CN105385987B - Tungsten surface high-temp anti oxidation layer and preparation method thereof - Google Patents
Tungsten surface high-temp anti oxidation layer and preparation method thereof Download PDFInfo
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- CN105385987B CN105385987B CN201510664159.8A CN201510664159A CN105385987B CN 105385987 B CN105385987 B CN 105385987B CN 201510664159 A CN201510664159 A CN 201510664159A CN 105385987 B CN105385987 B CN 105385987B
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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
- C23C10/36—Embedding in a powder mixture, i.e. pack cementation only one element being diffused
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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
- C23C10/36—Embedding in a powder mixture, i.e. pack cementation only one element being diffused
- C23C10/44—Siliconising
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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
- C23C10/60—After-treatment
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Abstract
The present invention discloses a kind of preparation method of tungsten surface high-temp anti oxidation layer, including：It is smooth that tungsten base material is polished to surface, and ungrease treatment of deoiling is carried out to polished surface；By treated, tungsten base material is embedded to molybdenum penetration enhancer, is then heat-treated in inert atmosphere, and impurity is removed after cooling, and obtaining tungsten surface has the semi-finished product of tungsten solid solution layer；The semi-finished product are placed in nitrogen atmosphere and are heat-treated, impurity is removed after cooling, obtain the precast body that tungsten surface is molybdenum nitride and Tungsten nitride coatings；And precast body is embedded in silication penetration enhancer, it is then heat-treated in inert atmosphere, impurity is removed after cooling, obtain the finished product that tungsten substrate surface is W-Mo-N-Si systems high-temperature oxidation resistant layer.The invention further relates to a kind of tungsten surface high-temp anti oxidation layers obtained by the above method.
Description
Technical field
The present invention relates to a kind of tungsten surface high-temp anti oxidation layers and preparation method thereof.
Background technology
High density tungsten sill be widely used in defence and military, mechano-electronic, space flight and aviation, metallurgical mine, oil coal,
The fields such as clock and watch ornaments.There are not wear-resisting, inoxidizability is poor, the corrosion of easy sweat stain and color dimness etc. lack for the tungsten material of non-coating
It falls into.
CN101195285 discloses a kind of coating tungsten product, including tungsten base material, is coated with thickness on the tungsten base material
3-30 μm of TiN or Cu (surplus)-(15-45) %Zn- (0.1-1.5) %Ni- (0.5-1) %Al2O3Alloy-coated
Layer.The coating tungsten product can effectively improve the anti-of tungsten sill surface under the conditions of guarantee tungsten sill high relative density
Oxidisability, wearability, perspiration resistance corrosivity and property bright in luster etc. integrate performance.However, the coating tungsten product is to use
CVD or PVD methods obtain, and preparation process is complex, production cost is higher, and there are the compactness of coating poor, coating
The problems such as structure and phase of poor, the uncontrollable coating of thermal matching between matrix, thus directly affect the height of tungsten
The warm usage service life.Du Zhiqiang obtains coating using electroplating technology in tungsten base powder metallurgy material, and technique is electrolytic degreasing-cyaniding
Copper facing-plating bright copper-bright nickel plating, but the binding force of part and coating is not still high, while finding that part edge has corrosion existing
As thickness of coating is uneven, and corrosion resistance is also not achieved using standard.
Invention content
A kind of tungsten surface high-temp anti oxidation layer of present invention offer and preparation method thereof, can effectively solve above-mentioned ask
Topic.
The present invention provides a kind of preparation method of tungsten surface high-temp anti oxidation layer, wherein includes the following steps：
It is smooth that tungsten base material is polished to surface, and ungrease treatment of deoiling is carried out to polished surface；
By treated, tungsten base material is embedded to molybdenum penetration enhancer, is then heat-treated in inert atmosphere, goes to clean after cooling
Matter, obtaining tungsten surface has the semi-finished product of tungsten solid solution layer；
The semi-finished product are placed in nitrogen atmosphere and are heat-treated, remove impurity after cooling, obtaining tungsten surface is
The precast body of molybdenum nitride and Tungsten nitride coatings；And
Precast body is embedded in silication penetration enhancer, is then heat-treated in inert atmosphere, impurity is removed after cooling, obtains metal
Tungsten substrate surface is the finished product of W-Mo-N-Si systems high-temperature oxidation resistant layer.
Further, the preparation method of the molybdenum penetration enhancer includes：
Weigh the molybdenum powder that mass fraction is 10~40 parts, the NH that mass fraction is 1~20 part4Cl, mass fraction be 40~
89 parts of Al2O3, ball milling 1~10 hour after mixing；And
Under vacuum conditions, 100~150 DEG C of temperature drying 10~30 minutes.
Further, a diameter of 500 nanometers to 10 microns of the molybdenum powder.
Further, tungsten base material is embedded to molybdenum penetration enhancer and the temperature being heat-treated is 850~1100 DEG C, heat preservation
Time is 1~24 hour.
Further, tungsten base material is embedded to molybdenum penetration enhancer and the temperature being heat-treated is 900~1000 DEG C, heat preservation
Time is 4~10 hours.
Further, described that semi-finished product are placed in 1000~1500 DEG C of temperature being heat-treated in nitrogen atmosphere, nitridation
Time is 1~24 hour, and the flow velocity of nitrogen is 50~500mL/min.
Further, the preparation method of the silication penetration enhancer includes：
It is 40~89 by silica flour, the NaF that mass fraction is 1~10 part and mass fraction that mass fraction is 10~50 parts
The Al of part2O3, ball milling 1~10 hour after mixing；And
Under vacuum conditions, 80~100 DEG C of temperature drying 10~60 minutes.
Further, it is 800~1400 DEG C that precast body is embedded to the temperature being heat-treated in silication penetration enhancer, soaking time 1
~24 hours.
Further, it is 900~1000 DEG C that precast body is embedded to the temperature being heat-treated in silication penetration enhancer, soaking time 5
~10 hours.
The present invention also provides a kind of tungsten surface high-temp anti oxidation layers, are coated on a tungsten substrate surface, wherein institute
It is W-Mo-N-Si systems protective layer to state high-temperature oxidation resistant layer.
Tungsten surface high-temp anti oxidation layer provided by the invention and preparation method thereof, has the advantages that：
(1) present invention uses the in-situ reaction of molybdenum+nitridation+silication.Compared with prior art, it the advantage is that and be not required to
Expensive device, preparation process is simple, at low cost, can handle complex-shaped tungsten product and protective layer structure and phase are controllable.
(2) present invention is formed on tungsten surface with (W by in-situ reactionxMo1-x)Si2Solid solution phase is to advocate peace on a small quantity
Si3N4The composite layer of phase.Mo elements be introduced into effectively reduce in high-temperature oxidation process diffusion rate from Si to intrinsic silicon, it is bright
Aobvious " degeneration " for slowing down silicide coating.Compared with prior art, the high-temperature oxidation resistance of coating tungsten product material of the present invention is more
Excellent, coat inside defect is less.
(3) antioxygenic property of the tungsten surface high-temp anti oxidation layer obtained can reach complete grade of oxidation resistance, from
And the defects of tungsten sill inoxidizability is poor, easy sweat stain corrosion and color is dim can be solved.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail.It is understood that tool described herein
Body embodiment is used only for explaining the present invention rather than limitation of the invention.It is anti-that the present invention provides a kind of tungsten surface high-temp
The preparation method of oxide layer, includes the following steps：
It is smooth to be polished to surface, and carries out ungrease treatment of deoiling to polished surface by S1 for tungsten base material；
S2, by treated, tungsten base material is embedded to molybdenum penetration enhancer, is then heat-treated in inert atmosphere, is removed after cooling
Impurity, obtaining tungsten surface has the semi-finished product of tungsten solid solution layer；
The semi-finished product are placed in nitrogen atmosphere and are heat-treated by S3, remove impurity after cooling, obtain tungsten surface
For the precast body of molybdenum nitride and Tungsten nitride coatings；And
Precast body is embedded in silication penetration enhancer, is then heat-treated in inert atmosphere by S4, removes impurity after cooling, obtains
Tungsten substrate surface is the finished product of W-Mo-N-Si systems high-temperature oxidation resistant layer.
In step sl, it is described to polished surface deoil ungrease treatment the step of include：
Tungsten base material after the polishing is immersed in a volatile organic solvent and is cleaned by S11；And
Tungsten base material after cleaning is taken out and is dried up by S12.
The volatile organic solvent is used to dissolve grease on substrate surface, can be selected from methanol, ethyl alcohol, propyl alcohol,
Acetone, ether and its mixture.
In step s 2, the molybdenum penetration enhancer can be obtained by following steps：
S21 weighs the molybdenum powder that mass fraction is 10~40 parts, the NH that mass fraction is 1~20 part4Cl, mass fraction are
40~89 parts of Al2O3, ball milling 1~10 hour after mixing, it is preferred that weigh the molybdenum powder that mass fraction is 20~30 parts, mass parts
The NH that number is 10~15 parts4Cl, the Al that mass fraction is 60~80 parts2O3, it is furthermore preferred that it is 25~30 parts to weigh mass fraction
Molybdenum powder, mass fraction is 12~15 parts of NH4Cl, the Al that mass fraction is 60~70 parts2O3；And
S22, under vacuum conditions, the drying 10~30 minutes of 100~150 DEG C of temperature.
In the step s 21, the diameter of the molybdenum powder is preferably 500 nanometers to 10 microns；It is furthermore preferred that the molybdenum powder is straight
Diameter is preferably 1 micron to 5 microns.It is demonstrated experimentally that when the diameter of molybdenum powder is excessive, tungsten metallic substrate surface, diameter can not be penetrated into
It is too small, it is relatively easy to generate reunion, is also unfavorable for penetrating into tungsten metallic substrate surface.
The temperature that tungsten base material is embedded to molybdenum penetration enhancer and is heat-treated can be 850~1100 DEG C, and protect
The warm time is 1~24 hour, and heating rate is 5~15 DEG C/min.Preferably, tungsten base material is embedded to molybdenum penetration enhancer and carried out
The temperature of heat treatment is 900~1000 DEG C, and soaking time is 4~10 hours.Experiment is found, in 900~1000 DEG C of temperature ranges
Molybdenum inside may be implemented quickly to penetrate into.
In step s3, described that semi-finished product are placed in 1000~1500 DEG C of temperature being heat-treated in nitrogen atmosphere, nitrogen
It is 1~24 hour to change the time, and the flow velocity of nitrogen is 50~500mL/min, and heating rate is 5~15 DEG C/min.
In step s 4, the preparation method of the silication penetration enhancer includes：
Silica flour, the NaF that mass fraction is 1~10 part and mass fraction that mass fraction is 10~50 parts are 40 by S41
~89 parts of Al2O3, ball milling 1~10 hour after mixing, preferably, silica flour that mass fraction is 20~30 parts, mass fraction 1
The Al that~5 parts of NaF and mass fraction is 70~80 parts2O3, more preferably, mass fraction be 25~30 parts silica flour, quality
The Al that the NaF and mass fraction that number is 2~4 parts are 75~80 parts2O3；And
S42, under vacuum conditions, the drying 10~60 minutes of 80~100 DEG C of temperature.
The diameter of the silica flour is preferably 500 nanometers to 10 microns；It is furthermore preferred that the diameter of the silica flour is preferably 1 micro-
Rice is to 5 microns.It is demonstrated experimentally that when the diameter of silica flour is excessive, tungsten metallic substrate surface can not be penetrated into, diameter is too small, more holds
It is also easy to produce reunion, is also unfavorable for penetrating into tungsten metallic substrate surface.
Further, it is 800~1400 DEG C that precast body is embedded to the temperature being heat-treated in silication penetration enhancer, soaking time 1
~24 hours.Preferably, it is 900~1000 DEG C precast body to be embedded to the temperature that is heat-treated in silication penetration enhancer, soaking time is 5~
10 hours.
The embodiment of the present invention also provides one kind and obtaining tungsten surface high-temp anti oxidation layer by the above method, is coated on one
Tungsten substrate surface, and, the high-temperature oxidation resistant layer is W-Mo-N-Si systems protective layer.W-Mo-N-Si systems protective layer by
Include Mo, N and Si successively from inside to outside.The thickness of W-Mo-N-Si systems protective layer is 500 nanometers~10 microns, it is preferred that
The thickness of W-Mo-N-Si systems protective layer is 1 micron~5 microns, it is furthermore preferred that the thickness of W-Mo-N-Si systems protective layer
Degree is 2 microns~3 microns.
Embodiment 1：
It is smooth that tungsten base material with sand paper is polished to surface, and is put into absolute ethyl alcohol and carries out ungrease treatment of deoiling
Afterwards, it dries up；Pretreated tungsten base material is placed in the alumina crucible for filling molybdenum penetration enhancer, molybdenum in the molybdenum penetration enhancer
Powder, NH4Cl and Al2O3Mass ratio be 30: 10: 60, alumina crucible is put into heating furnace and is heated, and be passed through nitrogen progress
Protection rises to 950 DEG C with the heating rate of 10 DEG C/min and keeps the temperature 5 hours, cools to room temperature after heat preservation with the furnace, then take
Go out to be placed in distilled water and boil 10min, rinsed with deionized water, absolute ethyl alcohol wiping drying, it is tungsten to obtain tungsten surface
The semi-finished product of molybdenum solid solution layer；Semi-finished product are placed in atmosphere furnace, 99.99% nitrogen that flow is 300mL/min are passed through, with 5
DEG C/heating rate of min cools to room temperature with the furnace after rising to 1000 DEG C of heat preservations 20 hours, then takes out sample, it is clear with ultrasonic wave
10min is washed, absolute ethyl alcohol wiping drying obtains the precast body that tungsten surface is molybdenum nitride and tungsten nitride layer；Precast body is set
In the alumina crucible for filling silication penetration enhancer, silica flour, NaF and Al in the silication penetration enhancer2O3Mass ratio be 20：5: 75, by oxygen
Change aluminium crucible, which is put into heating furnace, to be heated, and is passed through nitrogen and is protected, and 1000 DEG C are risen to simultaneously with the heating rate of 15 DEG C/min
Heat preservation 15 hours, cools to room temperature with the furnace after heat preservation, then take out to be placed in distilled water and boil 10min, use deionization
Water rinses, and absolute ethyl alcohol wiping drying obtains the finished product that tungsten basal body surface is W-Mo-N-Si systems protective layer.
Embodiment 2：
It is smooth that tungsten base material with sand paper is polished to surface, and is put into absolute ethyl alcohol and carries out ungrease treatment of deoiling
Afterwards, it dries up；Pretreated tungsten base material is placed in the alumina crucible for filling molybdenum penetration enhancer, molybdenum in the molybdenum penetration enhancer
Powder, NH4Cl and Al2O3Mass ratio be 20：15: 65, alumina crucible is put into heating furnace and is heated, and is passed through nitrogen progress
Protection rises to 1000 DEG C with the heating rate of 10 DEG C/min and keeps the temperature 5 hours, cools to room temperature after heat preservation with the furnace, then
Taking-up, which is placed in distilled water, boils 10min, is rinsed with deionized water, and absolute ethyl alcohol wiping drying, obtaining tungsten surface is
The semi-finished product of tungsten solid solution layer；Semi-finished product are placed in atmosphere furnace, 99.99% nitrogen that flow is 300mL/min is passed through, with
The heating rate of 5 DEG C/min rise to 1000 DEG C heat preservation 20 hours after cool to room temperature with the furnace, then take out sample, it is clear with ultrasonic wave
10min is washed, absolute ethyl alcohol wiping drying obtains the precast body that tungsten surface is molybdenum nitride and tungsten nitride layer；Precast body is set
In the alumina crucible for filling silication penetration enhancer, silica flour, NaF and Al in the silication penetration enhancer2O3Mass ratio be 30：10: 60, it will
Alumina crucible is put into heating furnace and heats, and is passed through nitrogen and is protected, and 1400 DEG C are risen to the heating rate of 15 DEG C/min
And keep the temperature 15 hours, cool to room temperature after heat preservation with the furnace, then take out and be placed in distilled water and boil 10min, spend from
Sub- water rinses, and absolute ethyl alcohol wiping drying obtains the finished product that tungsten basal body surface is W-Mo-N-Si systems protective layer.
Embodiment 3：
It is smooth that tungsten base material with sand paper is polished to surface, and is put into absolute ethyl alcohol and carries out ungrease treatment of deoiling
Afterwards, it dries up；Pretreated tungsten base material is placed in the alumina crucible for filling molybdenum penetration enhancer, molybdenum in the molybdenum penetration enhancer
Powder, NH4Cl and Al2O3Mass ratio be 40：5: 55, alumina crucible is put into heating furnace and is heated, and is passed through nitrogen and is protected
Shield rises to 1100 DEG C with the heating rate of 10 DEG C/min and keeps the temperature 5 hours, cools to room temperature after heat preservation with the furnace, then take
Go out to be placed in distilled water and boil 10min, rinsed with deionized water, absolute ethyl alcohol wiping drying, it is tungsten to obtain tungsten surface
The semi-finished product of molybdenum solid solution layer；Semi-finished product are placed in atmosphere furnace, 99.99% nitrogen that flow is 300mL/min are passed through, with 5
DEG C/heating rate of min cools to room temperature with the furnace after rising to 1300 DEG C of heat preservations 20 hours, then takes out sample, it is clear with ultrasonic wave
10min is washed, absolute ethyl alcohol wiping drying obtains the precast body that tungsten surface is molybdenum nitride and tungsten nitride layer；Precast body is set
In the alumina crucible for filling silication penetration enhancer, silica flour, NaF and Al in the silication penetration enhancer2O3Mass ratio be 40：10: 50, it will
Alumina crucible is put into heating furnace and heats, and is passed through nitrogen and is protected, and 1400 DEG C are risen to the heating rate of 15 DEG C/min
And keep the temperature 15 hours, cool to room temperature after heat preservation with the furnace, then take out and be placed in distilled water and boil 10min, spend from
Sub- water rinses, and absolute ethyl alcohol wiping drying obtains the finished product that tungsten basal body surface is W-Mo-N-Si systems protective layer.
The phase composition of high-temperature oxidation resistant silication layer obtained by above three embodiments is identical with institutional framework, and difference lies in work
The difference of skill, the diffraction peak intensity and thickness of layer phase composition are different, but obtained structure all even compacts, in metallurgy between interface
Combinations of states, it is not cracked the defects of.W-Mo-N-Si tungsten sill is tested in 1600 DEG C of big compression rings using cyclic oxidation
High-temperature oxidation resistance under border is still intact after showing tungsten sample oxidation 300 hours, and surface forms the glass-film of smooth densification.
According to the rating scale of national standard, W-Mo-N-Si based materials reach completely anti-oxidant in the antioxygenic property of 1600 DEG C of atmospheric environments
Grade.
Note that above are only presently preferred embodiments of the present invention and institute's application technology principle.It will be appreciated by those skilled in the art that
The present invention is not limited to specific embodiments described here, can carry out for a person skilled in the art it is various it is apparent variation,
It readjusts and substitutes without departing from protection scope of the present invention.Therefore, although being carried out to the present invention by above example
It is described in further detail, but the present invention is not limited only to above example, without departing from the inventive concept, also
May include other more equivalent embodiments, and the scope of the present invention is determined by scope of the appended claims.
Claims (5)
1. a kind of preparation method of tungsten surface high-temp anti oxidation layer, which is characterized in that include the following steps：
It is smooth that tungsten base material is polished to surface, and ungrease treatment of deoiling is carried out to polished surface；
By treated, tungsten base material is embedded to molybdenum penetration enhancer, is then heat-treated in inert atmosphere, removes impurity after cooling, obtains
There are the semi-finished product of tungsten solid solution layer to tungsten surface；The preparation method of the molybdenum penetration enhancer includes：
Weigh the molybdenum powder that mass fraction is 10~40 parts, the NH that mass fraction is 1~20 part4Cl, mass fraction are 40~89 parts
Al2O3, ball milling 1~10 hour after mixing；And under vacuum conditions, 100~150 DEG C of temperature drying 10~30 minutes；The molybdenum
A diameter of 1 micron to 5 microns of powder；
The semi-finished product are placed in nitrogen atmosphere and are heat-treated, impurity is removed after cooling, it is nitridation to obtain tungsten surface
The precast body of molybdenum and Tungsten nitride coatings；And
Precast body is embedded in silication penetration enhancer, is then heat-treated in inert atmosphere, impurity is removed after cooling, obtains tungsten base
Material surface is the finished product of W-Mo-N-Si systems high-temperature oxidation resistant layer；The preparation method of the silication penetration enhancer includes：
It it is 40~89 parts by silica flour, the NaF that mass fraction is 1~10 part and mass fraction that mass fraction is 10~50 parts
Al2O3, ball milling 1~10 hour after mixing；And under vacuum conditions, 80~1100 DEG C of temperature drying 10~60 minutes；The silicon
A diameter of 1 micron to 5 microns of powder.
2. the preparation method of tungsten surface high-temp anti oxidation layer according to claim 1, which is characterized in that by tungsten base
Material is embedded to molybdenum penetration enhancer and the temperature being heat-treated is 850~1100 DEG C, and soaking time is 1~24 hour.
3. the preparation method of tungsten surface high-temp anti oxidation layer according to claim 2, which is characterized in that by tungsten base
Material is embedded to molybdenum penetration enhancer and the temperature being heat-treated is 900~1000 DEG C, and soaking time is 4~10 hours.
4. the preparation method of tungsten surface high-temp anti oxidation layer according to claim 1, which is characterized in that it is described will half at
Product are placed in 1000~1500 DEG C of temperature being heat-treated in nitrogen atmosphere, and nitridation time is 1~24 hour, and the flow velocity of nitrogen
For 50~500mL/min.
5. the preparation method of tungsten surface high-temp anti oxidation layer according to claim 1, which is characterized in that bury precast body
It is 800~1400 DEG C to enter the temperature being heat-treated in silication penetration enhancer, and soaking time is 1~24 hour.
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| CN111996485A (en) * | 2020-07-15 | 2020-11-27 | 深圳艾利门特科技有限公司 | Tungsten-based material with high-temperature insulating coating and preparation method thereof |
| CN112226728B (en) * | 2020-10-15 | 2022-06-07 | 厦门理工学院 | Tungsten product with oxidation-resistant coating and preparation method thereof |
| CN113957438B (en) * | 2021-10-26 | 2024-03-12 | 昆明理工大学 | Preparation method of metal tungsten high-temperature oxidation-resistant gallium-based composite coating |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534469A (en) * | 2011-11-25 | 2012-07-04 | 厦门虹鹭钨钼工业有限公司 | High temperature anti-oxidation coating molybdenum material and preparation method thereof |
| CN102534617A (en) * | 2012-02-21 | 2012-07-04 | 西安建筑科技大学 | Method for preventing molybdenum and molybdenum alloys from being oxidized |
| CN103409718A (en) * | 2013-05-15 | 2013-11-27 | 厦门虹鹭钨钼工业有限公司 | High-temperature oxidation-resistant molybdenum material and production method thereof |
| CN104630699A (en) * | 2015-01-27 | 2015-05-20 | 航天材料及工艺研究所 | Method for preparing oxidation resistant coating on surface of niobium alloy material |
| CN104831231A (en) * | 2015-05-11 | 2015-08-12 | 长安大学 | Method for preparing anti-oxidation permeated layer on surface of molybdenum or molybdenum alloy |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6028903B2 (en) * | 1979-10-30 | 1985-07-08 | 三菱重工業株式会社 | Surface treatment method for metal materials |
-
2015
- 2015-10-15 CN CN201510664159.8A patent/CN105385987B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534469A (en) * | 2011-11-25 | 2012-07-04 | 厦门虹鹭钨钼工业有限公司 | High temperature anti-oxidation coating molybdenum material and preparation method thereof |
| CN102534617A (en) * | 2012-02-21 | 2012-07-04 | 西安建筑科技大学 | Method for preventing molybdenum and molybdenum alloys from being oxidized |
| CN103409718A (en) * | 2013-05-15 | 2013-11-27 | 厦门虹鹭钨钼工业有限公司 | High-temperature oxidation-resistant molybdenum material and production method thereof |
| CN104630699A (en) * | 2015-01-27 | 2015-05-20 | 航天材料及工艺研究所 | Method for preparing oxidation resistant coating on surface of niobium alloy material |
| CN104831231A (en) * | 2015-05-11 | 2015-08-12 | 长安大学 | Method for preparing anti-oxidation permeated layer on surface of molybdenum or molybdenum alloy |
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