CN104862639A - Preparation method of high-temperature-resistant, heat-corrosion-resistant and abrasion-resistant coating and penetrating agent - Google Patents

Preparation method of high-temperature-resistant, heat-corrosion-resistant and abrasion-resistant coating and penetrating agent Download PDF

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CN104862639A
CN104862639A CN201510284741.1A CN201510284741A CN104862639A CN 104862639 A CN104862639 A CN 104862639A CN 201510284741 A CN201510284741 A CN 201510284741A CN 104862639 A CN104862639 A CN 104862639A
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resistant
penetration enhancer
coating
temperature
heat
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CN104862639B (en
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李涌泉
耿桂宏
孙玉芳
蒋亮
陈炜晔
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North Minzu University
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North Minzu University
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Abstract

The invention relates to a preparation method of a high-temperature-resistant, heat-corrosion-resistant and abrasion-resistant coating and a penetrating agent. The penetrating agent is characterized by comprising the following components in percentage by weight: 6-10 percent of Cr, 4-8 percent of Si, 2-6 percent of Al, 1-2 percent of Y2O3, 6-10 percent of AlCl3 and the balance of Al2O3. The preparation method of the high-temperature-resistant, heat-corrosion-resistant and abrasion-resistant coating and the penetrating agent have the benefits that a Cr-Al-Si-Y penetrating layer is prepared on the surface of a TiAl alloy, the technical problem of poor in high-temperature resistance, heat corrosion resistance and abrasion resistance of the TiAl alloy is solved, the process is stable and reliable, the coating binding force is good, and tissues are uniform and compact; moreover, the penetrating agent has the advantages of being simple in process, convenient in operation, high in efficiency, low in cost, easy in implementation and the like. The binding force is detected by adopting an edge filing method, a scratching method, a friction method and a polishing method, the binding force between a coating layer and a matrix is good, and a high-temperature oxidation test, a frictional wear test and a heat corrosion test show that the coating has excellent performance.

Description

A kind of preparation technology of high temperature resistant heat and corrosion resistant anti-scuff coating and penetration enhancer thereof
Technical field
The present invention relates to a kind of preparation technology and penetration enhancer thereof of high temperature resistant heat and corrosion resistant anti-scuff coating.
Background technology
TiAl intermetallic compound has the features such as high specific strength, specific rigidity, high creep resistance, is one of contenders of following high-performance gas turbine engine high-temperature structural material.But, the antioxidant property of TiAl alloy is poor, wear resistance is not enough, be difficult to meet its requirement at high temperature used, simultaneously under the hydrochloride thermal etching environment more than 800 DEG C, TiAl alloy is very fast causes material failure to be destroyed by corrosion, therefore needs to prepare coating to improve its above-mentioned performance at alloy surface.
In recent years, the research relating to TiAl alloy mainly concentrates on sufacings such as adopting plasma spraying, chemical treatment and thermospray and improves on its resistance to high temperature oxidation or friction and wear behavior, rarely has discussion to its hot corrosion resistance.Mainly there is following problem: oxidation in TiAl alloy military service operating mode, wearing and tearing and thermal etching destroy and occur simultaneously, and the solution of Single-issue cannot meet the military service operating mode of TiAl alloy harshness, also cannot improve its service life.
Summary 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, the high temperature resistant heat and corrosion resistant wear resistance of TiAl alloy can be significantly improved, bonding force can be obtained good, evenly, fine and close infiltration layer, thus improve the high temperature resistant heat and corrosion resistant wear resistance of TiAl alloy, and have technique simple, easy to operate, with low cost, be easy to realize, advantage that efficiency is high, be suitable for producing and application;
Two of object of the present invention is to provide penetration enhancer used in a kind of above-mentioned preparation technology.
A kind of penetration enhancer, its special feature is, according to weight percent, it consists of: 6%-10%Cr, 4%-8%Si, 2%-6%Al, 1%-2%Y 2o 3, 6%-10%AlCl 3, surplus is Al 2o 3.
Wherein Cr, Si, Al, Y 2o 3, AlCl 3and Al 2o 3be Powdered, and Al 2o 3be no more than 200 orders.
A preparation technology for high temperature resistant heat and corrosion resistant anti-scuff coating, its special feature is, comprises the steps:
(1) alkali cleaning: TiAl alloy sample or workpiece being placed in temperature is 65 ~ 80 DEG C of alkaline washs, soaks 10 ~ 15 minutes;
(2) wash: the sample after alkali cleaning or workpiece use water are rinsed, then dries up stand-by;
(3) ball milling: according to the record in claim 1, is placed in grinding in ball grinder and makes its final size scope be 20-50 μm by the penetration enhancer prepared;
(4) dry: the penetration enhancer after ball milling is dried;
(5) embed: the penetration enhancer of drying is loaded crucible, and sample or workpiece are imbedded in penetration enhancer, make not contact between adjacent samples or workpiece;
(6) shove charge is sealed: sealed by crucible and be placed in vacuum oven, and applying argon gas protection;
(7) pack cementation: vacuum oven is warming up to 900-920 DEG C, insulation 0.5h follow-up continuing is warming up to 1080-1100 DEG C, cools to room temperature with the furnace after insulation 1.5-2.5h;
(8) cleaning, drying: the sample use water after pack cementation is rinsed, then uses alcohol washes, finally dry.
In step (1), alkaline wash adopts the sodium hydroxide solution of 0.1-0.2mol/L.
Specifically being placed in temperature in step (4) is that the baking oven of 100-150 DEG C is incubated 1-2h and dries.
In step (6), sealing specifically refers to that the collocation method of this silicon sol and aluminium sesquioxide specifically adds the Al of 1 ~ 1.2kg at every 1L silicon sol with silicon sol and aluminium sesquioxide sealing 2o 3rear mixing.
Step specifically rises to 900-920 DEG C with the temperature rise rate of 15-20 DEG C/min in (7), rises to 1080-1100 DEG C, then cool to room temperature with the furnace after being incubated 1.5-2.5h after insulation 0.5h with the temperature rise rate of 15-20 DEG C/min.
Dry in step (8) and specifically at 50-100 DEG C, dry 3-5min.
The invention has the beneficial effects as follows: the present invention has prepared Cr-Al-Si-Y infiltration layer on TiAl alloy surface, solve the technical barrier of TiAl alloy high temperature resistant heat and corrosion resistant wear resistance difference, process stabilizing is reliable, coating binding force is good, homogeneous microstructure, densification; And have that technique is simple, easy to operate, efficiency is high, with low cost, be easy to the advantages such as realization.Adopt the methods such as file limit method, scratch method, rubbing manipulation and polishing processes to detect bonding force, coating and matrix show extraordinary bonding force, and high-temperature oxidation test, frictional wear experiment and thermal etching experiment show that coating has good performance.
Accompanying drawing explanation
Fig. 1 is the infiltration layer cross section microstructure figure under embodiment 1 (insulation 1.5h) condition;
Fig. 2 is the infiltration layer cross section microstructure figure under embodiment 2 (insulation 2h) condition;
Fig. 3 is the infiltration layer cross section microstructure figure under embodiment 3 (insulation 2.5h) condition;
Fig. 4 is the layer surface macro morphology figure under embodiment 1 (insulation 1.5h) condition;
Fig. 5 is the layer surface macro morphology figure under embodiment 2 (insulation 2h) condition;
Fig. 6 is the layer surface macro morphology figure under embodiment 3 (insulation 2.5h) condition;
Fig. 7 is the layer surface microscopic appearance figure under embodiment 1 (insulation 1.5h) condition;
Fig. 8 is the layer surface microscopic appearance figure under embodiment 2 (insulation 2h) condition;
Fig. 9 is the layer surface microscopic appearance figure under embodiment 3 (insulation 2.5h) condition;
Figure 10 is that position view is detected in the infiltration layer cross section under embodiment 1 (insulation 1.5h) condition;
Figure 11 is the infiltration layer cross sectional elements distribution plan that Figure 10 detects position;
Figure 12 is that position view is detected in the infiltration layer cross section under embodiment 2 (insulation 2h) condition;
Figure 13 is the infiltration layer cross sectional elements distribution plan that Figure 12 detects position;
Figure 14 is that position view is detected in the infiltration layer cross section under embodiment 3 (insulation 2.5h) condition;
Figure 15 is the infiltration layer cross sectional elements distribution plan that Figure 14 detects position.
Embodiment
At present, the technology of preparing of the wear-resistant Cr-Al-Si-Y infiltration layer of titanium aluminum alloy surface refractory heat and corrosion resistant and application thereof still belong to blank.The technology of preparing of the Cr-Al-Si-Y infiltration layer therefore studied and realize possessing above-mentioned performance is significant in the application of aviation industry to titanium aluminum alloy.
The technical solution adopted for the present invention to solve the technical problems comprises the following steps:
1. alkali cleaning: sample or workpiece being placed in temperature is 65 ~ 80 DEG C of alkaline washs, soaks 10 ~ 15 minutes;
2. wash: use flowing water to rinse on the sample after alkali cleaning or workpiece, dry up;
3. configure penetration enhancer, the penetration enhancer prepared is placed in grinding in ball grinder 4h, refinement penetration enhancer particle;
4. penetration enhancer being placed in temperature is that the baking oven of 100 DEG C is incubated 1h and dries;
5. the penetration enhancer after oven dry is loaded crucible, and sample is imbedded in penetration enhancer, between adjacent samples, keep certain distance;
6. the crucible that sample is housed added a cover and use silicon sol and aluminium sesquioxide (collocation method: every 1L silicon sol adds 1 ~ 1.2kgAl 2o 3mixing) sealing is placed in vacuum oven, and applying argon gas protection;
7. vacuum oven intensification 50min to 900 DEG C, to 1080 DEG C after 900 DEG C of insulation 0.5h follow-up temperature 10min of continuing rising, after 1080 DEG C of insulation 1.5-2.5h with stove to room temperature;
8. use flowing water to rinse on the sample after pack cementation, then dry, terminate.
Diffusion agent formulation provided by the present invention, specifically comprises following content:
1. element is oozed: 6%-10%Cr, 4%-8%Si, 2%-6%Al, 1%-2%Y 2o 3
2. catalyzer: 6%-10%AlCl 3(analytical pure)
3. weighting material: Al 2o 3(≤200 order)
Present approach provides a kind of preparation of high temperature resistant heat and corrosion resistant anti-scuff coating, this coating adopts pack cementation legal system standby by Cr, Al, Si, Y quaternary, this coating achieves oozes altogether in the quaternary of Cr, Al, Si, the Y on TiAl alloy surface, improves the high temperature resistant heat and corrosion resistant wear resistance of TiAl alloy simultaneously.
Embodiment 1:
1. alkali cleaning: TiAl alloy sample being placed in temperature is 65 DEG C of alkaline washs (alkaline wash adopts the sodium hydroxide solution of 0.1mol/L), soaks 10 minutes; 2. wash: use flowing water to rinse on the sample after alkali cleaning; Dry up; 3. prepare penetration enhancer: accurately take penetration enhancer according to quantity, the proportioning of penetration enhancer is by weight percentage: 8%Cr powder, 6%Si powder, 4%Al powder, 8%AlCl 3powder (analytical pure), 2%Y 2o 3powder, all the other are aluminium oxide powder (≤200 order); 4. ball milling: the penetration enhancer prepared is placed in grinding in ball grinder, makes it fully mix, and refinement penetration enhancer particle is to being no more than 200 orders; 5. dry: the penetration enhancer after ball milling being placed in temperature is that the baking oven of 100 DEG C is incubated 1h and dries; 6. embed: the penetration enhancer of drying is loaded corundum crucible, and sample is imbedded in penetration enhancer, and make between adjacent samples, to keep certain distance (>=5cm); 7. seal: the crucible that sample is housed is added a cover and uses silicon sol and aluminium sesquioxide (collocation method: every 1L silicon sol adds the Al of 1.1kg 2o 3mixing) sealing after, be placed in vacuum oven and applying argon gas protection; 8. pack cementation: vacuum oven is intensification 50min to 900 DEG C at the uniform velocity, to 1080 DEG C after the 10min that continues at the uniform velocity to heat up, cools to room temperature with the furnace after 900 DEG C of insulation 0.5h after 1080 DEG C of insulation 1.5h; 9. cleaning, drying: use flowing water to rinse on the sample after pack cementation, then use alcohol washes, then dry, specifically dry 3min at 100 DEG C, terminate.
Embodiment 2:
1. alkali cleaning: it is 65 DEG C of alkaline washs (alkaline wash adopts the sodium hydroxide solution of 0.1-0.2mol/L) that sample of TiAl alloy being had a try is placed in temperature, soaks 10 minutes; 2. wash: use flowing water to rinse on the sample after alkali cleaning; Dry up; 3. prepare penetration enhancer: accurately take penetration enhancer according to quantity, the proportioning of penetration enhancer is by weight percentage: 8%Cr powder, 6%Si powder, 4%Al powder, 8%AlCl 3powder (analytical pure), 2%Y 2o 3powder, all the other are aluminium oxide powder (≤200 order); 4. ball milling: the penetration enhancer prepared is placed in grinding in ball grinder, makes it fully mix, and refinement penetration enhancer particle is to being no more than 200 orders; 5. dry: the penetration enhancer after ball milling being placed in temperature is that the baking oven of 100 DEG C is incubated 1h and dries; 6. embed: the penetration enhancer of drying is loaded corundum crucible, and sample is imbedded in penetration enhancer, keep certain distance (>=5cm) between adjacent samples, 7. seal: the crucible that sample is housed is added a cover and uses silicon sol and aluminium sesquioxide sealing to be placed on also applying argon gas protection in vacuum oven; 8. pack cementation: vacuum oven is intensification 50min to 900 DEG C at the uniform velocity, to 1080 DEG C after the 10min that continues at the uniform velocity to heat up, cools to room temperature with the furnace after 900 DEG C of insulation 0.5h after 1080 DEG C of insulation 2h; 9. cleaning, drying: use flowing water to rinse on the sample after pack cementation, then use alcohol washes, then dry, dry 5min at 60 DEG C, terminate.
Embodiment 3:
1. alkali cleaning: it is 65 DEG C of alkaline washs (alkaline wash adopts the sodium hydroxide solution of 0.1-0.2mol/L) that sample of TiAl alloy being had a try is placed in temperature, soaks 10 minutes; 2. wash: use flowing water to rinse on the sample after alkali cleaning; Dry up; 3. prepare penetration enhancer: accurately take penetration enhancer according to quantity, the proportioning of penetration enhancer is by weight percentage: 8%Cr powder, 6%Si powder, 4%Al powder, 8%AlCl 3powder (analytical pure), 2%Y 2o 3powder, all the other are aluminium oxide powder (≤200 order); 4. ball milling: the penetration enhancer prepared is placed in grinding in ball grinder, makes it fully mix, and refinement penetration enhancer particle is to being no more than 200 orders; 5. dry: the penetration enhancer after ball milling being placed in temperature is that the baking oven of 100 DEG C is incubated 1h and dries; 6. embed: the penetration enhancer of drying is loaded corundum crucible, and sample is imbedded in penetration enhancer, keep certain distance (>=5cm) between adjacent samples, 7. seal: the crucible that sample is housed is added a cover and uses silicon sol and aluminium sesquioxide sealing to be placed on also applying argon gas protection in vacuum oven; 8. pack cementation: vacuum oven is intensification 50min to 900 DEG C at the uniform velocity, to 1080 DEG C after the 10min that continues at the uniform velocity to heat up, cools to room temperature with the furnace after 900 DEG C of insulation 0.5h after 1080 DEG C of insulation 2.5h; 9. cleaning, drying: use flowing water to rinse on the sample after pack cementation, then use alcohol washes, then dry, dry 3min at 90 DEG C, terminate.

Claims (8)

1. a penetration enhancer, is characterized in that, according to weight percent, it consists of: 6%-10%Cr, 4%-8%Si, 2%-6%Al, 1%-2%Y 2o 3, 6%-10%AlCl 3, surplus is Al 2o 3.
2. a kind of penetration enhancer as claimed in claim 1, is characterized in that: wherein Cr, Si, Al, Y 2o 3, AlCl 3and Al 2o 3be Powdered, and Al 2o 3be no more than 200 orders.
3. a preparation technology for high temperature resistant heat and corrosion resistant anti-scuff coating, is characterized in that, comprise the steps:
(1) alkali cleaning: TiAl alloy sample or workpiece being placed in temperature is 65 ~ 80 DEG C of alkaline washs, soaks 10 ~ 15 minutes;
(2) wash: the sample after alkali cleaning or workpiece use water are rinsed, then dries up stand-by;
(3) ball milling: according to the record in claim 1, is placed in grinding in ball grinder and makes its final size scope be 20-50 μm by the penetration enhancer prepared;
(4) dry: the penetration enhancer after ball milling is dried;
(5) embed: the penetration enhancer of drying is loaded crucible, and sample or workpiece are imbedded in penetration enhancer, make not contact between adjacent samples or workpiece;
(6) shove charge is sealed: sealed by crucible and be placed in vacuum oven, and applying argon gas protection;
(7) pack cementation: vacuum oven is warming up to 900-920 DEG C, insulation 0.5h follow-up continuing is warming up to 1080-1100 DEG C, cools to room temperature with the furnace after insulation 1.5-2.5h;
(8) cleaning, drying: the sample use water after pack cementation is rinsed, then uses alcohol washes, finally dry.
4. the preparation technology of a kind of high temperature resistant heat and corrosion resistant anti-scuff coating as claimed in claim 3, is characterized in that: in step (1), alkaline wash adopts the sodium hydroxide solution of 0.1-0.2mol/L.
5. the preparation technology of a kind of high temperature resistant heat and corrosion resistant anti-scuff coating as claimed in claim 3, is characterized in that: being specifically placed in temperature in step (4) is that the baking oven of 100-150 DEG C is incubated 1-2h and dries.
6. the preparation technology of a kind of high temperature resistant heat and corrosion resistant anti-scuff coating as claimed in claim 3, it is characterized in that: in step (6), sealing specifically refers to that the collocation method of this silicon sol and aluminium sesquioxide specifically adds the Al of 1 ~ 1.2kg at every 1L silicon sol with silicon sol and aluminium sesquioxide sealing 2o 3rear mixing.
7. the preparation technology of a kind of high temperature resistant heat and corrosion resistant anti-scuff coating as claimed in claim 3, it is characterized in that: step specifically rises to 900-920 DEG C with the temperature rise rate of 15-20 DEG C/min in (7), rise to 1080-1100 DEG C with the temperature rise rate of 15-20 DEG C/min after insulation 0.5h, then cool to room temperature with the furnace after being incubated 1.5-2.5h.
8. the preparation technology of a kind of high temperature resistant heat and corrosion resistant anti-scuff coating as claimed in claim 3, is characterized in that: dry in step (8) and specifically at 50-100 DEG C, dry 3-5min.
CN201510284741.1A 2015-05-29 2015-05-29 The preparation technology and its penetration enhancer of a kind of high temperature resistant heat and corrosion resistant anti-scuff coating Expired - Fee Related CN104862639B (en)

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CN105839048A (en) * 2016-04-08 2016-08-10 北方民族大学 High-temperature alloy oxidation-resistance and corrosion-resistant protective coating
CN106435460A (en) * 2016-10-18 2017-02-22 中国矿业大学 Niobium alloy surface high-temperature abrasion resisting coating and preparation method thereof
CN106521405A (en) * 2016-10-25 2017-03-22 北方民族大学 Impregnation agent for surface modification of nickel base alloy and utilization method of impregnation agent
CN107164722A (en) * 2017-06-23 2017-09-15 江苏双勤民生冶化设备制造有限公司 A kind of alloy surface coating and preparation method thereof
CN107779813A (en) * 2017-12-23 2018-03-09 北方民族大学 The preparation technology and its penetration enhancer of titanium-aluminium alloy surface C r Al Ce Y thermal protection coatings
CN109385600A (en) * 2017-08-02 2019-02-26 深圳先进技术研究院 Titanium-aluminium alloy part with compisite seeping layer and preparation method thereof, titanium-aluminium alloy part with diamond coatings and preparation method thereof
CN109689595A (en) * 2016-07-18 2019-04-26 圣戈班工业陶瓷罗登塔尔有限责任公司 On the surface with the roller for roll-type furnace of at least one coating

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CN1431338A (en) * 2002-01-10 2003-07-23 北京航空航天大学 Method for preparing coat of aluminide with chrome modified for enhancing performance of high heat oxidation resistance of TiAl alloy
CN102485934A (en) * 2010-12-01 2012-06-06 沈阳黎明航空发动机(集团)有限责任公司 Method for preparing hollow blade inner chamber diffusion layer with high temperature resistance, oxidation resistance and corrosion resistance
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CN109385600A (en) * 2017-08-02 2019-02-26 深圳先进技术研究院 Titanium-aluminium alloy part with compisite seeping layer and preparation method thereof, titanium-aluminium alloy part with diamond coatings and preparation method thereof
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