CN111850370B - Preparation method of coarse-grain WC-Co hard alloy - Google Patents
Preparation method of coarse-grain WC-Co hard alloy Download PDFInfo
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- 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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- 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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- 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
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/52—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50
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Abstract
The invention discloses a preparation method of a coarse-grain WC-Co hard alloy, which comprises the following steps: (1) pretreating WC powder; (2) preparing an activating solution, and then activating the WC powder; (3) filtering, drying and activating the WC powder, and performing heat treatment reduction to obtain WC activated powder with metal Co particles attached to the surface; (4) preparing a plating solution; (5) placing WC activated powder, C powder and W powder with metal Co particles attached to the surfaces in a plating solution for chemical plating, filtering, cleaning and vacuum drying to obtain WC/C/W/Co coarse-crystal composite powder; (6) adding the WC/C/W/Co coarse crystal composite powder into a forming agent, pressing into a blank, and sintering into the WC-Co hard alloy. The method prepares the coarse-grain WC-Co hard alloy with the grain size of more than 2 mu m by in-situ reaction sintering, and the grain size, the hardness, the transverse rupture strength and the impact toughness of the coarse-grain WC-Co hard alloy are excellent.
Description
Technical Field
The invention relates to a preparation method of hard alloy; more particularly, relates to a preparation method of a coarse-grain WC-Co hard alloy.
Background
The hard alloy is a composite material with high hardness, high wear resistance, excellent red hardness, excellent heat stability, excellent corrosion resistance, high strength and excellent toughness. Among them, the macrocrystalline WC-Co cemented carbide has excellent hardness, wear resistance and high toughness, and is widely applied to the fields of ground mining tools, tunnel boring cutters and the like. The preparation of the coarse-grain WC-Co hard alloy is characterized in that WC powder with the average grain size of more than 20mm is usually prepared into WC/Co composite powder with the grain size meeting and uniform dispersion by a wet milling method with moderate ball milling strength, however, the grain size of WC particles is difficult to control during ball milling, so that the distribution of WC particles in the fired alloy is lower than or exceeds the range of 2-5 mm coarse-grain standard, and finally, only the WC-Co hard alloy with broad-peak grain distribution is obtained, and the strength and toughness of the broad-peak coarse-grain WC-Co hard alloy are lower than those of the narrow-peak distribution alloy when the grain sizes are the same. In addition, the composite powder with high uniformity obtained by ball milling brings higher residual stress to WC particles, which is also not beneficial to the improvement of alloy performance.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a preparation method for preparing a coarse-grain WC-Co hard alloy with narrow peak distribution, good hardness, good transverse rupture strength and good impact toughness.
The technical scheme is as follows: the preparation method of the coarse-grain WC-Co hard alloy comprises the following steps:
(1) performing ball milling on the coarse WC powder, cleaning, and drying in vacuum to obtain pretreated WC powder;
(2) adding CoSO4·7H2O and NaH2PO2·7H2Dissolving O in the solution to prepare an activation solution, and adding the WC powder treated in the step (1) into the activation solution for activation;
(3) filtering, drying and activating the WC powder, and performing heat treatment reduction to obtain WC activated powder with metal Co particles attached to the surface;
(4) adding CoSO4·7H2O and Na2C6H5O7·2H2Dissolving O in water, complexing, and sequentially adding H3BO3And NaH2PO2·7H2O is prepared into plating solution;
(5) placing WC activated powder, C powder and W powder with metal Co particles attached to the surfaces in a plating solution, stirring in a water bath, adjusting the pH value of the plating solution to 10-12, carrying out chemical plating at 70-90 ℃, filtering, cleaning and drying in vacuum to obtain WC/C/W/Co coarse-grain composite powder;
(6) adding the WC/C/W/Co coarse crystal composite powder into a forming agent, pressing into a blank, and sintering into the WC-Co hard alloy.
In the step 1, alloy balls with the diameter of 10-13 mm are adopted for ball milling, and the ball-to-material ratio is 1-3: 1; CoSO in activating solution in step 24·7H2O and Na2C6H5O7·2H2The O concentration is 50-60 g/L respectively, and the volume ratio is 1: 1-2, wherein the activation temperature is 50-60 ℃, and the activation time is 20-30 min; in the step 3, the heat treatment temperature is 300-400 ℃, and the time is 2-3 h; CoSO in step 44·7H2The concentration of O is 45-60 g/L, Na2C6H5O7·2H2The concentration of O is 50-60 g/L, H3BO3The concentration is 25-30 g/L, NaH2PO2·7H2The concentration of O is 30-40 g/L; preheating the plating solution to 70-90 ℃ before adjusting the pH value of the plating solution in the step 5; in the step 5, the total ratio of C powder to W powder in the WC/C/W/Co coarse-grain composite powder is 5-10 wt.%, and the mass ratio of the C powder to the W powder is 1: 1516, 5-10 wt% of a Co coating; and 6, the forming agent is SD-E rubber, the content of the forming agent accounts for 1.5-2.5 wt% of the total powder, the pressing pressure of the pressed blank is 20-100 MPa, the sintering temperature is 1400-1450 ℃ under the vacuum condition during sintering, and the temperature is kept for 1-2 hours under the pressure of 1-10 Pa after sintering.
The synthesis principle is as follows: according to the invention, WC/C/W/Co coarse-grain composite powder is obtained in a carbon powder and tungsten powder synergistic coating mode, the two kinds of powder are filled between cobalt particles in the nucleation growth process of the cobalt on the surface of tungsten carbide to form a C/W/Co coating, so that the two kinds of powder are dispersed more uniformly and the uniform growth of the cobalt layer is ensured, the WC/C/W/Co coarse-grain composite powder finally obtained by synergistic coating is a structure that W and C particles are embedded in the Co coating, and finally, in a liquid phase sintering process, the carbon powder and the tungsten powder react in situ in a liquid phase of the cobalt to promote the rapid growth of the coarse-grain WC grains and simultaneously form a high-performance WC and high-strength phase interface, so that the coarse-grain WC-Co hard alloy with high comprehensive performance is finally obtained.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: the coarse-grain WC-Co hard alloy with the grain size larger than 2 mu m is prepared by in-situ reaction sintering, and has excellent grain size, hardness, transverse fracture strength and impact toughness.
Detailed Description
Example 1
(1) Ball-milling 500g of coarse WC powder with the particle size of 10-15 mu m in a roller ball mill by using absolute alcohol as a wet milling medium, wherein the content of the absolute alcohol is 200mL/kg, the diameter of a milling ball is 13mm, and the ball-material ratio is 3: 1; carrying out ball milling for 12h, and then carrying out vacuum drying to obtain pretreated WC powder;
(2) 50g of CoSO4·7H2O and 50g of NaH2PO2·7H2Dissolving O in distilled water to obtain 1L of activating solution, placing 100g of pretreated WC powder in 1L of activating solution, mechanically stirring, and activating at 50 deg.C for 30 min;
(3) filtering, drying and activating the WC powder, and performing heat treatment in a muffle furnace at 400 ℃ for 2h to obtain WC activated powder with metal Co particles attached to the surface;
(4) 55g CoSO4·7H2O and 50g Na2C6H5O7·2H2Dissolving O in 800mL of distilled water, fully complexing, and sequentially adding 25g H3BO3And 40g NaH2PO2·7H2Preparing 900mL of plating solution by using O;
(5) then 24.82g of WC activated powder, 2.9g C powder and 0.19g W powder were placed in the bath, mechanically stirred in a water bath at 80 ℃, pH 11 was adjusted with NaOH, distilled water was added to make the bath 1L, and electroless plating was performed at 80 ℃ for 60min, followed by filtration, washing and vacuum drying to obtain 31.04g of WC/0.614 wt.% C/9.386 wt.% W/10 wt.% Co composite powder.
(6) Adding 2.5 wt.% of SD-E forming agent into WC/0.614 wt.% C/9.386 wt.% W/10 wt.% Co composite powder, granulating, sieving with an 80-mesh sieve, and press-forming under the pressure of 20 MPa; and sintering the pressed blank under a vacuum condition, wherein the sintering temperature is 1400 ℃, and the heat preservation time is 1h, so as to obtain the WC-Co hard alloy.
Example 2
(1) Ball-milling 500g of coarse WC powder with the particle size of 10-15 mu m in a roller ball mill by using absolute alcohol as a wet milling medium, wherein the content of the absolute alcohol is 200mL/kg, the diameter of a milling ball is 13mm, and the ball material-ball material ratio is 3: 1; carrying out ball milling for 12h, and then carrying out vacuum drying to obtain pretreated WC powder;
(2) 50g of CoSO4·7H2O and 50g of NaH2PO2·7H2Dissolving O in distilled water to obtain 1L of activating solution, placing 100g of pretreated WC powder in 1L of activating solution, mechanically stirring, and activating at 50 deg.C for 30 min;
(3) filtering, drying and activating the WC powder, and performing heat treatment in a muffle furnace at 300 ℃ for 3h to obtain WC activated powder with metal Co particles attached to the surface;
(4) 50g of CoSO4·7H2O and 50g Na2C6H5O7·2H2Dissolving O in 800mL of distilled water, fully complexing, and sequentially adding 25g H3BO3And 30g NaH2PO2·7H2Preparing 900mL of plating solution by using O;
(5) then 15.6g of WC activated powder, 0.12g C powder and 1.83g W powder were placed in the bath and mechanically stirred at 70 ℃ in a water bath, pH 11 was adjusted with NaOH, distilled water was added to make the bath 1L, and electroless plating was performed at 70 ℃ for 60min, followed by filtration, washing and vacuum drying to obtain 19.48g of WC/0.307 wt.% C/4.693 wt.% W/8 wt.% Co composite powder.
(6) Adding 2.5 wt.% SD-E forming agent into WC/0.614 wt.% C/9.386 wt.% W/10 wt.% Co composite powder, granulating, sieving with an 80-mesh sieve, and press-forming under the pressure of 20 MPa; and sintering the pressed blank under a vacuum condition, wherein the sintering temperature is 1450 ℃, and the heat preservation time is 1h, so that the WC-Co hard alloy is obtained.
Comparative example 1
The differences between this comparative example and example 1 are: c powder and W powder are not added in the chemical plating step, and WC/10 wt.% Co composite powder is prepared after chemical plating.
Comparative example 2
The difference between this comparative example and example 2 is: the ball milling pretreatment of the coarse WC powder was not performed.
The results of performance tests on examples 1-2 and comparative examples 1-2 are shown in table 1, and it can be seen from the table that the pores in the four coarse-grain cemented carbides are basically consistent, the average grain size of the cemented carbides of examples 1-2 is greater than 2 μm, the coated C/W/Co coating is uniform, the C and W particles are uniformly dispersed, and the prepared coarse-grain cemented carbides have superior hardness, transverse rupture strength and impact toughness, while the coarse-grain cemented carbides of comparative examples 1 and 2, which are prepared without adding carbon powder and tungsten powder, have slightly lower grain size, hardness, strength and impact toughness, and the latter has larger grain size due to the fact that tungsten carbide powder is not pretreated, and is easy to generate aggregated WC grains to cause performance reduction.
TABLE 1 results of Performance test conducted on examples 1-2 and comparative examples 1-2
Claims (9)
1. The preparation method of the coarse-grain WC-Co hard alloy is characterized by comprising the following steps of:
(1) performing ball milling on the coarse WC powder particles, cleaning, and drying in vacuum to obtain pretreated WC powder, wherein alloy balls with the diameter of 10-13 mm are adopted for ball milling, and the ball-to-material ratio is 1-3: 1;
(2) adding CoSO4·7H2O and NaH2PO2·7H2Dissolving O in the solution to prepare an activation solution, and adding the WC powder treated in the step (1) into the activation solution for activation;
(3) filtering, drying and activating the WC powder, and performing heat treatment reduction to obtain WC activated powder with metal Co particles attached to the surface;
(4) adding CoSO4·7H2O and Na2C6H5O7·2H2Dissolving O in water, complexing, and sequentially adding H3BO3And NaH2PO2·7H2O is prepared into plating solution;
(5) placing WC activated powder, C powder and W powder with metal Co particles attached to the surfaces in a plating solution, stirring in a water bath, adjusting the pH value of the plating solution to 10-12, carrying out chemical plating at 70-90 ℃, filtering, cleaning and drying in vacuum to obtain WC/C/W/Co coarse-grain composite powder;
(6) adding the WC/C/W/Co coarse-grain composite powder into a forming agent, pressing into a blank, and sintering into the WC-Co hard alloy.
2. The method for preparing a macrocrystalline WC-Co cemented carbide as claimed in claim 1, wherein the CoSO in the activation solution in step 24·7H2O and NaH2PO2·7H2The O concentration is 50-60 g/L respectively, and the volume ratio is 1: 1-2, the activation temperature is 50-60 ℃, and the activation time is 20-30 min.
3. The method for preparing the macrocrystalline WC-Co hard alloy according to claim 1, wherein the heat treatment temperature in step 3 is 300-400 ℃ and the time is 2-3 h.
4. The method for preparing a macrocrystalline WC-Co cemented carbide according to claim 1, wherein the CoSO in step 4 is4·7H2The concentration of O is 45-60 g/L, Na2C6H5O7·2H2The concentration of O is 50-60 g/L, H3BO3The concentration is 25-30 g/L, NaH2PO2·7H2The concentration of O is 30-40 g/L.
5. The method for preparing a macrocrystalline WC-Co hard alloy as recited in claim 1, wherein the plating solution is preheated to 70-90 ℃ before the pH value of the plating solution is adjusted in the step 5.
6. The method for preparing the macrocrystalline WC-Co hard alloy according to claim 1, wherein in the step 5, the total ratio of C powder to W powder in the WC/C/W/Co macrocrystalline composite powder is 5-10 wt.%, and the mass ratio of C powder to W powder is 1: 15-16 wt% of Co coating.
7. The method for preparing a macrocrystalline WC-Co hard alloy as recited in claim 1, wherein the molding agent in step 6 is SD-E rubber, and the content of the molding agent is 1.5-2.5 wt.% of the total powder.
8. The method for preparing a macrocrystalline WC-Co hard alloy as recited in claim 1, wherein the green compact pressing pressure in the step 6 is 20-100 MPa.
9. The method for preparing the macrocrystalline WC-Co hard alloy according to claim 1, wherein the sintering temperature in the step 6 is 1400-1450 ℃ under vacuum condition during sintering, and the temperature is kept at 1-10 Pa for 1-2 h after sintering.
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| CN102534341B (en) * | 2012-02-27 | 2013-11-06 | 中南大学 | Method for eliminating WC (Wolfram Carbide) grain fragmentation at phase boundary between ultra-coarse grain hard alloy and super-coarse grain hard alloy |
| CN102560216B (en) * | 2012-02-27 | 2013-08-28 | 中南大学 | Preparation method of dense coated composite powder and super coarse and extra coarse grained cemented carbide |
| CN106191609B (en) * | 2016-08-30 | 2018-01-16 | 华南理工大学 | A kind of preparation method of the double mesostructure WC Co hard alloy of high-performance |
| CN106756160A (en) * | 2016-11-10 | 2017-05-31 | 无锡市明盛强力风机有限公司 | A kind of preparation method of cermet material |
| CN106756390B (en) * | 2016-12-01 | 2019-05-03 | 株洲硬质合金集团有限公司 | A kind of hard alloy and preparation method thereof containing slab-shaped tungsten carbide crystal grain |
| CN106636837B (en) * | 2017-01-23 | 2018-02-13 | 四川理工学院 | A kind of preparation method of super crude crystal WC Co hard alloy |
| CN109338197A (en) * | 2018-11-06 | 2019-02-15 | 河海大学 | A kind of preparation method of high-compactness WC/Co composite material hard alloy |
| CN110387497A (en) * | 2019-08-28 | 2019-10-29 | 河海大学 | A kind of preparation method of super coarse-grain WC-Co hard alloy |
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