CN108239716A - A kind of preparation method for having nitrogen-yttrium-zirconium hard coat tungsten nickel - Google Patents
A kind of preparation method for having nitrogen-yttrium-zirconium hard coat tungsten nickel Download PDFInfo
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- CN108239716A CN108239716A CN201611212383.4A CN201611212383A CN108239716A CN 108239716 A CN108239716 A CN 108239716A CN 201611212383 A CN201611212383 A CN 201611212383A CN 108239716 A CN108239716 A CN 108239716A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3464—Sputtering using more than one target
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2204/00—End product comprising different layers, coatings or parts of cermet
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Abstract
The invention discloses a kind of preparation methods for having nitrogen-yttrium-zirconium hard coat tungsten nickel, tungsten nickel prepared by this method, solve the problems, such as often occur " nickel pond " and hole in traditional fine grained cemented carbide preparation process, to improve the comprehensive performance of alloy, using direct current and rf reactive co-sputtering method, by the way that Y target power outputs is controlled to prepare high rigidity nitrogen-yttrium-zirconium coating in cemented carbide substrate surfaces under the conditions of certain deposition pressure, temperature, nitrogen partial pressure etc..
Description
Technical field
The present invention relates to alloy material manufacturing fields, and in particular to a kind of system for having nitrogen-yttrium-zirconium hard coat tungsten nickel
Preparation Method.
Background technology
Hard alloy has the spies such as high intensity, high rigidity, excellent wearability, heat resistance and good corrosion resistance
Point, therefore it is widely used in the working environments such as high pressure, high rotating speed, high temperature, Korrosionsmedium
WC-Ni hard alloy has high intensity, high rigidity, excellent wearability, heat resistance and good corrosion resistance
The features such as, therefore it is widely used in the working environments such as high pressure, high rotating speed, high temperature, Korrosionsmedium.Since Ni belongs to face-centered cubic
(F.c.c) crystallographic system, plasticity is fine, is easily plastically deformed during wet-milling, forms the Ni powder balls of sheet.Industrial production with
Ni will be grown as the Ball-milling Time of the hard alloy of binding agent, even in this way, cannot guarantee that the uniform refinement of Ni powder, this is
Based on Ni powder, there is the Refining Mechanisms completely different with Co powder.
Mainly WC grain is refined, by stringent technology controlling and process, reduces hole by adding alloying element in the prior art
And the methods of defect, improves the performance of WC-Ni hard alloy.The WC-Ni mixtures prepared using conventional method are in vacuum-sintering
Under the conditions of often there is " nickel pond " and hole." nickel pond " and hole can seriously affect the comprehensive performance of alloy, such as intensity, wear-resisting
Property, corrosion resistance etc..
By selecting suitable coating material and coating production, can improve hard alloy hardness, it is wear-resisting with
And high temperature oxidation resistance, so as to improve the service life of hard alloy.In these coated carbides, the nitrogen of transition element
Compound coating is since it is with high hardness, excellent wear and corrosion behavior and chemical stability, past 20
It several years, is widely used in a variety of applications.
Invention content
The present invention provides a kind of preparation method for having nitrogen-yttrium-zirconium hard coat tungsten nickel, and tungsten nickel prepared by this method closes
Gold solves the problems, such as often occur " nickel pond " and hole in traditional fine grained cemented carbide preparation process, to improve the synthesis of alloy
Performance, using direct current and rf reactive co-sputtering method, by controlling Y under the conditions of certain deposition pressure, temperature, nitrogen partial pressure etc.
Target power output prepares high rigidity nitrogen-yttrium-zirconium coating in matrix surface.
To achieve these goals, the present invention provides a kind of preparation sides for having nitrogen-yttrium-zirconium hard coat tungsten nickel
Method, this method comprises the following steps：
(1) matrix is prepared
Mixed powder is prepared by following composition by weight
Tungsten carbide, 90.1%-92.8%, 0.8-1 μm of Fisher particle size；
Nickel powder, 5%-6%, 0.5-1.0 μm of Fisher particle size；
Chromium carbide, surplus；
The mixed powder of said ratio is subjected to wet-milling；Wherein Ball-milling Time Discrete control；First by carbide powder and additive
Chromium carbide adds in ball grinding cylinder wet-milling 12-16 hours, adds nickel powder wet-milling 14-18 hours；
The mixture slurry that ball milling is finished is dried；
Dry pack is pressed into the compacting product of required shape；
Compacting product are placed on high temperature sintering in sintering furnace, sintering temperature is 1450-1470 DEG C, soaking time 70-90min,
Sintering pressure is 4.5-5.0Mpa, obtains tungsten nickel matrix；
(2) substrate pretreated
Described matrix pre-processes, and can be ground polishing, ultrasonic cleaning and ion source cleaning successively；
(3) pre-sputtering
The condition of the pre-sputtering is, substrate temperature is 300 DEG C, is passed through argon gas, adjust in sputter chamber operating pressure to
The Dc source power of 1Pa, Zr target is 200W, and the radio-frequency power supply power of Y targets is 100W, and the pre-sputtering time is 10min, with
Nitride, oxide of target material surface etc. is removed, improves the sputter rate of target；The argon gas and nitrogen gas purity can be
The purity of 99.99%, Zr target can be that the purity of 99.995%, Y targets can be 99.9%；
(4) sputtering sedimentation
The condition of the sputtering sedimentation is, after pre-sputtering, is passed through argon gas and nitrogen, total flux 60sccm,
Middle nitrogen flow is 10%-15%, and the operating pressure of deposition is 0.2-0.3Pa, and the Dc source power of Zr targets is 250W, Y
The radio-frequency power supply power of target is 100-150W, and two target surfaces are in 90 °, common aura regional alignment hard alloy substrate, sputtering
Time is 90min, and substrate temperature is 300 DEG C；The argon gas and nitrogen gas purity can be that the purity of 99.99%, Zr targets can be
The purity of 99.995%, Y target can be 99.9%.
Preferably, in the step (2), the grinding and polishing can be first on the boart boart wheel disc of 600 mesh by matrix
Corase grinding 10min is carried out, fine grinding 10min, then the diamond polishing with W2.5 are then carried out on the boart boart wheel disc of 1200 mesh
Powder is polished, the ultrasonic cleaning uniformly bright to specimen surface, can clean the matrix after grinding and polishing in the following order,
Acetone is cleaned by ultrasonic 5min → absolute ethyl alcohol for use, the ion source cleaning that is cleaned by ultrasonic 5min → drying, can be used Hall from
Component carries out matrix cleaning 5min, and pressure is 2 × 10-2Pa, substrate temperature are 300 DEG C, and argon gas flux is 10sccm, is biased
For -100V, cathode current 29.5A, cathode voltage 19V, anode current 7A, anode voltage 80V, to remove matrix table
The adsorbed gas in face and impurity improve depositing coating and the bond strength and quality of forming film of matrix.
According to tungsten nickel prepared by the above method, the purpose for significantly improving and controlling materials microstructure structure is can reach,
The tungsten nickel strength of materials prepared and hardness is enabled to reach perfect matching, high comprehensive performance.
Specific embodiment
Embodiment one
Mixed powder is prepared by following composition by weight：
Tungsten carbide, 90.1%, 0.8-1 μm of Fisher particle size；
Nickel powder, 5%, 0.5-1.0 μm of Fisher particle size；
Chromium carbide, surplus.
The mixed powder of said ratio is subjected to wet-milling；Wherein Ball-milling Time Discrete control；First by carbide powder and additive
Chromium carbide adds in ball grinding cylinder wet-milling 12 hours, adds nickel powder wet-milling 14 hours.
The mixture slurry that ball milling is finished is dried.
Dry pack is pressed into the compacting product of required shape.
Compacting product are placed on high temperature sintering in sintering furnace, sintering temperature is 1450 DEG C, soaking time 70-90min, sintering pressure
Power is 4.5Mpa, obtains tungsten nickel matrix.
Substrate pretreated, described matrix pretreatment can be ground polishing, ultrasonic cleaning and ion source cleaning successively.Institute
Grinding and polishing is stated, can matrix be first subjected to corase grinding 10min on the boart boart wheel disc of 600 mesh, then in the Buddha's warrior attendant of 1200 mesh
Fine grinding 10min is carried out on stone sand wheel disc, then be polished with the diamond polishing powder of W2.5 it is uniformly bright to specimen surface, it is described
It is cleaned by ultrasonic, the matrix after grinding and polishing can be cleaned in the following order, it is clear that acetone is cleaned by ultrasonic 5min → absolute ethyl alcohol ultrasound
It is for use to wash 5min → drying, ion source cleaning can be used hall ion source and carry out cleaning 5min to matrix, pressure for 2 ×
10-2Pa, substrate temperature are 300 DEG C, and argon gas flux is 10sccm, is biased as -100V, cathode current 29.5A, and cathode voltage is
19V, anode current 7A, anode voltage 80V to remove the adsorbed gas of matrix surface and impurity, improve depositing coating
With the bond strength and quality of forming film of matrix.
Pre-sputtering, the condition of the pre-sputtering are that substrate temperature is 300 DEG C, are passed through argon gas, adjust in sputter chamber and work
Pressure is to 1Pa, and the Dc source power of Zr targets is 200W, and the radio-frequency power supply power of Y targets is 100W, and the pre-sputtering time is
10min to remove the nitride of target material surface, oxide etc., improves the sputter rate of target；The argon gas and nitrogen gas purity can
Purity for 99.99%, Zr targets can be that the purity of 99.995%, Y targets can be 99.9%.
Sputtering sedimentation, the condition of the sputtering sedimentation is, after pre-sputtering, is passed through argon gas and nitrogen, total flux is
60sccm, wherein nitrogen flow are 10%, and the operating pressure of deposition is 0.2Pa, and the Dc source power of Zr targets is 250W, Y
The radio-frequency power supply power of target is 100W, and two target surfaces are in 90 °, common aura regional alignment hard alloy substrate, sputtering time
For 90min, substrate temperature is 300 DEG C；The argon gas and nitrogen gas purity can be that the purity of 99.99%, Zr targets can be
The purity of 99.995%, Y target can be 99.9%.
Embodiment two
Mixed powder is prepared by following composition by weight：
Tungsten carbide, 92.8%, 0.8-1 μm of Fisher particle size；
Nickel powder, 6%, 0.5-1.0 μm of Fisher particle size；
Chromium carbide, surplus.
The mixed powder of said ratio is subjected to wet-milling；Wherein Ball-milling Time Discrete control；First by carbide powder and additive
Chromium carbide adds in ball grinding cylinder wet-milling 16 hours, adds nickel powder wet-milling 18 hours.
The mixture slurry that ball milling is finished is dried.
Dry pack is pressed into the compacting product of required shape.
Compacting product are placed on high temperature sintering in sintering furnace, sintering temperature is 1470 DEG C, soaking time 90min, sintering pressure
For 5.0Mpa, tungsten nickel matrix is obtained.
Substrate pretreated, described matrix pretreatment can be ground polishing, ultrasonic cleaning and ion source cleaning successively.Institute
Grinding and polishing is stated, can matrix be first subjected to corase grinding 10min on the boart boart wheel disc of 600 mesh, then in the Buddha's warrior attendant of 1200 mesh
Fine grinding 10min is carried out on stone sand wheel disc, then be polished with the diamond polishing powder of W2.5 it is uniformly bright to specimen surface, it is described
It is cleaned by ultrasonic, the matrix after grinding and polishing can be cleaned in the following order, it is clear that acetone is cleaned by ultrasonic 5min → absolute ethyl alcohol ultrasound
It is for use to wash 5min → drying, ion source cleaning can be used hall ion source and carry out cleaning 5min to matrix, pressure for 2 ×
10-2Pa, substrate temperature are 300 DEG C, and argon gas flux is 10sccm, is biased as -100V, cathode current 29.5A, and cathode voltage is
19V, anode current 7A, anode voltage 80V to remove the adsorbed gas of matrix surface and impurity, improve depositing coating
With the bond strength and quality of forming film of matrix.
Pre-sputtering, the condition of the pre-sputtering are that substrate temperature is 300 DEG C, are passed through argon gas, adjust in sputter chamber and work
Pressure is to 1Pa, and the Dc source power of Zr targets is 200W, and the radio-frequency power supply power of Y targets is 100W, and the pre-sputtering time is
10min to remove the nitride of target material surface, oxide etc., improves the sputter rate of target；The argon gas and nitrogen gas purity can
Purity for 99.99%, Zr targets can be that the purity of 99.995%, Y targets can be 99.9%.
Sputtering sedimentation, the condition of the sputtering sedimentation is, after pre-sputtering, is passed through argon gas and nitrogen, total flux is
60sccm, wherein nitrogen flow are 15%, and the operating pressure of deposition is 0.3Pa, and the Dc source power of Zr targets is 250W, Y
The radio-frequency power supply power of target is 150W, and two target surfaces are in 90 °, common aura regional alignment hard alloy substrate, sputtering time
For 90min, substrate temperature is 300 DEG C；The argon gas and nitrogen gas purity can be that the purity of 99.99%, Zr targets can be
The purity of 99.995%, Y target can be 99.9%.
Claims (2)
1. a kind of preparation method for having nitrogen-yttrium-zirconium hard coat tungsten nickel, this method comprises the following steps：
(1) matrix is prepared
Mixed powder is prepared by following composition by weight
Tungsten carbide, 90.1%-92.8%, 0.8-1 μm of Fisher particle size；
Nickel powder, 5%-6%, 0.5-1.0 μm of Fisher particle size；
Chromium carbide, surplus；
The mixed powder of said ratio is subjected to wet-milling；Wherein Ball-milling Time Discrete control；First carbide powder and additive are carbonized
Chromium adds in ball grinding cylinder wet-milling 12-16 hours, adds nickel powder wet-milling 14-18 hours；
The mixture slurry that ball milling is finished is dried；
Dry pack is pressed into the compacting product of required shape；
Compacting product are placed on high temperature sintering in sintering furnace, sintering temperature is 1450-1470 DEG C, soaking time 70-90min, sintering
Pressure is 4.5-5.0Mpa, obtains tungsten nickel matrix；
(2) substrate pretreated
Described matrix pre-processes, and can be ground polishing, ultrasonic cleaning and ion source cleaning successively；
(3) pre-sputtering
The condition of the pre-sputtering is, substrate temperature is 300 DEG C, is passed through argon gas, adjusts in sputter chamber operating pressure to 1Pa,
The Dc source power of Zr targets is 200W, and the radio-frequency power supply power of Y targets is 100W, and the pre-sputtering time is 10min, with removal
Nitride, oxide of target material surface etc. improve the sputter rate of target；The argon gas and nitrogen gas purity can be 99.99%, Zr
The purity of target can be that the purity of 99.995%, Y targets can be 99.9%；
(4) sputtering sedimentation
The condition of the sputtering sedimentation is, after pre-sputtering, is passed through argon gas and nitrogen, wherein total flux 60sccm, nitrogen
Throughput is 10%-15%, and the operating pressure of deposition is 0.2-0.3Pa, and the Dc source powers of Zr targets is 250W, Y targets
Radio-frequency power supply power for 100-150W, two target surfaces are in 90 °, common aura regional alignment hard alloy substrate, sputtering time
For 90min, substrate temperature is 300 DEG C；The argon gas and nitrogen gas purity can be that the purity of 99.99%, Zr targets can be
The purity of 99.995%, Y target can be 99.9%.
2. the method as described in claim 1, which is characterized in that in the step (2), the grinding and polishing can be by matrix
Corase grinding 10min first is carried out on the boart boart wheel disc of 600 mesh, then carries out fine grinding on the boart boart wheel disc of 1200 mesh
10min, then, the ultrasonic cleaning uniformly bright to specimen surface is polished with the diamond polishing powder of W2.5, it can will grind
Matrix after polishing cleans in the following order, and acetone ultrasonic cleaning 5min → absolute ethyl alcohol ultrasonic cleaning 5min → drying is for use,
The ion source cleaning can be used hall ion source and cleaning 5min carried out to matrix, and pressure is 2 × 10-2Pa, substrate temperature are
300 DEG C, argon gas flux is 10sccm, is biased as -100V, cathode current 29.5A, cathode voltage 19V, and anode current is
7A, anode voltage 80V, to remove the adsorbed gas of matrix surface and impurity, the combination for improving depositing coating and matrix is strong
Degree and quality of forming film.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611212383.4A CN108239716A (en) | 2016-12-25 | 2016-12-25 | A kind of preparation method for having nitrogen-yttrium-zirconium hard coat tungsten nickel |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611212383.4A CN108239716A (en) | 2016-12-25 | 2016-12-25 | A kind of preparation method for having nitrogen-yttrium-zirconium hard coat tungsten nickel |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109630547A (en) * | 2018-12-13 | 2019-04-16 | 武汉东顺汽车配件有限公司 | Automobile antifriction bush and its preparation process |
| CN115161608A (en) * | 2022-07-06 | 2022-10-11 | 烟台大学 | Preparation method of ZrYAgN nano solid solution film with high hydrophobicity and self-lubrication |
-
2016
- 2016-12-25 CN CN201611212383.4A patent/CN108239716A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109630547A (en) * | 2018-12-13 | 2019-04-16 | 武汉东顺汽车配件有限公司 | Automobile antifriction bush and its preparation process |
| CN115161608A (en) * | 2022-07-06 | 2022-10-11 | 烟台大学 | Preparation method of ZrYAgN nano solid solution film with high hydrophobicity and self-lubrication |
| CN115161608B (en) * | 2022-07-06 | 2023-10-27 | 烟台大学 | Preparation method of ZrYAgN nano solid solution film with high hydrophobicity and self-lubrication |
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Application publication date: 20180703 |