CN1527071A - Reflector with protective metal layer of strengthened adhesion and its making process - Google Patents
Reflector with protective metal layer of strengthened adhesion and its making process Download PDFInfo
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- CN1527071A CN1527071A CNA031358799A CN03135879A CN1527071A CN 1527071 A CN1527071 A CN 1527071A CN A031358799 A CNA031358799 A CN A031358799A CN 03135879 A CN03135879 A CN 03135879A CN 1527071 A CN1527071 A CN 1527071A
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Abstract
The reflector with high reflectivity and protective metal layer of strengthened adhesion includes substrate and successively deposited protective metal or alloy layer of Cr, Ti and Ni; metal Al or Ag layer; SiO2 or Al2O3 layer; and TiO2 layer successively deposited on the substrate. The reflector has high reflectivity, excellent durability, powerful adhesion of the compact protective metal layer to the substrate to block the corrosion of the free ion in the substrate to the metal Al or Ag layer. The making process of the reflector is also provided. The present invention has less deposited layers, simplified making process and apparatus and is suitable for industrial production in high efficiency and low cost.
Description
Technical field:
The present invention is relevant with catoptron, and is special relevant with high reflection mirror that contains coat of metal and manufacture method thereof.
Background technology:
The patent disclosure of application number 00130782 a kind of catoptron, depositing Al, MgF successively on the glass basis of polishing
2, TiO
2Layer forms reflectance coating.As everyone knows, the adhesion of Al and glass (or plastics) is more weak, and its reason is that the sputter threshold energy of Al almost is minimum, uses Ar
+Sputter is 13ev only, thereby the kinetic energy of the Al particle that sputters is also low, so it is just poor to be deposited on the adhesion of the Al layer on the glass (or plastics), and occurs flaws such as pin hole easily, has a strong impact on mirror-quality, has reduced minute surface to the reflection of light rate.Free ion pair Al layer causes corrosion in the glass baseplate in addition, has reduced minute surface serviceable life.
For the defective of the poor adhesive force that solves Al and matrix (glass, plastics etc.) and the flaw that pin hole brought, the patent disclosure of application number 01119452 another kind of aluminium reflector and preparation method, deposition nonmetal medium film SiO makes ground floor on glass basis, depositing Al forms the second layer of aluminium reflective film on ground floor, deposits MgF on the second layer
2Formation deposits CeO as the 3rd layer of transparent protective film on the 3rd layer
2Formation deposits SiO as the 4th layer of transparent protective film on the 4th layer
2Formation is as the layer 5 of transparent protective film.This patent employing deposition nonmetal medium film SiO on glass basis makes ground floor, but nonmetal medium film SiO can not fine solution Al or Ag and matrix (glass, plastics etc.) between the not strong defective of adhesion, can not effectively stop in the matrix dissociated ion to the corrosion of Al or Ag, and this patent is at MgF
2Need substep realization under 80 ℃～300 ℃ higher temperature environment during layer deposition, sedimentary deposit is many, the technological requirement height, the equipment complexity is unfavorable for large-scale production, and production efficiency is low, cost is high, environment temperature is higher during in addition owing to plated film, and plastic material can't use as matrix material.
The patent disclosure of application number 01122099.6 with the high reflection mirror of Ag as reflective coating, compare adhesion and the corrosion resistivity that has improved rete with the disclosed catoptron of JP2-109003A and JP11-64612A, this high reflection mirror comprises matrix, and depositing Ti Ox (wherein 1≤X≤2), Ag, Al successively
2O
3, TiO
2, or on matrix, deposit SiOx (wherein 1≤X≤2), Cr, Ag, Al successively
2O
3, TiO
2Its substantial improvements is to substitute SiOx with TiOx to improve Ag layer and SiOx adhesion not so good and can occur peeling off or cracking defect; or depositing the Cr layer on the SiOx layer again improves above-mentioned defective; thereby the working routine more than bringing; as continuous large-scale production; the deposition of TiOx or SiOx deielectric-coating all is the comparison difficulty, and main is that the complexity of production equipment is increased, so production efficiency is low, production cost is high.
Summary of the invention:
In view of the foregoing, the objective of the invention is to provide a kind of high reflection mirror that strengthens adhesion between matrix and Al layer or the Ag layer and can effectively stop the coat of metal that dissociated ion in the matrix corrodes Al layer or Ag layer that has in order to overcome above deficiency.This catoptron has the strong and high reflectivity of adhesion of good corrosion resistivity, rete and matrix.
Another object of the present invention is in order to provide a kind of because the rete number that is deposited reduces; but the complexity of simplified manufacturing technique and equipment; easier realization large-scale industrial production; enhance productivity the manufacture method of the high reflection mirror that the coat of metal that strengthens adhesion is arranged that reduces production costs.
The object of the present invention is achieved like this:
The present invention has the high reflection mirror of the coat of metal that strengthens adhesion to comprise matrix, and Al layer or Ag layer are deposited on the SiO on Al layer or the Ag layer
2Layer or Al
2O
3Layer is deposited on SiO
2Layer or Al
2O
3TiO on the layer
2Layer is characterized in that depositing the coat of metal of the alloy that strengthens elemental metals Cr that adhesion between matrix and Al layer or the Ag layer can stop effectively that also dissociated ion in the matrix corrodes Al layer or Ag layer or Ti or Ni or this elemental metals between matrix and Al layer or Ag layer.Because the sputter threshold energy of coat of metal such as Cr layer exceeds nearly one times than Al; and coat of metal is very fine and close; the hardness height, thereby can play the effect of flaws such as strengthening adhesion and minimizing pin hole and can stop effectively that dissociated ion is to the corrosion of Al layer in the glass substrate.The light reflectivity that this high reflection mirror film ties up to the visible light wave range scope can be higher than 97%.
Above-mentioned matrix is glass or plastics.
Above-mentioned metal coating layer thickness is 0.1～10nm.
The thickness of above-mentioned Al layer is 40～120nm, and the thickness of Ag layer is 50～300nm.
Above-mentioned SiO
2Layer, TiO
2Layer, Al
2O
3The thickness of layer is λ/4, and λ wherein is design predominant wavelength.
The manufacture method of high reflection mirror of the present invention is: matrix is through the cleaning machine cleaning and through cold; hot blast drying and/or the oven dry of hot case; enter the preceding lock chamber of continuous magnetron sputtering production line then; after slightly vacuumizing; enter preceding holding chamber; after treating that its vacuum arrives the setting requirement; enter buffering I chamber; cushion the I chamber this moment; the vacuum of the first filming chamber and buffering II chamber has reached the setting requirement; charge into working gas Ar; plate the coat of metal of the alloy of one deck elemental metals Cr or Ti or Ni or this elemental metals earlier in the magnetron sputtering mode with direct current or intermediate frequency power supply; plate one deck Al or Ag with direct current or intermediate frequency power supply in the magnetron sputtering mode again; enter insulated chamber through buffering II chamber; the vacuum of this chamber keeps setting requirement; workpiece enters buffering III chamber then; cushion the III chamber this moment; second; the vacuum of the 3rd coating chamber and buffering IV chamber has reached the setting requirement; charge into working gas Ar; with intermediate frequency power supply sputter Si or Al and Ti target, to controlling reacting gas O by plasma emission spectral intensity monitor closed loop balance control device (PEM)
2Amount carry out sufficient reactive sputtering, make SiO
2Or Al
2O
3Thickness reach λ/4 (λ is main design wavelength), TiO
2Thickness reach λ/4 (λ is main design wavelength), behind buffering IV chamber, enter the back holding chamber, enter the back lock chamber then, promptly finish the making of whole high reflection mirror after workpiece goes out after the lock chamber, it is characterized in that and to control reacting gas O with plasma emission spectral intensity monitor closed loop balance control device (PEM) under the normal temperature state or under heated condition
2Amount carry out sufficient reactive sputtering deposits elemental metals Cr or Ti or Ni or this elemental metals successively on matrix alloying metal protective seam, Al layer or Ag layer, SiO
2Layer or Al
2O
3Layer and TiO
2Layer.
The present invention has deposited between basic unit and Al layer or Ag layer and can strengthen adhesion between matrix and Al layer or the Ag layer and can stop effectively that dissociated ion is to the protective seam of Al layer or the corrosion of Ag layer, so have the advantage that the adhesion of good corrosion resistivity, rete and matrix is strong, reflectivity is high in the matrix.
The inventive method is owing to the rete number that is deposited reduces, but the easier realization large-scale industrial production of simplified manufacturing technique and equipment, the production efficiency height, production cost reduces.
Description of drawings:
Fig. 1 is a high reflection mirror structural representation of the present invention.
Fig. 2 is Fig. 1 high reflection mirror production method process flow diagram.
Fig. 3 is a PEM closed loop balance control device structural representation.
Fig. 4 is another structural representation of high reflection mirror of the present invention.
Embodiment:
Fig. 1 is the cut-open view of first embodiment of high reflection mirror of the present invention.Referring to Fig. 1, earlier clean and do and/or the glass basis 1 of hot case oven dry through hot and cold wind through cleaning machine, Cr layer 2 is to adopt pure Cr target, be deposited on the glass substrate 1 in the magnetron sputtering mode with direct current or intermediate frequency power supply, thickness is 2nm (also can select at 1～10nm), by this transition bed, improves the adhesion of the Al layer 3 that plates subsequently, and prevent that dissociated ion is to the corrosion of Al layer, because the sputter threshold energy Ar of Cr in the glass substrate
+Be sputtered to 22ev, exceed nearly one times than Al, and the Cr layer is very fine and close, the hardness height, thereby can play the effect of flaws such as strengthening adhesion and minimizing pin hole and can stop effectively that dissociated ion is to the corrosion of Al layer in the glass substrate, facts have proved that this coating can not cause reducing the reflectivity of highly reflecting films system yet in visible-range; Al layer 3 is main metallic reflectors of high reflection mirror film system, adopts the sputter of DC power supply, and thickness is 90nm (also can select between 40～120mm), has best reflectivity to guarantee the Al layer; SiO
2Layer 4 and TiO
2Layer 5 is formed enhancing reflectance coating system, SiO
2Be deposited upon on the Al layer TiO
2Be deposited upon SiO
2On the layer, reach the purpose that improves reflectivity, SiO
2And TiO
2Layer all adopts twin intermediate frequency reaction magnetocontrol sputtering to prepare SiO
2Thicknesses of layers be λ/4 (λ is main design wavelength), TiO
2The thickness of rete is λ/4 (λ is main design wavelength), by changing SiO
2And TiO
2The various combination of thicknesses of layers can change the optical reflection family curve of highly reflecting films, makes it satisfy needed reflected value.Can satisfy production with above film layer structure and thickness, be particularly suitable for the use of the high reflection mirror of RPTV the high reflection mirror red, yellow, that the selective reflection of blue light requires.This film system sees Table the available reflectivity of various optical wavelength:
| Wavelength (nm) | 400 | ?450 | ?500 | ?550 | ?600 | ?650 | ?700 |
| Reflectivity R (%) | 92.5 | ?95 | ?95 | ?94.6 | ?93.5 | ?91.5 | ?88.2 |
Fig. 2 is the production method process flow diagram of Fig. 1 high reflection mirror.Glass basis cleaning machine in matting 6 cleans and does through hot and cold wind that (also can carry out heated baking to matrix does drying up operation 7,90 ℃～110 ℃ of heating-up temperatures), lock chamber 9 before feeding platform enters then, after slightly being evacuated to 2Pa, holding chamber 10 before entering treats that its vacuum arrives 5 * 10
-3Behind the Pa, enter buffering I chamber 11, at this moment, the base vacuum of buffering I chamber, the first filming chamber 12 and buffering II chamber 13 has reached 2 * 10
-3Pa charges into working gas Ar to 3 * 10
-1Pa with DC magnetron sputtering last layer Cr, uses DC magnetron sputtering one deck Al earlier again, and thickness 40～120nm enters insulated chamber 14 through buffering II chamber, and the vacuum of this chamber should keep being better than 5 * 10
-3Pa, workpiece enters buffering III chamber 15 then, and the base vacuum of buffering III chamber, second, third coating chamber 16,17 and buffering IV chamber 18 has reached 2 * 10
-3Pa charges into working gas Ar to 3 * 10
-1Pa starts Si and Ti target with intermediate frequency power supply, to controlling reacting gas O by PEM closed loop balance control device
2Amount carry out sufficient reactive sputtering, make SiO
2Thickness be λ/4 (λ is main design wavelength, is 500 as λ); TiO
2Thickness be λ/4 (λ is main design wavelength such as λ=500, and thickness is 125), behind buffering IV chamber, enter back holding chamber 19, the vacuum of this chamber should keep being better than 5 * 10
-3Pa enters back lock chamber 20 then, and the vacuum of this chamber is 2Pa, promptly finishes the making of whole high reflection mirror after workpiece goes out after the lock chamber.
Sequence number 21,22,23 is respectively measuring station 21, overlay film station 22, blanking bench 23 among the figure.
Fig. 3 is PEM closed loop balance control device control principle figure.PEM closed loop balance control device 24 comprises the optical emitting detector 25 that is contained in the operating room, with the optical emitting detector, the PID ratio infinitesimal analysis arithmetic and control unit 26 that intermediate frequency power supply connects, the piezo electric valve 27 that is contained on the O2 delivery pipe is connected with PID by reacting gas stream pipeline 28.Sequence number 29,30,31,32,33 is respectively mass flowmeter among the figure, intermediate frequency power supply, base material, two magnetron cathode.
Fig. 4 is another structural representation of high reflection mirror of the present invention.Glass basis 1 cleans through pre-treatment earlier, and carries out the described rete in normal temperature deposit back after with hot and cold wind water being dried up, and also can carry out depositing the described rete in back behind the heated baking to substrate.Cr layer 2 is to adopt pure Cr target, and on glass substrate 1, thickness is 3nm, because the sputter threshold energy Ar of Cr with the DC sputtering sedimentation
+Sputter is 22ev, more much higher than Ag (being 15ev), and the Cr film is very fine and close, the hardness height, thereby can play enhancing adhesion and stop the corrosion of glass substrate dissociated ion to Ag, and this coating can not cause reducing the reflectivity of highly reflecting films system yet in visible-range; Ag layer 34 is main metallic reflectors of high reflection mirror film system, adopts the DC magnetron sputtering, and the thickness of rete is 95nm (also can between 50～300nm), should guarantee that the Ag layer has best reflectivity; Al
2O
3Layer 35 adopts twin medium frequency reactive sputtering to be deposited on the Ag layer 34, and deposits superincumbent TiO subsequently
2 Layer 5 constitutes protective seam and forms the film system that increases reflectivity, because Al
2O
3Layer is a kind of film of densification, so can form the stable rete that opposing fully is moist and scratch, thickness is λ/4 (λ is that main design wavelength such as λ are 500); TiO
2Layer 5 is formed on Al
2O
3On the layer 35, form the high refractive index layer that increases reflection configuration, adopt twin medium frequency reactive sputtering method preparation, thickness is λ/4 (λ is that main design wavelength such as λ are 500).Pass through Al
2O
3Layer 35 and TiO
2 Layer 5 combination more can embody the high reflection characteristic of Ag.The light reflectivity that this high reflection mirror film ties up to the visible light wave range scope can be higher than 97%.Simultaneously,, can change the reflective character curve of highly reflecting films system, be adjusted in the reflectivity of the variant wave band of visible light, make it satisfy the demand of various different occasions main design wavelength lambda various combination.
Claims (6)
1, the high reflection mirror of the coat of metal that strengthens adhesion is arranged, comprise matrix, Al layer or Ag layer are deposited on the SiO on Al layer or the Ag layer
2Layer or Al
2O
3Layer is deposited on SiO
2Layer or Al
2O
3TiO on the layer
2Layer is characterized in that depositing the coat of metal of the alloy that strengthens elemental metals Cr that adhesion between matrix and Al layer or the Ag layer can stop that also dissociated ion in the matrix corrodes Al layer or Ag layer or Ti or Ni or this elemental metals between matrix and Al layer or Ag layer.
2, the high reflection mirror that the coat of metal that strengthens adhesion is arranged as claimed in claim 1 is characterized in that described matrix is glass or plastics.
3, the high reflection mirror that the coat of metal that strengthens adhesion is arranged as claimed in claim 1 or 2, the thickness that it is characterized in that coat of metal is 0.1～10nm.
4, the high reflection mirror that the coat of metal that strengthens adhesion is arranged as claimed in claim 1 or 2, the thickness that it is characterized in that the Al layer is 40～120nm, the thickness of Ag layer is 50～300nm.
5, the high reflection mirror that the coat of metal that strengthens adhesion is arranged as claimed in claim 1 or 2 is characterized in that SiO
2Layer, TiO
2Layer, Al
2O
3The thickness of layer is λ/4, and λ wherein is design predominant wavelength.
6; the manufacture method that the high reflection mirror of the coat of metal that strengthens adhesion is arranged as claimed in claim 1; may further comprise the steps: matrix is through the cleaning machine cleaning and through cold; hot blast drying and/or the oven dry of hot case; enter the preceding lock chamber of continuous magnetron sputtering production line then; after slightly vacuumizing; enter preceding holding chamber; after treating that its vacuum arrives the setting requirement; enter buffering I chamber; cushion the I chamber this moment; the vacuum of the first filming chamber and buffering II chamber has reached the setting requirement; charge into working gas Ar; plate the coat of metal of the alloy of one deck elemental metals Cr or Ti or Ni or this elemental metals earlier in the magnetron sputtering mode with direct current or intermediate frequency power supply; plate one deck Al or Ag with direct current or intermediate frequency power supply in the magnetron sputtering mode again; enter insulated chamber through buffering II chamber; the vacuum of this chamber keeps setting requirement; workpiece enters buffering III chamber then; cushion the III chamber this moment; second; the vacuum of the 3rd coating chamber and buffering IV chamber has reached the setting requirement; charge into working gas Ar; with intermediate frequency power supply sputter Si or Al and Ti target, to controlling reacting gas O by plasma emission spectral intensity monitor closed loop balance control device (PEM)
2Amount carry out sufficient reactive sputtering, make SiO
2Or Al
2O
3Thickness reach λ/4, λ is main design wavelength, TiO
2Thickness reach λ/4, λ is main design wavelength, behind buffering IV chamber, enter the back holding chamber, enter the back lock chamber then, promptly finish the making of whole high reflection mirror after workpiece goes out after the lock chamber, it is characterized in that and to control reacting gas O with plasma emission spectral intensity monitor closed loop balance control device under the normal temperature state or under heated condition
2Amount carry out sufficient reactive sputtering deposits the alloy of elemental metals Cr or Ti or Ni or this elemental metals successively on matrix coat of metal, Al layer or Ag layer, SiO
2Layer or Al
2O
3Layer and TiO
2Layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031358799A CN1527071A (en) | 2003-09-23 | 2003-09-23 | Reflector with protective metal layer of strengthened adhesion and its making process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031358799A CN1527071A (en) | 2003-09-23 | 2003-09-23 | Reflector with protective metal layer of strengthened adhesion and its making process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1527071A true CN1527071A (en) | 2004-09-08 |
Family
ID=34286346
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA031358799A Pending CN1527071A (en) | 2003-09-23 | 2003-09-23 | Reflector with protective metal layer of strengthened adhesion and its making process |
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|---|---|
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|---|---|---|---|---|
| CN103210112A (en) * | 2010-11-17 | 2013-07-17 | 新日铁住金高新材料株式会社 | Metal foil for base material |
| CN104267452A (en) * | 2014-10-18 | 2015-01-07 | 中山市创科科研技术服务有限公司 | Reflecting mirror compounded with mirror surface film layers based on tin film and preparation method of reflecting mirror |
| CN104345362A (en) * | 2014-10-18 | 2015-02-11 | 中山市创科科研技术服务有限公司 | Metallic film reflector and manufacturing method thereof |
| CN105334557A (en) * | 2015-11-10 | 2016-02-17 | 东莞鑫泰玻璃科技有限公司 | High-reflection sun light reflection mirror and manufacturing method thereof |
| CN105725385A (en) * | 2016-03-08 | 2016-07-06 | 金华金灿水晶有限公司 | Vacuum plating rhinestone and manufacturing method thereof |
| CN106222612A (en) * | 2016-07-29 | 2016-12-14 | 郑州航空工业管理学院 | A kind of for energy-conservation hydrophobic transparent film of civil aircraft air port glass and preparation method thereof |
| CN106324731A (en) * | 2016-10-28 | 2017-01-11 | 宜昌南玻显示器件有限公司 | Multi-functional reflective film of on-board exterior mirror and preparation method |
| US9902134B2 (en) | 2010-11-17 | 2018-02-27 | Nippon Steel & Sumikin Materials Co., Ltd. | Metal foil for base material and producing method thereof |
| CN108008476A (en) * | 2017-12-22 | 2018-05-08 | 武汉大学 | A kind of laser generator reflecting plate |
| CN109628894A (en) * | 2018-12-29 | 2019-04-16 | 润坤(上海)光学科技有限公司 | A kind of preparation method of far ultraviolet high reflective mirror |
| CN114369791A (en) * | 2021-12-24 | 2022-04-19 | 重庆四联特种装备材料有限公司 | Method for improving white spots on surface of metal film |
-
2003
- 2003-09-23 CN CNA031358799A patent/CN1527071A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI558478B (en) * | 2010-11-17 | 2016-11-21 | 新日鐵高新材料股份有限公司 | Metal foil for base material |
| CN103210112A (en) * | 2010-11-17 | 2013-07-17 | 新日铁住金高新材料株式会社 | Metal foil for base material |
| US9296180B2 (en) | 2010-11-17 | 2016-03-29 | Nippon Stell & Sumikin Materials Co., Ltd. | Metal foil for base material |
| US9902134B2 (en) | 2010-11-17 | 2018-02-27 | Nippon Steel & Sumikin Materials Co., Ltd. | Metal foil for base material and producing method thereof |
| CN104267452A (en) * | 2014-10-18 | 2015-01-07 | 中山市创科科研技术服务有限公司 | Reflecting mirror compounded with mirror surface film layers based on tin film and preparation method of reflecting mirror |
| CN104345362A (en) * | 2014-10-18 | 2015-02-11 | 中山市创科科研技术服务有限公司 | Metallic film reflector and manufacturing method thereof |
| CN104267452B (en) * | 2014-10-18 | 2016-07-13 | 中山市创科科研技术服务有限公司 | A kind of preparation method of the reflecting mirror being compounded with based on stannum film mirror rete |
| CN105334557A (en) * | 2015-11-10 | 2016-02-17 | 东莞鑫泰玻璃科技有限公司 | High-reflection sun light reflection mirror and manufacturing method thereof |
| CN105725385A (en) * | 2016-03-08 | 2016-07-06 | 金华金灿水晶有限公司 | Vacuum plating rhinestone and manufacturing method thereof |
| CN106222612A (en) * | 2016-07-29 | 2016-12-14 | 郑州航空工业管理学院 | A kind of for energy-conservation hydrophobic transparent film of civil aircraft air port glass and preparation method thereof |
| CN106324731A (en) * | 2016-10-28 | 2017-01-11 | 宜昌南玻显示器件有限公司 | Multi-functional reflective film of on-board exterior mirror and preparation method |
| CN108008476A (en) * | 2017-12-22 | 2018-05-08 | 武汉大学 | A kind of laser generator reflecting plate |
| CN108008476B (en) * | 2017-12-22 | 2019-09-10 | 武汉大学 | A kind of laser generator reflecting plate |
| CN109628894A (en) * | 2018-12-29 | 2019-04-16 | 润坤(上海)光学科技有限公司 | A kind of preparation method of far ultraviolet high reflective mirror |
| CN114369791A (en) * | 2021-12-24 | 2022-04-19 | 重庆四联特种装备材料有限公司 | Method for improving white spots on surface of metal film |
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