after the oven dry in the processing that outgases in the reducing atmosphere stove of described base substrate.
The pretreatment process of second kind of optical filming material, this method comprises the steps:
(1), selects the material powder of optical filming material for use;
(2), be 700～1400 ℃ with the above-mentioned raw materials powder in temperature, pressure is that vacuum hot pressing formation prepares biscuit under 10～40Mpa condition;
(3) with biscuit sintering in high temperature sintering furnace of above-mentioned preparation, the constant temperature sintering is 2～4 hours under 900～1800 ℃ of conditions of sintering temperature, the preparation base substrate;
(4), with the dimensioned moulding of base substrate in strict accordance with the coating equipment crucible, be pretreated optical filming material.
The pretreatment process of the pretreatment process of second kind of optical filming material and first kind of optical filming material is, the processing that do not outgas of the pretreatment process of second kind of optical filming material can prepare the pretreated optical filming material of zinc oxide (ZnO).
In the pretreatment process of second kind of above-mentioned optical filming material, in described step (1), the purity of described material powder is 99.9%～99.99%; Its granularity D
50Be 1-50 μ m.
In the pretreatment process of second kind of above-mentioned optical filming material, in described step (1), the granularity D of described material powder
50Be 1-10 μ m.
In the pretreatment process of second kind of above-mentioned optical filming material, in described step (2), the biscuit relative density is controlled at 80%～99%.
In the pretreatment process of second kind of above-mentioned optical filming material, in described step (4), with the dimensioned moulding of base substrate in strict accordance with the coating equipment crucible, base substrate is as follows according to the detailed process of the dimensioned moulding of crucible: the base substrate that high temperature sintering is handled utilizes the dimensioned moulding in strict accordance with crucible of surface grinding machine, cylindrical grinder, and dimensional precision is controlled at below the 0.1mm.
The pretreatment process of the third optical filming material, this method comprises the steps:
(1), selects the material powder of optical filming material for use;
(2), be 700～1400 ℃ with the above-mentioned raw materials powder in temperature, pressure is that vacuum hot pressing formation prepares biscuit under 10～40Mpa condition;
(3), with the dimensioned moulding of biscuit in strict accordance with the coating equipment crucible, be pretreated optical filming material.
The pretreatment process of the pretreatment process of the third optical filming material and first kind of optical filming material is that the pretreatment process of the third optical filming material i.e. not degassing processing, does not have high temperature sintering again, can prepare titanium sesquioxide (Ti
2O
3) pretreated optical filming material, five oxidation Tritanium/Trititanium (Ti
3O
5) pretreated optical filming material.
In the pretreatment process of the third above-mentioned optical filming material, in described step (1), the purity of described material powder is 99.9%～99.99%; Its granularity D
50Be 1-50 μ m.
In the pretreatment process of the third above-mentioned optical filming material, in described step (1), the granularity D of described material powder
50Be 1-10 μ m.
In the pretreatment process of the third above-mentioned optical filming material, in described step (2), the biscuit relative density is controlled at 80%～99%.
In the pretreatment process of the third above-mentioned optical filming material, in described step (3), with the dimensioned moulding of biscuit in strict accordance with the coating equipment crucible, biscuit is as follows according to the detailed process of the dimensioned moulding of crucible: the biscuit of vacuum hot pressing formation preparation is utilized the dimensioned moulding in strict accordance with crucible of surface grinding machine, cylindrical grinder, and dimensional precision is controlled at below the 0.1mm.
Wherein, in above-mentioned three kinds of methods, the time of material powder vacuum hot pressing formation is 30-80 minute in described step (2), is preferably 40 minutes.
Advantage of the present invention is:
Invention is at ordinary electronic rifle evaporation shortcoming, and special coupled ion bundle assistant depositing equipment has proposed pretreated optical filming material of a kind of new optical filming material----and pretreatment process thereof.In above-mentioned three kinds of methods of the present invention, total technological step is to adopt vacuum hot pressing formation to prepare biscuit.Pretreated optical filming material has following characteristics: 1) high compactionization, relative density reach more than 90%, and some is near the theoretical density of material; 2), carry out particular procedure by processing method of the present invention and lose the part lattice oxygen for the high refractive index oxide optical filming material.This materials similar is handled in having passed through the premelt before the vacuum plating.
Description of drawings
Used crucible scantlings of the structure synoptic diagram when Fig. 1 is the electron gun evaporation plated film
Embodiment
The step of preparation process of pretreated optical filming material of the present invention is as follows:
1) select the suitable feedstock powder for use, general purity is 99.9%～99.99%; Granularity D
50The powder that is preferably 1-10 μ m for 1-50 μ m is a raw material.
2) be 700～1400 ℃ in temperature, pressure is that vacuum hot pressing formation prepares biscuit under 10～40Mpa condition.
3) the biscuit relative density is controlled at 80%～95%.
4) with biscuit high temperature sintering in high temperature sintering furnace of above-mentioned preparation, the constant temperature sintering is 2～4 hours under 900～1800 ℃ of conditions of sintering temperature.
5) base substrate that above-mentioned high temperature sintering is handled utilizes the dimensioned moulding in strict accordance with crucible of surface grinding machine, cylindrical grinder, and dimensional precision is controlled at below the 0.1mm; The scantlings of the structure of crucible as shown in Figure 1, crucible used when being the electron gun evaporation plated film shown in Figure 1.Pretreated optical filming material of the present invention is a kind of material in strict accordance with this crucible size making, energy completely filled crucible.Wherein, TD is the upper edge diameter of crucible; H is the height of crucible; θ is the pitch angle of crucible wall; C is the crucible wall thickness.Therefore, the profile of pretreated optical filming material is round table-like, and its upper edge diameter is: Td=TD-2C/cos θ; Height h=H-C; The pitch angle is θ.
6) material that processes is cleaned, dries.
7) in the reducing atmosphere stove to the processing that outgases of above-mentioned base substrate.Reducing atmosphere can be H
2, or H
2And N
2Gas mixture or other reducing atmosphere source be 1000～1700 ℃ in temperature and handled 2～6 hours down.
8) be pretreated optical filming material through resulting material after the above-mentioned processing.
Pretreated optical filming material preparation process of the present invention is different from the premelt process of vacuum plating, and the material that the present invention is prepared is also not all really melted.The salient features of material handles by metallurgical technology rather than fusing realizes.At the difference of material, select for use the processing parameter among the preparation technology also different.
Embodiment 1, titanium dioxide (TiO
2) preparation of pretreated optical filming material
1) selects that purity is 99.99%, D for use
50TiO for 3-5 μ m
2Powder is a raw material;
2) be 1000 ℃ in temperature, pressure is that vacuum hot pressing formation prepares biscuit under the 20Mpa condition;
3) the biscuit relative density is controlled at more than 90%;
4) with biscuit high temperature sintering in high temperature sintering furnace of above-mentioned preparation, 1600 ℃ of following constant temperature sintering 4 hours;
5) base substrate that above-mentioned high temperature sintering is handled utilizes the dimensioned moulding in strict accordance with crucible of surface grinding machine, cylindrical grinder, and dimensional precision is controlled at below the 0.1mm;
6) material that processes is cleaned, dries;
7) in the reducing atmosphere stove to the processing that outgases of above-mentioned base substrate.Reducing atmosphere is selected H for use
2And N
2Gas mixture (H
2/ N
2=1: 100 volume ratios), being 1400 ℃ in temperature under the pressure 1atm handled 5 hours down.
8) prepared TiO
2The optical filming material relative density reaches 99%, and adopting the electron probe microanalysis oxygen level is 39.8%, and oxygen loss rate is 6%, but is TiO by stoichiometry match molecular formula
1.979
9) be pre-treatment TiO through resulting material after the above-mentioned processing
2Optical filming material
Embodiment 2, tantalum pentoxide (Ta
2O
5) pretreated optical filming material
1) selects that purity is 99.99%, D for use
50Ta for 5-10 μ m
2O
5Powder is a raw material;
2) be 1400 ℃ in temperature, pressure is that vacuum hot pressing formation prepares biscuit under the 23Mpa condition;
3) the biscuit relative density is controlled at more than 90%;
4) with biscuit high temperature sintering in high temperature sintering furnace of above-mentioned preparation, 1600 ℃ of following constant temperature sintering 4 hours;
5) base substrate that above-mentioned high temperature sintering is handled utilizes the dimensioned moulding in strict accordance with crucible of surface grinding machine, cylindrical grinder, and dimensional precision is controlled at below the 0.1mm;
6) material that processes is cleaned, dries;
7) in the reducing atmosphere stove to the processing that outgases of above-mentioned base substrate.Reducing atmosphere is selected H for use
2And N
2Gas mixture (H
2/ N
2=1: 100 volume ratios), being 1400 ℃ in temperature under the pressure 1atm handled 5 hours down.
8) prepared Ta
2O
5The optical filming material relative density reaches 96%, adopt electron probe microanalysis oxygen level 17.84%, but oxygen loss rate 1.5% is Ta by stoichiometry match molecular formula
2O
4.91
9) be pre-treatment Ta through resulting material after the above-mentioned processing
2O
5Optical filming material
The pretreated optical filming material of embodiment 3 zinc oxide (ZnO)
1) selects that purity is 99.99%, D for use
50For the ZnO powder of 3-5 μ m is a raw material;
2) be 900 ℃ in temperature, pressure is that vacuum hot pressing formation prepares biscuit under the 15Mpa condition;
3) the biscuit relative density is controlled at more than 90%;
4) with biscuit high temperature sintering in high temperature sintering furnace of above-mentioned preparation, 1100～1650 ℃ of following constant temperature sintering 4 hours;
5) above-mentioned biscuit is utilized the dimensioned moulding in strict accordance with crucible of surface grinding machine, cylindrical grinder, dimensional precision is controlled at below the 0.1mm;
6) material that processes is cleaned, dries;
7) because ZnO material film plating technology is controlled easily, do not need oxygen loss processing in advance;
8) be pre-treatment ZnO optical filming material through resulting material after the above-mentioned processing.
Embodiment 4 titanium sesquioxide (Ti
2O
3) preparation of pretreated optical filming material
1) selects that purity is 99.99%, D for use
50TiO for 3-5 μ m
2Powder and purity are 99.9%, D
50For the metal Ti powder of 30-50 μ m is a raw material;
2) according to the ratio that contains Ti powder 17.8 weight % with TiO
2The two mixed of powder and Ti powder was mixed 4 hours in the dry type mixer;
3) be 1000 ℃ in temperature, pressure is that vacuum hot pressing formation prepares biscuit under the 20Mpa;
4) the biscuit relative density is controlled at more than 98%;
5) above-mentioned vacuum hot pressing formation is prepared biscuit and utilize the dimensioned moulding in strict accordance with crucible of surface grinding machine, cylindrical grinder, dimensional precision is controlled at below the 0.1mm;
6) material that processes is cleaned, dries;
7) prepared Ti
2O
3The optical filming material relative density reaches 99%, and adopting the electron probe microanalysis oxygen level is 33.24%, same TiO
2Comparing the oxygen loss amount is 6.8%, but is Ti by stoichiometry match molecular formula
2O
2.988
8) be pre-treatment Ti through resulting material after the above-mentioned processing
2O
3Optical filming material
Embodiment 5 five oxidation Tritanium/Trititanium (Ti
3O
5) preparation of pretreated optical filming material
1) selects that purity is 99.99%, D for use
50TiO for 3-5 μ m
2Powder and purity are 99.9%, D
50For the metal Ti powder of 30-50 μ m is a raw material;
2) according to the ratio that contains Ti powder 11.8 weight % with TiO
2The two mixed of powder and Ti powder was mixed 4 hours in the dry type mixer;
3) be 1000 ℃ in temperature, pressure is that vacuum hot pressing formation prepares biscuit under the 20Mpa;
4) the biscuit relative density is controlled at more than 98%;
5) above-mentioned vacuum hot pressing formation is prepared biscuit and utilize the dimensioned moulding in strict accordance with crucible of surface grinding machine, cylindrical grinder, dimensional precision is controlled at below the 0.1mm;
6) material that processes is cleaned, dries;
7) prepared Ti
3O
5The optical filming material relative density reaches 99%, and adopting the electron probe microanalysis oxygen level is 35.53%, same TiO
2Comparing the oxygen loss amount is 4.51%, but is Ti by stoichiometry match molecular formula
3O
4.950
8) be pre-treatment Ti through resulting material after the above-mentioned processing
2O
3Optical filming material.
Embodiment 6 adopts the prepared pre-treatment TiO of embodiment 1
2The plated film experiment of optical filming material
The equipment that is adopted has: (1) coating equipment: the Optorun OTSC-1300 that has Assisted by Ion Beam; (2) ion source: 170mmRF source.
Title material: pre-treatment titanium dioxide; Molecular formula: TiO
1.979Size: TD=26mm, H=17mm, C=4mm, θ=15 °.
Carry out the processing parameter of the plated film experiment of optical filming material: in (1) pumpdown time, pressure in vacuum tank drops to 3.0 * 10 from normal atmosphere
-3Pa:45min; (2) fritting time: 20min; (3) fritting final vacuum: 3.0 * 10
-3Pa; (4) plated film vacuum tightness: 1.0～2.0 * 10
-2Pa; (5) thin-film refractive index: 2.35.
When adopting conventional particles or patch material plated film, the fritting time is different different according to charge amount, generally be about about 10min, but each charging is few, and the recovery of vacuum chamber vacuum needs a large amount of time.Therefore compare with traditional optical filming material, when using pretreated optical filming material plated film of the present invention, because the crucible loadings is largely increased, and for the continuous production multilayer film, can reduce reinforced number of times, save the plenty of time, therefore adopt pretreated optical filming material plated film can significantly improve production efficiency.
Claims (7)
1, a kind of pretreatment process for preparing pre-treatment titanium dioxide or tantalum pentoxide optical filming material, it is characterized in that: this method comprises the steps:
(1), to select titanium dioxide or tantalum pentoxide for use be material powder, the purity of described material powder is 99.9%～99.99%, its granularity D
50Be 1-50 μ m;
(2), be 700～1400 ℃ with the above-mentioned raw materials powder in temperature, pressure is that vacuum hot pressing formation prepares biscuit under 10～40Mpa condition, the biscuit relative density is controlled at 80%～99%;
(3) with biscuit sintering in high temperature sintering furnace of above-mentioned preparation, the constant temperature sintering is 2～4 hours under 900～1800 ℃ of conditions of sintering temperature, the preparation base substrate;
(4), with the dimensioned moulding of base substrate in strict accordance with the coating equipment crucible;
(5), in the reducing atmosphere stove, be under 1000～1700 ℃ of conditions in temperature, above-mentioned base substrate is outgased handled 2～6 hours, be pre-treatment titanium dioxide or tantalum pentoxide optical filming material through resulting material after the above-mentioned processing.
2, the pretreatment process of optical filming material according to claim 1 is characterized in that: in described step (1), and the granularity D of described material powder
50Be 1-10 μ m.
3, the pretreatment process of optical filming material according to claim 1, it is characterized in that: in described step (4), with the dimensioned moulding of base substrate in strict accordance with the coating equipment crucible, base substrate is as follows according to the detailed process of the dimensioned moulding of crucible: the base substrate that high temperature sintering is handled utilizes the dimensioned moulding in strict accordance with crucible of surface grinding machine, cylindrical grinder, and dimensional precision is controlled at below the 0.1mm.
4, the pretreatment process of optical filming material according to claim 1 is characterized in that: in described step (5), the reducing atmosphere in the described reducing atmosphere stove is H
2, or H
2And N
2Gas mixture, perhaps use other reducing atmosphere source, the processing that outgases of reducing atmosphere stove promptly, after the dimensioned moulding of base substrate according to crucible, is cleaned, is put into after the oven dry in the processing that outgases in the reducing atmosphere stove of described base substrate.
5, a kind of pretreatment process for preparing pre-treatment zinc oxide optical filming material, it is characterized in that: this method comprises the steps:
(1), to select zinc oxide for use be material powder, the purity of described material powder is 99.9%～99.99%, its granularity D
50Be 1-50 μ m;
(2), be 700～1400 ℃ with the above-mentioned raw materials powder in temperature, pressure is that vacuum hot pressing formation prepares biscuit under 10～40Mpa condition, the biscuit relative density is controlled at 80%～99%;
(3) with biscuit sintering in high temperature sintering furnace of above-mentioned preparation, the constant temperature sintering is 2～4 hours under 900～1800 ℃ of conditions of sintering temperature, the preparation base substrate;
(4), with the dimensioned moulding of base substrate in strict accordance with the coating equipment crucible, be pre-treatment zinc oxide optical filming material.
6, the pretreatment process of optical filming material according to claim 5 is characterized in that: in described step (1), and the granularity D of described material powder
50Be 1-10 μ m.
7, the pretreatment process of optical filming material according to claim 5, it is characterized in that: in described step (4), with the dimensioned moulding of base substrate in strict accordance with the coating equipment crucible, base substrate is as follows according to the detailed process of the dimensioned moulding of crucible: the base substrate that high temperature sintering is handled utilizes the dimensioned moulding in strict accordance with crucible of surface grinding machine, cylindrical grinder, and dimensional precision is controlled at below the 0.1mm.
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| 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 |
| CN105887182A (en) * | 2014-12-15 | 2016-08-24 | 盱眙新远光学科技有限公司 | Preparation technology of trititanium pentoxide crystal |
| CN106904967B (en) * | 2017-02-21 | 2020-08-04 | 成都超纯应用材料有限责任公司 | Preparation method of high-density tantalum pentoxide film material |
| CN112110725B (en) * | 2020-09-01 | 2022-12-09 | 有研资源环境技术研究院(北京)有限公司 | High-density annular oxide coating material and preparation method thereof |
| 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 |
| CN113200569A (en) * | 2021-04-07 | 2021-08-03 | 巨玻固能(苏州)薄膜材料有限公司 | Coating material and preparation method and application thereof |
| CN113121224B (en) * | 2021-04-15 | 2022-09-06 | 有研资源环境技术研究院(北京)有限公司 | Preparation method of annular high-density tantalum pentoxide coating material |
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| 纳米氧化锌常压/超高压下的烧结及其结构与性能. 秦秀娟.. 2005 |
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