CN1185363C - Metal ceramic film - Google Patents
Metal ceramic film Download PDFInfo
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- CN1185363C CN1185363C CN 01136648 CN01136648A CN1185363C CN 1185363 C CN1185363 C CN 1185363C CN 01136648 CN01136648 CN 01136648 CN 01136648 A CN01136648 A CN 01136648A CN 1185363 C CN1185363 C CN 1185363C
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E10/40—Solar thermal energy, e.g. solar towers
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Abstract
The present invention discloses a metal nitride/oxide ceramic film, a production method and device thereof, and a high-temperature resistant solar heat collecting pipe containing the metal nitride/oxide ceramic film. The metal nitride or oxide ceramic film is a multilayer composite film, wherein metal Nb/Ti and alloy groups thereof are embedded in the multilayer composite film. The preparation method comprises: a metal nitride or oxide film and an Nb/Ti group layer are alternatively formed on a substrate by magnetron sputtering, wherein the metal nitride/oxide is prepared from metal by sputtering under the existence of argon and nitrogen/O2, and the Nb/Ti group layer is prepared from metal Nb/Ti and alloys thereof by sputtering under the existence of argon.
Description
The present invention relates to a kind of nitride or oxide cermets film and manufacture method thereof, more particularly, the nitride or the oxide cermets film that relate to the nanocluster that is embedded with refractory metal Nb, Ti, this film has optionally absorption spectrum, can be used as optical thin film and solar selectively absorbing membrane.
The solar selectively absorbing coating that industry at present in enormous quantities is produced mainly is the mixture of aluminium (Al) and aluminium nitride (AlN), metallic aluminium is distributed in the metal aluminum nitride pottery according to the ratio of setting, prepare the multilayer film of selected thickness, this composite membrane has the selectivity absorptive character to 300nm to infrared light, have intensive in the solar radiation zone and absorb, and be full impregnated ir radiation.The composite membrane of said aluminium (Al) and aluminium nitride (AlN) generally is mainly used in the domestic hot water device because of not having high high-temp stability.
Except that the composite membrane of above-mentioned aluminium (Al) and aluminium nitride (AlN), people have also developed laminated films such as chromic oxide, chromium-nitrogen, chromium-carbon, titanium-nitrogen, titanium-carbon, titanium-nitrogen-carbon, zirconium-nitrogen-carbon, nickel-carbon, nickel-nitrogen, molybdenum-carbon, stainless steel-carbon for many years, though wherein have and severally be used to commercially produce as the solar energy heating coating, but because problem such as manufacturing process is complicated and cost is too high is unsuitable for being extensive use of.Absorbing membranous layer with high-temperature stability has metal-Al
2O
3And metal-SiO
2Mixture, though this material has been used to commercially produce, owing to reasons such as preparation method's complexity, it costs an arm and a leg.
In addition, the application people is in No. 96102331.7 Chinese patent application specification sheets of University of Sydney, Australia, discloses a kind of solar energy selective absorption surface coating and manufacture method thereof.Specifically, a kind of sputtering method of employing two target electrodes is disclosed, this method is included under the existence of at least a reactant gases, make the reaction of a target electrode and reactant gases, another target electrode has adopted non-reacting metal, not with the reactant gases effect, the sputter simultaneously of two target electrodes forms solar selectively absorbing coating.Wherein with the target electrode aluminium or the magnesium of reactant gases reaction, another electrode can be selected: tungsten, tungstenalloy, stainless steel, nickel, nickelalloy, each gold of nickel chromium triangle, platinum, iridium, starve, ruthenium, rhodium, rhenium, molybdenum, molybdenum alloy and gold.Temperature or high temperature modification solar energy decalescence films during this invention can be produced.In warm cast adopted low-cost stainless steel, but the suitable solar energy heat collection pipe of production prices.For the high temperature modification pipe, the metallic substance that is adopted costs an arm and a leg, and preparation difficulty, and for example, though though tungsten is extraordinary material as the high temperature pipe, it smelts difficult, and the technical difficulty that makes target is very big, so fail industrialization so far.
It is known for those of ordinary skill in the art that nitride or oxide cermets have excellent optical property, for example TiO
2, AlN, Al2O
3, TiN etc. all has specific separately optical property.Picture TiO
2Film is to the outer photoabsorption of purple light, and visible light can pass through, and purified AlN film is transparent to visible light.
The inventor is through concentrating on studies, each have specific spectrum property though find nitride or oxide cermets film, but, pass through particular processing, for example adopt to mix, ion implantation, means such as element that the cluster embedding is selected, can change the optical property of metallic cermet films, to satisfy the needs of specific end use.Realized the present invention thus.
The object of the invention is to provide a kind of composite cermet film with good thermal stability.
Another purpose of the present invention is to provide a kind of preparation method with composite cermet film of good thermal stability.
Another purpose of the present invention is to provide a kind of device of making nitride or oxide cermets film.
Another purpose of the present invention is to provide a kind of solar energy heat collection pipe with composite cermet film of good high high-temp stability.
In order to reach the foregoing invention purpose, the invention provides following technical proposal:
A kind of nitride or oxide cermets film is characterized in that said metallic cermet films is a kind of multi-layer compound film, wherein is embedded with the cluster of Nb or Ti metal or its alloy.Said metal nitride or oxide compound are aluminium nitride or aluminum oxide.The first layer of said multi-layer compound film and last one deck are metal nitride or oxide skin.Every layer thickness is in tens to tens nanometer range in the said multi-layer compound film.
The manufacture method of a kind of nitride or oxide cermets film, this method is included on the substrate and alternately forms metal nitride or thin oxide layer and Nb or Ti cluster layer respectively by magnetron sputtering, wherein said metal nitride or oxide compound are that the reactive sputtering by aluminium is formed in the presence of argon gas and nitrogen or oxygen, said Nb or Ti cluster layer in the presence of argon gas by sputter Nb or Ti metal and alloy formation thereof.Wherein at first be metal nitride or oxide skin with the last thin layer that forms.Wherein said metal is an aluminium, and said metal nitride or oxide compound are aluminium nitride or aluminum oxide.
A kind of device of making nitride or oxide cermets film, this device comprises a sputter vacuum chamber that two target electrodes are set, in wherein said two target electrodes, one is the aluminium target, another is Nb or Ti target, these two target electrodes lay respectively at the both sides in the vacuum chamber, be provided with the metal titanium isolated screen between two target electrodes, there is certain space between this isolated screen and the vacuum-chamber wall, so that sample pipe or substrate pass through, all there is argon gas to feed in said two branch target chambers, the nitrogen access tube is positioned at metallic aluminium target sputtering chamber, and as far as possible away from Nb or Ti target sputtering chamber, so that substrate is between metallic target and nitrogen access tube.
A kind of solar energy heat collection pipe of the composite cermet film with good high high-temp stability with the aforesaid method manufacturing, this solar energy heat collection pipe comprises the metal aluminium lamination, Nb and/or Ti layer and aluminium nitride antireflection layer.
Specifically, the present invention selects metal niobium and/or titanium for use, adopts magnetron sputtering technique to carry out the nanocluster embedding method, and the intrinsic optical property of AlN metallic cermet films is carried out modification, make it have good thermostability, to satisfy the requirement that absorbs solar energy film as selectivity.
The metallic cermet films that bag reason Nb, Ti provided by the present invention roll into a ball a small bundle of straw, etc. for silkworms to spin cocoons on has been selected for use and the different moiety of various films of the prior art, and is embedded with Nb, Ti metal, makes the composite cermet film have good thermostability.In addition because Nb, Ti and nitrogen can react in sputter procedure, for guarantee to produce purified Nb as far as possible, the Ti metal is rolled into a ball a small bundle of straw, etc. for silkworms to spin cocoons on, should be noted that selecting for use of isolation between target chamber and polymeric barrier layer materials in the preparation.
The method for preparing the metallic cermet films of embedding Nb of the present invention, Ti metal group a small bundle of straw, etc. for silkworms to spin cocoons on has multiple, ion beam sputtering entrapping method for example, many targets of multicell magnetic control dc sputtering etc.Because it is adopt the ionic fluid embedding method, with high costs and do not have a practicality.The present invention adopts magnetron sputtering technique to carry out the method for AlN nano thin-film embedding metal nano group a small bundle of straw, etc. for silkworms to spin cocoons on, and this method comprises:
Select Nb, Ti generation material as metal group a small bundle of straw, etc. for silkworms to spin cocoons on of embedding, and the target electrode that Nb or Ti metal are used as sputter, adopt magnetic control d.c. sputtering technology, under Ar gas work atmosphere, with Ar ion bombardment target material surface with certain energy, atom or atomic group a small bundle of straw, etc. for silkworms to spin cocoons on of Nb or Ti are sputtered out, constantly deposit on the base material.
Selecting metal A l as target electrode, is Ar gas at working gas, and reactant gases is under the condition of nitrogen, carries out the magnetic control d.c. sputtering and generate purified AlN film on base material.In conjunction with above-mentioned two kinds of steps, carry out the composite cermet film that repeatable operation can wherein be embedded with Nb or Ti and alloy cluster thereof, the composite cermet film that obtains comprises the metal aluminium lamination, Nb and/or Ti layer and aluminium nitride antireflection layer.Every layer thickness of said composite cermet film is tens to tens nanometers.
In order to produce purified Nb, Ti metal group a small bundle of straw, etc. for silkworms to spin cocoons on, do not wish at Nb, the gas that responds in the Ti sputter procedure exists, in sputtering equipment, be provided with two vacuum chambers for this reason, be respectively the sputtering chamber of Al target and the sputtering chamber of Nb or Ti target, two sputtering chambers are supplied with Ar gas simultaneously, Al target sputtering chamber also will be supplied with N gas, the surface of this print reactive sputtering in Al target sputtering chamber generates skim AlN (nanometer scale), print is delivered in vacuum chamber in the sputtering chamber of Nb or Ti target then, one deck Nb that sputter generates, the Ti nanocluster is attached on the AlN film, then print is sent Al target sputtering chamber again back to, prepare the AlN film again, the sputtering chamber of again print being delivered to Nb or Ti target then prepares Nb, Ti nanocluster layer continues to come and go according to the method, makes needed composite film at last.
At different practical application request, need carry out the adjustment of thickness, the adjustment of embedding metal group a small bundle of straw, etc. for silkworms to spin cocoons on component to this composite film, the thickness of different layers and metal group a small bundle of straw, etc. for silkworms to spin cocoons on component are adjustable.For example to prepare the solar selectively absorbing membrane, according to present commodity design, need substrate that the layer of metal reflective coating is arranged, on this layer reflecting layer, prepare absorbing membranous layer, prepare one deck deflection surfaces coating at last on absorbing membranous layer, this last one deck can be selected AlN for use.The intermediary absorbing membranous layer can be used the metallic cermet films of embedding Nb, Ti metal group a small bundle of straw, etc. for silkworms to spin cocoons on.
In order in mass production, to improve production rate and to reduce product cost, can simplify the inventive method, form preferred embodiment.Promptly, at a sputter vacuum chamber, two target electrode (Al have been installed, Nb or Ti), lay respectively at the both sides of vacuum chamber, the isolated screen that one metal titanium is arranged between two targets, isolated screen is with sputter vacuum chamber separated into two parts, leave a fixed gap between isolated screen and vacuum-chamber wall, allow that print or Glass tubing pass through between the space, this might make a spot of reaction gas originally be leaked in Nb or the Ti target sputtering chamber, and argon gas feeds in the middle of two targets, can supply with two sputtering chamber argon gas simultaneously, nitrogen tube is positioned at Al target sputtering chamber, and as far as possible away from Nb or Ti sputtering chamber, nitrogen tube is positioned at outside the sputter print (or solar energy glass pipe), that is to say the print (or Glass tubing) between Al target and tracheae, nitrogen partial pressure is little, adjust an amount of, but with AL target adequate reaction, the amount that leaks to another sputtering chamber by the gap is very little, can guarantee Nb or Ti target works better so substantially, even remaining nitrogen and Nb or Ti target response are arranged, its nitrogenize resultant does not influence the performance of film.Buffer action is played in the shielding of intermediary titanium metal, can adsorb nitrogen when work, and is favourable to isolating nitrogen.
Description of drawings:
Fig. 1 is the three target magnetic control sputtering schematic representation of apparatus that adopt among the present invention.This device is by vacuum chamber 13, vacuum pump group 12 (mechanical pump, molecular pump, push-pull valve are formed), three magnetic control planar targets 8,9,11, sputter is overlapped mass flowmeters 1, working gas 2 with constant current power supply 10, two, reactant gases 3, print support and well heater 4, print rotating mechanism 5, compositions such as baffle plate 6 and sample substrate 7.
Fig. 2 is the diagrammatic cross-section of the manufacturing installation of high temperature resistant solar energy heat collection pipe of the present invention.Wherein 20 is vacuum chamber, and 18 is the aluminium target, and 17 is the niobium target, and 15 is the target protection screen, the 16th, and Glass tubing, the 19th, the shielding of titanium plate, 14 is the argon gas input channel, 22 is the nitrogen input channel, the 21st, rotary bracket.23 and 24 is two constant current power supplies.
Fig. 3 is the schematic cross-section of the manufacturing installation of high temperature resistant solar energy heat collection pipe of the present invention.Wherein identical among the implication of symbol and Fig. 2.
The present invention is described in detail below by following examples, but scope of the present invention is not limited to this.
Embodiment 1.
Adopt three target magnetic control sputtering devices shown in Figure 1 can make the metallic cermet films of embedding Nb of the present invention, Ti group a small bundle of straw, etc. for silkworms to spin cocoons on.
Specifically, substrate 7 can be selected sheet glass or tinsel for use, will clean before installing, and system vacuum is evacuated to 3 * 10 after installing substrate
-3Pa sends into argon gas (Ar) through mass flowmeter 1 then, regulates push-pull valve simultaneously, and when argon flow amount was 10sccm, the vacuum tightness of vacuum chamber was 9 * 10
-1Pa after tolerance mixes up, connects sputter with constant current power supply 10, positive source ground connection, and link to each other with substrate, power cathode is connected with target.Three targets are respectively Al target 8, Nb target 9, Ti target 11, and the distance of target and substrate is 5-7cm, and every target has power supply separately.First operation Al target, the preparation aluminium nitride film is sent into nitrogen (N) through a mass flowmeter, and nitrogen flow is 1-4sccm, and its flow size is regulated according to the generation situation of metal ceramics thin film, sputtering current 200mA, voltage 280V, sputtering time 7 minutes.Close the aluminium target power supply behind sputter one deck aluminium nitride, and off-response gas nitrogen, only keep partial pressure of ar gas, connect the shielding power supply of niobium target (or titanium target), beginning sputter niobium, group's a small bundle of straw, etc. for silkworms to spin cocoons on of embedding niobium on the aluminium nitride film that has prepared, sputtering current 200mA at this moment, voltage 350V, sputtering time 4 minutes is (if select titanium metal for use, electric current is 120mA, voltage 350V, sputtering time 2min).After niobium (or titanium) sputter is finished, and close the niobium target power supply, open the nitrogen mass flowmeter, regulate nitrogen partial pressure such as preceding, the sputter aluminium nitride film is opened the nitrogen mass flowmeter again, regulate nitrogen partial pressure such as preceding, sputter aluminium nitride film again, same sputtering time.After this step finishes, sputter niobium again as described above, condition is constant.The repetition that comes and goes successively is 6-10 time like this, film thickness decision number of times as required.Add one deck aluminium nitride film at last, thickness is thicker, the about 15-20 of sputtering time minute.After preparation is finished, close gas, close power supply, close the pump group.
Embodiment 2
Adopt Fig. 2 and device preparation shown in Figure 3 to be used for the solar energy heat collection pipe of hot conditions.The selective absorption film of this solar energy heat collection pipe can tolerate 400 ℃ temperature.The specific absorption α of this thermal-collecting tube＞94%, emissivity＜5%.
Specifically, solar energy heat collection pipe of the present invention can be made according to the following steps: will the system of taking out vacuumize and reach 3 * 10
-3Behind the Pa, earlier sputter layer of aluminum (or copper, as increasing a copper target with copper) reflectance coating on Glass tubing 16 during this layer of sputter metallic membrane, need be sent into argon gas earlier, and regulating vacuum tightness is 8 * 10
-1Pa connects shielding power supply 23, and working current 20-30A is in the about 440V of operating voltage, sputtering time 2 minutes.After the reflecting layer prepared, at this moment the preparation of beginning selective absorbing film will feed nitrogen, and nitrogen is micro-, and preparing pure aluminium nitride needs 40-50sccm approximately, regulates according to circumstances, after controlled atmosphere is good, opens two power supplys simultaneously, and aluminium target 18 is started working with 17 starting the arc of niobium target.In the aluminium target chamber, reactive sputtering generates aluminium nitride film on Glass tubing 16, Glass tubing is mounted in to be placed on the carriage 21, it goes to the niobium target chamber by the aluminium target chamber, beginning embedding metal niobium on aluminium nitride film, go to the aluminium target chamber then again and continue to generate aluminium nitride film, the metal ceramics thin film of the continuous preparation embedding niobium cluster of like this going round and beginning again.In this process, the working conditions of aluminium target chamber is constant, its supply current is 24-35A, voltage is about 250-350V, the sputtering condition of niobium target chamber will constantly be regulated, so that obtain to have the aluminium nitride film of different metal content of niobium, its supply current is from 18-14A, be changed to 10-7A, voltage fades to about 350V from 450V.The adjusting of niobium target current voltage determines according to film layer structure, if select graded films for use, and the niobium metal content gradual change from high to low in the aluminium nitride film, therefore, what electric current and voltage can gradual changes diminishes.If select double membrane structure, the first layer is the aluminium nitride film of high metal content, and the second layer is the rete of low-metal content, and the electric current of the first layer is decided to be 18-14A, relevant voltage about 450V, second layer electric current 10-7A, relevant voltage is about 350V.The about 10-15 of the preparation time of this layer metal ceramics thin film minute, decide on size of current.After finishing this step, close the niobium target power supply.Beginning sputter one deck aluminium nitride antireflective coating, about 10-15 of time minute.After sputter is intact, powered-down, close gas circuit.
Effect of the present invention
Composite cermet film of the present invention and since therein embedding the refractory metal niobium and/or The nanocluster of titanium has improved the high-temperature stability of composite cermet film, tool widely Body ground says that composite cermet film of the present invention has good under 400 ℃ high temperature Stability. By adopting method and apparatus of the present invention, so that high temperatures is good Composite cermet film and high temperature resistant solar energy heat collection pipe create possibility, improving In the time of properties of product, reduced production cost.
Claims (7)
1. the nitride of an aluminium or oxide cermets film is characterized in that, this metallic cermet films is a kind of multi-layer compound film, wherein are embedded with Nb, Ti metal or its alloying element.
2. the nitride of aluminium as claimed in claim 1 or oxide cermets film, wherein the first layer of said multi-layer compound film and last one deck are aluminium nitride or alumina layer.
3. the nitride of the aluminium described in claim 1 or 2 or oxide cermets film is characterized in that, in the said multi-layer compound film every layer thickness several in tens nanometer range.
4. the manufacture method of the nitride of an aluminium or oxide cermets film, this method is included on the substrate by magnetron sputtering and alternately forms the nitride of aluminium or thin oxide layer and Nb, Ti cluster layer, wherein the nitride of said aluminium or oxide compound form by the sputtered aluminum metal in the presence of argon gas and nitrogen or oxygen, and said Nb or Ti cluster layer form by sputter Nb, Ti metal or its alloy in the presence of argon gas.
5. the manufacture method of the nitride of aluminium as claimed in claim 4 or oxide cermets film, wherein at first and the last thin layer that forms be the nitride or the oxide skin of aluminium.
6. make the nitride of aluminium or the device of oxide cermets film for one kind, this device comprises a sputter vacuum chamber that two target electrodes are set, in wherein said two target electrodes, one is the aluminium target, another is Nb or Ti target, these two target electrodes lay respectively at the both sides in the vacuum chamber, be provided with the metal titanium isolated screen between two target electrodes, there is certain space between this isolated screen and the vacuum-chamber wall, be able to substrate and pass through, all be provided with the argon gas access tube in said two target electrodes, the nitrogen access tube is positioned at the metallic target sputtering chamber, and as far as possible away from Nb or Ti target sputtering chamber, so that substrate is between metallic target and nitrogen access tube.
7. a high temperature resistant solar energy heat collection pipe is characterized in that its top coat comprises the metal aluminium lamination, Nb and/or Ti layer and aluminium nitride antireflection layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01136648 CN1185363C (en) | 2001-10-25 | 2001-10-25 | Metal ceramic film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01136648 CN1185363C (en) | 2001-10-25 | 2001-10-25 | Metal ceramic film |
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| CN1414133A CN1414133A (en) | 2003-04-30 |
| CN1185363C true CN1185363C (en) | 2005-01-19 |
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| CN 01136648 Expired - Fee Related CN1185363C (en) | 2001-10-25 | 2001-10-25 | Metal ceramic film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012544B (en) * | 2007-03-02 | 2010-11-03 | 殷志强 | Thin film of nichrome-chromium-aluminium-yttrium-nitrogen-oxygen material |
| CN101854131B (en) * | 2009-04-01 | 2012-10-03 | 中国科学院金属研究所 | High-temperature-resistant selective solar energy-absorbing film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4953278B2 (en) * | 2006-03-08 | 2012-06-13 | 三菱マテリアル株式会社 | Hydrogen permeation separation thin film with excellent hydrogen permeation separation performance |
| CN101298659B (en) * | 2007-04-30 | 2010-12-01 | 汉达精密电子(昆山)有限公司 | Manufacturing method of insulation heat-conducting metal substrate |
| CN101182132B (en) * | 2007-11-27 | 2010-12-15 | 日出东方太阳能股份有限公司 | Low-temperature solar energy selective absorption coating and preparation method thereof |
| CN101572996B (en) * | 2008-04-29 | 2011-12-07 | 汉达精密电子(昆山)有限公司 | Method for forming conducting wire on insulated heat-conducting metal substrate in a vacuum sputtering way |
| CN101839575B (en) * | 2010-03-25 | 2012-10-10 | 常州龙腾太阳能热电设备有限公司 | Inner tube suitable for trench type thermal-collecting tube of solar thermal power generation and film coating method thereof |
| CN102534497A (en) * | 2012-03-29 | 2012-07-04 | 德州金亨新能源有限公司 | High temperature selective absorption coating based on stainless steel material and manufacture method thereof |
| CN103343317A (en) * | 2013-07-11 | 2013-10-09 | 南京大学 | Preparation method of TiO2 nanoparticle antireflective film based on nanocluster beam deposition system |
| KR20160092357A (en) * | 2015-01-27 | 2016-08-04 | 삼성전자주식회사 | Amorphous and nano nitride composite thin film, method for forming the same and electronic divice with the same |
-
2001
- 2001-10-25 CN CN 01136648 patent/CN1185363C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012544B (en) * | 2007-03-02 | 2010-11-03 | 殷志强 | Thin film of nichrome-chromium-aluminium-yttrium-nitrogen-oxygen material |
| CN101854131B (en) * | 2009-04-01 | 2012-10-03 | 中国科学院金属研究所 | High-temperature-resistant selective solar energy-absorbing film and preparation method thereof |
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| CN1414133A (en) | 2003-04-30 |
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