CN104862639B - The preparation technology and its penetration enhancer of a kind of high temperature resistant heat and corrosion resistant anti-scuff coating - Google Patents
The preparation technology and its penetration enhancer of a kind of high temperature resistant heat and corrosion resistant anti-scuff coating Download PDFInfo
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- CN104862639B CN104862639B CN201510284741.1A CN201510284741A CN104862639B CN 104862639 B CN104862639 B CN 104862639B CN 201510284741 A CN201510284741 A CN 201510284741A CN 104862639 B CN104862639 B CN 104862639B
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Abstract
The present invention relates to a kind of preparation technology of high temperature resistant heat and corrosion resistant anti-scuff coating and its penetration enhancer.Be characterized in, according to percentage by weight consisting of：6% 10%Cr, 4% 8%Si, 2% 6%Al, 1% 2%Y2O3, 6% 10%AlCl3, surplus is Al2O3.The beneficial effects of the invention are as follows：The present invention is prepared for Cr Al Si Y infiltration layers on TiAl alloy surface, solves the technical barrier of TiAl alloy high temperature resistant heat and corrosion resistant wear resistance difference, and process stabilizing is reliable, coating binding force is good, even tissue, densification；And have the advantages that technique be simple and convenient to operate, efficiency high, it is with low cost, be easily achieved.Adhesion is detected using methods such as file side method, scarification, rubbing manipulation and polishing processes, coating shows extraordinary adhesion with matrix, high-temperature oxidation test, frictional wear experiment and heat erosion experiment show that coating has good performance.
Description
Technical field
The present invention relates to a kind of preparation technology of high temperature resistant heat and corrosion resistant anti-scuff coating and its penetration enhancer.
Background technology
The features such as TiAl intermetallic compound has high specific strength, specific stiffness, high creep resistance, is following high-performance gas
One of contenders of turbogenerator high-temperature structural material.However, the antioxygenic property of TiAl alloy is poor, wearability
It is not enough, it is difficult to meet its requirement used at high temperature, while under the hydrochloric acid salt hot corrosion environment more than 800 DEG C, TiAl is closed
Gold causes material failure to be destroyed by corrosion quickly, it is therefore desirable in alloy surface prepares coating to improve its above-mentioned performance.
In recent years, the research for being related to TiAl alloy is concentrated mainly on using plasma spraying, chemical treatment and thermal spraying etc.
Sufacing is improved on its resistance to high temperature oxidation or friction and wear behavior, rarely has discussion to its hot corrosion resistance.Be primarily present with
Lower problem：Aoxidize, wear and tear and heat erosion destruction generation simultaneously in TiAl alloy military service operating mode, the solution of Single-issue can not be met
The harsh military service operating mode of TiAl alloy, can not also improve its service life.
The content of the invention
An object of the present invention is to provide a kind of preparation technology of high temperature resistant heat and corrosion resistant anti-scuff coating, can be notable
TiAl alloy high temperature resistant heat and corrosion resistant wear resistance is improved, results in that adhesion is good, uniform, fine and close infiltration layer, so as to carry
High TiAl alloy high temperature resistant heat and corrosion resistant wear resistance, and be simple and convenient to operate with technique, it is with low cost, be easy to real
The existing, advantage of efficiency high, suitable for producing and applying；
The second object of the present invention is to provide penetration enhancer used in a kind of above-mentioned preparation technology.
A kind of penetration enhancer, it is particular in that, according to percentage by weight consisting of：6%-10%Cr, 4%-8%Si,
2%-6%Al, 1%-2%Y2O3, 6%-10%AlCl3, surplus is Al2O3。
Wherein Cr, Si, Al, Y2O3、AlCl3And Al2O3It is powdered, and Al2O3No more than 200 mesh.
A kind of preparation technology of high temperature resistant heat and corrosion resistant anti-scuff coating, it is particular in that, comprises the following steps：
(1) alkali cleaning：TiAl alloy sample or workpiece are placed in temperature in 65~80 DEG C of alkali wash waters, to soak 10~15 points
Clock；
(2) wash：Sample or workpiece after alkali cleaning is rinsed with water, then dried up stand-by；
(3) ball milling：According to the record in claim 1, the penetration enhancer prepared is placed in into grinding in ball mill makes its final
Particle size range is 20-50 μm；
(4) dry：By the penetration enhancer drying after ball milling；
(5) embed：The penetration enhancer dried is loaded crucible, and in sample or workpiece embedment penetration enhancer, make adjacent samples or
Do not contacted between workpiece；
(6) shove charge is sealed：It is placed in after crucible is sealed in vacuum drying oven, and argon filling gas shielded；
(7) pack cementation：Vacuum drying oven is continuously heating to 1080-1100 DEG C, insulation after being warming up to 900-920 DEG C, insulation 0.5h
1.5-2.5h after cool to room temperature with the furnace；
(8) cleaning, drying：Sample after pack cementation is rinsed with water, then with alcohol washes, finally dried.
Alkali wash water uses 0.1-0.2mol/L sodium hydroxide solution in step (1).
The specific temperature that is placed in is dried for insulation 1-2h in 100-150 DEG C of baking oven in step (4).
Sealing specifically refers to be sealed with Ludox and alundum (Al2O3) in step (6), the Ludox and alundum (Al2O3)
Collocation method is specifically the Al that 1~1.2kg is added in every 1L Ludox2O3After mix.
It is specifically to be risen to 15-20 DEG C/min heating rate after 900-920 DEG C, insulation 0.5h with 15-20 in step (7)
DEG C/min heating rate rises to 1080-1100 DEG C, then be incubated after 1.5-2.5h and cool to room temperature with the furnace.
Drying is specifically to dry 3-5min at 50-100 DEG C in step (8).
The beneficial effects of the invention are as follows：The present invention is prepared for Cr-Al-Si-Y infiltration layers on TiAl alloy surface, solves
The technical barrier of TiAl alloy high temperature resistant heat and corrosion resistant wear resistance difference, process stabilizing is reliable, and coating binding force is good, tissue is equal
Even, densification；And have the advantages that technique be simple and convenient to operate, efficiency high, it is with low cost, be easily achieved.Using file side method, draw
The methods such as trace method, rubbing manipulation and polishing processes detect that coating shows extraordinary adhesion, high temperature with matrix to adhesion
Oxidation test, frictional wear experiment and heat erosion experiment show that coating has good performance.
Brief description of the drawings
Fig. 1 is the infiltration layer section microstructure figure under the conditions of embodiment 1 (insulation 1.5h)；
Fig. 2 is the infiltration layer section microstructure figure under the conditions of embodiment 2 (insulation 2h)；
Fig. 3 is the infiltration layer section microstructure figure under the conditions of embodiment 3 (insulation 2.5h)；
Fig. 4 is the layer surface macro morphology figure under the conditions of embodiment 1 (insulation 1.5h)；
Fig. 5 is the layer surface macro morphology figure under the conditions of embodiment 2 (insulation 2h)；
Fig. 6 is the layer surface macro morphology figure under the conditions of embodiment 3 (insulation 2.5h)；
Fig. 7 is the layer surface microscopic appearance figure under the conditions of embodiment 1 (insulation 1.5h)；
Fig. 8 is the layer surface microscopic appearance figure under the conditions of embodiment 2 (insulation 2h)；
Fig. 9 is the layer surface microscopic appearance figure under the conditions of embodiment 3 (insulation 2.5h)；
Figure 10 is the infiltration layer section test position schematic diagram under the conditions of embodiment 1 (insulation 1.5h)；
Figure 11 is the infiltration layer cross sectional elements distribution map of Figure 10 test positions；
Figure 12 is the infiltration layer section test position schematic diagram under the conditions of embodiment 2 (insulation 2h)；
Figure 13 is the infiltration layer cross sectional elements distribution map of Figure 12 test positions；
Figure 14 is the infiltration layer section test position schematic diagram under the conditions of embodiment 3 (insulation 2.5h)；
Figure 15 is the infiltration layer cross sectional elements distribution map of Figure 14 test positions.
Embodiment
At present, the technology of preparing of the wear-resistant Cr-Al-Si-Y infiltration layers of titanium-aluminium alloy surface refractory heat and corrosion resistant and its should
With still belonging to blank.Therefore study and realize that the technology of preparing for the Cr-Al-Si-Y infiltration layers for possessing above-mentioned performance is being navigated to titanium-aluminium alloy
The application of empty industrial circle is significant.
The technical solution adopted for the present invention to solve the technical problems comprises the following steps：
1. alkali cleaning：Sample or workpiece are placed in temperature in 65~80 DEG C of alkali wash waters, to soak 10~15 minutes；
2. wash：Sample or workpiece after alkali cleaning is rinsed using circulating water, dried up；
3. penetration enhancer is configured, the penetration enhancer prepared is placed in ball mill and grinds 4h, penetration enhancer particle is refined；
4. penetration enhancer is placed in into insulation 1h in the baking oven that temperature is 100 DEG C to be dried；
5. the penetration enhancer after drying is loaded crucible, and sample is embedded in penetration enhancer, certain distance is kept between adjacent samples；
6. the crucible equipped with sample is capped and uses Ludox and alundum (Al2O3) (collocation method：1 is added per 1L Ludox
~1.2kgAl2O3Mixing) it is placed in vacuum drying oven after sealing, and argon filling gas shielded；
7. vacuum drying oven heats up 50min to 900 DEG C, to 1080 DEG C after 900 DEG C of follow-up temperature 10min of continuing rising of insulation 0.5h,
With stove to room temperature after 1080 DEG C of insulation 1.5-2.5h；
8. the sample after pack cementation is rinsed using circulating water, then dried, terminated.
Diffusion agent formulation provided by the present invention, specifically includes herein below：
1. element is oozed：6%-10%Cr, 4%-8%Si, 2%-6%Al, 1%-2%Y2O3
2. catalyst：6%-10%AlCl3(analysis is pure)
3. filler：Al2O3(≤200 mesh)
Present approach provides a kind of preparation of high temperature resistant heat and corrosion resistant anti-scuff coating, the coating is by Cr, Al, Si, Y
Quaternary is prepared using pack cementation method, and the coating realizes the quaternary permeation in Cr, Al, Si, the Y on TiAl alloy surface, carried simultaneously
The high high temperature resistant heat and corrosion resistant wear resistance of TiAl alloy.
Embodiment 1：
1. alkali cleaning：TiAl alloy sample is placed in into temperature, and for 65 DEG C of alkali wash waters, (alkali wash water uses 0.1mol/L hydroxide
Sodium solution) in, soak 10 minutes；2. wash：Sample after alkali cleaning is rinsed using circulating water；Drying；3. penetration enhancer is prepared：According to quantity
Penetration enhancer accurately is weighed, the proportioning of penetration enhancer is by weight percentage：8%Cr powder, 6%Si powder, 4%Al powder, 8%AlCl3Powder (analysis
It is pure), 2%Y2O3Powder, remaining is aluminium oxide powder (≤200 mesh)；4. ball milling：The penetration enhancer prepared is placed in ball mill and ground
Mill, is sufficiently mixed it, and refinement penetration enhancer particle is to no more than 200 mesh；5. dry：It is 100 that penetration enhancer after ball milling is placed in into temperature
DEG C baking oven in insulation 1h dried；6. embed：The penetration enhancer dried is loaded corundum crucible, and sample is embedded to penetration enhancer
In, and make to keep certain distance (>=5cm) between adjacent samples；7. seal：The crucible that will be equipped with sample is capped and uses silicon molten
Glue and alundum (Al2O3) (collocation method：1.1kg Al is added per 1L Ludox2O3Mixing) sealing after, be placed in vacuum drying oven and fill
Argon gas is protected；8. pack cementation：Vacuum drying oven at the uniform velocity heats up 50min to 900 DEG C, continues at the uniform velocity to heat up after being incubated 0.5h at 900 DEG C
To 1080 DEG C after 10min, room temperature is cooled to the furnace after being incubated 1.5h at 1080 DEG C；9. cleaning, drying：By the sample after pack cementation
Rinsed, then with alcohol washes, then dried using circulating water, 3min is dried at specifically 100 DEG C, terminated.
Embodiment 2：
1. alkali cleaning：TiAl alloy sample of having a try is placed in temperature (alkali wash water is using 0.1-0.2mol/L's for 65 DEG C of alkali wash waters
Sodium hydroxide solution) in, soak 10 minutes；2. wash：Sample after alkali cleaning is rinsed using circulating water；Drying；3. prepare and ooze
Agent：Penetration enhancer is accurately weighed according to quantity, and the proportioning of penetration enhancer is by weight percentage：8%Cr powder, 6%Si powder, 4%Al powder, 8%AlCl3
Powder (analysis is pure), 2%Y2O3Powder, remaining is aluminium oxide powder (≤200 mesh)；4. ball milling：The penetration enhancer prepared is placed in ball milling
Ground in machine, be sufficiently mixed it, refinement penetration enhancer particle is to no more than 200 mesh；5. dry：Penetration enhancer after ball milling is placed in temperature
Dried to be incubated 1h in 100 DEG C of baking ovens；6. embed：The penetration enhancer dried is loaded corundum crucible, and sample is embedded to
In penetration enhancer, certain distance (>=5cm) is kept between adjacent samples, is 7. sealed：The crucible that will be equipped with sample is capped and uses Ludox
And be placed in after alundum (Al2O3) sealing in vacuum drying oven and argon filling gas shielded；8. pack cementation：Vacuum drying oven at the uniform velocity heats up 50min to 900
DEG C, continue after 900 DEG C of insulation 0.5h after at the uniform velocity heating 10min to 1080 DEG C, room is cooled to the furnace after being incubated 2h at 1080 DEG C
Temperature；9. cleaning, drying：Sample after pack cementation is rinsed using circulating water, then with alcohol washes, then dried, at 60 DEG C
5min is dried, is terminated.
Embodiment 3：
1. alkali cleaning：TiAl alloy sample of having a try is placed in temperature (alkali wash water is using 0.1-0.2mol/L's for 65 DEG C of alkali wash waters
Sodium hydroxide solution) in, soak 10 minutes；2. wash：Sample after alkali cleaning is rinsed using circulating water；Drying；3. prepare and ooze
Agent：Penetration enhancer is accurately weighed according to quantity, and the proportioning of penetration enhancer is by weight percentage：8%Cr powder, 6%Si powder, 4%Al powder, 8%AlCl3
Powder (analysis is pure), 2%Y2O3Powder, remaining is aluminium oxide powder (≤200 mesh)；4. ball milling：The penetration enhancer prepared is placed in ball milling
Ground in machine, be sufficiently mixed it, refinement penetration enhancer particle is to no more than 200 mesh；5. dry：Penetration enhancer after ball milling is placed in temperature
Dried to be incubated 1h in 100 DEG C of baking ovens；6. embed：The penetration enhancer dried is loaded corundum crucible, and sample is embedded to
In penetration enhancer, certain distance (>=5cm) is kept between adjacent samples, is 7. sealed：The crucible that will be equipped with sample is capped and uses Ludox
And be placed in after alundum (Al2O3) sealing in vacuum drying oven and argon filling gas shielded；8. pack cementation：Vacuum drying oven at the uniform velocity heats up 50min to 900
DEG C, continue after 900 DEG C of insulation 0.5h after at the uniform velocity heating 10min to 1080 DEG C, cooled to the furnace after being incubated 2.5h at 1080 DEG C
Room temperature；9. cleaning, drying：Sample after pack cementation is rinsed using circulating water, then with alcohol washes, then dried, 90 DEG C
Lower drying 3min, terminates.
Claims (8)
1. a kind of penetration enhancer, it is characterised in that according to percentage by weight consisting of：6%-10%Cr, 4%-8%Si, 2%-6%
Al, 1%-2%Y2O3, 6%-10%AlCl3, surplus is Al2O3。
2. a kind of penetration enhancer as claimed in claim 1, it is characterised in that：Wherein Cr, Si, Al, Y2O3、AlCl3And Al2O3It is powder
Last shape, and Al2O3No more than 200 mesh.
3. a kind of preparation technology of high temperature resistant heat and corrosion resistant anti-scuff coating, it is characterised in that comprise the following steps：
(1) alkali cleaning：TiAl alloy sample or workpiece are placed in temperature in 65~80 DEG C of alkali wash waters, to soak 10~15 minutes；
(2) wash：Sample or workpiece after alkali cleaning is rinsed with water, then dried up stand-by；
(3) ball milling：According to the record in claim 1, the penetration enhancer prepared is placed in into grinding in ball mill makes its final size
Scope is 20-50 μm；
(4) dry：By the penetration enhancer drying after ball milling；
(5) embed：The penetration enhancer dried is loaded crucible, and sample or workpiece are embedded in penetration enhancer, makes adjacent samples or workpiece
Between do not contact；
(6) shove charge is sealed：It is placed in after crucible is sealed in vacuum drying oven, and argon filling gas shielded；
(7) pack cementation：Vacuum drying oven is continuously heating to 1080-1100 DEG C after being warming up to 900-920 DEG C, insulation 0.5h, is incubated 1.5-
Cool to room temperature after 2.5h with the furnace；
(8) cleaning, drying：Sample after pack cementation is rinsed with water, then with alcohol washes, finally dried.
4. a kind of preparation technology of high temperature resistant heat and corrosion resistant anti-scuff coating as claimed in claim 3, it is characterised in that：Step
(1) alkali wash water uses 0.1-0.2mol/L sodium hydroxide solution in.
5. a kind of preparation technology of high temperature resistant heat and corrosion resistant anti-scuff coating as claimed in claim 3, it is characterised in that：Step
(4) the specific temperature that is placed in is dried for insulation 1-2h in 100-150 DEG C of baking oven in.
6. a kind of preparation technology of high temperature resistant heat and corrosion resistant anti-scuff coating as claimed in claim 3, it is characterised in that：Step
(6) sealing specifically refers to be sealed with Ludox and alundum (Al2O3) in, and the collocation method of the Ludox and alundum (Al2O3) is specific
It is the Al that 1~1.2kg is added in every 1L Ludox2O3After mix.
7. a kind of preparation technology of high temperature resistant heat and corrosion resistant anti-scuff coating as claimed in claim 3, it is characterised in that：Step
(7) it is specifically to be risen to 15-20 DEG C/min heating rate after 900-920 DEG C, insulation 0.5h with 15-20 DEG C/min heating in
Speed rises to 1080-1100 DEG C, then is incubated after 1.5-2.5h and cools to room temperature with the furnace.
8. a kind of preparation technology of high temperature resistant heat and corrosion resistant anti-scuff coating as claimed in claim 3, it is characterised in that：Step
(8) drying is specifically to dry 3-5min at 50-100 DEG C in.
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| CN105839048B (en) * | 2016-04-08 | 2018-06-19 | 北方民族大学 | A kind of high temperature alloy oxidation and corrosion protective coating and penetration enhancer |
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| CN106435460B (en) * | 2016-10-18 | 2018-10-12 | 中国矿业大学 | A kind of niobium alloy surface high-temp wear-resistant coating and preparation method thereof |
| CN106521405B (en) * | 2016-10-25 | 2018-08-24 | 北方民族大学 | A kind of penetration enhancer and its application method of the modification of nickel-base alloy surface |
| CN107164722B (en) * | 2017-06-23 | 2018-12-25 | 江苏双勤新能源科技有限公司 | A kind of alloy surface coating and preparation method thereof |
| CN109385600B (en) * | 2017-08-02 | 2023-11-03 | 深圳先进技术研究院 | Titanium-aluminum alloy piece with composite infiltration layer and preparation method thereof, and titanium-aluminum alloy piece with diamond coating and preparation method thereof |
| CN107779813B (en) * | 2017-12-23 | 2020-01-31 | 北方民族大学 | Preparation process of Cr-Al-Ce-Y thermal protection coating on surface of titanium-aluminum alloy and penetrating agent thereof |
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