CN1594644A - Preparation method for TiOxNy highly effective solar photo-thermal conversion film - Google Patents
Preparation method for TiOxNy highly effective solar photo-thermal conversion film Download PDFInfo
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- CN1594644A CN1594644A CN 200410028010 CN200410028010A CN1594644A CN 1594644 A CN1594644 A CN 1594644A CN 200410028010 CN200410028010 CN 200410028010 CN 200410028010 A CN200410028010 A CN 200410028010A CN 1594644 A CN1594644 A CN 1594644A
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Abstract
A TiOxNy highly effective solar energy light-heat conversion film preparation method comprises the following steps: (1) cleaning ailming substrate (2) opening vacuum coating chamber, placing ailming substrate on sample pivoted frame (3) baking vacuum coating chamber and turning on corresponding pump cooling water system, vacuum-pumping to background vacuum (4)letting Ar into vacuum coating chamber through mass flowmeter, adjusting air pressure for sputtering (5)starting direct current target power, ionizing Ar, adjusting power sputtering current, presputtering to remove target surface compound of Ti metallic target (6) introducing nitrogen and oxygen through mass flowmeter for reactive sputtering, segmental or continuous adjusting filming parameter, depositing in turn absorption layer and chemical compound reduced reflecting layer of different metal content, (7)stopping the machine and picking out film sample. The inventive process is environment friendly. Said film has property of high light-heat conversion efficiency and long life, can be broadly applied to heat collecting surface of solar energy light-heat conversion field.
Description
Affiliated technical field
The present invention relates to a kind of method for preparing the spectral selectivity absorbing membrane material of high-efficiency solar photo-thermal conversion with magnetron sputtering technology.
Background technology
The most direct valid approach of sun power utilization becomes solar energy converting heat energy to be used exactly, and the height of solar energy collector efficient is mainly determined by two factors, and the one, heat collector is to the receptivity of solar radiation; The 2nd, the heat lost by radiation degree of heat collector.The total principle that improves its efficient be to absorb as much as possible solar radiant energy and try one's best reduce thermosteresis, have good absorptive character and itself have only small amount of thermal radiating surface and the spectral selectivity absorbing membrane is exactly a short-wave radiation to the sun, thereby using the solar spectral selective absorbing membrane is one of the effective measures the most that improve collector efficiency.Realize best solar energy thermal conversion, the thermal-arrest material that is adopted just must satisfy following two conditions: (i.e. 0.3 μ m≤λ≤2.5 μ m) have the high specific absorption α that tries one's best in the solar spectrum scope; (being λ＞2.5 μ m) has alap radiation loss in thermal radiation wavelength scope, and alap emissivity is promptly arranged.The coated material that possesses this characteristic promptly is called as spectral selective absorbing coating.For solar energy collector, obtain satisfied photo-thermal conversion efficiency, the selectivity absorbing material is a prerequisite efficiently, is the sport technique segment of a key.Using solar water heater is an active and effective supplementary means that solves China's energy and environment problem at present.China's solar energy heat absorbing material annual production in 2003 has broken through 1,000 ten thousand square metres/year, the output value is above 10,000,000,000 yuans, wherein about 1/3rd be to use the plate type solar heat-absorbing plate core, especially in provinces such as southern chinas, the use of plate water-heater has comparative advantage, plate in addition water-heater is easier organically to be combined with building, and growth momentum is good, has good market outlook.
The preparation method of present domestic coated material mainly contains: spraying, electrochemical process (anodic oxidation etc.) and magnetron sputtering method etc.Magnetron sputtering preparation process has more application in the glass-vacuum tube coating for selective absorption at home.But in the preparation of flat-plate collector heat absorbing coating, what people still adopted in a large number is methods such as spraying or plating.Spraying method has at the bottom of the cost, advantage of simple technology, but the ubiquity coating adhesion is poor, easily peel off, shortcomings such as emittance height, and equally with electrochemical process there is a pollution problem, adopt magnetron sputtering method to prepare the spectral selectivity absorbing membrane, then can overcome these shortcomings, improve photo-thermal conversion efficiency and coating work-ing life, it is fast that while magnetron sputtering technique method has thin film deposition speed, the even film layer densification, be convenient to characteristics such as big area film forming and technology environmental protection, when preparation plate type solar energy heat collector plate core coating, help building extensive horizontal continuous and automatic production line, enhance productivity, further reduce cost.
The problem of an outwardness of existing electron tubes type solar energy collector is that valve tube is difficult for making the building block one-piece construction and combines with building, therefore, more external main flat solar water heaters of developed country account for more than 92% of market, as material of construction, realize sun power utilization and architecture-integral, promote being extensive use of of photo-thermal products such as solar water heater, solar airconditioning, and the expansion of photo-thermal product category and use range will increase the demand to solar spectral selective film heat-absorbing plate core again greatly.Research solar spectral selective absorbing membrane is for improving the efficient of photo-thermal conversion on the one hand, prepare necessary condition for making better solar energy collector, also prepare the different spectral selectivity absorbing membrane of color and luster on the other hand, make it to have decorative effect, can be directly used in as the functional architecture material and use, thereby organically combine with building, this also is the inexorable trend of solar energy industry development.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing the spectral selectivity absorbing membrane material of high-efficiency solar photo-thermal conversion with magnetron sputtering technology.
Principle of the present invention is according to solar spectrum and the thermal-radiating characteristics of heat collector absorbing surface, the solar radiant energy that arrives ground mainly concentrates in the wavelength region of 0.3-2.5 micron, the thermal radiation that absorbing surface sent of heat collector then mainly concentrates in the wavelength region of 2.5-30 micron, these two kinds of radiating energy are in the different wavelength regions, have only energy seldom partly to be co-located in the very narrow wavelength region, satisfy following two conditions for making selective absorption surface: (promptly 0.3 μ m＜λ＜2.5 μ m have the high specific absorption a that tries one's best in the solar spectrum scope; (being λ＞2.5 μ m) has alap radiation loss in thermal radiation wavelength scope, and alap emissivity is promptly arranged.The rete of deposit multilayer heterogeneity and metal content on copper base, optical constant difference between each rete, specific refractory power and optical extinction coefficient increase progressively from top to bottom, the CONTROL PROCESS condition realizes the coupling of optical constant, determine that each suitable layer thickness can reach good shortwave and absorb and the anti-reflection effect, infrared band has good through performance simultaneously, the film system that also can prepare grading structure in addition, the copper base of light is positioned at bottom, the high infrared reflection of dependence copper base forms the infrared high reflection of whole selective absorption surface, thereby whole film cording has low thermal emissivity.Ti is a magnesium-yttrium-transition metal, the compound color of various valence states has difference, therefore different compounds is formed will cause film color difference, utilize this point can suitably regulate sputtering technology, the composition and the thickness of compound are changed, regulate the color of film, satisfy people's requirement different color.
The preparation method of a kind of TiOxNy high-efficiency solar photo-thermal switching film provided by the invention may further comprise the steps:
(1) clean film plating substrate;
(2) open vacuum film coating chamber, on the sample pivoted frame, place cleaned film plating substrate;
(3), vacuumize and reach base vacuum 2 * 10 at 50～180 ℃ of following baking vacuum film coating chambers and open the respective cylinder cooling water system
-3～8 * 10
-3Pa;
(4) feed argon gas by mass flowmeter in vacuum film coating chamber, flow is 30～50sccm, regulates vacuum film coating chamber sputter operating air pressure to 0.3～1.0Pa;
(5) start direct current Ti cathodic power source, the ionization argon gas is regulated power supply sputtering current to 5～7A, and the surface compound of Ti target is removed in pre-sputter, keeps fresh target material surface;
(6) introduce nitrogen simultaneously and oxygen carries out reactive sputtering through mass flowmeter, sectional-regulated or regulate sputtering current, reaction gas flow, film plating substrate temperature, target-substrate distance continuously from, sputter operating air pressure and sputtering time filming parameter, deposit the absorption layer and the compound antireflection layer of different metal content successively;
(7) shut down, take out film sample.
For the film plating substrate plate core of band lead welding pipe, storing temperature is regulated between 50～100 ℃ in the step of the present invention (3); For ultra-sonic welded or not with the plated film copper base of copper pipe, Heating temperature can reach 180 ℃ or higher.
Pre-sputtering current is 3～7A in the step of the present invention (5), under the situation of discharge stability, directly adopts the pre-sputter of big electric current or progressively strengthens pre-sputtering current, and the main purpose of pre-sputter is to remove the target surface compound, guarantees the stable and repeated of coating process.
Sectional-regulated filming parameter is respectively in the step of the present invention (6): the plated film stage one: argon gas 30～50sccm, oxygen 3～10sccm, nitrogen 3～10sccm, sputtering current 3～7A, 50～200 ℃ of film plating substrate temperature, target-substrate distance be from 4～10cm, sputter operating air pressure 0.4～0.9Pa, the rotary sample pivoted frame, sputter 4～8min; The plated film stage two: argon gas 30～50sccm, oxygen 6～15sccm, nitrogen 3～16sccm, sputtering current 4～7A, 50～200 ℃ of film plating substrate temperature, target-substrate distance is from 4～10cm, sputter operating air pressure 0.4～0.9Pa, rotary sample pivoted frame, sputter 10～20min.
The filming parameter of regulating continuously in the step of the present invention (6) is: argon gas 30～50sccm, oxygen base runoff 5～10sccm, sputtering current 3～7A, 50～200 ℃ of film plating substrate temperature, target-substrate distance be from 4～10cm, sputter operating air pressure 0.4～0.9Pa, the rotary sample pivoted frame, regulate nitrogen flow to 8～16sccm gradually, every 5min flow increases progressively 0.8～1.8sccm, sputter 30～45min.
Can continue in the step of the present invention (6) sticking power and the intensity of film plating substrate baking heating with enhanced film, identical in baking condition and the step (3).Target-substrate distance is from 4～10cm in the step (6), nitrogen and oxygen flow ratio divide two stages to regulate, perhaps nitrogen and oxygen flow are regulated in gradual change continuously, keep other processing condition constant, regulate target-substrate distance from the film that can obtain different compound compositions, therefore the film color and luster that obtains and being of different shades, the thin film sputtering operating air pressure keeps low pressure 0.4～0.9Pa, can reduce the target etching under this condition, prolong target life, and easily obtain stable glow discharge, reduce the particle mean free path, obtain good coating quality, coating film thickness is controlled at below the 150nm, the absorber thickness that wherein high metal content and low-metal content are formed is at 50～120nm, and antireflection layer thickness 30～70nm, rotary sample pivoted frame can obtain good plated film homogeneity.The TiO that the present invention is prepared
xN
yThe solar spectral selective absorbing membrane comprises the copper base of light, be three layers to four layers the structure or the structure of gradual change, each rete metal content is different with the compound composition, as the composition of each stratification compound and metal content and optical constant are changed, regulate the composition of metal content and Ti compound, can regulate the film color, as blueness, purple, coffee color etc.
The prepared selective solar spectrum absorbing membrane of the present invention has the characteristics of photo-thermal conversion efficiency height and long service life, can be widely used in the thermal-arrest surface in solar energy thermal conversion field.The present invention will promote the clean environment firendly production and the widespread use on flat plate collector of spectral selectivity film, and development solar energy thermal utilization technology is had positive pushing effect.
Embodiment
Embodiment 1
Operation steps: 1) pollution layer and the zone of oxidation of removal copper coin wicking surface; 2) the copper coin core is placed on the magnetron sputtering machine specimen holder, target-substrate distance is from 5cm; 3) vacuumize and toast the raising vacuum quality, set 60 ℃ of storing temperatures, base vacuum reaches 5 * 10
-3Pa; 4) introduce argon gas 42sccm through mass flowmeter, regulate vacuum degree in vacuum chamber to 0.5Pa; 5) open cathodic power source, sputtering current 5A, pre-sputtered with Ti target surface cleaning is handled; 6) revolution specimen holder and logical oxygen 8sccm, nitrogen 4sccm keep sputter operating air pressure 0.5Pa, electric current 5A, sputter 5min; 7) logical oxygen 8sccm, nitrogen 8sccm keep sputter operating air pressure 0.5Pa, electric current 5A, sputter 15min; 8) shut down.
Technical indicator:
The film absorption rate reaches 0.94, infrared emittance 0.07.
The film color and luster is even, is mazarine.
Paste to tear through Pressuresensitive Tape and do not come off, have excellent mechanical performances.
Embodiment 2
Operation steps: 1) pollution layer and the zone of oxidation of removal copper coin wicking surface; 2) the copper coin core is placed on the magnetron sputtering machine specimen holder, target-substrate distance is from 5cm; 3) vacuumize and toast the raising vacuum quality, set 90 ℃ of storing temperatures, base vacuum reaches 5 * 10
-3Pa:4) introduce argon gas 42sccm through mass flowmeter, regulate vacuum degree in vacuum chamber to 0.5Pa; 5) open cathodic power source, sputtering current 5A, pre-sputtered with Ti target surface cleaning is handled; 6) revolution specimen holder and logical oxygen 10sccm, nitrogen 4sccm keep sputter operating air pressure 0.6Pa, electric current 5A, sputter 5min; 7) logical oxygen 10sccm, nitrogen 12sccm keep sputter operating air pressure 0.6Pa, regulate sputtering current to 5.5A, sputter 15min; 8) shut down.
Technical indicator:
The film absorption rate reaches 0.92, infrared emittance 0.12.
The film color and luster is even, is hyacinthine.
Paste to tear through Pressuresensitive Tape and do not come off, have excellent mechanical performances.
Embodiment 3
Operation steps: 1) pollution layer and the zone of oxidation of removal copper coin wicking surface; 2) the copper coin core is placed on the magnetron sputtering machine specimen holder, target-substrate distance is from 7cm; 3) vacuumize and toast the raising vacuum quality, set 180 ℃ of storing temperatures, base vacuum reaches 8 * 10
-3Pa; 4) introduce argon gas 42sccm through mass flowmeter, regulate vacuum degree in vacuum chamber to 0.5Pa; 5) open cathodic power source, sputtering current 5A, pre-sputtered with Ti target surface cleaning is handled; 6) revolution specimen holder and logical oxygen 8sccm, nitrogen are regulated 1～8sccm gradually, and every 5min flow increases progressively 1sccm, keep sputter operating air pressure 0.5Pa, electric current 5A, sputter 40min; 7) shut down.
Technical indicator:
The film absorption rate reaches 0.92, infrared emittance 0.15.
The film color and luster is even, is light blue.
Paste to tear through Pressuresensitive Tape and do not come off, have excellent mechanical performances.
Claims (4)
1, a kind of preparation method of TiOxNy high-efficiency solar photo-thermal switching film may further comprise the steps:
(1) clean film plating substrate;
(2) open vacuum film coating chamber, on the sample pivoted frame, place cleaned film plating substrate;
(3), vacuumize and reach base vacuum 2 * 10 at 50～180 ℃ of following baking vacuum film coating chambers and open the respective cylinder cooling water system
-3～8 * 10
-3Pa;
(4) feed argon gas by mass flowmeter in vacuum film coating chamber, flow is 30～50sccm, regulates vacuum film coating chamber sputter operating air pressure to 0.3～1.0Pa;
(5) start direct current Ti cathodic power source, the ionization argon gas is regulated power supply sputtering current to 5～7A, and the surface compound of Ti target is removed in pre-sputter, keeps fresh target material surface;
(6) introduce nitrogen simultaneously and oxygen carries out reactive sputtering through mass flowmeter, sectional-regulated or regulate sputtering current, reaction gas flow, film plating substrate temperature, target-substrate distance continuously from, sputter operating air pressure and sputtering time filming parameter, deposit the absorption layer and the compound antireflection layer of different metal content successively;
(7) shut down, take out sample.
2, preparation method according to claim 1 is characterized in that in the step (3) that storing temperature is regulated for the film plating substrate plate core of band lead welding pipe between 50～100 ℃; For ultra-sonic welded or not with the plated film copper base of copper pipe, Heating temperature can reach 180 ℃ or higher.
3, preparation method according to claim 1 is characterized in that sectional-regulated filming parameter is respectively in the step (6):
The plated film stage one: argon gas 30～50sccm, oxygen 3～10sccm, nitrogen 3～10sccm, sputtering current 3～7A, 50～200 ℃ of film plating substrate temperature, target-substrate distance is from 4～10cm, sputter operating air pressure 0.4～0.9Pa, rotary sample pivoted frame, sputter 4～8min;
The plated film stage two: argon gas 30～50sccm, oxygen 6～15sccm, nitrogen 3～16sccm, sputtering current 4～7A, 50～200 ℃ of film plating substrate temperature, target-substrate distance is from 4～10cm, sputter operating air pressure 0.4～0.9Pa, rotary sample pivoted frame, sputter 10～20min.
4, preparation method according to claim 1, it is characterized in that the filming parameter of regulating continuously in the step (6) is: argon gas 30～50sccm, oxygen base runoff 5～10sccm, sputtering current 3～7A, 50～200 ℃ of film plating substrate temperature, target-substrate distance is from 4～10cm, sputter operating air pressure 0.4～0.9Pa, the rotary sample pivoted frame is regulated nitrogen flow to 8～16sccm gradually, every 5min flow increases progressively 0.8～1.8sccm, sputter 30～45min.
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|---|---|---|---|
| CNB2004100280102A CN1302148C (en) | 2004-07-12 | 2004-07-12 | Preparation method for TiOxNy highly effective solar photo-thermal conversion film |
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|---|---|---|---|
| CNB2004100280102A CN1302148C (en) | 2004-07-12 | 2004-07-12 | Preparation method for TiOxNy highly effective solar photo-thermal conversion film |
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| CN1594644A true CN1594644A (en) | 2005-03-16 |
| CN1302148C CN1302148C (en) | 2007-02-28 |
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