CN101629263A - Ultrafine cemented carbide and preparation method and application thereof - Google Patents
Ultrafine cemented carbide and preparation method and application thereof Download PDFInfo
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- CN101629263A CN101629263A CN200910115934A CN200910115934A CN101629263A CN 101629263 A CN101629263 A CN 101629263A CN 200910115934 A CN200910115934 A CN 200910115934A CN 200910115934 A CN200910115934 A CN 200910115934A CN 101629263 A CN101629263 A CN 101629263A
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Abstract
The invention discloses ultrafine cemented carbide which comprises the following components in raw materials in percentage by weight: 8.0-9.0 percent of Co, 0.5-1.0 percent of TaC and the balance of WC including 0.3-2.0 percent of Cr3C2; and the preparation method comprises the steps of blending, wet milling, spray drying, pressure molding and sintering. The invention definitely limits the optimized technical conditions of all the components in the raw materials and the optimized process conditions of all the steps of preparation; the ultrafine cemented carbide has good hardness property and good strength property: the transverse rupture strength is equal to or higher than 2800 MPa, the hardness is equal to or higher than 92.5 HRA, the coercive force is 26-35 KA/m and the average grain size of the WC is 200-400 nm. And the invention also discloses application of the ultrafine cemented carbide in the preparation of cemented carbide tools.
Description
Technical field
The invention belongs to field of powder metallurgy, particularly a kind of WC-Co ultra-fine cemented carbide and its production and application.
Background technology
The WC-Co Wimet is widely used in fields such as mechanical workout, oil, mine, mould and structure wearing piece because of having high intensity, hardness and good wear resistance and oxidation-resistance.According to the grain fineness number of WC in the alloy, generally the WC-Co Wimet is divided into ultra-fine cemented carbide and nano hard alloy.The Wimet grain fineness number grade scale of ISO/TC190 Technical Committee is defined as nano hard alloy to grain fineness number less than the Wimet of 0.2 μ m (200nm), and is grain fineness number that the Wimet of 0.2 μ m (200nm)～0.5 μ m (500nm) is defined as ultra-fine cemented carbide.Ultra-fine cemented carbide has premium propertiess such as high strength, high rigidity, high-wearing feature, has satisfied the development of modern industry and extraordinary difficult-to-machine material. thereby ultra-fine cemented carbide is the focus of international Wimet science and industrial community research always over nearly 10 years.
The preparation of ultra-fine cemented carbide generally will be passed through processing steps such as batching, wet-milling, drying, moulding and sintering.In the many pieces of patent documentations of publication number 1544675A, 1480546A, 1775973A and 1827264A, different ratios of raw materials is all disclosed, the for example granularity of WC powder and Co powder, the selection of grain growth inhibitor, the ultra-fine cemented carbide preparation method of DIFFERENT WET abrasive stick spare, different sintering process.But other performances of all unqualified WC powder of above-mentioned patent documentation and Co powder and grain growth inhibitor such as total carbon content, combined carbon amount, uncombined carbon amount, oxygen level etc., do not disclose the concrete processing condition of exsiccant yet; And the quality of ultra-fine cemented carbide is subjected to respectively to go on foot the of great impact of production technique, if controlling of production process is improper, be easy in alloy, produce defectives such as microporosity, glomerocryst, cobalt pond, grain growth and folder are thick, thereby have influence on the over-all properties of ultra-fine cemented carbide.
Summary of the invention
The purpose of this invention is to provide a kind of production technique that respectively goes on foot and fully optimize ultra-fine cemented carbide of back preparation and its production and application.
In order to address the above problem, the present invention at first discloses a kind of ultra-fine cemented carbide, and the composition of its raw material and weight percent are the Co powder of 8.0-9.0%, the TaC powder of 0.5-1.0%, and surplus is for containing Cr
3C
2The WC powder, Cr
3C
2Weight percent in WC is 0.3-2.0%; The technical qualification of described each component are:
Table 1 Co powder technical qualification
????????????????????????????????????????????????????????????????????????????
Purity % Fisher particle size (μ n) loose density (g/cm
3) D
50(μ m) oxygen % carbon %
≥99.0????≤1.0???????????0.40～0.75???????≤8????????≤0.60????≤0.05
????????????????????????????????????????????????????????????????????????????
Table 2 TaC technical qualification
????????????????????????????????????????????????????????????????????
Fisher particle size (μ m) total carbon % uncombined carbon %
≤1.5????????????≤6.25????≤0.10
????????????????????????????????????????????????????????????????????
Table 3 WC powder technical qualification
????????????????????????????????????????????????????????????????????
Fsss (μ m) total carbon % combined carbon % uncombined carbon % oxygen %
≤0.8????????6.10-6.20????≥6.10??????≤0.05????????≤0.08
????????????????????????????????????????????????????????????????????
The present invention preferably contains 0.3-1.0 (weight) %Cr
3C
2WC.
Contain Cr
3C
2WC the commercial goods has been arranged, its preparation technology is roughly:
A) calcination
Ammonium paratungstate (APT) raw material is added in the rotary kiln, under about 600-800 ℃ of temperature, feed ammonia, keep furnace reduction atmosphere, ammonium paratungstate (APT) generates blue tungsten or purple tungsten under high temperature and faint reducing atmosphere, and its net reaction is:
B) reduction
Blue tungsten behind the calcination or purple tungsten were passed through 2-5 hour in reduction furnace, and 600-900 ℃ high temperature under hydrogen shield atmosphere, is reduced into the average metal tungsten powder of Fei Shi, and its chemical equation is:
C) carbonization
Metal tungsten powder is mixed under protection of inert gas with carbon black, chromium sesquioxide powder, pass through 1200-1500 ℃ high temperature then in carbide furnace, feed purified hydrogen and mediate and protective atmosphere, reaction generates wolfram varbide and chromium carbide.
W+C→WC
Cr
2O
3+C→Cr
3C
2+CO
2↑
Process is pulverized then, sieving obtains the tungsten-carbide powder that contains chromium carbide that granularity meets the requirements.Described tungsten-carbide powder must vacuumize or feed protection of inert gas before use.
Cr
3C
2Prepare with WC, not only can suppress in the WC generative process WC crystalline effectively and grow up, and Cr
3C
2Distribution ground is more even around the WC molecule, during afterwards with Co powder, TaC powder sintering, also can suppress growing up of WC grain better.
Described ultrafine hard alloy preparation method comprises batching, wet-milling, spraying drying, compression molding and sintering, and concrete processing step is as follows:
1) batching: prepare satisfactory Co powder, TaC powder and contain Cr according to formula rate
3C
2The WC powder, Cr
3C
2Weight percent with respect to WC is 0.4-2.0%;
2) wet-milling: the raw material powder that will prepare material adds ball mill, ratio of grinding media to material is 3-6: 1, do wet grinding media with alcohol, liquid-solid ratio is 300-500ml/Kg, the paraffin that accounts for described raw material 1.8-2.3 (weight) % is poured ball mill into, always wet-milling time: 60-80 hour with form 0.3-1.0hr before raw material adds of melt liquid;
3) spraying drying: the slip that step 2 wet-milling is good carries out in spray-drying tower, and spraying drying gets compound, and processing parameter is as follows:
Slip solid content: 70%-80%,
The combination of nozzle vortex sheet: 1.1,1.2,
Atomizing pressure: 800-1200Kpa,
Oil heater oil temperature :≤300 ℃,
Tower internal pressure :≤4.0Kpa,
Oxygen level in the tower :≤3.5%,
Tower body N
2The gas temperature in :≤200 ℃,
Tower body N
2The gas temperature out :≤100 ℃,
Whirlwind pressure reduction: 1.0-1.5Kpa,
The eluting column temperature out :≤35 ℃,
Material temperature :≤40 ℃;
4) compression moulding: the compound compression moulding that under specific mo(u)lding pressure 3-8MPa, step 3 is obtained;
5) sintering: carry out sintering in pressure sintering furnace, pressure-controlling is at 3-8MPa, and processing parameter is as follows:
300 ℃----550 ℃ of dewaxing sections 100-200min,
1100 ℃---1380 ℃ of pre-burning section 30-120min,
1390 ℃---1500 ℃ of sintering stage 40-100min;
In described spray-drying process, preferred tower internal pressure is 2.4-3.0Kpa; Tower body N
2The gas temperature in is 150-250 ℃; Tower body N
2The gas temperature in is 80-120 ℃.
In described sintering process, the optimizing technology parameters in each stage is:
370 ℃----450 ℃ of dewaxing sections 120-180min,
1200 ℃---1260 ℃ of pre-burning section 40-60min,
1390 ℃---1425 ℃ of sintering stage 50-90min.
In the described spray-drying process, " nozzle vortex sheet combination: 1.1,1.2 " refers to the diameter of vortex sheet.
In the described wet-milling step, the paraffin of Jia Ruing uses as forming agent in advance.
WC mean grain size in the ultra-fine cemented carbide of employing method for preparing is 200-400nm, cross-breaking strength 〉=2800Mpa, and hardness 〉=92.5HRA, Coercive Force are 26-35KA/m, porosity is A02, B00, C00.
Porosity of the present invention is meant hole shared volume percent in material, and is very big to the over-all properties influence of ultra-fine cemented carbide.Have data to show: if can make the complete densification of alloy, the over-all properties of alloy can improve (ultra-fine cemented carbide quality Control during Production, powder metallurgy technology, 2007,25 (4): 284-288) more than 15%.Porosity utilizes the opticmicroscope metallographic method to measure, that is: according to " metallographic of Wimet porosity and non-ization and carbon is measured " (GB/T3489-1983), the Wimet metallographic sample that makes is amplified 100 times (or 200 times) under opticmicroscope, compares definite grade with normal pictures..Be divided into A, B, C and greater than 25 microns hole four classes according to the size of hole and classification.The category-A hole is the hole less than 10 microns, is divided into A02, A04, four ranks of A06, A08, does not find that the category-A hole is A00.The category-B hole is the hole of 10-25 micron, is divided into B02, B04, four ranks of B06, B08, does not find that the category-B hole is B00.C class hole is that graphite is mingled with, and is divided into C02, C04, four ranks of C06, C08, does not find that C class hole is C00.The present invention 1) select suitable, fine APT raw material for use, be equipped with suitable calcining-reduction-carbonization technique, make the WC raw material can carbonization fully and controlled the content of oxygen and carbon in the powder stock well, and adopt the filling with inert gas to handle in the wrapping process, avoid the oxidation of material; 2) optimize wet-grinding technology and relative device; 3) technology of optimization compression molding; 4) optimize sintering process, clear and definite sintering temperature, sintering pressure and the best of breed between the time.By the optimization to above-mentioned processing step, the porosity of ultra-fine cemented carbide of the present invention is A02, B00, C00, does not have the hole and the graphite impurities of 10-25 micron, thereby has guaranteed described ultra-fine cemented carbide good comprehensive performances.Also explanation simultaneously, the processing parameter of each step all can influence the performance and the quality of ultra-fine cemented carbide in the preparation process, has only optimization, has combined each parameter, could guarantee the quality of final ultra-fine cemented carbide.
It will be appreciated by those skilled in the art that in the ultra-fine cemented carbide of the present invention except described component, also may contain in production, the raw material inevitably trace impurity, but these trace impurities do not influence the performance of described ultra-fine cemented carbide.
The present invention also provides described ultra-fine cemented carbide to be applied to prepare the matrix of no cutting tool coated with hard alloy or cutting tool coated with hard alloy: the compound that spraying drying is obtained promptly obtains the matrix of described no cutting tool coated with hard alloy or cutting tool coated with hard alloy according to the shape compression moulding of described cutter through described sintering step.
For wear resistance and the hardness that improves cutter, on the matrix of described cutting tool coated with hard alloy, apply one or more layers hardness height, metal or nonmetallic compound film that wear resistance is good, TiC for example, TiAlN, Al
2O
3Deng, obtain cutting tool coated with hard alloy.
The preparation method of inserted tool coating has a lot, comprises vapour deposition, thermospray, thermo-chemical treatment, thermal response diffusion deposition, collosol and gel etc.Vapour deposition is used many, the preparation coating quality is good, progressively become the leading of cutter coat preparation method. gas phase deposition technology be divided into chemical vapour deposition (chemical vapor deposition.CVD) and physical vapor deposition (physical vapor deposition, PVD).
On a kind of inserted tool matrix that utilizes the method for the invention preparation, adopt the PVD coating, carry out the TiAlN coating of high Al content, can obtain smooth surface, PVD coated chip that processing characteristics is stable, this cutter have good resistance to wear, the ability of anti-tipping blade, resistance to high temperature oxidation, be mainly used in steel alloy, stainless screw thread semi-finishing and precision work, also can be used for non-threaded semi-finishing and precision work, the more non-coated cutting tool of its working (machining) efficiency improves more than 2 times.In the cutting comparative test, but 90 of this kind coated cutting tool processing parts number of packages average out to, and the cutter (trade mark IC908) of the similar coatings that external leading company produces but 60 of processing parts number of packages average out to, the former compares the latter and improves 1.5 times of working (machining) efficiencies.
Studies show that except granularity, the quality of various components is very big to the over-all properties influence of ultra-fine cemented carbide in the raw material.The present invention defines the preferable range of WC powder, Co powder, TaC powder total carbon content, combined carbon content, free carbon content and oxygen level etc.Generally all think VC and Cr
3C
2Be the grow up preferably combination of inhibitor of WC grain, but the mean grain size 200nm of WC～400nm in the ultra-fine cemented carbide of sinter molding of the present invention prove TaC and Cr
3C
2Combination also can play the effect that the good restraining WC grain is grown up.
Because powder metallurgy relates to complicated physics, chemical process, therefore, nearly tens of the processing parameters that each step such as wet-milling, spraying drying, compression molding, sintering relates to.Each parameter all can influence the performance of final ultra-fine W-Co Wimet even trickle variation.For example, foregoing porosity and raw material, wet-milling, compression molding, agglomerating relation.The present invention on the basis of big quantity research, the clear and definite preferred processing conditions in each step such as wet-milling, spraying drying, compression molding, sintering.Preferred by above-mentioned mass parameter, processing parameter, ultra-fine cemented carbide of the present invention has good hardness and intensity over-all properties: the WC mean grain size is 200-400nm, cross-breaking strength 〉=2800Mpa, hardness 〉=92.5HRA, Coercive Force is 26-35KA/m, and porosity is A02, B00, C00.
Realize ultrafine hard alloy preparation method of the present invention, do not need to increase new production unit, every processing condition are controlled in strictness on the existing equipment basis, can not increase the production cost of described ultra-fine cemented carbide.
Embodiment
The invention will be further described below in conjunction with embodiment, but these embodiment can not be interpreted as limitation of the present invention.
WC powder described in the embodiment all is meant and contains Cr
3C
2The WC powder, the percentage ratio among the embodiment is all represented weight percentage.
The manufacturer and the trade mark of the used WC powder of embodiment, Co powder, TaC powder see Table 4
Table 4
| Classification | Manufacturer | The specification trade mark |
| The WC powder | Xiamen Golden Egret Special Alloy Co., Ltd | GWC006 or GWC008 |
| The Co powder | The U.S. new and high technology of Green limited-liability company | ??GEM-3 |
| The TaC powder | Changsha Wing High-Tech New Materials Co., Ltd. | ??TaC-1 |
The technical qualification of WC powder, Co powder, TaC powder see Table 1-3
Embodiment 1
1) batching:
The 8.0%Co powder, 0.5%TaC powder, the WC powder of surplus, wherein Cr
3C
2Content be 0.5%.
2) wet-milling
Do wet grinding media with alcohol, ratio of grinding media to material is 5: 1, and liquid-solid ratio is 350ml/Kg, account for join raw material 2.3% paraffin pour ball mill into form 0.3.hr before raw material adds of melt liquid, total wet-milling time: 70 hours;
3) spraying drying
The slip that obtains after wet-milling is finished is sent into spray-drying tower, makes compound; Spray-dired processing condition are:
The slip solid content: 70%,
The combination of nozzle vortex sheet: 1.1,1.2,
Atomizing pressure: 800Kpa,
Oil heater oil temperature: 200 ℃,
Tower internal pressure: 4.5Kpa,
Oxygen level in the tower: 2.0%,
Tower body N
2The gas temperature in: 150 ℃,
Tower body N
2The gas temperature out: 80 ℃,
Whirlwind pressure reduction: 1.5Kpa,
The eluting column temperature out: 25 ℃,
Material temperature: 30 ℃.
4) compression molding
The compression molding under 8MPa of spraying drying gained compound.
5) sintering
Sintering under the 5.5MPa pressure in pressure sintering furnace, processing parameter is:
550 ℃ of dewaxing section 100min,
1350 ℃ of pre-burning section 50min,
1420 ℃ of sintering stage 100min.
The ultra-fine cemented carbide cutter that makes, cross-breaking strength 3000Mpa, hardness 92.8HRA, Coercive Force are 30KA/m, and porosity is A02, B00, C00, and the WC mean grain size is 350nm.
Embodiment 2
The processing parameter in each step sees Table 5, through the step identical as embodiment 1, and the ultra-fine cemented carbide cutter that makes, cross-breaking strength 3200Mpa, hardness 92.5HRA, Coercive Force are 31KA/m, and porosity is A02, B00, C00, and the WC mean grain size is 340nm.
Embodiment 3
The processing parameter in each step sees Table 5, through the step identical as embodiment 1, and the ultra-fine cemented carbide cutter that makes, cross-breaking strength 3300Mpa, hardness 92.8HRA, Coercive Force are 33KA/m, and porosity is A02, B00, C00, and the WC mean grain size is 320nm.
Embodiment 4
The processing parameter in each step sees Table 5, through the step identical as embodiment 1, and the ultra-fine cemented carbide cutter that makes, cross-breaking strength 3180Mpa, hardness 92.7HRA, Coercive Force are 31KA/m, and porosity is A02, B00, C00, and the WC mean grain size is 300nm.
Embodiment 5
The processing parameter in each step sees Table 5, through the step identical as embodiment 1, and the ultra-fine cemented carbide cutter that makes, cross-breaking strength 3340Mpa, hardness 93HRA, Coercive Force are 33KA/m, and porosity is A02, B00, C00, and the WC mean grain size is 290nm.
Embodiment 6
The processing parameter in each step sees Table 5, through the step identical as embodiment 1, and the ultra-fine cemented carbide cutter that makes, cross-breaking strength 3270Mpa, hardness 92.9HRA, Coercive Force are 32KA/m, and porosity is A02, B00, C00, and the WC mean grain size is 330nm.
Embodiment 7
The processing parameter in each step sees Table 5, through the step identical as embodiment 1, and the ultra-fine cemented carbide cutter that makes, cross-breaking strength 3330Mpa, hardness 92.5HRA, Coercive Force are 34KA/m, and porosity is A02, B00, C00, and the WC mean grain size is 310nm.
Embodiment 8
The processing parameter in each step sees Table 5, through the step identical as embodiment 1, and the ultra-fine cemented carbide cutter that makes, cross-breaking strength 3260Mpa, hardness 92.5HRA, Coercive Force are 33KA/m, and porosity is A02, B00, C00, and the WC mean grain size is 330nm.
Table 5 embodiment 2-8 process parameter table
A: the weight percent of described component in the total raw material powder; B:Cr
3C
2Weight percent in the WC powder.
Embodiment 9
Ultra-fine cemented carbide cutter with embodiment 2 preparations is a matrix, carries out the PVD coating of TiAlN, obtains ultra-fine cemented carbide coated cutting tool (trade mark THK201); The proximate ultra-fine cemented carbide PVD of coated material coated cutting tool (trade mark IC908) with external certain company's production cuts contrast then, and test-results sees Table 6.
The result shows that the various performance parameters of THK201 is identical with IC908, and more durable, but 60 of certain external cutter processing parts number of packages average out to, but 90 of THK201 processing parts number of packages average out to, average working (machining) efficiency improves 1.5 times.
Table 6 cutting comparative test
Claims (13)
1, a kind of ultra-fine cemented carbide, the composition of its raw material and weight percent are the Co powder of 8.0-9.0%, the TaC powder of 0.5-1.0%, and surplus is for containing Cr
3C
2The WC powder, Cr
3C
2Weight percent in WC is 0.3-2.0%; The purity of wherein said Co powder 〉=99.00%, Fisher particle size≤1.0 μ m, loose density are 0.40～0.75g/cm
3, D
50≤ 8 μ m, oxygen level≤0.60%, carbon content≤0.05%, the Fisher particle size of described TaC powder≤1.5 μ m, total carbon content≤6.25%, free carbon content≤0.10%, the described 0.3-2.0%Cr that contains
3C
2Fisher particle size≤0.8 μ m, the total carbon content of WC powder be 6.10～6.20%, combined carbon content 〉=6.10%, free carbon content≤0.05%, oxygen level≤0.08%; WC mean grain size in the described ultra-fine cemented carbide is 200-400nm, cross-breaking strength 〉=2800Mpa, and hardness 〉=92.5HRA, Coercive Force are 26-35KA/m, porosity is A02, B00, C00; Described ultra-fine cemented carbide prepares through following steps:
1) batching: prepare satisfactory Co powder, TaC powder and contain Cr according to formula rate
3C
2The WC powder;
2) wet-milling: the raw material powder that will prepare material adds ball mill, ratio of grinding media to material is 3-6: 1, do wet grinding media with alcohol, liquid-solid ratio is 300-500ml/Kg, the paraffin that accounts for described raw material 1.8-2.3 (weight) % is poured ball mill into, always wet-milling time: 60-80 hour with form 0.3-1.0hr before raw material adds of melt liquid;
3) spraying drying: the slip that step 2 wet-milling is good carries out in spray-drying tower, and spraying drying gets compound, and processing parameter is as follows:
Slip solid content: 70%-80%,
Nozzles combine: 1.1,1.2 (combinations of vortex sheet),
Atomizing pressure: 800-1200Kpa,
Oil heater oil temperature :≤300 ℃,
Tower internal pressure :≤4.5Kpa,
Oxygen level in the tower :≤3.5%,
Tower body N
2Gas temperature in: 120-280 ℃,
Tower body N
2Gas temperature out: 60-150 ℃,
Whirlwind pressure reduction: 1.0-1.5Kpa,
The eluting column temperature out :≤35 ℃,
Material temperature :≤40 ℃;
4) compression moulding: the compound compression moulding that under specific mo(u)lding pressure 3-8MPa, step 3 is obtained;
5) sintering: carry out sintering in pressure sintering furnace, pressure-controlling is at 3-8MPa, and processing parameter is:
300 ℃----550 ℃ of dewaxing sections 100-200min,
1100 ℃---1380 ℃ of pre-burning section 30-120min,
1390 ℃---1500 ℃ of sintering stage 40-100min;
2, a kind of ultra-fine cemented carbide according to claim 1 is characterized in that: described WC powder contains the Cr of 0.4-1.0 (weight) %
3C
2
3, a kind of ultra-fine cemented carbide according to claim 1 is characterized in that: in the described spray-drying process, the tower internal pressure is 2.4-3.0Kpa.
4, a kind of ultra-fine cemented carbide according to claim 1 is characterized in that: in the described spray-drying process, and tower body N
2The gas temperature in is 150-250 ℃.
5, a kind of ultra-fine cemented carbide according to claim 1 is characterized in that: in the described spray-drying process, and tower body N
2The gas temperature in is 80-120 ℃.
6, a kind of ultra-fine cemented carbide according to claim 1 is characterized in that: in the described sintering process, the processing parameter in each stage is:
370 ℃----450 ℃ of dewaxing sections 120-180min,
1200 ℃---1260 ℃ of pre-burning section 40-60min,
1390 ℃---1425 ℃ of sintering stage 50-90min.
7, the described ultrafine hard alloy preparation method of a kind of claim 1 comprises batching, wet-milling, spraying drying, compression molding and sintering, and concrete processing step is as follows:
1) batching: 8.0-9.0 (weight) %Co powder, 0.5-1.0 (weight) %TaC powder and surplus contain Cr
3C
2The WC powder, Cr
3C
2Weight percent with respect to WC is 0.3-2.0%; The purity of wherein said Co powder 〉=99.00%, Fisher particle size≤1.0 μ m, loose density are 0.40～0.75g/cm
3, D
50≤ 8 μ m, oxygen level≤0.60%, carbon content≤0.05%, the Fisher particle size of described TaC powder≤1.5 μ m, total carbon content≤6.25%, free carbon content≤0.10%, the Fisher particle size of described WC powder≤0.8 μ m, total carbon content are 6.00～6.20%, combined carbon content 〉=6.10%, free carbon content≤0.05%, oxygen level≤0.08%;
2) wet-milling: the raw material powder that will prepare material adds ball mill, ratio of grinding media to material is 3-6: 1, do wet grinding media with alcohol, liquid-solid ratio is 300-500ml/Kg, the paraffin that accounts for described raw material 1.8-2.3 (weight) % is poured ball mill into, always wet-milling time: 60-80 hour with form 0.3-1.0hr before raw material adds of melt liquid;
3) spraying drying: the slip that step 2 wet-milling is good carries out in spray-drying tower, and spraying drying gets compound, and processing parameter is as follows:
Slip solid content: 70%-80%,
Nozzles combine: 1.1,1.2 (combinations of vortex sheet),
Atomizing pressure: 800-1200Kpa,
Oil heater oil temperature :≤300 ℃,
Tower internal pressure :≤4.5Kpa,
Oxygen level in the tower :≤3.5%,
Tower body N
2The gas temperature in :≤250 ℃,
Tower body N
2The gas temperature out :≤120 ℃,
Whirlwind pressure reduction: 1.0-1.5Kpa,
The eluting column temperature out :≤35 ℃,
Material temperature :≤40 ℃;
4) compression moulding: the compound compression moulding that under specific mo(u)lding pressure 3-8MPa, step 3 is obtained;
5) sintering: carry out sintering in pressure sintering furnace, pressure-controlling is at 3-8MPa, and processing parameter is as follows:
300 ℃----550 ℃ of dewaxing sections 100-200min,
1100 ℃---1380 ℃ of pre-burning section 30-120min,
1390 ℃---1500 ℃ of sintering stage 40-100min.
8, preparation method according to claim 3 is characterized in that: described WC powder contains the Cr of 0.4-1.0 (weight) %
3C
2
9, preparation method according to claim 3 is characterized in that: in the described spray-drying process, the tower internal pressure is 2.4-3.0Kpa.
10, a kind of ultra-fine cemented carbide according to claim 1 is characterized in that: in the described spray-drying process, and tower body N
2The gas temperature in is 150-250 ℃.
11, a kind of ultra-fine cemented carbide according to claim 1 is characterized in that: in the described spray-drying process, and tower body N
2The gas temperature in is 80-120 ℃.
12, a kind of ultra-fine cemented carbide according to claim 1 is characterized in that: in the described sintering process, the processing parameter in each stage is:
370 ℃----450 ℃ of dewaxing sections 120-180min,
1200 ℃---1260 ℃ of pre-burning section 40-60min,
1390 ℃---1425 ℃ of sintering stage 50-90min.
13, the described ultra-fine cemented carbide of a kind of claim 1 is applied to prepare the matrix of no cutting tool coated with hard alloy or cutting tool coated with hard alloy, it is characterized in that: the compound that spraying drying is obtained promptly obtains the matrix of described no cutting tool coated with hard alloy or cutting tool coated with hard alloy according to the shape compression moulding of described cutter through described sintering step.
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| CN 200910115934 CN101629263B (en) | 2009-08-06 | 2009-08-06 | Ultrafine cemented carbide and preparation method and application thereof |
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