CN101935166A - Method for preparing high-temperature oxidization resistant glass ceramic coating - Google Patents
Method for preparing high-temperature oxidization resistant glass ceramic coating Download PDFInfo
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- CN101935166A CN101935166A CN 201010263966 CN201010263966A CN101935166A CN 101935166 A CN101935166 A CN 101935166A CN 201010263966 CN201010263966 CN 201010263966 CN 201010263966 A CN201010263966 A CN 201010263966A CN 101935166 A CN101935166 A CN 101935166A
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- ceramic coating
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- resistant glass
- titanium alloy
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Abstract
The invention relates to a method for preparing a high-temperature oxidization resistant glass ceramic coating, which comprises the following steps of: firstly, after drying glass, carrying out dry ball milling to obtain glass powder; adding the glass powder into a solvent to prepare slurry by full stirring; pretreating the surface of an industrial pure titanium or titanium alloy sample; then coating the slurry on the surface of the pretreated sample; and after drying the sampled coated with the slurry, sintering to obtain the high-temperature oxidization resistant glass ceramic coating on the surface of the sample. according to the glass ceramic coating formed on the surfaces of industrial pure titanium and titanium alloy, the oxygen content of the surface of the titanium alloy is effectively reduced, the titanium alloy can be prevented from being oxidized to form a porous TiO2 film, oxygen is avoided being permeated into a matrix and the high-temperature oxidization resistant capability of the industrial pure titanium or the titanium alloy is greatly improved, serious interdiffusion between the coating and a substrate is avoided because of high compatibility between the coating and the substrate, thereby good protecting effect on the industrial pure titanium and the titanium alloy is obtained.
Description
Technical field
The invention belongs to the high-temperature oxidation resistant coating technical field, particularly a kind of preparation method of high-temperature oxidation resistant glass ceramic coating.
Background technology
Pure titanium has corrosive abilities such as good salt tolerant, seawater and nitric acid, has higher specific tenacity and less mass density simultaneously.The intensity of high purity titanium is not high, but after the alloying, its intensity can be suitable with high-strength steel, also has simultaneously certain middle high-temperature oxidation resistance, because industrially pure titanium and titanium alloy have outstanding characteristics such as light specific gravity, specific tenacity height, strong, the middle temperature antioxidant property of resistance to corrosion be stable, therefore are widely used in aerospace and chemical field.But, the crisp principal element that influences its thermostability that becomes of the oxidation of titanium alloy and oxygen at high temperature, the titanium alloy oxidation forms porous TiO on the one hand
2Film, protective value is poor; Oxygen is penetrated in the matrix and with titanium formation sosoloid alloy plasticity is obviously descended on the other hand.
Glass coating and glass ceramic coating have thermostability that good stopping property becomes reconciled, good unreactiveness, high-temperature stability and superior mechanical property are arranged is industrially pure titanium and the effective coated material of other titanium alloy high-temperature oxidation protections.But at high temperature the viscosity of glass coating is flowing in coating and forms crackle and cavity, thereby loses the protection to matrix.And glass ceramic coating has the inherent high-temperature viscosity can avoid forming crackle and cavity by the existence and the uniform distribution of crystalline phase.Be easy to obtain the thermal expansivity close by the composition of adjusting the glass-ceramic coating in addition, so just minimizing breaking and produce the chance of defective at the thermal cycling floating coat with matrix.
Summary of the invention
The technical problem to be solved in the present invention is: at the shortcoming and the deficiency of prior art existence, provide that a kind of preparation method is simple, preparation cost is low, and be suitable for the preparation method of the high-temperature oxidation resistant glass ceramic coating of suitability for industrialized production, prepared glass ceramic coating has improved industrially pure titanium or Titanium Alloys at High Temperature resistance of oxidation.
At above-mentioned technical problem, the present invention proposes following technical scheme.
A kind of preparation method of high-temperature oxidation resistant glass ceramic coating comprises the steps:
(1) take by weighing raw material and mix compound, described compound is by the SiO of 30-40%
2, the K of 5-15%
2O, the B of 10-20%
2O
3, the TiO of 5-20%
2, the Al of 15-20%
2O
3, the MgO of 10-20% and the CoO of 1-6% form;
(2) compound is melted in the electric furnace of Si-Mo rod, the compound after the fusing is made frit through shrend, and frit oven dry back is also crossed 200-300 purpose sieve with dry ball milling and obtained glass powder, glass powder is added in the solvent make slurry through fully stirring;
(3) pre-treatment is carried out on the surface of industrially pure titanium or titanium alloy sample, then slurry is coated in pretreated specimen surface, to be coated with the sample of slurry in 80-100 ℃ of insulation 10-20 minute, the stove that after the insulation sample is placed argon gas atmosphere promptly made the high-temperature oxidation resistant glass ceramic coating at specimen surface in 1000-1250 ℃ of sintering 5-30 minute.
Described solvent is meant the mixture of dehydrated alcohol or dehydrated alcohol and polyvinyl alcohol.
Described pre-treatment is meant hot degreasing and sandblasting.
Described slurry applies pickling process or the cold spraying method of adopting.
Beneficial effect of the present invention is embodied in: the preparation method of glass ceramic coating of the present invention, technology is simple, and is with low cost.At the glass ceramic coating of industrially pure titanium and titanium alloy surface formation, reduced the oxygen level of titanium alloy surface effectively, can stop the titanium alloy oxidation to form porous TiO
2Film; can stop oxygen to be penetrated in the matrix again; industrially pure titanium or Titanium Alloys at High Temperature resistance of oxidation have not only been improved greatly; and consistency is good between coating and the base material; also avoided mutual diffusion serious between coating and the base material, thereby industrially pure titanium and titanium alloy have been played good protective action.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1: at first, press massfraction with 35% SiO
2, 5% K
2O, 10% B
2O
3, 15% TiO
2, 17% Al
2O
3, 15% MgO and 3% CoO mix compound; Secondly, compound is melted in the electric furnace of Si-Mo rod, compound after the fusing is made frit through shrend, 200-300 purpose sieve is also crossed with dry ball milling in frit oven dry back obtain glass powder, glass powder is added in the dehydrated alcohol make slurry through fully stirring; At last, surface to industrially pure titanium or titanium alloy sample refers to hot degreasing and sandblasting, adopt pickling process that slurry is coated in pretreated specimen surface then, to be coated with the sample of slurry in 80 ℃ of insulations 20 minutes, after the insulation sample placed the argon gas atmosphere stove in 1150 ℃ of sintering 15 minutes, promptly make the high-temperature oxidation resistant glass ceramic coating at specimen surface.Coat-thickness is about 100 μ m.The industrially pure titanium that applies behind the glass ceramic coating shows good resistance of oxidation at 800 ℃, and oxidation do not see the glass ceramic coating cracking in 150 hours and peel off, and the industrially pure titanium that does not apply glass ceramic coating promptly saw 800 ℃ of oxidations that oxide skin peeled off in 15 hours.Apply behind the glass ceramic coating industrially pure titanium 1000 ℃ of performances certain resistance of oxidation, oxidation is disbonding after 30 hours, and the industrially pure titanium that does not apply glass ceramic coating promptly saw 1000 ℃ of oxidations that oxide skin peeled off in 5 hours.
Embodiment 2: at first, press massfraction with 35% SiO
2, 10% K
2O, 15% B
2O
3, 5% TiO
2, 15% Al
2O
3, 15% MgO and 5% CoO mix compound; Secondly, compound is melted in the electric furnace of Si-Mo rod, compound after the fusing is made frit through shrend, frit oven dry back with dry ball milling and cross 200-300 purpose sieve and obtain glass powder, is added dehydrated alcohol and polyvinyl alcohol to make slurry through abundant stirring in the mixture of arbitrary proportion with glass powder; At last, surface to industrially pure titanium or titanium alloy sample refers to hot degreasing and sandblasting, adopt the cold spraying method that slurry is coated in pretreated specimen surface then, to be coated with the sample of slurry in 100 ℃ of insulations 10 minutes, after the insulation sample placed the argon gas atmosphere stove in 1050 ℃ of sintering 10 minutes, promptly make the high-temperature oxidation resistant glass ceramic coating at specimen surface.Coat-thickness is about 80 μ m.Apply the Ti-38Al-14TiO of glass ceramic coating
2Alloy shows good resistance of oxidation at 800 ℃, and oxidation do not see glass ceramic coating cracking in 100 hours and peel off, and does not apply the Ti-38Al-14TiO of glass ceramic coating
2Promptly saw 800 ℃ of oxidations that oxide skin peeled off in 15 hours.Apply the Ti-38Al-14TiO of glass ceramic coating
2Alloy shows at 1000 ℃-resistance of oxidation of Ding, and oxidation is disbonding after 40 hours, and does not apply the Ti-38Al-14TiO of glass ceramic coating
2Promptly saw 1000 ℃ of oxidations that oxide skin peeled off in 15 hours.
Embodiment 3: at first, press massfraction with 30% SiO
2, 5% K
2O, 20% B
2O
3, 10% TiO
2, 15% Al
2O
3, 15% MgO and 5% CoO mix compound; Secondly, compound is melted in the electric furnace of Si-Mo rod, compound after the fusing is made frit through shrend, 200-300 purpose sieve is also crossed with dry ball milling in frit oven dry back obtain glass powder, glass powder is added in the dehydrated alcohol make slurry through fully stirring; At last, surface to industrially pure titanium or titanium alloy sample refers to hot degreasing and sandblasting, adopt pickling process that slurry is coated in pretreated specimen surface then, to be coated with the sample of slurry in 100 ℃ of insulations 20 minutes, after the insulation sample placed the argon gas atmosphere stove in 1150 ℃ of sintering, 20 minutes, promptly make the high-temperature oxidation resistant glass ceramic coating at specimen surface.Coat-thickness is about 100 μ m.Apply the Ti-35Al-16TiO of glass ceramic coating
2-9Nb
2O
5Show good resistance of oxidation at 800 ℃, oxidation do not see glass ceramic coating cracking in 150 hours and peels off, and do not apply the Ti-35Al-16TiO of glass ceramic coating
2-9Nb
2O
5Promptly saw 800 ℃ of oxidations that oxide skin peeled off in 20 hours.Apply the Ti-35Al-16TiO of glass ceramic coating
2-9Nb
2O
5Show certain resistance of oxidation at 1000 ℃, oxidation sees glass ceramic coating cracking and peels off after 35 hours, and do not apply the Ti-35Al-16TiO of glass ceramic coating
2-9Nb
2O
5Promptly saw 1000 ℃ of oxidations that oxide skin peeled off in 10 hours
Embodiment 4: at first, press massfraction with 35% SiO
2, 15% K
2O, 15% B
2O
3, 7% TiO
2, 15% Al
2O
3, 10% MgO and 3% CoO mix compound; Secondly, compound is melted in the electric furnace of Si-Mo rod, compound after the fusing is made frit through shrend, frit oven dry back with dry ball milling and cross 200-300 purpose sieve and obtain glass powder, is added dehydrated alcohol and polyvinyl alcohol to make slurry through abundant stirring in the mixture of arbitrary proportion with glass powder; At last, surface to industrially pure titanium or titanium alloy sample refers to hot degreasing and sandblasting, adopt the cold spraying method that slurry is coated in pretreated specimen surface then, to be coated with the sample of slurry in 100 ℃ of insulations 20 minutes, after the insulation sample placed the argon gas atmosphere stove in 1150 ℃ of sintering 20 minutes, promptly make the high-temperature oxidation resistant glass ceramic coating at specimen surface.Coat-thickness is about 100 μ m.Apply the Ti-36Al-16TiO behind the glass ceramic coating
2-6Nb
2O
5Show good resistance of oxidation at 800 ℃, oxidation do not see glass ceramic coating cracking in 180 hours and peels off, and do not apply the Ti-36Al-16TiO of glass ceramic coating
2-6Nb
2O
5Promptly saw 800 ℃ of oxidations that oxide skin peeled off in 25 hours.Apply the Ti-36Al-16TiO behind the glass ceramic coating
2-6Nb
2O
5Show certain resistance of oxidation at 1000 ℃, oxidation just sees glass ceramic coating cracking and peels off after 40 hours, and do not apply the Ti-36Al-16TiO of glass ceramic coating
2-6Nb
2O
5Promptly saw 1000 ℃ of oxidations that oxide skin peeled off in 15 hours.
Embodiment 5: at first, press massfraction with 40% SiO
2, 5% K
2O, 12% B
2O
3, 15% TiO
2, 15% Al
2O
3, 12% MgO and 1% CoO mix compound; Secondly, compound is melted in the electric furnace of Si-Mo rod, compound after the fusing is made frit through shrend, 200-300 purpose sieve is also crossed with dry ball milling in frit oven dry back obtain glass powder, glass powder is added in the dehydrated alcohol make slurry through fully stirring; At last, surface to industrially pure titanium or titanium alloy sample refers to hot degreasing and sandblasting, adopt the cold spraying method that slurry is coated in pretreated specimen surface then, to be coated with the sample of slurry in 85 ℃ of insulations 18 minutes, after the insulation sample placed the argon gas atmosphere stove in 1000 ℃ of sintering 30 minutes, promptly make the high-temperature oxidation resistant glass ceramic coating at specimen surface.
Embodiment 6: at first, press massfraction with 32% SiO
2, 6% K
2O, 10% B
2O
3, 20% TiO
2, 15% Al
2O
3, 11% MgO and 6% CoO mix compound; Secondly, compound is melted in the electric furnace of Si-Mo rod, compound after the fusing is made frit through shrend, 200-300 purpose sieve is also crossed with dry ball milling in frit oven dry back obtain glass powder, glass powder is added in the dehydrated alcohol make slurry through fully stirring; At last, surface to industrially pure titanium or titanium alloy sample refers to hot degreasing and sandblasting, adopt pickling process that slurry is coated in pretreated specimen surface then, to be coated with the sample of slurry in 90 ℃ of insulations 15 minutes, after the insulation sample placed the argon gas atmosphere stove in 1250 ℃ of sintering 5 minutes, promptly make the high-temperature oxidation resistant glass ceramic coating at specimen surface.
Embodiment 7: at first, press massfraction with 30% SiO
2, 5% K
2O, 13% B
2O
3, 10% TiO
2, 20% Al
2O
3, 20% MgO and 2% CoO mix compound; Secondly, compound is melted in the electric furnace of Si-Mo rod, compound after the fusing is made frit through shrend, 200-300 purpose sieve is also crossed with dry ball milling in frit oven dry back obtain glass powder, glass powder is added in the dehydrated alcohol make slurry through fully stirring; At last, surface to industrially pure titanium or titanium alloy sample refers to hot degreasing and sandblasting, adopt the cold spraying method that slurry is coated in pretreated specimen surface then, to be coated with the sample of slurry in 95 ℃ of insulations 12 minutes, after the insulation sample placed the argon gas atmosphere stove in 1100 ℃ of sintering 20 minutes, promptly make the high-temperature oxidation resistant glass ceramic coating at specimen surface.
Claims (4)
1. the preparation method of a high-temperature oxidation resistant glass ceramic coating is characterized in that comprising the steps:
1) at first, presses the SiO of massfraction with 30-40%
2, the K of 5-15%
2O, the B of 10-20%
2O
3, the TiO of 5-20%
2, the A1 of 15-20%
2O
3, the MgO of 10-20% and the CoO of 1-6% mix compound;
2) secondly, compound is melted in the electric furnace of Si-Mo rod, the compound after the fusing is made frit through shrend, 200-300 purpose sieve is also crossed with dry ball milling in frit oven dry back obtain glass powder, glass powder is added in the solvent make slurry through fully stirring;
3) last, pre-treatment is carried out on surface to industrially pure titanium or titanium alloy sample, then slurry is coated in pretreated specimen surface, to be coated with the sample of slurry in 80-100 ℃ of insulation 10-20 minute, place the argon gas atmosphere stove in 1000-1250 ℃ of sintering 5-30 minute on sample after the insulation, promptly make the high-temperature oxidation resistant glass ceramic coating at specimen surface.
2. according to the preparation method of the described a kind of high-temperature oxidation resistant glass ceramic coating of claim 1, it is characterized in that: described solvent is dehydrated alcohol or dehydrated alcohol and the polyvinyl alcohol mixture with arbitrary proportion.
3. according to the preparation method of the described a kind of high-temperature oxidation resistant glass ceramic coating of claim 1, it is characterized in that: described pre-treatment is meant hot degreasing and sandblasting.
4. according to the preparation method of the described a kind of high-temperature oxidation resistant glass ceramic coating of claim 1, it is characterized in that: described slurry applies pickling process or the cold spraying method of adopting.
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|---|---|---|---|
| CN 201010263966 CN101935166A (en) | 2010-08-26 | 2010-08-26 | Method for preparing high-temperature oxidization resistant glass ceramic coating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010263966 CN101935166A (en) | 2010-08-26 | 2010-08-26 | Method for preparing high-temperature oxidization resistant glass ceramic coating |
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| Publication Number | Publication Date |
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Family
ID=43388771
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| CN102260086A (en) * | 2011-05-19 | 2011-11-30 | 武汉长利玻璃有限责任公司 | Ceramic coating capable of resisting high-temperature corrosion for protecting hanging part in tin bath of float glass and preparation method thereof |
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-
2010
- 2010-08-26 CN CN 201010263966 patent/CN101935166A/en active Pending
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Application publication date: 20110105 |