CN1904127A - Tungsten/iridium composite coating layer for carbon material antioxidation and its preparation method - Google Patents
Tungsten/iridium composite coating layer for carbon material antioxidation and its preparation method Download PDFInfo
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- CN1904127A CN1904127A CN 200610041120 CN200610041120A CN1904127A CN 1904127 A CN1904127 A CN 1904127A CN 200610041120 CN200610041120 CN 200610041120 CN 200610041120 A CN200610041120 A CN 200610041120A CN 1904127 A CN1904127 A CN 1904127A
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- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 title claims abstract description 82
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910052741 iridium Inorganic materials 0.000 title claims abstract description 81
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 44
- 229910052721 tungsten Inorganic materials 0.000 title claims description 78
- 239000010937 tungsten Substances 0.000 title claims description 78
- 239000011247 coating layer Substances 0.000 title claims description 46
- 239000002131 composite material Substances 0.000 title claims description 32
- 238000002360 preparation method Methods 0.000 title claims description 25
- 230000003064 anti-oxidating effect Effects 0.000 title claims description 8
- 239000010410 layer Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims description 29
- 239000011248 coating agent Substances 0.000 claims description 27
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 238000005275 alloying Methods 0.000 claims description 14
- KRQUFUKTQHISJB-YYADALCUSA-N 2-[(E)-N-[2-(4-chlorophenoxy)propoxy]-C-propylcarbonimidoyl]-3-hydroxy-5-(thian-3-yl)cyclohex-2-en-1-one Chemical compound CCC\C(=N/OCC(C)OC1=CC=C(Cl)C=C1)C1=C(O)CC(CC1=O)C1CCCSC1 KRQUFUKTQHISJB-YYADALCUSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 230000008859 change Effects 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 230000007704 transition Effects 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims 1
- 208000002599 Smear Layer Diseases 0.000 abstract 1
- 239000002344 surface layer Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 45
- 229910052799 carbon Inorganic materials 0.000 description 35
- 238000000034 method Methods 0.000 description 17
- 229910002804 graphite Inorganic materials 0.000 description 10
- 239000010439 graphite Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 6
- 230000003078 antioxidant effect Effects 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002574 poison Substances 0.000 description 3
- 231100000614 poison Toxicity 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 206010011376 Crepitations Diseases 0.000 description 1
- IUHFWCGCSVTMPG-UHFFFAOYSA-N [C].[C] Chemical class [C].[C] IUHFWCGCSVTMPG-UHFFFAOYSA-N 0.000 description 1
- IGUHATROZYFXKR-UHFFFAOYSA-N [W].[Ir] Chemical compound [W].[Ir] IGUHATROZYFXKR-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 description 1
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- Physical Vapour Deposition (AREA)
Abstract
This invention relates to a type of carbon material wolfram/iridium smear layer used for antioxygen. The feature is wolfram and carbon material contact directly to form intermediate layer, and iridium and wolfram contact directly to form surface layer.
Description
Technical field
The present invention relates to a kind of tungsten/tungsten/iridium composite coating layer and preparation method thereof, particularly relate to a kind of carbon material anti oxidation tungsten/tungsten/iridium composite coating layer and preparation method thereof.
Background technology
Carbon material comprises graphite simple substance material and carbon/carbon composite, density is little, specific tenacity is big, anti-thermal shock, creep resistance, intensity raises with temperature between 1000 ℃~2200 ℃, is applied in multiple empty day aircraft such as strategic missile bullet, airship return capsule, the space shuttle leading edge of a wing.Yet,, therefore solve the bottleneck that the carbon material anti oxidation problem is the carbon material widespread use because carbon material generates carbon monoxide or carbonic acid gas volatilization promptly reacting with oxidizing atmosphere more than 400 ℃.At present, develop multiple ceramic oxidation resistant coating both at home and abroad, satisfied application demand between the carbon material high temperature, short time.Since the invention sixties in the last century carbon/carbon composite, still there has not been a kind of oxidation resistant coating that carbon/carbon composite is worked long hours in high-temperature oxidation environment.
2443 ℃ of precious metal iridium fusing points have an excellent high temperature oxidation resistance because of saturation steam forces down, oxygen permeability is low, are unique metals that still has good mechanical properties in the air more than 1600 ℃, and are not reacting with carbon below 2280 ℃.Because the excellent antioxidant performance that has of iridium and and carbon do not react, so the carbon-based material surface is applied with iridium coating layer and is become an important channel of improving its antioxidant property.As far back as the sixties in 20th century, the United States Air Force material laboratory is a precursor with iridium halogenide, adopt chemical Vapor deposition process to prepare iridium coating layer at graphite surface, but halogenide precursor volatility is relatively poor, and deposition is low, to equipment and substrate seriously corroded.
In " Journal of Materials Science Letters " the 12nd volume the 18th phase magazine of publishing on September 15th, 1993 " Iridium coatings on carbon-carbon composites produced by two different sputteringmethods:a comparative study " (P1411-1412) literary composition disclose with the method for physical vaporous deposition at carbon/carbon composite surface preparation iridium coating layer.This method is a target plate with the iridium plate, makes the iridium volatilization form steam by electron-bombardment, deposits to the carbon/carbon composite surface, forms iridium coating layer through 1700 ℃ of thermal treatments again.The advantage of this method is that cost is low, and technology is simple; The shortcoming of this method is that iridium coating layer and carbon/carbon composite bonding force are low, and scour resistance is poor, and coatingsurface has crackle, and antioxidant property is also poor.
In " Carbon " the 39th volume the 7th phase magazine of publishing June calendar year 2001 " A novel laser technique foroxidation-resistant coating of carbon-carbon composite " (P991-999) literary composition method for preparing iridium coating layer with the induced with laser chemical thermal decomposition is disclosed.This method is raw material with the iridium chloride, makes its distillation become gaseous state under the high temperature, carries out chemical heat then and decompose under induced with laser, generates iridium and chlorine, and iridium is deposited on the carbon/carbon composite surface and forms iridium coating layer, and the chlorine volatilization is overflowed.The advantage of this method is the iridium coating layer densification, and antioxidant effect is good; The shortcoming of this method is that iridium coating layer and carbon/carbon composite bonding strength are low, and scour resistance is low.
In " solid-rocket technology " the 29th volume the 1st phase magazine of publishing in February, 2006 " mocvd method prepares the microstructure of multilayer iridium coating layer " (P56-59) literary composition method that the organic alkoxide chemical Vapor deposition process of metal prepares iridium coating layer is disclosed.This method is to be raw material with praseodynium iridium, will send into the constant temperature chemical vapor deposition chamber after its distillation, and the thermolysis of praseodynium iridium forms iridium coating layer at charcoal material surface.The advantage of this method is that iridium coating layer is even, can obtain fine and close iridium coating layer by chemical vapour deposition repeatedly; This method shortcoming is the cost height, praseodynium iridium price up to 1100 yuan/gram, and iridium coating layer and charcoal are nonwetting, a large amount of crackles of generation after the pyroprocessing, anti-oxidant scour resistance is low.
Summary of the invention
Technical problem to be solved by this invention provides a kind of carbon material anti oxidation with tungsten/tungsten/iridium composite coating layer, it is characterized in that tungsten and carbon material directly contact the formation middle layer, and iridium directly contacts the formation upper layer with tungsten coating.To the outside gradient transition, metallurgical binding does not have the sudden change of composition and mechanical property to tungsten coating in the carbon material top layer.To the outside gradient transition, metallurgical binding does not have the sudden change of composition and mechanical property to iridium coating layer in the tungsten coating.
Another technical problem to be solved by this invention provides a kind of preparation method of above-mentioned tungsten/tungsten/iridium composite coating layer, it is characterized in that being target plate with the tungsten plate earlier, prepares tungsten coating by the double-deck glow plasma surface alloying at carbon material surface.Be negative electrode with tungsten plate and carbon material in the vacuum glow discharge device, vacuum chamber housing is public anode, between anode and two negative electrodes tunable voltage dc power supply is set respectively.Be evacuated to final vacuum, send into argon gas, light aura, the alloying element particle of source electrode tungsten target is sputtered out, and is deposited on carbon material surface, forms surface alloying layer by High temperature diffusion.And then be that target plate passes through the double-deck glow plasma surface alloying at tungsten coating surface preparation iridium coating layer with the iridium plate.Be negative electrode with iridium plate and the carbon material that has been coated with tungsten in the vacuum glow discharge device, vacuum chamber housing is public anode, between anode and two negative electrodes tunable voltage dc power supply is set respectively.Be evacuated to final vacuum, send into argon gas, light aura, the alloying element particle of source electrode iridium target is sputtered out, and is deposited on the tungsten coating surface, forms surface alloying layer by High temperature diffusion.
Source electrode and negative electrode are equipped with a cover direct supply respectively, and voltage output range is 0~2000V, and adjustable continuously, and two cover power supplys are public anode with the vacuum chamber housing of ground connection.
Discharge air pressure is 13.3~133Pa, and final vacuum is not less than 0.1Pa, source potential-800V~-2000V, the workpiece current potential-200V~-1000V.
Two cathode spacings are 10mm~50mm in the vacuum glow discharge device.
A kind of carbon material anti oxidation tungsten/tungsten/iridium composite coating layer preparation method is characterized in that comprising following sequential steps:
(1) with carbon material 1800~2200 ℃ of pyroprocessing, make in the carbon material volatilization of low melting point impurity, avoid tungsten target in the coating preparation process, iridium target to poison;
(2) tungsten plate and carbon material are packed into vacuum glow discharge device is a negative electrode with tungsten plate and carbon material, and vacuum chamber housing is public anode, and tungsten plate and carbon material spacing are 10mm~50mm;
(3) be evacuated to final vacuum, send into argon gas, light aura, the alloying element particle of source electrode tungsten target is sputtered out, and is deposited on carbon material surface;
(4) cut off the power supply behind the certain hour, the vacuum glow discharge device is opened in inflation;
(5) change the tungsten plate with the iridium plate, adjust iridium plate and carbon material spacing, spacing is 10mm~50mm;
(6) be evacuated to final vacuum, send into argon gas, light aura, the alloying element particle of source electrode iridium target is sputtered out, and is deposited on the tungsten coating surface;
(7) cut off the power supply behind the certain hour, vacuum electric-discharge device is opened in inflation, finishes tungsten/tungsten/iridium composite coating layer preparation.
Major advantage of the present invention is: (1) tungsten coating can penetrate into carbon material inside, and the penetrating layer of formation and carbon material bonding strength height have improved the anti-ablation ability of iridium coating layer; (2) tungsten coating and the carbon material generation wolfram varbide that reacts has improved adhesive force of coatings; (3) Zhi Bei iridium coating layer free of pinholes, finer and close more than the iridium coating layer of physical vapor deposition and chemical vapour deposition, resistance of oxidation is strong; (4) preparation temperature height, iridium coating layer does not shrink in the thermal cycling process, does not crack; (5) iridium coating layer does not have the sudden change at interface from the inner outwards gradient transition of carbon material, does not have stress mutation, and the iridium coating layer thermal shock resistance is good; (6) iridium coating layer and tungsten coating generate high melting compound tungsten iridium by reaction, have improved the bonding force between iridium coating layer and the tungsten coating; (7) technology simple controllable, carbon material physical dimension smooth finish retentivity is good, need not secondary processing; (8) be starting material with the iridium plate, 300~500 yuan of every grams, iridium coating layer output efficiency are 50%, and the metal alkoxide chemical vapour deposition is a raw material with praseodynium iridium, 1500~2000 yuan of every grams, iridium coating layer output efficiency only are 15%, thereby the present invention greatly reduces the iridium coating layer cost.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1 prepares tungsten/tungsten/iridium composite coating layer at graphite surface
(1) with graphite 2000 ℃ of pyroprocessing, make in the graphite volatilization of low melting point impurity, avoid tungsten target in the coating preparation process, iridium target to poison;
(2) tungsten plate and graphite are packed into vacuum glow discharge device is a negative electrode with tungsten plate and graphite, and vacuum chamber housing is public anode, and tungsten plate and graphite spacing are 40mm;
(3) be evacuated to final vacuum, send into argon gas, light aura, the alloying element particle of source electrode tungsten target is sputtered out, and is deposited on graphite surface;
Outage after (4) 10 hours, vacuum electric-discharge device is opened in inflation;
(5) change the tungsten plate with the iridium plate, adjust iridium plate and carbon material spacing to 20mm;
(6) be evacuated to final vacuum, send into argon gas, light aura, the alloying element particle of source electrode iridium target is sputtered out, and is deposited on the tungsten coating surface;
Outage after (7) 20 hours, the vacuum glow discharge device is opened in inflation, finishes graphite surface tungsten/tungsten/iridium composite coating layer preparation.
Embodiment 2 is at carbon/carbon composite surface preparation tungsten/tungsten/iridium composite coating layer
(1) with carbon/carbon composite 1900 ℃ of pyroprocessing, make in the carbon/carbon composite volatilization of low melting point impurity, avoid tungsten target in the coating preparation process, iridium target to poison;
(2) tungsten plate and carbon/carbon composite are packed into vacuum glow discharge device is a negative electrode with tungsten plate and carbon/carbon composite, and vacuum chamber housing is public anode, and tungsten plate and carbon/carbon composite spacing are 35mm;
(3) be evacuated to final vacuum, send into argon gas, light aura, the alloying element particle of source electrode tungsten target is sputtered out, and is deposited on the carbon/carbon composite surface;
Outage after (4) 5 hours, the vacuum glow discharge device is opened in inflation;
(5) change the tungsten plate with the iridium plate, adjust iridium plate and carbon material spacing to 10mm;
(6) be evacuated to final vacuum, send into argon gas, light aura, the alloying element particle of source electrode iridium target is sputtered out, and is deposited on the tungsten coating surface;
Outage after (7) 10 hours, the vacuum glow discharge device is opened in inflation, finishes carbon/carbon composite surface tungsten/tungsten/iridium composite coating layer preparation.
Claims (10)
1. a carbon material anti oxidation is characterized in that with tungsten/tungsten/iridium composite coating layer tungsten and carbon material directly contact the formation middle layer, and iridium directly contacts the formation upper layer with tungsten coating.
2. according to claims 1 described compound coating, it is characterized in that tungsten coating in the carbon material top layer to the outside gradient transition, metallurgical binding does not have the sudden change of composition and mechanical property.
3. according to claims 1 described compound coating, it is characterized in that iridium coating layer in the tungsten coating to the outside gradient transition, metallurgical binding does not have the sudden change of composition and mechanical property.
4. a carbon material anti oxidation is with the preparation method of tungsten/tungsten/iridium composite coating layer, it is characterized in that being target plate with the tungsten plate earlier, prepare tungsten coating by the double-deck glow plasma surface alloying at carbon material surface, and then be that target plate passes through the double-deck glow plasma surface alloying at tungsten coating surface preparation iridium coating layer with the iridium plate.
5. according to claims 4 described preparation methods, when it is characterized in that preparing tungsten coating, be negative electrode with tungsten plate and carbon material in the vacuum glow discharge device, vacuum chamber housing is public anode, between anode and two negative electrodes tunable voltage dc power supply is set respectively.
6. according to claims 4 described preparation methods, when it is characterized in that preparing iridium coating layer, be negative electrode with iridium plate and the carbon material that has been coated with tungsten in the vacuum glow discharge device, vacuum chamber housing is public anode, between anode and two negative electrodes tunable voltage dc power supply is set respectively.
7. according to claims 4 described preparation methods, it is characterized in that source electrode and negative electrode are equipped with a cover direct supply respectively, voltage output range is 0~2000V, and adjustable continuously, and two cover power supplys are public anode with the vacuum chamber housing of ground connection.
8. according to claims 4 described preparation methods, the air pressure that it is characterized in that discharging is 13.3~133Pa, and final vacuum is not less than 0.1Pa, source potential-800V~-2000V, the workpiece current potential-200V~-1000V.
9. according to claims 4 described preparation methods, the spacing that it is characterized in that two negative electrodes in the vacuum glow discharge device is 10mm~50mm.
10. according to claims 4 described preparation methods, it is characterized in that comprising following sequential steps:
(1) with carbon material 1800~2200 ℃ of pyroprocessing;
(2) tungsten plate and carbon material being packed in the vacuum glow discharge device, is negative electrode with tungsten plate and carbon material, and vacuum chamber housing is public anode;
(3) be evacuated to final vacuum, send into argon gas, light aura;
(4) cut off the power supply behind the certain hour, the vacuum glow discharge device is opened in inflation;
(5) change the tungsten plate with the iridium plate, adjust iridium plate and carbon material spacing;
(6) be evacuated to final vacuum, send into argon gas, light aura;
(7) cut off the power supply behind the certain hour, the vacuum glow discharge device is opened in inflation, finishes tungsten/tungsten/iridium composite coating layer preparation.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103144356A (en) * | 2013-03-12 | 2013-06-12 | 南京航空航天大学 | High-conductivity composite carbon fiber and preparation method thereof |
CN108070859A (en) * | 2017-12-14 | 2018-05-25 | 西北有色金属研究院 | Refractory metal surfaces lamellar composite Ir/W high-temperature oxidation resistant coatings and preparation method thereof |
CN108866502A (en) * | 2018-06-21 | 2018-11-23 | 太原理工大学 | A kind of titanium alloy surface high temperature coatings and preparation method thereof |
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CN101445391B (en) * | 2008-12-23 | 2011-04-27 | 南京航空航天大学 | Method for infiltrating tungsten carbide on the surface of carbon material |
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JPH08253874A (en) * | 1995-03-16 | 1996-10-01 | Kawasaki Steel Corp | High adhesion oxidation resistant coating film for c/c composite material and its formation |
EP0850899B1 (en) * | 1996-12-24 | 2001-05-16 | Sulzer Metco AG | Method of coating carbon or carbon containing nonmetallic substrates and substrate coated thereby |
CN1136331C (en) * | 1999-02-11 | 2004-01-28 | 太原理工大学 | Pulse glow discharge plasma surface metallurgical technology |
CN1451505A (en) * | 2002-04-16 | 2003-10-29 | 西北有色金属研究院 | Carbon based composite material and titanium alloy soldering method |
CN1318352C (en) * | 2005-08-11 | 2007-05-30 | 中国科学院山西煤炭化学研究所 | Preparation method of charcoal material surface gradient coating for resisting oxidation |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103144356A (en) * | 2013-03-12 | 2013-06-12 | 南京航空航天大学 | High-conductivity composite carbon fiber and preparation method thereof |
CN108070859A (en) * | 2017-12-14 | 2018-05-25 | 西北有色金属研究院 | Refractory metal surfaces lamellar composite Ir/W high-temperature oxidation resistant coatings and preparation method thereof |
CN108866502A (en) * | 2018-06-21 | 2018-11-23 | 太原理工大学 | A kind of titanium alloy surface high temperature coatings and preparation method thereof |
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