CN103302917A - Dual-absorption-layer TiON weather-resistant photothermal coating and preparation method thereof - Google Patents
Dual-absorption-layer TiON weather-resistant photothermal coating and preparation method thereof Download PDFInfo
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- CN103302917A CN103302917A CN201310201135XA CN201310201135A CN103302917A CN 103302917 A CN103302917 A CN 103302917A CN 201310201135X A CN201310201135X A CN 201310201135XA CN 201310201135 A CN201310201135 A CN 201310201135A CN 103302917 A CN103302917 A CN 103302917A
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Abstract
The invention relates to a dual-absorption-layer TiON weather-resistant photothermal coating and a preparation method thereof. Copper, aluminum or ferrite stainless steel is used as a substrate, and the coating orderly comprises a Ti film infrared reflection layer, a TiON film first absorption sublayer, a TiON film second absorption sublayer and a SixNy film antireflection layer. The preparation method comprises the following steps of: firstly, introducing argon and performing direct current sputtering with Ti as a target material and copper, aluminum or ferrite stainless steel as a substrate; then injecting nitrogen with the flow of 5-9sccm and oxygen with the flow of 1-4sccm to perform sputtering, and performing sputtering by regulating nitrogen flow to be 9-15sccm and regulating the oxygen flow to be 3-5sccm; finally, adjusting the substrate to be directed at the Si target material, and performing sputtering by regulating the nitrogen flow to be 15-25sccm and regulating the oxygen flow to be 0sccm. The solar selective photothermal absorption coating is excellent in weather resistance, can be used for preparing flat solar absorber plate cores, and has better application prospect.
Description
Technical field
The present invention relates to a kind of solar selectively photo-thermal absorber coatings and preparation method thereof, belong to the preparing technical field of composite film material.
Background technology
Solar selectively photo-thermal absorber coatings is for the Core Feature part that absorbs solar energy in the solar thermal collector.It is a thin film system with sandwich construction, comprises the infrared external reflection bottom, absorbed layer and the anti-reflection layer that are attached to substrate surface.
Solar selectively absorbing coating converts solar energy into heat energy, raise in the temperature of this process floating coat and base material, and with the infrared thermal wave form to the environmental radiation energy.In order to improve energy gain and loss ratio, require this coating system can fully absorb the part of concentration of energy in the earthbound solar energy spectrum, simultaneously less to the environmental radiation infrared thermal wave, this i.e. the selective application requirements that absorbs.So-called " the selective absorption ", in the application's context, the light absorption that refers to this coating system has selectively spectrum and have higher absorptance α value in solar energy spectrum wavelength 0.3--2.5 micrometer range, has low transmitting ratio ε value in the infrared range of spectrum beyond 2.5 microns.
Solar absorption is solar selectively absorbing coating system two most important light thermal property indexs with infrared emission than ε than α, wherein solar absorption depends on the selection of absorbed layer and anti-reflection layer than α, and infrared emission depends primarily on the selection of infrared external reflection primer than ε, and is subject to the impact of absorbed layer.Usually, the material of infrared external reflection bottom requirement is satisfied on base material or its surface because of employing, and becomes the part of solar selectively absorbing coating system.
Up to now, for the sunshine in the 0.3--2.5 micron wave length scope, adopt commercially available solar thermal collector or the solar heat-collection plate core of vacuum coating technology preparation, its absorptance can reach about 0.93, and the infrared emission ratio drops to below 0.1.In the practice, when the solar absorption of coating for selective absorption than in 0.92 to 0.96(high solar absorptance theoretical value) between the time, absorption efficiency has been difficult to have the variation of practical significance.
Utilize magnetron sputtering technology to prepare solar selectively absorbing coating, sequentially generally comprise following steps:
1) adopt the metal base with high infrared reflectance, or with the metal deposition of tool high infrared reflectance on base material (such as stainless steel) surface, form the infrared external reflection bottom;
2) deposit absorbed layer at the infrared external reflection bottom, inject flow by continuously changing reacting gas, produce different absorption subgrades; The chemical composition of whole absorbed layer changes in gradient.
3) deposit anti-reflection layer at absorbed layer, be generally ceramic material (oxide or nitride).
Magnetron sputtering process carries out in vacuum chamber as shown in Figure 2, and wherein magnetic field and electric field intersect vertically, near the cycloid motion so that electronics is spinned negative electrode (being target).Electronics clashes into ar atmo and causes it to become argon ion in motion process, and discharges a new free electron.Argon ion bombards target under the effect of electric field, the target particle deposition that it sputters is near the base material the anode; Secondary electron assists to form spontaneous glow discharge, so that sputter procedure is continued as the sputter byproduct.The power supply of magnetron sputtering can use dc source, the pulse power, midfrequent AC power supply, radio-frequency power supply or be used in combination above-mentioned several power supply.
Can obtain the various metals thin-film material by magnetically controlled DC sputtering, this utilization inert gas (being generally argon gas) is the sputter medium.Can obtain multiple ceramic membrane or metal-ceramic composite film material by reaction magnetocontrol sputtering, these ceramic materials are that metal targets and active gases reaction generate.Inert gas and active gases can inject vacuum chamber by air inlet pipe separately or after mixing.In sputter coating, keep vacuum with vavuum pump.The gas inject flow is take sccm as unit, the per minute gas inject amount of namely calculating take gas volume under the status of criterion (unit is as cubic centimetre).
In the vacuum coating practice, must be according to volume and the factor testing and measuring technology parameters such as shape, vavuum pump pumping efficiency and vacuum coating power of vacuum chamber, to prepare satisfactory thin-film material.The main technologic parameters of adjustable comprises injection flow, vacuum coating power and the sputtering time etc. of various gases.Vacuum coating power is larger, and the rete sedimentation rate is faster; And sputtering time is basically only relevant with thicknesses of layers.When plated metal-ceramic composite film material, in order to obtain specific component ratio, when improving vacuum coating power, need to correspondingly increase the injection flow of reacting gas.Easily cause reacting unstability and power is excessive, reduce the uniformity of membranous layer ingredient and thickness.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of double absorption layer TiON weatherability photo-thermal coating double absorption layer TiON weatherability photo-thermal coating, the core absorbed layer of this coating partly adopts the biabsorption sublayer structure, can realize the high efficiency preparation by " two-step method ", technique is easy to regulation and control, finish the good weatherability of coating, be suitable for hot operation in vacuum or air, its solar absorption ratio is greater than 0.93, and the infrared emission ratio is less than 0.1.
The technical scheme that the present invention takes is:
A kind of double absorption layer TiON weatherability photo-thermal coating double absorption layer TiON weatherability photo-thermal coating as base material, is followed successively by Ti film infrared reflecting layer, TiON film the first absorption subgrade, TiON film the second absorption subgrade, Si with copper, aluminium or ferritic stainless steel
xN
yThe film anti-reflection layer, Ti film infrared reflecting layer is controlled at 50-100nm, and TiON film first absorbs the subgrade THICKNESS CONTROL at 50-150nm, and TiON film second absorbs the subgrade THICKNESS CONTROL at 50-150nm, Si
xN
yFilm anti-reflection layer THICKNESS CONTROL is at 20-60nm.
The preparation method of above-mentioned coating comprises that step is as follows:
(1) first base material is carried out surface clean, then in vacuum chamber, utilize BP unipolar pulse grid bias power supply that base material is carried out reverse sputtering and clean, activate by Ions Bombardment;
(2) argon gas of injection flow 35-45sccm, pressure remains on 0.5-1pa, and adjust revoluting motor matrix is in over against the position of metal Ti target, sputter 10min, rotating speed 15r/min, spacing 10cm, d.c. sputtering power are 2.2-2.5w/cm
2
(3) adopt the metal Ti target, when passing into 35-45sccm Ar gas, the injection flow is that nitrogen and the flow of 5-9sccm is the oxygen of 1-4sccm, and power remains on 2.2-2.5w/cm
2, first reactive sputtering 10min; The adjustment nitrogen flow is 9-15sccm, oxygen flow 3-5sccm, and power remains on 2.2-2.5w/cm
2Keep dc source and spinning motor in opening, reactive sputtering 10min again, rotating speed and spacing remain unchanged;
(4) base material is in over against the position of conduction Si target, when passing into 35-45sccm Ar gas, regulate nitrogen flow to 15-25sccm, oxygen flow to 0sccm, open Si target dc source and spinning motor, adjust sputtering power to 1.7-2.2w/cm
2, sputter 5min, rotating speed and distance values remain unchanged.
The present invention selects copper, aluminium or thermal conductivity factor large, and the ferritic stainless steel that the coefficient of expansion is little, good in oxidation resistance, anti-stress corrosion performance are good is as base material.First base material is carried out surface clean, then in vacuum chamber, utilize BP unipolar pulse grid bias power supply that base material is carried out reverse sputtering and clean, by Ions Bombardment, improve its surface-active, strengthen the adhesion of base material and infrared reflecting layer.Form metal-ceramic composite absorbent layer by the magnetically controlled DC sputtering Titanium as infrared reflecting layer, titanium and oxygen, the sputter of nitrogen element reaction, silicon and nitrogen reactive sputtering form infrared anti-reflection layer, the three sequentially forms, and jointly consists of the solar selectively absorbing coating system.
This coating for selective absorption is that described nonmetal gas is oxygen and nitrogen by the composite film material of titanium and nonmetal gas reaction sputtering sedimentation and silicon and the preparation of nonmetal gas reaction sputtering sedimentation.The solar selectively photo-thermal absorber coatings good weatherability that the present invention is prepared can be used for preparing flat panel solar heat collecting plate core, and application prospect is good.It is 94.9% ± 1% that the inventive method has successfully prepared absorptivity, and emissivity is less than 10%(multi-disc average) large scale sample (see figure 4).Compare with similar products at home and abroad, the titanium oxynitrides photo-thermal coating of applicant's preparation is on the leading domestic level, and is very approaching with international most advanced level, and technique is simple, convenient easy row.After 48 hours, absorptivity reduces less than 2% sample, satisfies the instructions for use of solar thermal collector more than middle temperature (200 ° of C) through 285 ° of C bakings.The present invention has also repeated preparation by batch, has showed stability and the maturity of this technology.
Description of drawings
Fig. 1 is double absorption layer TiON weatherability photo-thermal coating structure of the present invention;
Fig. 2 is magnetron sputtering apparatus;
Fig. 3 sputter schematic diagram;
Fig. 4 flat plate collector photo-thermal coating comparison diagram;
(a) the TiON flat plate collector photo-thermal coating sample (30*15cm) that utilizes the inventive method to prepare; (b) the blue film (100*200cm) of the whole plate of import flat plate collector photo-thermal coating-" German blue titanium ";
Fig. 5 the present invention makes the abosrption spectrogram of TiON gradient coating sample (30*15cm/ sheet); Wherein the high-absorbility of sample is 96.1%, and minimum is 93.4%, and the average absorption rate is 94.9%, and all samples emissivity all is lower than 10%.
Wherein, 1 is base material, and 2 is Ti film infrared reflecting layer, and 3a is that TiON film first absorbs subgrade, 3b is that TiON film second absorbs subgrade, and 4 is Si
xN
yThe film anti-reflection layer, 5 is air inlet, and 6a is the rectangle magnetic control target, and 6b is the rectangle magnetic control target, and 7 is substrate frame, 8 is chip bench.
The specific embodiment
Main experimental facilities of the present invention is the magnetic control film coating machine, and product type is TSU-600.The magnetron sputtering vacuum chamber structure of this equipment mainly comprises air inlet 5, two rectangle magnetic control target 6a and 6b, substrate frame 7 and chip bench 8 as shown in Figure 2.The magnetron sputtering chamber of this equipment is with the mechanical pump realization low vacuum of bleeding, again by the molecular pump pumping high vacuum to being lower than 10
-4Pa.
A kind of double absorption layer TiON weatherability photo-thermal coating as base material 1, is followed successively by Ti film infrared reflecting layer 2, TiON film the first absorption subgrade 3a, TiON film the second absorption subgrade 3b, Si with copper, aluminium or ferritic stainless steel
xN
yFilm anti-reflection layer 4, Ti film infrared reflecting layer 2 is controlled at 50-100nm, and TiON film first absorbs subgrade 3a THICKNESS CONTROL at 50-150nm, and TiON film second absorbs subgrade 3b THICKNESS CONTROL at 50-150nm, Si
xN
yFilm anti-reflection layer 4 THICKNESS CONTROL are at 20-60nm.
The preparation method of double absorption layer TiON weatherability photo-thermal coating:
(1) inject the argon gas of flow 35-40sccm in the chamber by air inlet pipe, the conditioning equipment flow-limiting valve makes chamber pressure remain on 1-2pa, opens the unipolar pulse bias generator and matrix is carried out reverse sputtering cleans 10min, and d.c. sputtering power is 2.2w/cm
2, by Ions Bombardment, improve its surface-active, strengthen the adhesion of base material and infrared reflecting layer.
(2) base material cleans and to close grid bias power supply after complete, continue logical 35-40sccm argon gas, the conditioning equipment flow-limiting valve makes chamber pressure remain on 0.5pa, adjusting revoluting motor is in over against the position of rectangle magnetic control target (metal Ti target) 6a matrix, open Ti target dc source and spinning motor, sputter 10min, rotating speed 15r/min, spacing 10cm, adjusting d.c. sputtering power is 2.2w/cm
2, preparation Ti metallic film is as infrared reflecting layer.
(3) continue logical 35-40sccm argon gas, the flow that reinjects is that nitrogen and the flow of 5-7sccm is the oxygen of 1-2sccm, and power remains on 2.2w/cm
2, first reactive sputtering 10min, the TiON film of reactive sputtering absorbs subgrade as first.
The adjustment nitrogen flow is 9-10sccm, oxygen flow 3-5sccm, keeps dc source and spinning motor in opening, and power remains on 2.2w/cm
2, sputter 10min, rotating speed and spacing remain unchanged, and preparation TiON film absorbs subgrade as second.
(4) complete Ti target dc source and the spinning motor of closing of preparation.Regulate revoluting motor to change substrate location, base material is in over against the position of rectangle magnetic control target (conduction Si target) 6b.Pass into the 35-40sccm argon gas, regulate nitrogen flow to 15-20sccm, oxygen flow to 0sccm.Open Si target dc source and spinning motor, adjust sputtering power to 1.7w/cm
2, sputter 5min, rotating speed and distance values remain unchanged, preparation Si
xN
yFilm is as anti-reflection layer.
The preparation method of double absorption layer TiON weatherability photo-thermal coating:
(1) inject the argon gas of flow 40-45sccm in the chamber by air inlet pipe, the conditioning equipment flow-limiting valve makes chamber pressure remain on 1-3pa, opens the unipolar pulse bias generator and matrix is carried out reverse sputtering cleans 20min, and d.c. sputtering power is 2.5w/cm
2, by Ions Bombardment, improve its surface-active, strengthen the adhesion of base material and infrared reflecting layer.
(2) base material cleans and to close grid bias power supply after complete, continue logical 40-45sccm argon gas, the conditioning equipment flow-limiting valve makes chamber pressure remain on 1pa, adjusting revoluting motor is in over against the position of rectangle magnetic control target (metal Ti target) 6a matrix, open Ti target dc source and spinning motor, sputter 10min, rotating speed 15r/min, spacing 10cm, adjusting d.c. sputtering power is 2.5w/cm
2, preparation Ti metallic film is as infrared reflecting layer.
(3) continue logical 40-45sccm argon gas, the flow that reinjects is that nitrogen and the flow of 7-9sccm is the oxygen of 3-4sccm, and power remains on 2.5w/cm
2, first reactive sputtering 10min, the TiON film of reactive sputtering absorbs subgrade as first.
The adjustment nitrogen flow is 12-15sccm, oxygen flow 4-5sccm, keeps dc source and spinning motor in opening, and power remains on 2.5w/cm
2, sputter 10min, rotating speed and spacing remain unchanged, and preparation TiON film absorbs subgrade as second.
(4) complete Ti target dc source and the spinning motor of closing of preparation.Regulate revoluting motor to change substrate location, base material is in over against the position of rectangle magnetic control target (conduction Si target) 6b.Pass into the 40-45sccm argon gas, regulate nitrogen flow to 20-25sccm, oxygen flow to 0sccm.Open Si target dc source and spinning motor, adjust sputtering power to 2.2w/cm
2, sputter 5min, rotating speed and distance values remain unchanged, preparation Si
xN
yFilm is as anti-reflection layer.
Claims (3)
1. a double absorption layer TiON weatherability photo-thermal coating is characterized in that, as base material, is followed successively by Ti film infrared reflecting layer, TiON film the first absorption subgrade, TiON film the second absorption subgrade, Si with copper, aluminium or ferritic stainless steel
xN
yThe film anti-reflection layer, Ti film infrared reflecting layer is controlled at 50-100nm, and TiON film first absorbs the subgrade THICKNESS CONTROL at 50-150nm, and TiON film second absorbs the subgrade THICKNESS CONTROL at 50-150nm, Si
xN
yFilm anti-reflection layer THICKNESS CONTROL is at 20-60nm.
2. a kind of double absorption layer TiON weatherability photo-thermal coating according to claim 1 is characterized in that, with ferritic stainless steel as base material.
3. the preparation method of a double absorption layer TiON weatherability photo-thermal coating comprises that step is as follows:
(1) first base material is carried out surface clean, then in vacuum chamber, utilize BP unipolar pulse grid bias power supply that base material is carried out reverse sputtering and clean, activate by Ions Bombardment;
(2) argon gas of injection flow 35-45sccm, pressure remains on 0.5-1pa, and adjust revoluting motor matrix is in over against the position of metal Ti target, sputter 10min, rotating speed 15r/min, spacing 10cm, d.c. sputtering power are 2.2-2.5w/cm
2
(3) adopt the metal Ti target, when passing into 35-45sccm Ar gas, the injection flow is that nitrogen and the flow of 5-9sccm is the oxygen of 1-4sccm, and power remains on 2.2-2.5w/cm
2, first reactive sputtering 10min; The adjustment nitrogen flow is 9-15sccm, oxygen flow 3-5sccm, and power remains on 2.2-2.5w/cm
2Keep dc source and spinning motor in opening, reactive sputtering 10min again, rotating speed and spacing remain unchanged;
(4) base material is in over against the position of conduction Si target, when passing into 35-45sccm Ar gas, regulate nitrogen flow to 15-25sccm, oxygen flow to 0sccm, open Si target dc source and spinning motor, adjust sputtering power to 1.7-2.2w/cm
2, sputter 5min, rotating speed and distance values remain unchanged.
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Cited By (6)
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| CN104505436A (en) * | 2014-12-18 | 2015-04-08 | 福建新越金属材料科技有限公司 | Selective solar heat absorption coating with low emission ratio and preparation method for selective solar heat absorption coating |
| CN104930735A (en) * | 2015-03-24 | 2015-09-23 | 江苏奥蓝工程玻璃有限公司 | Solar absorbing film and preparation method thereof |
| CN105698416A (en) * | 2016-03-01 | 2016-06-22 | 江苏贝德莱特太阳能科技有限公司 | Selective solar absorbing coating for flat-plate solar collector |
| CN109651853A (en) * | 2018-12-04 | 2019-04-19 | 哈尔滨工业大学（深圳） | Stable MoSi in a kind of high temperature air2-SiO2Compound photo-thermal coating and preparation method thereof |
| TWI659118B (en) * | 2018-06-06 | 2019-05-11 | 國立中興大學 | Solar absorption device |
| CN110595084A (en) * | 2019-10-11 | 2019-12-20 | 中国科学院兰州化学物理研究所 | Metal gradual-change high-temperature solar energy absorption coating and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104505436A (en) * | 2014-12-18 | 2015-04-08 | 福建新越金属材料科技有限公司 | Selective solar heat absorption coating with low emission ratio and preparation method for selective solar heat absorption coating |
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| CN109651853A (en) * | 2018-12-04 | 2019-04-19 | 哈尔滨工业大学（深圳） | Stable MoSi in a kind of high temperature air2-SiO2Compound photo-thermal coating and preparation method thereof |
| CN110595084A (en) * | 2019-10-11 | 2019-12-20 | 中国科学院兰州化学物理研究所 | Metal gradual-change high-temperature solar energy absorption coating and preparation method thereof |
| CN110595084B (en) * | 2019-10-11 | 2021-08-24 | 中国科学院兰州化学物理研究所 | Metal gradual-change high-temperature solar energy absorption coating and preparation method thereof |
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Effective date of registration: 20201222 Address after: 246001 e-commerce Industrial Park, NO.48 Renmin Road, Yingjiang District, Anqing City, Anhui Province Patentee after: Wang Zhao Address before: 250061 Qianfo campus, Shandong University, 17923 Jingshi Road, Lixia District, Jinan City, Shandong Province Patentee before: OuYang Jun |
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