CN107082639A - High-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof - Google Patents

High-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof Download PDF

Info

Publication number
CN107082639A
CN107082639A CN201710268531.2A CN201710268531A CN107082639A CN 107082639 A CN107082639 A CN 107082639A CN 201710268531 A CN201710268531 A CN 201710268531A CN 107082639 A CN107082639 A CN 107082639A
Authority
CN
China
Prior art keywords
zirconium oxide
tungsten disulfide
composite self
purity
disulfide composite
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710268531.2A
Other languages
Chinese (zh)
Inventor
不公告发明人
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing Jinli New Material Co.,Ltd.
Original Assignee
Nanjing Cloud Qijin Rui New Material Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing Cloud Qijin Rui New Material Co Ltd filed Critical Nanjing Cloud Qijin Rui New Material Co Ltd
Priority to CN201710268531.2A priority Critical patent/CN107082639A/en
Publication of CN107082639A publication Critical patent/CN107082639A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/486Fine ceramics
    • C04B35/488Composites
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/62695Granulation or pelletising
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225Yttrium oxide or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/446Sulfides, tellurides or selenides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567Treatment time
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/77Density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention provides a kind of brand-new high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof.The present invention is mixed and mechanical alloying with nanoscale curing tungsten powder using nanoscale yttrium stable zirconium oxide powder with the method for high-energy ball milling to powder, and add dispersant, binding agent and deionized water ball milling turn into slurry, then granulated by the method for centrifugal spray granulation, it is compressing by isostatic cool pressing, it is made finally by the method for HIP sintering, the present invention has the advantages that high compact high-strength degree lubricity is good, not only technique and equipment are simple by the present invention, cost is low, high income, energy consumption is low, production efficiency is high, it is adapted to industrialized production, and result in steady quality, coefficient of friction is small, the tiny controllable zirconium oxide tungsten disulfide composite self-lubricating ceramics of crystal grain, process of the present invention is without Environment pollution, it is a kind of new low cost, the preparation method of the high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics of steady quality.

Description

High-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof
Technical field
The invention belongs to material preparation process technical field, and in particular to a kind of high-purity high-strength high-ductility zirconium oxide tungsten disulfide Composite self-lubricating ceramics and preparation method thereof.
Background technology
The research tendency of self-lubricating technology with the development of science and technology, non-environmental-pollution, friction durability length, low friction, The solid lubricant of selfreparing the high-tech areas such as electronics, biology, communication, space flight and aviation apply it is more and more extensive. Solid self lubricant material enjoys common people to pay close attention to as the most promising developing direction of lubricating area, and following research is mainly concentrated The studying of theoretical research, novel solid self-lubricating material in self-lubricating material, the studying of new self-lubricating mode, new material Expect several aspects such as structure design.Ceramics have very excellent mechanical property at high temperature, are especially suitable for applying at high temperature. In numerous structural ceramics, zirconia ceramics with transformation toughening effect because causing increasing concern, with extensive Application prospect.ZrO2Ceramics belong to new ceramics, with very excellent physics, chemical property, not only in scientific research field Through as focus, and also it is widely applied in the industrial production, is refractory material, high-temperature structural material and electronic material Important source material.Moreover, ZrO2High high-temp stability, heat-proof quality preferably, optimum does ceramic coating and high-temperature wearable material Material.But the too high shortcoming of friction factor, the application of zirconia ceramics is seriously limited, is studied with zirconia ceramics material Deepen continuously, self-lubricating material research seems necessary.Using zirconium oxide as wear-resistant matrix, compound kollag to prepare certainly Lubrication composite ceramics is considered as a kind of material under high temperature that solves and lubricates important approach, although at present both at home and abroad to zirconia ceramics The existing Primary Study of material, but early stage is also in the system research of its self-lubrication ceramic, and with modern science and skill The development of art, in view of the more extensive high-temperature self-lubrication of temperature applicability is researched and developed in an urgent demand of the field such as aerospace, the energy and machinery Material.
Chinese patent 200710077310.3 provides a kind of Zirconia ceramics with graphite lubrication powder, the ceramic surface Graphite concentration is higher than inside.A kind of sliding bearing of Zirconia ceramics with graphite lubrication powder is provided simultaneously, and the bearing includes axle There is the endoporus that a support shaft core is rotated at core and axle sleeve, the axle sleeve center.One kind is also provided and carries graphite lubrication powder zirconium oxide pottery The manufacture method of porcelain, it comprises the following steps:Sintering obtains common zirconia ceramics, and common zirconia ceramics adsorbs graphite lubrication Agent powder.
Chinese patent 95121439.X provides a kind of zirconium oxide-graphite self-lubricating composite ceramic material.By nanometer ZrO2 (Y2O33%mol)Ceramic powder, by adding a certain amount of graphitic lubricant and sintering aid batch mixing, through pre-molding, compared with low temperature The lower Fast Sintering of degree, can obtain compact zirconia-graphite composite ceramic material that relative density is 97%, obtained composite ceramics Material has higher hardness, and good antifriction and abrasion resistance are shown under water lubrication.
Chinese patent 201410590493.9 provides a kind of self lubricity nozzle ceramics, by the raw material of following parts by weight It is made:Graphite 3-4, fluorographite 1-2, molybdenum disulfide 1-2, glass microballoon 0.3-0.4, fluorite 4-6, potassium nitrate 1-2, sodium fluoride 1-2, superfine zirconia powder 20-24, kaolin 65-70, tetraethyl orthosilicate 3-4, sodium hydroxide 2-3, appropriate deionized water, ethanol In right amount, auxiliary agent 4-6;The ceramic quality of the invention is fine and smooth, and stomata is few, is not pulverized easily;By adding graphite, fluorographite so that Ceramics have self lubricity, can extend nozzle service life;By using the auxiliary agent of the invention, by increasing capacitance it is possible to increase ceramic surface light Slip, wearability and heat resistance.
Chinese patent 201110327284.1 provides a kind of aluminium oxide ceramics self-lubricating composite and preparation method thereof. Material is made up of aluminum oxide, zirconium oxide and compounded lubricant, and top layer is alumina layer, and wall is alumina-silica zirconium layer, material Material is prepared with laying-cold pressing-heat pressing process.Material has excellent mechanics and tribological property, the wide (room temperature of adaptive temperature scope concurrently ~1000 DEG C), it can be used as the lubrication and encapsulant under extreme severe rugged environment (high temperature, burn into special atmosphere etc.).
Chinese patent 201410630575.1 provides a kind of cutting tool self-lubricating abrasion-resistant ceramics, by following parts by weight Raw material be made:Bismuth sulfide 2-3, diethanol amine 2-3, ammonium sulfate 2-3, magnesium chloride 2-3, carbide slurry 2-3, graphene oxide 2-3, KOH0.6-0.8, Emulsifier EL-60 0.2-0.3, magnesia 3-4, titanium boride 36-40, nano tungsten trioxide 4-5, titanium carbide 30-35, beryllium oxide 3-5, silver powder 1-2, appropriate amount of ethanol, appropriate deionized water, polyacrylic acid 1-1.5, polyethylene glycol 1.2-1.6, Wear-resistant auxiliary agent 4-5;The ceramics of the invention add the resistance to elevated temperatures of ceramics by adding nano tungsten trioxide;The ceramics have The features such as having high temperature resistant, large carrying capacity, self-lubricating, thermal shock resistance and high abrasion, it is adaptable to make cutting tool;By making With the wear-resistant auxiliary agent of the invention, by increasing capacitance it is possible to increase ceramic wearability and heat resistance.
Chinese patent 201210242669.2 provides a kind of self-lubricating solid high-temperature wearable powder composition and its compound The preparation method of coating.By mass percentage, the composition of the powder composition includes:Nickel 14%~17.5%, chromium 3%~3.5%, carbon Change the tungsten disulfide 25%~30% of chromium 49%~52.5% and Surface coating nickel-phosphor alloy;Using laser melting and coating technique by the powder Composition is prepared into self-lubricating solid high-temperature wearable composite coating.The invention is with NiCr-Cr3C2Composite powder is metallic matrix, multiple Coating is closed by ceramic wear-resisting phase and Metal toughened phase composition, WS2For solid lubrication phase, and in WS2Powder particle surface is using chemistry The method of plating coats one layer of micron order Ni-P alloy, increases WS2Heat endurance and chemical stability, can effectively suppress WS2Swashing Decomposition and evaporation in light cladding process, increase its compatibility with metallic matrix, and the composite coating has high temperature from profit Sliding wear-resisting characteristic.
Existing composite self-lubricating ceramic technology proportioning is complicated, and technical process is relative complex, use graphite lubrication pattern more, no The production of features part can be used for.
The content of the invention
It is complicated in order to solve prior art proportioning, it is impossible to meet accurate self-lubrication ceramic production purposes, the invention provides A kind of brand-new high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof.The purpose of the present invention exists In overcoming the shortcoming of prior art, there is provided the self-lubrication ceramic preparation side that high-purity yttrium stable zirconium oxide and high-purity tungsten disulfide are combined Method, using nanoscale yttrium stable zirconium oxide powder and nanoscale curing tungsten powder powder mix with the method for high-energy ball milling with Mechanical alloying, is then granulated by the method for centrifugal spray granulation, compressing by isostatic cool pressing, finally by heat The method of isostatic sintering is made, the present invention have the advantages that high compact high-strength degree lubricity is good, the present invention not only technique with set Standby simple, cost is low, and high income, energy consumption is low, and production efficiency is high, is adapted to industrialized production, and result in steady quality, crystalline substance The tiny controllable zirconium oxide tungsten disulfide composite self-lubricating ceramics of grain, process of the present invention is a kind of new low without Environment pollution The preparation method of cost, the high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics of steady quality.
The ceramic relative density of high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating of the present invention is 99% ~ 100%, host element purity is 99.9% ~ 99.999%, and bending strength is 1000 ~ 1600MPa, and coefficient of friction is 0.03 ~ 0.2, crystal grain Size is 0.5 ~ 20 micron, and Vickers hardness is HV1200 ~ 2000.
Preferably, the relative density of described high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics is 99.5%~100%。
Preferably, the host element purity of described high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics is 99.99%~99.999%。
Preferably, the bending strength of described high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics is 1200 ~1600MPa。
Preferably, the coefficient of friction of described high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics is 0.05 ~0.15。
Preferably, the crystallite dimension of described high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics is 1 ~ 5 Micron.
The host element of high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating of the present invention ceramics is zirconium oxide, Three kinds of yittrium oxide and tungsten disulfide, described host element purity are the percentage by weight of three kinds of host element weight and gross weight.
In order to reach above-mentioned use requirement, the technical scheme that the present invention is used is high-purity high-strength high-ductility zirconium oxide tungsten disulfide The preparation method of composite self-lubricating ceramics, methods described is comprised the following steps that.
(1)Nano level yttrium stable zirconium oxide powder and curing tungsten powder are weighed according to a certain percentage, and two kinds of nano powders are put Enter in ball grinder, high-energy ball milling processing is carried out with high energy ball mill.
(2)In step(1)Binding agent, dispersant and deionized water are put into the good mixed powder of middle ball milling, continues ball milling, obtains Obtain mixed powder slurry.
(3)By step(2)Middle acquisition mixed powder slurry is put into progress granulation processing in centrifugal spraying granulator.
(4)By step(3)The pelletizing of middle acquisition is put into progress isostatic cool pressing processing in isostatic cool pressing gum cover.
(5)By step(4)Middle acquisition isostatic cool pressing blank is put into steel capsule, and high temperature insostatic pressing (HIP) jacket is made.
(6)By step(5)The high temperature insostatic pressing (HIP) jacket of middle acquisition carries out degreasing degassing process.
(7)By step(6)Jacket after the degassing of middle acquisition is put into progress HIP sintering processing in hot isostatic press.
(8)By step(7)The ceramic ingot that middle HIP sintering is finished takes out, and removes jacket, produces high-purity high-strength high Tough zirconium oxide tungsten disulfide composite self-lubricating ceramics.
(9)Measuring process(8)The density of middle zirconium oxide tungsten disulfide composite self-lubricating ceramics, purity, coefficient of friction, crystal grain Size, bending strength and hardness.
The present invention is high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof, in order to allow this Invention to above-mentioned steps effectively, it is necessary to refine, and specific thinning parameter is as follows.
Step(1)In, the molar percentage of yittrium oxide is 3 ~ 10% in the yttrium stable zirconium oxide powder of selection.
Step(1)In, the percentage by weight of described yttrium stable zirconium oxide powder is 80% ~ 99.9%, and surplus is tungsten disulfide.
Step(1)In, the primary particle size of described yttrium stable zirconium oxide powder is 1 ~ 100 nanometer.
Step(1)In, the primary particle size of described curing tungsten powder is 1 ~ 100 nanometer.
Step(1)In, the purity of described yttrium stable zirconium oxide powder is 99.9 ~ 99.999%.
Step(1)In, the purity of described curing tungsten powder is 99.9 ~ 99.999%.
Step(1)In, described mixed powder Ball-milling Time is 2 ~ 12 hours.
Preferably, step(1)In, the molar percentage of yittrium oxide is 3 ~ 5% in the yttrium stable zirconium oxide powder of selection..
Preferably, step(1)In, the percentage by weight of the yttrium stable zirconium oxide powder of selection is 90% ~ 99.9%, and surplus is two Tungsten sulfide.
Preferably, step(1)In, the yttrium stable zirconium oxide powder primary particle size of selection is 10 ~ 40 nanometers.
Preferably, step(1)In, the curing tungsten powder primary particle size of selection is 10 ~ 40 nanometers.
Preferably, step(1)In, the Ball-milling Time of described mixed powder is 4 ~ 12 hours.
Step(2)In, the binding agent of selection includes at least one of polyvinyl alcohol, polyvinyl chloride.
Step(2)In, the dispersant of selection is at least one of ethanol, n-butanol, polyethylene glycol.
Step(2)In, described mixed slurry Ball-milling Time is 2 ~ 12 hours.
Preferably, step(2)In, the binding agent of selection is polyvinyl alcohol.
Preferably, step(2)In, the dispersant of selection is polyethylene glycol.
Step(3)In, described pelletizing particle diameter is that D50 is 10 ~ 200 microns.
Preferably, step(3)In, described pelletizing particle diameter is that D50 is 20 ~ 100 microns.
Step(4)In, described isostatic cool pressing gum cover material is one kind in polyurethane, black rubber.
Step(4)In, described isostatic cool pressing processing pressure is 200 ~ 500MPa, and the dwell time is 5 ~ 30 minutes.
Preferably, step(4)In, the isostatic cool pressing gum cover material of selection is polyurethane.
Preferably, step(4)In, the isostatic cool pressing processing pressure of selection is 300 ~ 400MPa, and the dwell time is 10 ~ 15 points Clock.
Step(5)In, described high temperature insostatic pressing (HIP) jacket is welded using argon arc welding.
Step(6)In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes first stage degassing process, second stage degreasing Processing and phase III degassing process.
Step(6)In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes first stage degassing process parameter for temperature 100 ~ 300 degree, 2 ~ 24 hours processing times, degassing keeps pressure in jacket to be 1.0 × 10-2~5.0×10-2Pa。
Step(6)In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes second stage ungrease treatment parameter for temperature 400 ~ 1000 degree, 2 ~ 48 hours processing times, degassing keeps pressure in jacket to be 1.0 × 10-2~5.0×10-2Pa。
Step(6)In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes phase III degassing process parameter for temperature 100 ~ 300 degree, 2 ~ 24 hours processing times, degassing keeps pressure in jacket to be 1.0 × 10-3~5.0×10-3Pa。
Preferably, step(6)In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes first stage degassing process parameter and is 200 ~ 300 degree of temperature, 12 ~ 24 hours processing times, degassing keeps pressure in jacket to be 1.0 × 10-2~5.0×10-2Pa。
Preferably, step(6)In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes second stage ungrease treatment parameter and is 400 ~ 800 degree of temperature, 12 ~ 24 hours processing times, degassing keeps pressure in jacket to be 1.0 × 10-2~5.0×10-2Pa。
Preferably, step(6)In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes phase III degassing process parameter and is 200 ~ 300 degree of temperature, 12 ~ 24 hours processing times, degassing keeps pressure in jacket to be 1.0 × 10-3~5.0×10-3Pa。
Step(7)In, described HIP sintering technique is 100 ~ 170MPa of sintering pressure, sintering temperature is 1000 ~ 1400 DEG C, sintering time is 2 ~ 10 hours.
Preferably, step(7)In, described HIP sintering technique is 140 ~ 170MPa of sintering pressure, sintering temperature For 1100 ~ 1300 DEG C, sintering time is 2 ~ 4 hours.
Step(9)In, described density measuring instrument is Archimedes's drainage density of solid detector.
Step(9)In, described purity detecting instrument is inductively coupled plasma atomic emission spectrometer.
Step(9)In, described friction coefficient measuring apparatus device is coefficient of friction detector.
Step(9)In, described crystallite dimension measuring instrument is SEM.
Step(9)In, described bending strength measuring instrument measures testing machine for three-point bending.
Step(9)In, described hardness measurement instrument is Vickers.
Step(9)In, the relative density of described zirconium oxide tungsten disulfide composite self-lubricating ceramics is 99 ~ 100%.
Step(9)In, the purity of described zirconium oxide tungsten disulfide composite self-lubricating ceramics is 99.9 ~ 99.999%.
Step(9)In, the coefficient of friction of described zirconium oxide tungsten disulfide composite self-lubricating ceramics is 0.03 ~ 0.2.
Step(9)In, the crystallite dimension of described zirconium oxide tungsten disulfide composite self-lubricating ceramics is 0.5 ~ 20 micron.
Step(9)In, the bending strength of described zirconium oxide tungsten disulfide composite self-lubricating ceramics is 1000 ~ 1600MPa.
Step(9)In, the hardness of described zirconium oxide tungsten disulfide composite self-lubricating ceramics is HV1200 ~ 2000.
Embodiment
The present invention relates to a kind of high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof, tool Body implementation steps are as follows.
(1)From the yttrium stable zirconium oxide powder that yittrium oxide molar percentage is 3%, by weight yttrium stable zirconium oxide powder:Two Vulcanize tungsten powder=9:1 weighs nano level yttrium stable zirconium oxide powder and curing tungsten powder, and the primary particle size of yttrium stable zirconium oxide powder is 40 nanometers, the primary particle size of curing tungsten powder is 50 nanometers, and the purity of yttrium stable zirconium oxide powder is 99.99%, curing tungsten powder Purity is 99.99%, and two kinds of nano powders are put into ball grinder, and high-energy ball milling is carried out with high energy ball mill and is handled 8 hours.
(2)In step(1)Polyvinyl alcohol, polyethylene glycol and deionized water are put into the good mixed powder of middle ball milling, continues ball Mill 8 hours, obtains mixed powder slurry.
(3)By step(2)Middle acquisition mixed powder slurry, which is put into centrifugal spraying granulator, carries out granulation as D50=57 The pelletizing of micron.
(4)By step(3)The pelletizing of middle acquisition is put into progress isostatic cool pressing processing in polyurethane isostatic cool pressing gum cover, place Reason pressure is 380MPa, and the dwell time is 12 minutes.
(5)By step(4)Middle acquisition isostatic cool pressing blank is put into steel capsule, and high temperature insostatic pressing (HIP), which is made, with argon arc welding welding uses Jacket.
(6)By step(5)The high temperature insostatic pressing (HIP) jacket of middle acquisition carries out degreasing degassing process, first stage degassing process parameter For 260 degree of temperature, 12 hours processing times, degassing keeps pressure in jacket to be 1.0 × 10-2~5.0×10-2Pa, second stage Ungrease treatment parameter is 580 degree of temperature, and 18 hours processing times, degassing keeps pressure in jacket to be 1.0 × 10-2~5.0×10- 2Pa, phase III degassing process parameter be 260 degree of temperature, 18 hours processing times, degassing keep jacket in pressure be 1.0 × 10-3~5.0×10-3Pa。
(7)By step(6)Jacket after the degassing of middle acquisition is put into progress HIP sintering processing in hot isostatic press, HIP sintering technique is sintering pressure 150MPa, and sintering temperature is 1150 DEG C, and sintering time is 5 hours.
(8)By step(7)The ceramic ingot that middle HIP sintering is finished takes out, and removes jacket, produces high-purity high-strength high Tough zirconium oxide tungsten disulfide composite self-lubricating ceramics.
(9)Measuring process(8)The relative density of middle zirconium oxide tungsten disulfide composite self-lubricating ceramics is 99.6%, and purity is 99.9691%, coefficient of friction is 0.08, and grain size is 4.7 microns, and bending strength is 1221MPa, and hardness is HV1608.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all according to the present invention The equivalent change or modification that Spirit Essence is made, should all cover within the scope of the present invention.

Claims (10)

1. a kind of high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof, it is characterised in that specific Step is as follows:
(1)Nano level yttrium stable zirconium oxide powder and curing tungsten powder are weighed, two kinds of nano powders are put into ball grinder and use high energy Ball mill carries out high-energy ball milling processing;
(2)In step(1)Binding agent, dispersant and deionized water are put into the good mixed powder of middle ball milling, continues ball milling, is mixed Close powdery pulp;
(3)By step(2)Middle acquisition mixed powder slurry is put into progress granulation processing in centrifugal spraying granulator;
(4)By step(3)The pelletizing of middle acquisition is put into progress isostatic cool pressing processing in isostatic cool pressing gum cover;
(5)By step(4)Middle acquisition isostatic cool pressing blank is put into steel capsule, and high temperature insostatic pressing (HIP) jacket is made;
(6)By step(5)The high temperature insostatic pressing (HIP) jacket of middle acquisition carries out degreasing degassing process;
(7)By step(6)Jacket after the degassing of middle acquisition is put into progress HIP sintering processing in hot isostatic press;
(8)By step(7)The ceramic ingot that middle HIP sintering is finished, which takes out, removes jacket;
(9)Measuring process(8)The density of middle zirconium oxide tungsten disulfide composite self-lubricating ceramics, purity, coefficient of friction, crystal grain chi Very little, bending strength and hardness.
2. high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics according to claim 1 and its preparation side Method, it is characterised in that:Step(1)In, the percentage by weight of described yttrium stable zirconium oxide powder is 80% ~ 99.9%, and surplus is two Tungsten sulfide.
3. high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics according to claim 1 and its preparation side Method, it is characterised in that:Step(1)In, the purity of described yttrium stable zirconium oxide powder is 99.9 ~ 99.999%.
4. high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics according to claim 1 and its preparation side Method, it is characterised in that:Step(1)In, the purity of described curing tungsten powder is 99.9 ~ 99.999%.
5. high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics according to claim 1 and its preparation side Method, it is characterised in that:Step(9)In, the relative densities of described zirconium oxide tungsten disulfide composite self-lubricating ceramics for 99 ~ 100%。
6. high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics according to claim 1 and its preparation side Method, it is characterised in that:Step(9)In, the purity of described zirconium oxide tungsten disulfide composite self-lubricating ceramics for 99.9 ~ 99.999%。
7. high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics according to claim 1 and its preparation side Method, it is characterised in that:Step(9)In, the coefficient of frictions of described zirconium oxide tungsten disulfide composite self-lubricating ceramics for 0.03 ~ 0.2。
8. high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics according to claim 1 and its preparation side Method, it is characterised in that:Step(9)In, the crystallite dimension of described zirconium oxide tungsten disulfide composite self-lubricating ceramics is 0.5 ~ 20 Micron.
9. high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics according to claim 1 and its preparation side Method, it is characterised in that:Step(9)In, the bending strengths of described zirconium oxide tungsten disulfide composite self-lubricating ceramics for 1000 ~ 1600MPa。
10. high-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics according to claim 1 and its preparation side Method, it is characterised in that:Step(9)In, the hardness of described zirconium oxide tungsten disulfide composite self-lubricating ceramics for HV1200 ~ 2000。
CN201710268531.2A 2017-04-23 2017-04-23 High-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof Pending CN107082639A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710268531.2A CN107082639A (en) 2017-04-23 2017-04-23 High-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710268531.2A CN107082639A (en) 2017-04-23 2017-04-23 High-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof

Publications (1)

Publication Number Publication Date
CN107082639A true CN107082639A (en) 2017-08-22

Family

ID=59611497

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710268531.2A Pending CN107082639A (en) 2017-04-23 2017-04-23 High-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof

Country Status (1)

Country Link
CN (1) CN107082639A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109554693A (en) * 2018-12-12 2019-04-02 山东大学 A kind of metal surface wear resistant friction reducing zirconia ceramics coating and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH034100A (en) * 1989-06-01 1991-01-10 Toshiba Corp Lubrication mechanism
CN2140444Y (en) * 1993-02-08 1993-08-18 包维兴 Ceramic bearing having surface specially treated
CN1412150A (en) * 2002-11-19 2003-04-23 中国科学院兰州化学物理研究所 Self-lubricating ceramic composite material and its preparation process
CN104439247A (en) * 2014-12-30 2015-03-25 山东昊轩电子陶瓷材料有限公司 Molybdenum alloy target preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH034100A (en) * 1989-06-01 1991-01-10 Toshiba Corp Lubrication mechanism
CN2140444Y (en) * 1993-02-08 1993-08-18 包维兴 Ceramic bearing having surface specially treated
CN1412150A (en) * 2002-11-19 2003-04-23 中国科学院兰州化学物理研究所 Self-lubricating ceramic composite material and its preparation process
CN104439247A (en) * 2014-12-30 2015-03-25 山东昊轩电子陶瓷材料有限公司 Molybdenum alloy target preparation method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109554693A (en) * 2018-12-12 2019-04-02 山东大学 A kind of metal surface wear resistant friction reducing zirconia ceramics coating and preparation method thereof

Similar Documents

Publication Publication Date Title
Akhtar A critical review on self-lubricating ceramic-composite cutting tools
EP1801248B1 (en) Wear resistant low friction coating composition and method for coating
WO2020093784A1 (en) Multi-component composite sulfide solid lubricating film, preparation method therefor and use thereof
Chen et al. Composition versus friction and wear behavior of plasma sprayed WC–(W, Cr) 2C–Ni/Ag/BaF2–CaF2 self-lubricating composite coatings for use up to 600° C
Ouyang et al. Fabrication and high-temperature tribological properties of self-lubricating NiCr–BaMoO4 composites
CN103484814A (en) Preparation method of titanium boride based inorganic composite coating
Mazumder et al. An overview of fluoride-based solid lubricants in sliding contacts
CN103834824B (en) A kind of soap-free emulsion polymeization phase carboloy and its preparation method
CN109706370A (en) A kind of fabricated in situ MAX phase enhances the preparation method of nickel-base high-temperature lubricating composite
Yan et al. Nd: YAG laser cladding Ni base alloy/nano-h-BN self-lubricating composite coatings
CN105112760A (en) TiAl-based high-temperature self-lubricating alloy material and application thereof
Chen et al. Mechanical properties and microstructure of Al2O3/Ti (C, N)/CaF2@ Al2O3 self-lubricating ceramic tool
Ibrahim et al. Enhancing the tribological properties of NiAl based nano-composites for aerospace bearing applications
Chen et al. Mechanical properties and microstructure of Al2O3/TiC based self-lubricating ceramic tool with CaF2@ Al (HO) 3
Torkamani et al. Electrodeposition of Nickel matrix composite coatings via various Boride particles: A review
Ren et al. Tribological behaviour of Ni/WC–MoS2 composite coatings prepared by jet electrodeposition with different nano-MoS2 doping concentrations
Lyu et al. Microstructure and mechanical properties of WC–Ni multiphase ceramic materials with NiCl2· 6H2O as a binder
Sukumaran et al. A review on the scope of using calcium fluoride as a multiphase coating and reinforcement material for wear resistant applications
Guo et al. Laser cladding NiCrBSi/TiN/h-BN self-lubricating wear resistant coating on Ti–6Al–4V surface
Sun et al. High temperature tribological properties of NiAl-Ag2Mo2O7 composite coatings prepared by spark plasma sintering
Wang et al. The effect of tungsten introduction on the tribological properties of Si3N4 ceramics paired with GCr15 steel under nonlubricated conditions
CN107082639A (en) High-purity high-strength high-ductility zirconium oxide tungsten disulfide composite self-lubricating ceramics and preparation method thereof
Li et al. Effect of multilayer core-shell microstructure on mechanical properties of Ti (C, N) based self-lubricating cermet materials
Ayyappadas et al. An investigation on tribological and electrical behaviour of conventional and microwave processed copper-graphite composites
Deng et al. Investigation on the Tribological Behaviors of As-Sprayed Al2O3 Coatings Sealed with MoS2 Dry Film Lubricant

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right
TA01 Transfer of patent application right

Effective date of registration: 20200529

Address after: 210000 room 505, building 2, No.2, Shuanglong street, Qinhuai District, Nanjing, Jiangsu Province

Applicant after: Nanjing Jinli New Material Co.,Ltd.

Address before: 210022, room 2, building 2, 506 Shuanglong street, Qinhuai District, Jiangsu, Nanjing, China

Applicant before: NANJING ZIRAE NEW MATERIAL Co.,Ltd.

WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20170822