CN109161772A - The preparation method of ultra-fine cemented carbide - Google Patents
The preparation method of ultra-fine cemented carbide Download PDFInfo
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- CN109161772A CN109161772A CN201811050920.9A CN201811050920A CN109161772A CN 109161772 A CN109161772 A CN 109161772A CN 201811050920 A CN201811050920 A CN 201811050920A CN 109161772 A CN109161772 A CN 109161772A
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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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- 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
Abstract
The present invention relates to a kind of preparation methods of ultra-fine cemented carbide, comprising the following steps: chromium carbide, vanadium carbide, tantalum carbide and wet grinding media are added in wet milk pre- wet-milling 30~60 minutes；Tungsten carbide powder, cobalt powder, forming agent, dispersing agent and the wet grinding media that granularity is 1.3~1.6 microns are added in wet milk and carry out Wet blend-milling；And the mixed slurry obtained after the completion of wet-milling is spray-dried, is pressed and molded, is sintered to obtain ultra-fine cemented carbide.The preparation method of ultra-fine cemented carbide of the invention is practical, it is easy to accomplish industrialized production can significantly improve the profit margin of ultra-fine cemented carbide production.
Description
Technical field
The present invention relates to CEMENTED CARBIDE PRODUCTION technical field more particularly to a kind of preparation methods of ultra-fine cemented carbide.
Background technique
During CEMENTED CARBIDE PRODUCTION, the sight that main material original particle size and alloy product grain size match is followed mostly
It reads, such as production grain size is 0.8 micron of tungsten-cobalt series hard alloy, just uses granularity for 0.8 micron of tungsten carbide powder conduct
Raw material.
Ultra-fine cemented carbide refers to hard alloy of the grain size between 0.5~0.2 micron, in the prior art, Chang Cai
It is prepared with the tungsten carbide powder that granularity is 0.5~0.2 micron.However, the tungsten carbide powder large specific surface area under the granularity, exist with
Lower problem: it is easy to reunite when wet-milling, cause mixing uniformity poor；Active force is big between powder when compression molding, and press power is caused to become
Greatly, the defects of mold is easily damaged, and green compact is also easy to produce layering, crackle；Oxidizable in production process, control carbon difficulty increases；At
It needs to add more forming agents during type, causes the difficulty of sintering removing forming agent to increase, the time is elongated；The small carbon of granularity
It is relatively high to change tungsten powder price.
Summary of the invention
The present invention, which provides one kind, can overcome the above problem, and particle tungsten carbide powder prepares the super of ultra-fine cemented carbide in
The preparation method of thin hard alloy.
The present invention provides a kind of preparation method of ultra-fine cemented carbide, comprising the following steps:
Chromium carbide, vanadium carbide, tantalum carbide and wet grinding media are added in wet milk pre- wet-milling 30~60 minutes；
Tungsten carbide powder, cobalt powder, forming agent, dispersing agent and the wet grinding media that granularity is 1.3~1.6 microns are added wet
Wet blend-milling is carried out in grinding machine；And
The mixed slurry obtained after the completion of wet-milling is spray-dried, is pressed and molded, is sintered to obtain ultra-fine hard and close
Gold.
The preparation method of ultra-fine cemented carbide provided by the invention, compression moulding smaller using specific surface area, easy and cost
Lower middle particle tungsten carbide powder, by reasonable preparation chromium carbide, vanadium carbide, tantalum carbide additional amount and adjust wet-grinding technology and relative device,
Prepare the ultra-fine cemented carbide that grain size is 0.5 μm or so.The preparation method of the ultra-fine cemented carbide is practical, is easy to real
Existing industrialized production, can significantly improve the profit margin of ultra-fine cemented carbide production.
Detailed description of the invention
Fig. 1 is the metallographic deep etch micro-structure diagram for the hard alloy bar that embodiment 1 obtains in the present invention.
Fig. 2 is the metallographic deep etch micro-structure diagram for the hard alloy bar that comparative example 1 obtains in the present invention.
Fig. 3 is the metallographic deep etch micro-structure diagram for the hard alloy bar that embodiment 2 obtains in the present invention.
Fig. 4 is the metallographic deep etch micro-structure diagram for the hard alloy bar that comparative example 2 obtains in the present invention.
Fig. 5 is the metallographic deep etch micro-structure diagram for the hard alloy bar that embodiment 3 obtains in the present invention.
Fig. 6 is the metallographic deep etch micro-structure diagram for the hard alloy bar that embodiment 4 obtains in the present invention.
Fig. 7 is the metallographic deep etch micro-structure diagram for the hard alloy bar that comparative example 3 obtains in the present invention.
Specific embodiment
The present invention provides a kind of preparation method of ultra-fine cemented carbide, use in particle tungsten carbide powder prepared for raw material it is brilliant
Granularity is the ultra-fine cemented carbide of 0.5 microns.Specifically, the preparation method of the ultra-fine cemented carbide mainly includes following step
It is rapid:
Chromium carbide, vanadium carbide, tantalum carbide and wet grinding media are added in wet milk pre- wet-milling 30~60 minutes；
Wet milk is added in tungsten carbide powder, cobalt powder, forming agent, dispersing agent and wet grinding media that granularity is 1.3~1.6 microns
Middle carry out Wet blend-milling；And
The mixed slurry obtained after the completion of wet-milling is spray-dried, is pressed and molded, is sintered to obtain ultra-fine hard and close
Gold.
Further, the additional amount of chromium carbide is the 0.5~1.0% of tungsten carbide powder and cobalt powder gross mass.Vanadium carbide adds
Enter 0.4~0.6% that amount is tungsten carbide powder and cobalt powder gross mass.The additional amount of tantalum carbide is tungsten carbide powder and cobalt powder gross mass
0.6~1.0%.Cobalt powder accounts for the 6~12% of tungsten carbide powder and cobalt powder gross mass.
It should be noted that chromium carbide, vanadium carbide and tantalum carbide have the function of that crystal grain is inhibited to grow up, thus as addition
Agent is mixed during wet-milling with tungsten carbide powder and cobalt powder.However the particle of commercially available such additives is thicker, partial size is general
All at 2~3 microns, direct addition is unfavorable for it and is dispersed in tungsten carbide powder and cobalt powder.
In the preparation method of ultra-fine cemented carbide provided by the invention, chromium carbide, vanadium carbide and tantalum carbide are first added wet
Pre- wet-milling certain time in grinding machine not only makes its particle carry out physical thinning, additionally it is possible to it be made to be dispersed in the table of mill ball
Face can preferably be dispersed in tungsten carbide powder and cobalt powder, more have then when carrying out Wet blend-milling with tungsten carbide powder and cobalt powder
The effect that it inhibits crystal grain to grow up conducive to performance.
Further, wet grinding media is any one of alcohol, hexane, heptane, acetone and gasoline.Forming agent be paraffin,
Any one of ethyl cellulose and polyethylene glycol.Dispersing agent is oleic acid or soybean amine.
Embodiment 1
The chromium carbide of 0.5 mass parts, the vanadium carbide of 0.4 mass parts, the tantalum carbide of 0.6 mass parts and alcohol are added first
Pre- wet-milling 60 minutes in wet milk；It then is 1.3 microns of tungsten carbide powder by the granularity of 92 mass parts, cobalt powder, the stone of 8 mass parts
Wax, oleic acid and alcohol are added in wet milk and carry out Wet blend-milling 48 hours；Finally by the mixed slurry obtained after the completion of wet-milling into
Row spray drying, compression molding are that specification is the rodlike of D4 × 75, sintering to obtain hard alloy bar.
Comparative example 1
Comparative example 1 and the preparation method of embodiment 1 are almost the same, the difference is that: the granularity of tungsten carbide powder is 0.4
Micron；Do not need pre- wet-grinding technology and relative device, directly by the chromium carbide of 0.4 mass parts, the vanadium carbide of 0.35 mass parts, 92 mass parts grain
Degree is 0.4 micron of tungsten carbide powder, cobalt powder, paraffin, oleic acid and the alcohol of 8 mass parts are added in wet milk and carry out Wet blend-milling 48
Hour obtains mixed slurry.
It should be noted that the technological parameter of spray drying, compression molding and sintering in embodiment 1 and comparative example 1
It is roughly the same.
The hard alloy bar that embodiment 1 and comparative example 1 obtain is tested for the property, microstructure is observed and measures crystal grain
Size, as a result as shown in table 1, Fig. 1 and Fig. 2.Wherein, table 1 is the hard of the hard alloy bar that embodiment 1, comparative example 1 obtain respectively
Degree, bending strength and grain size test/measurement result, Fig. 1 are that the metallographic deep etch for the hard alloy bar that embodiment 1 obtains is aobvious
Micro-structure figure, Fig. 2 are the metallographic deep etch micro-structure diagram for the hard alloy bar that comparative example 1 obtains.
The performance test results for the hard alloy bar that 1 embodiment 1 of table is obtained with comparative example 1
| Hardness (HV30) | Bending strength (Mpa) | Grain size (μm) | |
| Embodiment 1 | 1810 | 4300 | 0.5 |
| Comparative example 1 | 1850 | 4000 | 0.47 |
According to table 1, Fig. 1 and Fig. 2 it is found that the hard alloy bar that embodiment 1 and comparative example 1 obtain has similar hardness, resists
Curved intensity and grain size.The above results show to use in particle (granularity is 1.3 micron) tungsten carbide powder, by being added and closing
Reason configuration chromium carbide, vanadium carbide, tantalum carbide can obtain the hard that grain size is 0.5 microns to inhibit crystal grain to grow up
Alloy bar, and the hard alloy bar of the tungsten carbide powder preparation of particle and use ultra-fine grain in using (granularity is 0.4 micron)
Tungsten carbide powder preparation hard alloy bar similar performance, meet the standard of current same specification product.
Embodiment 2
The chromium carbide of 1.0 mass parts, the vanadium carbide of 0.6 mass parts, the tantalum carbide of 1.0 mass parts and alcohol are added first
Pre- wet-milling 60 minutes in wet milk；Then by the granularity of 88 mass parts be 1.6 microns tungsten carbide powder, 12 mass parts cobalt powder,
Paraffin, oleic acid and alcohol are added in wet milk and carry out Wet blend-milling 72 hours；The mixed slurry that will finally be obtained after the completion of wet-milling
Being spray-dried, being pressed and molded as specification is the rodlike of D4 × 75, sintering to obtain hard alloy bar.
Comparative example 2
Comparative example 2 and the preparation method of embodiment 2 are almost the same, the difference is that: the granularity of tungsten carbide powder is 0.4
Micron；Do not need pre- wet-grinding technology and relative device, directly by the chromium carbide of 0.4 mass parts, the vanadium carbide of 0.35 mass parts, 88 mass parts grain
Degree is 0.4 micron of tungsten carbide powder, cobalt powder, paraffin, oleic acid and the alcohol of 12 mass parts are added in wet milk and carry out Wet blend-milling
72 hours acquisition mixed slurries.
It should be noted that the technological parameter of spray drying, compression molding and sintering in embodiment 2 and comparative example 2
It is roughly the same.
The hard alloy bar that embodiment 2 and comparative example 2 obtain is tested for the property, microstructure is observed and measures crystal grain
Size, as a result as shown in table 2, Fig. 3 and Fig. 4.Wherein, table 2 is the hard of the hard alloy bar that embodiment 2, comparative example 2 obtain respectively
Degree, bending strength and grain size measurement/measurement result, Fig. 3 are that the metallographic deep etch for the hard alloy bar that embodiment 2 obtains is aobvious
Micro-structure figure, Fig. 4 are the metallographic deep etch micro-structure diagram for the hard alloy bar that comparative example 2 obtains.
The performance test results for the hard alloy bar that 2 embodiment 2 of table is obtained with comparative example 2
| Hardness (HV30) | Bending strength (Mpa) | Grain size (μm) | |
| Embodiment 1 | 1700 | 4100 | 0.5 |
| Comparative example 1 | 1710 | 4000 | 0.5 |
According to table 2, Fig. 3 and Fig. 4 it is found that the hard alloy bar that embodiment 2 and comparative example 2 obtain has similar hardness, resists
Curved intensity and grain size.The above results also indicate that use in particle (granularity is 1.6 micron) tungsten carbide powder, by be added simultaneously
To inhibit crystal grain to grow up, can obtain grain size is the hard of 0.5 microns for reasonable disposition chromium carbide, vanadium carbide, tantalum carbide
Matter alloy bar, and (granularity is micro- for 0.4 with ultra-fine grain is used for the hard alloy bar of the tungsten carbide powder preparation of particle in using
Rice) tungsten carbide powder preparation hard alloy bar similar performance, meet the standard of current same specification product.
Embodiment 3
The chromium carbide of 1.0 mass parts, the vanadium carbide of 0.5 mass parts, the tantalum carbide of 0.7 mass parts and alcohol are added first
Pre- wet-milling 60 minutes in wet milk；Then by the granularity of 90 mass parts be 1.4 microns tungsten carbide powder, 10 mass parts cobalt powder,
Paraffin, oleic acid and alcohol are added in wet milk and carry out Wet blend-milling 72 hours；The mixed slurry that will finally be obtained after the completion of wet-milling
Being spray-dried, being pressed and molded as specification is the rodlike of D4 × 75, sintering to obtain hard alloy bar.
Embodiment 4
Embodiment 4 and the preparation method of embodiment 3 are almost the same, the difference is that: chromium carbide, vanadium carbide and carbonization
The time consuming of prewetting of tantalum is 30 minutes.
Comparative example 3
Comparative example 3 and the preparation method of embodiment 3 are almost the same, the difference is that: chromium carbide, vanadium carbide, carbonization
Tantalum directly carries out Wet blend-milling 72 hours with tungsten carbide powder, cobalt powder, paraffin, oleic acid and alcohol without pre- wet-milling.
It should be noted that the work of embodiment 3, embodiment 4 and spray drying, compression molding and sintering in comparative example 3
Skill parameter is also roughly the same.
Embodiment 3, embodiment 4 and the hard alloy bar obtained with comparative example 3 are tested for the property, observe microstructure
And grain size is measured, as a result as shown in table 3, Fig. 5, Fig. 6 and Fig. 7.Wherein, table 3 is embodiment 3, embodiment 4 and comparative example 3
Hardness, bending strength and the grain size measurement/measurement result of the hard alloy bar obtained respectively, Fig. 5 are what embodiment 3 obtained
The metallographic deep etch micro-structure diagram of hard alloy bar, Fig. 6 are that the metallographic deep etch for the hard alloy bar that embodiment 4 obtains is micro-
Structure chart, Fig. 7 are the metallographic deep etch micro-structure diagram for the hard alloy bar that comparative example 3 obtains.
The performance test results for the hard alloy bar that 3 embodiment 3~4 of table is obtained with comparative example 3
| Hardness (HV30) | Bending strength (Mpa) | Grain size (μm) | |
| Embodiment 3 | 1760 | 4100 | 0.5 |
| Embodiment 4 | 1740 | 4200 | 0.5 |
| Comparative example 3 | 1700 | 4000 | 0.58 |
According to table 3, Fig. 5 to Fig. 7 it is found that compared with comparative example 3, the hard alloy bar of embodiment 3 and the acquisition of embodiment 4
Hardness and bending strength are more preferable, and crystal grain is smaller.The above results show wet-milling in the process first by chromium carbide, vanadium carbide, tantalum carbide
It carries out 30~60 minutes crystal grain for being conducive to further decrease hard alloy bar of pre- wet-milling and improves its performance.
The above is only embodiments of the present invention, are not intended to limit the scope of the invention, all to utilize the present invention
Equivalent structure or equivalent flow shift made by specification and accompanying drawing content is applied directly or indirectly in other relevant technologies
Field is included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of ultra-fine cemented carbide, it is characterised in that: the following steps are included:
Chromium carbide, vanadium carbide, tantalum carbide and wet grinding media are added in wet milk pre- wet-milling 30~60 minutes；
Wet milk is added in tungsten carbide powder, cobalt powder, forming agent, dispersing agent and the wet grinding media that granularity is 1.3~1.6 microns
Middle carry out Wet blend-milling；And
The mixed slurry obtained after the completion of wet-milling is spray-dried, is pressed and molded, is sintered to obtain ultra-fine cemented carbide.
2. preparation method as described in claim 1, it is characterised in that: the additional amount of the chromium carbide be the tungsten carbide powder with
The 0.5~1.0% of the cobalt powder gross mass.
3. preparation method as described in claim 1, it is characterised in that: the additional amount of the vanadium carbide be the tungsten carbide powder with
The 0.4~0.6% of the cobalt powder gross mass.
4. preparation method as described in claim 1, it is characterised in that: the additional amount of the tantalum carbide be the tungsten carbide powder with
The 0.6~1.0% of the cobalt powder gross mass.
5. preparation method as described in claim 1, it is characterised in that: the cobalt powder accounts for the tungsten carbide powder and the cobalt powder is total
The 6~12% of quality.
6. preparation method as described in claim 1, it is characterised in that: the wet grinding media is alcohol, hexane, heptane, acetone
And any one of gasoline.
7. preparation method as described in claim 1, it is characterised in that: the forming agent is paraffin, ethyl cellulose and poly- second
Any one of glycol.
8. preparation method as described in claim 1, it is characterised in that: the dispersing agent is oleic acid or soybean amine.
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| CN112921198A (en) * | 2021-01-08 | 2021-06-08 | 晋城鸿刃科技有限公司 | Preparation method of ultra-coarse grain hard alloy |
| CN112935241A (en) * | 2021-01-23 | 2021-06-11 | 晋城鸿刃科技有限公司 | Molding agent and molding method of hard alloy |
| CN114855018A (en) * | 2022-04-28 | 2022-08-05 | 晋城鸿智纳米光机电研究院有限公司 | Preparation method of nano hard alloy |
| CN115044795A (en) * | 2022-06-21 | 2022-09-13 | 株洲硬质合金集团有限公司 | Nano WC-Co hard alloy and preparation method thereof |
| CN115287487A (en) * | 2022-04-28 | 2022-11-04 | 晋城鸿智纳米光机电研究院有限公司 | Preparation method of nano hard alloy |
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