CN100445427C - Production of titanium and titanium-alloy glass ceramic coating - Google Patents
Production of titanium and titanium-alloy glass ceramic coating Download PDFInfo
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- CN100445427C CN100445427C CNB2005100480334A CN200510048033A CN100445427C CN 100445427 C CN100445427 C CN 100445427C CN B2005100480334 A CNB2005100480334 A CN B2005100480334A CN 200510048033 A CN200510048033 A CN 200510048033A CN 100445427 C CN100445427 C CN 100445427C
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- 239000002241 glass-ceramic Substances 0.000 title claims abstract description 42
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000010936 titanium Substances 0.000 title claims abstract description 34
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 32
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 32
- 238000005524 ceramic coating Methods 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title abstract 2
- 239000000843 powder Substances 0.000 claims abstract description 33
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011521 glass Substances 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 13
- 239000000956 alloy Substances 0.000 claims abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims description 27
- 239000011248 coating agent Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 13
- 238000005488 sandblasting Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 8
- 235000011194 food seasoning agent Nutrition 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 229910000883 Ti6Al4V Inorganic materials 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 230000004927 fusion Effects 0.000 claims description 2
- 230000004071 biological effect Effects 0.000 abstract description 8
- 239000007943 implant Substances 0.000 abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-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
- 238000007664 blowing Methods 0.000 abstract 1
- 230000008468 bone growth Effects 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000002386 leaching Methods 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- 239000004576 sand Substances 0.000 abstract 1
- 210000000988 bone and bone Anatomy 0.000 description 14
- 239000012890 simulated body fluid Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 9
- 238000001228 spectrum Methods 0.000 description 8
- 230000012010 growth Effects 0.000 description 6
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 6
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 6
- 210000001519 tissue Anatomy 0.000 description 6
- 239000011575 calcium Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 239000011435 rock Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 231100000614 poison Toxicity 0.000 description 3
- 230000007096 poisonous effect Effects 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000002513 implantation Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000007750 plasma spraying Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000017423 tissue regeneration Effects 0.000 description 2
- 229910014497 Ca10(PO4)6(OH)2 Inorganic materials 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 206010039361 Sacroiliitis Diseases 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 239000003462 bioceramic Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 210000000629 knee joint Anatomy 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 210000002381 plasma Anatomy 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
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- Prostheses (AREA)
Abstract
Production of titanium and titanium alloy glass ceramic coating is carried out by mixing raw materials, drying, heating while melting, press to prepare glass, grinding into powder, adding into methanol to prepare slurry, sand blowing by alumina, immersing pure titanium, Ti6A14V, Ti29Nb13Ta4.6Zr and Ti24Nb4Zr7.6Sn alloy into mixed solution, leaching and high-temperature sintering to obtain the final product. The glass ceramic consists of CaO and P205 80-90mol%, Na2O 4-7mol%, TiO2 and ZrO2 residues. It is non-toxic, has better biological activity and binding ability. It can be used to induce implant surface bone growth.
Description
Technical field:
The present invention relates to biological coating field and glass-ceramic field, surface active coating preparation field when particularly relating to titanium or titanium alloy as hard tissue repair and equivalent material is specially a kind of method for preparing the titanium or titanium alloy glass ceramic coating.
Background technology:
In developed country, sacroiliitis and fracture are the one of the main reasons that causes the elderly to walk.In Japan, replace the operation of artificial femoral joint and artificial knee joint and just reach 100,000 examples every year, so joint prosthesis and artificial bone that the market development has a quality steady in a long-term have great importance.Document [1]: Li Qing sees reference. and the titanium alloy surface coatings applications is in the research of biological bone. biological orthopaedics material and clinical study .2004,1[3]: 45-49.Titanium or titanium alloy becomes important hard tissue repair and equivalent material because of its excellent mechanical property, corrosion resistance and excellent biological compatibility.Yet titanium or titanium alloy belongs to bio-inert material, and when it was directly implanted as planting body, the surface can be surrounded by the collagen protein of organism, with planting body and biological scleroseptum from, implantation for a long time causes loosening easily, is difficult to and biological bone forming mortise.Artificial growth body and the synestotic prerequisite of biological bone forming are: the artificial growth body in vivo, its surface will form and the similar phosphatic rock of osseous tissue.In a single day the artificial growth surface has formed and the similar phosphatic rock of biological osseous tissue, it is foreign matter that biological cell just can not identify it, and with its be considered as the similar of biological bone and with the damage biological bone grow, plant the bone grafting sprout cell from the teeth outwards apace, just formed firm Chemical bond between the phosphatic rock of biological bone and the phosphatic rock of artificial growth surface, last and biological bone becomes one.Document [2]: L.L.Hench sees reference, R.J.Splinter, W.C.Allen and T.K.Greenlee.Bonding mechanisms at the interface of ceramic prosthetic materials.Journalof Biomedical Materials Research Symposium.1971,2:117-141.Discover 45S5
Bio-vitric (Na
2O-CaO-SiO
2-P
2O
5System), Ceravital devitrified glass (Na
2O-K
2O-MgO-CaO-P
2O
5-SiO
2System), A-W biological glass ceramic (MgO-CaO-SiO
2-P
2O
5System), (HA consists of the hydroxyapatite bioactive pottery: Ca
10(PO
4)
6(OH)
2) or the like in the implantable bioartificial body, can not coated by the fibering film, can be in the bone forming mortise.Document [3] sees reference: L.L.Hench.Bioceramics.Journal of American Ceramics Society.1998,81[7]: 1705-1728.Therefore, if can then can bring into play the metal excellent mechanical property, make the surface have characteristics such as biocompatibility and biological activity again in titanium or titanium alloy surface preparation one deck biological glass ceramic coating.Plasma spraying hydroxyapatite is the method for preparing activated coating commonly used clinically.But plasma spraying at high temperature carries out, and coated component and crystalline structure are restive, and the equipment requirements height, the cost costliness, and long-term the implantation has loosening tendency.Document [4] sees reference: F.Li, Q.L.Feng
Z.Cui, H.D.Li and H.Schubert.A simple biomimeticmethod for calcium phosphate coating.Surface and Coatings Technology, 2002,154:88-93.
The present invention be based upon on the existing glass-ceramic basis (number of patent application: 200510047283.6, application is said: 2005.9.28), adopt simple technology, low cost equipment in the titanium or titanium alloy surface preparation glass ceramic coating.This glass ceramic coating does not contain SiO
2, there is not poisonous element, have good biological activity.Simultaneously, this coating has higher Ca/P ratio and the composition similar with human body hard tissue, can be used as human body hard tissue and substitutes and repair materials.When this coating is implanted as implant, be expected to bring into play good mechanical property of titanium or titanium alloy and the good biological activity of coating, be expected the faster growth that guides new bone more strongly.
Summary of the invention:
The purpose of this invention is to provide a kind of method for preparing the titanium or titanium alloy glass ceramic coating.The coating that adopts this method to obtain does not contain SiO
2, there is not poisonous element, have good biological activity, it has similar composition with human body hard tissue, can be used as human body
Tissue substitute and repair materials.
Technical scheme of the present invention is:
The invention provides a kind of method for preparing the titanium or titanium alloy glass ceramic coating, the preparation of coating comprises the coating and the sintering of the preparation of glass ceramic powder, titanium or titanium alloy pre-treatment and coating, and concrete steps are as follows:
(1) preparation of glass ceramic powder
Used glass-ceramic is CaO-P
2O
5-Na
2O-TiO
2-ZrO
2Glass ceramic powder, the consisting of of glass ceramic powder: CaO and P
2O
5Total content is at 80～90mol%, Na
2The content of O is at 4～7mol%, and all the other are TiO
2And ZrO
2, Ca and P mol ratio are 0.5～1.5, ZrO
2Content at 0.5～10mol%; With CaCO
3, Na
2CO
3, TiO
2, ZrO
2And H
3PO
4Be raw material, by described composition raw material mixed that the formulate glass slurries are smashed into 5～10 μ m powder after drying to pieces, be heated to 1300～1400 ℃ of fusions and insulation, soaking time is 0.5～1 hour; Take out then and be poured on that punching press gets glass-ceramic on the stainless-steel sheet, the gained glass sphere is worn into 1～10 μ m powder promptly get glass
Ceramic powder;
(2) titanium or titanium alloy pre-treatment
Through the aluminum oxide sandblasting, reaching surfaceness is 1～5 μ m with the titanium or titanium alloy alloy;
(3) coating of coating and sintering
Ball milling gained glass ceramic powder is made into methanol slurry, the titanium or titanium alloy after the sandblasting is immersed fully, lixiviate then, in air after the seasoning in resistance furnace sintering.
Described glass-ceramic concentration of methanol solution is 0.01～2M, and lixiviate speed is 0.5～5mm/s, and sintering temperature is respectively 700～900 ℃, and sintering time is 0.5～3 hour.
Titanium or titanium alloy of the present invention adopts pure titanium, Ti6Al4V, Ti29Nb13Ta4.6Zr or Ti24Nb4Zr7.6Sn.
The coating that adopts the inventive method preparation main component behind 700 ℃, 800 ℃ and 900 ℃ of sintering is β-Ca
3(PO
4)
2And β-Ca
2P
2O
7
Adopt the coating of the inventive method preparation to have good biological activity, soaking in simulated body fluid (SBF) promptly had hydroxyapatite to generate in 4 days.
The coating of employing the inventive method preparation and titanium or titanium alloy basal body binding force are greater than 15MPa.
The invention has the beneficial effects as follows:
Glass ceramic coating of the present invention does not contain SiO
2, there is not poisonous element, have good biological activity, soaking in simulated body fluid promptly had hydroxyapatite to generate in 4 days; This coating and titanium or titanium alloy matrix have than high-bond (greater than 15MPa).This coating has higher Ca/P ratio and the composition similar with human body hard tissue, can be used as human body hard tissue and substitutes and repair materials.When this coating is implanted as implant, be expected to bring into play good mechanical property of titanium or titanium alloy and the good biological activity of coating, be expected the faster growth that guides new bone more strongly.
Description of drawings:
Fig. 1 glass powder 2# the pure titanium surface-coated after the sandblast and behind 700 ℃ of sintering pattern in kind;
Fig. 2 glass powder 2# after sandblast pure titanium surface-coated and at 700 ℃ of sintering rear surface X-ray diffracting spectrums;
Fig. 3 glass powder 4# after sandblast Ti6Al4V alloy slice surface-coated and at 900 ℃ of sintering rear surface X-ray diffracting spectrums;
Fig. 4 glass powder 9# after sandblast Ti24Nb4Zr7.6Sn alloy slice surface-coated and at 800 ℃ of sintering rear surface X-ray diffracting spectrums;
Fig. 5 glass powder 9# after sandblast Ti24Nb4Zr7.6Sn alloy slice surface-coated and at 800 ℃ of agglomerating surface topography maps;
Fig. 6 glass powder 9# is at Ti24Nb4Zr7.6Sn alloy slice surface-coated after the sandblast and the surface topography map 800 ℃ of sintering soak 4 days then in simulated body fluid (SBF) after;
Fig. 7 glass powder 3# is at Ti29Nb13Ta4.6Zr alloy slice surface-coated after the sandblast and the surface topography map 800 ℃ of sintering soak 4 days then in simulated body fluid (SBF) after;
Fig. 8 glass powder 3# is at Ti29Nb13Ta4.6Zr alloy slice surface-coated after the sandblast and the surperficial X-ray diffracting spectrum 800 ℃ of sintering soak 4 days then in simulated body fluid (SBF) after.
Embodiment:
Embodiment 1
Use analytical pure CaCO
3, Na
2CO
3, TiO
2, ZrO
2And H
3PO
4(weight concentration 85%) presses the described 1～10# composition of table 1 glass pulp for preparation of raw material, with electric blender raw material mixed, and places 50 ℃ of loft drier inner drying 24h then.Raw material after the drying is smash powdered (granularity is 5-10 μ m) place the inherent 1350 ℃ of insulation 0.5h of platinum crucible, taking-up immediately is poured on the stainless-steel sheet and quick punching press promptly gets glass.
Table 1CaO-P
2O
5-Na
2O-TiO
2-ZrO
2The glass composition
Embodiment 2
Gained glass 2# ball milling is become powder (granularity is 1～10 μ m).The glass-ceramic powder is made into the 0.01M methanol slurry, pure titanium rod is inserted with the fine rule suspension after particle diameter is 0.5mm aluminum oxide sandblasting (surfaceness is 1 μ m), to carry on the 1mm/s speed, in air, be incubated 1 hour at 700 ℃ of resistance furnaces after the seasoning, furnace cooling.Grand design in kind as shown in Figure 1, its coatingsurface X-ray diffracting spectrum is as shown in Figure 2.
Embodiment 3
Gained glass 4# ball milling is become powder (granularity is 1～10 μ m).The glass-ceramic powder is made into the 2M methanol slurry, the Ti6Al4V alloy slice is inserted with the fine rule suspension after particle diameter is 3mm aluminum oxide sandblasting (surfaceness is 5 μ m), to carry on the 5mm/s speed, in air, be incubated 1 hour at 900 ℃ of resistance furnaces after the seasoning, furnace cooling.Its coatingsurface X-ray diffracting spectrum as shown in Figure 3.
Embodiment 4
Gained glass 9# ball milling is become powder (granularity is 1～10 μ m).The glass-ceramic powder is made into the 0.05M methanol slurry, the Ti24Nb4Zr7.6Sn alloy slice is inserted with the fine rule suspension after particle diameter is 2mm aluminum oxide sandblasting (surfaceness is 2.5 μ m), to carry on the 2mm/s speed, in air, be incubated 1 hour at 800 ℃ of resistance furnaces after the seasoning, furnace cooling.Its coatingsurface X-ray diffracting spectrum as shown in Figure 4.
Embodiment 5
37 ℃ of immersions are after 4 days in simulated body fluid (table 2) with embodiment 4 gained glass ceramic coatings, and the surface has hydroxyapatite to generate.Microscopic appearance soaked the back microscopic appearance as shown in Figure 6 as shown in Figure 5 before it soaked.
Ionic concn (mM) in blood plasma in table 2 human body and the simulated body fluid (SBF)
Embodiment 6
Gained glass 3# ball milling is become powder (granularity is 1～10 μ m).The glass-ceramic powder is made into the 0.05M methanol slurry, the Ti29Nb13Ta4.6Zr alloy slice is inserted with the fine rule suspension after particle diameter is 2mm aluminum oxide sandblasting (surfaceness is 2.5 μ m), to carry on the 1mm/s speed, in air, be incubated 1 hour at 800 ℃ of resistance furnaces after the seasoning, furnace cooling.37 ℃ of immersions are after 4 days in simulated body fluid (table 2) then, and the surface has hydroxyapatite to generate, and its pattern such as Fig. 7 show that surperficial X-ray diffracting spectrum as shown in Figure 8.
The Ti24Nb4Zr7.6Sn alloy is processed into 5 * 5 * 30mm sample, after 1mm aluminum oxide sandblasting (surfaceness is 1.5 μ m), insert in the glass-ceramic slurries that the 0.05M composition is 2# with the fine rule suspension, to carry on the 2mm/s speed, in air, be incubated 1 hour at 800 ℃ of resistance furnaces after the seasoning, furnace cooling.The stainless steel steel epoxy resin E-44 adhesive solidification of coat side and same size.This sample is in the test of MTS stretching experiment machine, and breaking tenacity is 15MPa, and fracture occurs in Resins, epoxy one side.
Claims (4)
1, a kind of method for preparing the titanium or titanium alloy glass ceramic coating is characterized in that: the preparation of coating comprises the coating and the sintering of the preparation of glass ceramic powder, titanium or titanium alloy pre-treatment and coating, and concrete steps are as follows:
(1) preparation of glass ceramic powder
Used glass-ceramic is CaO-P
2O
5-Na
2O-TiO
2-ZrO
2Glass ceramic powder, the consisting of of glass ceramic powder: CaO and P
2O
5Total content is at 80～90mol%, Na
2The content of O is at 4～7mol%, and all the other are TiO
2And ZrO
2, Ca and P mol ratio are 0.5～1.5, ZrO
2Content at 0.5～10mol%; With CaCO
3, Na
2CO
3, TiO
2, ZrO
2And H
3PO
4Be raw material, by described composition raw material mixed that the formulate glass slurries are smashed into 5～10 μ m powder after drying to pieces, be heated to 1300～1400 ℃ of fusions and insulation, soaking time is 0.5～1 hour; Take out then and be poured on that punching press gets glass-ceramic on the stainless-steel sheet, the gained glass sphere is worn into 1～10 μ m powder promptly get glass ceramic powder;
(2) titanium or titanium alloy pre-treatment
Through the aluminum oxide sandblasting, reaching surfaceness is 1～5 μ m with the titanium or titanium alloy alloy;
(3) coating of coating and sintering
Ball milling gained glass ceramic powder is made into methanol slurry, the titanium or titanium alloy after the sandblasting is immersed fully, lixiviate then, in air after the seasoning in resistance furnace sintering.
2, according to the described method for preparing the titanium or titanium alloy glass ceramic coating of claim 1, it is characterized in that: in the described step 2, the aluminum oxide particle diameter is 0.5～3mm.
3, according to the described method for preparing the titanium or titanium alloy glass ceramic coating of claim 1, it is characterized in that: in the described step 3, described glass-ceramic concentration of methanol solution is 0.01～2M, lixiviate speed is 0.5～5mm/s, sintering temperature is respectively 700～900 ℃, and sintering time is 0.5～3 hour.
4, according to the described method for preparing the titanium or titanium alloy glass ceramic coating of claim 1, it is characterized in that: titanium or titanium alloy adopts pure titanium, Ti6Al4V, Ti29Nb13Ta4.6Zr or Ti24Nb4Zr7.6Sn.
Priority Applications (1)
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|---|---|---|---|
| CNB2005100480334A CN100445427C (en) | 2005-12-16 | 2005-12-16 | Production of titanium and titanium-alloy glass ceramic coating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100480334A CN100445427C (en) | 2005-12-16 | 2005-12-16 | Production of titanium and titanium-alloy glass ceramic coating |
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|---|---|
| CN1982504A CN1982504A (en) | 2007-06-20 |
| CN100445427C true CN100445427C (en) | 2008-12-24 |
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| CNB2005100480334A Expired - Fee Related CN100445427C (en) | 2005-12-16 | 2005-12-16 | Production of titanium and titanium-alloy glass ceramic coating |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI477388B (en) * | 2012-07-04 | 2015-03-21 | Darfon Materials Corp | Method of fabricating casing and casing therefrom |
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| CN100587115C (en) * | 2007-12-27 | 2010-02-03 | 南京航空航天大学 | Self-peeling vitreous coating preventing hydrogen permeation for titanium or titanium alloy and preparation method thereof |
| CN101618230B (en) * | 2008-07-01 | 2013-03-27 | 叶南辉 | Method for manufacturing biomedical glass ceramic material |
| CN101884807B (en) * | 2010-06-24 | 2013-06-26 | 同济大学 | Preparation method for borate antibacterial glass coating with bioactivity and application thereof |
| CN102230100B (en) * | 2011-07-01 | 2013-03-06 | 湖南科技大学 | Method for preparing Ti-Nb-Zr-Sn alloy by using powder metallurgical process |
| CN102886072A (en) * | 2012-10-09 | 2013-01-23 | 天津大学 | Degraded glass ceramic thin film for medical magnesium alloy surface and preparation method of degraded glass ceramic thin film |
| CN103469207B (en) * | 2013-08-16 | 2015-06-03 | 中国科学院金属研究所 | High-temperature oxidation resistant and corrosion resistant glass ceramic composite coating and preparation technology thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5178901A (en) * | 1989-12-02 | 1993-01-12 | Agency Of Industrial Science & Technology | Titanium metal-coating material, method for production thereof, method for coating therewith, and product coated therewith |
| US5196381A (en) * | 1990-01-16 | 1993-03-23 | E. I. Du Pont De Nemours And Company | Metaphosphate glass composition |
| US6130178A (en) * | 1998-04-16 | 2000-10-10 | Corning Incorporated | Strong miserite glass-ceramics |
-
2005
- 2005-12-16 CN CNB2005100480334A patent/CN100445427C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5178901A (en) * | 1989-12-02 | 1993-01-12 | Agency Of Industrial Science & Technology | Titanium metal-coating material, method for production thereof, method for coating therewith, and product coated therewith |
| US5196381A (en) * | 1990-01-16 | 1993-03-23 | E. I. Du Pont De Nemours And Company | Metaphosphate glass composition |
| US6130178A (en) * | 1998-04-16 | 2000-10-10 | Corning Incorporated | Strong miserite glass-ceramics |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI477388B (en) * | 2012-07-04 | 2015-03-21 | Darfon Materials Corp | Method of fabricating casing and casing therefrom |
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| Publication number | Publication date |
|---|---|
| CN1982504A (en) | 2007-06-20 |
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