CN102191421B - Ultrafine hard alloy with gradient structure and preparation process thereof - Google Patents
Ultrafine hard alloy with gradient structure and preparation process thereof Download PDFInfo
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Abstract
The invention discloses an ultrafine hard alloy with a gradient structure and a preparation process thereof. In the ultrafine hard alloy, one or more metal elements of Co, Ni and Fe serves as a binding phase, WC and a cubic-phase compound serve as a hard phase, wherein the cubic-phase compound is a carbide and/or carbonitride of transition metals Ti, Ta and Nb. The ultrafine hard alloy comprises the following components in percentage by weight: 4 to 12 percent of binding phase, 0.4 to 1.2 percent of cubic-phase compound and the balance of WC. The ultrafine hard alloy is provided with a surface layer gradient structure. The binding phase is accumulated in the surface layer gradient structure but the cubic-phase compound is not in the surface layer gradient structure nearly. The average particle size of the WC in the hard phase is 0.6 to 1.0 um and the average particle size of the cubic-phase compound is 0.5 to 1.5 times that of the WC. The preparation process comprises four steps, namely preparing raw materials, ball-milling and blending, pressing and molding, and sintering, wherein the step of sintering sequentially comprises three stages, namely sintering by raising the temperature, sintering by keeping the temperature, and sintering and cooling. The hard alloy prepared by the process has the advantages of high abrasion resistance, high strength of cutting edges, high plastic deformation resistance and the like.
Description
Technical field
The present invention relates to metal cutting and use the inserted tool field, relate in particular to a kind of wimet and preparation method thereof.
Background technology
Carbide chip is widely used in the metal cutting manufacture field, the carbide blade base that turning is used generally by mean particle size between the WC of 1 μ m～5 μ m, mean particle size between cube phase carbide of 1 μ m～5 μ m or the metal bonding phase composite of carbonitride and 5wt.%～15wt.%.The performance of wimet can be optimized through adjustment WC and grain graininess cube mutually, bond phase volume fraction and carbon content.Can improve wear resistance, hot hardness, oxidation-resistance and the corrosion resistance of wimet through adding a certain amount of cube of phase compound.Yet though cube phase compound hardness ratio WC is high, its fragility is also big, and therefore the intensity and the toughness of wimet can descend behind the adding cube phase compound.And cube phase compound assembles easily in sintering process and grows up, especially when wc grain size carefully the time gathering of cube phase compound grow up the performance of wimet is sharply descended.Therefore, in order to weaken cube phase compound to wimet intensity and flexible influence, turning generally is prepared into carbide blade base has the gradient-structure that the rich bonding in top layer does not have cube phase compound mutually.
In the patent documentation of relevant gradient hard alloy in early days (like US4548786A american documentation literature, US5484468A american documentation literature); Cube phase carbide content is generally all more than 5wt.%, and so high content can cause in the sintering process cube phase carbide to assemble to grow up and dissolving is separated out and grown up.The granularity of WC and cube phase carbide all more than 1 μ m, has therefore limited the range of application of wimet in the prior art; In addition, when cube phase carbide content is low, also have problems, the gradient layer thickness that mainly shows as sintering formation is too big, and is difficult in the thickness of control gradient layer under the situation that does not influence other performances of wimet.
Summary of the invention
The technical problem that the present invention will solve is the deficiency that overcomes prior art, and the ultra-fine cemented carbide of the gradient-structure that a kind of wear resistance is good, cutting edge strength is high, the plasticity_resistant deformation ability is strong is provided, the also corresponding preparation technology that a kind of this ultra-fine cemented carbide is provided.
For solving the problems of the technologies described above; The technical scheme that the present invention proposes is a kind of ultra-fine cemented carbide of gradient-structure; This ultra-fine cemented carbide is as the bonding phase with one or more metallic elements among Co, Ni, the Fe; With WC and compound cube mutually as the hard phase, said cube of carbide and/or the carbonitride that the phase compound is transition metal Ti, Ta, Nb, the content of said bonding phase is 4wt.%～12wt.%; The content of said cube of phase compound is 0.4wt.%～1.2wt.%, and all the other are mainly WC; Said ultra-fine cemented carbide is provided with the top layer gradient-structure; Be enriched with bonding in the gradient-structure of said top layer mutually but contain described cube of phase compound hardly, the Co average content in the gradient-structure of said top layer is 1～2 times of nominal Co content in the said ultra-fine cemented carbide; The said hard mean particle size of middle WC mutually is 0.6 μ m～1.0 μ m, and the mean particle size of said cube of phase compound is 0.5～1.5 times of WC.
In the ultra-fine cemented carbide of above-mentioned gradient-structure, said hard mutually in mean particle size 0.8 μ m～1.0 μ m more preferably of WC.
In the ultra-fine cemented carbide of above-mentioned gradient-structure, the granularity of said cube of phase compound is preferably 0.8～1.2 times of wc grain size.
In the ultra-fine cemented carbide of above-mentioned gradient-structure, the Co average content in the gradient-structure of said top layer is preferably 1～1.5 times of nominal Co content in the said ultra-fine cemented carbide.
In the ultra-fine cemented carbide of above-mentioned gradient-structure, the thickness of said top layer gradient-structure is preferably 10 μ m～50 μ m, most preferably is 10 μ m～30 μ m.
In the ultra-fine cemented carbide of above-mentioned gradient-structure; The content of said cube of phase compound is preferably 0.4wt.%～1.0wt.% (more preferably at 0.6wt.%～0.8wt.%), and the atomic ratio of Ti/ (Ti+Ta+Nb) (more preferably 0.4～0.6) between 0.3～0.8.
In the ultra-fine cemented carbide of above-mentioned gradient-structure, the atomic ratio of the N/Ti in the said ultra-fine cemented carbide is between 0.1～0.5 (more preferably 0.2～0.4) preferably.
As a total technical conceive; The present invention also provides a kind of preparation technology of ultra-fine cemented carbide of gradient-structure; Said preparation technology comprises preparation of raw material, ball mill mixing, compression moulding and four steps of sintering; Said sintering step comprises intensification sintering, heat preservation sintering and sintering cooling three phases successively, it is characterized in that:
Said intensification sintering is meant: the crude green body after the said compression moulding is placed under the vacuum environment; Sinter to 1100 ℃～1300 ℃ (preferably sintering to 1150 ℃～1250 ℃); (preferably be incubated 20min～40min) at this interval insulation of temperature control first 5min～60min; Continue to be warming up to 1340 ℃～1370 ℃ then, feed 20mbar～80mbar rare gas element again, under protection of inert gas, sinter to 1410 ℃～1450 ℃;
Said heat preservation sintering is meant: above-mentioned sinter to 1410 ℃～1450 ℃ temperature after, feed the nitrogen of 10mbar～100mbar, insulation 30min～90min;
Said sintering cooling is meant: after the above-mentioned heat preservation sintering stage finishes; Under original nitrogen atmosphere, be cooled to the cooling warm area of 1300 ℃～1100 ℃ (preferred 1250 ℃～1200 ℃) earlier; Under hydrogen atmosphere, be cooled to room temperature at last, obtain the ultra-fine cemented carbide of gradient-structure.
Compared with prior art, the invention has the advantages that:
At first; The inventive method can be prepared a kind of ultra-fine cemented carbide of gradient-structure; This ultra-fine cemented carbide has ultra fine grain size; Cutting tool with its preparation possesses higher wear resistance, cutting edge strength and high temperature resistance plastic deformation ability, is suitable as very much the basic material of stainless steel, superalloy and cast iron finishing tool;
Secondly, ultra-fine cemented carbide of the present invention has the top layer gradient-structure that rich bonding does not have cube phase mutually, and this makes cutting tool have good cutting edge strength and shock resistance;
Once more, sintering process of the present invention can improve the toughness of ultra-fine cemented carbide, passes through N simultaneously
2Atmosphere can accurately be controlled top layer gradient-structure thickness.
Description of drawings
Fig. 1 is the electron photomicrograph of the ultra-fine cemented carbide of gradient-structure in the embodiment of the invention 2, and the scribe area of the white among Fig. 1 is represented top layer gradient-structure tissue, and atrament wherein is the bonding phase, and white mass is WC, and grey matter is a cube phase compound.
Fig. 2 is the local amplification electron Photomicrograph of the following core of Fig. 1 mesexine gradient-structure tissue, and atrament wherein is the bonding phase, and white mass is WC, and grey matter is a cube phase compound.
Embodiment
Below in conjunction with specific embodiment the present invention is further described.
Embodiment 1:
A kind of ultra-fine cemented carbide of gradient-structure of the present invention; This ultra-fine cemented carbide is as the bonding phase with metal Co; With WC and compound cube mutually as the hard phase; This cube phase compound comprises TiCN, TiC, TaNbC (sosoloid that TaC and NbC form), and wherein the atomic ratio of Ti/ (Ti+Ta+Nb) is 0.46; The content of bonding phase Co is 6wt.%; The content of cube phase compound is 0.9wt.% (comprising the TaC of 0.5wt.%, the NbC of 0.2wt.% and the TiC of 0.2wt.%); Also comprise the N (atomic ratio of N/Ti is 0.34 in the present embodiment) of 0.02wt.% in the ultra-fine cemented carbide, all the other are mainly WC.The hard mean particle size of middle WC mutually is 0.8 μ m, and the mean particle size of cube phase compound TiCN and TiC is 1.0 μ m, and the granularity of cube phase compound TaNbC is 1.2 μ m, and the mean particle size of metal Co is 1.5 μ m.This ultra-fine cemented carbide is provided with the thick top layer gradient-structure of 25 μ m, is enriched with bonding in the gradient-structure of top layer mutually but contain a cube phase compound hardly, and the Co average content that is arranged in the top layer gradient-structure is 1.2 times of said ultra-fine cemented carbide nominal Co content.
The ultra-fine cemented carbide of the gradient-structure of present embodiment is to prepare through following steps:
At first, prepare mixing raw material powder (raw material powder comprises Co powder, TiCN, TiC, TaNbC and WC, and the concrete proportioning of raw material can be confirmed according to the routine techniques means by those skilled in the art) in proportion; Mixed raw material powder obtains the blade crude green body through ball mill mixing, compression moulding; Then crude green body is carried out sintering, sintering step comprises intensification sintering, heat preservation sintering and sintering cooling three phases successively: earlier the crude green body after the compression moulding is placed under the vacuum environment, sinter to 1200 ℃; Under this temperature, be incubated 30min; Continue to be warming up to 1350 ℃ then, feed the 40mbar argon gas again, under argon shield, sinter to 1410 ℃; Under 1410 ℃ of temperature, begin insulation, holding stage begins to feed 40mbar nitrogen, keeps the sintering furnace atmosphere to be cooled to 1200 behind the insulation 60min
oC, cool to room temperature under hydrogen atmosphere subsequently obtains the ultra-fine cemented carbide of gradient-structure.
Embodiment 2:
A kind of ultra-fine cemented carbide of gradient-structure of the present invention as depicted in figs. 1 and 2, this ultra-fine cemented carbide be with metal Co as the bonding phase, with cube compound is as the hard phase mutually, this cube phase compound comprises TiCN and TiC with WC; The content of bonding phase Co is 6wt.%, and the content of cube phase compound is 0.6wt.%, also comprises the N (atomic ratio of N/Ti is 0.3 in the present embodiment) of 0.02wt.% in the ultra-fine cemented carbide, and all the other are mainly WC.The hard mean particle size of middle WC mutually is 0.8 μ m, and the mean particle size of cube phase compound TiCN and TiC is 1.0 μ m, and the mean particle size of metal Co is 1.5 μ m.This ultra-fine cemented carbide is provided with the thick top layer gradient-structure of 36.24 μ m; Be enriched with bonding in the gradient-structure of top layer mutually but contain a cube phase compound hardly, the Co average content that is arranged in the top layer gradient-structure is 1.2 times of said ultra-fine cemented carbide nominal Co content.
The ultra-fine cemented carbide of the gradient-structure of present embodiment is to prepare through following steps:
At first, prepare mixing raw material powder (raw material powder comprises Co powder, TiCN, TiC and WC, and the concrete proportioning of raw material can be confirmed according to the routine techniques means by those skilled in the art) in proportion; Mixed raw material powder obtains the blade crude green body through ball mill mixing, compression moulding; Then crude green body is carried out sintering, sintering step comprises intensification sintering, heat preservation sintering and sintering cooling three phases successively: earlier the crude green body after the compression moulding is placed under the vacuum environment, sinter to 1200 ℃; Under this temperature, be incubated 30min; Continue to be warming up to 1350 ℃ then, feed the 40mbar argon gas again, under argon shield, sinter to 1410 ℃; Under 1410 ℃ of temperature, begin insulation, holding stage begins to feed 50mbar nitrogen, keeps the sintering furnace atmosphere to be cooled to 1200 ℃ behind the insulation 60min, and cool to room temperature under hydrogen atmosphere subsequently obtains the ultra-fine cemented carbide of gradient-structure.
Embodiment 3:
A kind of ultra-fine cemented carbide of gradient-structure of the present invention, this ultra-fine cemented carbide be with metal Co as the bonding phase, with cube compound is as the hard phase mutually, this cube phase compound comprises TiCN and TiC with WC; The content of bonding phase Co is 6wt.%, and the content of cube phase compound is 0.6wt.%, also comprises the N (atomic ratio of N/Ti is 0.45 in the present embodiment) of 0.08wt.% in the ultra-fine cemented carbide, and all the other are mainly WC.The hard mean particle size of middle WC mutually is 0.6 μ m, and the mean particle size of cube phase compound TiCN and TiC is 0.8 μ m, and the mean particle size of metal Co is 1.5 μ m.This ultra-fine cemented carbide is provided with the thick top layer gradient-structure of 40 μ m, is enriched with bonding in the gradient-structure of top layer mutually but contain a cube phase compound hardly, and the Co average content that is arranged in the top layer gradient-structure is 1.15 times of said ultra-fine cemented carbide nominal Co content.
The ultra-fine cemented carbide of the gradient-structure of present embodiment is to prepare through following steps:
At first, prepare mixing raw material powder (raw material powder comprises Co powder, TiCN, TiC and WC, and the concrete proportioning of raw material can be confirmed according to the routine techniques means by those skilled in the art) in proportion; Mixed raw material powder obtains the blade crude green body through ball mill mixing, compression moulding; Then crude green body is carried out sintering, sintering step comprises intensification sintering, heat preservation sintering and sintering cooling three phases successively: earlier the crude green body after the compression moulding is placed under the vacuum environment, sinter to 1250 ℃; Under this temperature, be incubated 20min; Continue to be warming up to 1350 ℃ then, feed the 40mbar argon gas again, under argon shield, sinter to 1410 ℃; Under 1410 ℃ of temperature, begin insulation, holding stage begins to feed 60mbar nitrogen, keeps the sintering furnace atmosphere to be cooled to 1200 ℃ behind the insulation 60min, and cool to room temperature under hydrogen atmosphere subsequently obtains the ultra-fine cemented carbide of gradient-structure.
Comparative Examples 1:
A kind of thin carbide blade base, its composition comprises: N and the WC of the Nb of the Co of 6wt.%, the Ta of 0.5wt.%, 0.2wt.%, the Ti of 0.2wt.%, 0.08wt.%.The preparation raw material of this thin carbide blade base is WC, TiCN+TiC, TaNbC and Co powder, and granularity is respectively 0.8 μ m, 1.0 μ m, 1.2 μ m and 1.5 μ m; Prepare mixed powder in proportion, be pressed into the blade crude green body, sinter wimet into according to existing common sintering process then through behind the ball milling.
Comparative Examples 2:
A kind of thin carbide blade base, its composition comprises: N and the WC of the Co of 6wt.%, the Ti of 0.6wt.%, 0.08wt.%.The preparation raw material of this thin carbide blade base is WC, TiCN+TiC and Co powder, and granularity is respectively 0.8 μ m, 1.0 μ m and 1.5 μ m; Prepare mixed powder in proportion, be pressed into the blade crude green body, sinter wimet into according to existing common sintering process then through behind the ball milling.
Comparative Examples 3:
A kind of thin carbide blade base, its composition comprises: N and the WC of the Nb of the Co of 6wt.%, the Ta of 3wt.%, 2wt.%, the Ti of 2wt.%, 0.1wt.%.The preparation raw material of this thin carbide blade base is WC, TiCN+TiC, TaNbC and Co powder, and granularity is respectively 2.5 μ m, 2.0 μ m, 1.5 μ m and 1.5 μ m; Prepare mixed powder in proportion, be pressed into the blade crude green body, sinter wimet into according to existing sintering process then through behind the ball milling.
Respectively the mechanical property of the carbide blade base of the foregoing description 1～3 and Comparative Examples 1～3 is tested, measures 5 data at least for every group, get its MV, test result such as following table 1:
Table 1: carbide blade base Mechanics Performance Testing result
| Numbering | Bending strength (MPa) | Microhardness (MPa) | Fracture toughness property (MPam 1/2） | Gradient thickness (μ m) |
| Embodiment 1 | 2430 | 1780 | 9.8 | 25 |
| Embodiment 2 | 2580 | 1740 | 9.9 | 36.24 |
| Embodiment 3 | 2640 | 1780 | 10.2 | 40 |
| Comparative Examples 1 | 2100 | 1750 | 9.5 | 60 |
| Comparative Examples 2 | 2230 | 1740 | 9.4 | 65 |
| Comparative Examples 3 | 2250 | 1600 | 10.1 | 10 |
Visible by last table 1, the bending strength of carbide blade base of the present invention has improved 10%～20%, and microhardness and fracture toughness property all have the raising of certain amplitude simultaneously.In addition, can adjust the thickness of wimet top layer gradient-structure easily according to method of the present invention, the scope of adjustment can reach 10 μ m～80 μ m.
Claims (8)
1. the ultra-fine cemented carbide of a gradient-structure; This ultra-fine cemented carbide is as the bonding phase with one or more metallic elements among Co, Ni, the Fe; With WC and compound cube mutually as the hard phase, said cube of carbide and/or the carbonitride that the phase compound is transition metal Ti, Ta, Nb, the content of said bonding phase is 4wt.%～12wt.%; The content of said cube of phase compound is 0.4wt.%～1.2wt.%, and all the other are mainly WC; It is characterized in that: said ultra-fine cemented carbide is provided with the top layer gradient-structure; Be enriched with bonding in the gradient-structure of said top layer mutually but contain described cube of phase compound hardly, the Co average content in the gradient-structure of said top layer is 1～2 times of nominal Co content in the said ultra-fine cemented carbide; The said hard mean particle size of middle WC mutually is 0.6 μ m～1.0 μ m, and the mean particle size of said cube of phase compound is 0.5～1.5 times of WC; The thickness of said top layer gradient-structure is 10 μ m～50 μ m; The atomic ratio of Ti/ (Ti+Ta+Nb) is between 0.3～0.8 in said cube of phase compound; The atomic ratio of N/Ti in the said ultra-fine cemented carbide is between 0.1～0.5.
2. the ultra-fine cemented carbide of gradient-structure according to claim 1 is characterized in that: said hard mutually in the mean particle size of WC be 0.8 μ m～1.0 μ m.
3. the ultra-fine cemented carbide of gradient-structure according to claim 1, it is characterized in that: the granularity of said cube of phase compound is 0.8～1.2 times of wc grain size.
4. the ultra-fine cemented carbide of gradient-structure according to claim 1 is characterized in that: the Co average content in the gradient-structure of said top layer is 1～1.5 times of nominal Co content in the said ultra-fine cemented carbide.
5. the ultra-fine cemented carbide of gradient-structure according to claim 1, it is characterized in that: the content of said cube of phase compound is 0.4wt.%～1.0wt.%.
6. preparation technology like the ultra-fine cemented carbide of each described gradient-structure in the claim 1～5; Said preparation technology comprises preparation of raw material, ball mill mixing, compression moulding and four steps of sintering; Said sintering step comprises intensification sintering, heat preservation sintering and sintering cooling three phases successively, it is characterized in that:
Said intensification sintering is meant: the crude green body after the said compression moulding is placed under the vacuum environment; Sinter to 1100 ℃～1300 ℃; At this interval insulation of temperature control first 5min～60min; Continue to be warming up to 1340 ℃～1370 ℃ then, feed 20mbar～80mbar argon gas again, under argon shield, sinter to 1410 ℃～1450 ℃;
Said heat preservation sintering is meant: above-mentioned sinter to 1410 ℃～1450 ℃ temperature after, feed the nitrogen of 10mbar～100mbar, insulation 30min～90min;
Said sintering cooling is meant: after the above-mentioned heat preservation sintering stage finishes, under original nitrogen atmosphere, be cooled to 1300 ℃～1100 ℃ cooling warm area earlier, under hydrogen atmosphere, be cooled to room temperature at last.
7. the preparation technology of the ultra-fine cemented carbide of gradient-structure according to claim 6; It is characterized in that: in the said intensification sintering stage; Said temperature control first interval is controlled at 1150 ℃～1250 ℃, this first the interval soaking time of temperature control be 20min～40min.
8. according to the preparation technology of the ultra-fine cemented carbide of claim 6 or 7 described gradient-structures, it is characterized in that: at said sintering colling stages, said cooling warm area is controlled at 1250 ℃～1200 ℃.
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| CN105950937B (en) * | 2016-05-23 | 2018-01-16 | 株洲钻石切削刀具股份有限公司 | A kind of carbide chip and preparation method thereof |
| CN106001561B (en) * | 2016-06-03 | 2018-10-23 | 广东工业大学 | A kind of multistage composite cermet, preparation method and shield cutter |
| CN106048360B (en) * | 2016-07-11 | 2018-03-27 | 中南大学 | A kind of surface has hard alloy of double-deck gradient-structure and preparation method thereof |
| CN108085556A (en) * | 2017-12-21 | 2018-05-29 | 洛阳名力科技开发有限公司 | A kind of preparation method of WC-Fe-Ni-Co hard alloy |
| CN112251658B (en) * | 2020-10-22 | 2021-11-26 | 常州润睿特种合金有限公司 | Ultrafine grain gradient hard alloy and preparation method and application method thereof |
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