CN1207580C - Wide-angle and wide-spectrum reflective film and manufacturing method thereof - Google Patents
Wide-angle and wide-spectrum reflective film and manufacturing method thereof Download PDFInfo
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- CN1207580C CN1207580C CNB03141527XA CN03141527A CN1207580C CN 1207580 C CN1207580 C CN 1207580C CN B03141527X A CNB03141527X A CN B03141527XA CN 03141527 A CN03141527 A CN 03141527A CN 1207580 C CN1207580 C CN 1207580C
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- Prior art keywords
- evaporation
- rete
- transition bed
- wide
- reflectance coating
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- Expired - Fee Related
Links
- 238000001228 spectrum Methods 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title description 2
- 230000007704 transition Effects 0.000 claims abstract description 34
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 239000011521 glass Substances 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims description 28
- 238000001704 evaporation Methods 0.000 claims description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 22
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 22
- 238000000576 coating method Methods 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 22
- 239000011248 coating agent Substances 0.000 claims description 21
- 239000011651 chromium Substances 0.000 claims description 16
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 15
- 229910052804 chromium Inorganic materials 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 11
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- 229910052763 palladium Inorganic materials 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 11
- 239000010936 titanium Substances 0.000 claims description 11
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 8
- 239000004411 aluminium Substances 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 230000003287 optical effect Effects 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 5
- 230000002787 reinforcement Effects 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 4
- 238000005566 electron beam evaporation Methods 0.000 claims description 4
- 239000010946 fine silver Substances 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims description 4
- 238000002207 thermal evaporation Methods 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 238000010894 electron beam technology Methods 0.000 claims description 3
- 238000001659 ion-beam spectroscopy Methods 0.000 claims description 3
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000007747 plating Methods 0.000 abstract description 3
- 238000002310 reflectometry Methods 0.000 abstract description 3
- 230000003595 spectral effect Effects 0.000 abstract description 3
- 230000003014 reinforcing effect Effects 0.000 abstract 1
- -1 silver (aluminium) Chemical compound 0.000 description 9
- 239000010944 silver (metal) Substances 0.000 description 9
- 238000005728 strengthening Methods 0.000 description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000001579 optical reflectometry Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- MEYZYGMYMLNUHJ-UHFFFAOYSA-N tunicamycin Natural products CC(C)CCCCCCCCCC=CC(=O)NC1C(O)C(O)C(CC(O)C2OC(C(O)C2O)N3C=CC(=O)NC3=O)OC1OC4OC(CO)C(O)C(O)C4NC(=O)C MEYZYGMYMLNUHJ-UHFFFAOYSA-N 0.000 description 1
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- Physical Vapour Deposition (AREA)
Abstract
The wide-angle and wide-spectrum reflecting film includes glass substrate, and first transition layer, second transition layer, metal film layer and reinforcing film layer deposited successively on the glass substrate. The invention is characterized in that a plating double-transition layer structure is adopted, the whole film layer can resist high temperature and deliquescence, and the film layer, the film layer and the substrate are not easy to fall off, and the spectral reflectivity is high.
Description
Technical field
The present invention relates to reflectance coating, particularly a kind of high performance wide angle and wide spectrum reflectance coating and preparation method thereof.
Background technology
The network technology of information age, the needs of the information of sharing and aggregate information are become increasingly conspicuous, this has brought up the very big demand that jumbotron is shown, traditional with CRT as the display technique of image forming source because its large volume, big weight and the restriction that is subjected to self brightness, become the bottleneck that limits its development gradually, generation and what come is with LCD (Liquid Crystal Display), DLP (DigitalLight Processing), LCOS (Liquid Crystal on Silicon) is the large screen projection display system of mechanism, is that the display system of mechanism is fast with its response speed especially with DLP, the light utilization efficiency height, characteristics such as high-res and gaining great popularity.
But the performance quality of this key element of the photoconductive tube in the DLP display system (light tunnel) becomes constraint always, and it further improves bottleneck of performance.The wide angle and wide spectrum reflectance coating that is used for light pipe system of existing technology made has following deficiency:
(1). spectral reflectivity is low;
(2). poor adhesive force between rete and the substrate and between rete and the rete comes off easily;
(3). high temperature resistantly and moisture resistance separate indifferently, the environment of high temperature or deliquescence can make film surface sustain damage easily, and spectrum is easy to generate drift.
Summary of the invention
The technical problem to be solved in the present invention is to overcome above-mentioned the deficiencies in the prior art, a kind of wide angle and wide spectrum reflectance coating and preparation method thereof is provided, this reflectance coating not only has good optical reflectivity, and difficult drop-off between rete and the substrate, have the good high temperature resistant and moisture resistance characteristic of separating simultaneously.
Technical solution of the present invention is as follows:
A kind of wide angle and wide spectrum reflectance coating comprises substrate of glass, it is characterized in that on substrate of glass evaporation has first transition bed, metallic diaphragm and reinforcement rete successively, also has second transition bed between described first transition bed and metallic diaphragm.
Described first transition bed is that high-purity chromium evaporation forms, and thickness is 20~100nm.
Described first transition bed is to be formed by high purity nickel or palladium or titanium evaporation, and its thickness is 20~100nm.
Described metallic diaphragm is to be formed greater than 99.9% fine silver evaporation by purity, and its thickness is 130~4000nm.
Described metallic diaphragm is to be formed greater than 99.9% fine aluminium evaporation by purity, and its thickness is 130~4000nm.
Described second transition bed be by the composite material of first buffer layer material and metallic diaphragm material simultaneously evaporation form, the atomic percent that these two kinds of materials mix is 30%/70%~70%/30%, the thickness of whole rete is 10~100nm.
Described reinforcement rete is the combination rete that is staggered to form by the high and low refractive index material, and its film is LH, or LHLH, and its low-index material is selected MgF for use
2Or Al
2O
3, its high-index material is selected ZrO for use
2Or TiO
2Or HfO
2Or ZnS or ZnSe, L, the optical thickness of H layer are 80nm~150nm.
Described first, second transition bed and metal film adopt thermal evaporation, ion beam sputtering or magnetron sputtering method to be coated with, and strengthening membrane adopts electron beam evaporation method.
The preparation method of described wide angle and wide spectrum reflectance coating comprises following step:
1. the organic solvent ultrasonic cleaning is used earlier in the cleaning of substrate of glass, cleans with ion gun before the evaporation;
2. according to the design of rete, select the deposition material of each rete;
3. substrate of glass is placed in the vacuum chamber, and its vacuum degree control is 9 * 10
-4~2 * 10
-1Pa;
4. earlier at substrate of glass evaporation first transition bed;
5. evaporation second transition bed on first transition bed;
6. evaporation metal rete on second transition bed;
7. by optical control method or duration control method, be coated with the reinforcement rete with electron beam on the metallic diaphragm surface.
Advantage of the present invention and characteristics
(1) characteristics one of the present invention are to adopt and are coated with two transition layer structures, and first transition bed is selected crome metal (nickel, palladium, titanium).Because the affinity of itself and glass surface is more intense, therefore present good adhesion, when be coated with at the first excessive laminar surface after by chromium (nickel, palladium, titanium) silver (aluminium) mixed membranous layer second excessive layer, owing to exist in the time of chromium (nickel, palladium, titanium) silver (aluminium) two kinds of elements, so this layer can all show good affinity and adhesion simultaneously and between the first excessive layer and fine silver (aluminium) rete.Therefore not only therefore present good hot matching effect owing to it has good excessive property simultaneously in conjunction with firm between first three tunic and the substrate, thereby it is injury-free not come off through rete after the hot and humid processing, its spectrum does not produce drift simultaneously.。
(2) adopt MgF2 in the enhancement Layer, Al2O3 is as directly combination between low-index material and argent (aluminium) film, because MgF2, between the characteristic of Al2O3 itself it and the silver good adhesion is arranged, and because L, H is a dielectric layer, and the adhesion between them is very firm, therefore can not come off between whole enhancement Layer and the silver (aluminium).
(3) since strengthening membrane have a spectral reflectivity height.
(4) whole rete can high temperature resistant moisture resistance separating, and between the rete, be not easy to come off between rete and the substrate.
Description of drawings
Fig. 1 is the structural representation of wide angle and wide spectrum reflectance coating of the present invention
Among the figure: the 1-substrate of glass 2-first transition bed 3-second transition bed 4-metal level 5-strengthens rete
Embodiment
The structure of wide angle and wide spectrum reflectance coating of the present invention as shown in Figure 1.Wherein
First transition bed 2 forms for high-purity chromium (nickel, palladium, titanium) (purity is 90%-100%) evaporation, and THICKNESS CONTROL is between 20-100nm;
Second transition bed 3 adopts the rete of the composite material that evaporation chromium (nickel, palladium, titanium) silver (aluminium) two kinds of materials simultaneously obtain for chromium (nickel, palladium, titanium) silver (aluminium) mixolimnion, the ratio of both atomic percents can range of control between 30%/70%~70%/30%, the one-tenth-value thickness 1/10 of whole rete is between 10-100nm;
Argent (aluminium) rete 4 forms greater than 99.9% fine silver (aluminium) evaporation for purity, and thickness is between 130nm~4000nm;
Strengthening rete 5 is the rete combinations that become by high low-index material interleaved set: if the optical thickness of every layer of every floor height refraction materials film with H represent, the optical thickness of every layer of low-index material rete represents with L, then the film of strengthening membrane system can be LH, perhaps is LHLH.L, the size of H is any one value in the 80nm-150nm scope.Wherein low-index material can be selected MgF for use
2, Al
2O
3, high index of refraction can be selected ZrO for use
2, TiO
2, HfO
2, ZnS, ZnSe etc.
The evaporation process of various coatings and method
Substrate of glass 1 at first will add ultrasonic cleaning with organic solvent before putting into vacuum chamber, will clean with ion gun before evaporation;
All metal level 2.3.4 materials can select for use thermal evaporation, ion beam sputtering or magnetron sputtering mode to finish;
Strengthening rete 5 usefulness electron beam evaporation plating modes finishes;
The vacuum degree control of whole process is 9 * 10
-4Pa~2 * 10
-1Pa can adopt baking simultaneously, and temperature range can be controlled in 80~300 ℃;
Production order: at first on substrate of glass evaporation chromium (nickel, palladium, titanium) as the first excessive layer, then at the second excessive layer of the composite material of evaporation chromium (nickel, palladium, titanium) silver (aluminium) formation simultaneously on the basis of the first excessive layer, the 3rd step certain thickness silver of evaporation (aluminium) film on the surface of the second excessive layer, the method by optics control is coated with the designed strengthening membrane in front at silver (aluminium) laminar surface with electron beam at last.
Be several embodiments of the present invention in the following table, all embodiment finish in same plated film vacuum chamber, and the substrate of film is a glass, and vacuum tightness is better than 5 * 10
-3Pa, first and second transition bed and argent (aluminium) film adopt thermal evaporation to be coated with mode, and the purity of Coating Materials is all greater than 99.9%, and strengthening membrane adopts the electron beam evaporation plating mode.Substrate all was to adopt ultrasonic cleaning earlier before plated film, cleaned with organic solvent then.
The meaning of 0.64Cr0.36Ag is Cr in this rete in the table, and elements atomic percentage is respectively 64% and 36% among the Ag two, and other is analogized.
Above-mentioned reflectance coating can not wanted the second excessive layer yet, shown in embodiment 5.
The sample of the foregoing description all has good optical property, rete is high temperature resistant, moisture resistance separating do not come off.
The embodiment table
The case numbering | First transition bed | Second transition bed | Silver (aluminium) film | Strengthening membrane |
Embodiment 1 | Chromium (thickness 20nm) | 0.64Cr0.36Ag (40nm) | Ag(250nm) | Film structure: LH L:MgF 2 H:TiO 2 L=H=100nm |
Embodiment 2 | Chromium (thickness 35nm) | 0.52Cr0.48Ag (50nm) | Ag(285nm) | Film structure: LH L:MgF 2 H:TiO 2 L=H=100nm |
Embodiment 3 | Chromium (thickness 35nm) | 0.52Cr0.48Ag (57nm) | Ag(1000nm) | Film structure: LHLH L:Al 2O 3 H:ZrO 2 L=H=110nm |
Embodiment 4 | Chromium (thickness 100nm) | 0.47Cr0.53Ag (50nm) | Ag(400nm) | Film structure: LHLH L:MgF 2 H:TiO 2 L=H=125nm |
Embodiment 5 | Chromium (thickness 100nm) | 0.0nm | Ag(900nm) | Film structure: LHLH L:MgF 2 H:TiO 2 L=H=125nm |
Embodiment 6 | Chromium (thickness 45nm) | 0.52Cr0.48Al (50nm) | Al(285nm) | Film structure: LHLH L:MgF 2 H:TiO 2 L=H=125nm |
Embodiment 7 | Nickel (thickness 35nm) | 0.52Ni0.48Ag (20nm) | Ag(600nm) | Film structure: LHLH L:MgF 2 H:ZrO 2 L=H=125nm |
Embodiment 8 | Palladium (thickness 35nm) | 0.52Pd0.48Ag (57nm) | Ag(1200nm) | Film structure: LHLH L:MgF 2 H:ZnSe L=H=125nm |
Embodiment 9 | Titanium (thickness 35nm) | 0.52Ti0.48Ag (90nm) | Ag(1500nm) | Film structure: LHLH L:MgF 2 H:HfO 2 L=H=125nm |
Claims (9)
1, a kind of wide angle and wide spectrum reflectance coating, comprise substrate of glass (1), it is characterized in that on substrate of glass (1) evaporation has first transition bed (2), metallic diaphragm (4) and strengthens rete (5) successively, second transition bed (3) in addition between described first transition bed (2) and metallic diaphragm (4).
2, wide angle and wide spectrum reflectance coating according to claim 1 is characterized in that described first transition bed (2) forms for high-purity chromium evaporation, and thickness is 20~100nm.
3, wide angle and wide spectrum reflectance coating according to claim 1 is characterized in that described first transition bed (2) is to be formed by high purity nickel or palladium or titanium evaporation, and its thickness is 20~100nm.
4, wide angle and wide spectrum reflectance coating according to claim 1 is characterized in that described metallic diaphragm (4) is to be formed greater than 99.9% fine silver evaporation by purity, and its thickness is 130~4000nm.
5, wide angle and wide spectrum reflectance coating according to claim 4 is characterized in that described metallic diaphragm (4) is to be formed greater than 99.9% fine aluminium evaporation by purity, and its thickness is 130~4000nm.
6, wide angle and wide spectrum reflectance coating according to claim 1, it is characterized in that described second transition bed (3) be by the composite material of first transition bed (2) material and metallic diaphragm (4) material simultaneously evaporation form, the atomic percent that these two kinds of materials mix is 30%/70%~70%/30%, and the thickness of whole rete is 10~100nm.
7, wide angle and wide spectrum reflectance coating according to claim 1 is characterized in that described reinforcement rete (5) is the combination rete that is staggered to form by the high and low refractive index material, and its film is LH, or LHLH, and its low-index material is selected MgF for use
2Or Al
2O
3, its high-index material is selected ZrO for use
2Or TiO
2Or HfO
2Or ZnS or ZnSe, L, the optical thickness of H layer are 80nm~150nm.
8, wide angle and wide spectrum reflectance coating according to claim 1, it is characterized in that described first transition bed (2), second transition bed (3) and metallic diaphragm (4) adopt thermal evaporation, ion beam sputtering or magnetron sputtering method to be coated with, and strengthen rete (5) and adopt electron beam evaporation method.
9, a kind of preparation method of wide angle and wide spectrum reflectance coating is characterized in that comprising following step:
The organic solvent ultrasonic cleaning is used earlier in the cleaning of substrate of glass (1), cleans with ion gun before the evaporation;
According to the design of rete, the deposition material of selected each rete;
Substrate of glass (1) is placed in the vacuum chamber, and its vacuum degree control is 9 * 10
-4~2 * 10
-1Pa;
Tide over layer (2) at substrate of glass (1) evaporation first earlier;
Go up evaporation second transition bed (3) at first transition bed (2);
Go up evaporation metal rete (4) at second transition bed (3);
By optical control method or duration control method, be coated with reinforcement rete (5) with electron beam on metallic diaphragm (4) surface.
Priority Applications (1)
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CNB03141527XA CN1207580C (en) | 2003-07-11 | 2003-07-11 | Wide-angle and wide-spectrum reflective film and manufacturing method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB03141527XA CN1207580C (en) | 2003-07-11 | 2003-07-11 | Wide-angle and wide-spectrum reflective film and manufacturing method thereof |
Publications (2)
Publication Number | Publication Date |
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CN1477407A CN1477407A (en) | 2004-02-25 |
CN1207580C true CN1207580C (en) | 2005-06-22 |
Family
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CN103811625A (en) * | 2012-11-05 | 2014-05-21 | 江苏稳润光电有限公司 | Process for improving LED light emission efficiency |
CN103698826B (en) * | 2013-11-21 | 2015-09-30 | 中国科学院上海技术物理研究所 | A kind of Polarization-state phase-adjustable wide-spectrum catoptron |
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CN105738989A (en) * | 2016-04-19 | 2016-07-06 | 中国科学院上海光学精密机械研究所 | High-dispersion lens structure based on HGTI |
CN107092046A (en) * | 2017-04-26 | 2017-08-25 | 上海默奥光学薄膜器件有限公司 | A kind of high reflective mirror of wide spectrum |
CN108196329B (en) * | 2017-12-19 | 2020-05-01 | 中国航空工业集团公司洛阳电光设备研究所 | Preparation method of medium-wave infrared medium reinforced metal high-reflection film |
CN109445008B (en) * | 2018-11-12 | 2024-06-18 | 江西兆九光电技术有限公司 | Depolarization beam splitter prism and film coating method thereof |
CN112962064A (en) * | 2021-02-01 | 2021-06-15 | 国家纳米科学中心 | High-temperature-resistant optical reflecting film and preparation method and application thereof |
CN114231922B (en) * | 2021-11-30 | 2022-09-02 | 北京理工大学 | VO (volatile organic compound) 2 Method for preparing base multilayer film structure and product thereof |
CN114933422B (en) * | 2022-05-17 | 2024-05-24 | 长兴旗滨节能玻璃有限公司 | Anti-reflection coated glass and preparation method thereof |
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2003
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