CN104557039A - Intermediate-refraction index evaporation coating material, as well as preparation technique and application thereof - Google Patents
Intermediate-refraction index evaporation coating material, as well as preparation technique and application thereof Download PDFInfo
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- CN104557039A CN104557039A CN201410815306.2A CN201410815306A CN104557039A CN 104557039 A CN104557039 A CN 104557039A CN 201410815306 A CN201410815306 A CN 201410815306A CN 104557039 A CN104557039 A CN 104557039A
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Abstract
The invention provides an intermediate-refraction index evaporation coating material, as well as a preparation technique and application thereof. The material comprises lanthanum oxide, aluminium oxide, silicon dioxide and an 8% polyvinyl alcohol solution with the mass ratio of 30:20:1:13. The preparation technique comprises the steps of mixing reaction, pressure molding, high-temperature sintering and the like. According to the preparation technique which adopts the evaporation coating material to prepare an evaporation coating film, a vacuum evaporation coating machine in the type of Nanguang ZZS600 is selected, a series of coating parameters are set up for carrying out evaporation coating on the evaporation coating material to obtain a single-layer film. The evaporation coating material, the preparation technique and application thereof have the advantages that the specific single-layer film with the refraction index of 1.75 can be prepared, the evaporation coating material has good stability, is stable in use for preparing multi-layer films, and is an ideal intermediate-refraction index evaporation coating material.
Description
Technical field
The present invention relates to specific refractory power structural evaporation coating film material and preparation technology thereof in one, and in utilizing, specific refractory power structural evaporation coating film material prepares the technique of unitary film.
Background technology
Initial anti-reflection film, it mainly plates individual layer low refractive index film on optical substrate material, utilize the anti-reflection effect of material low-refraction that the transmitance of base material is promoted, this film can make the transmitance of base material be promoted to about 98.5% from 96%.
The process of contemporary optics eyeglass, anti-reflection effect is had higher requirement, the preparation of anti-reflection film, by original single specific refractory power, basic, normal, high multiple specific refractory power is till now used alternatingly, and utilizes the effect of optical interference, is reduced to minimum by substrate luminous reflectance, its day by day perfect technique, has higher requirement to the making of optical filming material.
Summary of the invention
One of the technical problem to be solved in the present invention, is to provide specific refractory power structural evaporation coating film material in one.
The present invention realizes one of above-mentioned technical problem like this: specific refractory power structural evaporation coating film material in one, comprises lanthanum trioxide, aluminium sesquioxide and silicon-dioxide that mass ratio is 30:20:1.
Further, also comprise 8% polyvinyl alcohol water solution, and mass ratio 8% polyvinyl alcohol water solution: silicon-dioxide=13:1.
The technical problem to be solved in the present invention two, is the preparation technology providing a kind of described middle specific refractory power structural evaporation coating film material.
The present invention realizes above-mentioned technical problem two like this: a kind of preparation technology of described middle specific refractory power structural evaporation coating film material, and its working method is as follows:
(1) batch mixing reaction: be that the lanthanum trioxide of 30:20:1:13, aluminium sesquioxide, silicon-dioxide and 8% polyvinyl alcohol water solution mix by mass ratio, be placed in airtight reactor and react at least 8h, obtains reactant;
(2) compression moulding: utilize dry powder prilling machine to be pressed by reactant, then screen cloth sieves;
(3) high temperature sintering: select 1700 DEG C of Si-Mo rod high temperature atmosphere sintering ovens and alumina crucible to carry out high temperature sintering to the reactant after (2) process, obtain product; Wherein, the temperature curve of high temperature sintering is as follows:
0-1000 DEG C, temperature rise rate is 1.5-3 DEG C/min;
1000-1500 DEG C, temperature rise rate 0.7-1.5 DEG C/min;
1500 DEG C, insulation 4-6h;
Power-off, Temperature fall.
The technical problem to be solved in the present invention three, is to provide a kind of described middle specific refractory power structural evaporation coating film material to prepare the technique of unitary film.
The present invention realizes above-mentioned technical problem three like this: a kind of described middle specific refractory power structural evaporation coating film material prepares the technique of evaporation coating, select southern light ZZS600 type vacuum evaporating coating machine, evaporation coating is carried out to obtain unitary film to described middle specific refractory power structural evaporation coating film material, and filming parameter is as follows:
Select substrate: corning glass 80 × 80 × 0.3mm
Plated film initial depression: 3.0 × 10-3pa
Oxygenation flow: 4sccm
DP temperature: 260 DEG C
Heating temperature: 300 DEG C
Vaporator rate: 2A/s
Spot size: x=20%, y=20%
Film thickness: 500nm.
Preferably, the specific refractory power of described unitary film is 1.75.
The invention has the advantages that: can prepare the unitary film that specific specific refractory power is 1.75, middle specific refractory power structural evaporation coating film material has satisfactory stability, and it uses stable in the preparation of multilayer film, is a kind of desirable middle specific refractory power structural evaporation coating film material.
Embodiment
Specific refractory power structural evaporation coating film material in one, comprises lanthanum trioxide, aluminium sesquioxide, silicon-dioxide and 8% polyvinyl alcohol water solution that mass ratio is 30:20:1:13.The specific refractory power of the unitary film obtained by described middle specific refractory power structural evaporation coating film material is 1.75.
Wherein, lanthanum trioxide La
2o
3: purity more than 99.9%, meso-position radius 10-30 μm.
Aluminium sesquioxide Al
2o
3: purity more than 99.99%, meso-position radius 0.5-1.5 μm.
Silicon-dioxide SiO
2: purity more than 99.95, meso-position radius 3-8 μm.
The preparation technology of described middle specific refractory power structural evaporation coating film material, its working method is as follows:
(1) batch mixing reaction: be that the lanthanum trioxide of 30:20:1:13, aluminium sesquioxide, silicon-dioxide and 8% polyvinyl alcohol water solution mix by mass ratio, be placed in airtight reactor and react at least 8h, obtains reactant; There is violent thermopositive reaction in lanthanum trioxide meeting and moisture.
(2) compression moulding: utilize dry powder prilling machine to be pressed by reactant, and shaping reactant granular size is 1.5-3.5mm, then screen cloth sieves;
(3) high temperature sintering: select 1700 DEG C of Si-Mo rod high temperature atmosphere sintering ovens and alumina crucible (selecting of container, reactant can be made to pollute or reaction from other materials, ensure the product purity after sintering, for the product stability of later stage plated film provides safeguard) high temperature sintering is carried out to the reactant after (2) process, obtain middle specific refractory power structural evaporation coating film material.Wherein, the temperature curve of high temperature sintering is as follows:
0-1000 DEG C, temperature rise rate is 1.5-3 DEG C/min;
1000-1500 DEG C, temperature rise rate 0.7-1.5 DEG C/min;
1500 DEG C, insulation 4-6h (gap each other filled by each material, and in structure, covalent linkage, ionic linkage again rupture and combine, and forms stable product);
Power-off, Temperature fall.
Select southern light ZZS600 type vacuum evaporating coating machine, plated film verification is carried out to middle specific refractory power structural evaporation coating film material of the present invention, select Japanese Shimadzu UV2550 spectrophotometer to carry out specific refractory power verification to obtained unitary film.
Wherein, filming parameter is as follows:
Type: southern light ZZS600 type vacuum evaporating coating machine
Select substrate: corning glass 80 × 80 × 0.3mm
Plated film initial depression: 3.0 × 10-3pa
Oxygenation flow: 4sccm
DP temperature: 260 DEG C
Heating temperature: 300 DEG C
Vaporator rate: 2A/s
Spot size: x=20%, y=20%
Film thickness: 500nm.
With the unitary film that the test of Shimadzu UV2550 spectrophotometer is obtained, described in Essential Macleod software simulation, the specific refractory power of unitary film is 1.75, and stable refractive index value can be reached under above-mentioned filming parameter condition, therefore middle specific refractory power structural evaporation coating film material of the present invention is applicable to the use of current optical monolayer film and multilayer film.
Current high permeability optical monolayer film is mainly used in opticmicroscope, projector, photographic camera, the optical electron product scopes such as pick up camera, especially Powerful Light Microscope and the use of associated components to multi-layered antireflection coating have very high requirement, middle specific refractory power structural evaporation coating film material of the present invention, not only with low-refraction Coating Materials MgF2, SiO2 etc. combine good, also be combined well with the high refractive index such as zirconium white, lanthanium titanate Coating Materials, using stable in the preparation of multilayer film, is a kind of desirable middle specific refractory power structural evaporation coating film material.
The present invention utilizes the character that lanthanum trioxide, aluminium sesquioxide, silicon-dioxide are single separately, material microscopic gaps is filled mutually, be configured to the middle specific refractory power structural evaporation coating film material of the mutual supplement with each other's advantages of perfect performance, its satisfactory stability is that later stage plated film use lays the first stone, its can provide specific specific refractory power be 1.75 unitary film, also for the structural evaporation coating film material of the more excellent properties of post-production provides Process ba-sis.
Claims (5)
1. a specific refractory power structural evaporation coating film material in, is characterized in that: comprise lanthanum trioxide, aluminium sesquioxide and silicon-dioxide that mass ratio is 30:20:1.
2. middle specific refractory power structural evaporation coating film material as claimed in claim 1, is characterized in that: also comprise 8% polyvinyl alcohol water solution, and mass ratio 8% polyvinyl alcohol water solution: silicon-dioxide=13:1.
3. a preparation technology for middle specific refractory power structural evaporation coating film material as claimed in claim 1, is characterized in that: its working method is as follows:
(1) batch mixing reaction: be that the lanthanum trioxide of 30:20:1:13, aluminium sesquioxide, silicon-dioxide and 8% polyvinyl alcohol water solution mix by mass ratio, be placed in airtight reactor and react at least 8h, obtains reactant;
(2) compression moulding: utilize dry powder prilling machine to be pressed by reactant, then screen cloth sieves;
(3) high temperature sintering: select 1700 DEG C of Si-Mo rod high temperature atmosphere sintering ovens and alumina crucible to carry out high temperature sintering to the reactant after (2) process, obtain product; Wherein, the temperature curve of high temperature sintering is as follows:
0-1000 DEG C, temperature rise rate is 1.5-3 DEG C/min;
1000-1500 DEG C, temperature rise rate 0.7-1.5 DEG C/min;
1500 DEG C, insulation 4-6h;
Power-off, Temperature fall.
4. the technique utilizing the middle specific refractory power structural evaporation coating film material described in claim 1 to prepare unitary film, it is characterized in that: select southern light ZZS600 type vacuum evaporating coating machine, evaporation coating is carried out to obtain unitary film to described middle specific refractory power structural evaporation coating film material, and filming parameter is as follows:
Select substrate: corning glass 80 × 80 × 0.3mm
Plated film initial depression: 3.0 × 10-3pa
Oxygenation flow: 4sccm
DP temperature: 260 DEG C
Heating temperature: 300 DEG C
Vaporator rate: 2A/s
Spot size: x=20%, y=20%
Film thickness: 500nm.
5. in utilization as claimed in claim 4, specific refractory power structural evaporation coating film material prepares the technique of unitary film, it is characterized in that: the specific refractory power of described unitary film is 1.75.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106019417A (en) * | 2016-08-08 | 2016-10-12 | 北京富兴凯永兴光电技术有限公司 | Low-refractive-index optical coating material |
CN110713382A (en) * | 2019-10-24 | 2020-01-21 | 福建阿石创新材料股份有限公司 | Coating material and preparation method and application thereof |
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CN110713382A (en) * | 2019-10-24 | 2020-01-21 | 福建阿石创新材料股份有限公司 | Coating material and preparation method and application thereof |
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