CN103862038A - Extra-coarse hard alloy parcel powder and preparation method thereof - Google Patents
Extra-coarse hard alloy parcel powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses extra-coarse hard alloy parcel powder and a preparation method thereof. The preparation method comprises the steps of adding tungsten carbide powder of which the average Fisher particle size is 3-8 microns and other hard phase carbide powder of which the average Fisher particle size is 0.5-1.5 microns into a soluble cobalt salt solution, wherein the tungsten carbide powder and the hard phase carbide powder are used as a nucleating agent; performing chemical coprecipitation wrapping reaction on ammonium oxalate serving as a precipitator to enable the produced cobalt oxalate to be precipitated to the surfaces of the tungsten carbide powder and the hard phase carbide powder, and performing filtration, washing, drying and hydrogen reduction to obtain hard alloy parcel powder. The extra-coarse hard alloy parcel powder comprises the following components in percentage by weight: 6-12 percent of cobalt, 0-2 percent of crystalline grain inhibitor and the balance being tungsten carbide, wherein the average Fisher particle size of the tungsten carbide is 3-8 microns.
Description
Technical field
The present invention relates to parcel powder of a kind of super thick carbide alloy and preparation method thereof.
Background technology
Super thick carbide alloy has higher red hardness and good thermal fatigue resistance, thermal shock resistance, is widely used in the fields such as mining, road breaking and stamping die under extreme operating condition condition, cold heading die, roll.The heavily loaded coal winning machine cutting bit that external large-scale coal-winning machine is supporting and hard rock mole all adopt the carbide alloy of grain size higher than 4 μ m.When the grain size of tungsten carbide reaches 5 μ m when above, carbide alloy is in keeping better intensity, can obviously change its plasticity, product reliability improves greatly, and at present China is difficult to prepare grain size and reaches the super thick carbide alloy that 5 μ m are above, microstructure is good, combination property is high.
Batch mixing process in tradition CEMENTED CARBIDE PRODUCTION is all used wet-grinding technology and relative device, by tungsten carbide and Binder Phase metal dust, take alcohol or gasoline etc. as wet grinding media, more than ball milling 20h, is evenly distributed so that mix phase constituent element in ball mill by certain ratio of grinding media to material.But wet-grinding technology and relative device is applied to the super thick carbide alloy of preparation has obvious drawback: in wet-milling process, coarse grained tungsten carbide second particle and primary particle are easily broken, therefore prepare the required raw material tungsten-carbide powder granularity of super thick carbide alloy and need reach tens even more than tens microns, and carburizing temperature is high in the tungsten-carbide powder preparation process of large particle diameter, cause great energy consumption; Ball milling causes powder particle fragmentation, crystal formation distortion, and powder size is difficult to control; Meanwhile, the required Ball-milling Time of wet-milling is long, and the wet grinding media consumptions such as alcohol, gasoline are large, improved production cost.Therefore, preparation technology's problem of tungsten carbide-cobalt composite powder is the key point of preparation high-performance, the super thick carbide alloy of low cost.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, provide a kind of excellent quality super thick carbide alloy parcel powder, this powder can be used for the super thick carbide alloy of production performance excellence.The present invention also provides the preparation method of this powder, and the method flow process is simple, with short production cycle and cost is low.
In order to achieve the above object, technical scheme provided by the invention is:
Described super thick carbide alloy parcel powder, is characterized in that, described super thick carbide alloy parcel powder comprises the component of following percentage by weight:
Cobalt 6～12%
Grain inhibitor 0～2%
Surplus is tungsten carbide;
The average Fisher particle size of described tungsten carbide is 3～8 μ m.
Cobalt is evenly wrapped in tungsten carbide and grain inhibitor surface.
Preferably, described grain inhibitor is selected from one or more in titanium carbide, ramet, niobium carbide, vanadium carbide or chromium carbide.
Preferably, the average Fisher particle size of described grain inhibitor is 0.5～1.5 μ m.
Above-mentioned super thick carbide alloy parcel powder is that cobalt powder preparation flow is combined with powder mixed process, utilizes chemical coprecipitation encapsulation reaction and hydrogen reduction reaction and prepares, and the concrete steps that the super thick carbide alloy of preparation 100g wraps up powder are as follows:
(1), by water-soluble 24.2～59.2g cobalt saline compound, being mixed with concentration is 65～91.5gL
-1cobalt salt solution, under 50～80 ℃ of water bath condition, heat;
(2) 88～94g tungsten carbide and 0～2g grain inhibitor are added in the aqueous solution of the cobalt salt after heating, 50～80 ℃ of constant temperature obtain mixed slurry after stirring 30～60min;
(3) by 15.9～31.8g (NH
4)
2c
2o
4h
2o is water-soluble, and compound concentration is 34.1～68.2gL
-1ammonium oxalate solution, under 50～80 ℃ of water bath condition, heat;
(4) ammonium oxalate solution after heating is all added in mixed slurry as precipitating reagent, 50～80 ℃ of constant temperature stir 30～60min, then stop heating, continue to stir 30～60min, make the cobalt oxalate precipitation generating be wrapped in carbide particle surface; Slip to be mixed be cooled to 25 ℃ following after, successively after filtration, washing and dry, obtain super thick carbide alloy parcel powder presoma;
(5) be 1～4m by super thick carbide alloy parcel powder presoma in 450～600 ℃, hydrogen flowing quantity
3under the condition of/min, reduce 1～2.5h, make cobalt oxalate be reduced into cobalt, obtain super thick carbide alloy parcel powder.
Preferably, the described cobalt saline compound of step (1) is CoCl
26H
2o, CoSO
47H
2o or Co (NO
3)
26H
2o.
Preferably, the described cobalt salt of step (1) is cobalt chloride, cobaltous sulfate or cobalt nitrate.
Preferably, described being dried of step (4) is freeze-day with constant temperature 1～3h under 100～120 ℃ of conditions.
Preferably, the described washing of step (4) is with water purification washing 1～2 time.
It is that the tungsten-carbide powder of 3～8 μ m and average Fisher particle size are that other hard phase carbide powders of 0.5～1.5 μ m are as nucleating agent that this method adopts average Fisher particle size, join in solubility cobalt salt solution, take ammonium oxalate as precipitating reagent, utilize chemical coprecipitation encapsulation reaction, make the cobalt oxalate producing deposit to tungsten-carbide powder and other hard phase carbide powder surfaces, through filtration, washing, the dry and super thick carbide alloy parcel powder of hydrogen reducing acquisition.This method can replace conventional wet grinding process, and the parcel powder size controllability of preparation is good, and technological process is simple, and cost is low, can prepare average crystal grain degree≤4 μ m by this parcel powder, and institutional framework is even, the super thick carbide alloy of excellent combination property.
Compared with prior art, beneficial effect of the present invention is:
(1) in this super thick composite hard alloy powder, cobalt powder distributes more even between hard phase powder, has reduced the possibility that forms reunion big particle and cobalt pond defect after super thick sintering cemented carbide.Tungsten-carbide powder particle size distribution is narrow, and controllability is good, by this powder can prepare institutional framework evenly, the super thick carbide alloy of excellent performance.
(2) this super thick composite hard alloy powder preparing technique process flow process is simple, with short production cycle, and does not add other reducing agents, nontoxic.
(3) this super thick composite hard alloy powder technology of preparing has overcome the problem that in conventional wet grinding process batch mixing process, tungsten carbide size significantly reduces, and the tungsten carbide raw material powder particle size of use has reduced by 2～4 times, is conducive to save the energy, reduces cost.
Accompanying drawing explanation
Fig. 1 is the XRD spectral line of the tungsten-cobalt carbide parcel powder prepared of this invention;
Fig. 2 is the macro morphology photo of the tungsten-cobalt carbide parcel powder prepared of this invention;
Fig. 3 is the microscopic appearance photo of the tungsten-cobalt carbide parcel powder prepared of this invention;
Fig. 4 is the super thick and stiff matter alloy microstructure photo with the tungsten-cobalt carbide parcel powder preparation of this invention.
The specific embodiment
embodiment 1
The super thick carbide alloy parcel powder of tungsten carbide-6wt% cobalt.
It is the tungsten-carbide powder 94g of 3 μ m that nucleating agent uses average Fisher particle size.By 24.2g CoCl
26H
2o is soluble in water, is mixed with 65gL
-1coCl
2solution, heating water bath to 50 ℃.Pour tungsten-carbide powder into CoCl
2in solution, constant temperature mechanical agitation 30min.By soluble in water 15.9g ammonium oxalate, preparation 68.2gL
-1ammonium oxalate solution, heating water bath to 50 ℃.Then ammonium oxalate solution is all poured in mixed slurry as precipitating reagent, constant temperature mechanical agitation 30min, then stop heating, continue mechanical agitation 60min, make the cobalt oxalate precipitation generating be wrapped in carbide particle surface, after slip is cooled to 25 ℃, filter, with water purification washing 1 time, then in the thermostatic drying chamber of 120 ℃, dry 1h obtains wrapping up powder presoma.To wrap up powder presoma reduces in hydrogen reducing furnace.Reduction temperature is 450 ℃, and hydrogen flowing quantity is 1m
3/ min, recovery time 2.5h, makes cobalt oxalate be reduced into cobalt, obtains super thick carbide alloy parcel powder.In parcel powder, the content 6g of cobalt, tungsten carbide content 94g.
embodiment 2
The super thick carbide alloy parcel powder of tungsten carbide-0.5wt% vanadium carbide-8wt% cobalt.
It is that tungsten carbide and the average Fisher particle size of 4 μ m is the vanadium carbide powder of 1.5 μ m that nucleating agent uses average Fisher particle size.Wherein, tungsten-carbide powder is 91.5g, and vanadium carbide powder is 0.5g.By 32.3gCoCl
26H
2o is soluble in water, is mixed with 65gL
-1coCl
2solution, heating water bath to 60 ℃.Pour tungsten-carbide powder and vanadium carbide powder into CoCl
2in solution, constant temperature mechanical agitation 40min.By soluble in water 21.2g ammonium oxalate, preparation 34.1gL
-1ammonium oxalate solution, heating water bath to 60 ℃.Then ammonium oxalate solution is all poured in mixed slurry as precipitating reagent, constant temperature mechanical agitation 50min, then stop heating, continue mechanical agitation 40min, make the cobalt oxalate precipitation generating be wrapped in carbide particle surface, after slip is cooled to 25 ℃, filter, with water purification washing 2 times, then in the thermostatic drying chamber of 100 ℃, dry 3h obtains wrapping up powder presoma.To wrap up powder presoma reduces in hydrogen reducing furnace.Reduction temperature is 500 ℃, and hydrogen flowing quantity is 2m
3/ min, recovery time 2h, makes cobalt oxalate be reduced into cobalt, obtains super thick carbide alloy parcel powder.In parcel powder, the content 8g of cobalt, tungsten carbide content 91.5g, vanadium carbide content 0.5g.
embodiment 3
The super thick carbide alloy parcel powder of tungsten carbide-1.5wt% chromium carbide-9wt% cobalt.
It is that tungsten carbide and the average Fisher particle size of 4.5 μ m is the chromium carbide powder of 1.6 μ m that nucleating agent uses average Fisher particle size.Wherein, tungsten-carbide powder is 89.5g, and chromium carbide powder is 1.5g.By 43gCoSO
47H
2o is soluble in water, is mixed with 77.5gL
-1coSO
4solution, heating water bath to 70 ℃.Pour tungsten-carbide powder and chromium carbide powder into CoSO
4in solution, constant temperature mechanical agitation 40min.By soluble in water 23.9g ammonium oxalate, preparation 68.2gL
-1ammonium oxalate solution, heating water bath to 70 ℃.Then ammonium oxalate solution is all poured in mixed slurry as precipitating reagent, constant temperature mechanical agitation 40min, then stop heating, continue mechanical agitation 60min, make the cobalt oxalate precipitation generating be wrapped in carbide particle surface, after slip is cooled to 25 ℃, filter, with water purification washing 2 times, then in the thermostatic drying chamber of 110 ℃, dry 2h obtains wrapping up powder presoma.To wrap up powder presoma reduces in hydrogen reducing furnace.Reduction temperature is 550 ℃, and hydrogen flowing quantity is 3m
3/ min, recovery time 2h, makes cobalt oxalate be reduced into cobalt, obtains super thick carbide alloy parcel powder.In parcel powder, the content 9g of cobalt, tungsten carbide content 89.5g, chromium carbide content 1.5g.
embodiment 4
The super thick carbide alloy parcel powder of tungsten carbide-0.5wt% titanium carbide-0.5wt% vanadium carbide-10wt% cobalt.
It is that titanium carbide and the average Fisher particle size that the tungsten carbide of 5.5 μ m, average Fisher particle size are 2.9 μ m is the vanadium carbide powder of 1.5 μ m that nucleating agent uses average Fisher particle size.Wherein, tungsten-carbide powder is 89g, and titanium carbide powder is 0.5g, and vanadium carbide powder is 0.5g.By 47.7gCoSO
47H
2o is soluble in water, is mixed with 77.5gL
-1coSO
4solution, heating water bath to 80 ℃.Pour tungsten carbide, titanium carbide and vanadium carbide powder into CoSO
4in solution, constant temperature mechanical agitation 60min.By soluble in water 26.5g ammonium oxalate, preparation 68.2gL
-1ammonium oxalate solution, heating water bath to 80 ℃.Then ammonium oxalate solution is all poured in mixed slurry as precipitating reagent, constant temperature mechanical agitation 60min, then stop heating, continue mechanical agitation 60min, make the cobalt oxalate precipitation generating be wrapped in carbide particle surface, after slip is cooled to 20 ℃, filter, with water purification washing 2 times, then in the thermostatic drying chamber of 120 ℃, dry 1h obtains wrapping up powder presoma.To wrap up powder presoma reduces in hydrogen reducing furnace.Reduction temperature is 550 ℃, and hydrogen flowing quantity is 2m
3/ min, recovery time 2h, makes cobalt oxalate be reduced into cobalt, obtains super thick carbide alloy parcel powder.In parcel powder, the content 9g of cobalt, tungsten carbide content 89g, titanium carbide content 0.5g, vanadium carbide content 0.5g.
The super thick carbide alloy parcel powder of tungsten carbide-0.5wt% titanium carbide-1wt% ramet (niobium)-11wt% cobalt.
It is that titanium carbide and the average Fisher particle size that the tungsten carbide of 6.5 μ m, average Fisher particle size are 2.9 μ m is ramet (niobium) powder of 0.9 μ m that nucleating agent uses average Fisher particle size.Wherein, tungsten-carbide powder is 87.5g, and titanium carbide powder is 0.5g, and ramet (niobium) powder is 1g.By 54.3gCo (NO
3)
26H
2o is soluble in water, is mixed with 91.5gL
-1co (NO
3)
2solution, heating water bath to 80 ℃.Pour tungsten carbide, titanium carbide and ramet (niobium) powder into Co (NO
3)
2in solution, constant temperature mechanical agitation 40min.By soluble in water 29.1g ammonium oxalate, preparation 34.1gL
-1ammonium oxalate solution, heating water bath to 80 ℃.Then ammonium oxalate solution is all poured in mixed slurry as precipitating reagent, constant temperature mechanical agitation 60min, then stop heating, continue mechanical agitation 60min, make the cobalt oxalate precipitation generating be wrapped in carbide particle surface, after slip is cooled to 20 ℃, filter, with water purification washing 2 times, then in the thermostatic drying chamber of 120 ℃, dry 1.5h obtains wrapping up powder presoma.To wrap up powder presoma reduces in hydrogen reducing furnace.Reduction temperature is 500 ℃, and hydrogen flowing quantity is 2m
3/ min, recovery time 2.5h, makes cobalt oxalate be reduced into cobalt, obtains super thick carbide alloy parcel powder.In parcel powder, the content 11g of cobalt, tungsten carbide content 87.5g, titanium carbide content 0.5g, ramet (niobium) content 1g.
embodiment 6
The super thick carbide alloy parcel powder of tungsten carbide-2wt% ramet (niobium)-12wt% cobalt.
It is that the tungsten carbide of 8 μ m, average Fisher particle size are that average Fisher particle size is ramet (niobium) powder of 1.2 μ m that nucleating agent uses average Fisher particle size.Wherein, tungsten-carbide powder is 86g, and ramet (niobium) powder is 2g.By 59.2g Co (NO
3)
26H
2o is soluble in water, is mixed with 91.5gL
-1co (NO
3)
2solution, heating water bath to 70 ℃.Pour tungsten-carbide powder and ramet (niobium) powder into Co (NO
3)
2in solution, constant temperature mechanical agitation 50min.By soluble in water 31.8g ammonium oxalate, preparation 68.2gL
-1ammonium oxalate solution, heating water bath to 70 ℃.Then ammonium oxalate solution is all poured in mixed slurry as precipitating reagent, constant temperature mechanical agitation 50min, then stop heating, continue mechanical agitation 50min, make the cobalt oxalate precipitation generating be wrapped in carbide particle surface, after slip is cooled to 25 ℃, filter, with water purification washing 2 times, then in the thermostatic drying chamber of 100 ℃, dry 3h obtains wrapping up powder presoma.To wrap up powder presoma reduces in hydrogen reducing furnace.Reduction temperature is 600 ℃, and hydrogen flowing quantity is 4m
3/ min, recovery time 1h, makes cobalt oxalate be reduced into cobalt, obtains super thick carbide alloy parcel powder.In parcel powder, the content 12g of cobalt, tungsten carbide content 86g, ramet (niobium) content 2g.
Claims (7)
1.
a kind ofsuper thick carbide alloy parcel powder, is characterized in that, described super thick carbide alloy parcel powder comprises the component of following percentage by weight:
Cobalt 6～12%
Grain inhibitor 0～2%
Surplus is tungsten carbide;
The average Fisher particle size of described tungsten carbide is 3～8 μ m.
2. super thick carbide alloy parcel powder as claimed in claim 1, is characterized in that, described grain inhibitor is selected from one or more in titanium carbide, ramet, niobium carbide, vanadium carbide or chromium carbide.
3. super thick carbide alloy parcel powder as claimed in claim 2, is characterized in that, the average Fisher particle size of described grain inhibitor is 0.5～1.5 μ m.
4. the preparation method of super thick carbide alloy parcel powder as described in claims 1 to 3 any one, is characterized in that, preparation 100g is super, and thick carbide alloy parcel powder comprises the steps:
(1), by water-soluble 24.2～59.2g cobalt saline compound, being mixed with concentration is 65～91.5gL
-1cobalt salt solution, under 50～80 ℃ of water bath condition, heat;
(2) 88～94g tungsten carbide and 0～2g grain inhibitor are added in the aqueous solution of the cobalt salt after heating, 50～80 ℃ of constant temperature obtain mixed slurry after stirring 30～60min;
(3) by 15.9～31.8g (NH
4)
2c
2o
4h
2o is water-soluble, and compound concentration is 34.1～68.2gL
-1ammonium oxalate solution, under 50～80 ℃ of water bath condition, heat;
(4) ammonium oxalate solution after heating is all added in mixed slurry, 50～80 ℃ of constant temperature stir 30～60min, then stop heating, continue to stir 30～60min, slip to be mixed be cooled to 25 ℃ following after successively after filtration, washing and dry, obtain super thick carbide alloy parcel powder presoma;
(5) be 1～4m by super thick carbide alloy parcel powder presoma in 450～600 ℃, hydrogen flowing quantity
3under the condition of/min, reduce 1～2.5h, obtain super thick carbide alloy parcel powder.
5. method as claimed in claim 4, is characterized in that, the described cobalt saline compound of step (1) is CoCl
26H
2o, CoSO
47H
2o or Co (NO
3)
26H
2o.
6. method as claimed in claim 4, is characterized in that, the described cobalt salt of step (1) is cobalt chloride, cobaltous sulfate or cobalt nitrate.
7. method as claimed in claim 4, is characterized in that, described being dried of step (4) is freeze-day with constant temperature 1～3h under 100～120 ℃ of conditions.
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| CN113857474A (en) * | 2021-09-01 | 2021-12-31 | 河海大学 | Preparation method of WC surface-coated Co powder added with Ce element |
| CN113774264A (en) * | 2021-09-16 | 2021-12-10 | 中交隧道工程局有限公司 | Preparation method of coarse-grain WC-Co-X hard alloy based on addition of ultrafine powder |
| CN113774264B (en) * | 2021-09-16 | 2022-08-26 | 中交隧道工程局有限公司 | Preparation method of coarse-grain WC-Co-X hard alloy based on adding superfine powder |
| CN114535588A (en) * | 2022-01-07 | 2022-05-27 | 中交隧道工程局有限公司 | Co/Ni Co-coated WC powder and preparation method thereof |
| CN115608984A (en) * | 2022-12-14 | 2023-01-17 | 矿冶科技集团有限公司 | Preparation method of mechanical mixed coating powder and coating powder |
| CN117385248A (en) * | 2023-10-17 | 2024-01-12 | 株洲金佰利硬质合金有限公司 | Ultra-coarse-grain WC-Co hard alloy and preparation method thereof |
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