CN108285346A - A kind of preparation method for the tungsten nickel material having silicon coating - Google Patents
A kind of preparation method for the tungsten nickel material having silicon coating Download PDFInfo
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- CN108285346A CN108285346A CN201810187228.4A CN201810187228A CN108285346A CN 108285346 A CN108285346 A CN 108285346A CN 201810187228 A CN201810187228 A CN 201810187228A CN 108285346 A CN108285346 A CN 108285346A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
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- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
- C04B35/5626—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on tungsten carbides
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
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Abstract
The invention discloses a kind of preparation methods for the tungsten nickel material having silicon coating, tungsten nickel material prepared by this method solves the problems, such as often occur " nickel pond " and hole in traditional fine grained cemented carbide preparation process, multi-layer film structure can not only hinder the migration of Lacking oxygen, the present invention to carry out PVA/SiO to tungsten nickel material surface2Complex sol surface modification treatment so that the surface even compact of tungsten nickel material, film substrate bond strength height, good mechanical performance.
Description
Technical field
The present invention relates to alloy material manufacturing fields, and in particular to a kind of preparation for the tungsten nickel material having silicon coating
Method.
Background technology
WC-Ni hard alloy has high intensity, high rigidity, excellent abrasion resistance, 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, and plastic deformation is easy to happen 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 binder, 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
Improve the performance of WC-Ni hard alloy with the methods of defect.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..
Silica dioxide gel has heat-insulating property is good, nanostructure is controllable, corrosion resistance and good, biocompatibility are excellent etc.
Feature, but SiO2Gel has that adhesion strength is low if being directly coated on alloy surface, it is therefore desirable to introduce film forming agent
It is modified.Polyvinyl alcohol is a kind of nontoxic, transparent polyhydroxy based high-polymer, when as a kind of organic coupling agent and SiO2It is molten
Glue has good combination effect.On the one hand, SiO can be made2Dissolved adhesiveness increase and it is good with the binding performance of Ti-Ni matrixes,
To effectively improve the bond strength of coating;On the other hand, PVA solvents can also effectively fill SiO2Colloidal sol is forming gel mistake
The hole gap formed in journey, improves the performances such as the consistency, wearability, hardness of coating.
Invention content
The present invention provides a kind of preparation method for the tungsten nickel material having silicon coating, tungsten nickel material prepared by this method
Solve the problems, such as in traditional fine grained cemented carbide preparation process " nickel pond " and hole often occur, multi-layer film structure not only can be with
The migration of Lacking oxygen, the present invention is hindered to carry out PVA/SiO to tungsten nickel material surface2Complex sol surface modification treatment so that tungsten
The surface even compact of nickel material, film substrate bond strength height, good mechanical performance.
To achieve the goals above, the present invention provides a kind of preparation method for the tungsten nickel material having silicon coating,
This method comprises the following steps:
(1)Prepare matrix
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
Ball grinding cylinder wet-milling 12-16 hours is added in chromium, adds nickel powder wet-milling 14-18 hours;
The mixture slurry drying that ball milling is finished;
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)First 8-10 weight account polyethylene alcohol is stirred evenly and is slowly added into 20 DEG C of the pure water of 90-100 parts by weight,
Polyvinyl alcohol solvent is slowly warming up to 80-90 DEG C again after impregnating 15-18h and stirs acceleration dissolving, obtains uniform, water white transparency
Polyvinyl alcohol solvent;
3-5 parts by weight metasilicic acid ethyl esters are sequentially added into polyvinyl alcohol solvent, and a small amount of hydrochloric acid and ethylene glycol is added dropwise, finally
35-45 DEG C of constant temperature stirs 2-4h in constant temperature blender with magnetic force, and polyvinyl alcohol/SiO is obtained after standing 3-5h2Uniform sol body;
(4)It will be totally immersed into polyvinyl alcohol/SiO by pretreated matrix2Uniform sol body simultaneously impregnates 15-20s, then with vertical
Straight pulling machine is lifted with the rate of 3-6mm/min on matrix to liquid level respectively, and dry 25-30min, then exists in air at room temperature
Dry 40 min in drying box, repeat dip-coating, drying 4-6 times;
The sintering processes for carrying out different temperatures under inert gas protection, 680-700 is raised to the heating rate of 5-10 DEG C/min
DEG C, 30-50min postcoolings are sintered, product is obtained.
The present invention has following advantages:
(1)Tungsten nickel material prepared by this method, which solves, often there is " nickel pond " and hole in traditional fine grained cemented carbide preparation process
The problem of, multi-layer film structure can not only hinder the migration of Lacking oxygen;
(2)The present invention carries out PVA/SiO to tungsten nickel material surface2Complex sol surface modification treatment so that the table of tungsten nickel material
Face even compact, film substrate bond strength height, good mechanical performance.
Specific implementation mode
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
Ball grinding cylinder wet-milling 12 hours is added in chromium carbide, adds nickel powder wet-milling 14 hours.
The mixture slurry drying that ball milling is finished.
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 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, and pressure is 2 ×
10-2Pa, substrate temperature are 300 DEG C, and argon gas flux is 10sccm, and bias is -100V, cathode current 29.5A, and cathode voltage is
19V, anode current 7A, anode voltage 80V improve depositing coating to remove adsorbed gas and the impurity of matrix surface
With the bond strength and quality of forming film of matrix.
First 8 weight account polyethylene alcohol are stirred evenly and are slowly added into 20 DEG C of the pure water of 90 parts by weight, 15h is impregnated
Afterwards again by polyvinyl alcohol solvent be slowly warming up to 80 DEG C and stir acceleration dissolving, obtain uniformly, the polyvinyl alcohol of water white transparency it is molten
Agent;3 parts by weight metasilicic acid ethyl esters are sequentially added into polyvinyl alcohol solvent, and a small amount of hydrochloric acid and ethylene glycol is added dropwise, finally in perseverance
35 DEG C of constant temperature stir 2h in warm magnetic stirring apparatus, and polyvinyl alcohol/SiO is obtained after standing 3h2Uniform sol body.
It will be totally immersed into polyvinyl alcohol/SiO by pretreated matrix2Uniform sol body simultaneously impregnates 15s, then with vertically
Pulling machine is lifted with the rate of 3mm/min on matrix to liquid level respectively, dry 25min in air at room temperature, then in drying box
40 min of middle drying repeats dip-coating, drying 4 times;Under inert gas protection carry out different temperatures sintering processes, with 5 DEG C/
The heating rate of min is raised to 680-700 DEG C, is sintered 30min postcoolings, obtains product.
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
Ball grinding cylinder wet-milling 16 hours is added in chromium carbide, adds nickel powder wet-milling 18 hours.
The mixture slurry drying that ball milling is finished.
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, and pressure is 2 ×
10-2Pa, substrate temperature are 300 DEG C, and argon gas flux is 10sccm, and bias is -100V, cathode current 29.5A, and cathode voltage is
19V, anode current 7A, anode voltage 80V improve depositing coating to remove adsorbed gas and the impurity of matrix surface
With the bond strength and quality of forming film of matrix.
First 10 weight account polyethylene alcohol are stirred evenly and are slowly added into 20 DEG C of the pure water of 100 parts by weight, are impregnated
Polyvinyl alcohol solvent is slowly warming up to 90 DEG C again after 18h and stirs acceleration dissolving, obtains uniform, water white transparency polyvinyl alcohol
Solvent;5 parts by weight metasilicic acid ethyl esters are sequentially added into polyvinyl alcohol solvent, and a small amount of hydrochloric acid and ethylene glycol is added dropwise, and are finally existed
45 DEG C of constant temperature stir 4h in constant temperature blender with magnetic force, and polyvinyl alcohol/SiO is obtained after standing 5h2Uniform sol body.
It will be totally immersed into polyvinyl alcohol/SiO by pretreated matrix2Uniform sol body simultaneously impregnates 20s, then with vertically
Pulling machine is lifted with the rate of 6mm/min on matrix to liquid level respectively, dry 30min in air at room temperature, then in drying box
40 min of middle drying repeats dip-coating, drying 6 times;Under inert gas protection carry out different temperatures sintering processes, with 10 DEG C/
The heating rate of min is raised to 700 DEG C, is sintered 50min postcoolings, obtains product.
Claims (1)
1. a kind of preparation method for the tungsten nickel material having silicon coating, this method comprises the following steps:
(1)Prepare matrix
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
Ball grinding cylinder wet-milling 12-16 hours is added in chromium, adds nickel powder wet-milling 14-18 hours;
The mixture slurry drying that ball milling is finished;
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)First 8-10 weight account polyethylene alcohol is stirred evenly and is slowly added into 20 DEG C of the pure water of 90-100 parts by weight,
Polyvinyl alcohol solvent is slowly warming up to 80-90 DEG C again after impregnating 15-18h and stirs acceleration dissolving, obtains uniform, water white transparency
Polyvinyl alcohol solvent;
3-5 parts by weight metasilicic acid ethyl esters are sequentially added into polyvinyl alcohol solvent, and a small amount of hydrochloric acid and ethylene glycol is added dropwise, finally
35-45 DEG C of constant temperature stirs 2-4h in constant temperature blender with magnetic force, and polyvinyl alcohol/SiO is obtained after standing 3-5h2Uniform sol body;
(4)It will be totally immersed into polyvinyl alcohol/SiO by pretreated base material2Uniform sol body simultaneously impregnates 15-20s, then with vertical
Straight pulling machine is lifted with the rate of 3-6mm/min on base material to liquid level respectively, and dry 25-30min, then exists in air at room temperature
Dry 40 min in drying box, repeat dip-coating, drying 4-6 times;
The sintering processes for carrying out different temperatures under inert gas protection, 680-700 is raised to the heating rate of 5-10 DEG C/min
DEG C, 30-50min postcoolings are sintered, product is obtained.
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Citations (8)
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CN1559988A (en) * | 2004-02-19 | 2005-01-05 | 西安交通大学 | Process for preparing porous silicon dioxide thin flm by polyvinyl alcohol as molding board |
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CN102557447A (en) * | 2011-11-07 | 2012-07-11 | 中南大学 | Thermal barrier coating on surface of nickel alloy matrix and preparation method of thermal barrier coating |
CN103588469A (en) * | 2013-11-05 | 2014-02-19 | 中国航空工业集团公司北京航空材料研究院 | Method for preparing ceramic-based high temperature abradable seal coating layer based on sol-gel |
CN105695837A (en) * | 2014-11-26 | 2016-06-22 | 自贡硬质合金有限责任公司 | Preparation method of WC-Ni fine grain cemented carbide |
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2018
- 2018-03-07 CN CN201810187228.4A patent/CN108285346A/en active Pending
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CN1559988A (en) * | 2004-02-19 | 2005-01-05 | 西安交通大学 | Process for preparing porous silicon dioxide thin flm by polyvinyl alcohol as molding board |
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CN101481117A (en) * | 2009-01-22 | 2009-07-15 | 上海交通大学 | SiO2 sol gel solution and method for preparing piezoelectric particle surface SiO2 coating |
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CN103588469A (en) * | 2013-11-05 | 2014-02-19 | 中国航空工业集团公司北京航空材料研究院 | Method for preparing ceramic-based high temperature abradable seal coating layer based on sol-gel |
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