CN110408811A - A kind of method that in-situ authigenic tungsten boride strengthens CuW alloy - Google Patents
A kind of method that in-situ authigenic tungsten boride strengthens CuW alloy Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention discloses a kind of method that in-situ authigenic tungsten boride strengthens CuW alloy, W powder, B powder and induction copper powder are uniformly mixed, and compression moulding, obtain tungsten green compact；Tungsten green compact is put into atmosphere sintering furnace and is sintered, W skeleton is obtained；It is put into the graphite crucible for being covered with graphite paper after fine copper block is placed on above W skeleton, carries out infiltration in sintering furnace to get to in-situ authigenic tungsten boride and strengthen CuW alloy.The method that a kind of in-situ preparation tungsten boride of the present invention strengthens CuW alloy, by using sintering infiltration method in CuW material in-situ preparation ceramic phase W2B to improve the arc ablation resistance performance of CuW contact material, while strengthening CuW material using in-situ preparation tungsten boride since the presence of low work function ceramic phase disperses electric arc effectively, avoids the particle surface pollution of reinforced phase.
Description
Technical field
The invention belongs to electrical material technical fields, and in particular to a kind of in-situ authigenic tungsten boride strengthens the side of CuW alloy
Method.
Background technique
CuW material combine tungsten high-melting-point, high rigidity, high Burning corrosion resistance and resistance fusion welding, low thermal expansion coefficient with
And the highly conductive of copper, high thermal conductivity, good plasticity, therefore the electrical contact being used as in various high-voltage switch gears extensively.With
The Implement Construction of extra-high voltage grid, it is desirable that CuW electrical contact contact material has the ability of bigger breaking current, higher proof voltage
The service life of intensity and overlength.Contact will bear the ablation of high-voltage arc in interrupting process.Especially super, extra-high
In the breaker of pressure in use, since voltage is higher, it is easier to which the failure for causing electrical contact leads to contact material strength reduction.
It finally will lead to CuW electrical contact material to fail and the disjunction circuit that cannot succeed.Therefore, with the development of high-voltage switch gear, need into
One step improves its arc ablation resistance performance.
Existing research shows that tungsten basal body intensity rises with temperature and is remarkably decreased, the intensity at 1000 DEG C in CuW alloy
Only the 20%~40% of room temperature intensity.Therefore, general using being added in tungsten basal body in order to improve the elevated temperature strength of tungsten basal body
A small amount of Second Phase Particle carries out dispersion-strengtherning, the elevated temperature strength of Lai Tigao tungsten basal body, but the addition of Second Phase Particle usually can
The pollution of output particle surface, and method complexity higher cost.
Summary of the invention
The object of the present invention is to provide a kind of methods that in-situ authigenic tungsten boride strengthens CuW alloy, to improve CuW material
Arc ablation resistance performance, reaction in-situ solves particle surface pollution problem brought by additional reinforced phase.
The technical scheme adopted by the invention is that a kind of in-situ authigenic tungsten boride strengthens the method for CuW alloy, specifically according to
Following steps are implemented:
Step 1, powder, green compact are mixed:
W powder, B powder and induction copper powder are uniformly mixed, compression moulding obtains tungsten green compact；
Step 2, it is sintered:
The tungsten green compact that step 1 obtains is put into atmosphere sintering furnace and is sintered, W skeleton is obtained；
Step 3, infiltration:
Be put into the graphite crucible for being covered with graphite paper after clean fine copper block is placed on above W skeleton, in sintering furnace into
Row infiltration strengthens CuW alloy to get to in-situ authigenic tungsten boride.
The features of the present invention also characterized in that:
In step 1 B powder additive amount be W silty amount 0~1.0%, induce copper powder additive amount be W silty amount 5~
10%.
The partial size of W powder is 1~50 μm in step 1, and the partial size of B powder is 0.2~50 μm, and inducing the partial size of copper powder is 5~100
μm。
150~500MPa of pressing pressure in step 1,30~90s of dwell time.
In step 2 in sintering process, sintering temperature is 800~1200 DEG C, and soaking time is 1~3h.
Hydrogen is passed through in step 2 in atmosphere sintering furnace.
600~1000 DEG C first are warming up to 5~20 DEG C/min heating rate in step 2 sintering process, keeps the temperature 0.5~2h,
800~1200 DEG C are warming up to 10~30 DEG C/min speed again, soaking time is 1~3h.
During step 3 infiltration, infiltrating temperature is 1200~1400 DEG C, and soaking time is 1~3h.
800~1200 DEG C first are risen to the heating rate of 5~20 DEG C/min during step 3 infiltration, keeps the temperature 1~3h, so
After be warming up to 1200~1400 DEG C, keep the temperature 1~3h.
The beneficial effects of the present invention are: a kind of in-situ authigenic tungsten boride of the present invention strengthens the method for CuW alloy, by using
In-situ preparation tungsten boride strengthens CuW material, avoids the pollution of reinforced phase particle surface, and preparation process is more convenient, reduces and adds
Enter the process of mixing to save time and cost.
Detailed description of the invention
Fig. 1 is the process flow chart for the method that a kind of in-situ authigenic tungsten boride of the present invention strengthens CuW alloy；
Fig. 2 is the hardness and conductivity test result figure of different B additive amount CuW alloys；
Fig. 3 is the XRD analysis figure that the present invention prepares sample；
Fig. 4 is to different W2The CuW alloy of B content carries out the SEM ablation edge pattern after 50 electrical breakdowns, wherein scheming a
For CuW alloy, figure b is 0.6%B content in-situ preparation W2The CuW alloy of B.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
The method that a kind of in-situ authigenic tungsten boride of the present invention strengthens CuW alloy, process as shown in Figure 1, specifically according to
Lower step is implemented:
Step 1, powder is mixed:
The W powder for being 1~50 μm by granularity, 0.2~50 μm of B powder and 5~100 μm of induction copper powder, are put into V-type mixing
In machine, 4~8h of mixing under 50r~80r/min is uniformly mixed.
Wherein B powder additive amount is 0~1.0%, purity > 99.9% of W silty amount, and inducing the additive amount of copper powder is W silty
The 5~10% of amount；
Step 2, compression moulding:
The powder mixed through step 1 is filled in rigid die, using hydraulic press compression moulding, pressing pressure 150
~500MPa, 30~90s of dwell time obtain tungsten green compact；
Step 3, it is sintered:
The tungsten green compact that step 2 suppresses is put into atmosphere sintering furnace, the purity of inspection hydrogen after hydrogen 40min is passed through,
Hydrogen is lighted after confirmation safety, is started to warm up after opening cooling water, is warming up to 600~1000 with 5~20 DEG C/min heating rate
DEG C, 0.5~2h is kept the temperature, then be warming up to 800~1200 DEG C with 10~30 DEG C/min speed, soaking time is 1~3h, furnace cooling
To room temperature, W skeleton is obtained；
Step 4, infiltration:
Fine copper block is polished to be put into after clean drying is placed on above W skeleton and is completed in the graphite crucible of graphite paper in advance, then
It is put into sintering furnace, after being passed through hydrogen 40min, examines hydrogen purity, light hydrogen after confirming safety, open power supply and start to add
Heat is heated to 800~1200 DEG C with the heating rate of 5~20 DEG C/min, keeps the temperature 1~3h, be then warming up to 1200~1400 DEG C,
1~2h is kept the temperature, room temperature is finally cooled to the cooling rate of 5~30 DEG C/min, obtains in-situ preparation W2The CuW alloy of B.
The present invention prepares in-situ authigenic W using process for sintering and infiltration2It is dirty to avoid reinforced phase particle surface for the CuW material of B
Dye reduces and mixed process is added to save time and cost, due to the W of low work function2B effectively disperses electric arc, thus
Improve the arc ablation resistance performance of CuW contact material, while CuW contact material hardness also with higher, side of the invention
Method simple process, preparation process are more convenient compared with outer addition.
Embodiment 1
Weigh the W powder that average grain diameter is 1 μm, B powder (average grain diameter is at 0.2 μm).B powder additive amount is W silty amount
The induction copper powder (average grain diameter is at 5 μm) of 0.2% and W silty amount 5% carries out mixing 4 on the V-type batch mixer of 80r/min
Hour, hydraulic press compression moulding is used after mixed, obtains W green compact.Pressing pressure 350MPa, dwell time 50s.W green compact is set
In graphite crucible, then crucible is put into atmosphere sintering furnace, after being passed through hydrogen 40min, examines hydrogen purity, confirmation safety
After light hydrogen, after opening cooling water, begin to warm up, heated up with the heating rate of 8 DEG C/min, when sintering temperature is 600 DEG C,
1000 DEG C are warming up to 10 DEG C/min speed again after heat preservation 1.5h, soaking time 1h.Room temperature is naturally cooled to furnace, obtains W
Skeleton.Surface fine copper block will be cleared up again to be stacked to above W skeleton, and then crucible is put into atmosphere sintering furnace, is passed through hydrogen
After 40min, hydrogen purity is examined, hydrogen is lighted after confirming safety, after opening cooling water, begins to warm up, with the heating of 5 DEG C/min
Speed heating after keeping the temperature 3h, is again heated to 1200 DEG C, 3h is kept the temperature, finally with the drop of 5 DEG C/min when infiltrating temperature is 900 DEG C
Warm speed is cooled to room temperature, obtains and contains W2The CuW alloy of B phase.
Embodiment 2
Weigh the W powder that average grain diameter is 15 μm, B powder (average grain diameter is at 25 μm).B powder additive amount is W silty amount
The induction copper powder (average grain diameter is at 60 μm) of 0.4% and W silty amount 8%, carries out mixing on the V-type batch mixer of 50r/min
8 hours, hydraulic press compression moulding is used after mixed, obtains W green compact.Pressing pressure 400MPa, dwell time 50s.W green compact is set
In graphite crucible, then crucible is put into atmosphere sintering furnace, after being passed through hydrogen 40min, examines hydrogen purity, confirmation safety
After light hydrogen, after opening cooling water, begin to warm up, heated up with the heating rate of 20 DEG C/min, when sintering temperature is 800 DEG C
When, 950 DEG C, soaking time 2h are warming up to 15 DEG C/min speed again after keeping the temperature 1h, room temperature is naturally cooled to furnace, obtains W
Skeleton.The fine copper block for clearing up surface is stacked to above W skeleton again, then crucible is put into atmosphere sintering furnace, is passed through hydrogen
After gas 40min, hydrogen purity is examined, hydrogen is lighted after confirming safety, after opening cooling water, begins to warm up, with 10 DEG C/min's
Heating rate heating after keeping the temperature 1.5h, is again heated to 1250 DEG C, 2 hours is kept the temperature, finally with 20 when infiltrating temperature is 950 DEG C
DEG C/cooling rate of min is cooled to room temperature, obtain in-situ authigenic W2The CuW alloy of B.
Embodiment 3
Weigh the W powder that average grain diameter is 15 μm, B powder (average grain diameter is at 30 μm).B powder additive amount is W silty amount
The induction copper powder (average grain diameter is at 30 μm) of 0.6% and W silty amount 7%, carries out mixing on the V-type batch mixer of 60r/min
6 hours, hydraulic press compression moulding is used after mixed, obtains W green compact.Pressing pressure 150MPa, dwell time 90s.W green compact is set
In graphite crucible, then crucible is put into atmosphere sintering furnace, after being passed through hydrogen 40min, examines hydrogen purity, confirmation safety
After light hydrogen, after opening cooling water, begin to warm up, heated up with the heating rate of 10 DEG C/min, when sintering temperature is 1000 DEG C
When, after keeping the temperature 1.5h, then with 20 DEG C/min speed 1200 DEG C are warming up to, soaking time 1h naturally cools to room temperature with furnace, obtains
Obtain W skeleton.The fine copper block for clearing up surface is stacked to above W skeleton again, then crucible is put into atmosphere sintering furnace, is passed through
After hydrogen 40min, hydrogen purity is examined, hydrogen is lighted after confirming safety, after opening cooling water, begins to warm up, with 15 DEG C/min
Heating rate heating after keeping the temperature 2h, be again heated to 1400 DEG C when infiltrating temperature is 1200 DEG C, keep the temperature 1 hour, finally with
The cooling rate of 30 DEG C/min is cooled to room temperature, obtains in-situ authigenic W2The CuW alloy of B.
Embodiment 4
Weigh the W powder that average grain diameter is 20 μm, B powder (average grain diameter is at 30 μm).B powder additive amount is W silty amount
The induction copper powder (average grain diameter is at 40 μm) of 0.8% and W silty amount 9%, carries out mixing on the V-type batch mixer of 55r/min
7 hours, hydraulic press compression moulding is used after mixed, obtains W green compact.Pressing pressure 500MPa, dwell time 30s.W green compact is set
In graphite crucible, then crucible is put into atmosphere sintering furnace, after being passed through hydrogen 40min, examines hydrogen purity, confirmation safety
After light hydrogen, after opening cooling water, begin to warm up, heated up with the heating rate of 18 DEG C/min, when sintering temperature is 850 DEG C
When, after keeping the temperature 1.5h, then with 30 DEG C/min speed 1000 DEG C are warming up to, soaking time 3h naturally cools to room temperature with furnace, obtains
Obtain W skeleton.The fine copper block for clearing up surface is stacked to above W skeleton again, then crucible is put into atmosphere sintering furnace, is passed through
After hydrogen 40min, hydrogen purity is examined, hydrogen is lighted after confirming safety, after opening cooling water, begins to warm up, with 18 DEG C/min
Heating rate heating after keeping the temperature 2h, be again heated to 1350 DEG C when infiltrating temperature is 800 DEG C, keep the temperature 1.5 hours, finally with
The cooling rate of 15 DEG C/min is cooled to room temperature, obtain in-situ authigenic W2The CuW alloy of B.
Embodiment 5
Weigh the W powder that average grain diameter is 50 μm, B powder (average grain diameter is at 50 μm).B powder additive amount is W silty amount
The induction copper powder (average grain diameter is at 100 μm) of 1.0% and W silty amount 10%, is mixed on the V-type batch mixer of 70r/min
Material 6 hours uses hydraulic press compression moulding after mixed, obtains W green compact.Pressing pressure 350MPa, dwell time 30s.By W green compact
It is placed in graphite crucible, then crucible is put into atmosphere sintering furnace, after being passed through hydrogen 40min, examine hydrogen purity, confirmation peace
Hydrogen is lighted after complete, after opening cooling water, is begun to warm up, is heated up with the heating rate of 20 DEG C/min, when sintering temperature is 700 DEG C
When, after keeping the temperature 2h, then with 20 DEG C/min speed 1200 DEG C, soaking time 2h are warming up to, naturally cool to room temperature with furnace, obtained
W skeleton.The fine copper block for clearing up surface is stacked to above W skeleton again, then crucible is put into atmosphere sintering furnace, is passed through hydrogen
After gas 40min, hydrogen purity is examined, hydrogen is lighted after confirming safety, after opening cooling water, begins to warm up, with 20 DEG C/min's
Heating rate heating after keeping the temperature 1.5h, is again heated to 1200 DEG C when infiltrating temperature is 1000 DEG C, keeps the temperature 2 hours, finally with
The cooling rate of 15 DEG C/min is cooled to room temperature, obtain in-situ authigenic W2The CuW alloy of B.
The in-situ authigenic W that above-described embodiment is prepared2The CuW alloy of B, in the TDR-40A single crystal growing furnace of repacking into
The experiment of row vacuum breakdown.Test proves that the embodiment sample after addition B element all realizes effective dispersion of electric arc,
Improve the arc ablation resistance performance of material.
Fig. 2 is the hardness and conductivity test result of different B additive amount materials.As can be seen that molten by using fine copper block
The W skeleton containing B element is seeped, the CuW alloy with certain degree of hardness and conductivity, still, excessive W can be obtained2B is generated can shadow
Ring material conductivity.
Fig. 3 is the XRD analysis that the present invention prepares sample, it can be seen that the CuW alloy that sintering and infiltration obtains after addition B element
In in situ generated W2B phase.
Fig. 4 is that the SEM ablation shape after 50 electrical breakdowns is carried out to CuW alloy and 0.6%B content in-situ preparation CuW alloy
Looks.Ablation situation is slighter at CuW alloy (as shown in figure b) face anode tungsten needle of addition 0.6%B, and ablated surface is generally
Relatively flat, the region of rhegmalypt distribution is larger, shows the trend of the oriented surrounding random motion of electric arc, due to W2The presence of B,
Electric arc has a degree of dispersion.
Claims (9)
1. a kind of method that in-situ authigenic tungsten boride strengthens CuW alloy, which is characterized in that be specifically implemented according to the following steps:
Step 1, powder, green compact are mixed:
W powder, B powder and induction copper powder are uniformly mixed, compression moulding obtains tungsten green compact；
Step 2, it is sintered:
The tungsten green compact that step 1 obtains is put into atmosphere sintering furnace and is sintered, W skeleton is obtained；
Step 3, infiltration:
It is put into the graphite crucible for being covered with graphite paper after clean fine copper block is placed on above W skeleton, is melted in sintering furnace
It seeps and strengthens CuW alloy to get to in-situ authigenic tungsten boride.
2. the method that a kind of in-situ authigenic tungsten boride according to claim 1 strengthens CuW alloy, which is characterized in that described
B powder additive amount is the 0~1.0% of W silty amount in step 1, and inducing the additive amount of copper powder is the 5~10% of W silty amount.
3. the method that a kind of in-situ authigenic tungsten boride according to claim 1 strengthens CuW alloy, which is characterized in that described
The partial size of W powder is 1~50 μm in step 1, and the partial size of B powder is 0.2~50 μm, and inducing the partial size of copper powder is 5~100 μm.
4. the method that a kind of in-situ authigenic tungsten boride according to claim 1 strengthens CuW alloy, which is characterized in that described
150~500MPa of pressing pressure in step 1,30~90s of dwell time.
5. the method that a kind of in-situ authigenic tungsten boride according to claim 1 strengthens CuW alloy, which is characterized in that described
In step 2 in sintering process, sintering temperature is 800~1200 DEG C, and soaking time is 1~3h.
6. the method that a kind of in-situ authigenic tungsten boride according to claim 1 strengthens CuW alloy, which is characterized in that described
Hydrogen is passed through in step 2 in atmosphere sintering furnace.
7. the method that a kind of in-situ authigenic tungsten boride according to claim 1 strengthens CuW alloy, which is characterized in that described
600~1000 DEG C first are warming up to 5~20 DEG C/min heating rate in step 2 sintering process, keep the temperature 0.5~2h, then with 10~
30 DEG C/min speed is warming up to 800~1200 DEG C, and soaking time is 1~3h.
8. the method that a kind of in-situ authigenic tungsten boride according to claim 1 strengthens CuW alloy, which is characterized in that described
During step 3 infiltration, infiltrating temperature is 1200~1400 DEG C, and soaking time is 1~3h.
9. the method that a kind of in-situ authigenic tungsten boride according to claim 1 strengthens CuW alloy, which is characterized in that described
800~1200 DEG C first are risen to the heating rate of 5~20 DEG C/min during step 3 infiltration, 1~3h is kept the temperature, is then warming up to
1200~1400 DEG C, keep the temperature 1~3h.
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Cited By (5)
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| CN110791674A (en) * | 2019-11-13 | 2020-02-14 | 哈尔滨工业大学 | Preparation method of refractory carbide particle reinforced tungsten copper infiltrated composite material |
| CN111961901A (en) * | 2020-08-12 | 2020-11-20 | 西安理工大学 | Preparation method of in-situ authigenic WC reinforced WCu dual-gradient-structure composite material |
| CN112086307A (en) * | 2020-08-12 | 2020-12-15 | 西安理工大学 | Preparation method of in-situ synthesized WC reinforced WCu moving arc contact surface layer |
| CN113151706A (en) * | 2021-03-17 | 2021-07-23 | 西安理工大学 | Low friction coefficient WB2Preparation method of/CuSn 10 composite material |
| WO2021189798A1 (en) * | 2020-03-23 | 2021-09-30 | 陕西斯瑞新材料股份有限公司 | Method for preparing cuw90 material by using spherical tungsten powder |
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| CN112086307A (en) * | 2020-08-12 | 2020-12-15 | 西安理工大学 | Preparation method of in-situ synthesized WC reinforced WCu moving arc contact surface layer |
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| CN112086307B (en) * | 2020-08-12 | 2022-11-18 | 西安理工大学 | Preparation method of in-situ synthesized WC reinforced WCu moving arc contact surface layer |
| CN113151706A (en) * | 2021-03-17 | 2021-07-23 | 西安理工大学 | Low friction coefficient WB2Preparation method of/CuSn 10 composite material |
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