CN101148747A - Hot spraying WC/Co powder and coating preparation - Google Patents
Hot spraying WC/Co powder and coating preparation Download PDFInfo
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- CN101148747A CN101148747A CNA2007101501426A CN200710150142A CN101148747A CN 101148747 A CN101148747 A CN 101148747A CN A2007101501426 A CNA2007101501426 A CN A2007101501426A CN 200710150142 A CN200710150142 A CN 200710150142A CN 101148747 A CN101148747 A CN 101148747A
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Abstract
The invention discloses a hot spraying WC/Co powder and a coating preparation method. The powder is a composite powder containing cobalt: 5-25%, carbon: 5-6 percent of tungsten and the balance of tungsten, and the tungsten is in a spherical particle structure, the particle size of the tungsten is less than or equal to 150 mu m, and the main body of the tungsten is in the range of 15-90 mu m. The preparation of the powder comprises the following steps: 1) screening, cleaning and drying pure tungsten powder; 2) spheroidizing tungsten powder; 3) carbonizing spherical tungsten powder; 4) the cobalt coats the spherical tungsten carbide. The preparation of the coating of the hot spraying WC/Co powder is that the cobalt tungsten carbide powder is used for preparing the coating by adopting supersonic flame spraying, and the requirements are as follows: the coating is compact and uniform, is tightly combined with the matrix, has the porosity of less than 1 percent, the powder deposition rate of 51.9 percent and the microhardness of 894HV0.2. The powder disclosed by the invention has the characteristics of high density, good fluidity and uniform component distribution, has good impact resistance, toughness and good bonding property with a matrix, is very high in density, improves the performance of a metal ceramic wear-resistant coating, and is widely applied to the fields of aerospace, metallurgy, machinery and the like.
Description
Technical field
The present invention relates to a kind of.Particularly relate to a kind of coating density height, hardness and bonding strength are big, have good wearability, the hot spraying WC/Co powder and the coating preparation of solidity to corrosion, resistance to fatigue.
Background technology
The inventor of modern Wimet at first proposed to produce Wimet with powder metallurgy process in nineteen twenty-three.The technology that he is proposed in patent, still use in the WC-Co hard alloy production process today.Nineteen twenty-six, German Krupp (Krupp) company at first carries out the industrial production of Wimet.At present, existing in the world about 45 countries can produce Wimet, and wherein there are China, Russia, the U.S., Sweden, Japan, Germany, Britain and France in major country of production man.
The basic characteristics of Wimet are:
1. have very high hardness and wear resistance, especially valuable is to still have high hardness under the higher temperature: as at 600 ℃ the time, hardness is higher than the normal temperature hardness of rapid steel, and hardness is higher than the normal temperature hardness of carbon steel in the time of 1000 ℃.
2. have very high Young's modulus, be generally (4～7) * 10
4Kg/mm
2Good rigidly at normal temperatures.
3. have very high ultimate compression strength, can be up to 600kg/mm
2
4. have more stable chemical, the Wimet of some trade mark can be acidproof, alkaline-resisting, even obvious oxidation does not at high temperature take place yet.
5. low thermal expansivity.
The These characteristics of Wimet makes it occupy critical role at aspects such as modern tool material, high-abrasive material, high temperature resistant and corrosion resistant materials.
(theoretical density is 19.3g/cm for the high-melting-point of tungsten (3380 ± 10 ℃), high-density
3) and the high rigidity characteristic make it in civilian and national defense industry, have special purpose., not only with a long history in the world wide to the research and development experience last 100 years of tungsten powder and tungsten carbide powder, and in the ascendant.The research and development of tungsten powder and tungsten carbide powder is subjected to the attention of countries in the world always.Research work over past ten years is extensive especially.And the application of tungsten powder and tungsten carbide powder is also more increasingly extensive, demand improves day by day.The product performance required standard is also improved and strictness accordingly day by day.
Traditional used for hot spraying composite powder generally adopts mechanical mixing and sintering crushing method to produce.The tungsten carbide-base hot spray powder is to be base material with the wolfram varbide, is the composite powder of bonding phase with the cobalt.It is to adopt a certain proportion of tungsten carbide powder and cobalt powder to form by mechanically mixing that mechanical mixing is produced the tungsten carbide-base hot spraying powder, its essence only is a kind of powder mix, and can not be referred to as composite powder, though this method has characteristics such as processing method is simple, production cost is lower, but there are tungsten carbide powder and cobalt powder blended lack of homogeneity, quality instability, the problem that is used for its coating each several part mechanical property consistence difference after the thermospray is so seldom use at present.And the sintering crushing method is that tungsten carbide powder is mixed with cobalt powder, after sintering the tungsten carbide-base alloy into, form through Mechanical Crushing again, though the dusty spray that adopts this method to produce belongs to composite powder, but powder is generally coarse corner angle shape, there are problems such as the out-of-shape of powder, mobile difference, are difficult to reach the spraying coating process requirement; This powder dust and NOISE ON ENVIRONMENT in process of production is seriously polluted simultaneously.
Contriver's square wave, Sun Hai, Mu Kuntong, applied for a kind of Wc-Co alloys powder in moonlight, Ceng Keli; it is basic raw material that this powder preparation method adopts common tungsten-carbide powder, cobalt; processing method with routine; mixed grinding is even; 1300 ℃ of presintering is 2 hours under argon atmospher protection; again 1300 ℃ of following sintering 15 hours, broken powder process.Its application content is referring to " a kind of Wc-Co alloys powder ", and publication number is: CN1584092A, application number is: CN03134123.3.
In recent years, the spherical powder of refractory metal and compound thereof has purposes more and more widely, and globular tungsten powder is exactly one of this class powder.POROUS TUNGSTEN with the globular tungsten powder preparation has more uniform hole, therefore it replaces conventional tungsten powder just gradually, be used to make the POROUS TUNGSTEN parts, negative electrode as the highpowerpulse microwave tube, the barium-tungsten dispense cathode of electron tube, the strainer of metals such as fusion Zn, Al, Mg, Bi, Hg, the transpiring material of rocket, the carrier of catalyst or catalyst, location thruster of man-made satellite or the like.In field of thermal spray, spherical powder is not only mobile fine, and the coating that obtains has better wear resistance.The powder metallurgy pressed compact that globular tungsten powder is made shrinks very even in sintering process, can realize good size control.Therefore also can prepare spherical cobalt wolfram varbide hot spray powder by spray-drying process-sintering, this powder morphology rule, spheroidization are good, and the technological process of production is lacked, but have certain problem, not enough as the powder agglomeration density, hole is big, apparent density of powder is less, and composition profiles is inhomogeneous etc.
Contriver's stone is built the production method that China, Yin Gang, Li Weiqin, He Xianfeng, Cao Wanli have applied for a kind of tungsten carbide base ball shaped thermal spray coating powder; it is base material that this method adopts wolfram varbide; serves as to bond mutually with cobalt or cobalt with chromium; by wet-milling configuration slip, spray drying granulation, sintering under hydrogen shield; at last to agglomerating powder calibrate, thereby obtain the object ball shaped thermal spray coating powder.Its application content is referring to " production method of tungsten carbide base ball shaped thermal spray coating powder ", and publication number is: CN1686644A, application number is: CN200510020875.9.
Cobalt coats a kind of common methods that conventional wolfram varbide is a preparation kennametal powder, but because the out-of-shape of wolfram varbide own causes back uneven components, the problems such as mobile difference of coating.Has purposes widely in the manufacturing of cermet composite coating, the especially carbide/metal composite coating wear member in fields such as Aeronautics and Astronautics, metallurgy, mine, oil and chemical industry and the reparation.Adopt the spherical cobalt tungsten-carbide powder good fluidity of this method preparation, the loose density height satisfies the needs of thermospray.Utilize this powder to prepare the cobalt tungsten carbide coating by thermospray, coating densification, even, tight with matrix bond, porosity is low, has excellent wear-resisting, corrosion resisting property.
Summary of the invention
Technical problem to be solved by this invention is, coating density height is provided, and hardness and bonding strength are big, has good wearability, the hot spraying WC/Co powder and the coating preparation of solidity to corrosion, resistance to fatigue.
The technical solution adopted in the present invention is: a kind of hot spraying WC/Co powder and coating preparation.Wherein hot spraying WC/Co powder contains cobalt, carbon and tungsten, wherein, cobalt: 5～25%, carbon: 5～6%, tungsten is surplus.Described powder is compound powder, its powder grain pattern spherical in shape, and its granularity≤150 μ m, its main body is at 15～90 mu m ranges.
The preparation of described powder comprises the steps:
1) the pure tungsten powder is sieved, the tungsten powder of getting 15～100 mu m ranges is standby, and it is cleaned, dries processing; 2) tungsten powder nodularization: the pure tungsten powder is carried out the atmospheric plasma spheroidizing, sieve after the collection, the globular tungsten powder of getting granularity 15～100 mu m ranges is standby; 3) globular tungsten powder carbonization: with the globular tungsten powder and the carbon black ball mill mixing that have prepared, high temperature cabonization in carbide furnace, the tungsten carbide powder ball milling of coming out of the stove 0.5～3 hour sieves, and the spherical tungsten carbide powder of getting granularity 15～100 mu m ranges is standby; 4) cobalt coats spherical tungsten carbide: utilize high pressure hydro-thermal hydrogen reduction method, preparation cobalt bag spherical tungsten carbide.
Described the pure tungsten powder is carried out the atmospheric plasma spheroidizing, be that the raw material tungsten powder is carried out carrying out the atmospheric plasma nodularization after the thorough drying, working gas is an argon gas, powder feeding gas is a nitrogen, nodularization voltage 65～80V, electric current 450～550A, powder feed rate 30～60g/min, jet length 30～60mm, main air stream amount 1600～1800, with the fused tungsten particle directly spray into cool off in the water globular tungsten powder.
In the globular tungsten powder carbonization: getting the carbon black median size is 0.3～0.6 μ m, carries out mixing and ball milling according to quality percentage composition 5～8% and globular tungsten powder, and the ball milling time is 2～10 hours.
Described in carbide furnace high temperature cabonization be: the powder mix behind the ball milling is put into carbide furnace, under 1600～2200 ℃ of hydrogen shield atmosphere, is incubated 3～8 hours.
Described high pressure hydro-thermal hydrogen reduction method prepares cobalt bag spherical tungsten carbide, at first to tungsten carbide powder purify, alligatoring, hydrophilicity-imparting treatment, include strong base solution processing, strong acid solution processing and sensitization, activation treatment, then with the cobalt sulfate solution for preparing with handle after spheroidized tungsten carbide powder and catalyzer pack into and react in the container, its temperature of reaction is 110～200 ℃, and reaction pressure is 0.1～0.4MPa; Carry out the cobalt tungsten-carbide powder that solid-liquid separation, washing and drying, screening get product after the discharging, wherein the quality percentage composition of cobalt is 5～25%.
The coating preparation of use hot spraying WC of the present invention/Co powder is, use the cobalt tungsten-carbide powder, adopt hypersonic flame spraying to prepare coating, spray parameters: oxygen flow is 1500～2500, kerosene oil flow 20～25, powder feeding 3～8, carrier gas 10～15 requires: coating densification, even, tight with matrix bond, porosity is less than 1%, powder deposition rate 51.9%, and microhardness reaches 894HV
0.2
The coating preparation of use hot spraying WC of the present invention/Co powder can also be that use cobalt tungsten-carbide powder adopts air plasma spraying to prepare coating, spray parameters: electric current 700～850A, main gas 50～60, inferior gas 20～30, powder feeding 2～5, carrier gas 10～15; Require: coating densification, evenly, tight with matrix bond, porosity is less than 1%, powder deposition rate 52.2%, microhardness reaches 873.6HV
0.2
Hot spraying WC of the present invention/Co powder and coating preparation in conjunction with the advantage of cladded type powder and spherical powder, developed cobalt and coated spherical tungsten-carbide powder and preparation method thereof, and coating preparation.Make powder have the characteristics of density height, good fluidity, distributed components concurrently, the demand that better adapts to thermospray, and improve the performance of metal ceramic wear-resisting coating simultaneously, have good shock resistance, toughness and with the matrix good binding, density is very high, is widely used in fields such as aerospace, metallurgy, machinery.Thermospray tungsten carbide ceramics coating has remarkable advantages in wear resistance, solidity to corrosion, resistance to fatigue, and preparation speed is fast, and cost is low, and environment is good.
Description of drawings
Fig. 1 is the surface topography design sketch of plasma spheroidization tungsten powder of the present invention;
Fig. 2 is the surface topography design sketch of cobalt bag spherical tungsten carbide powder of the present invention.
Embodiment
Below in conjunction with embodiment hot spraying WC of the present invention/Co powder and coating preparation are made a detailed description.
Hot spraying WC of the present invention/Co powder and coating preparation be, will be after washing, dry, screening by the pure tungsten powder, again through granulation, nodularization, the globular tungsten powder of atmospheric plasma spheroidizing; Globular tungsten powder and carbon black after will handling carry out mixing and ball milling again, carry out high temperature cabonization and handle under protective atmosphere, obtain the spherical tungsten carbide powder; Prepare cobalt through high pressure hydro-thermal hydrogen reduction method again and coat spherical tungsten carbide nucleocapsid composite powder.Adopt hypersonic flame spraying or air plasma spraying method to prepare the cobalt tungsten carbide coating.
Hot spraying WC of the present invention/Co powder contains: cobalt, carbon and tungsten, wherein, and cobalt: 5～25%, carbon: 5～6%, tungsten is surplus.Described coated powder is compound powder, its powder grain pattern spherical in shape, and its granularity≤150 μ m, its main body is at 15～90 mu m ranges.
Hot spraying WC of the present invention/Co powder is prepared by following steps:
1) the pure tungsten powder is sieved, the tungsten powder of getting 15～100 mu m ranges is standby, and it is cleaned, dries processing;
2) tungsten powder nodularization: the pure tungsten powder is carried out the atmospheric plasma spheroidizing, sieve after the collection, the globular tungsten powder of getting granularity 15～100 mu m ranges is standby;
Described the pure tungsten powder is carried out the atmospheric plasma spheroidizing, be that the raw material tungsten powder is carried out carrying out the atmospheric plasma nodularization after the thorough drying, working gas is an argon gas, powder feeding gas is a nitrogen, nodularization voltage 65～80V, electric current 450～550A, powder feed rate 30～60g/min, jet length 30～60mm, main air stream amount 1600～1800, with the fused tungsten particle directly spray into cool off in the water globular tungsten powder.
3) globular tungsten powder carbonization: with the globular tungsten powder and the carbon black ball mill mixing that have prepared, high temperature cabonization in carbide furnace, the tungsten carbide powder ball milling of coming out of the stove 0.5～3 hour sieves, and the spherical tungsten carbide powder of getting granularity 15～100 mu m ranges is standby;
In the globular tungsten powder carbonization: getting the carbon black median size is 0.3～0.6 μ m, carries out mixing and ball milling according to quality percentage composition 5～8% and globular tungsten powder, and the ball milling time is 2～10 hours.Described in carbide furnace high temperature cabonization be: the powder mix behind the ball milling is put into carbide furnace, under 1600～2200 ℃ of hydrogen shield atmosphere, is incubated 3～8 hours.
4) cobalt coats spherical tungsten carbide: utilize high pressure hydro-thermal hydrogen reduction method, preparation cobalt bag spherical tungsten carbide.
At first to tungsten carbide powder purify, alligatoring, hydrophilicity-imparting treatment, mainly comprise strong base solution processing, strong acid solution processing and sensitization, activation treatment, then with the cobalt sulfate solution for preparing with handle after spheroidized tungsten carbide powder and catalyzer pack into and react in the container, its temperature of reaction is 110～200 ℃, and reaction pressure is 0.1～0.4MPa; Carry out the cobalt tungsten-carbide powder that solid-liquid separation, washing and drying, screening get product after the discharging, wherein the quality percentage composition of cobalt is 5～25%.Described cobalt tungsten-carbide powder granularity≤150 μ m, its main body is at 15～90 mu m ranges.
The coating preparation of use hot spraying WC of the present invention/Co powder is, use the cobalt tungsten-carbide powder, adopt hypersonic flame spraying to prepare coating, spray parameters: oxygen flow is 1500～2500, kerosene oil flow 20～25, powder feeding 3～8, carrier gas 10～15 requires: coating densification, even, tight with matrix bond, porosity is less than 1%, powder deposition rate 51.9%, and microhardness reaches 894HV
0.2
The coating preparation of use hot spraying WC/Co powder of this can also be that use cobalt tungsten-carbide powder adopts air plasma spraying to prepare coating, spray parameters: electric current 700～850A, main gas 50～60, inferior gas 20～30, powder feeding 2～5, carrier gas 10～15; Require: coating densification, evenly, tight with matrix bond, porosity is less than 1%, powder deposition rate 52.2%, microhardness reaches 873.6HV
0.2
Provide specific embodiment below.
Embodiment 1:
The pure tungsten powder is sieved, and the tungsten powder of getting 500g15～100 mu m ranges cleans, dries.Above tungsten powder is carried out the atmospheric plasma nodularization, and working gas is an Ar gas, and powder feeding gas is N
2Gas, nodularization voltage 75V, electric current 500A, powder feed rate 55g/min, jet length 45mm, main air stream amount 1650.The fused tungsten particle directly sprayed in the water cool off.Globular tungsten powder and the 25g carbon black of getting granularity 15～90 mu m ranges after the collection carried out mixing and ball milling 2 hours, and the material behind the ball milling is put into carbide furnace and be incubated 4 hours at 2000 ℃ under hydrogen shield atmosphere, and ball milling sieved in 1 hour more afterwards.Get tungsten-carbide powder strong acid, highly basic and sensitization, the activation treatment of granularity 15～90 mu m ranges.Afterwards the cobalt sulfate solution for preparing and tungsten-carbide powder after the nodularization and catalyzer are packed into and react in the container.Temperature of reaction is 180 ℃, and reaction pressure is 0.2MPa.Carry out solid-liquid separation, washing and drying, the screening powder that gets product after the discharging.The flowability of this sphere WC-Co powder is 10.8s/50g, and loose density is 6.78g/cm
3
Adopt air plasma spraying to prepare coating in the powder of above preparation, spray parameters is electric current 700～850A, main gas 40, inferior gas 25, powder feeding 3.5, carrier gas 12.5.Coating densification, evenly, tight with matrix bond, porosity is less than 1%, powder deposition rate 52.2%, microhardness reaches 873.6HV
0.2
Embodiment 2:
The pure tungsten powder is sieved, and the tungsten powder of getting 500g15～100 mu m ranges cleans, dries.Above tungsten powder is carried out the atmospheric plasma nodularization, and working gas is an Ar gas, and powder feeding gas is N
2Gas, nodularization voltage 70V, electric current 500A, powder feed rate 50g/min, jet length 50mm, main air stream amount 1600.The fused tungsten particle directly sprayed in the water cool off.Globular tungsten powder and the 25g carbon black of getting granularity 15～90 mu m ranges after the collection carried out mixing and ball milling 3 hours, and the material behind the ball milling is put into carbide furnace and be incubated 5 hours at 2000 ℃ under hydrogen shield atmosphere, and ball milling sieved in 1 hour more afterwards.Get tungsten-carbide powder strong acid, highly basic and sensitization, the activation treatment of granularity 15～90 mu m ranges.Afterwards the cobalt sulfate solution for preparing and tungsten-carbide powder after the nodularization and catalyzer are packed into and react in the container.Temperature of reaction is 200 ℃, and reaction pressure is 0.2MPa.Carry out solid-liquid separation, washing and drying, the screening powder that gets product after the discharging.The flowability of this sphere WC-Co powder is 10.5s/50g, and loose density is 6.69g/cm
3
Adopt hypersonic flame spraying to prepare coating in the powder of above preparation, oxygen flow is 2000, kerosene oil flow 22.5, powder feeding 3～8, carrier gas 12.5.Coating densification, evenly, tight with matrix bond, porosity is less than 1%, powder deposition rate 51.9%, microhardness reaches 894HV
0.2
Claims (9)
1. hot spraying WC/Co powder is characterized in that described powder contains cobalt, carbon and tungsten, wherein, cobalt: 5～25%, carbon: 5～6%, tungsten is surplus.
2. hot spraying WC according to claim 1/Co powder is characterized in that, described powder is compound powder, its powder grain pattern spherical in shape, and its granularity≤150 μ m, its main body is at 15～90 mu m ranges.
3. hot spraying WC according to claim 1/Co powder is characterized in that the preparation of described powder comprises the steps:
1) the pure tungsten powder is sieved, the tungsten powder of getting 15～100 mu m ranges is standby, and it is cleaned, dries processing;
2) tungsten powder nodularization: the pure tungsten powder is carried out the atmospheric plasma spheroidizing, sieve after the collection, the globular tungsten powder of getting granularity 15～100 mu m ranges is standby;
3) globular tungsten powder carbonization: with the globular tungsten powder and the carbon black ball mill mixing that have prepared, high temperature cabonization in carbide furnace, the tungsten carbide powder ball milling of coming out of the stove 0.5～3 hour sieves, and the spherical tungsten carbide powder of getting granularity 15～100 mu m ranges is standby;
4) cobalt coats spherical tungsten carbide: utilize high pressure hydro-thermal hydrogen reduction method, preparation cobalt bag spherical tungsten carbide.
4. hot spraying WC according to claim 3/Co powder, it is characterized in that, described the pure tungsten powder is carried out the atmospheric plasma spheroidizing, is that the raw material tungsten powder is carried out carrying out the atmospheric plasma nodularization after the thorough drying, working gas is an argon gas, powder feeding gas is a nitrogen, nodularization voltage 65～80V, electric current 450～550A, powder feed rate 30～60g/min, jet length 30～60mm, main air stream amount 1600～1800, with the fused tungsten particle directly spray into cool off in the water globular tungsten powder.
5. hot spraying WC according to claim 3/Co powder, it is characterized in that, in the globular tungsten powder carbonization: getting the carbon black median size is 0.3～0.6 μ m, carries out mixing and ball milling according to quality percentage composition 5～8% and globular tungsten powder, and the ball milling time is 2～10 hours.
6. hot spraying WC according to claim 3/Co powder is characterized in that, described in carbide furnace high temperature cabonization be: the powder mix behind the ball milling is put into carbide furnace, under 1600～2200 ℃ of hydrogen shield atmosphere, is incubated 3～8 hours.
7. hot spraying WC according to claim 3/Co powder, it is characterized in that, described high pressure hydro-thermal hydrogen reduction method prepares cobalt bag spherical tungsten carbide, at first to tungsten carbide powder purify, alligatoring, hydrophilicity-imparting treatment, include strong base solution processing, strong acid solution processing and sensitization, activation treatment, then with the cobalt sulfate solution for preparing with handle after spheroidized tungsten carbide powder and catalyzer pack into and react in the container, its temperature of reaction is 110～200 ℃, and reaction pressure is 0.1～0.4MPa; Carry out the cobalt tungsten-carbide powder that solid-liquid separation, washing and drying, screening get product after the discharging, wherein the quality percentage composition of cobalt is 5～25%.
8. a coating preparation of using hot spraying WC/Co powder is characterized in that, uses the cobalt tungsten-carbide powder, adopt hypersonic flame spraying to prepare coating, spray parameters: oxygen flow is 1500～2500, kerosene oil flow 20～25, powder feeding 3～8, carrier gas 10～15, require: coating densification, even, tight with matrix bond, porosity is less than 1%, powder deposition rate 51.9%, microhardness reaches 894HV
0.2
9. a coating preparation of using hot spraying WC/Co powder is characterized in that, uses the cobalt tungsten-carbide powder, adopts air plasma spraying to prepare coating, spray parameters: electric current 700～850A, main gas 50～60, inferior gas 20～30, powder feeding 2～5, carrier gas 10～15; Require: coating densification, evenly, tight with matrix bond, porosity is less than 1%, powder deposition rate 52.2%, microhardness reaches 873.6HV
0.2
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2007
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