CN105861981B - A kind of method that niobium or niobium alloy surface low-temperature prepare tungsten functional coating - Google Patents
A kind of method that niobium or niobium alloy surface low-temperature prepare tungsten functional coating Download PDFInfo
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- CN105861981B CN105861981B CN201610272296.1A CN201610272296A CN105861981B CN 105861981 B CN105861981 B CN 105861981B CN 201610272296 A CN201610272296 A CN 201610272296A CN 105861981 B CN105861981 B CN 105861981B
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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
- C23C10/02—Pretreatment of the material to be coated
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- Engineering & Computer Science (AREA)
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Abstract
A kind of method that niobium or niobium alloy surface low-temperature prepare tungsten functional coating, comprising the following steps: S1, by matrix surface polishing treatment, described matrix includes niobium, niobium alloy or combinations thereof；S2 will react in the matrix embedment embedding penetration enhancer after polishing, wherein embedding temperature is 200-300 DEG C, soaking time 1-10h, the embedding penetration enhancer includes evenly dispersed WCl6Powder, activator and Al2O3Powder, and WCl in the embedding penetration enhancer6The ratio of powder is 25-55wt.%；S3, matrix and vacuum drying after heat preservation, after cleaning embedding.The present invention uses investment, and matrix is put into WCl6Embedding penetration enhancer in, matrix and embedding penetration enhancer obtain coating without high temperature or the method for pressurization, reduce the requirement to equipment in 200 DEG C of -300 DEG C of generations diffusion reactions, suitable large-scale production.
Description
Technical field
The present invention relates to the technical fields of prepares coating more particularly to a kind of niobium or niobium alloy surface low-temperature to prepare tungsten function
The method of coating.
Background technique
When aerospace, nuclear industry and gas turbine work, blade must bear 1000 DEG C~1200 DEG C of high temperature.It is Ni-based
High temperature is limited (about 1400 DEG C) by itself fusing point, and the service temperature upper limit is only 1100 DEG C, therefore develops higher use
The high-temperature structural material of temperature is imperative.Niobium belongs to VB race refractory metal, is bcc structure, with high-melting-point (2468
DEG C), high-intensitive, good ductility and thermal conductivity, the crisp transition temperature of modeling-low (- 160 DEG C), medium density (8.6 g/cm3)
The characteristics of, since niobium and its alloy have good physics and chemical characteristic, it is expected to replace nickel-base alloy in 21 beginnings of the century
As aerospace structure part material.
But just metal niobium only has stable chemical property under certain conditions, in order to make it have better stabilization
Property, corrosion resistance, need to carry out niobium and niobium alloy surface protective treatment, thus play protection, it is wear-resisting, strengthen, reparation etc.
Reason.At present commonly by adding the alloying elements such as Al, Ti into metal niobium, to improve the anti-oxidant corruption of niobium alloy itself
Erosion ability, or apply protective coating on the surface thereof.The method of alloying is limited by alloying element additive amount, when addition member
When element is more than critical quantity, the mechanical property of alloy can be significantly reduced.And if addition element amount is insufficient, it does not have to niobium matrix
Protective action.Surface covering protection is to take into account niobium alloy mechanical behavior under high temperature and the effective approach of antioxygenic property.With
The heat-resisting alloy and noble metal that iron, nickel and chromium are matrix are often by as alloy coat, but heat-resisting alloy coating and niobium alloy
The binding force of substrate is poor, relatively low using temperature, and high temperature easily corrodes peeling under washing away, and coated porous mentions for oxygen atom
A large amount of diffusion admittances are supplied, the counterdiffusion between protective layer when used for a long time and substrate niobium alloy forms brittlement phase, leads to niobium
Alloy substrate failure, and there are techniques cumbersome, at high cost problem.
Summary of the invention
The purpose of the present invention is to overcome the shortcomings of the existing technology, provides a kind of niobium using investment or niobium alloy surface
The method of low temperature preparation tungsten functional coating.
In order to solve the above technical problems, present invention employs following technical measures:
A kind of method that niobium or niobium alloy surface low-temperature prepare tungsten functional coating, comprising the following steps:
S1, by matrix surface polishing treatment, described matrix includes niobium, niobium alloy or combinations thereof；
S2 will react in the matrix embedment embedding penetration enhancer after polishing, wherein embedding temperature is 200-300 DEG C, soaking time
For 1-10h, the embedding penetration enhancer includes evenly dispersed WCl6Powder, activator and Al2O3Powder, and WCl in the embedding penetration enhancer6
The ratio of powder is 25-55wt.%；
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 30-65
wt.%.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 located on polishing disk by S11, the polishing disk be equipped with polishing pad, the polishing pad with a thickness of
3-3.5mm；
S12, adds lapping liquid between described matrix and the polishing disk, and the lapping liquid uses abrasive grain for W0.5
Diamond grinding fluid, lapping liquid pH value is about 10；And
S13, the polishing disk rotation polish described matrix, wherein time 8-20min.
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 10-15wt.%, and the ratio of the Al2O3 powder is 50-65 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, wherein ultrasonic treatment time be 5 ~
30min and S32, at a temperature of 80-90 DEG C, vacuum drying.
As a further improvement, the embedding temperature is 250-300 DEG C.
A kind of niobium or niobium alloy composite material are made according to above-mentioned method, including matrix and are coated on described
The tungsten functional coating of matrix surface, described matrix are niobium or niobium alloy, and tungstenic amount is 2-20 wt.% in the tungsten functional coating,
Surplus is niobium or niobium alloy.
As a further improvement, tungsten functional coating obtained with a thickness of 2-20mm.
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 200 DEG C of -300 DEG C of generation diffusion reactions, so that tungsten functional coating be made.Matrix
It is combined with tungsten functional coating, has the advantages that tungsten functional coating even compact.And it is obtained without high temperature or the method for pressurization
Coating is obtained, the requirement to equipment is reduced, is suitble to large-scale production.
2, pre-treatment is done to matrix using diamond grinding fluid, can be suitably used for complex-shaped matrix.And investment also can
It is suitable for complex-shaped matrix prepares coating well.In this way, complex-shaped matrix prepares coating can also use this side
Method, 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 niobium as made from investment or niobium alloy composite material have tungsten functional coating, and tungsten functional coating
Middle tungstenic amount is 2-20 wt.%, tungsten functional coating with a thickness of 2-20mm, tungsten functional coating have excellent machinery, chemistry and
Electrical property has the advantages that wear-resisting, anti-corrosion and heat shielding, effectively extends the use of matrix on matrix after plating functional coating
Service life.
Detailed description of the invention
Attached drawing 1 is the flow diagram for the method that niobium or niobium alloy surface low-temperature of the present invention prepares tungsten functional coating；
Attached drawing 2 is that the Nb-W that niobium or niobium alloy surface low-temperature of the present invention is prepared in the embodiment of the method 2 of tungsten functional coating is applied
Layer cross section figure；
Attached drawing 3 is the Nb-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 that niobium or niobium alloy surface low-temperature prepare tungsten functional coating, comprising the following steps:
S1, by matrix surface polishing treatment, described matrix includes niobium, niobium alloy or combinations thereof；
S2 will react in the matrix embedment embedding penetration enhancer after polishing, wherein embedding temperature is 200-300 DEG C, soaking time
For 1-10h, the embedding penetration enhancer includes evenly dispersed WCl6Powder, activator and Al2O3Powder, and WCl in the embedding penetration enhancer6
The ratio of powder is 25-55wt.%；
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 200 DEG C of -300 DEG C of generation diffusion reactions, so that tungsten functional coating be made.Matrix with
Tungsten functional coating is combined, and has the advantages that tungsten functional coating even compact.And it is obtained without high temperature or the method for pressurization
Coating reduces the requirement to equipment, is suitble to large-scale production.Wherein, Al2O3Powder is that one kind prevents bond powders, prevents from spreading
Powder bonding is in matrix surface when reaction.Select Al2O3Powder is more appropriate, and SiO also can be selected certainly2Etc. preventing bond powders.
The ratio of the activator is 10-15wt.%, and the ratio of the Al2O3 powder is 30-65 wt.%.Wherein, activator
It is preferred that or mixtures thereof NaF powder, NH4Cl powder.Preferably, embedding penetration enhancer is by WCl6Powder, activator and Al2O3Powder composition, the packet
The ratio for burying WCl6 powder in penetration enhancer is 35-45wt.%, and the ratio of the activator is 10-15wt.%, the ratio of the Al2O3 powder
Example is 50-65 wt.%.When WCl6 powder and activator ratio are close to 4:1, the acceleration of activator can reach preferable
Effect, therefore the ratio of activator can be controlled in this ratio, without adding excessive activator, reduce activator
Usage amount reduces cost.When WCl6 powder and Al2O3 powder ratio are close to 4:6, few powder bondings shows on matrix surface
As can guarantee and be tightly combined between tungsten functional coating and matrix.
The step of polishing treatment by matrix surface includes:
Described matrix is located on polishing disk by S11, the polishing disk be equipped with polishing pad, the polishing pad with a thickness of
3-3.5mm；S12, adds lapping liquid between described matrix and the polishing disk, and the lapping liquid uses abrasive grain for W0.5
Diamond grinding fluid, lapping liquid pH value is about 10；S13, the polishing disk rotation polish described matrix, wherein when
Between be 8-20min；And S14, it is 5-30min that the matrix after polishing, which is put into dehydrated alcohol, and carries out ultrasonic treatment time.
Pre-treatment is done to matrix using diamond grinding fluid, can be suitably used for complex-shaped matrix.And investment also can be very
Good is suitable for complex-shaped matrix prepares coating.In this way, complex-shaped matrix prepares coating also can in this way,
It easily realizes continuous production, resource and the energy can be further saved, reduce cost.
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 250-300 DEG C.Selecting this temperature can make diffusion reaction have faster speed, and can obtain one
A thicker tungsten functional coating makes the thickness of coating not less than 2mm.
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, wherein ultrasonic treatment time be 5 ~
30min.And S32, at a temperature of 80-90 DEG C, vacuum drying.
A kind of niobium or niobium alloy composite material are made according to above-mentioned method, including matrix and are coated on described
The functional coating of matrix surface, described matrix are niobium or niobium alloy, and tungstenic amount is 2-20 wt.% in the tungsten functional coating, remaining
Amount is niobium or niobium alloy.Tungsten functional coating obtained with a thickness of 2-20mm.Functional coating has excellent machinery, chemistry and electricity
Performance has the advantages that wear-resisting, anti-corrosion and heat shielding on matrix after plating functional coating, and effectively extend matrix uses the longevity
Life.
Embodiment 2:
The specific ratio for embedding penetration enhancer is WCl6: 40wt.%, NaF or NH4Cl:10wt.%, Al2O3: 60wt.%.Embedding is anti-
At once, the temperature of heat preservation is 300 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 A in, the weight ratio of tungsten has reached 69.12wt.%, 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. a kind of method that niobium or niobium alloy surface low-temperature prepare tungsten functional coating, which comprises the following steps:
S1, by matrix surface polishing treatment, described matrix includes niobium, niobium alloy or combinations thereof；
S2 will react in the matrix embedment embedding penetration enhancer after polishing, wherein embedding temperature is 200-300 DEG C, soaking time 1-
10h, the embedding penetration enhancer includes evenly dispersed WCl6Powder, activator and Al2O3Powder, and WCl in the embedding penetration enhancer6Powder
Ratio is 25-55wt.%, and the ratio of the activator is 10-15wt.%, the Al2O3The ratio of powder is 30-65wt.%；
S3, matrix and vacuum drying after heat preservation, after cleaning embedding.
2. the method that niobium according to claim 1 or niobium alloy surface low-temperature prepare tungsten functional coating, it is characterised in that: institute
Stating activator includes NaF powder, NH4Or mixtures thereof Cl powder.
3. the method that niobium according to claim 1 or niobium alloy surface low-temperature prepare tungsten functional coating, it is characterised in that: institute
It states and includes: by the step of matrix surface polishing treatment
Described matrix is located on polishing disk by S11, the polishing disk be equipped with polishing pad, the polishing pad with a thickness of 3-
3.5mm；
S12, adds lapping liquid between described matrix and the polishing disk, and the lapping liquid uses abrasive grain for the gold of W0.5
Hard rock lapping liquid, lapping liquid pH value are about 10；And
S13, the polishing disk rotation polish described matrix, wherein time 8-20min.
4. the method that niobium according to claim 3 or niobium alloy surface low-temperature prepare tungsten functional coating, it is characterised in that:
After step S13, further comprises step S14, the matrix after polishing is put into dehydrated alcohol and carries out ultrasonic treatment time
For 5-30min.
5. the method that niobium according to claim 1 or niobium alloy surface low-temperature prepare tungsten functional coating, it is characterised in that: institute
State WCl in embedding penetration enhancer6The ratio of powder is 35-45wt.%, and the ratio of the activator is 10-15wt.%, the Al2O3Powder
Ratio be 50-65wt.%.
6. the method that niobium according to claim 1 or niobium alloy surface low-temperature prepare tungsten functional coating, it is characterised in that: institute
Matrix and the step of vacuum drying after stating cleaning embedding include:
S31 is first cleaned up the matrix after the embedding with ultrasonic wave, wherein and ultrasonic treatment time is 5~30min, with
And
S32, at a temperature of 80-90 DEG C, vacuum drying.
7. the method that niobium according to claim 1 or niobium alloy surface low-temperature prepare tungsten functional coating, it is characterised in that: institute
Stating embedding temperature is 250-300 DEG C.
8. niobium or niobium 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 niobium or niobium alloy, are contained in the tungsten functional coating
Tungsten amount is 2-20wt.%, and surplus is niobium or niobium alloy.
9. niobium according to claim 8 or niobium alloy composite material, it is characterised in that: tungsten functional coating obtained
With a thickness of 2-20mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610272296.1A CN105861981B (en) | 2016-04-28 | 2016-04-28 | A kind of method that niobium or niobium alloy surface low-temperature prepare tungsten functional coating |
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| CN201610272296.1A CN105861981B (en) | 2016-04-28 | 2016-04-28 | A kind of method that niobium or niobium alloy surface low-temperature prepare tungsten functional coating |
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Citations (4)
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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 |
| 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 |
-
2016
- 2016-04-28 CN CN201610272296.1A patent/CN105861981B/en active Active
Patent Citations (4)
| 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 |
| 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 |
Non-Patent Citations (3)
| Title |
|---|
| "Coatings of Nb-base alloy by Cr and/or Al pack cementations and its oxidation behavior in air at 1273-1473K";Michihisa Fukumoto et al.;《Materials Transactions》;20030224;第44卷(第4期);第731-735页 |
| "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 |
| "铌基合金包埋渗法制备抗氧化硅涂层及其组织形成";赵陆翔等;《中国有色金属学报》;20070415;第17卷(第4期);第596-601页 |
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