CN105839048B - A kind of high temperature alloy oxidation and corrosion protective coating and penetration enhancer - Google Patents
A kind of high temperature alloy oxidation and corrosion protective coating and penetration enhancer Download PDFInfo
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- CN105839048B CN105839048B CN201610217051.9A CN201610217051A CN105839048B CN 105839048 B CN105839048 B CN 105839048B CN 201610217051 A CN201610217051 A CN 201610217051A CN 105839048 B CN105839048 B CN 105839048B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/52—Embedding in a powder mixture, i.e. pack cementation more than one element being diffused in one step
- C23C10/54—Diffusion of at least chromium
- C23C10/56—Diffusion of at least chromium and at least aluminium
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Abstract
The present invention a kind of nickel base superalloy oxidation and corrosion protective coating penetration enhancer and the preparation process of the coating are disclosed, the protective coating penetration enhancer according to weight percent consisting of:5 10%Cr, 10% 20%Al, 1% 2%Y2O3, 6% 10%NH4Cl, surplus Al2O3.The preparation process of its coating is:It first accurately weighs according to quantity and prepares the protective coating penetration enhancer, then ball milling is carried out, it is dry, after drying crucible is packed into sample, sealing shove charge is placed in Muffle furnace, and Muffle furnace heats up 40 60min to 1050~1070 DEG C, with stove to 600 DEG C after 1050~1070 DEG C of 2 3h of heat preservation, taking-up is cooled to room temperature, last cleaning, drying.Can prepare Cr Al Y co-penetration layers on nickel-base alloy surface using protective coating penetration enhancer of the present invention, solve the technical barrier of nickel-base alloy high temperature resisting corrosion resisting poor performance, stable preparation process is reliable, coating binding force is good, even tissue, densification, coating layer thickness is controllable;And have many advantages, such as it is simple for process, easy to operate, efficient, of low cost, be easily achieved.
Description
Technical field:
It is prepared the present invention relates to a kind of nickel base superalloy oxidation and corrosion protective coating penetration enhancer and using the penetration enhancer anti-
Protect the preparation process of coating.
Background technology:
The high temperature alloys such as nickel-base alloy are widely used on the parts such as blade of aviation engine, turbine blade,
Its service condition is harsh, is vulnerable to high-temperature oxydation and heat erosion.Therefore the general requirement of high temperature alloy must be provided simultaneously with two aspects
Performance requirement, i.e., excellent mechanical behavior under high temperature and high temperature resisting corrosion resisting, but both be conflict, it is difficult to take into account.
The above-mentioned performance of alloy is mainly improved by alloying and process for modifying surface at present.Alloyage process improves its high-temperature oxydation
Performance has certain limitation, and can significantly reduce its mechanical property.And by process for modifying surface prepares coating, due to matrix
Alloy and protective coating can be designed individually, so the alloy component for applying protective coating is strong in the high temperature for keeping alloy enough
Alloy component surface has excellent high temperature resisting corrosion resisting performance again when spending.
Chromium compounds coating fusing point is high, good thermal stability, excellent corrosion resistance, is suitable for the high temperature antioxygen of high temperature alloy
Chemoprevention is protected.But single chromium compounds coating leads in it easily cracked, meeting in coating during simultaneous oxidation due to brittleness itself
Larger internal stress is generated, surface film oxide is caused to peel off and lose protectiveness, therefore, it is necessary to add other elements to carry out it
It is modified.The elements such as Al, Y are improving coating compactness and its with the binding force of matrix, the low-alloyed oxidation rate of drop and improving oxygen
Anti-strip ability for changing film etc. has remarkable result.
At present, the Cr-Al-Y co-penetration layers that method prepares on nickel base superalloy surface high temperature resisting corrosion resisting are oozed by diffusion
Technology of preparing and its application still belong to blank.Therefore, study and realize the corrosion resistant Cr-Al-Y of nickel base superalloy surface oxidation-resistant
The technology of preparing of coating is of great significance to nickel base superalloy engineer application.
Invention content:
It is an object of the invention to provide a kind of high temperature resisting corrosion resisting protective coating penetration enhancer and utilization for nickel base superalloy
The penetration enhancer prepares the preparation process of protective coating, which there is preparation process to be simple and convenient to operate, is of low cost, is easy
In realize, it is efficient the advantages of, suitable for producing and applying.
To achieve the above object, the present invention takes following technical scheme:
A kind of high temperature alloy oxidation and corrosion protective coating penetration enhancer, according to weight percent consisting of:5-10%Cr,
10%-20%Al, 1%-2%Y2O3, 6%-10%NH4Cl, surplus Al2O3。
Cr, Al, Y in the composition of the protective coating penetration enhancer2O3、NH4Cl and Al2O3It is powdered, and Al2O3It is no more than
250 mesh.
A kind of preparation process of high temperature alloy oxidation and corrosion protective coating provided by the invention, includes the following steps:
S1:Surface preparation:By removings such as the oxide skin of nickel-based alloy sample or workpiece surface, burs, sample is kept
Surface cleaning;
S2:Alkali cleaning:Said sample or workpiece are placed in temperature in 65~80 DEG C of alkali wash waters, to impregnate 10~15min;
S3:Washing:Sample after above-mentioned alkali cleaning or workpiece are rinsed using circulating water, then drying is for use;
S4:Prepare protective coating penetration enhancer:The protective coating penetration enhancer is prepared, is according to weight percent composition:5-
10%Cr powder, 10%-20%Al powder, 1%-2%Y2O3Powder, 6%-10%NH4Cl powder, remaining is Al2O3(≤250 mesh);
S5:Ball milling:Above-mentioned prepared protective coating penetration enhancer is placed in ball mill and grinds 1-3h, makes its ingredient uniform,
And crystal grain thinning can be played the role of;
S6:It is dry:Protective coating penetration enhancer after ball milling is placed in the baking oven that temperature is 100-150 DEG C and keeps the temperature 0.5-1h
Afterwards, it is dried;
S7:Embedding:Protective coating penetration enhancer after above-mentioned drying is packed into crucible, and above-mentioned for use sample or workpiece are buried
Enter in protective coating, make not contact between adjacent samples or workpiece;
S8:Seal shove charge:Crucible is capped, is placed in Muffle furnace using Ludox and alundum (Al2O3) sealing,
0.5h is kept the temperature at 100-150 DEG C, Ludox and alundum (Al2O3) sealant is fully cured, wherein Ludox and alundum (Al2O3)
Configuration method be every 1L Ludox add in 1~1.2kgAl2O3After mix;
S9:Pack cementation:Muffle furnace heats up 40-60min to 1050~1070 DEG C, and 2- is kept the temperature under the conditions of 1050~1070 DEG C
With stove to 600 DEG C after 3h, taking-up is cooled to room temperature;
S10:Cleaning, drying:Sample after pack cementation is rinsed using circulating water, then with alcohol washes, last natural wind
It is dry.
Alkali wash water uses 75~100g/LNaOH solution or 20~25g/LNa in step S23PO4Solution.
A kind of high temperature alloy oxidation and corrosion protective coating penetration enhancer of the present invention is by Cr powder, Al powder, Y2O3Powder, NH4Cl powder
And Al2O3 is formed, wherein Cr, Al, Y2O3To be oozed element, NH4Cl is catalyst, Al2O3For filler, realized using the penetration enhancer
Cr, Al, Y on nickel-base alloy surface is ternary co-osmosized, and prepared coating improves the high temperature resisting corrosion resisting of nickel-base alloy
Energy.
The beneficial effects of the present invention are:Using the high temperature alloy oxidation and corrosion protective coating penetration enhancer in nickel-base alloy
Surface is prepared for Cr-Al-Y co-penetration layers, solves the technology of nickel-base alloy high temperature resisting corrosion resisting (especially heat erosion) poor performance
Problem, the preparation technology of coating is reliable and stable, coating binding force is good, even tissue, densification, coating layer thickness is controllable.It is oozed using this
Agent prepare coating have many advantages, such as it is simple for process, easy to operate, efficient, of low cost, be easily achieved, using file side method,
The methods of scarification, rubbing manipulation and polishing processes, is detected binding force, and coating shows extraordinary binding force with matrix, high
Warm oxidation test and heat erosion experiment show that coating has good performance.
Description of the drawings:
Fig. 1 is the Cr-Al-Y co-penetration layer surface topography maps that are obtained using the embodiment of the present invention 1;
Fig. 2 is the Cr-Al-Y permeation layer cross section microstructure figures that are obtained using the embodiment of the present invention 1;
Fig. 3 is the Cr-Al-Y co-penetration layer surface topography maps that are obtained using the embodiment of the present invention 2;
Fig. 4 is the Cr-Al-Y permeation layer cross section microstructure figures that are obtained using the embodiment of the present invention 2;
Fig. 5 is the Cr-Al-Y co-penetration layer surface topography maps that are obtained using the embodiment of the present invention 3;
Fig. 6 is the Cr-Al-Y permeation layer cross section microstructure figures that are obtained using the embodiment of the present invention 3;
Fig. 7 is the Cr-Al-Y co-penetration layer cross sectional elements distribution maps that are obtained using the embodiment of the present invention 1.
Specific embodiment:
Technical scheme of the present invention is further described in the following with reference to the drawings and specific embodiments.
High temperature alloy oxidation and corrosion protective coating penetration enhancer of the present invention, in percentage by weight, specifically comprises:
(1) element is oozed:5-10%Cr, 10%-20%Al, 1%-2%Y2O3
(2) catalyst:6%-10%NH4Cl (analysis is pure)
(3) filler:Al2O3(≤250 mesh)
Cr, Al, Y in the composition of the protective coating penetration enhancer2O3、NH4Cl and Al2O3It is powdered, and Al2O3It is no more than
250 mesh.
The preparation process of high temperature alloy oxidation and corrosion protective coating of the present invention, includes the following steps:
S1:Surface preparation:By removings such as the oxide skin of nickel-based alloy sample or workpiece surface, burs, sample is kept
Surface cleaning;
S2:Alkali cleaning:Said sample or workpiece are placed in temperature in 65~80 DEG C of alkali wash waters, to impregnate 10~15min;
S3:Washing:Sample after above-mentioned alkali cleaning or workpiece are rinsed using circulating water, then drying is for use;
S4:Prepare protective coating penetration enhancer:The protective coating penetration enhancer is prepared, is according to weight percent composition:5-
10%Cr powder, 10%-20%Al powder, 1%-2%Y2O3Powder, 6%-10%NH4Cl powder, remaining is Al2O3(≤250 mesh);
S5:Ball milling:Above-mentioned prepared protective coating penetration enhancer is placed in ball mill and grinds 1-3h, makes its ingredient uniform,
And crystal grain thinning can be played the role of;
S6:It is dry:Protective coating penetration enhancer after ball milling is placed in the baking oven that temperature is 100-150 DEG C and keeps the temperature 0.5-1h
Afterwards, it is dried;
S7:Embedding:Protective coating penetration enhancer after above-mentioned drying is packed into crucible, and above-mentioned for use sample or workpiece are buried
Enter in protective coating penetration enhancer, make not contact between adjacent samples or workpiece;
S8:Seal shove charge:Crucible is capped, is placed in Muffle furnace using Ludox and alundum (Al2O3) sealing,
0.5h is kept the temperature at 100-150 DEG C, Ludox and alundum (Al2O3) sealant is fully cured, wherein Ludox and alundum (Al2O3)
Configuration method be every 1L Ludox add in 1~1.2kgAl2O3After mix;
S9:Pack cementation:Muffle furnace heats up 40-60min to 1050~1070 DEG C, and 2- is kept the temperature under the conditions of 1050~1070 DEG C
With stove to 600 DEG C after 3h, taking-up is cooled to room temperature;
S10:Cleaning, drying:Sample after pack cementation is rinsed using circulating water, then with alcohol washes, last natural wind
It is dry.
Embodiment 1:
1. surface preparation:By removings such as the oxide skin of nickel-based alloy sample or workpiece surface, burs, sample table is kept
It cleans in face;2. alkali cleaning:Sample or workpiece are placed in temperature in 65 DEG C of alkali wash waters, to impregnate 15min;3. it washes:After alkali cleaning
Sample or workpiece are rinsed using circulating water, and then drying is for use;4. prepare protective coating penetration enhancer:It accurately weighs, protects according to quantity
The proportioning of coating penetration enhancer is by weight percentage:5%Cr powder, 10%Al powder, 6%NH4Cl (analysis is pure), 1%Y2O3Powder, remaining
For Al2O3Powder (≤250 mesh);5. ball milling:Prepared protective coating penetration enhancer is placed in ball mill and grinds 1-3h, makes its ingredient
Uniformly, and crystal grain thinning can be played the role of, refinement penetration enhancer particle is to no more than 200 mesh;6. it dries:Protection after ball milling is applied
Layer penetration enhancer is placed in the baking oven that temperature is 100 DEG C after heat preservation 1h, is dried;7. it embeds:By the protective coating penetration enhancer after drying
Corundum crucible is packed into, and in for use sample or workpiece embedment protective coating penetration enhancer, makes to keep between adjacent samples or workpiece
Certain distance (for example, at least 1cm);8. it seals:Crucible is capped, Muffle is placed on using Ludox and alundum (Al2O3) sealing
In stove, 0.5h is kept the temperature at 150 DEG C, Ludox and alundum (Al2O3) sealant is fully cured, wherein Ludox and three oxidations
The configuration method of two aluminium is that the Al of 1.0kg is added in every 1L Ludox2O3After mix;9. pack cementation:Muffle furnace heating 40-60min
To 1070 DEG C (temperature-rise periods keep substantially at the uniform velocity), kept the temperature at 1070 DEG C after 2h with stove to after 600 DEG C, taking-up is cooled to room temperature;
10. cleaning, drying:Sample after pack cementation is rinsed using circulating water, then with alcohol washes, last natural air drying.
Embodiment 2:
1. surface preparation:By removings such as the oxide skin of nickel-based alloy sample or workpiece surface, burs, sample table is kept
It cleans in face;2. alkali cleaning:Sample or workpiece are placed in temperature in 70 DEG C of alkali wash waters, to impregnate 12min;3. it washes:After alkali cleaning
Sample or workpiece are rinsed using circulating water, and then drying is for use;4. prepare protective coating penetration enhancer:It accurately weighs, protects according to quantity
The proportioning of coating penetration enhancer is by weight percentage:8%Cr powder, 15%Al powder, 8%NH4Cl (analysis is pure), 1.5%Y2O3Powder,
Remaining is Al2O3Powder (≤250 mesh);5. ball milling:Prepared protective coating penetration enhancer is placed in ball mill and grinds 1-3h, make its into
Divide uniformly, and crystal grain thinning can be played the role of, refinement penetration enhancer particle is to no more than 200 mesh;6. it dries:By the protection after ball milling
Coating penetration enhancer is placed in the baking oven that temperature is 120 DEG C after heat preservation 40min, is dried;7. it embeds:By the protective coating after drying
Penetration enhancer is packed into corundum crucible, and in for use sample or workpiece embedment protective coating, makes to keep between adjacent samples or workpiece
Certain distance (for example, at least 1cm);8. it seals:Crucible is capped, Muffle is placed on using Ludox and alundum (Al2O3) sealing
In stove, 0.5h is kept the temperature at 100 DEG C, Ludox and alundum (Al2O3) sealant is fully cured, wherein Ludox and three oxidations
The configuration method of two aluminium is to add in 1.0kgAl in every 1L Ludox2O3After mix;9. pack cementation:Muffle furnace heating 40-60min is extremely
1060 DEG C (temperature-rise periods keep substantially at the uniform velocity) are kept the temperature after 2.5h with stove at 1060 DEG C to after 600 DEG C, and taking-up is cooled to room temperature;
10. cleaning, drying:Sample after pack cementation is rinsed using circulating water, then with alcohol washes, last natural air drying.
Embodiment 3:
1. surface preparation:By removings such as the oxide skin of nickel-based alloy sample or workpiece surface, burs, sample table is kept
It cleans in face;2. alkali cleaning:Sample or workpiece are placed in temperature in 80 DEG C of alkali wash waters, to impregnate 10min;3. it washes:After alkali cleaning
Sample or workpiece are rinsed using circulating water, and then drying is for use;4. prepare protective coating penetration enhancer:It accurately weighs, protects according to quantity
The proportioning of coating penetration enhancer is by weight percentage:10%Cr powder, 20%Al powder, 10%NH4Cl (analysis is pure), 2%Y2O3Powder,
Remaining is Al2O3Powder (≤250 mesh);5. ball milling:Prepared protective coating penetration enhancer is placed in ball mill and grinds 1-3h, make its into
Divide uniformly, and crystal grain thinning can be played the role of, refinement penetration enhancer particle is to no more than 200 mesh;6. it dries:By the protection after ball milling
Coating penetration enhancer is placed in the baking oven that temperature is 150 DEG C after heat preservation 0.5h, is dried;7. it embeds:By the protective coating after drying
Penetration enhancer is packed into corundum crucible, and in for use sample or workpiece embedment protective coating penetration enhancer, makes between adjacent samples or workpiece
Keep certain distance (for example, at least 1cm);8. it seals:Crucible is capped, is placed on using Ludox and alundum (Al2O3) sealing
In Muffle furnace, 0.5h is kept the temperature at 120 DEG C, Ludox and alundum (Al2O3) sealant is fully cured, wherein Ludox and three
The configuration method of Al 2 O is to add in 1.0kgAl in every 1L Ludox2O3After mix;9. pack cementation:Muffle furnace heating 40-
60min to 1050 DEG C (temperature-rise period keep substantially at the uniform velocity) is kept the temperature after 3h with stove at 1050 DEG C to after 600 DEG C, and taking-up is cooled to
Room temperature;10. cleaning, drying:Sample after pack cementation is rinsed using circulating water, then with alcohol washes, last natural air drying is
It can.
As shown in Fig. 1~7, the Cr-Al-Y co-penetration layer surface topographies that are obtained using 1~embodiment of the embodiment of the present invention 3
Figure and section microstructure figure and cross sectional elements distribution map are visible:Cr, Al, Y element realize permeation, entire quality layer
Well.
Claims (3)
1. a kind of high temperature alloy oxidation and corrosion protective coating penetration enhancer, it is characterised in that:According to weight percent consisting of:
5-10%Cr, 10%-20%Al, 1%-2%Y2O3, 6%-10%NH4Cl, surplus Al2O3;The composition of the protective coating penetration enhancer
Middle Cr, Al, Y2O3、NH4Cl and Al2O3It is powdered, and Al2O3No more than 250 mesh.
2. a kind of preparation process of high temperature alloy oxidation and corrosion protective coating, it is characterised in that:Include the following steps:
S1:Surface preparation:By removings such as the oxide skin of nickel-based alloy sample or workpiece surface, burs, sample or work are kept
Part surface cleaning;
S2:Alkali cleaning:Said sample or workpiece are placed in temperature in 65~80 DEG C of alkali wash waters, to impregnate 10~15min;
S3:Washing:Sample after above-mentioned alkali cleaning or workpiece are rinsed using circulating water, then drying is for use;
S4:Prepare protective coating penetration enhancer:The protective coating penetration enhancer is prepared, is according to weight percent composition:5-10%
Cr powder, 10%-20%Al powder, 1%-2%Y2O3Powder, 6%-10%NH4Cl powder, remaining is Al2O3, and Al2O3≤ 250 mesh;
S5:Ball milling:Above-mentioned prepared protective coating penetration enhancer is placed in ball mill and grinds 1-3h, makes its ingredient uniform, and energy
Play the role of crystal grain thinning;
S6:It is dry:Protective coating penetration enhancer after ball milling is placed in the baking oven that temperature is 100-150 DEG C after heat preservation 0.5-1h, into
Row drying;
S7:Embedding:Protective coating penetration enhancer after above-mentioned drying is packed into crucible, and above-mentioned for use sample or workpiece are embedded to and prevented
It protects in coating penetration enhancer, makes not contact between adjacent samples or workpiece;
S8:Seal shove charge:Crucible is capped, is placed in Muffle furnace using Ludox and alundum (Al2O3) sealing, in 100-150
0.5h is kept the temperature at DEG C, Ludox and alundum (Al2O3) sealant is fully cured, wherein the configuration of Ludox and alundum (Al2O3)
Method is to add in 1~1.2kgAl in every 1L Ludox2O3After mix;
S9:Pack cementation:Muffle furnace heats up 40-60min to 1050~1070 DEG C, after keeping the temperature 2-3h under the conditions of 1050~1070 DEG C
With stove to 600 DEG C, taking-up is cooled to room temperature;
S10:Cleaning, drying:Sample after pack cementation or workpiece are rinsed using circulating water, it is last natural then with alcohol washes
It air-dries.
3. a kind of preparation process of high temperature alloy oxidation and corrosion protective coating according to claim 2, feature exist
In:Alkali wash water described in step S2 uses 75~100g/L NaOH solutions or 20~25g/L Na3PO4Solution.
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Cited By (1)
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CN108914054A (en) * | 2018-07-17 | 2018-11-30 | 北方民族大学 | The preparation process and its penetration enhancer of nickel-base alloy surface oxidation-resistant heat and corrosion resistant Cr-Si-B-Y coating |
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CN107401194A (en) * | 2017-08-04 | 2017-11-28 | 安徽省宁国市亚晨碾磨铸件有限责任公司 | A kind of excavator high-strength wearable bucket tooth and its preparation technology |
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 |
CN108546909B (en) * | 2018-05-11 | 2020-06-23 | 中南大学 | Liquid penetrant for aluminum-nickel slurry on surface of nickel-based superalloy and preparation method of liquid penetrant |
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CN104862639A (en) * | 2015-05-29 | 2015-08-26 | 北方民族大学 | Preparation method of high-temperature-resistant, heat-corrosion-resistant and abrasion-resistant coating and penetrating agent |
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CN102115866A (en) * | 2009-12-30 | 2011-07-06 | 中国科学院金属研究所 | NiCrAIY coating for nickel base high temperature alloy and preparation method thereof |
CN103060747A (en) * | 2012-12-13 | 2013-04-24 | 北京航空航天大学 | Method for preparing Y modified CoAlNi coating on Ni-based high temperature alloy by embedding infiltration process |
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CN108914054A (en) * | 2018-07-17 | 2018-11-30 | 北方民族大学 | The preparation process and its penetration enhancer of nickel-base alloy surface oxidation-resistant heat and corrosion resistant Cr-Si-B-Y coating |
CN108914054B (en) * | 2018-07-17 | 2020-07-10 | 北方民族大学 | Preparation process of oxidation-resistant hot corrosion-resistant Cr-Si-B-Y coating on surface of nickel-based alloy and penetrating agent thereof |
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