CN106756392A - A kind of oil field preparation method of WC Co carboloy nozzles - Google Patents
A kind of oil field preparation method of WC Co carboloy nozzles Download PDFInfo
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- CN106756392A CN106756392A CN201611156686.9A CN201611156686A CN106756392A CN 106756392 A CN106756392 A CN 106756392A CN 201611156686 A CN201611156686 A CN 201611156686A CN 106756392 A CN106756392 A CN 106756392A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
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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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Abstract
The invention provides a kind of oil field preparation method of WC Co carboloy nozzles, after Co powder, WC powder and TaC, NbC dispensing through wet-milling, drying, mix binder, compressing, de- forming agent, sintering described WC Co hard alloy be obtained；During dispensing, in terms of the material gross weight 100% after dispensing, Co powder accounts for 8.5~13wt%, TaC/NbC and accounts for 0.35~0.55wt%；Balance of WC.In the present invention, the collaboration of material and proportioning described in blending process, suppression crystal grain is contributed to grow up, help to improve the alloy microstructure after sintering, so as to improve alloy ductility, elevated temperature strength and hardness, improve alloy heat shock resistance, thermal fatigue resistance, purification crystal boundary, increase interface binding power, Co distributed mutuallies evenly, make the toughness of alloy and wearability greatly be unified.
Description
Technical field
The present invention relates to a kind of preparation method of hard alloy, and in particular to a kind of WC- of nozzle for oilfield
The preparation method of Co hard alloy.
Background technology
Hard alloy is with refractory carbide (WC, Ti C, Cr of one or more high rigidity, high-modulus2C3) it is base
Body, with a kind of heterogeneous composite material that magnesium-yttrium-transition metal (Fe, Co, Ni etc.) or other alloys are constituted as Binder Phase.It is this multiple
Closing structural material has high rigidity, high-wearing feature, the red hardness of ceramics, and higher-strength and toughness with metal；And it is this
Special " double high " performance target that exactly material researcher is pursued.
Tungsten-cobalt carbide is exactly the model of " double high " hard alloy or cermet.Its trade mark is by YG and averagely containing cobalt
The percentage composition of amount.For example, YG8, represents average WCo=8%, remaining is the tungsten-cobalt series hard alloy of tungsten carbide.Due to WC-
The superior performance of Co hard alloy and be widely used in wire drawing die, cutting element, corrosion-resistant part and structure member, it is such as high
Plunger and fluid cylinder, finishing roller, the top hammer of diamond synthesis, the roll of steel wire rolling mill, paper knife of pressure vessel etc.；Open in oil field
Nozzle of brill etc..
At present, in oil nozzle field using the tungsten-cobalt alloy that most hard alloy is that cobalt content is (7~9) %.Should
The preparation method of class alloy is generally comprised WC powder and CO powder through dispensing, wet-milling, drying, mixes binder granulation, compressing, de-
The steps such as forming agent, sintering.The wearability and toughness of such alloy are typically conflict：With the increase of Co contents, toughness
Strengthened, and wearability is then more and more lower, the two can not take into account, do not improved at present by the regulation to Co contents more than
Ground.Therefore, the use scope of the alloy is restricted.
Prior art also has the preparation method of some hard alloy, such as Chinese patent of Publication No. CN101985717A
It is raw material that document is disclosed and uses super thick tungsten carbide and cobalt powder, is pre-mixed, and is subsequently adding forming agent and is pressed into agglomerate, is put into
Degreasing and pre-burning are carried out in debinding furnace.Cobalt powder and nano Co will be again added after agglomerates after pre-burning2W4C dispensings and wet again
Mill, then using conventional compressing and sintering method, obtain extra-coarse grained hard alloy；Be still present technological process compared with
Long, energy consumption is higher, easily brings the shortcoming of impurity into.
The Chinese patent literature of Publication No. CN102383020A discloses a kind of ultrathin hard alloy with high hardness, the alloy
Using superfine carbide WC as hard phase, using Co as Binder Phase, using VC, NbC and TaC as inhibitor, the group of the alloy
It is as follows into composition and weight content：WC：90~90.4%, Co：8%, VC：0.2~0.6%, NbC：0.6%, TaC：0.8%.
The crystal grain that there is obtained alloy material in the preparation process of the hard alloy in existing oil field nozzle field is uneven,
The technical problem such as toughness and thermal fatigue are poor, hole is on the high side, wear no resistance.
The content of the invention
For solve uneven crystal grain common in prepared by existing oil field alloy, toughness and thermal fatigue it is poor,
The technical problem that hole is on the high side, wear no resistance etc., the invention provides a kind of oil field preparation side of WC-Co hard alloy nozzle
A kind of method, it is desirable to provide nozzle product that can effectively coordinate hard alloy oil tooth, with the use for coordinating oil field dentition to arrange,
So as to improve the combination property of oil field tooth series alloy, expand the range of application of mine alloy, for oily dentition row field provides
The alloy of super quality and competitive price.
A kind of oil field preparation method of WC-Co hard alloy nozzle, after Co powder, WC powder and TaC, NbC dispensing through wet-milling,
Dry, mix binder, compressing, de- forming agent, the prepared described WC-Co hard alloy of sintering；During dispensing, after dispensing
Material gross weight 100% is counted, and Co powder accounts for 8.5~13wt%, TaC/NbC and accounts for 0.35~0.55wt%；Balance of WC.
In the present invention, in blending process, by the collaboration of described material and proportioning, contribute to suppression crystal grain to grow up, have
Help improve the alloy microstructure after sintering, so as to improve alloy ductility, elevated temperature strength and hardness, improve alloy heat resistanceheat resistant punching
Hit, thermal fatigue resistance, purify crystal boundary, increase interface binding power, Co distributed mutuallies evenly, obtain the toughness of alloy and wearability
To greatly unification.
Preferably, during dispensing, in terms of the material gross weight 100% after dispensing, Co powder accounts for 8.5~12wt%, TaC/NbC
Account for 0.35~0.45wt%, balance of WC.
Further preferably, during dispensing, in terms of the material gross weight 100% after dispensing, Co powder accounts for 8.5~10wt%, TaC/
NbC accounts for 0.35~0.40wt%, balance of WC.
Preferably, the Fisher particle size of described WC powder is 11~25 μm.
Further preferably, 19~25 μm of the Fisher particle size of WC powder；More preferably 20~23 μm.
Still more preferably, the total carbon content of described WC powder is 6.10~6.15%, copmbined-carbon >=6.10%, free carbon
≤ 0.05%, oxygen content≤0.08%.
Preferably, before dispensing, carbonization treatment is carried out to described WC powder, the temperature of described carbonization treatment process is
2100~2400 DEG C；Process time is 1~2h.
In the present invention, the WC supersonic sieves after carbonization treatment is processed get the pretreatment WC powder of 90~160 mesh.
Preferably, Co powder Fisher particle size is 1.45~4.5 μm；More preferably 1.5~3.5 μm；More preferably 1.7
~2.0 μm.
Still more preferably, purity >=99.00% of described Co powder, 1.7~2.0 μm of Fisher particle size, apparent density are
0.40~0.75g/cm3, D50≤8 μm, oxygen content≤0.60%, carbon content≤0.05%.
In the present invention, sintering process is：Sequentially pass through a section of 300 DEG C~550 DEG C it is degreasing sintered, 1100 DEG C~1380 DEG C
Two sections of vacuum-sinterings and 1390 DEG C~1500 DEG C of three sections of pressure sinterings, the pressure of pressure sintering is under 2~3MPa；Institute is obtained
The WC-Co hard alloy stated.
At a temperature of described multi-steps sintering, one degreasing sintered time is 100~200min；Two sections of vacuum-sintering
Time is 30~120min；Three times of pressure sintering are 40~100min.
Further preferably, at a temperature of described multi-steps sintering, one degreasing sintered time is 170~200min；Two
The time of section vacuum-sintering is 85~110min；Three times of pressure sintering are 60~70min；Stress control is in 2.5MPa.
A kind of oil field preparation method of WC-Co hard alloy nozzle, comprises the following steps：
Step (1)：Pretreatment：
From the WC raw materials of high temperature cabonization, wherein, the Fisher particle size of WC powder is 11~25 μm, is then sieved through sonic oscillation again
Get 90~160 grades of area's pretreatments, sieve the WC powder of selected use granularity normal distribution relatively narrower；
Step (2)：Dispensing：By Co powder, the pretreatment WC powder for obtaining of step (1) and TaC, NbC mixing, dispensing；Its
In, in terms of the material gross weight 100% after dispensing, Co powder accounts for 8.5~13wt%, TaC/NbC and accounts for 0.35~0.55wt%；Surplus
It is WC；
Step (3)：Wet-milling：Atoleine, the mixed material of step (2) and wet grinding media ball milling mixing are obtained into slurry；
Step (4)：Spray drying：
Slurry obtained in step (3) is spray-dried in spray drying tower, compound is obtained；
Step (5)：It is compressing：
The compressing base substrate of compound that step 4 is obtained；
Step (6)：Gradient sintering：
By the base substrate of step (5) sequentially pass through a section of 300 DEG C~550 DEG C it is degreasing sintered, 1100 DEG C~1380 DEG C two
Section vacuum-sintering and 1390 DEG C~1500 DEG C of three sections of pressure sinterings, the pressure of pressure sintering is under 2~3MPa；Described in being obtained
WC-Co hard alloy.
In the present invention, by carrying out the carbonization again and sonic oscillation screening of the pretreatment to WC, coordinate the technique
Dispensing, wet-milling, spray drying and compressing, then in conjunction with being sintered under described gradient sintering program, contribute to system
It is standby obtain having concurrently excellent abrasive resistance and toughness, the trade mark is complete and WC-Co hard alloy of high comprehensive performance, and then contribute to
Change oil well spud in during hard alloy utilization present situation.
In the present invention, in step (1), the WC raw materials at a temperature of described high temperature cabonization, its carburizing temperature requirement be
2000~2200 DEG C, the carbonization treatment time is 1~2 hour.
In step (1), the supersonic frequency of sonic oscillation multi-stage screening is 20~30KHz.
In step (1), the WC products sonic oscillation screening under described supersonic frequency after high temperature cabonization, collection 90~
160 grades of powder in area；The powder in 90~160 grades of described areas refers to that the powder of 90~160 mesh is chosen in screening.
It is preferred that choosing the pretreatment WC powder of 90~120 mesh.
In the present invention, by described pretreatment WC powder and described Co powder by described quality than dispensing, contribute into
The combination property of the obtained Hardmetal materials of one step lifting.
In step (3), add the mixed material weight that weight is step (2) the 1.8~2.3% of atoleine.
In step (3), atoleine 0.3~1.0h (hour) before mixed slurry goes out machine pours into ball mill；Wet-milling process
In, the weight ratio of ball material is 3: 1；Wet grinding media is done with alcohol, liquid-solid ratio is 300~350ml/Kg；Total wet-milling time is 20~
32 hours.
In the present invention, using paraffin as forming agent.Wet-milling process is carried out in ball mill, and prior to mixed material 0.3
The time of~1.0h adds described atoleine, and described wet grinding media and abrasive material is then added again, is added according to described
Ratio carries out wet ground, and slurry is obtained.
The liquid-solid ratio that wet grinding media is added is the liquid volume and atoleine, the mixed material of step (2) of wet grinding media
The ratio of weight；As：The wet grinding media of 300~350ml is added per kg atoleines, the mixed material of step (2).
The solid content of slurry obtained in step (3) is 70%~80wt%.That is to say, in slurry obtained in step (3), Gu
The weight of body portion accounts for 70%~80wt% of slurry weight.
The slurry of the solid content is carried out into spray-drying process.
Preferably, in step (4), atomizing pressure is 800~1200Kpa；Atomization temperature is 120~280 DEG C.
Further preferably, in step (4), the slurry of step (3) is spray-dried in spray drying tower, technique ginseng
Number is：Slurry solid content：70%~80%；Nozzle vortex piece combination：1.1mm, 1.2mm；Atomizing pressure：800~
1200Kpa；Oil heater oil temperature：≤300℃；Tower pressure interior force：≤4.5Kpa；Oxygen content in tower：≤ 3.5%；Tower body N2Gas enters
Mouth temperature：120~280 DEG C；Tower body N2Gas outlet temperature：60~150 DEG C；Whirlwind pressure difference：1.0~1.5Kpa；Eluting column is exported
Temperature：≤35℃；Material temperature：≤40℃.
Still more preferably, in step (4), atomizing pressure is 900~1100Kpa；Atomization temperature is 180~220 DEG C.
In the present invention, by the obtained compound compression process of spray drying, preferably, in step (5), compressing mistake
The specific mo(u)lding pressure of journey is 3~8MPa；More preferably 5~6MPa.
The base substrate suppressed sinter through multisection type of the present invention, help to be obtained with excellent abrasive resistance and toughness and
The Hardmetal materials of excellent combination property.
At a temperature of described multi-steps sintering, in step (6), one degreasing sintered time is 100~200min；Two sections
The time of vacuum-sintering is 30~120min；Three times of pressure sintering are 40~100min.
Further preferably, at a temperature of described multi-steps sintering, in step (6), one degreasing sintered time is 170~
200min；Two times of vacuum-sintering are 85~110min；Three times of pressure sintering are 60~70min；Stress control
In 2.5MPa.
In the present invention, a kind of preferred oil field preparation method of WC-Co hard alloy nozzle specifically includes following step
Suddenly：
Step (1)：Pretreatment：From 19~25 μm described of Fisher particle size, through 2000~2200 DEG C of high temperature cabonization WC
Raw material；WC powder after high temperature cabonization is being carried out into multi-stage screening using sonic oscillation mode, supersonic frequency is 20~30KHz,
90~160 grades of area's WC powders of selection enter subsequent processing；
Step (2)：Dispensing：By Co powder, WC powder and TaC, NbC dispensing；In terms of the material gross weight 100% after dispensing, Co
Powder accounts for 8.5~10wt%, TaC/NbC and accounts for 0.35~0.45wt%；Balance of WC；
1.5~3.5 μm of the Fisher particle size of described Co powder；
Step (3)：Wet-milling：By raw material weight 1.8~2.3% paraffin in the form of melt liquid before slurry goes out machine
0.3~1.0h pours into ball mill, and the raw material powder with honest material is added into ball mill, and the weight ratio of ball material is 3: 1, and wet-milling is done with alcohol
Medium, liquid-solid ratio is 300~350ml/Kg, total wet-milling time：26~32 hours；
Step (4)：Spray drying：The good slurry of step (3) wet-milling is spray-dried in spray drying tower, is obtained mixed
Material is closed, technological parameter is as follows：Slurry solid content：70%~80% nozzle vortex piece combination：1.1mm, 1.2mm atomization pressure
Power：800~1200Kpa oil heater oil temperatures：≤ 300 DEG C of tower pressure interior forces：Oxygen content in≤4.5Kpa towers：≤ 3.5% tower body N2
Gas inlet temperature：120~280 DEG C of tower body N2 gas outlet temperatures：60~150 DEG C of whirlwind pressure differences：1.0~1.5Kpa eluting columns are exported
Temperature：≤ 35 DEG C of material temperatures：≤40℃
Step (5)：It is compressing：The compound for obtaining step 4 under 3~8MPa of specific mo(u)lding pressure is compressing；
Step (6)：Sintering：It is sintered in pressure sintering furnace, technological parameter is：300 DEG C~550 DEG C sintering 170~
200min；1100 DEG C~1380 DEG C 85~110min of vacuum-sintering；1390 DEG C~1500 DEG C 60~70min of pressure sintering；Pressure
Control is in 2.5MPa.
Beneficial effect
1st, the hardness average out to HRA 90.1 of YG09 trade mark hard alloy prepared by the inventive method, bending strength average out to
3220Mpa。
2nd, this project uses nozzle product suitable for the large-scale oil of manufacture, and with simple, practical effect.
3rd, due to the addition of grain growth inhibitor TaC/NbC, alloy structure has obtained obvious improvement after sintering, improves
Alloy ductility, elevated temperature strength and hardness, improve alloy heat shock resistance, thermal fatigue resistance, purify crystal boundary, increase interface cohesion
Power, Co distributed mutuallies evenly, make the toughness of alloy and wearability greatly be unified.
Specific implementation method：
Embodiment 1
Step (1)：Pretreatment：
From 23 μm described of Fisher particle size, total carbon content be 6.13%, copmbined-carbon >=6.10%, free carbon≤
0.05%th, oxygen content≤0.08, through 2000~2200 DEG C of high temperature cabonization WC raw materials；WC powder after high temperature cabonization is being used
Sonic oscillation mode carries out multi-stage screening, and supersonic frequency is 20~30KHz, and 120 grades of area's WC powders of selection enter subsequent processing
Step (2)：Dispensing：
By Co powder, WC powder and TaC, NbC dispensing；In terms of the material gross weight 100% after dispensing, Co powder account for 9.0wt%,
TaC/NbC accounts for 0.41wt%；Balance of WC；
1.85 μm of the Fisher particle size of described Co powder；
Step (3)：Wet-milling：
Poured into by the 1.8~2.3% of raw material weight paraffin 0.3~1.0h before slurry goes out machine in the form of melt liquid
Ball mill, ball mill is added by the raw material powder with honest material, and the weight ratio of ball material is 3: 1, and wet grinding media is done with alcohol, and liquid-solid ratio is
320ml/Kg, total wet-milling time：28 hours；
Step (4)：Spray drying：
The good slurry of step (3) wet-milling is spray-dried in spray drying tower, compound is obtained, technological parameter is such as
Under：Slurry solid content：70%~80% nozzle vortex piece combination：1.1mm, 1.2mm atomizing pressure：800~1200Kpa oil
Heater oil temperature：≤ 300 DEG C of tower pressure interior forces：Oxygen content in≤4.5Kpa towers：≤ 3.5% tower body N2Gas inlet temperature：120~
280 DEG C of tower body N2Gas outlet temperature：60~150 DEG C of whirlwind pressure differences：1.0~1.5Kpa eluting column outlet temperatures：≤ 35 DEG C of material temperatures：
≤40℃
Step (5)：It is compressing：
The compound for obtaining step 4 under 3~8MPa of specific mo(u)lding pressure is compressing；
Step (6)：Sintering：
It is sintered in pressure sintering furnace, technological parameter is：300 DEG C~550 DEG C dewaxing section 188min；1100 DEG C~
1380 DEG C of vacuum pre-burning section 90min；1390 DEG C~1500 DEG C pressure sintering section 60min, moulding pressure is controlled in 2.5MPa.
Tungsten-cobalt hard alloy (compact dimensions are 6.5*5.25*20 μm of the standardized product) sample that will be obtained by the present embodiment
This 100 are detected, wherein, the WC mean grain sizes of described hard alloy are 5.4 μm, cross-breaking strength >=
3200Mpa, hardness 90.0HRA, coercive force are 3.5KA/m, and metallographic porosity is A01, B00, C00.
Embodiment 2
Step (1)：Pretreatment：
From 19 μm described of Fisher particle size, total carbon content be 6.14%, copmbined-carbon >=6.10%, free carbon≤
0.05%th, oxygen content≤0.08, through 2000~2200 DEG C of high temperature cabonization WC raw materials；WC powder after high temperature cabonization is being used
Sonic oscillation mode carries out multi-stage screening, and supersonic frequency is 20~30KHz, and 100 grades of area's WC powders of selection enter subsequent processing
Step (2)：Dispensing：
By Co powder, WC powder and TaC, NbC dispensing；In terms of the material gross weight 100% after dispensing, Co powder account for 9.0wt%,
TaC/NbC accounts for 0.38wt%；Balance of WC；
3.40 μm of the Fisher particle size of described Co powder；
Step (3)：Wet-milling：
Poured into by the 1.8~2.3% of raw material weight paraffin 0.3~1.0h before slurry goes out machine in the form of melt liquid
Ball mill, ball mill is added by the raw material powder with honest material, and the weight ratio of ball material is 3: 1, and wet grinding media is done with alcohol, and liquid-solid ratio is
310ml/Kg, total wet-milling time：26 hours；
Step (4)：Spray drying：
The good slurry of step (3) wet-milling is spray-dried in spray drying tower, compound is obtained, technological parameter is such as
Under：Slurry solid content：70%~80% nozzle vortex piece combination：1.1mm, 1.2mm atomizing pressure：800~1200Kpa oil
Heater oil temperature：≤ 300 DEG C of tower pressure interior forces：Oxygen content in≤4.5Kpa towers：≤ 3.5% tower body N2Gas inlet temperature：120~
280 DEG C of tower body N2Gas outlet temperature：60~150 DEG C of whirlwind pressure differences：1.0~1.5Kpa eluting column outlet temperatures：≤ 35 DEG C of material temperatures：
≤40℃
Step (5)：It is compressing：
The compound for obtaining step 4 under 3~8MPa of specific mo(u)lding pressure is compressing；
Step (6)：Sintering：
It is sintered in pressure sintering furnace, technological parameter is：300 DEG C~550 DEG C dewaxing section 200min；1100 DEG C~
1380 DEG C of vacuum pre-burning section 85min；1390 DEG C~1500 DEG C pressure sintering section 70min, moulding pressure is controlled in 2.5MPa.
Tungsten-cobalt hard alloy (compact dimensions are 6.5*5.25*20 μm of the standardized product) sample that will be obtained by the present embodiment
This 100 are detected, wherein, the WC mean grain sizes of described hard alloy are 4.8 μm, cross-breaking strength >=
3100Mpa, hardness 89.2HRA, coercive force are 3.8KA/m, and metallographic porosity is A02, B00, C00.
Embodiment 3
Step (1)：Pretreatment：
From 24 μm described of Fisher particle size, total carbon content be 6.13%, copmbined-carbon >=6.10%, free carbon≤
0.05%th, oxygen content≤0.08, through 2000~2200 DEG C of high temperature cabonization WC raw materials；WC powder after high temperature cabonization is being used
Sonic oscillation mode carries out multi-stage screening, and supersonic frequency is 20~30KHz, and 90 grades of area's WC powders of selection enter subsequent processing
Step (2)：Dispensing：
By Co powder, WC powder and TaC, NbC dispensing；In terms of the material gross weight 100% after dispensing, Co powder account for 9.0wt%,
TaC/NbC accounts for 0.54wt%；Balance of WC；
4.5 μm of the Fisher particle size of described Co powder；
Step (3)：Wet-milling：
Poured into by the 1.8~2.3% of raw material weight paraffin 0.3~1.0h before slurry goes out machine in the form of melt liquid
Ball mill, ball mill is added by the raw material powder with honest material, and the weight ratio of ball material is 3: 1, and wet grinding media is done with alcohol, and liquid-solid ratio is
330ml/Kg, total wet-milling time：32 hours；
Step (4)：Spray drying：
The good slurry of step (3) wet-milling is spray-dried in spray drying tower, compound is obtained, technological parameter is such as
Under：Slurry solid content：70%~80% nozzle vortex piece combination：1.1mm, 1.2mm atomizing pressure：800~1200Kpa oil
Heater oil temperature：≤ 300 DEG C of tower pressure interior forces：Oxygen content in≤4.5Kpa towers：≤ 3.5% tower body N2Gas inlet temperature：120~
280 DEG C of tower body N2Gas outlet temperature：60~150 DEG C of whirlwind pressure differences：1.0~1.5Kpa eluting column outlet temperatures：≤ 35 DEG C of material temperatures：
≤40℃
Step (5)：It is compressing：
The compound for obtaining step 4 under 3~8MPa of specific mo(u)lding pressure is compressing；
Step (6)：Sintering：
It is sintered in pressure sintering furnace, technological parameter is：300 DEG C~550 DEG C dewaxing section 170min；1100 DEG C~
1380 DEG C of vacuum pre-burning section 110min；1390 DEG C~1500 DEG C pressure sintering section 60mine, moulding pressure is controlled in 2.5MPa.
Tungsten-cobalt hard alloy (compact dimensions are 6.5*5.25*20 μm of the standardized product) sample that will be obtained by the present embodiment
This 100 are detected, wherein, the WC mean grain sizes of described hard alloy are 5.8 μm, cross-breaking strength >=
2900Mpa, hardness 88.3HRA, coercive force are 4.0KA/m, and metallographic porosity is A02, B00, C00.
Comparative example 1
Step (1)：Pretreatment：
From 21 μm described of Fisher particle size, total carbon content be 6.13%, copmbined-carbon >=6.10%, free carbon≤
0.05%th, oxygen content≤0.08, through 2000~2200 DEG C of high temperature cabonization WC raw materials；WC powder after high temperature cabonization is being used
Sonic oscillation mode carries out multi-stage screening, and supersonic frequency is 20~30KHz, and 90 grades of area's WC powders of selection enter subsequent processing
Step (2)：Dispensing：
By Co powder, WC powder and TaC, NbC dispensing；In terms of the material gross weight 100% after dispensing, Co powder account for 9.0wt%,
TaC/NbC accounts for 0.60wt%；Balance of WC；
4.5 μm of the Fisher particle size of described Co powder；
Step (3)：Wet-milling：
Poured into by the 1.8~2.3% of raw material weight paraffin 0.3~1.0h before slurry goes out machine in the form of melt liquid
Ball mill, ball mill is added by the raw material powder with honest material, and the weight ratio of ball material is 3: 1, and wet grinding media is done with alcohol, and liquid-solid ratio is
330ml/Kg, total wet-milling time：32 hours；
Step (4)：Spray drying：
The good slurry of step (3) wet-milling is spray-dried in spray drying tower, compound is obtained, technological parameter is such as
Under：Slurry solid content：70%~80% nozzle vortex piece combination：1.1mm, 1.2mm atomizing pressure：800~1200Kpa oil
Heater oil temperature：≤ 300 DEG C of tower pressure interior forces：Oxygen content in≤4.5Kpa towers：≤ 3.5% tower body N2Gas inlet temperature：120~
280 DEG C of tower body N2Gas outlet temperature：60~150 DEG C of whirlwind pressure differences：1.0~1.5Kpa eluting column outlet temperatures：≤ 35 DEG C of material temperatures：
≤40℃
Step (5)：It is compressing：
The compound for obtaining step 4 under 3~8MPa of specific mo(u)lding pressure is compressing；
Step (6)：Sintering：
It is sintered in pressure sintering furnace, technological parameter is：300 DEG C~550 DEG C dewaxing section 170min；1100 DEG C~
1380 DEG C of vacuum pre-burning section 110min；1390 DEG C~1500 DEG C pressure sintering section 80min, moulding pressure is controlled in 2.5MPa.
Tungsten-cobalt hard alloy (compact dimensions are 6.5*5.25*20 μm of the standardized product) sample that will be obtained by the present embodiment
This 100 are detected, wherein, the WC mean grain sizes of described hard alloy are 5.8 μm, cross-breaking strength >=
2600Mpa, hardness 90.3HRA, coercive force are 3.0KA/m, and metallographic porosity is A04, B02, C00.
Claims (10)
1. a kind of oil field preparation method of WC-Co hard alloy nozzle, it is characterised in that Co powder, WC powder and TaC, NbC dispensing
By wet-milling, drying, mix binder, compressing, de- forming agent, the prepared described WC-Co hard alloy of sintering；During dispensing,
In terms of the material gross weight 100% after dispensing, Co powder accounts for 8.5~13wt%, TaC/NbC and accounts for 0.35~0.55wt%；It is balance of
WC。
2. the oil field as claimed in claim 1 preparation method of WC-Co hard alloy nozzle, it is characterised in that during dispensing, with
Material gross weight 100% after dispensing is counted, and Co powder accounts for 8.5~12wt%, and TaC/NbC accounts for 0.35~0.45wt%, balance of WC.
3. the oil field as claimed in claim 2 preparation method of WC-Co hard alloy nozzle, it is characterised in that during dispensing, with
Material gross weight 100% after dispensing is counted, and Co powder accounts for 8.5~10wt%, and TaC/NbC accounts for 0.35~0.40wt%, balance of WC.
4. the preparation method of WC-Co hard alloy nozzle of the oil field as described in any one of claims 1 to 3, it is characterised in that
The Fisher particle size of described WC powder is 11~25 μm.
5. the oil field as claimed in claim 4 preparation method of WC-Co hard alloy nozzle, it is characterised in that Co powder Fei Shi
Granularity is 1.45~4.5 μm.
6. the oil field as claimed in claim 5 preparation method of WC-Co hard alloy nozzle, it is characterised in that described WC
The total carbon content of powder is 6.10~6.15%, copmbined-carbon >=6.10%, free carbon≤0.05%, oxygen content≤0.08%；
Purity >=99.00% of described Co powder, 1.7~2.0 μm of Fisher particle size, apparent density be 0.40~0.75g/cm3,
D50≤8 μm, oxygen content≤0.60%, carbon content≤0.05%.
7. the preparation method of WC-Co hard alloy nozzle of the oil field as described in claim 1 or 6, it is characterised in that dispensing
Before, carbonization treatment is carried out to described WC powder, the temperature of described carbonization treatment process is 2100~2400 DEG C；Process time is
1~2h.
8. the oil field as claimed in claim 7 preparation method of WC-Co hard alloy nozzle, it is characterised in that at carbonization
WC supersonic sieves after reason treatment get the pretreatment WC powder of 90~160 mesh.
9. the preparation method of WC-Co hard alloy nozzle of the oil field as described in claim 1 or 8, it is characterised in that sintered
Cheng Wei：Sequentially pass through degreasing sintered a section of 300 DEG C~550 DEG C, 1100 DEG C~1380 DEG C of two sections of vacuum-sinterings and 1390 DEG C
~1500 DEG C of three sections of pressure sinterings, the pressure of pressure sintering is under 2~3MPa；Described WC-Co hard alloy is obtained.
10. the oil field as claimed in claim 1 preparation method of WC-Co hard alloy nozzle, it is characterised in that including following
Step：
Step (1)：Pretreatment：From 19~25 μm described of Fisher particle size, through 2000~2200 DEG C of high temperature cabonization WC raw materials；
WC powder after high temperature cabonization is being carried out into multi-stage screening using sonic oscillation mode, supersonic frequency is 20~30KHz, selection 90
~160 grades of area's WC powders enter subsequent processing；
Step (2)：Dispensing：By Co powder, WC powder and TaC, NbC dispensing；In terms of the material gross weight 100% after dispensing, Co powder is accounted for
8.5~10wt%, TaC/NbC account for 0.35~0.45wt%；Balance of WC；
1.5~3.5 μm of the Fisher particle size of described Co powder；
Step (3)：Wet-milling：By raw material weight 1.8~2.3% paraffin in the form of melt liquid 0.3 before slurry goes out machine
~1.0h pours into ball mill, and the raw material powder with honest material is added into ball mill, and the weight ratio of ball material is 3: 1, and doing wet-milling with alcohol is situated between
Matter, liquid-solid ratio is 300~350ml/Kg, total wet-milling time：26~32 hours；
Step (4)：Spray drying：The good slurry of step (3) wet-milling is spray-dried in spray drying tower, must be mixed
Material, technological parameter is as follows：Slurry solid content：70%~80% nozzle vortex piece combination：1.1mm, 1.2mm atomizing pressure：
800~1200Kpa oil heater oil temperatures：≤ 300 DEG C of tower pressure interior forces：Oxygen content in≤4.5Kpa towers：≤ 3.5% tower body N2 gas enters
Mouth temperature：120~280 DEG C of tower body N2 gas outlet temperatures：60~150 DEG C of whirlwind pressure differences：1.0~1.5Kpa eluting columns outlet temperature
Degree：≤ 35 DEG C of material temperatures：≤40℃
Step (5)：It is compressing：The compound for obtaining step 4 under 3~8MPa of specific mo(u)lding pressure is compressing；
Step (6)：Sintering：It is sintered in pressure sintering furnace, technological parameter is：300 DEG C~550 DEG C sintering 170~
200min；1100 DEG C~1380 DEG C 85~110min of vacuum-sintering；1390 DEG C~1500 DEG C 60~70min of pressure sintering；Pressure
Control is in 2.5MPa.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108149111A (en) * | 2017-12-04 | 2018-06-12 | 株洲夏普高新材料有限公司 | Hard alloy suitable for cutting of hardened steel and preparation method thereof |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624673A (en) * | 2009-08-14 | 2010-01-13 | 北京工业大学 | Industrialized preparation method of WC-Co hard alloy with low cost and high performance |
| CN102618768A (en) * | 2012-05-04 | 2012-08-01 | 自贡金谷高新材料有限公司 | Hard alloy assembly for tunneling cutterhead of shield machine |
| CN102676902A (en) * | 2012-05-15 | 2012-09-19 | 赣州海盛钨钼集团有限公司 | Ultra-thick hard alloy, and preparation method and application thereof |
| CN103173672A (en) * | 2013-03-22 | 2013-06-26 | 株洲钻石切削刀具股份有限公司 | WC-Co (Wolfram Carbide-Cobalt) hard alloy with Ta/Nb (Tantalum/Niobium) solid solution dispersedly distributed and preparation method thereof |
| CN103540781A (en) * | 2013-05-14 | 2014-01-29 | 自贡金盾硬质合金有限公司 | Method for producing ultra-coarse grain cemented carbide through utilizing high energy stirring and ball-milling technology |
| CN105764637A (en) * | 2013-11-29 | 2016-07-13 | 三菱综合材料株式会社 | Diamond-coated cemented carbide cutting tool, and method for producing same |
| CN105945292A (en) * | 2016-07-04 | 2016-09-21 | 株洲肯特硬质合金有限公司 | Diamond composite sheet and preparing method thereof |
-
2016
- 2016-12-14 CN CN201611156686.9A patent/CN106756392A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624673A (en) * | 2009-08-14 | 2010-01-13 | 北京工业大学 | Industrialized preparation method of WC-Co hard alloy with low cost and high performance |
| CN102618768A (en) * | 2012-05-04 | 2012-08-01 | 自贡金谷高新材料有限公司 | Hard alloy assembly for tunneling cutterhead of shield machine |
| CN102676902A (en) * | 2012-05-15 | 2012-09-19 | 赣州海盛钨钼集团有限公司 | Ultra-thick hard alloy, and preparation method and application thereof |
| CN103173672A (en) * | 2013-03-22 | 2013-06-26 | 株洲钻石切削刀具股份有限公司 | WC-Co (Wolfram Carbide-Cobalt) hard alloy with Ta/Nb (Tantalum/Niobium) solid solution dispersedly distributed and preparation method thereof |
| CN103540781A (en) * | 2013-05-14 | 2014-01-29 | 自贡金盾硬质合金有限公司 | Method for producing ultra-coarse grain cemented carbide through utilizing high energy stirring and ball-milling technology |
| CN105764637A (en) * | 2013-11-29 | 2016-07-13 | 三菱综合材料株式会社 | Diamond-coated cemented carbide cutting tool, and method for producing same |
| CN105945292A (en) * | 2016-07-04 | 2016-09-21 | 株洲肯特硬质合金有限公司 | Diamond composite sheet and preparing method thereof |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108149111A (en) * | 2017-12-04 | 2018-06-12 | 株洲夏普高新材料有限公司 | Hard alloy suitable for cutting of hardened steel and preparation method thereof |
| CN109022996A (en) * | 2018-09-14 | 2018-12-18 | 河源富马硬质合金股份有限公司 | A kind of cemented carbide material towards non-ferrous metals processing |
| CN109022997A (en) * | 2018-09-14 | 2018-12-18 | 河源富马硬质合金股份有限公司 | A kind of high tough high-wearing feature polycrystalline cemented carbide material |
| CN109487142A (en) * | 2018-12-03 | 2019-03-19 | 株洲硬质合金集团有限公司 | A kind of thermal crack resistant mixed crystal hard alloy and preparation method thereof |
| CN109266939A (en) * | 2018-12-05 | 2019-01-25 | 株洲江钨博大硬面材料有限公司 | A kind of high-densit WC-WB-Co spherical powder hard material and preparation method thereof |
| CN109266939B (en) * | 2018-12-05 | 2020-07-24 | 株洲江钨博大硬面材料有限公司 | Preparation method of high-density WC-WB-Co spherical powder hard-face material |
| CN112453407A (en) * | 2020-11-05 | 2021-03-09 | 三阳纺织有限公司 | Manufacturing method of sliding part, sliding part and textile machine applying sliding part |
| CN112453407B (en) * | 2020-11-05 | 2021-12-24 | 三阳纺织有限公司 | Manufacturing method of sliding part, sliding part and textile machine applying sliding part |
| CN114131025A (en) * | 2021-12-01 | 2022-03-04 | 自贡长城表面工程技术有限公司 | Hard alloy radial bearing and production method thereof |
| CN114131025B (en) * | 2021-12-01 | 2023-08-04 | 自贡长城表面工程技术有限公司 | Cemented carbide radial bearing and production method thereof |
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