CN115747550A - TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material and preparation method thereof - Google Patents
TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material and preparation method thereof Download PDFInfo
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- CN115747550A CN115747550A CN202211513870.XA CN202211513870A CN115747550A CN 115747550 A CN115747550 A CN 115747550A CN 202211513870 A CN202211513870 A CN 202211513870A CN 115747550 A CN115747550 A CN 115747550A
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- 239000002131 composite material Substances 0.000 title claims abstract description 53
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 39
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000010937 tungsten Substances 0.000 title claims abstract description 37
- 239000002245 particle Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 74
- 238000005245 sintering Methods 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000011812 mixed powder Substances 0.000 claims abstract description 27
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 14
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000004321 preservation Methods 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 14
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 230000004927 fusion Effects 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 3
- 238000007545 Vickers hardness test Methods 0.000 description 2
- 238000001887 electron backscatter diffraction Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention discloses a preparation method of a TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material, which comprises the following steps: step 1, respectively weighing TiC powder and W powder, and uniformly mixing the two powders to obtain mixed powder; step 2, performing high-energy ball milling on the mixed powder obtained in the step 1; and 3, putting the mixed powder subjected to ball milling into a die, cold-pressing the mixed powder into a blank, and sintering the blank in a spark plasma sintering device to obtain the material. The method improves the strength and wear resistance of the tungsten-based composite material, and can meet the application of the tungsten-based composite material in the field of nuclear fusion devices. Also provides a TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material and a preparation method of the TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material.
Background
The metal tungsten has the characteristics of high melting point (about 3410 ℃), corrosion resistance, low thermal expansion coefficient and the like, so that the metal tungsten is widely applied to the advanced fields of aerospace, nuclear fusion devices and the like. However, because the grain interatomic bonding force of the VIB group elements such as W, mo and the like is low, W grains are easy to become coarse in the sintering process, and the problems of room temperature brittleness, recrystallization brittleness, radiation brittleness and the like of metal W are easy to occur. In addition, due to the density of W (19.3 g/cm) 3 ) Higher, making W difficult to work in some weight-constrained components. At present, two methods can improve the performance of metal tungsten, namely adding rare metal or rare metal oxide and adding hard phase carbide (TiC, zrC and the like). Because rare metals are expensive and are not suitable for mass production, the carbide of the hard phase is low in price and has obvious strengthening effect, and the comprehensive mechanical property of the tungsten-based composite material can be effectively improved. In addition, the high-energy ball milling is carried out on the original powder, so that the powder is highly uniform and refined, and energy is provided for subsequent sintering. However, the conventional powder sintering technology is easy to introduce impurity gases such as O, H and the like, and the sintering quality is seriously influenced.
Disclosure of Invention
The invention aims to provide a preparation method of a TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material, which improves the strength and wear-resistance of the tungsten-based composite material and can meet the application of the tungsten-based composite material in the field of nuclear fusion devices.
The second purpose of the invention is to provide a TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material.
The first technical scheme adopted by the invention is that the preparation method of the TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material comprises the following steps:
and 3, placing the mixed powder subjected to ball milling into a die, performing cold pressing to obtain a green body, and sintering in discharge plasma sintering equipment to obtain the material.
The present invention is also characterized in that,
in the step 1, the two kinds of powder in the obtained mixed powder comprise the following components in percentage by mass: 6 to 10 percent of TiC powder, the balance being W powder, the sum of the mass percent of the components is 100 percent; the added TiC powder is nano-scale powder.
In the step 1, uniformly mixing the weighed TiC powder and W powder in a V-shaped powder mixer for 8-12 hours;
In step 2, the grinding ball used for the high-energy ball milling is Al 2 O 3 Grinding balls, wherein the ball material ratio is 10, and the ratio of large balls to medium balls is 2;
in the step 3, when the spark plasma sintering is carried out, the sintering temperature is 1600-1750 ℃, and the sintering heat preservation time is 30-40 min.
In the step 3, the axial pressure of 20 MPa-30 MPa is kept in the sintering temperature rise and heat preservation process, and the pressure is kept stably at 0.5 MPa-1.0 MPa in the cooling process.
The second technical scheme adopted by the invention is that the TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material is prepared by adopting the method.
The invention has the beneficial effects that:
the TiC particles added in the method can inhibit the growth of W grains, and the TiC powder generates lattice distortion in the high-energy ball milling process to cause a large amount of free C, the C and W generate in-situ reaction in the sintering process to promote the densification of sintering, and in addition, WC and W generated by the in-situ reaction 2 The second phase such as C not only effectively improves the wear resistance of the composite material, but also improves the strength of the tungsten-based composite material. TiC and other second phases are uniformly distributed on the tungsten crystal boundary, so that dislocation migration is effectively hindered, and the problem that the application strength and the wear resistance of metal tungsten in the tip field are insufficient is solved. Meanwhile, SPS plasma sintering is adopted in the method, the method has the characteristics of high temperature rise speed, short sintering time, controllable tissue structure and the like, and has great advantages for preparing the tungsten-based composite material, and the prepared tungsten-based composite material has excellent mechanical properties.
Drawings
FIG. 1 is a microstructure of a W-10wt% TiC composite SEM prepared in example 5 of the present invention;
FIG. 2 is the EBSD results of W-10wt% TiC composite material prepared in inventive example 5;
FIG. 3 is an XRD result of W-10wt% TiC composite material prepared in example 5 of the present invention;
FIG. 4 is the hardness value of W-10wt% TiC composite material prepared in example 5 of the present invention, in 6 times of micro Vickers hardness test;
FIG. 5 is a graph of the room temperature compressive stress strain of the W-10wt% TiC composite prepared in example 5 of the present invention;
FIG. 6 is a graph showing the frictional wear curve of W-10wt% TiC composite material, prepared in example 5 of the present invention;
FIG. 7 is a microstructure of the wear surface of the W-10wt% TiC composite SEM prepared in example 5 of the present invention.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
The invention provides a preparation method of a TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material, which comprises the following steps:
in the step 1, the two kinds of powder in the obtained mixed powder comprise the following components in percentage by mass: 6 to 10 percent of TiC powder, and the balance of W powder, wherein the sum of the mass percentages of the components is 100 percent; the added TiC powder is nano-scale powder.
In the step 1, uniformly mixing the weighed TiC powder and W powder in a V-shaped powder mixer for 8-12 hours;
In step 2, the grinding ball used for the high-energy ball milling is Al 2 O 3 Grinding balls, wherein the ball material ratio is 10, and the ratio of large balls to medium balls is 2;
and 3, putting the mixed powder subjected to ball milling into a die, cold-pressing the die into a green body, and sintering the green body in a Spark Plasma Sintering (SPS) device to obtain the composite material.
In the step 3, when the spark plasma sintering is carried out, the sintering temperature is 1600-1750 ℃, and the sintering heat preservation time is 30-40 min.
In the step 3, the axial pressure of 20 MPa-30 MPa is kept in the sintering temperature rise and heat preservation processes, and the pressure is kept stably at 0.5 MPa-1.0 MPa in the cooling process; the prepared TiC particle reinforced tungsten-based composite material is a W- (6-10 wt%) TiC composite material.
The invention provides a TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material which is prepared by adopting the method.
Example 1: tiC particle reinforced tungsten-based composite Material (W-6 wt% TiC)
Weighing TiC powder and W powder with the mass fractions of 6% and 94% respectively, and uniformly mixing the two kinds of powder in a V-shaped powder mixer for 8 hours; the uniformly mixed powder was filled into a ball ink tank and 2ml of ethanol medium was added, using Al 2 O 3 Grinding balls, wherein the ball-to-material ratio is 10, the ratio of large balls to medium balls of the grinding balls is 2; placing the powder subjected to high-energy ball milling into a die, separating the powder from the die and an upper die and a lower die by using graphite paper, and then performing SPS discharge plasma sintering at the sintering heat preservation temperature of 1700 ℃ for 30min; the axial pressure of 30MPa is kept in the sintering temperature rise and heat preservation processes, and the pressure is kept stable at 1.0MPa in the cooling process.
Example 2: tiC particle-reinforced tungsten matrix composite Material (W-7wt% TiC)
Weighing 7% and 93% of TiC powder and W powder by mass, and uniformly mixing the two kinds of powder in a V-shaped powder mixer for 10 hours; the uniformly mixed powder was filled into a ball ink tank and 2ml of ethanol medium was added, using Al 2 O 3 Grinding balls, wherein the ball-to-material ratio is 10, the ratio of large balls to medium balls of the grinding balls is 2; and (3) placing the powder subjected to high-energy ball milling into a die, separating the powder from the die and an upper die and a lower die by using graphite paper, and then performing SPS discharge plasma sintering, wherein the sintering heat preservation temperature is 1600 ℃, and the sintering heat preservation time is 35min. The axial pressure of 20MPa is kept in the sintering temperature rise and heat preservation processes, and the pressure is kept stably at 0.5MPa in the cooling process.
Example 3: tiC particle reinforced tungsten-based composite Material (W-8wt% TiC)
Weighing TiC powder and W powder with mass fractions of 8% and 92% respectively, and uniformly mixing the two kinds of powder in a V-shaped powder mixer for 12 h; the uniformly mixed powder was filled into a ball ink tank and 2ml of ethanol medium was added, using Al 2 O 3 Grinding balls, wherein the ball-to-material ratio is 10, the ratio of large balls to medium balls to small balls is 2; placing the powder subjected to high-energy ball milling into a die, separating the powder from the die and an upper die and a lower die by using graphite paper, and then performing SPS discharge plasma sintering, wherein the sintering heat preservation temperature is 1650 ℃, and the sintering heat preservation time is 30min; and the axial pressure of 25MPa is kept in the sintering temperature rise and heat preservation processes, and the pressure is kept stably at 0.7MPa in the cooling process.
Example 4: tiC particle-reinforced tungsten matrix composite Material (W-9wt% TiC)
Weighing 9% and 91% of TiC powder and W powder by mass, and uniformly mixing the two kinds of powder in a V-shaped powder mixer for 8 hours; the uniformly mixed powder was filled into a ball ink tank and 2ml of ethanol medium was added, using Al 2 O 3 Grinding balls, wherein the ball-to-material ratio is 10, the ratio of large balls to medium balls of the grinding balls is 2; placing the powder subjected to high-energy ball milling into a die, separating the powder from the die and an upper die and a lower die by using graphite paper, and then performing SPS discharge plasma sintering at the sintering heat preservation temperature of 1750 ℃ for 40min; the axial pressure of 30MPa is kept in the sintering temperature rise and heat preservation processes, and the pressure is kept stable at 1.0MPa in the cooling process.
Example 5: tiC particle-reinforced tungsten-based composite Material (W-10wt% TiC)
Weighing 10% and 90% of TiC powder and W powder by mass, and uniformly mixing the two kinds of powder in a V-shaped powder mixer for 8 hours; the uniformly mixed powder was filled into a ball ink tank and 2ml of ethanol medium was added, using Al 2 O 3 Grinding balls, wherein the ball material ratio is 10,the ball milling time is 4 hours, and the powder collected after the ball milling is dried in a drying box at the temperature of 45 ℃ for 20 hours; placing the powder subjected to high-energy ball milling into a die, separating the powder from the die and an upper die and a lower die by using graphite paper, and then performing SPS (spark plasma sintering) discharge plasma sintering, wherein the sintering heat preservation temperature is 1700 ℃, and the sintering heat preservation time is 30min; the axial pressure of 30MPa is kept in the sintering temperature rise and heat preservation processes, and the pressure is kept stable at 1.0MPa in the cooling process.
FIG. 1 is the microstructure morphology of the W-10wt% TiC composite SEM, it can be observed that the surface of the W-10wt% TiC composite appears as a continuous elongated-bar network structure; FIG. 2 is the W-10wt% TiC composite EBSD results, statistically, the average size of W grains is about 0.36 μm; FIG. 3 is the XRD result of TiC composite material, measured by weight% of W-10wt%, except for W phase and TiC phase, additionally W 2 Appearance of C phase and Ti phase, W 2 The in-situ generation of C has positive effects on improving the hardness and strength of the tungsten-based composite material; FIGS. 4 and 5 are hardness values and room temperature compressive stress strain curves of the W-10wt% TiC composite material in 6 micro-Vickers hardness tests, which shows that the micro-Vickers hardness of the W-10wt% TiC reaches 962HV, and the ultimate compressive strength reaches 2511MPa; FIG. 6 is a graph showing the abrasion friction curve of the W-3wt% TiC composite material, the abrasion friction test shows that the friction coefficient of the W-3wt% TiC composite material is stabilized at 0.60, FIG. 7 shows the microstructure morphology of the friction surface under the SEM of the W-10wt% TiC composite material, and it is observed that a large amount of friction film appears on the abrasion surface of the W-10wt% TiC composite material, and the appearance of the friction film plays a role of self-lubrication, thereby improving the abrasion resistance of the W-10wt% TiC composite material.
Claims (8)
- A preparation method of a TiC particle reinforced high-strength high-wear-resistance tungsten-based composite material is characterized by comprising the following steps:step 1, respectively weighing TiC powder and W powder, and uniformly mixing the two powders to obtain mixed powder;step 2, carrying out high-energy ball milling on the mixed powder obtained in the step 1;and 3, putting the mixed powder subjected to ball milling into a die, cold-pressing the mixed powder into a blank, and sintering the blank in a spark plasma sintering device to obtain the material.
- 2. The method of preparing a TiC particle reinforced high strength high wear resistant tungsten matrix composite material of claim 1, wherein in step 1, the mass percentage of two powders in the obtained mixed powder is: 6 to 10 percent of TiC powder, the balance being W powder, the sum of the mass percent of the components is 100 percent; the added TiC powder is nano-scale powder.
- 3. The method of claim 1, wherein in step 1, the TiC particles and the W powder are mixed uniformly in a V-type powder mixer for 8 to 12 hours.
- 4. The preparation method of the TiC particle-reinforced high-strength high-wear-resistance tungsten-based composite material as claimed in claim 1, wherein in the step 2, the powder uniformly mixed in the step 1 is placed in a ball milling tank, an ethanol medium is added, the ball milling tank is pumped to a sub-vacuum state by using a mechanical pump, then argon gas is introduced for protection, after ball milling is carried out for 4h to 8h, the powder collected after ball milling is dried in a drying oven at the temperature of 40 ℃ to 50 ℃ for 20h to 24 h; wherein the mass of the ethanol medium accounts for 0.5-1 wt% of the mixed powder obtained in the step 1.
- 5. The method of preparing a TiC particle-reinforced high-strength high-wear-resistance tungsten-based composite material of claim 1, wherein in the step 2, the grinding balls used in the high-energy ball milling are Al 2 O 3 Grinding balls, wherein the ball material ratio is 10, and the ratio of large balls to medium balls is 2.
- 6. The method of claim 1, wherein in step 3, the sintering temperature is 1600 ℃ to 1750 ℃ and the sintering temperature is 30min to 40min during spark plasma sintering.
- 7. The method of claim 1, wherein in step 3, axial pressure of 20 to 30MPa is maintained during sintering temperature rise and heat preservation, and pressure is kept stable at 0.5 to 1.0MPa during cooling.
- A TiC particle-reinforced high-strength high-wear-resistance tungsten-based composite material, characterized by being prepared by the method of any one of claims 1 to 7.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103602868A (en) * | 2013-12-07 | 2014-02-26 | 西北有色金属研究院 | Preparation method of high-density fine-grain W-TiC alloy material |
| WO2021027824A1 (en) * | 2019-08-12 | 2021-02-18 | 河南科技大学 | Tungsten-base alloy material and preparation method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103602868A (en) * | 2013-12-07 | 2014-02-26 | 西北有色金属研究院 | Preparation method of high-density fine-grain W-TiC alloy material |
| WO2021027824A1 (en) * | 2019-08-12 | 2021-02-18 | 河南科技大学 | Tungsten-base alloy material and preparation method therefor |
Non-Patent Citations (1)
| Title |
|---|
| 谈军等: "放电等离子烧结制备超细晶粒W-TiC复合材料", 稀有金属材料与工程, vol. 40, no. 11, pages 1990 - 1993 * |
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