CN103614713B - Method for preparing high-temperature composite coating on niobium-based surface by utilizing sol-gel method - Google Patents

Method for preparing high-temperature composite coating on niobium-based surface by utilizing sol-gel method Download PDF

Info

Publication number
CN103614713B
CN103614713B CN201310651291.6A CN201310651291A CN103614713B CN 103614713 B CN103614713 B CN 103614713B CN 201310651291 A CN201310651291 A CN 201310651291A CN 103614713 B CN103614713 B CN 103614713B
Authority
CN
China
Prior art keywords
niobium
base alloy
time
zinc
coating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310651291.6A
Other languages
Chinese (zh)
Other versions
CN103614713A (en
Inventor
李伟洲
刘伟
秦泽华
周敏
许安
陈泉志
杨阳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangxi University
Original Assignee
Guangxi University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangxi University filed Critical Guangxi University
Priority to CN201310651291.6A priority Critical patent/CN103614713B/en
Publication of CN103614713A publication Critical patent/CN103614713A/en
Application granted granted Critical
Publication of CN103614713B publication Critical patent/CN103614713B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Chemically Coating (AREA)

Abstract

The invention discloses a method for preparing a high-temperature composite coating on a niobium-based surface by utilizing a sol-gel method. The method comprises the following steps: step 1, pretreating a niobium-based alloy specimen; step 2, preparing an intermediate bonding layer of the niobium-based alloy specimen in a chemical treatment manner; step 3, preparing Al2O sol-gel; step 4, performing dip-coating and drying; and step 5, performing vacuum heat treatment, thereby obtaining the high-temperature-resistant oxidation coating containing the intermediate bonding layer. The method has the advantages that 1, the process equipment is simple and easy to operate; the components of the coating are uniform and are controllable in thickness; the influence of the high temperature on the tissue property of a niobium substrate is avoided due to the adoption of a low heat treatment temperature; 2, the internal stress caused by the difference of thermal expansion coefficients between the substrate and the coating is effectively reduced under the action of the intermediate bonding layer, so that the combination between the coating with the substrate is improved; the capability of the coating for protecting the substrate from being oxidized is improved.

Description

A kind of niobium primary surface sol-gel method prepares the method for combined high temperature coating
Technical field
The invention belongs to and prepare high-temperature oxidation resistant coating technology on alloy substrate.Specifically a kind of niobium primary surface sol-gel method prepares the method for combined high temperature coating.The method employing is prepared middle close binder raising colloidal sol and is coagulated
Glue legal system for the combination between coating and matrix, thus reaches the oxidation resistant object of raising coating.
Background technology
Along with further developing of aeronautical and space technology, improving constantly of the thrust-weight ratios such as aerospacecraft, the use temperature of aircraft engine can reach more than 1200 DEG C, and rocket then reaches higher temperature, and traditional superalloy can not meet people's demand.The good characteristic of niobium alloy becomes one of important candidate material of thermal structure part in Aeronautics and Astronautics and nuclear industry.But niobium alloy is easily oxidized, just there is " pest " oxidation in pure niobium 600 DEG C.Improve niobium base high-temperature oxidation resistant mainly through coating protection at present, main method has fused slurry method, pack cementation method etc.
The preparation method of above-mentioned coating can see complex process, and thermal treatment temp is high, has a strong impact on substrate performance.Prepared coating due to and the thermal expansivity of matrix between there are differences and cause coating easy to crack, come off.And the patent be combined with matrix about improving coating rarely has report.
Such as CN201010591716 discloses a kind of aluminium (alcohol) salt hydrolysis preparation preparation Al 2o 3the method of coating.The colloidal sol prepared directly is coated in surface of metal product heat-treat, obtains Al 2o 3coating.Al 2o 3thermal expansivity 8.3 ~ 9.3 × 10 -6k -1, the thermal expansivity of niobium-base alloy is 7.2 × 10 ﹣ 6k ﹣ 1, because coating to there are differences with the thermal expansivity of niobium alloy and crystalline network is different, internal stress can be produced under high temperature and cause coating to crack coming off and lose the effect of protection matrix.CN103388137A has invented a kind of method of Electroless Plating Ni-p nano-coating, to the metal base material of oil removal treatment, carries out Electroless Plating Ni-p nano-coating, reaches certain thickness and namely obtain Ni-p nano-coating.Research finds that Ni-p coating has and suppresses crackle to produce and expansion effect, when reaching a timing when closing phosphorus amount in Ni-p coating, its structure is non-crystalline state, there is not crystal boundary, subgrain boundary, dislocation, fault, namely there is no the defect that common metal crystallization is all, therefore likely improve oxide coating and intermetallic combination.
The present invention improves coating by a kind of method that chemical pre-treatment and collosol and gel combine and is combined with niobium matrix, effectively solves coating itself with niobium matrix in conjunction with bad, reduce easily produce cracking in process under arms, obscission causes coating failure.
Summary of the invention
The object of the invention there are provided a kind of method that the primary surface of niobium simply and easily sol-gel method prepares combined high temperature coating.
The technical scheme that the present invention solves the problems of the technologies described above is:
Niobium primary surface sol-gel method prepares a method for combined high temperature coating, operates according to the following steps:
The first step: niobium-base alloy sample pretreatment:
With dehydrated alcohol, acetone cleaning and degreasing respectively after the pre-grinding of niobium-base alloy sample, drier after ultrasonic cleaning.
Second step: niobium-base alloy sample middle close binder is prepared in chemical treatment:
Prepare middle close binder step as follows:
1. electrochemical deoiling
By pretreated niobium-base alloy sample 15 ~ 40g/L Na 3pO 412H 2o, 10 ~ 30g/LNa 2cO 3with 5 ~ 15g/L Na 2siO 3the mixed solution of composition soaks under temperature 50 ~ 60 DEG C of conditions, and soak time is 4 ~ 5min, obtains the niobium-base alloy sample after the oil removing removal of impurity.
2. soda acid corrodes
1) 5 ~ 20g/L NaOH of the niobium-base alloy sample after the oil removing removal of impurity is carried out alkali erosion under temperature 20 ~ 30 DEG C of conditions, alkali erosion time is 10 ~ 20s.
2) the niobium-base alloy sample 20 ~ 80g/L H after alkali being corroded 2sO 4under temperature 20 ~ 30 DEG C of conditions, carry out acid attack, the acid attack time is 10 ~ 20s, is corroded niobium-base alloy specimen surface is fully activated by soda acid.
3. first time soaks zinc
Soda acid is corroded niobium-base alloy sample 40 ~ 80g/L NaOH, the 2 ~ 8g/LKNaC after process 4h 4o 6h 2o, 2 ~ 8g/L ZnO, 26g/LFeCl 36H 2o1 ~ 3g/L NaNO 3the mixed solution of composition carries out the reaction of first time leaching zinc under temperature 20-30 DEG C of condition, and galvanizing time is 20 ~ 60s.Niobium-base alloy specimen surface rough porous after first time leaching zinc, sticking power is bad, has small amounts film to remain unavoidably simultaneously.
4. move back zinc
By the niobium-base alloy sample 30 ~ 70g/L HNO after first time leaching zinc 3carry out moving back zinc under temperature 20 ~ 30 DEG C of conditions, moving back the zinc time is 60 ~ 90s, and the niobium-base alloy specimen surface after moving back zinc presents uniform active state.
5. second time soaks zinc
Niobium-base alloy sample 100 ~ 140g/L NaOH, 40 ~ 60g/L KNaC after zinc will be moved back 4h 4o 6h 2o, 10 ~ 30g/LZnO, 1 ~ 3g/L FeCl 36H 2o and 1 ~ 3g/L NaNO 3the mixed solution of composition carries out second time and soaks zinc under temperature is 20 ~ 30 DEG C of conditions, and second time galvanizing time is 10 ~ 30s, and the niobium-base alloy specimen surface after second time leaching zinc obtains thin and careful zinc layers.
6. chemical treatment
By the niobium-base alloy sample 20 ~ 30g/L NiSO after second time leaching zinc 46H 2o, 20 ~ 40g/LNaH 2pO 2h 2o, 15 ~ 25g/L CH 3cOONa, 15 ~ 25g/LNa 3c 6h 5o 7with 5 ~ 15g/L NH 4the mixed solution of Cl composition carries out chemical treatment under temperature is 70 ~ 90 DEG C of conditions, and chemical process time is 30 ~ 60min, after chemical treatment, obtain one deck middle close binder at niobium-base alloy specimen surface.
3rd step: Al 2prepared by O collosol and gel
Aluminum isopropylate 20.4g is dissolved in 270ml distilled water, is heated to 70 ~ 85 DEG C, uses HNO 3regulate pH to 2 ~ 3, after all dissolving, constant temperature stirs 1 ~ 2h and makes it be hydrolyzed, and puts into encloses container subsequently and in 85 ~ 95 DEG C of water bath with thermostatic control 8 ~ 10h, namely ageing 2 ~ 4d obtains stable Al 2o 3colloidal sol;
4th step: dip-coating, drying
Niobium-base alloy sample second step being obtained one deck middle close binder by crystal pulling method to immerse in colloidal sol dip-coating 3 times, lifts out liquid level with 4 ~ 6cm/min pull rate, then dry under room temperature;
5th step: vacuum heat treatment
Be 2 ~ 6 × 10 by the niobium-base alloy sample after the 4th step process in vacuum tightness -2thermal treatment under Pa condition, vacuum tightness heat-treat condition: be heated to 500 DEG C of insulation 10h with 4 ~ 6 DEG C/min heat-up rate and cool to room temperature with identical heating rate with the furnace after 900 DEG C of insulation 5h again, namely obtain containing middle close binder high temperature coatings.
Advantage of the present invention:
1. the present invention has successfully prepared compound coating respectively on niobium-base alloy surface, and processing unit is simple, easy handling, and coating ingredients is even.
2. middle close binder effectively reduces the internal stress produced by thermal expansivity difference between matrix and coating, improves the combination of coating and matrix, improves coating protection matrix from oxidation.
3. adopt lower thermal treatment temp, thus avoid high temperature on the impact of niobium matrix performance.
4. the present invention is applicable to the specimen surface of complex shape, and coating uniform and thickness can control.
Accompanying drawing explanation
Fig. 1 is Al of the present invention 2o 3coatingsurface SEM microscopic appearance figure.
Fig. 2 is Al of the present invention 2o 3coating XRD figure is composed.
Fig. 3 is Al of the present invention 2o 3coating 950 DEG C of oxidation kinetics graphic representations.
Fig. 4 is Al of the present invention 2o 3coating 1050 DEG C of oxidation kinetics graphic representations.
Fig. 5 is Al of the present invention 2o 3coating 1050 DEG C of high temperature oxidation 19h rear interface shape appearance figures.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
Niobium primary surface sol-gel method prepares the method for combined high temperature coating:
The first step: niobium-base alloy sample pretreatment:
With dehydrated alcohol, acetone cleaning and degreasing respectively after the pre-grinding of niobium-base alloy sample, drier after ultrasonic cleaning.
Second step: niobium-base alloy sample middle close binder is prepared in chemical treatment:
Prepare middle close binder step as follows:
1. electrochemical deoiling
By pretreated niobium-base alloy sample 15g/L Na 3pO 412H 2o, 10g/L Na 2cO 3and 5g/LNa 2siO 3the mixed solution of composition soaks under temperature 50 C condition, and soak time is 4min, obtains the niobium-base alloy sample after the oil removing removal of impurity.
2. soda acid corrodes
1) the niobium-base alloy sample 5g/L NaOH after the oil removing removal of impurity is carried out alkali erosion under temperature 20 DEG C of conditions, alkali erosion time is 10s.
2) the niobium-base alloy sample 20g/L H after alkali being corroded 2sO 4under temperature 20 DEG C of conditions, carry out acid attack, the acid attack time is 10s, is corroded niobium-base alloy specimen surface is fully activated by soda acid.
3. first time soaks zinc
Soda acid is corroded niobium-base alloy sample 40g/L NaOH, the 2g/L KNaC after process 4h 4o 6h 2o, 2g/L ZnO, 2g/LFeCl 36H 2o, 1g/L NaNO 3the mixed solution of composition carries out the reaction of first time leaching zinc under temperature 20 DEG C of conditions, and galvanizing time is 20s.Niobium-base alloy specimen surface rough porous after first time leaching zinc, sticking power is bad, has small amounts film to remain unavoidably simultaneously.
4. move back zinc
By the niobium-base alloy sample 30g/L HNO after first time leaching zinc 3carry out moving back zinc under temperature 20 DEG C of conditions, moving back the zinc time is 60s, and the niobium-base alloy specimen surface after moving back zinc presents uniform active state.
5. second time soaks zinc
Niobium-base alloy sample 100g/L NaOH, 40g/L KNaC after zinc will be moved back 4h 4o 6h 2o, 10g/LZnO, 1g/L FeCl 36H 2o and 1g/L NaNO 3the mixed solution of composition carries out second time and soaks zinc under temperature is 20 DEG C of conditions, and second time galvanizing time is 10s, and the niobium-base alloy specimen surface after second time leaching zinc obtains thin and careful zinc layers.
6. chemical treatment
By the niobium-base alloy sample 20g/L NiSO after second time leaching zinc 46H 2o, 20g/LNaH 2pO 2h 2o, 15g/L CH 3cOONa, 15g/LNa 3c 6h 5o 7with 5g/L NH 4the mixed solution of Cl composition carries out chemical treatment under temperature is 70 DEG C of conditions, and chemical process time is 30min, after chemical treatment, obtain one deck middle close binder at niobium-base alloy specimen surface.
3rd step: Al 2prepared by O collosol and gel
Aluminum isopropylate 20.4g is dissolved in 270ml distilled water, is heated to 70 DEG C, uses HNO 3regulate pH to 2, after all dissolving, constant temperature stirs 1h and makes it be hydrolyzed, and puts into encloses container subsequently and in 85 DEG C of water bath with thermostatic control 8h, namely ageing 2d obtains stable Al 2o 3colloidal sol;
4th step: dip-coating, drying
Niobium-base alloy sample second step being obtained one deck middle close binder by crystal pulling method to immerse in colloidal sol dip-coating 3 times, lifts out liquid level with 4cm/min pull rate, then dry under room temperature;
5th step: vacuum heat treatment
Be 2 ~ 6 × 10 by the niobium-base alloy sample after the 4th step process in vacuum tightness -2thermal treatment under Pa condition, vacuum tightness heat-treat condition: be heated to 500 DEG C of insulation 10h with 4 DEG C/min heat-up rate and cool to room temperature with identical heating rate with the furnace after 900 DEG C of insulation 5h again, namely obtain containing middle close binder high temperature coatings.Find that coatingsurface is complete as shown in Figure 1 by scanning electronic microscope, without coming off cracking phenomena, X-ray diffraction finds that coating is thinner, and X-ray has detected matrix phase, obviously can see matrix phase in Fig. 2, and coatingsurface is Al 2o 3phase.
Embodiment 2
Niobium primary surface sol-gel method prepares the method for combined high temperature coating:
The first step: niobium-base alloy sample pretreatment:
With dehydrated alcohol, acetone cleaning and degreasing respectively after the pre-grinding of niobium-base alloy sample, drier after ultrasonic cleaning.
Second step: niobium-base alloy sample middle close binder is prepared in chemical treatment:
Prepare middle close binder step as follows:
1. electrochemical deoiling
By pretreated niobium-base alloy sample 40g/L Na 3pO 412H 2o, 30g/L Na 2cO 3with 15g/L Na 2siO 3the mixed solution of composition soaks under temperature 60 C condition, and soak time is 5min, obtains the niobium-base alloy sample after the oil removing removal of impurity.
2. soda acid corrodes
1) the niobium-base alloy sample 20g/L NaOH after the oil removing removal of impurity is carried out alkali erosion under temperature 30 DEG C of conditions, alkali erosion time is 20s.
2) the niobium-base alloy sample 80g/L H after alkali being corroded 2sO 4under temperature 30 DEG C of conditions, carry out acid attack, the acid attack time is 20s, is corroded niobium-base alloy specimen surface is fully activated by soda acid.
3. first time soaks zinc
Soda acid is corroded niobium-base alloy sample 80g/L NaOH, the 8g/L KNaC after process 4h 4o 6h 2o, 8g/L ZnO, 6g/LFeCl 36H 2o, 3g/L NaNO 3the mixed solution of composition carries out the reaction of first time leaching zinc under temperature 30 DEG C of conditions, and galvanizing time is 60s.Niobium-base alloy specimen surface rough porous after first time leaching zinc, sticking power is bad, has small amounts film to remain unavoidably simultaneously.
4. move back zinc
By the niobium-base alloy sample 70g/L HNO after first time leaching zinc 3carry out moving back zinc under temperature 30 DEG C of conditions, moving back the zinc time is 90s, and the niobium-base alloy specimen surface after moving back zinc presents uniform active state.
5. second time soaks zinc
Niobium-base alloy sample 140g/L NaOH, 60g/L KNaC after zinc will be moved back 4h 4o 6h 2o, 30g/LZnO, 3g/L FeCl 36H 2o and 3g/L NaNO 3the mixed solution of composition carries out second time and soaks zinc under temperature is 30 DEG C of conditions, and second time galvanizing time is 30s, and the niobium-base alloy specimen surface after second time leaching zinc obtains thin and careful zinc layers.
6. chemical treatment
By the niobium-base alloy sample 30g/L NiSO after second time leaching zinc 46H 2o, 40g/LNaH 2pO 2h 2o, 25g/L CH 3cOONa, 25g/LNa 3c 6h 5o 7with 15g/L NH 4the mixed solution of Cl composition carries out chemical treatment under temperature is 90 DEG C of conditions, and chemical process time is 60min, after chemical treatment, obtain one deck middle close binder at niobium-base alloy specimen surface.
3rd step: Al 2prepared by O collosol and gel
Aluminum isopropylate 20.4g is dissolved in 270ml distilled water, is heated to 85 DEG C, uses HNO 3regulate pH to 3, after all dissolving, constant temperature stirs 2h and makes it be hydrolyzed, and puts into encloses container subsequently and in 95 DEG C of water bath with thermostatic control 10h, namely ageing 4d obtains stable Al 2o 3colloidal sol;
4th step: dip-coating, drying
Niobium-base alloy sample second step being obtained one deck middle close binder by crystal pulling method to immerse in colloidal sol dip-coating 3 times, lifts out liquid level with 6cm/min pull rate, then dry under room temperature;
5th step: vacuum heat treatment
Be 2 ~ 6 × 10 by the niobium-base alloy sample after the 4th step process in vacuum tightness -2thermal treatment under Pa condition, vacuum tightness heat-treat condition: be heated to 500 DEG C of insulation 10h with 6 DEG C/min heat-up rate and cool to room temperature with identical heating rate with the furnace after 900 DEG C of insulation 5h again, namely obtain containing middle close binder high temperature coatings.Constant temperature oxidation test finds that coating has very high oxidation resistent susceptibility 950 DEG C and 1050 DEG C as shown in Figure 3,4; 33% is improve with matrix phase ratio; the Cross Section Morphology of 1050 DEG C of high temperature oxidations as shown in Figure 5; coating coating and basal body interface place after 1050 DEG C of high temperature oxidation 19h create a little crackle, play a very good protection to matrix.

Claims (1)

1. niobium primary surface sol-gel method prepares a method for combined high temperature coating, it is characterized in that, operates according to the following steps:
The first step: niobium-base alloy sample pretreatment:
With dehydrated alcohol, acetone cleaning and degreasing respectively after the pre-grinding of niobium-base alloy sample, drier after ultrasonic cleaning;
Second step: niobium-base alloy sample middle close binder is prepared in chemical treatment:
Prepare middle close binder step as follows:
1) electrochemical deoiling
By pretreated niobium-base alloy sample 15 ~ 40g/L Na 3pO 412H 2o, 10 ~ 30g/LNa 2cO 3with 5 ~ 15g/L Na 2siO 3the mixed solution of composition soaks under temperature 50 ~ 60 DEG C of conditions, and soak time is 4 ~ 5min, obtains the niobium-base alloy sample after the oil removing removal of impurity;
2) soda acid corrodes
(1) 5 ~ 20g/L NaOH of the niobium-base alloy sample after the oil removing removal of impurity is carried out alkali erosion under temperature 20 ~ 30 DEG C of conditions, alkali erosion time is 10 ~ 20s;
(2) the niobium-base alloy sample 20 ~ 80g/L H after alkali being corroded 2sO 4under temperature 20 ~ 30 DEG C of conditions, carry out acid attack, the acid attack time is 10 ~ 20s, is corroded niobium-base alloy specimen surface is fully activated by soda acid;
3) first time soaks zinc
Soda acid is corroded niobium-base alloy sample 40 ~ 80g/L NaOH, the 2 ~ 8g/LKNaC after process 4h 4o 6h 2o, 2 ~ 8g/L ZnO, 26g/LFeCl 36H 2o1 ~ 3g/L NaNO 3the mixed solution of composition carries out the reaction of first time leaching zinc under temperature 20-30 DEG C of condition, and galvanizing time is 20 ~ 60s, the niobium-base alloy specimen surface rough porous after first time leaching zinc, and sticking power is bad, has small amounts film to remain unavoidably simultaneously;
4) zinc is moved back
By the niobium-base alloy sample 30 ~ 70g/L HNO after first time leaching zinc 3carry out moving back zinc under temperature 20 ~ 30 DEG C of conditions, moving back the zinc time is 60 ~ 90s, and the niobium-base alloy specimen surface after moving back zinc presents uniform active state;
5) second time soaks zinc
Niobium-base alloy sample 100 ~ 140g/L NaOH, 40 ~ 60g/L KNaC after zinc will be moved back 4h 4o 6h 2o, 10 ~ 30g/LZnO, 1 ~ 3g/L FeCl 36H 2o and 1 ~ 3g/L NaNO 3the mixed solution of composition carries out second time and soaks zinc under temperature is 20 ~ 30 DEG C of conditions, and second time galvanizing time is 10 ~ 30s, and the niobium-base alloy specimen surface after second time leaching zinc obtains thin and careful zinc layers;
6) chemical treatment
By the niobium-base alloy sample 20 ~ 30g/L NiSO after second time leaching zinc 46H 2o, 20 ~ 40g/LNaH 2pO 2h 2o, 15 ~ 25g/L CH 3cOONa, 15 ~ 25g/LNa 3c 6h 5o 7with 5 ~ 15g/L NH 4the mixed solution of Cl composition carries out chemical treatment under temperature is 70 ~ 90 DEG C of conditions, and chemical process time is 30 ~ 60min, after chemical treatment, obtain one deck middle close binder at niobium-base alloy specimen surface;
3rd step: Al 2o 3prepared by collosol and gel
Aluminum isopropylate 20.4g is dissolved in 270ml distilled water, is heated to 70 ~ 85 DEG C, uses HNO 3regulate pH to 2 ~ 3, after all dissolving, constant temperature stirs 1 ~ 2h and makes it be hydrolyzed, and puts into encloses container subsequently and in 85 ~ 95 DEG C of water bath with thermostatic control 8 ~ 10h, namely ageing 2 ~ 4d obtains stable Al 2o 3colloidal sol;
4th step: dip-coating, drying
Niobium-base alloy sample second step being obtained one deck middle close binder by crystal pulling method to immerse in colloidal sol dip-coating 3 times, lifts out liquid level with 4 ~ 6cm/min pull rate, then dry under room temperature;
5th step: vacuum heat treatment
Be 2 × 10 by the niobium-base alloy sample after the 4th step process in vacuum tightness -2~ 6 × 10 -2thermal treatment under Pa condition, vacuum tightness heat-treat condition: be heated to 500 DEG C of insulation 10h with 4 ~ 6 DEG C/min heat-up rate and cool to room temperature with identical heating rate with the furnace after 900 DEG C of insulation 5h again, namely obtain containing middle close binder high temperature coatings.
CN201310651291.6A 2013-12-05 2013-12-05 Method for preparing high-temperature composite coating on niobium-based surface by utilizing sol-gel method Active CN103614713B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310651291.6A CN103614713B (en) 2013-12-05 2013-12-05 Method for preparing high-temperature composite coating on niobium-based surface by utilizing sol-gel method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310651291.6A CN103614713B (en) 2013-12-05 2013-12-05 Method for preparing high-temperature composite coating on niobium-based surface by utilizing sol-gel method

Publications (2)

Publication Number Publication Date
CN103614713A CN103614713A (en) 2014-03-05
CN103614713B true CN103614713B (en) 2015-07-22

Family

ID=50165427

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310651291.6A Active CN103614713B (en) 2013-12-05 2013-12-05 Method for preparing high-temperature composite coating on niobium-based surface by utilizing sol-gel method

Country Status (1)

Country Link
CN (1) CN103614713B (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103938190B (en) * 2014-05-16 2016-04-06 西安建筑科技大学 The preparation method of a kind of molybdenum and molybdenum alloy surface oxidation resistant coating
CN104746059B (en) * 2015-04-10 2017-08-25 核工业理化工程研究院 Suppress the preparation method of the coating of metal uranium surface spontaneous combustion
CN105386013B (en) * 2015-11-16 2017-11-10 西安建筑科技大学 A kind of molybdenum or molybdenum alloy surface Pd CeO2The preparation method of Co nano coatings
CN113512742B (en) * 2021-04-23 2023-07-07 南昌航空大学 Pretreatment method for high-temperature alloy surface and electrodeposition method for high-temperature alloy surface

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3438028B2 (en) * 2000-11-29 2003-08-18 独立行政法人産業技術総合研究所 Nb3Si5Al2-Al2O3 two-layer coated Nb-based alloy and method for producing the same
CN102021545A (en) * 2010-12-16 2011-04-20 沈阳化工大学 Preparation method of Al2O3 coating with high temperature oxidation resistance
CN102251234B (en) * 2011-07-04 2012-10-24 成都理工大学 Method for preparing Al2O3 coated hard alloy based on sol-gel method
CN102531554B (en) * 2012-01-06 2013-03-27 天津大学 Hexaaluminate-embedded alumina composite coating and preparation method thereof

Also Published As

Publication number Publication date
CN103614713A (en) 2014-03-05

Similar Documents

Publication Publication Date Title
CN103614713B (en) Method for preparing high-temperature composite coating on niobium-based surface by utilizing sol-gel method
CN102345127B (en) Surface treatment method of superhydrophobic aluminum foil
CN100464007C (en) Process for preparing neodymium-iron-boron permanent magnetic material surface gradient function coating layer
CN104651908B (en) The preparation method and method for sealing of a kind of Mg alloy surface ceramic film
CN100408725C (en) Process for compound surface sheilding of metal magnesium and magnesium alloy
CN107779713B (en) A kind of beryllium alumin(i)um alloy and preparation method thereof
CN1900360A (en) Process for preparing magnesium alloy surface function gradient film
CN103668030A (en) Improved hot galvanizing method of iron handicraft or furniture
CN110565148B (en) Magnesium alloy black micro-arc oxidation film nano passivator and passivation method
CN113429820B (en) Oriented Mxene/Co conductive filler for anti-corrosion coating and preparation method thereof
CN104141138A (en) Preparation method of micro-arc oxidation-composite chemical nickel plating coating layer on surface of magnesium alloy
CN103668368A (en) Preparation process of molybdenum/palladium/silver laminar metal matrix composite
CN113106434A (en) Environment-friendly aluminum alloy chemical oxidation liquid and chemical oxidation method
CN102899703A (en) Silicate electrolyte and application of silicate electrolyte in magnesium alloy micro-arc oxidation film preparation
CN103320776B (en) A kind of antivacuum middle high temperature solar energy selective absorption coating compound antireflective film and preparation method thereof
CN104561980A (en) Surface treatment method for magnesium alloy
CN103484824B (en) Compoiste adhering layer material of a kind of anti-1200 DEG C of resistance to combustion gas thermal etchings of high temperature oxidation and preparation method thereof
CN104342683A (en) Magnesium alloy work-piece surface anti-corrosion conversion film treatment process
CN113215627A (en) Method for preparing super-hydrophobic zinc sulfide coating on surface of stainless steel
CN103695905B (en) A kind of method preparing composite nickel coating on magnesium alloy differential arc oxidation film surface
CN101892468A (en) Preparation method of chemically plating Ni-W-P ternary alloy on surface of Mg-Li alloy
Ji et al. Effect of titanium sol on sulfuric-citric acids anodizing of 7150 aluminum alloy
CN101358046B (en) Silicon oxide-containing nano paint, preparation method and application thereof
CN203080040U (en) Nano-porous surface structure of intensifying and boiling metal
CN114032547B (en) Alloy surface composite coating and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant