CN101570846B - Method using ion nitriding technology to prepare solar energy absorbing coating - Google Patents
Method using ion nitriding technology to prepare solar energy absorbing coating Download PDFInfo
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- CN101570846B CN101570846B CN2009100743535A CN200910074353A CN101570846B CN 101570846 B CN101570846 B CN 101570846B CN 2009100743535 A CN2009100743535 A CN 2009100743535A CN 200910074353 A CN200910074353 A CN 200910074353A CN 101570846 B CN101570846 B CN 101570846B
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- ion nitriding
- solar energy
- aluminium
- energy absorbing
- absorbing coating
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S70/00—Details of absorbing elements
- F24S70/20—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption
- F24S70/25—Coatings made of metallic material
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S70/00—Details of absorbing elements
- F24S70/20—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption
- F24S70/225—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption for spectrally selective absorption
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/40—Solar thermal energy, e.g. solar towers
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- Chemical & Material Sciences (AREA)
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- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The invention relates to a method using an ion nitriding technology to prepare a solar energy absorbing coating. In the method, an aluminum alloy tube is used as a cathode, and a gradually-varied aluminum nitride/aluminum (A1N-A1) solar energy absorbing coating with compositional gradient change is formed on the surface of the aluminum alloy tube by utilizing the ion nitriding technology. The method introduces a graphite source, enhances the heat absorbing efficiency of an aluminum nitride coating, increases solar absorbing efficiency and has the advantages of high seeping speed, uniform seeping layer, simple equipment, low cost, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of solar energy absorbing coating, specifically is a kind of using ion nitriding technology carries out solar energy absorbing coating on the aluminium-alloy pipe surface preparation method.
Background technology
" solar energy journal " that China renewable energy source association sponsors, January calendar year 2001, openly reported to have introduced in " complete glass vacuum sun thermal-collecting tube light-thermal characteristics " and on borosilicate glass 313 (BJ2TY), preset aluminium film bottom, utilize single target magnetic control sputtering technology to prepare gradual change aluminium-nitrogen laminated film and be absorption layer, aluminium-oxygen medium film is the solar energy absorbing coating technology of anti-reflection layer.Wherein, the specific absorption α of multilayer (gradual change) AlN/Al coating for selective absorption can reach 0.93, and reflectivity ε is about 0.05.The all-glass vacuum thermal-collecting tube of multilayer (gradual change) AlN/Al selective absorbing film is 900W/m in solar radiation
2The time, the empty temperature of shining reaches 270 ℃ in the thermal-collecting tube.
" the material heat treatment journal " that Chinese Mechanical Engineering Society sponsors, in August, 2008, openly reported to have introduced in " preparation of deposit aluminum nitride films and specificity analysis on the aluminium base " and utilized J GP2800 type ultra-high vacuum multifunctional magnetron sputtering equipment, (purity is 991999% to select the rafifinal target for use, Φ 75mm), 6061 aluminium are substrate base, the Ar of purity 99.999% and N
2For working gas prepares the AlN film.Wherein, substrate and Al sheet are through each 1h of grinding and polishing, and acetone ultrasonic cleaning 5min uses washed with de-ionized water again, puts into the sample chamber after nitrogen dries up.Base vacuum is better than 2 * 10 in the reaction chamber
-4Pa feeds Ar earlier the aluminium target is carried out the pre-sputter of 20min before the sputter, to remove oxide on surface, substrate does not heat during sputter.
Aforesaid method is to be substrate with glass or aluminium, utilize the method for magnetron sputtering to prepare aluminium nitride coating, its weak point is that prepared aluminium nitride coating is used for solar energy heat collection pipe and exists warm start slow in use, cost height, apparatus expensive and complicated operation during preparation.
Publication number is the patent of invention of CN1105340, adopt " method that aluminum oxide prepares aluminium nitride is continuously handled in carbonitriding ", carry out the prepared in reaction aluminium nitride with aluminum oxide, carbon, tackiness agent and nitrogen in reactor, this method is difficult to the preparation aluminium nitride film and therefore is difficult to as solar energy absorbing coating.
The contriver is at the solar energy absorbing coating of existing thermal-collecting tube of solar water heater, in conjunction with prior art, proposed to be different from the method that traditional magnetically controlled sputter method prepares the aluminium nitride solar energy absorbing coating, utilize vacuum ionic nitrogenize technology directly to generate aluminium nitride (AlN) coating that one deck has solar absorption function and component gradient variation on the aluminium-alloy pipe surface, because aluminium alloy has good thermal conductivity, aluminium nitride coating can be that heat energy transmits rapidly with the conversion of solar energy that absorbs.If in the vacuum ionic nitridation process, the blackness that Graphite Electrodes can further increase the AlN coating is set, improve the assimilated efficiency of solar energy absorbing coating.Because traditional solar energy absorbing coating aluminium nitride prepares on glass substrate by magnetically controlled sputter method, glass is compared with aluminium alloy, and its thermal conductivity differs greatly.Therefore, utilize ion nitriding technology to prepare solar energy absorbing coating, will improve the utilising efficiency of sun power greatly.
Summary of the invention
The problem to be solved in the present invention is existing solar energy absorbing coating aluminium nitride, on Glass tubing, adopt the magnetically controlled sputter method preparation, warm start is slow in use, used apparatus expensive and complicated operation when making, based on this, the applicant provides a kind of method of using ion nitriding technology to prepare solar energy absorbing coating.
The method of using ion nitriding technology to prepare solar energy absorbing coating of the present invention, the pretreatment process that comprises aluminium-alloy pipe, ion nitriding technology, this method is that pretreated aluminium-alloy pipe is inserted in the ion nitriding furnace, feed argon gas, at air pressure is under 20～60Pa, regulating voltage 400～600V, after the sputter clean, feed nitrogen or ammonia again, and after being pressurized to 200～400Pa, control argon gas and nitrogen volume ratio be 0.2～1 or argon gas and ammonia volume ratio be 0.5～1, be 500～800V in operating voltage, working temperature is under 240～500 ℃ ion nitriding to be carried out on the aluminium-alloy pipe surface, be incubated after 1～2 hour, generate the gradual change AlN-Al that component gradient changes, be solar energy absorbing coating on the aluminium-alloy pipe surface.
Further, the method of using ion nitriding technology to prepare solar energy absorbing coating of the present invention is to feed argon gas in being provided with the ion nitriding furnace of Graphite Electrodes, at air pressure is 40Pa, voltage is under the 550V after the sputter clean, feed nitrogen again, the volume ratio of control argon gas and nitrogen is 0.4, be pressurized to 400Pa, the adjusting voltage of supply is 700V, regulates graphite pole tension 500V, and keeping temperature is 450 ℃, ion nitriding is carried out on the aluminium-alloy pipe surface, be incubated 1 hour, generate the gradual change AlN-Al that component gradient changes, be solar energy absorbing coating on the aluminium-alloy pipe surface.
Further, the method of using ion nitriding technology to prepare solar energy absorbing coating of the present invention is to feed argon gas in being provided with the ion nitriding furnace of Graphite Electrodes, at air pressure is 30Pa, voltage is under the 450V after the sputter clean, feed ammonia again, the volume ratio of control argon gas and ammonia is 1.0, be pressurized to 350Pa, the adjusting voltage of supply is 650V, regulates graphite pole tension 400V, and keeping temperature is 400 ℃, ion nitriding is carried out on the aluminium-alloy pipe surface, be incubated 1.5 hours, generate the gradual change AlN-Al that component gradient changes, be solar energy absorbing coating on the aluminium-alloy pipe surface.
The present invention's employed Graphite Electrodes in technique scheme is netted, grid-like or flat sponge-type porous graphite electrode.The nitrogen that is fed in ion nitriding furnace is 99.99% high purity nitrogen.
The ion nitriding technology that the present invention will be applied to structured material is introduced the surface modification of aluminium alloy, the vacuum ionic nitriding treatment is carried out on the aluminium-alloy pipe surface after, make the AlN-Al solar energy absorbing coating of the gradual change that component gradient changes; Ion nitriding technology is applied to the preparation of solar energy absorbing coating, has further widened the Application Areas of vacuum ionic nitriding process.
The AlN-Al solar energy absorbing coating of the gradual change of using ion nitriding technology prepared composition graded of the present invention can absorb the more solar spectrum of broadband, and by the test contrast, the specific absorption α of this coating can reach 0.95, and reflectivity ε is about 0.04.
Compared with prior art, all-glass vacuum thermal-collecting tube is to plate multilayer (gradual change) AlN/Al coating for selective absorption on glass substrate, and wherein the heat conduction of AlN is 190W/ (mk), and the thermal conductivity of glass is 0.75W/ (mk); And the thermal conductivity 120-220W/ (mk) of aluminium alloy, the thermal conductivity of aluminium alloy more approaches the thermal conductivity of AlN than glass, in that heat waste is littler at the interface, more helps the conduction of heat in the heat transmission course.
The present invention is at the AlN-Al solar energy absorbing coating of the gradual change of aluminium-alloy pipe surface direct production component gradient variation, aluminium nitride that heat transfer efficiency is higher and aluminum alloy junction are altogether, successfully solved slow this problem of warm start of full-glass solar energy collecting vacuum tube, comprehensively improved the photo-thermal conversion efficiency of solar product, simplify technology simultaneously, reduced production cost.
Description of drawings
Fig. 1 is that AlN-Al of the present invention is coated with the layer cross section scanned photograph
Among the figure: the AlN/Al interface transition zone that can be observed bright diffusion layer and gradual change
Fig. 2 is the composition profiles graphic representation of AlN of the present invention
Among the figure: show that coat-thickness is about 8 μ m, composition changes in gradient
Fig. 3 is the XRD figure spectrum of AlN of the present invention
Among the figure: show that coating has the AlN compound to constitute, and present certain preferred orientation.
Specific embodiment
Below by specific embodiment the specific embodiment of the present invention is further detailed, it will be appreciated by persons skilled in the art that and realize, its described beneficial effect also can reach by specific embodiment.
Embodiment 1
One. at first adopt chemical treatment method, the cleaning aluminum alloy tube-surface makes itself and oil, dirt, rust, dirt, oxide film generation chemical reaction, generates easily molten material, makes pending aluminium-alloy pipe any surface finish.Concrete steps are as follows:
(1) be that 8%-10%, solution temperature are 40 ℃-60 ℃ NaOH solution etch 10-15 minute with aluminium-alloy pipe concentration;
(2) with cold water flush about about 2 minutes;
(3) in volume fraction is 30% dilute nitric acid solution, carry out neutralizing treatment, make the aluminium-alloy pipe any surface finish not have dirt;
(4), and use the scrub-brush outwash with 50 ℃～60 ℃ hot water injections 2～3 minutes;
(5) insert in 100 ℃～150 ℃ loft drier about 30 minutes of oven dry, stand-by.
Two. to aluminium-alloy pipe surface ion nitriding treatment
1. shove charge: with the two ends shutoff of pretreated aluminium-alloy pipe, on the machine frame of paperback in ion nitriding furnace;
2. pre-treatment: handle carrying out evacuation in the ion nitriding furnace, and charge into argon gas, carry out repeatedly 3 times, to reduce impurity in the stove, again the stove internal gas pressure is upgraded to 25Pa, regulating voltage 600V, bombard the aluminium-alloy pipe surface, reach the purpose of cleaning and activating aluminum alloy tube-surface.
3. heat up: regulate in the ion nitriding furnace ar pressure and regulate voltage of supply 700V to 50Pa, make temperature in the ion nitriding furnace reach 350 ℃ after, feed 99.99% high pure nitrogen (flow 0.6m again
3/ h), the vacuum ionic nitrogenize is carried out in insulation.
4. insulation: be incubated after 2 hours, slowly regulating voltage is lowered the temperature, after turn off argon gas and nitrogen, vacuumize, and the temperature in the ion nitriding furnace is dropped to room temperature, come out of the stove then, generate the gradual change AlN-Al that component gradient changes on the aluminium-alloy pipe surface, be solar energy absorbing coating.
The aluminium nitride coating that this example makes is not having the photo-thermal transformation efficiency under the condition of vacuum heat-insulating layer to be 86.2% of existing solar vacuum heat-collecting pipe finished product.
According to the method for embodiment 1, in ion nitriding furnace, set up mesh sponge type porous graphite source electrode, ion Plasma Nitriding Treatment is carried out on the aluminium-alloy pipe surface.After temperature is raised to 350 ℃, regulate graphite pole tension 400V, carry out ion nitriding, be incubated 2 hours.Slow cooling is come out of the stove, and generates the gradual change AlN-Al that component gradient changes on the aluminium-alloy pipe surface, is solar energy absorbing coating.
The aluminium nitride coating that this example makes is not having the photo-thermal transformation efficiency under the condition of vacuum heat-insulating layer to be 92.4% of existing solar vacuum heat-collecting pipe finished product.
Embodiment 3
According to the method for embodiment 1, in ion nitriding furnace, set up grid-like sponge-type porous graphite electrode, ion Plasma Nitriding Treatment is carried out on the aluminium-alloy pipe surface.At air pressure is 40Pa, voltage is under the 550V after the sputter clean, feeds 99.99% high pure nitrogen again, and the volume ratio of control argon gas and nitrogen is 0.4, be pressurized to 400Pa, the adjusting voltage of supply is 700V, regulates graphite pole tension 500V, and keeping temperature is 450 ℃, ion nitriding is carried out on the aluminium-alloy pipe surface, be incubated 1 hour, generate the gradual change AlN-Al that component gradient changes, be solar energy absorbing coating on the aluminium-alloy pipe surface.
The aluminium nitride coating that this example makes is not having the photo-thermal transformation efficiency under the condition of vacuum heat-insulating layer to be 91.6% of existing solar vacuum heat-collecting pipe finished product.
According to the method for embodiment 1, in ion nitriding furnace, set up flat sponge-type porous graphite electrode, ion Plasma Nitriding Treatment is carried out on the aluminium-alloy pipe surface.At air pressure is 30Pa, voltage is under the 450V after the sputter clean, feeds ammonia again, and the volume ratio of control argon gas and ammonia is 1.0, be pressurized to 350Pa, the adjusting voltage of supply is 650V, regulates graphite pole tension 400V, and keeping temperature is 400 ℃, ion nitriding is carried out on the aluminium-alloy pipe surface, be incubated 1.5 hours, generate the gradual change AlN-Al that component gradient changes, be solar energy absorbing coating on the aluminium-alloy pipe surface.
The aluminium nitride coating that this example makes is not having the photo-thermal transformation efficiency under the condition of vacuum heat-insulating layer to be 90.8% of existing solar vacuum heat-collecting pipe finished product.
Claims (5)
1. the method for a using ion nitriding technology to prepare solar energy absorbing coating, the pretreatment process that comprises aluminium-alloy pipe, ion nitriding technology, it is characterized in that pretreated aluminium-alloy pipe is inserted in the ion nitriding furnace, feed argon gas, at air pressure is under 20～60Pa, regulating voltage 400～600V, after the sputter clean, feed nitrogen or ammonia again, after being pressurized to 200～400Pa, control argon gas and nitrogen volume ratio be 0.2～1 or argon gas and ammonia volume ratio be 0.5～1, be 500～800V in operating voltage, working temperature is under 240～500 ℃ ion nitriding to be carried out on the aluminium-alloy pipe surface, be incubated after 1～2 hour, generate the gradual change AlN-Al that component gradient changes, be solar energy absorbing coating on the aluminium-alloy pipe surface.
2. the method for the described using ion nitriding technology to prepare solar energy absorbing coating of claim 1, it is characterized in that in being provided with the ion nitriding furnace of Graphite Electrodes, feeding argon gas, at air pressure is 40Pa, voltage is under the 550V after the sputter clean, feed nitrogen again, the volume ratio of control argon gas and nitrogen is 0.4, be pressurized to 400Pa, the adjusting voltage of supply is 700V, regulates graphite pole tension 500V, and keeping temperature is 450 ℃, ion nitriding is carried out on the aluminium-alloy pipe surface, be incubated 1 hour, generate the gradual change AlN-Al that component gradient changes, be solar energy absorbing coating on the aluminium-alloy pipe surface.
3. the method for the described using ion nitriding technology to prepare solar energy absorbing coating of claim 1, it is characterized in that in being provided with the ion nitriding furnace of Graphite Electrodes, feeding argon gas, at air pressure is 30Pa, voltage is under the 450V after the sputter clean, feed ammonia again, the volume ratio of control argon gas and ammonia is 1.0, be pressurized to 350Pa, the adjusting voltage of supply is 650V, regulates graphite pole tension 400V, and keeping temperature is 400 ℃, ion nitriding is carried out on the aluminium-alloy pipe surface, be incubated 1.5 hours, generate the gradual change AlN-Al that component gradient changes, be solar energy absorbing coating on the aluminium-alloy pipe surface.
4. the method for claim 2 or 3 described using ion nitriding technology to prepare solar energy absorbing coating is characterized in that Graphite Electrodes is netted, grid-like or flat sponge-type porous graphite electrode.
5. the method for the described using ion nitriding technology to prepare solar energy absorbing coating of claim 1 is characterized in that the nitrogen that feeds in the ion nitriding furnace is 99.99% high purity nitrogen.
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| CN2009100743535A CN101570846B (en) | 2009-05-12 | 2009-05-12 | Method using ion nitriding technology to prepare solar energy absorbing coating |
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| CN2009100743535A CN101570846B (en) | 2009-05-12 | 2009-05-12 | Method using ion nitriding technology to prepare solar energy absorbing coating |
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| CN101570846B true CN101570846B (en) | 2010-12-01 |
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| CN109695966B (en) * | 2019-01-18 | 2020-11-10 | 河北赛特驰实验器材销售有限公司 | New application of selective light absorption material and novel photo-thermal system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100142B (en) * | 1985-04-01 | 1987-07-22 | 清华大学 | Sputtered solar selective absorbing coating and its mfg |
| CN1013589B (en) * | 1986-07-21 | 1991-08-21 | 哈尔滨工业大学 | Process for nitriding of aluminium and alloy aluminium |
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2009
- 2009-05-12 CN CN2009100743535A patent/CN101570846B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100142B (en) * | 1985-04-01 | 1987-07-22 | 清华大学 | Sputtered solar selective absorbing coating and its mfg |
| CN1013589B (en) * | 1986-07-21 | 1991-08-21 | 哈尔滨工业大学 | Process for nitriding of aluminium and alloy aluminium |
Non-Patent Citations (4)
| Title |
|---|
| 殷志强，等.渐变Al-N/Al太阳选择吸收表面.《真空科学与技术》.1988,第8卷(第3期),1141-150. |
| 殷志强等.渐变Al-N/Al太阳选择吸收表面.《真空科学与技术》.1988,第8卷(第3期),1141-150. * |
| 金铨，等.铝合金离子渗氮层的组织结构研究.《材料科学与工艺》.1997,第5卷(第1期),24-27. |
| 金铨等.铝合金离子渗氮层的组织结构研究.《材料科学与工艺》.1997,第5卷(第1期),24-27. * |
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Assignee: Zhangjiagang City SunLink PV Co., Ltd. Assignor: Taiyuan University of Technology Contract record no.: 2011320010055 Denomination of invention: Method using ion nitriding technology to prepare solar energy absorbing coating Granted publication date: 20101201 License type: Exclusive License Open date: 20091104 Record date: 20110602 |
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