CN101776778A - Weather-resistant silver mirror and preparation method thereof - Google Patents
Weather-resistant silver mirror and preparation method thereof Download PDFInfo
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- CN101776778A CN101776778A CN201010118047A CN201010118047A CN101776778A CN 101776778 A CN101776778 A CN 101776778A CN 201010118047 A CN201010118047 A CN 201010118047A CN 201010118047 A CN201010118047 A CN 201010118047A CN 101776778 A CN101776778 A CN 101776778A
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- marquis
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Abstract
The invention discloses a weather-resistant silver mirror which is particularly suitable for trough solar thermal power generation and a preparation method thereof. The silver mirror orderly consists of a transparent substrate, a first Al2O3 adhesive layer, an Ag reflective layer, a second Al2O3 adhesive protective layer and a SiOx protective layer. The preparation method thereof comprises the step of orderly and respectively plating the first Al2O3 adhesive layer, the Ag reflective layer, the second Al2O3 adhesive protective layer and the SiOx protective layer by adopting a multi-target intermediate frequency response vertical magnetic control sputter to prepare the weather-resistant silver mirror of the invention. The finished product of the weather-resistant silver mirror of the invention has the characteristics of high reflectivity, reliable work, long service life and the like. The preparation method of the invention has the characteristics of advance, reasonability, low cost, low energy consumption, good quality of the finished product and the like.
Description
Technical field
The present invention relates to a kind of silver mirror of anti-marquis and preparation method thereof, be specifically related to a kind of crooked silver mirror of anti-marquis that focuses on efficient reflection of large tracts of land that is applicable to trough type solar power generation and preparation method thereof.
Background technology
People have arrived quite high level for the understanding of solar energy thermal-power-generating technology, and wherein trough type solar power generation technology had especially entered the commercial epoch already.
The trough type solar power generation technology is to utilize sun power (light) by efficient reflection silver mirror, exists on the heat pipe of WATER AS FLOW MEDIUM in the middle of focusing on, and makes the WATER AS FLOW MEDIUM supercharging of vaporizing within a short period of time, finally drives the turbodynamo generating by high pressure steam.
This shows, determine a key factor of described trough type solar power generation efficient, is the reflectivity of reflection silver mirror.The reflectivity of at present existing silver mirror is below 90%.Because described trough type solar power generation technical equipment, be that environment is worked down in the open, it will stand wind and frost sleet, in freezing winter and in sultry summer with atmosphere in the test of soda acid thing, therefore the reflectivity and the serviceable life of described silver mirror, both just become the key of described trough type solar power generation technical equipment and the problem of people's research.
In fact, the technology of preparing of silver mirror, before more than 100 years, people have just successfully grasped, and for example usually are used for shining the mirror of face in people's daily life.The scientific worker by experiment, being familiar with and having grasped silver is a kind of reflectorized material of cost performance excellence, and successfully silver is plated cloth on transparency carrier, for example plates cloth and made silver-colored catoptron on unorganic glass or organic glass.But because silver is lower with the binding ability (or claiming cohesive force) of transparency carrier, so that silver layer is easy to split away off from substrate very much; So people just plate one deck intermediate adhesive layer (Al for example earlier on described substrate
2O
3Tack coat), plate argentum reflecting layer on the intermediate adhesive layer surface again, and (the Al for example that plates layer protective layer on the argentum reflecting layer surface
2O
3Protective seam), CN1834701A is such such as the Chinese patent publication number, has obtained good effect, and uses in optical articles such as camera or projector.
Because the abominable degree of the working environment of the employed silver mirror of described solar energy thermal-power-generating technical equipment, be as different as light from darkness with the catoptron of described optical articles.Thereby research and develop a kind of reflectivity height, and reliable operation, the silver mirror of anti-marquis of long service life just becomes a vital urgent expectation of development solar energy thermal-power-generating technology.
Because Al
2O
3Intermediate adhesive layer or protective seam, or the thickness of coating of argentum reflecting layer, generally (Al below 200nm
2O
3Coating is 20~50nm, and silver layer is 150~200nm), and therefore, described coating is actually a kind of very thin plated film.
The scientific worker has developed the method that many kinds prepare described plated film, sol-gel process for example, thermal decomposition gunite, chemical vapour deposition technique and magnetron sputtering method or the like.The film evenness of membranous layer of sol-gel process preparation is difficult to control, and the film of thermal decomposition gunite and chemical vapour deposition technique preparation and the adhesion of substrate are relatively poor, come off easily.And magnetron sputtering method, it is good to obtain adhesion, the film that thickness is even and fine and close.But the general employing of this existing magnetron sputtering method is two target magnetic control sputtering methods, can't adapt to the demand of the silver mirror of the anti-marquis multielement multicoating of solar energy thermal-power-generating technical equipment.Therefore, research and develop a kind of preparation method who is applicable to the solar energy thermal-power-generating technical equipment silver mirror of anti-marquis, just become development solar energy thermal-power-generating technology with the same vital urgent expectation of the described silver mirror of anti-marquis of research and development.
Summary of the invention
The present invention aims to provide a kind of reflectivity height, reliable operation, and the silver mirror of anti-marquis of long service life is to satisfy the needs of solar energy thermal-power-generating technology cause.
It is reasonable that the present invention also aims to provide a kind of method, and the coating adhesion is strong, and preparation cost is lower, and the method for the above-mentioned silver mirror of anti-marquis of preparation that energy consumption is less relatively satisfies the production needs of the silver mirror of anti-marquis of the present invention.
The present invention realizes that its technical though that will realize purpose mainly contains two aspects.The one, at the Al of prior art
2O
3The protective seam surface increases monox (SiOx) protective seam.Give full play to the corrosion resistance of SiOx protective seam; moisture resistivity; characteristics such as wearing quality and rete are firm; effectively improve the weather resisteant energy and the serviceable life of the present invention's silver mirror of anti-marquis; the 2nd, adopt many targets intermediate frequency reaction magnetocontrol sputtering machine; and reasonable advanced person's preparation technology parameter is provided, with the quality of effective raising plated film with reduce preparation cost.
Based on above-mentioned technical though, the present invention realizes that the technical scheme of its 1st purpose is:
A kind of silver mirror of anti-marquis comprises transparency carrier, the Al of plating cloth on transparency carrier one side
2O
3Adhesive linkage, plating cloth is at an Al
2O
3The Ag reflection horizon on adhesive linkage surface, plating cloth is at the 2nd Al on surface, Ag reflection horizon
2O
3Bonding protective seam, its innovative point are, the 2nd Al
2O
3The surface plating of bonding protective seam is furnished with the SiOx protective seam.
Can understand by above given technical scheme,, effectively improve the reliability and the serviceable life of the present invention's silver mirror of anti-marquis work owing to the existence of SiOx protective seam.
The present invention also advocates, at the SiOx laminar surface, is coated with at least 2 layers of waterproofing protection macromolecule skin of paint.Because the existence of described macromolecule skin of paint can further improve the erosion-resisting ability of the present invention's silver mirror of anti-marquis, has further improved functional reliability and serviceable life.
The present invention advocates that also described SiOx protective seam is SiO protective seam or SiO
2Protective seam.That is to say the SiOx protective seam, is the oxide skin(coating) of silicon.But with regard to SiO and SiO
2And opinion, the former stability is poorer than the latter, and the preferred SiOx protective seam of the present invention is SiO
2Protective seam.
The present invention also advocates, is that internal layer macromolecule skin of paint is the fast dried silver mirror protective paint UE307 layer of bi-component epoxy under 2 layers the condition when described macromolecule skin of paint, and outer macromolecule skin of paint is the fast dried silver mirror protective paint UE312 layer of single-component epoxy; When described macromolecule skin of paint is more than 3 layers the time, then described bi-component UE307 layer is with the alternate layout of single component UE312 layer.Because the alternate layout of skin of paint more than 2 layers, its weather resisteant energy will be better.
The present invention advocates that also described transparency carrier is low iron ultra-white float glass.Certainly, do not get rid of the transparency carrier of high-purity organic glass as the anti-Hou Jing of the present invention.
What the present invention advocated, a described Al
2O
3The thickness of adhesive linkage is in 20~50nm scope; The thickness in described Ag reflection horizon in 150~200nm scope, described the 2nd Al
2O
3The thickness of bonding protective seam is in 20~50nm scope; The thickness of described SiOx protective seam is in 150~200nm scope.Evidence, given thickness of coating are reasonably definite.
The present invention advocates that also this silver mirror is large tracts of land and focuses on bending.Here given is the silver mirror of anti-marquis that is applicable to trough type solar power generation equipment, does not get rid of other shape certainly, for example is applicable to the silver mirror of anti-marquis of tower type solar energy thermal power generation equipment.
The present invention realizes that the technical scheme of its 2nd purpose is:
A kind of method for preparing the silver mirror of anti-marquis as claimed in claim 1, its innovative point are, adopt the many targets intermediate frequency with aluminium target, silicon target and silver-colored target to react vertical magnetron sputtering coater, in turn include the following steps;
(a) will carry out pretreated transparency carrier and pack in the coating chamber of described vertical magnetron sputtering coater, be evacuated to 3 * 10
-3Pa;
(b) argon gas of feeding 99.99% in coating chamber, flow 200sccm makes the coating chamber internal gas pressure reach 3 * 10
-1Pa;
(c) starting purity in argon gas atmosphere is 99.99% aluminium target; Give the coating chamber aerating oxygen, oxygen flow increases from 50sccm to 250sccm gradually; Start the intermediate frequency direct supply and give the power supply of aluminium target, voltage 800V, electric current 35A is at coating chamber air pressure 3 * 10
-1Under the condition of Pa, an Al is plated in sputter
2O
3When layer thickness reaches 20-50nm, stop oxygen supply, close the power supply of supplying with the aluminium target;
(d) continue for argon gas, flow is 200sccm, starts silver-colored target intermediate frequency direct supply, electric current 50A, power supply 500V, the air pressure 3 * 10 of coating chamber
-1Pa when sputter plating Ag thickness reaches 150nm-200nm, closes the power supply of supplying with silver-colored target;
(e) start the intermediate frequency direct supply to the power supply of aluminium target, electric current 35A, voltage 800V; For argon, oxygen supply, argon flow amount 200sccm, oxygen flow 50-250sccm increases gradually, coating chamber air pressure 3.5 * 10
-1Pa, the 2nd Al is plated in sputter
2O
3When layer thickness reached 20nm-50nm, powered-down stopped oxygen supply;
(f) start the intermediate frequency direct supply and power to silicon target, silicon target purity 99.999%, voltage 800V, electric current 40A, argon flow amount 200sccm, oxygen flow 50-250sccm increases gradually, the air pressure 4 * 10 of coating chamber
-1Pa, sputter plating SiO
xWhen layer thickness reached 150-200nm, powered-down stopped promptly to make the described silver mirror of anti-marquis for argon, oxygen supply.
The present invention also advocates, at f step plating SiO
xAfter the protective seam, also be included in SiO
xThe water conservation macromolecule skin of paint of setting up defences is sprayed on the protective seam surface; The spray of described skin of paint is established, be the described silver mirror of anti-marquis react from described intermediate frequency the vertical magnetron sputtering coater take out after, in physical environment, carry out.
The present invention also advocates, described macromolecule skin of paint is that alternate successively spray is established by the fast dried silver mirror protective paint UE307 of bi-component epoxy and two kinds of paint of the fast dried silver mirror protective paint UE312 of single-component epoxy.
After technique scheme is implemented, the reliable operation that the present invention's silver mirror of anti-marquis is had, long service life is applicable to characteristics such as all-weather long-term work, is conspicuous; The preparation of the present invention's silver mirror of anti-marquis, owing to adopted many targets intermediate frequency to react the method for vertical magnetron sputtering, and the following characteristics that had are conspicuous equally.(1) by sputter simple metal target, sputtered atom and active gases are reacted and form compound film, avoid preparing the hard to tackle of high pure target compound, and can control the stoichiometric proportion of film; (2) obtain highly purified metallic aluminium target easily, and the metallic aluminium target is easy to machine-shaping and is connected with magnetic control target; (3) the two targets of intermediate frequency anode and cathode each other, sputter effect height can effectively suppress to beat arc and eradicate the anode extinction tests, thus guaranteeing that sputtering sedimentation can be stablized carries out; (4) the metallic aluminium target is the good conductor of heat, is easy to cooling, has avoided the instability of the course of work; (5) can be at cryogenic conditions deposit Al
2O
3Film, and adopt silicon target to substitute SiO
2Target, thus preparation cost and energy consumption reduced, improved the adhesion of film forming; (6) goods Nai Houyin specular reflectivity height, reflectivity reach 〉=and 92%.
Description of drawings
Fig. 1 is the structural representation of a kind of embodiment of the present invention's silver mirror of anti-marquis.
Embodiment
One of embodiment, as shown in Figure 1:
A kind of silver mirror of anti-marquis that is specially adapted to the trough type solar power generation technical equipment comprises transparency carrier 1, the Al of plating cloth on transparency carrier 1 one sides
2O
3 Adhesive linkage 2, plating cloth is at an Al
2O
3The Ag reflection horizon 3 on adhesive linkage 2 surfaces, plating cloth is at the 2nd Al on 3 surfaces, Ag reflection horizon
2O
3Bonding protective seam 4, the two Al
2O
3Bonding protective seam 4 surface platings are furnished with SiOx protective seam 5.On SiOx layer 5 surface, also be coated with at least 2 layers of waterproofing protection macromolecule skin of paint 6.Described SiOx protective seam 5 is SiO
2Protective seam.Be that internal layer macromolecule skin of paint 6-1 is the fast dried silver mirror protective paint UE307 layer of bi-component epoxy under 2 layers the condition when described macromolecule skin of paint 6, outer macromolecule skin of paint 6-2 is the fast dried silver mirror protective paint UE312 layer of single-component epoxy.Described transparency carrier 1 is low iron ultra-white float glass.A described Al
2O
3The thickness of adhesive linkage 2 is in 20~50nm scope; The thickness in described Ag reflection horizon 3 in 150~200nm scope, described the 2nd Al
2O
3The thickness of bonding protective seam 4 is in 20~50nm scope; Described SiO
2The thickness of protective seam 5 is in 150~200nm scope.This silver mirror is large tracts of land and focuses on bending.
Two of embodiment,
A kind of preparation method as the silver mirror of anti-marquis as described in one of embodiment, carry out according to following steps successively:
In the coating chamber of a, the vertical coating machine of packing into after glass substrate cleaned, dries, vertical five target coating machines are vacuumized, reach 3 * 10 with the two targets of two pairs of intermediate frequencies and a direct current list target
-3Pa, aluminium target purity reaches 99.99%, and silicon target purity reaches 99.999%, and silver-colored target purity is 99.99%.
B, to the argon gas of the indoor feeding 99.99% of vacuum coating, flow 200sccm makes the coating chamber internal gas pressure reach 1.0 * 10
-1Pa.
C, start the aluminium target of the two targets of intermediate frequency in argon gas atmosphere, feed purity and be 99.99% purity oxygen, flow is increased to 250sccm from 50sccm, voltage 800V, and electric current 35A, coating chamber air pressure are 3.5 * 10
-1Pa opens the target sputter, sputter the one Al
2O
3After layer thickness reaches 20nm-50nm, stop oxygen supply, intermediate frequency power supply is closed.
D, the silver-colored target direct supply of startup, voltage 500V, electric current 50A continues for argon gas, flow 200sccm, air pressure reaches 3.5 * 10
-1Pa, sputter is silver-plated, when the Ag layer thickness reaches 120nm-200nm, closes direct supply.
E, startup intermediate frequency power supply are powered to the aluminium target, voltage 800V, and electric current 35A, argon flow amount 200sccm, aerating oxygen, flow is increased to 250sccm gradually by 50sccm, air pressure 3.5 * 10
-1Pa, the 2nd Al is plated in sputter
2O
3Layer, when thickness reached 20nm-50nm, powered-down stopped oxygen supply, stopped for argon gas.
F, startup intermediate frequency power supply, to the silicon target power supply, electric current 40A, voltage 800V, argon flow amount 200sccm, oxygen flow increases to 250sccm gradually by 50sccm, and coating chamber air pressure is 4.0 * 10
-1Pa, plating SiO
2When layer thickness reached 150nm-200nm, powered-down stopped to stop oxygen supply gas for argon gas.
G, will be through f step plating SiO
2The goods of rete take out in the coating chamber of described coating machine, to SiO
2Coating surface is successively sprayed the fast dried silver mirror protective paint UE312 layer of fast dried silver mirror protective paint UE312 layer of bi-component epoxy and single component ring gas, and the described skin of paint of each layer all dry processing, and its bake out temperature is 150 ℃, and drying time is 5min.Promptly make the present invention's silver mirror of anti-marquis.
The silver mirror of anti-marquis that the present invention is prepared, after tested its reflectivity reach 〉=92%; The routine test result shows under the simulation atmospheric conditions, its mission life-span reaches 〉=and 1000 days.Obtained very obvious effects.
The usable range of the present invention's silver mirror of anti-marquis, the restriction that not described by this instructions.
Claims (10)
1. the silver mirror of anti-marquis comprises transparency carrier (1), the Al of plating cloth on transparency carrier (1) one side
2O
3Adhesive linkage (2), plating cloth is at an Al
2O
3The Ag reflection horizon (3) on adhesive linkage (2) surface, plating cloth is at the 2nd Al on Ag reflection horizon (3) surface
2O
3Bonding protective seam (4) is characterized in that, the 2nd Al
2O
3The plating of bonding protective seam (4) surface is furnished with SiOx protective seam (5).
2. the silver mirror of anti-marquis according to claim 1 is characterized in that, on SiOx layer (5) surface, also is coated with at least 2 layers of waterproofing protection macromolecule skin of paint (6).
3. the silver mirror of anti-marquis according to claim 1 is characterized in that, described SiOx protective seam (5) is SiO protective seam or SiO
2Protective seam.
4. the silver mirror of anti-marquis according to claim 2, it is characterized in that, be under 2 layers the condition when described macromolecule skin of paint (6), internal layer macromolecule skin of paint (6-1) is the fast dried silver mirror protective paint UE307 layer of bi-component epoxy, outer macromolecule skin of paint (6-2) is the fast dried silver mirror protective paint UE312 layer of single-component epoxy; When described macromolecule skin of paint (6) is more than 3 layers the time, then described bi-component UE307 layer (6-1) is with the alternate layout of single component UE312 layer (6-2).
5. the silver mirror of anti-marquis according to claim 1 is characterized in that, described transparency carrier (1) is low iron ultra-white float glass.
6. the silver mirror of anti-marquis according to claim 1 is characterized in that, a described Al
2O
3The thickness of adhesive linkage (2) is in 20~50nm scope; The thickness in described Ag reflection horizon (3) in 150~200nm scope, described the 2nd Al
2O
3The thickness of bonding protective seam (4) is in 20~50nm scope; The thickness of described SiOx protective seam (5) is in 150~200nm scope.
7. according to the described silver mirror of anti-marquis of one of claim 1 to 6, it is characterized in that this silver mirror is large tracts of land and focuses on bending.
8. a method for preparing the silver mirror of anti-marquis as claimed in claim 1 is characterized in that, adopts the many targets intermediate frequency with aluminium target, silicon target and silver-colored target to react vertical magnetron sputtering coater, in turn includes the following steps;
(a) will carry out pretreated transparency carrier and pack in the coating chamber of described vertical magnetron sputtering coater, be evacuated to 3 * 10
-3Pa;
(b) argon gas of feeding 99.99% in coating chamber, flow 200sccm makes the coating chamber internal gas pressure reach 3 * 10
-1Pa;
(c) starting purity in argon gas atmosphere is 99.99% aluminium target; Give the coating chamber aerating oxygen, oxygen flow increases from 50sccm to 250sccm gradually; Start the intermediate frequency direct supply and give the power supply of aluminium target, voltage 800V, electric current 35A is at coating chamber air pressure 3 * 10
-1Under the condition of Pa, an Al is plated in sputter
2O
3When layer thickness reaches 20-50nm, stop oxygen supply, close the power supply of supplying with the aluminium target;
(d) continue for argon gas, flow is 200sccm, starts silver-colored target intermediate frequency direct supply, electric current 50A, power supply 500V, the air pressure 3 * 10 of coating chamber
-1Pa when sputter plating Ag thickness reaches 150nm-200nm, closes the power supply of supplying with silver-colored target;
(e) start the intermediate frequency direct supply to the power supply of aluminium target, electric current 35A, voltage 800V; For argon, oxygen supply, argon flow amount 200sccm, oxygen flow 50-250sccm increases gradually, coating chamber air pressure 3.5 * 10
-1Pa, the 2nd Al is plated in sputter
2O
3When layer thickness reached 20nm-50nm, powered-down stopped oxygen supply;
(f) start the intermediate frequency direct supply and power to silicon target, silicon target purity 99.999%, voltage 800V, electric current 40A, argon flow amount 200sccm, oxygen flow 50-250sccm increases gradually, the air pressure 4 * 10 of coating chamber
-1Pa, sputter plating SiO
xWhen layer thickness reached 150-200nm, powered-down stopped promptly to make the described silver mirror of anti-marquis for argon, oxygen supply.
9. the preparation method of the silver mirror of anti-marquis according to claim 8 is characterized in that, at f step plating SiO
xAfter the protective seam, also be included in SiO
xThe water conservation macromolecule skin of paint of setting up defences is sprayed on the protective seam surface; The spray of described skin of paint (6) is established, be the described silver mirror of anti-marquis react from intermediate frequency the vertical magnetron sputtering coater take out after, in physical environment, carry out.
10. the preparation method of the silver mirror of anti-marquis according to claim 9; it is characterized in that; described macromolecule skin of paint (6) is that alternate successively spray is established by the fast dried silver mirror protective paint UE307 of bi-component epoxy and two kinds of paint of the fast dried silver mirror protective paint UE312 of single-component epoxy.
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CN201010118047XA CN101776778B (en) | 2010-02-23 | 2010-02-23 | Preparation method of weather-resistant silver mirror |
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CN102183805A (en) * | 2011-05-07 | 2011-09-14 | 常州龙腾太阳能热电设备有限公司 | Light-gathering silver mirror for light-gathering solar thermal power generation |
CN102323632A (en) * | 2011-09-16 | 2012-01-18 | 常州工业技术玻璃有限公司 | Reflection silver mirror used for solar energy thermal power generation and manufacturing method thereof |
CN102809769A (en) * | 2012-08-12 | 2012-12-05 | 兰州大成科技股份有限公司 | Solar energy reflector and preparation method thereof |
CN103105011A (en) * | 2013-01-31 | 2013-05-15 | 中国科学院上海技术物理研究所 | Solar selective absorbing film series suitable for medium-high temperature heat usage and preparation method thereof |
CN103105011B (en) * | 2013-01-31 | 2015-05-13 | 中国科学院上海技术物理研究所 | Solar selective absorbing film series suitable for medium-high temperature heat usage and preparation method thereof |
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CN114265136A (en) * | 2021-12-22 | 2022-04-01 | 常州龙腾光热科技股份有限公司 | Condensation reflector with frost and snow prevention super-hydrophobic characteristic |
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CN101776778B (en) | 2012-04-25 |
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Address after: 213100 Changzhou Province, Wujin District, the town of cattle, the town of rainbow road, No. 26 Patentee after: ROYAL TECH CSP LIMITED Address before: 213163 Rainbow Road, Niu Tong Town, Wujin District, Jiangsu, Changzhou Patentee before: Changzhou Longteng Solar Energy Heating Equipment Co., Ltd. |