CN105603483B - A kind of preparation method of titanium-base alloy high temperature coatings - Google Patents
A kind of preparation method of titanium-base alloy high temperature coatings Download PDFInfo
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- CN105603483B CN105603483B CN201511027689.8A CN201511027689A CN105603483B CN 105603483 B CN105603483 B CN 105603483B CN 201511027689 A CN201511027689 A CN 201511027689A CN 105603483 B CN105603483 B CN 105603483B
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 53
- 239000000956 alloy Substances 0.000 title claims abstract description 53
- 238000000576 coating method Methods 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000010936 titanium Substances 0.000 claims abstract description 26
- 239000011248 coating agent Substances 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 18
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 18
- 239000011159 matrix material Substances 0.000 claims abstract description 17
- 230000003647 oxidation Effects 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004062 sedimentation Methods 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- -1 alkyl silicate Chemical compound 0.000 claims abstract description 6
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910000883 Ti6Al4V Inorganic materials 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 229910004349 Ti-Al Inorganic materials 0.000 claims description 2
- 229910004692 Ti—Al Inorganic materials 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 150000004702 methyl esters Chemical class 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 229910000838 Al alloy Inorganic materials 0.000 abstract description 19
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 abstract description 15
- 229910010038 TiAl Inorganic materials 0.000 description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- 235000019441 ethanol Nutrition 0.000 description 9
- 238000005498 polishing Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000004070 electrodeposition Methods 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000000151 deposition Methods 0.000 description 6
- 244000137852 Petrea volubilis Species 0.000 description 5
- 229910052681 coesite Inorganic materials 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 125000005909 ethyl alcohol group Chemical group 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000003026 anti-oxygenic effect Effects 0.000 description 2
- 238000005524 ceramic coating Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000005468 ion implantation Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000006193 liquid solution Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- PXFBZOLANLWPMH-UHFFFAOYSA-N 16-Epiaffinine Natural products C1C(C2=CC=CC=C2N2)=C2C(=O)CC2C(=CC)CN(C)C1C2CO PXFBZOLANLWPMH-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910010039 TiAl3 Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
A kind of preparation method of titanium-base alloy high temperature coatings, comprises the following steps：1) oxide on surface of titanium-based alloy matrix is removed first, is then cleaned, is dried；2) absolute ethyl alcohol, water and precursor alkyl silicate are mixed in proportion, adjusts pH of mixed to stir 2~48h at room temperature to 2.0~6.0, obtain precursor solution with acid；3) precursor solution prepared is added in two slot electrodes, using titanium-based alloy matrix as working electrode, platinized platinum or graphite are used as and electrode, electrode spacing controlled in 1 10cm, and control electric current density is 0.1mAcm‑2~5.0mAcm‑2, sedimentation time is 30s~2000s, washes after 40~150 DEG C of drying, obtains micro-nano oxide coating；4) titanium-base alloy that will be covered with micro-nano oxide coating is heat-treated 10~60min at 600~700 DEG C in atmosphere, that is, titanium-base alloy high temperature coatings are made.Preparation technology of the present invention is simple, has excellent adhesion between the coating and matrix of acquisition, is remarkably improved titanium-aluminium alloy high-temperature oxidation resistance.
Description
Technical field
The invention belongs to metal material resistance to high temperature oxidation field, and in particular to a kind of titanium-base alloy high temperature coatings
Preparation method.
Technical background
Titanium-aluminium alloy has the advantages that density is low, specific strength is high, modulus of elasticity is high, high temperature and creep resistance ability is good, is a kind of
The high-temperature material of great application prospect, it is applied to the high temperature parts such as aero-engine high pressure pressure fan and turbo blade.So
And the actual use temperature of titanium-aluminium alloy is limited in less than 750 DEG C, due at a higher temperature, titanium and aluminium and oxygen it is affine
Ability is similar, and that alloy surface is formed is TiO2And Al2O3Mixed layer, the growth rate of oxide-film quickly, are easily shelled
Fall.
To overcome the above insufficient, domestic and foreign scholars employ alloying, ion implantation, face coat and anodic oxidation etc.
Method is modified to improve the service temperature of titanium-aluminium alloy.Alloy design mainly includes two aspects, first, improving in TiAl alloy
Basic element Al content, this is no doubt advantageous to the improvement of its antioxygenic property, but Al content should not be too high, otherwise once separating out
Brittle TiAl3Its mechanical property will be influenceed.Second, by adding the third or a variety of alloying elements, such as：Nb,Sb,Si,
Cr, Y, although Mo etc. can also be effectively improved the high-temperature oxidation resistance of TiAl alloy, addition is too high to normally result in TiAl
Alloy mechanical property declines.Although ion implantation injection rate it is controllable, it is repeated preferably, the equipment being related to costly, production
It is less efficient, and to TiAl alloy composition change depth be limited to the shallower scope in surface (<1μm).And protective coating, such as
Metal coating MCrAl (Y), ceramic coating (such as SiO2、Al2O3And ZrO2Deng) and diffusion coating (such as Al, Si) although etc. can
Stop oxygen to matrix permeability as screen layer, but each still suffer from the problem of certain.Counterdiffusion between metal coating and matrix
More serious, interface easily separates out hard crisp phase, while produces Ke Kendaer holes, seriously reduces the bond strength of coating and matrix；
Ceramic coating internal stress is larger and relatively low with substrate combinating strength；Diffusion coating differs larger with matrix thermal coefficient of expansion.
The content of the invention
The purpose of the present invention is for existing titanium-aluminium alloy oxidation-resistance property deficiency, there is provided a kind of anti-height of titanium-base alloy
The preparation method of warm oxide covering, the coating obtained significantly improve antioxygenic property of the titanium-base alloy under 900 DEG C of high temperature.
A kind of preparation method of titanium-base alloy high temperature coatings, comprises the following steps：
1) oxide on surface of titanium-based alloy matrix is removed first, is then cleaned, is dried；
2) it is (50-100) according to volume ratio:(50-100)：(1~10) is by absolute ethyl alcohol, water and precursor silicic acid alkyl
Ester mixes, and then adjusts mixed system pH to 2.0~6.0 with acid, stirs 2~48h at room temperature, obtains precursor solution；
3) precursor solution prepared is added in two slot electrodes, using titanium-based alloy matrix as working electrode, platinized platinum or
Graphite, which is used as, to be controlled in 1-10cm electrode, electrode spacing, and control electric current density is -0.1mAcm-2~-5.0mAcm-2Enter
Row electro-deposition, sedimentation time are 30s~2000s, are dried working electrode washing after 40~150 DEG C after the completion of deposition, in titanium
Based alloy surface obtains micro-nano oxide coating；
4) will be covered with the titanium-base alloy of micro-nano oxide coating in atmosphere at 600~700 DEG C heat treatment 10~
60min, that is, titanium-base alloy high temperature coatings are made.
Further, described titanium-base alloy is the titanium-base alloy containing aluminium.
Further, described titanium-base alloy is selected from Ti3-Al、Ti-Al、Ti-Al3、Ti-6Al-4V、TiAlNb、Ti-
One kind in 47Al-2Cr-2Nb.
Further, in step 1), titanium-based alloy matrix can be polished with sand paper and removes oxide on surface；Cleaning reagent can be adopted
With acetone, ethanol etc., it is preferred to use ultrasound is cleaned multiple times.
Further, one kind in the preferred tetraethyl orthosilicate of described alkyl silicate (TEOS), methyl silicate (TMOS)
Or two kinds of mixing.
Further, in step 2), the acid that regulation pH is used can be hydrochloric acid (HCl), nitric acid (HNO3) or acetic acid (HAc),
Concentration is 0.5molL-1~2.0molL-1。
Further, in step 3), current density is preferably -1.0mAcm-2~-5.0mAcm-2。
Further, in step 3), sedimentation time is preferably 200s-600s.
Further, described preparation method is made up of step 1)~step 4).
The beneficial effects of the invention are as follows：
(1) micro/nano level SiO is prepared on titanium-base alloy surface by electro-deposition techniques in the present invention2Coating, the micro-nano
Rice SiO2There is chemical bonding effect in coating, thus have excellent adhesion with matrix；Then through low temperature in air (600~
700 DEG C) heat treatment, in the heat treatment process, SiO2Solid state reaction can occur with Ti the and Al elements in matrix, in gold
Metal surface forms continuous and fine and close glassy state protective layer, and the protective layer can prevent the oxygen in air from being spread to matrix, hinder simultaneously
Only the cation of metal inside is to external diffusion, and then improves the high temperature oxidation resistance of titanium-base alloy.
(2) preparation technology of the present invention is simple and convenient to operate, efficiency high, is easily achieved.
Brief description of the drawings
(curve 1 is naked TiAl alloy to the kinetic curve that Fig. 1 is 900 DEG C of constant temperature oxidation 100h, and curve 2 is TiAl alloy
According to embodiment 4 in tetraethoxysilane -2.0mAcm-2Sample obtained by electro-deposition 300s under current density).
Fig. 2 is not thermally treated SiO prepared by embodiment 42The electron scanning micrograph of coating.
Fig. 3 is electron scanning micrograph of the gained sample of embodiment 4 after 900 DEG C of constant temperature oxidation 100h.
Embodiment
Technical scheme is described further with specific embodiment below, but protection scope of the present invention is unlimited
In this：
Embodiment 1
With sand paper, by titanium-aluminium alloy sample, (titanium al atomic ratio is 1 first:1) polishing removes oxide on surface, then successively
It is cleaned by ultrasonic 10min in acetone and ethanol, it is finally stand-by with hot blast drying.Successively toward add in beaker 50mL absolute ethyl alcohols,
50mL water, 1mL tetraethyl orthosilicates (TEOS), use 0.5molL-1HAc adjusts pH to 2.0 or so, stirs 2h at room temperature and obtains preceding body
Liquid solution is stand-by.Using precursor solution as electrolyte, using the titanium-aluminium alloy sample of polishing cleaned, (titanium al atomic ratio is 1:1) make
For negative electrode, graphite electrode, which is used as, to be controlled in 1cm electrode, electrode spacing, and control electric current density is -0.1mAcm-2, sedimentation time
For 1000s, working electrode deionized water rinsing is obtained into micro-nano oxide coating after 40 DEG C of drying after the completion of deposition.
Then, the titanium-base alloy covered with micro-nano oxide coating is heat-treated 60min at 600 DEG C in atmosphere, that is, be made
High temperature coatings；Its high temperature oxidation resistance is assessed using the weightening of unit area after 900 DEG C of constant temperature oxidation 100h, had
Body result such as table 1.
1 naked TiAl alloy of table and the TiAl alloy sample experiment result covered with high temperature coatings
| Sample | Increase weight mg/cm2 |
| Naked TiAl alloy | 31.32 |
| TiAl alloy covered with high temperature coatings | 1.04 |
Embodiment 2
With sand paper, by titanium-aluminium alloy sample, (titanium al atomic ratio is 3 first:1) polishing removes oxide on surface, then successively
It is cleaned by ultrasonic 10min in acetone and ethanol, it is finally stand-by with hot blast drying.Successively toward add in beaker 100mL absolute ethyl alcohols,
75mL water, 10mL methyl silicates (TMOS), use 2.0molL-1HNO3PH to 6.0 or so is adjusted, before stirring 6h is obtained at room temperature
Body solution for later use.Using precursor solution as electrolyte, using the titanium-aluminium alloy sample of polishing cleaned, (titanium al atomic ratio is 3:1)
As negative electrode, graphite electrode, which is used as, to be controlled in 10cm electrode, electrode spacing, and control electric current density is -5.0mAcm-2, during deposition
Between be 30s, working electrode deionized water rinsing is obtained into micro-nano oxide coating after 150 DEG C of drying after the completion of deposition.
Then, the titanium-base alloy covered with micro-nano oxide coating is heat-treated 10min at 700 DEG C in atmosphere, that is, be made
High temperature coatings；High temperature oxidation resistance is assessed with embodiment 1, and experimental result is listed in table 2.
2 naked TiAl alloy of table and the Ti covered with high temperature coatings3Al alloy sample experimental results
| Sample | Increase weight mg/cm2 |
| Naked TiAl alloy | 31.32 |
| Ti covered with high temperature coatings3Al alloys | 1.58 |
Embodiment 3
With sand paper, by titanium-aluminium alloy sample, (titanium al atomic ratio is 3 first:1) polishing removes oxide on surface, then successively
It is cleaned by ultrasonic 10min in acetone and ethanol, it is finally stand-by with hot blast drying.Successively toward add in beaker 75mL absolute ethyl alcohols,
100mL water, 3mL tetraethyl orthosilicates (TEOS) and 2mL methyl silicates (TMOS), use 1.0molL-1HCl adjusts pH to 6.0 left
The right side, stirring 6h at room temperature, to obtain precursor solution stand-by.Using precursor solution as electrolyte, the titanium-aluminium alloy for polishing cleaned tries
(titanium al atomic ratio is 3 to sample:1) negative electrode is used as, graphite electrode, which is used as, to be controlled in 5cm, control electric current density electrode, electrode spacing
For -5.0mAcm-2, sedimentation time 30s, working electrode deionized water rinsing is obtained after 150 DEG C of drying after the completion of deposition
To micro-nano oxide coating.Then, by the titanium-base alloy covered with micro-nano oxide coating in atmosphere at 700 DEG C
10min is heat-treated, that is, high temperature coatings are made；High temperature oxidation resistance is assessed with embodiment 1, and experimental result is listed in table 3.
3 naked TiAl alloy of table and the Ti covered with high temperature coatings3Al alloy sample experimental results
| Sample | Increase weight mg/cm2 |
| Naked TiAl alloy | 31.32 |
| Ti covered with high temperature coatings3Al alloys | 1.28 |
Embodiment 4
With sand paper, by titanium-aluminium alloy sample, (titanium al atomic ratio is 1 first:1) polishing removes oxide on surface, then successively
It is cleaned by ultrasonic 10min in acetone and ethanol, it is finally stand-by with hot blast drying.Successively toward add in beaker 50mL absolute ethyl alcohols,
50mL water, 5mL tetraethyl orthosilicates (TEOS), use 1.0molL-1HCl adjusts pH to 3.0 or so, stirs 4h at room temperature and obtains preceding body
Liquid solution is stand-by.Using precursor solution as electrolyte, (titanium al atomic ratio is 1 to the titanium-aluminium alloy sample for polishing cleaned:1) conduct
Negative electrode, graphite electrode, which is used as, to be controlled in 5cm electrode, electrode spacing, and control electric current density is -2.0mAcm-2, sedimentation time is
300s, working electrode deionized water rinsing is obtained into micro-nano oxide coating after 100 DEG C of drying after the completion of deposition.With
Afterwards, the titanium-base alloy covered with micro-nano oxide coating is heat-treated 30min at 650 DEG C in atmosphere, that is, is made anti-
High-temperature oxydation coating；High temperature oxidation resistance is assessed with embodiment 1, and experimental result is listed in table 4.
4 naked TiAl alloy of table and the TiAl alloy sample experiment result covered with high temperature coatings
Embodiment 5
Specific steps are with embodiment 4, except that changing the titanium-aluminium alloy matrix used, high temperature oxidation resistance is commented
Estimate same embodiment 1, experimental result is listed in table 5.
The different titanium-aluminium alloy matrix experimental results of table 5
| Sample | Increase weight mg/cm2 |
| Ti3-Al | 1.41 |
| Ti-Al3 | 0.74 |
| Ti-6Al-4V | 1.58 |
| Ti-47Al-2Cr-2Nb | 0.67 |
Embodiment 6
Specific steps are with embodiment 4, except that changing SiO2Electrodeposition time, respectively 100s, 200s,
300s、600s.High temperature oxidation resistance is assessed with embodiment 1, and experimental result is listed in table 6.
The different electrodeposition time experimental results of table 6
| Sample | Increase weight mg/cm2 |
| 100s | 16.02 |
| 200s | 1.59 |
| 300s | 0.29 |
| 600s | 0.44 |
Embodiment 7
Specific steps are with embodiment 4, except that changing SiO2Electro-deposition current density, it is respectively -0.1mAcm-2、-0.5mAcm-2、-1.0mAcm-2、-2.0mAcm-2、-5.0mAcm-2.High temperature oxidation resistance is assessed with embodiment 1, experiment
As a result it is listed in table 7.
The different electro-deposition current density experimental results of table 7
Embodiment 8
Specific steps are with embodiment 4, except that changing into platinized platinum to electrode.High temperature oxidation resistance is assessed with implementation
Example 1, experimental result are listed in table 8.
The different experimental results to electrode of table 8
| Sample | Increase weight mg/cm2 |
| Platinized platinum | 0.38 |
| Graphite | 0.29 |
Claims (7)
1. a kind of preparation method of titanium-base alloy high temperature coatings, comprises the following steps：
1) oxide on surface of titanium-based alloy matrix is removed first, is then cleaned, is dried；Described titanium-base alloy is the titanium containing aluminium
Based alloy；
2) it is (50-100) according to volume ratio:(50-100)：(1~10) mixes absolute ethyl alcohol, water and precursor alkyl silicate
Close, adjust pH of mixed to stir 2~48h at room temperature to 2.0~6.0, obtain precursor solution with acid；
3) precursor solution prepared is added in two slot electrodes, using titanium-based alloy matrix as working electrode, platinized platinum or graphite
Controlled as to electrode, electrode spacing in 1-10cm, control electric current density is -0.1mAcm-2~-5.0mAcm-2Carry out electricity
Deposition, sedimentation time is 30s~2000s, washes after 40~150 DEG C of drying, micro-nano oxidation is obtained on titanium-base alloy surface
Thing coating；
4) will be covered with the titanium-base alloy of micro-nano oxide coating in atmosphere at 600~700 DEG C heat treatment 10~
60min, that is, titanium-base alloy high temperature coatings are made.
2. preparation method as claimed in claim 1, it is characterised in that：Described titanium-base alloy is selected from Ti3-Al、Ti-Al、Ti-
Al3, one kind in Ti-6Al-4V, TiAlNb, Ti-47Al-2Cr-2Nb.
3. preparation method as claimed in claim 1, it is characterised in that：Described alkyl silicate is tetraethyl orthosilicate or positive silicon
Sour methyl esters.
4. the preparation method as described in one of claims 1 to 3, it is characterised in that：In step (3), current density for-
1.0mA·cm-2~-5.0mAcm-2。
5. the preparation method as described in one of claims 1 to 3, it is characterised in that：In step (3), sedimentation time 200s-
600s。
6. preparation method as claimed in claim 4, it is characterised in that：In step (3), sedimentation time 200s-600s.
7. the preparation method as described in one of claims 1 to 3 or 6, it is characterised in that：Described preparation method by step 1)~
Step 4) forms.
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| CN106835227B (en) * | 2016-12-05 | 2018-11-13 | 浙江工业大学 | A method of titanium-base alloy high temperature oxidation resistance is improved based on halide effect and ceramic coating |
| CN106906505B (en) * | 2016-12-31 | 2019-01-08 | 浙江工业大学 | A method of ceramic coating is obtained based on halide effect and pretreatment and improves titanium-base alloy high temperature oxidation resistance |
| CN106906504B (en) * | 2016-12-31 | 2019-01-18 | 浙江工业大学 | One kind being based on halide effect and SiO2The method of waterglass composite ceramic coat raising titanium-base alloy high temperature oxidation resistance |
| CN107910193B (en) * | 2017-11-13 | 2020-04-28 | 吉科猛 | Nano porous metal/metal oxide hybrid structure material, preparation and energy storage application |
| CN108102447B (en) * | 2017-11-25 | 2020-01-10 | 浙江大学 | Preparation method and application of silica-doped modified protective coating |
| CN108588771B (en) * | 2018-04-03 | 2020-06-30 | 浙江工业大学 | Composite ceramic coating containing noble metal intermediate layer and preparation process thereof |
| CN108588796B (en) * | 2018-04-09 | 2020-01-10 | 浙江工业大学 | Ceramic coating dispersed with noble metal particles and preparation process thereof |
| CN109402693B (en) * | 2018-10-25 | 2020-10-16 | 浙江大学 | Preparation method and application of corrosion inhibitor-loaded mesoporous silica super-hydrophobic film |
| JP2023531126A (en) * | 2020-07-01 | 2023-07-21 | エリコン サーフェス ソリューションズ アーゲー、 プフェフィコン | Protective layer against environmental influences (environmental barrier layer) for Ti-Al materials |
| CN112899756B (en) * | 2021-01-14 | 2022-07-26 | 中山大学·深圳 | Preparation method of titanium alloy SiOC coating |
| CN113278973B (en) * | 2021-05-24 | 2022-06-21 | 中山大学 | Titanium-based alloy part with nickel-modified silicon-based protective coating and preparation method thereof |
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| EP2048266A1 (en) * | 2007-10-10 | 2009-04-15 | Nederlandse Organisatie voor toegepast-natuurwetenschappelijk Onderzoek TNO | Corrosion protective layer |
| CN101270494B (en) * | 2008-05-08 | 2010-06-30 | 重庆大学 | Galvano-chemistry preparation method for metallic face protection ceramic film |
| CN102677092B (en) * | 2012-05-30 | 2015-01-14 | 浙江大学 | Preparation method of titanium anode |
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