CN105714243B - The method of tantalum surface tungsten functional coating is prepared under a kind of low temperature - Google Patents
The method of tantalum surface tungsten functional coating is prepared under a kind of low temperature Download PDFInfo
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- CN105714243B CN105714243B CN201610272362.5A CN201610272362A CN105714243B CN 105714243 B CN105714243 B CN 105714243B CN 201610272362 A CN201610272362 A CN 201610272362A CN 105714243 B CN105714243 B CN 105714243B
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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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Abstract
The method of tantalum surface tungsten functional coating is prepared under a kind of low temperature, comprising the following steps: S1, by matrix surface polishing treatment, described matrix includes tantalum, tantalum alloy or combinations thereof；S2, it will be reacted in matrix embedment embedding penetration enhancer after polishing, wherein embedding temperature is 240-280 DEG C, soaking time 1-8h, the embedding penetration enhancer includes evenly dispersed WCl6 powder, activator and Al2O3 powder, and the ratio of WCl6 powder is 30-50wt.% in the embedding penetration enhancer；S3, matrix and vacuum drying after heat preservation, after cleaning embedding.The present invention uses investment, and matrix and embedding penetration enhancer are in 240-280 DEG C of generation diffusion reaction, so that tungsten functional coating be made.Matrix is combined with tungsten functional coating, has the advantages that functional coating even compact, and obtain coating without high temperature or the method for pressurization, reduces the requirement to equipment, be suitble to large-scale production.
Description
Technical field
The present invention relates to prepare tantalum surface tungsten functional coating under the technical field of prepares coating more particularly to a kind of low temperature
Method.
Background technique
Tantalum has high density, high-melting-point, corrosion-resistant, excellent elevated temperature strength, good processability and solderability and low
The excellent performances such as modeling/crisp transition temperature and a variety of industries such as be widely used in electronics, chemical industry, weapon.But tantalum metal price is expensive,
Corrosion resistance is poor in certain atmospheres.Tungsten have very high fusing point, boiling point, high intensity, hardness, very
Small electron work functon and good chemical stability.Tungsten coating is prepared in tantalum substrate material surface, is widely used as height
Wear-resisting, anti-corrosion and heatshield material under warm operating condition.And tungsten is added in tantalum can form tantalum tungsten solid solution type alloy, tungsten
Good solution strengthening effect is played in tantalum-tungsten alloy, its tensile strength and strain hardening rate can be improved.
There is researcher to form certain thickness Ta-W diffusion layer by vacuum electron beam welding and in conjunction with heat and other static pressuring processes,
But this preparation temperature is high, technique is cumbersome, there is a problem of that at high cost, energy consumption is high.It is normal that CVD method, which prepares pure tungsten coating,
Under pressure or lower pressure, using the halide or carbonyl compound gas of hydrogen and tungsten as raw material, in the substrate surface of specific temperature conditions
Tungsten coating is finally obtained by mutual reduction reaction, it can be direct using the preparation that CVD technique carries out tungsten coating to part
High-compactness, the tungsten coating of high-purity are obtained, but tantalum itself absorbs hydrogen and can become fragile, and is easily broken off, the method is not suitable for tantalum
The preparation of surface tungsten coating.
Summary of the invention
The purpose of the present invention is to overcome the shortcomings of the existing technology, provides and a kind of prepares tantalum table using in a low temperature of investment
The method of face tungsten functional coating.
In order to solve the above technical problems, present invention employs following technical measures:
The method of tantalum surface tungsten functional coating is prepared under a kind of low temperature, comprising the following steps:
S1, by matrix surface polishing treatment, described matrix includes tantalum, tantalum alloy or combinations thereof；
S2 will react in the matrix embedment embedding penetration enhancer after polishing, wherein embedding temperature is 240-280 DEG C, soaking time
For 1-8h, the embedding penetration enhancer includes evenly dispersed WCl6 powder, activator and Al2O3 powder, and WCl6 in the embedding penetration enhancer
The ratio of powder is 30-50wt.%；
S3, matrix and vacuum drying after heat preservation, after cleaning embedding.
The present invention can also be further perfect by following technical measures:
As a further improvement, the ratio of the activator is 10-15wt.%, the ratio of the Al2O3 powder is 35-
60wt.%。
As a further improvement, the activator includes or mixtures thereof NaF powder, NH4Cl powder.
As a further improvement, the step of polishing treatment by matrix surface, includes:
Described matrix is heated to certain temperature by S11, and buffing wax is uniformly applied on matrix；
S12 places a period of time, handles matrix using absorbent cotton；And
Matrix is put into polishing machine and polishes by S13, wherein alkalescence polishing liquid, time 5- are used in polishing process
15min。
As a further improvement, further comprising step S14 after step s 13, the matrix after polishing is put into anhydrous
It is 5-30min that ultrasonic treatment time is carried out in ethyl alcohol.
As a further improvement, the ratio of WCl6 powder is 35-45wt.%, the ratio of the activator in the embedding penetration enhancer
Example is 12-15wt.%, and the ratio of the Al2O3 powder is 40-53 wt.%.
As a further improvement, the step of matrix cleaned after embedding and vacuum drying, includes:
S31 is first cleaned up the matrix after the embedding with ultrasonic wave, and ultrasonic treatment time is 5 ~ 20min；And
S32, at a temperature of 90-100 DEG C, vacuum drying.
As a further improvement, the embedding temperature is 260-280 DEG C.
A kind of tantalum or tantalum alloy composite material obtained using the above method, including matrix and it is coated on the base
The tungsten functional coating in body surface face, described matrix are tantalum or tantalum alloy, and tungstenic amount is 1.5-18 wt.% in the tungsten functional coating.
As a further improvement, functional coating obtained with a thickness of 3-7mm.
Compared with prior art, the invention has the following advantages that
1, using investment, matrix is embedded in embedding penetration enhancer and is reacted, embedding penetration enhancer includes evenly dispersed WCl6Powder, work
Agent and Al2O3Powder.Matrix and embedding penetration enhancer are in 240-280 DEG C of generation diffusion reaction, so that tungsten functional coating be made.Matrix with
Tungsten functional coating is combined, and has the advantages that functional coating even compact.And it is applied without high temperature or the method for pressurization
Layer, reduces the requirement to equipment, is suitble to large-scale production.
2, investment can be suitable for complex-shaped matrix prepares coating well.In this way, complex-shaped matrix preparation
Coating also can in this way, and Yi Shixian continuous production can further save resource and the energy, reduce cost.
3, activator is added in embedding penetration enhancer, such as NaF powder or NH4Cl powder can accelerate the infiltration process of wolfram element.It is wrapping
It buries and Al is added in penetration enhancer2O3Powder can be effectively prevented powder sintered in matrix surface, the compactness extent of raising tungsten functional coating.
4, the tantalum as made from investment or tantalum alloy composite material have functional coating, and in tungsten functional coating
Tungstenic amount is 1.5-18 wt.%, functional coating with a thickness of 3-7mm, tungsten functional coating has excellent machinery, chemistry and electrical property
Can, on matrix after plating functional coating, tantalum or the poor problem of tantalum alloy corrosion resistance are overcome, preparation process is also overcomed
Middle tantalum or tantalum alloy absorb protium become fragile, easy fracture the problem of, effectively extend the service life of matrix.
Detailed description of the invention
Attached drawing 1 is the flow diagram that the method for tantalum surface tungsten functional coating is prepared under low temperature of the present invention；
Fig. 2 is the Ta-W coating cross sections figure in the preparation method embodiment 2 of tantalum surface functional coating of the present invention
Fig. 3 is the Ta-W coating energy spectrum diagram in attached drawing 2 at A.
Specific embodiment
Present invention is further described in detail with specific embodiment with reference to the accompanying drawing.
Embodiment 1:
Referring to FIG. 1, a kind of method for preparing tantalum surface tungsten functional coating under low temperature, comprising the following steps:
S1, by matrix surface polishing treatment, described matrix includes tantalum, tantalum alloy or combinations thereof；
S2 will react in the matrix embedment embedding penetration enhancer after polishing, wherein embedding temperature is 240-280 DEG C, soaking time
For 1-8h, the embedding penetration enhancer includes evenly dispersed WCl6 powder, activator and Al2O3 powder, and WCl6 in the embedding penetration enhancer
The ratio of powder is 30-50wt.%；
S3, matrix and vacuum drying after heat preservation, after cleaning embedding.
Using investment, matrix is embedded in embedding penetration enhancer and is reacted, embedding penetration enhancer includes evenly dispersed WCl6Powder, activation
Agent and Al2O3Powder.Matrix and embedding penetration enhancer are in 240-280 DEG C of generation diffusion reaction, so that tungsten functional coating be made.Matrix and tungsten
Functional coating is combined, and has the advantages that functional coating even compact.And coating is obtained without high temperature or the method for pressurization,
The requirement to equipment is reduced, large-scale production is suitble to.Investment can be suitable for complex-shaped matrix prepares coating well.
In this way, complex-shaped matrix prepares coating also can in this way, Yi Shixian continuous production can further save resource
And the energy, reduce cost.Wherein, Al2O3Powder is that one kind prevents bond powders, and powder bonding is in matrix table when preventing diffusion reaction
Face.Select Al2O3Powder is more appropriate, and SiO also can be selected certainly2Etc. preventing bond powders.Preferably, soaking time 2-5h,
In the soaking time in this section, matrix can sufficiently react with embedding penetration enhancer.
The ratio of the activator is 10-15wt.%, and the ratio of the Al2O3 powder is 35-60wt.%.Wherein, the work
Agent includes or mixtures thereof NaF powder, NH4Cl powder.Preferably, embedding penetration enhancer is by WCl6Powder, activator and Al2O3Powder composition, institute
The ratio for stating WCl6 powder in embedding penetration enhancer is 35-45wt.%, and the ratio of the activator is 12-15wt.%, the Al2O3 powder
Ratio be 40-53 wt.%.When WCl6 powder and activator ratio are close to 40:15, WCl6 powder is in preferable activity, favorably
It is diffused into matrix in wolfram element, without adding excessive activator, reduces the usage amount of activator, reduces cost.When
When WCl6 powder and Al2O3 powder ratio are close to 40:50, on matrix surface the phenomenon that few powder bondings, functional coating can guarantee
It is tightly combined between matrix.
The step of polishing treatment by matrix surface includes:
Described matrix is heated to certain temperature by S11, and buffing wax is uniformly applied on matrix；S12 places one
The section time handles matrix using absorbent cotton；And S13, matrix is put into polishing machine and is polished, wherein in polishing process
Use alkalescence polishing liquid, time 5-15min.The defects of butterfly in matrix hole can effectively be repaired using alkalescence polishing liquid.?
After step S13, step S14 is carried out, it is 5- that the matrix after polishing, which is put into dehydrated alcohol, and carries out ultrasonic treatment time
30min。
It will be in the step of being reacted in the matrix embedment embedding penetration enhancer after polishing: matrix and embedding penetration enhancer are placed in Al2O3Tubular type
In furnace, Al2O3Tube furnace has the characteristics that good heat insulating, water absorption rate are extremely low, to guarantee the ambient stable of embedding reaction.It is preferred that
, burying temperature is 260-280 DEG C.Selecting this temperature can make diffusion reaction have faster speed, and can obtain one
A thicker functional coating makes the thickness of coating not less than 3.5mm.
Matrix and the step of vacuum drying after the cleaning embedding include:
S31 is first cleaned up the matrix after the embedding with ultrasonic wave, and ultrasonic treatment time is 5 ~ 20min；And
S32, at a temperature of 90-100 DEG C, vacuum drying.
A kind of tantalum or tantalum alloy composite material obtained using the above method, including matrix and it is coated on the base
The tungsten functional coating in body surface face, described matrix are tantalum or tantalum alloy, and tungstenic amount is 1.5-18 wt.% in the tungsten functional coating.
Functional coating obtained with a thickness of 3-7mm.Tungsten functional coating has excellent machinery, chemistry and electrical property, plating on matrix
After functional coating, tantalum or the poor problem of tantalum alloy corrosion resistance are overcome, tantalum or tantalum alloy in preparation process are also overcomed
Absorb protium become fragile, easy fracture the problem of, effectively extend the service life of matrix.
Embodiment 2:
The specific ratio for embedding penetration enhancer is WCl6: 40wt.%, NaF or NH4Cl:15wt.%, Al2O3: 45wt.%.Embedding is anti-
At once, the temperature of heat preservation is 280 DEG C, soaking time 2h.
Such as Fig. 2 to Fig. 3, in matrix obtained, it is tightly combined between tungsten functional coating and matrix, no hole or crackle go out
It is existing.As shown in figure 3, close to matrix surface side spectrogram 1 in, the weight ratio of tungsten has reached 59.09 wt.%, can
See that the infiltration effect of wolfram element is fine.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent substitution, improvement and etc. done be should be included within the scope of the present invention.
Claims (9)
1. preparing the method for tantalum surface tungsten functional coating under a kind of low temperature, which comprises the following steps:
S1, by matrix surface polishing treatment, described matrix includes tantalum, tantalum alloy or combinations thereof；
S2 will react in the matrix embedment embedding penetration enhancer after polishing, wherein embedding temperature is 240-280 DEG C, soaking time 1-
8h, the embedding penetration enhancer includes evenly dispersed WCl6Powder, activator and Al2O3Powder, and WCl in the embedding penetration enhancer6The ratio of powder
Example is 30-50wt.%；The ratio of the activator is 10-15wt.%, the Al2O3The ratio of powder is 35-60wt.%；
S3, matrix and vacuum drying after heat preservation, after cleaning embedding.
2. preparing the method for tantalum surface tungsten functional coating under low temperature according to claim 1, it is characterised in that: the activation
Agent includes or mixtures thereof NaF powder, NH4Cl powder.
3. preparing the method for tantalum surface tungsten functional coating under low temperature according to claim 1, it is characterised in that: described by base
The step of body surface polishing treatment includes:
Described matrix is heated to certain temperature by S11, and buffing wax is uniformly applied on matrix；
S12 places a period of time, handles matrix using absorbent cotton；And
Matrix is put into polishing machine and polishes by S13, wherein alkalescence polishing liquid, time 5- are used in polishing process
15min。
4. preparing the method for tantalum surface tungsten functional coating under low temperature according to claim 3, it is characterised in that: in step
It further comprise step S14 after S13, it is 5- that the matrix after polishing, which is put into dehydrated alcohol, and carries out ultrasonic treatment time
30min。
5. preparing the method for tantalum surface tungsten functional coating under low temperature according to claim 1, it is characterised in that: the embedding
WCl in penetration enhancer6The ratio of powder is 35-45wt.%, and the ratio of the activator is 12-15wt.%, the Al2O3The ratio of powder
For 40-53wt.%.
6. preparing the method for tantalum surface tungsten functional coating under low temperature according to claim 1, it is characterised in that: the cleaning
The step of matrix after embedding and vacuum drying includes:
S31 is first cleaned up the matrix after the embedding with ultrasonic wave, wherein ultrasonic treatment time is 5~20min；With
And
S32, at a temperature of 90-100 DEG C, vacuum drying.
7. preparing the method for tantalum surface tungsten functional coating under low temperature according to claim 1, it is characterised in that: the embedding
Temperature is 260-280 DEG C.
8. tantalum or tantalum alloy composite material that any one of -7 methods obtain according to claim 1, it is characterised in that: including base
Body and the tungsten functional coating for being coated on described matrix surface, described matrix are tantalum or tantalum alloy, are contained in the tungsten functional coating
Tungsten amount is 1.5-18wt.%.
9. tantalum according to claim 8 or tantalum alloy composite material, it is characterised in that: tungsten functional coating obtained
With a thickness of 3-7mm.
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| CN201610272362.5A CN105714243B (en) | 2016-04-28 | 2016-04-28 | The method of tantalum surface tungsten functional coating is prepared under a kind of low temperature |
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| US3293069A (en) * | 1963-10-04 | 1966-12-20 | United Aircraft Corp | Coatings for columbium base alloys |
| EP0484130A2 (en) * | 1990-10-30 | 1992-05-06 | Kabushiki Kaisha Toshiba | High temperature heat-treating jig |
| CN101597739A (en) * | 2009-06-30 | 2009-12-09 | 北京科技大学 | A kind of borax salt bath tungstenized coating on steel matrix surface preparation method |
-
2016
- 2016-04-28 CN CN201610272362.5A patent/CN105714243B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3293069A (en) * | 1963-10-04 | 1966-12-20 | United Aircraft Corp | Coatings for columbium base alloys |
| EP0484130A2 (en) * | 1990-10-30 | 1992-05-06 | Kabushiki Kaisha Toshiba | High temperature heat-treating jig |
| CN101597739A (en) * | 2009-06-30 | 2009-12-09 | 北京科技大学 | A kind of borax salt bath tungstenized coating on steel matrix surface preparation method |
Non-Patent Citations (1)
| Title |
|---|
| "金属钨涂层制备工艺的研究进展";刘艳红等;《粉末冶金材料科学与工程》;20110615;第16卷(第3期);第315-322页 |
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