CN100532645C - Hydrogen or hydrogen isotope infiltration resisting vitreous vallation layer for titanium or titanium alloy and preparation method thereof - Google Patents
Hydrogen or hydrogen isotope infiltration resisting vitreous vallation layer for titanium or titanium alloy and preparation method thereof Download PDFInfo
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- CN100532645C CN100532645C CNB200710191962XA CN200710191962A CN100532645C CN 100532645 C CN100532645 C CN 100532645C CN B200710191962X A CNB200710191962X A CN B200710191962XA CN 200710191962 A CN200710191962 A CN 200710191962A CN 100532645 C CN100532645 C CN 100532645C
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- titanium
- hydrogen
- titanium alloy
- barrier layer
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 56
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 56
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 29
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000010936 titanium Substances 0.000 title claims abstract description 29
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000008595 infiltration Effects 0.000 title claims abstract description 11
- 238000001764 infiltration Methods 0.000 title claims abstract description 11
- 239000011521 glass Substances 0.000 claims abstract description 29
- 230000004888 barrier function Effects 0.000 claims abstract description 23
- 238000005516 engineering process Methods 0.000 claims abstract description 16
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 7
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 7
- 229910021538 borax Inorganic materials 0.000 claims abstract description 7
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000010288 sodium nitrite Nutrition 0.000 claims abstract description 7
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 7
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims description 32
- 239000011248 coating agent Substances 0.000 claims description 31
- 239000000843 powder Substances 0.000 claims description 29
- 239000011734 sodium Substances 0.000 claims description 13
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- KWKXNDCHNDYVRT-UHFFFAOYSA-N dodecylbenzene Chemical compound CCCCCCCCCCCCC1=CC=CC=C1 KWKXNDCHNDYVRT-UHFFFAOYSA-N 0.000 claims description 4
- 239000010977 jade Substances 0.000 claims description 4
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 239000012466 permeate Substances 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- GBCAVSYHPPARHX-UHFFFAOYSA-M n'-cyclohexyl-n-[2-(4-methylmorpholin-4-ium-4-yl)ethyl]methanediimine;4-methylbenzenesulfonate Chemical compound CC1=CC=C(S([O-])(=O)=O)C=C1.C1CCCCC1N=C=NCC[N+]1(C)CCOCC1 GBCAVSYHPPARHX-UHFFFAOYSA-M 0.000 claims description 2
- 125000000914 phenoxymethylpenicillanyl group Chemical group CC1(S[C@H]2N([C@H]1C(=O)*)C([C@H]2NC(COC2=CC=CC=C2)=O)=O)C 0.000 claims description 2
- 230000000155 isotopic effect Effects 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 8
- 230000006866 deterioration Effects 0.000 abstract description 4
- 230000004927 fusion Effects 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 abstract 2
- 239000000428 dust Substances 0.000 abstract 2
- 229910052751 metal Inorganic materials 0.000 abstract 2
- 239000002184 metal Substances 0.000 abstract 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 abstract 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 abstract 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 abstract 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 abstract 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 229910001610 cryolite Inorganic materials 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000010422 painting Methods 0.000 abstract 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 17
- 239000011159 matrix material Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 239000000126 substance Substances 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002320 enamel (paints) Substances 0.000 description 4
- 239000007769 metal material Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 231100000987 absorbed dose Toxicity 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 229910052722 tritium Inorganic materials 0.000 description 1
Landscapes
- Glass Compositions (AREA)
Abstract
A glassiness wall barrier layer for resisting infiltration of hydrogen or hydrogen isotopic element and process for preparation which is used in titanium or titanium alloy belongs to the protecting technology for metal surface. The glassiness barrier layer mixes glass dust and mill addition into slip glaze, 50-180 um barrier layer is prepared by painting the slip glaze on the surface of titanium or titanium alloy, coefficient of linear thermal expansion of the glass dust and mismatch degree of titanium or titanium alloy base body are less than 5%, components according to the percent by weight comprises SiO2 45-50, B2O3 11-16, one or two kinds of Na2O and K2O 10-15, one or two kinds of BaO and CeO2 6-11, none or one or multiple kinds of MoO3, CaO and Na3AlF6 0-8.5, one or multiple kinds of residues such as Al2O3, Cr2O3, TiO2 and Sb2O3, and the mill addition comprises agglomerants such as kaolin, borax, sodium nitrite, CMC, PVA and the like and water. The invention has simple preparation technology, easy operation and low cost, which is suitable for industrial production. The invention has less heat expansion mismatch and good combination with base body, effectively prevents hydrogen or hydrogen isotopic element and oxygen and the like from infiltrating or permeating into metal base body, and avoids the deterioration of mechanical properties of the structure and material of titanium or titanium alloy, the deterioration of working environment and the waste of resources in fusion reactor.
Description
Technical field:
The present invention relates to surface protection technique, a kind of prevention hydrogen isotope infiltration of structural metallic materials and top coat technology of thermal etching of being used for is provided especially.
Background technology:
In thermonuclear weapon and controllable thermonuclear reaction heap technology, hydrogen and isotropic substance thereof are main fuels the most, in military nuclear technique and fusion energy resource field critical role are arranged.Hydrogen also is one of of paramount importance green energy resource simultaneously, and the material of its transportation and storage and technology are also most important for a large amount of uses of this green energy resource.And hydrogen and isotropic substance thereof have strong perviousness in most of metallic substance, hydrogen and radioisotopic leakage thereof not only will cause the fuel charging capacity to increase, cause serious economy loss, and environment caused radiocontamination, personnel under this environment cause serious personal injury for long term operation, hydrogen embrittlement very easily takes place in the structural metallic materials of long service under high concentration of hydrogen and isotopic severe environment thereof simultaneously, and the mechanical property that causes material worsens, and causes immeasurable serious consequence.Therefore, fusion reactor structured material and hydrogen and isotopic transportation thereof and storage must have alap hydrogen and isotopic rate of permeation thereof with structured material.Hydrogen and isotropic substance thereof rate of permeation in most of stupaliths is very low, but the fragility and the non-compactness of pottery have limited its application.Therefore, generally acknowledge solution in the world, guaranteeing that material structure performance ground is suppressing hydrogen and isotopic infiltration thereof simultaneously what structural metallic materials surface preparation pottery anti-tritium diffusion layer had become this problem.
Study more ceramic barrier layer such as Al now
2O
3, Cr
2O
3, TiO
2, the subject matter that exists of TiC, TiN, SiC and their compound coating is that thermal expansivity (TEC) exists big mismatch with matrix, after being subjected to certain thermal shocking, produce bigger thermal stresses between coating and the matrix, and be easy to cause that coating separates with matrix, influence the resistance hydrogen of coating and the wall effect of isotopic osmosis thereof.And the preparation technology of partial coating and equipment requirements are higher, and production cost is higher, unfavorable with realize producing in enormous quantities.And seek a kind of can be good with matrix bond, the preparation technology that coefficient of thermal expansion mismatch is little is simple, novel hydrogen and isotopic osmosis barrier layer thereof with low cost have important science and practical significance.
Enamel coating is except that the performance of the many excellences with traditional ceramics coating; as high temperature resistance and chemical corrosion resistance, wear resistance and decorate properties; the most outstanding characteristics of enamel coating are that coating has the adjustable advantage of composition; it can be according to application prospect, performance requriements and the basic material of coating different; adjust the chemical constitution of coating by composition design, preparation is good with matrix bond to reach, the good enamel protective layer that satisfies service requirements of thermal shock resistance of matched coefficients of thermal expansion.And the preparation technology of coating is simple, with low cost, is suitable for the workpiece of different shape, possesses the background that quite sophisticated large-scale industrialization is produced again.Existing patent also mainly is at high temperature resistance and chemical corrosion and surface decoration, as 98114349.0,02109842.5,200510046720.2,200510046367.8,200510046363.X and patents such as 96102719.3.
Summary of the invention:
The object of the present invention is to provide a kind of coating, it can prepare with matrix bond good by simple process cheaply, and titanium that coefficient of thermal expansion mismatch is little or titanium alloy are with the glassiness barrier layer of novel resistance hydrogen or hydrogen isotope infiltration.
The invention provides a kind of titanium or the titanium alloy glassiness barrier layer with resistance hydrogen isotope infiltration, it is characterized in that: this glassiness barrier layer is to make by glass powder and mill addition are mixed and made into glaze slip, is made up of following by weight:
100 parts glass powder, mill addition is respectively by weight:
The kaolin of 3-6 part,
Borax of 2-5 part and in the Sodium Nitrite one or both,
0.1-1 CMC, PVA, sodium polyacrylate, n-Octanol, propyl carbinol, the dodecylbenzene semi-annular jade pendant of part
In the acid sodium one or more,
Water of 80-110 part or dehydrated alcohol,
The thermal linear expansion coefficient of used glass powder and titanium or titanium alloy substrate mismatch degree are less than 5%, and moiety is as follows by weight percentage:
45-50 SiO
2，
11-16 B
2O
3，
10-15 Na
2O and K
2Among the O one or both,
6-11 BaO and CeO
2In one or both,
0-8.5 MoO
3, CaO and Na
3AlF
6In not or one or more are arranged,
Surplus Al
2O
3, Cr
2O
3, TiO
2And Sb
2O
3In one or more.
Titanium of the present invention or the titanium alloy preparation method of the glassiness barrier layer of resistance hydrogen or hydrogen isotope infiltration, it is characterized in that: glass powder and mill addition are carried out ball milling be mixed and made into glaze slip, glaze slip is coated in titanium or titanium alloy surface makes powder coating by filming technology, the powder coating drying is placed in the air furnace under 900-1100 ℃ and fuses 15-30min, air cooling finally makes the thick glassiness barrier layer of 50-180 μ m at titanium or titanium alloy surface to room temperature.
The glassiness barrier layer that titanium of the present invention or titanium alloy permeate with resistance hydrogen or hydrogen isotope, it is characterized in that: glassiness barrier layer combines well with titanium or titanium alloy substrate, be Chemical bond, the thermal linear expansion coefficient of used glass powder and titanium or titanium alloy substrate mismatch degree be less than 5%, the thermal shock resistance excellence.
Glassiness barrier layer of the present invention in other hydrogen isotope infiltration barrier layer not only preparation technology simple, with low cost, burn till in air and finish, be suitable for suitability for industrialized production, and can stop hydrogen or hydrogen isotope and oxygen etc. to be penetrated into titanium or titanium alloy substrate effectively, and cause titanium or the deterioration of titanium alloy structure material mechanical performance, Working environment deterioration and the wasting of resources in the fusion reactor.
Description of drawings
Fig. 1 is (a) industrially pure titanium TA1 matrix, and (b) 700 ℃ of oxidation half an hour, what (c) three samples that are coated with glass coating carried out under 550 ℃, the hydrogen pressure of 5000Pa respectively that 1.5h fills the hydrogen test fills the hydrogen curve
Fig. 2 to be no matrix TE94 enamel coating carry out under 550 ℃, the hydrogen pressure of 5000Pa 1.5h fills hydrogen test fill the hydrogen curve
Embodiment:
Example 1
Sample TA1 plate is of a size of 30mm * 20mm * 3mm; The composition of the used TE94 type of glass coating glass powder is as follows by weight percentage:
48.81 SiO
2
11.58 B
2O
3
12.02 Na
2O and K
2O, both proportionings are about 3:1
10.55 BaO
8.11 CaO and Na
3AlF
6, both proportionings are about 3:1
Surplus Al
2O
3And TiO
2, both proportionings are about 1.7:1
Will be as follows according to glass powder and mill addition prescriptions by weight such as water, binding agent and fusing assistant that above composition makes:
100 parts glass powder
3 parts kaolin
4.3 the borax and the Sodium Nitrite of part, both proportionings are about 10:1
0.5 the CMC and the n-Octanol of part, both proportionings are about 2:1
100 parts water
Carry out ball milling and be mixed and made into slurry, preparing powder coating by simple filming technology through chamfering and surface-treated titanium or titanium alloy surface then, sintering 30min in the muffle furnace of back 950 ℃ under, the taking-up air cooling is to room temperature.And carry out the glassiness barrier layer that twice same operation makes 100 micron thickness.
Example 2
Sample TC4 plate is of a size of 30mm * 20mm * 3mm; The composition of the used TE89 type of glass coating glass powder is as follows by weight percentage:
45.89 SiO
2
15.03 B
2O
3
14.63 Na
2O and K
2O, both proportionings are about 4:3
7.31 BaO and CeO
2, both proportionings are about 5:1
5.8 MoO
3
Surplus Al
2O
3And Sb
2O
3, both proportionings are about 1:1
Will be as follows according to glass powder and mill addition prescriptions by weight such as water, binding agent and fusing assistant that above composition makes:
100 parts glass powder
3 parts kaolin
4.3 the borax and the Sodium Nitrite of part, both proportionings are about 10:1
0.5 the CMC and the propyl carbinol of part, both proportionings are about 2:1
100 parts water
Carry out ball milling and be mixed and made into slurry, preparing powder coating by simple filming technology through chamfering and surface-treated titanium or titanium alloy surface then, sintering 30min in the muffle furnace of back 970 ℃ under, the taking-up air cooling is to room temperature.And carry out three same operations and make 180 microns glassiness barrier layer.
Example 3
Sample TA1 plate is of a size of 30mm * 20mm * 3mm; The composition of the used TE90 type of glass coating glass powder is as follows by weight percentage:
45.74 SiO
2
14.98 B
2O
3
14.58 Na
2O and K
2O, both proportionings are about 3:2
7.29 BaO and CeO
2, both proportionings are about 5:1
Surplus Al
2O
3, Cr
2O
3And Sb
2O
3, three's proportioning is about 1:1:1
The glass powder and the mill addition prescriptions by weight such as water, binding agent and fusing assistant that will make according to above composition are:
100 parts glass powder
3 parts kaolin
4.3 part borax and Sodium Nitrite, both proportionings are about 10:1
1 part sodium polyacrylate, n-Octanol and dodecylbenzene semi-annular jade pendant acid sodium, the three joins
Than being about 3:2:5
100 parts water
Carry out ball milling and be mixed and made into slurry, preparing powder coating by simple filming technology through chamfering and surface-treated titanium or titanium alloy surface then, sintering 30min in the muffle furnace of back under 970 ℃ takes out air cooling to room temperature, makes the glassiness barrier layer of 50 micron thickness.
Example 4
Sample TA1 plate is of a size of 30mm * 20mm * 3mm; The composition of the used TE88 type of glass coating glass powder is as follows by weight percentage:
48.73 SiO
2
14.7 B
2O
3
15.28 Na
2O and K
2O, both proportionings are about 3:2
6.21 BaO and CeO
2, both proportionings are about 2:1
Surplus Al
2O
3, TiO
2And Sb
2O
3, three's proportioning is about glass powder and the mill addition prescriptions by weight such as water, binding agent and fusing assistant that 6:4:5 will make according to above composition and is:
100 parts glass powder
3 parts kaolin
4.3 the borax and the Sodium Nitrite of part, both proportionings are about 10:1
0.5 the dodecylbenzene semi-annular jade pendant of part acid sodium
90 parts dehydrated alcohol
Carry out ball milling and be mixed and made into slurry, preparing powder coating by simple filming technology through chamfering and surface-treated titanium or titanium alloy surface then, sintering 30min in the muffle furnace of back 970 ℃ under, the taking-up air cooling is to room temperature.And carrying out twice same operation, to make thickness be 100 microns glassiness barrier layer.
By the made glass coating surfacing of above example, dense structure, thickness is 50-180 μ m, draw coating and matrix mortise through titanium or titanium alloy/vitreous coating interface in conjunction with situation analysis and fall sphere test detection, and 550 ℃ of following shrends, cycling hot is impacted 50 coatings does not have cracking phenomena to occur.Fill resistance hydrogen or the hydrogen isotope infiltration wall effect that hydrogen is tested to check coating by carrying out 1.5h under 550 ℃, the hydrogen pressure of 5000Pa, the result as depicted in figs. 1 and 2, curve a shows that the saturation balance pressure of filling the hydrogen curve of the TA1 sample of handling through the deoxidation film is minimum among Fig. 1, otherwise hydrogen absorbed dose maximum in the three of the TA1 sample of handling through the deoxidation film then is described; Curve b be have annealed oxide film the TA1 sample fill the hydrogen curve, its saturation balance is pressed and is between curve a and the curve c, and a is significantly increased than curve, thereby its hydrogen obviously reduces than curve a as can be known, also just illustrates that TA1 has certain resistance hydrogen wall effect at the oxide film that 700 ℃ of backs of annealing down produce.And preparation has the saturation balance of the TA1 sample of TE94 vitreous coating to press maximum, illustrate that its saturated hydrogen is minimum, shown in curve c among Fig. 1, fill the hydrogen curve in conjunction with what the TE94 vitreous coating of no matrix shown in Figure 2 carried out under 550 ℃, the hydrogen pressure of 5000Pa that 1.5h fills the hydrogen test, can know a small amount of suction hydrogen shown in the c curve among Fig. 1 because the prepared vitreous coating in titanium or titanium alloy-based surface is inhaled due to the hydrogen, and be not penetrated on the matrix, this just proves that also enamel coating has very strong resistance hydrogen isotope infiltration wall effect.
Claims (2)
1, a kind of titanium or titanium alloy are with hindering the glassiness barrier layer that hydrogen or hydrogen isotope permeate, and it is characterized in that: this glassiness barrier layer comprises glass powder and mill addition, is made up of following by weight:
100 parts glass powder, mill addition is respectively by weight:
The kaolin of 3-6 part,
Borax of 2-5 part and Sodium Nitrite one or both,
0.1-1 CMC, PVA, sodium polyacrylate, n-Octanol, propyl carbinol and the dodecylbenzene semi-annular jade pendant of part
In the acid sodium one or more,
Water of 80-110 part or dehydrated alcohol,
The thermal linear expansion coefficient of described glass powder and titanium or titanium alloy substrate mismatch degree are less than 5%, and moiety is as follows by weight percentage:
45-50 SiO
2，
11-16 B
2O
3，
10-15 Na
2O and K
2Among the O one or both,
6-11 BaO and CaO
2In one or both,
0-8.5 MoO
3, CaO and Na
3AlF
6In one or more are arranged,
Surplus Al
2O
3, Cr
2O
3, TiO
2And Sb
2O
3In one or more.
2, described titanium of a kind of claim 1 or the titanium alloy preparation method of the glassiness barrier layer of resistance hydrogen or hydrogen isotope infiltration, it is characterized in that: glass powder and mill addition are carried out ball milling be mixed and made into glaze slip, glaze slip is coated in titanium or titanium alloy surface makes powder coating by filming technology, the powder coating drying is placed in the air furnace under 900-1100 ℃ and fuses 15-30min, air cooling finally makes the thick glassiness barrier layer of 50-180 μ m at titanium or titanium alloy surface to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200710191962XA CN100532645C (en) | 2007-12-27 | 2007-12-27 | Hydrogen or hydrogen isotope infiltration resisting vitreous vallation layer for titanium or titanium alloy and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200710191962XA CN100532645C (en) | 2007-12-27 | 2007-12-27 | Hydrogen or hydrogen isotope infiltration resisting vitreous vallation layer for titanium or titanium alloy and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101215710A CN101215710A (en) | 2008-07-09 |
| CN100532645C true CN100532645C (en) | 2009-08-26 |
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|---|---|---|---|
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|---|---|
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| CN106191727A (en) * | 2016-06-30 | 2016-12-07 | 西北有色金属研究院 | A kind of surface treatment method of titanium alloy thin material |
| CN107777873B (en) * | 2016-08-29 | 2020-09-08 | 深圳南玻应用技术有限公司 | Light guide plate glass and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5298332A (en) * | 1989-08-21 | 1994-03-29 | Corning Incorporated | Glass-ceramic coatings for titanium-based metal surfaces |
| CN1465745A (en) * | 2002-06-14 | 2004-01-07 | 中国科学院金属研究所 | Method of risisting high-temp. oxidation and heat corrosion for high-temp. alloy |
| CN1718641A (en) * | 2005-06-21 | 2006-01-11 | 沈阳工业大学 | Enamel powder for electrophoresis coating and its preparation |
-
2007
- 2007-12-27 CN CNB200710191962XA patent/CN100532645C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5298332A (en) * | 1989-08-21 | 1994-03-29 | Corning Incorporated | Glass-ceramic coatings for titanium-based metal surfaces |
| CN1465745A (en) * | 2002-06-14 | 2004-01-07 | 中国科学院金属研究所 | Method of risisting high-temp. oxidation and heat corrosion for high-temp. alloy |
| CN1718641A (en) * | 2005-06-21 | 2006-01-11 | 沈阳工业大学 | Enamel powder for electrophoresis coating and its preparation |
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