CN104789964B - A kind of preparation method of high-temperature alloy surface high-temperature insulating coating - Google Patents
A kind of preparation method of high-temperature alloy surface high-temperature insulating coating Download PDFInfo
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- CN104789964B CN104789964B CN201510133719.7A CN201510133719A CN104789964B CN 104789964 B CN104789964 B CN 104789964B CN 201510133719 A CN201510133719 A CN 201510133719A CN 104789964 B CN104789964 B CN 104789964B
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Abstract
The present invention discloses a kind of preparation method of high-temperature alloy surface high-temperature insulating coating, step：1) by high temperature alloy substrate surface preparation；2) one layer of Ti metal level is deposited on high temperature alloy substrate surface；3) continue to deposit one layer of Al metal level on Ti metal levels；4) by the Al metal level complete oxidations on high temperature alloy substrate surface, until oxidized portion Ti metal levels；5) multiple sealing pores are carried out to the coating surface after oxidation from high temperature insulating material, by the holes filling in coating；6) Al is sputtered on face coat2O3, by remaining gap filling in face coat；7) high temperature alloy substrate is heat-treated, makes Al in coating2O3Crystal formation to α-Al2O3Conversion.The present invention can be firmly combined with, and preparation technology is more flexible with higher efficiency system for a kind of coating still at high temperature with preferable insulating properties.
Description
Technical field
It is more particularly to a kind of still to there is good insulation properties coating to produce at high temperature the present invention relates to technical field of surface
The preparation method of product.
Background technology
High temperature alloy, be often referred at 760 DEG C-more than 1500 DEG C and certain stress condition under long-term work high-temperature metal
Material, with excellent elevated temperature strength and good anti-oxidant, resistance to corrosion, is broadly divided into iron-based high temp by matrix element and closes
Gold, nickel base superalloy, cobalt base superalloy three major types.In the last few years, with high temperature alloy in aerospace field not
It is disconnected to expand application, especially application of the nickel base superalloy in terms of military-civil gas turbine engines hot-end component, high temperature
The process for treating surface of alloy also increasingly obtains the attention of people, including surface insulated, corrosion resistance, wearability, thermal insulation
Deng the technical requirements for being all surface treatment, and in these requirements, good insulating properties is very important performance again under high temperature
One of.
Aluminum oxide coating layer is often used as metal watch due to having the advantages that high temperature resistant, corrosion-resistant, wear-resisting, dielectric strength are high
The insulating barrier in face, among these α-Al2O3It is most stable of crystal formation under normal temperature and high temperature again.There are many methods to can be used in system at present
The standby coating, conventional aluminum oxide electric insulation coating layer processing method has chemical vapor deposition, physical vapour deposition (PVD), colloidal sol-gel
Method, thermal oxidation method, plasma spraying etc..
However, to prepare aluminum oxide coating layer sedimentation rate slow for traditional CVD method, and preferably prepare film；It is molten
Glue-gel method and the thicker aluminum oxide coating layer short time consumption of thermal oxidation method preparation are long, and efficiency is low, are not suitable for producing in enormous quantities；Deng
Although plasma spray can prepare thicker aluminum oxide coating layer with high-speed, the aluminum oxide coating layer prepared is combined with matrix
Power is poor, and rough surface, hole are more.
Shortcoming for preparing aluminum oxide coating layer in above-mentioned traditional handicraft, the present invention proposes that a kind of efficiently to prepare high temperature exhausted
The method of edge combined oxidation aluminized coating.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of preparation method of high-temperature alloy surface high-temperature insulating coating,
And the coating properties are excellent.
To achieve the above object, the present invention is realized using following technical scheme：
A kind of preparation method of high-temperature alloy surface high-temperature insulating coating, is completed according to the following steps：
1) high temperature alloy substrate surface is polished flat, and is cleaned by ultrasonic totally with acetone, alcohol, deionized water successively,
Drying；
2) using magnetron sputtering technique pass through step 1) processing high temperature alloy substrate surface deposit one layer of Ti metal level,
Resulting Ti metal layer thickness is more than 1 μm；
3) continue to deposit one layer of Al metal level on Ti metal levels, resulting Al metal layer thickness is more than 1 μm；
4) by high temperature alloy substrate surface A l metal level complete oxidations, until oxidized portion Ti metal levels；
5) multiple sealing pores are carried out to the coating surface after oxidation from high temperature insulating material, the hole in coating is filled out
Fill, improve insulating properties；
6) Al is sputtered on face coat using magnetron sputtering technique2O3, by remaining gap filling in face coat；
7) by step 6) in the high temperature alloy substrate for preparing be put into Muffle furnace, in 1200 DEG C of heat treatments, make in coating
Al2O3Crystal formation to α-Al2O3Conversion.
Preferably, the step 2 is being performed) when, Ti metal layer thickness is preferably 1~100 μm.
Preferably, the step 3 is being performed) when, Al metal layer thickness is preferably 1~100 μm.
Preferably, the step 3 is being performed) when, one layer of Al metal is deposited using magnetron sputtering or the method for hot-dip
Layer.
Preferably, the step 4 is being performed) when, it is golden to the Al on surface using differential arc oxidation or the method for anodic oxidation
Belong to layer and carry out complete oxidation.
Preferably, the step 5 is being performed) when, from SiO2Colloidal sol or Al2O3Colloidal sol is used as packing material.
High temperature alloy substrate material used is nickel-base high-temperature alloy material in the present invention, exhausted for the high temperature that carries out sealing of hole
Edge material selection Al2O3Or SiO2.The high-temperature insulating coating thickness of preparation is 2-200 μm, and coating is mainly made up of aluminum oxide,
And the crystal formation of aluminum oxide is substantially all as α-Al2O3, do not contain or only contain a small amount of γ-Al2O3, the hole in coating is main
By SiO2Colloidal sol or Al2O3Colloidal sol is filled.Especially, the high-temperature insulating coating for preparing of the present invention is a kind of composite coating, mainly by
Hole and gap in alumina layer and following titanium oxide layer composition, coating is by Al2O3Or SiO2To fill.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention efficiently can prepare a kind of high-temperature insulation combined oxidation aluminized coating, the coating and base in high-temperature alloy surface
Bottom is firmly combined with, and the thickness of coating is easily controllable, and preparation process flexibility is strong, and coating has good insulation at high temperature
Performance.
Brief description of the drawings
By reading the detailed description made with reference to the following drawings to non-limiting example, further feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is the schematic flow sheet of an embodiment of preparation method of the present invention.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that to the ordinary skill of this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
It is the schematic flow sheet of the specific embodiment of the invention such as Fig. 1.Following examples are carried out with reference to the flow.
Embodiment 1：
In the present embodiment, using the method depositing Al metal level of magnetron sputtering, high temperature is closed using the method for differential arc oxidation
The Al metal layers of gold surface are complete, from SiO2Colloidal sol is used as sealing material.
1) nickel base superalloy substrate surface is polished flat, and it is dry with acetone, alcohol, deionized water ultrasonic cleaning successively
Only, and dry；
2) Ti metal levels are sputtered on the high temperature alloy substrate surface by pretreatment using magnetron sputtering technique, it is resulting
Ti metal layer thickness is 5 μm；
3) Al metal levels are sputtered on Ti metal levels using magnetron sputtering technique, resulting Al metal layer thickness is 14 μ
m；
4) using differential arc oxidization technique by the complete differential arc oxidation of Al metal levels, until 3 μm of differential arc oxidation Ti metal levels, are obtained
Most of crystal formation is α-Al2O3Face coat；
5) SiO is selected2Colloidal sol carries out sealing pores to coating surface：Corotation applies three SiO2Sol material, it is spun every time
30min is incubated at 400 DEG C to be solidified, make SiO afterwards2SiO is only left in organic solvent volatilization in colloidal sol2, most differential arc oxidation at last
Holes filling in face coat afterwards；
6) Al is sputtered on face coat using magnetron sputtering technique2O3, sputter Al2O3Thickness be 2 μm, surface is applied
Remaining gap filling in layer；
7) the high temperature alloy substrate for preparing combined oxidation aluminized coating is put into Muffle furnace, is incubated 2h at 1200 DEG C, makes painting
Al in layer2O3Crystal formation to α-Al2O3Conversion.
Embodiment 2
In the present embodiment, step be the same as Example 1 above, the difference is that selecting Al here2O3Colloidal sol is used as sealing material.
1) nickel base superalloy substrate surface is polished flat, and it is dry with acetone, alcohol, deionized water ultrasonic cleaning successively
Only, and dry；
2) Ti metal levels are sputtered on the high temperature alloy substrate surface by pretreatment using magnetron sputtering technique, it is resulting
Ti metal layer thickness is 5 μm；
3) Al metal levels are sputtered on Ti metal levels using magnetron sputtering technique, resulting Al metal layer thickness is 14 μ
m；
4) using differential arc oxidization technique by the complete differential arc oxidation of Al metal levels, until 3 μm of differential arc oxidation Ti metal levels, are obtained
Most of crystal formation is α-Al2O3Face coat；
5) Al is selected2O3Colloidal sol carries out sealing pores to coating surface：Here nano alumina sol is selected, using spin coating
Mode carry out sealing of hole, corotation is applied three times, it is spun every time after be incubated 30min at 500 DEG C and solidified, make in alumina sol
Organic solvent volatilizees, and brushes and finally is disposably sintered at 1000 DEG C after finishing for three times, most surface painting after differential arc oxidation at last
Holes filling in layer；
6) Al is sputtered on face coat using magnetron sputtering technique2O3, sputter Al2O3Thickness be 1 μm, surface is applied
Remaining gap filling in layer；
7) the high temperature alloy substrate for preparing combined oxidation aluminized coating is put into Muffle furnace, is incubated 2h at 1200 DEG C, makes painting
Al in layer2O3Crystal formation to α-Al2O3Conversion.
Embodiment 3
In the present embodiment, using the method depositing Al metal level of hot-dip, using the method for anodic oxidation by high temperature alloy
The Al metal layers on surface are complete, from SiO2Colloidal sol is used as sealing material.
1) nickel base superalloy substrate surface is polished flat, and it is dry with acetone, alcohol, deionized water ultrasonic cleaning successively
Only, and dry；
2) Ti metal levels are sputtered on the high temperature alloy substrate surface by pretreatment using magnetron sputtering technique, it is resulting
Ti metal layer thickness is 5 μm；
3) one layer of Al metal level is deposited on Ti metal levels using the method for hot-dip, resulting Al metal layer thickness is
20μm；
4) using anodizing technology by the complete anodic oxidation of Al metal levels, until 2 μm of anodic oxidation Ti metal levels；
5) SiO is selected2Colloidal sol carries out sealing pores to coating surface：Corotation applies three SiO2Sol material, it is spun every time
30min is incubated at 400 DEG C to be solidified, make SiO afterwards2SiO is only left in organic solvent volatilization in colloidal sol2, most anodic oxidation at last
Holes filling in face coat afterwards；
6) Al is sputtered on face coat using magnetron sputtering technique2O3, sputter Al2O3Thickness be 2 μm, surface is applied
Remaining gap filling in layer；
7) the high temperature alloy substrate for preparing combined oxidation aluminized coating is put into Muffle furnace, is incubated 2h at 1100 DEG C, makes painting
Al in layer2O3Crystal formation to α-Al2O3Conversion.
By the specific descriptions of above example, the purpose of the present invention, technical scheme and implementation result are further illustrated.
It is to be appreciated that the present invention is not limited to the above specific embodiments, those skilled in the art can be in claim
In the range of make various deformations or amendments, this have no effect on the present invention substantive content.
Claims (8)
1. a kind of preparation method of high-temperature alloy surface high-temperature insulating coating, it is characterised in that the described method comprises the following steps：
1) high temperature alloy substrate surface is polished flat, and is cleaned by ultrasonic clean, drying with acetone, alcohol, deionized water successively；
2) using magnetron sputtering technique pass through step 1) processing high temperature alloy substrate surface deposit one layer of Ti metal level, gained
The Ti metal layer thickness arrived is more than 1 μm；
3) continue to deposit one layer of Al metal level on Ti metal levels, resulting Al metal layer thickness is more than 1 μm；
4) by high temperature alloy substrate surface A l metal level complete oxidations, until oxidized portion Ti metal levels；
5) multiple sealing pores are carried out to the coating surface after oxidation from high temperature insulating material, by the holes filling in coating,
Improve insulating properties；
6) using magnetron sputtering technique through step 5) processing after face coat on sputter Al2O3, will be remaining in face coat
Gap filling；
7) by step 6) in the high temperature alloy substrate for preparing be put into Muffle furnace, in 800~1200 DEG C of heat treatments, make face coat
Middle Al2O3Crystal formation to α-Al2O3Conversion.
2. according to the method described in claim 1, it is characterised in that performing the step 3) when, using magnetron sputtering or
The method of hot-dip deposits one layer of Al metal level.
3. method according to claim 1 or 2, it is characterised in that performing the step 2) when, Ti metal layer thickness is
1~100 μm.
4. according to the method described in claim 1, it is characterised in that performing the step 4) when, using differential arc oxidation or
The method of anodic oxidation carries out complete oxidation to the Al metal levels on surface.
5. the method according to claim 1 or 4, it is characterised in that performing the step 3) when, Al metal layer thickness is
1~100 μm.
6. when according to the method described in claim 1, it is characterised in that performing the step 5), from SiO2Colloidal sol or
Al2O3Colloidal sol is used as packing material.
7. according to the method described in claim 1, it is characterised in that the high-temperature alloy surface high-temperature insulating coating is by aluminum oxide
Layer and following titanium oxide layer are constituted, and the hole and gap in coating are by Al2O3Or SiO2To fill.
8. the method according to claim 1 or 7, it is characterised in that the thickness of the high-temperature alloy surface high-temperature insulating coating
Spend for 2~200 μm.
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| CN110129851B (en) * | 2018-02-05 | 2020-11-03 | 美的集团股份有限公司 | Thermocouple, preparation method thereof and electric appliance |
| CN114717626B (en) * | 2022-05-10 | 2024-02-13 | 上海交通大学 | Method for prolonging service life of high-temperature alloy through prefabricated oxide film |
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