CN108611514B - A kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material and preparation method thereof - Google Patents
A kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material and preparation method thereof 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 belongs to the preparation field of welding electrode Cu-base composites, a kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material and preparation method thereof is disclosed: by mixed uniformly Cu-Zr-B4C mixed-powder, which is put into high-temperature tubular atmosphere furnace, is heated to 1250 DEG C, obtains ultra-fine ZrC particle and the ZrB containing Cu2Stick crystalline substance composite granule, then melting oxygen-free copper and the ultra-fine ZrC-ZrB containing Cu in vacuum melting furnace2The mixture of composite granule simultaneously applies magnetic stirring, to prepare ultra-fine ZrC particle-ZrB2Stick crystalline substance enhances copper base electrode material.The method of the present invention has the characteristics that at low cost, technique is simple, high production efficiency, reinforcement is tiny, is evenly distributed.
Description
Technical field
The invention belongs to the welding electrode preparation fields of copper base electrode material, are mainly used for electrode welder head, electrode cap
Deng, and in particular to a kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material and preparation method thereof.
Background technique
Spot welding is widely used in the industries such as automobile, instrument and aeronautical manufacture, bears high temperature and high pressure effect, copper often because being on active service
Alloy electrode is vulnerable and reduces production efficiency and influences quality of welding spot.With automatic welding and welding robot in modern production
Be widely used, there is an urgent need to develop the electrode materials for having both good electric conductivity and mechanical performance.It is insufficient to solve copper alloy performance
Effective way first is that preparing superfine ceramic Reinforced Cu-Base Composites.Existing research shows that nanometer Al2O3Particles Reinforced Cu
Based composites have good mechanical performance, but Al2O3(the resistance coefficient: 1020 × 10 of ceramics almost insulation-6Ω·
M), it is incorporated into the copper-based middle electric conductivity that can significantly reduce electrode.In comparison, ZrC, ZrB2Ceramics have high rigidity, Gao Rong
The advantages of point, good chemical stability, especially excellent electric conductivity are a kind of more preferably electrode material reinforcements.Cause
This, ultra-fine ZrC-ZrB in Copper substrate2The addition of ceramics, is expected to improve its mechanicalness while keeping copper good electric conductivity
Energy.ZrC-ZrB can be prepared by SHS technology2/ Cu composite material (Mengxian Zhang, Yanqiu Huo,
Min Huang,et al.The effect of B4C particle size on the reaction processand
product in the Cu-Zr-B4C system.Journal of Asian Ceramic Societies.2015,3:38-
43).This method short, low power consumption and other advantages with the time, but the porosity of SHS process product is too high, and strong hardness is too
It is low, it is actually difficult to directly use.Therefore, need to seek to be more suitable for ZrC-ZrB2/ Cu composite material and preparation method thereof.
The present invention proposes that a kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhances copper base electrode material and preparation method thereof,
This method is easy to operate, requires loose, product hardness height, voidage low convenient for control, to raw material.
Summary of the invention
In view of the above technical problems existing in the prior art, the present invention provides a kind of ultra-fine zirconium carbide particle-zirconium boride stick
Crystalline substance enhancing copper base electrode material and preparation method thereof, can improve its mechanical performance under the premise of keeping copper good electric conductivity, together
When efficiently solve the problems, such as that ultra-fine zirconium carbide and zirconium boride powder price are expensive, this method also has that equipment is simple, operation letter
Easily, the advantages such as low, high production efficiency, reinforcement is tiny, be evenly distributed, product hardness is high, voidage is low are required to raw material.
The present invention provides a kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material, which is characterized in that by
Oxygen-free copper, ultra-fine ZrC particle and ZrB2Stick crystalline substance is constituted, wherein copper content is 99.0~99.9wt.%, ultra-fine ZrC and ZrB2's
Total content is 0.1~1.0wt.%.
The present invention also provides above-mentioned ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material and its preparation sides
Method, preparation process comprise the steps of:
Step 1: with Cu powder, Zr powder and B4C powder is that raw material prepares the ultra-fine ZrC particle-ZrB containing Cu2Stick crystalline substance composite particles；
Step 2: the ultra-fine ZrC particle-ZrB by loose state containing Cu2Stick crystalline substance composite particles are ground into powder；
Step 3: by the ultra-fine ZrC particle-ZrB containing Cu2Stick crystalline substance composite granule and copper foil are put into glove box, are then existed
The ultra-fine ZrC particle-ZrB containing Cu is sealed with copper foil in inert gas environment2Stick crystalline substance composite granule；
Step 4: by oxygen-free copper block and the ultra-fine ZrC particle-ZrB containing Cu2Stick crystalline substance composite granule is put into vacuum melting furnace
In, wherein the ultra-fine ZrC particle-ZrB containing Cu2Stick crystalline substance composite granule is placed below oxygen-free copper block；After vacuum to be extracted, it will melt
Furnace is heated to 1200~1250 DEG C, melts oxygen-free copper block and is covered on the ultra-fine ZrC particle-ZrB containing Cu2Stick crystalline substance composite powder
The surface of body；Then 5~10min is kept the temperature, and apply magnetic stirring to make ZrC and ZrB2It is uniformly distributed in Cu liquid, is finally cast to
Ultra-fine ZrC particle-ZrB is obtained in metal die2Stick crystalline substance enhances copper base electrode material.
The specific preparation process of above-mentioned steps one comprises the steps of:
Step (1), with Cu powder, Zr powder and B4C powder is raw material, wherein Zr powder and B4C powder molar ratio is adding for 3, Cu powder
Dosage is 10wt.%~40wt.%；
Step (2), by load weighted Cu powder, Zr powder, B4C powder is mixed in inert gas environment in tumbling ball mill
It closes 10~14 hours, obtains Cu-Zr-B4C mixed-powder；
Step (3), by loose Cu-Zr-B4C mixed-powder is put into ceramic boat, then the ceramic boat that powder is housed
It is put into high-temperature tubular atmosphere furnace, then is arranged as inert gas environment；
Step (4) is heated high temperature process furnances by the heating rate of 20~30 DEG C/min, is increased to 1250 DEG C to temperature
Afterwards, loose state, the ultra-fine ZrC particle-ZrB containing Cu can be obtained to room temperature in furnace cooling2Stick crystalline substance composite particles.
The Cu powder, purity > 99%, 0.5~75 μm of average grain diameter.
The Zr powder, purity > 98%, partial size~45 μm.
The B4C powder, purity > 99%, average grain diameter are 14~28 μm.
The oxygen-free copper block, purity>99.97%, oxygen content<0.003%, content of impurities are not more than 0.03%.
The abrading-ball of the ball mill is ZrO2Abrading-ball, ZrO2The diameter of abrading-ball is 8mm, and the weight ratio of abrading-ball and powder is 10:
1, the revolving speed of ball mill is 50~70 rev/min.
The Ar gas, purity 99.999%.
The metal die is Alloy-steel mold.
The magnetic stirring, electric current are 20~30A.
The ultra-fine ZrC-ZrB of preparation2In ceramic Reinforced Cu base electrode material, ZrC average grain diameter < 100nm, ZrB2Stick crystalline substance
Diameter is 50nm~0.2 μm, ZrC-ZrB2The total content of composite ceramics is 0.1~1.0wt.%, remaining is Cu.
In above-mentioned steps (1), the Cu-Zr-B4The molar ratio of Zr powder and C powder is 3 in C mixed-powder, is otherwise reacted
It is incomplete, the ultra-fine ZrC-ZrB containing Cu2The B of meeting remained unreacted in composite granule4C or by-product Cu-Zr compound.
In above-mentioned steps (2), loading powder and abrading-ball are fitted into ball grinder in inert gas environment, machine can be prevented
The oxidation of the powder such as Zr in tool mechanical milling process.
In above-mentioned steps (3), the placement process of inert gas environment are as follows: high-temperature atmosphere furnace is first evacuated to 5~10Pa
Afterwards；Then Ar gas is poured to 0.06~0.08MPa, is evacuated, is inflated three times repeatedly；Ar gas finally is poured to high-temperature tubular atmosphere furnace
To normal pressure, it is continually fed into the Ar gas that flow is 0.5~0.7L/min.The Cu-Zr-B being fitted into ceramic boat4C mixed-powder is
Loose condition (of surface), with high-purity argon gas to high temperature process furnances prepurging three times, to exclude the air in burner hearth, prevent Zr in heating process
The oxidation of equal powder.
In above-mentioned steps (4), protective atmosphere Ar gas is continually fed into heating process, flow is 0.5~0.7L/min, to prevent
The only invasion of oxygen and the oxidation of Zr in heating process；Heating rate is 20~30 DEG C/min, too fast to will lead to ZrC-ZrB2Ceramics
Synthesis it is incomplete, will lead to ZrC-ZrB slowly excessively2The roughening of ceramics.
In above-mentioned steps two, the ultra-fine ZrC particle-ZrB by loose state containing Cu is needed2Stick crystalline substance is ground into powder, in favor of
ZrC-ZrB in subsequent fusion process2Ceramics being dispersed with stirring in copper liquid.
In above-mentioned steps three, by the nanometer ZrC-ZrB containing Cu2Powder and copper foil are put into glove box, extract vacuum backlash
Enter argon gas to normal pressure, then seals the ZrC-ZrB containing Cu with copper foil2Composite granule, to avoid ultra-fine ZrC-ZrB2Powder surface
Adsorb oxygen, the water in air.On the other hand, it prevents in subsequent fusion process, vacuumizing phase, powder is sucked away.
In above-mentioned steps four, the ultra-fine ZrC particle-ZrB2 stick crystalline substance composite granule containing Cu of copper foil sealing is placed on oxygen-free copper block
In the following, after preventing copper from melting, before stirring, nanometer ZrC-ZrB2 ceramics float on copper liquid surface and assemble；The temperature of melting is
1200~1250 DEG C, the mobility that will cause copper liquid when temperature is too low is poor, and stirring action is limited, and temperature is excessively high, is being cast to
In long-time cooling procedure after mold, because specific gravity is small segregation phenomenon occurs for ultra-fine ZrC, ZrB2；The magnetic of application stirs electricity
Stream is 20-30A, time 5-10min, to guarantee ultra-fine ZrC-ZrB2 composite ceramics being uniformly distributed in copper.
In the present invention, Cu flour additive agent is to the ultra-fine ZrC-ZrB containing Cu2Preparing for composite granule is most important.First, add
In thermal process, Cu can react to form Cu between 600~660 DEG C with Zr by solid-state diffusion10Zr7Equal compounds, with temperature
Raising, Cu10Zr7Cu-Zr liquid phase is molten at 895 DEG C, liquid phase is ZrC and ZrB2Formation provide shortcut, when Zr powder with
B4C powder dissolves in Cu-Zr liquid phase, Zr and B4C is combined into stable ZrC and ZrB by fast moving2Ceramics, accelerate ZrC and
ZrB2Synthesis, thus can complete synthesis ZrC and ZrB at 1250 DEG C2, low temperature facilitates ZrC and ZrB2The refinement of partial size.The
Two, as ZrC and ZrB2After being formed in liquid, Cu liquid will increase ZrC, ZrB2The distance between particle, thus contain ZrC and
ZrB2Contact with grow up.Third, Cu have good thermal conductivity, it is possible to increase the cooling rate of synthetic product in cooling procedure,
Product is reduced in the residence time of high temperature, prevents ZrC and ZrB2Grow up.
In the present invention, smelting temperature (1200~1250 DEG C) is with magnetic stirring (5~10min) at this temperature to composite wood
ZrC, ZrB in material2Ceramics keep ultra-fine state and its are uniformly distributed most important.Smelting temperature is too low, magnetic mixing time is too short,
Magnetic mixing effect can be then reduced, so as to cause ZrC-ZrB in composite material2The reunion of ceramics；Temperature is excessively high, magnetic mixing time mistake
Long, in composite material ZrC-ZrB2Meeting grow up, and occur segregation phenomenon in subsequent cooling process.
The present invention is that the preparation of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material opens a new think of
Road, compared with prior art, the invention has the following advantages: (1) utilizes Cu-Zr-B4The reaction synthesis of C mixed-powder contains Cu
Ultra-fine ZrC-ZrB2Composite granule, price ZrC, ZrB ultra-fine far below business2Powder, can reduce ultra-fine ZrC particle and
ZrB2Stick crystalline substance enhances composite material preparation cost；(2) ultra-fine ZrC-ZrB2Compound synthesis is a more slow process (~10
Minute), process control, thus the requirement much more relaxed to raw material, Cu-Zr-B4In C mixed-powder Cu content can 10~
40wt.% variation, the variation range of copper powder size are 0.5~75 μm, B4The size range of C is 14~28 μm；(3) super containing Cu
Thin ZrC-ZrB2Composite granule can be directly used for the preparation of Cu-base composites, save to ZrC-ZrB2The abstraction process of powder.
(4)ZrC-ZrB2The preparation process of/Cu electrode material is simple, and reinforcement is tiny, is evenly distributed；(5) in addition to particle reinforcing effect,
ZrC-ZrB2Ultra-fine ZrC, ZrB in/Cu composite material2Ceramics can be acted on by heterogeneous forming core, promote the refinement of Copper substrate, real
Existing refined crystalline strengthening, improves the mechanical performance of copper.
Detailed description of the invention
Fig. 1 is the ultra-fine ZrC-ZrB containing Cu in the embodiment of the present invention 32The XRD testing result of composite granule；
Fig. 2 is ultra-fine ZrC particle and ZrB in the embodiment of the present invention 32Stick crystalline substance enhances the shape after copper base electrode material corrosion
Looks.
Specific embodiment
In order to be easier to understand technological means of the invention, workflow and effect, below with reference to specific implementation case, into
One step illustrates.
Embodiment 1
A kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material, preparation process are as follows:
1, weighing: by the Cu powder of partial size~0.5 μm, the Zr powder of partial size~45 μm, partial size~14 μm B4C powder is in molar ratio
1.28:3:1 weighing raw material, raw materials are commercial powder.
2, mixing: by load weighted Cu powder, Zr powder, B4C powder and abrading-ball, ball grinder are put into vacuum glove box, wait take out
Argon gas is poured after vacuum to 5~10Pa to normal pressure, and abrading-ball and powder are fitted into ball grinder in inert gas environment, then will
The ball grinder of sealing is put into tumbling ball mill and mixes 10 hours, wherein abrading-ball ZrO2The weight of abrading-ball, abrading-ball and powder
Than being 60 rev/min for the revolving speed of 10:1, ball mill.
3, it charges: the Cu-Zr-B that will be mixed4C powder is put into Al2O3In ceramic boat, then the ceramic boat that powder is housed
It is put into high-temperature tubular atmosphere furnace, after shutting fire door, opening extraction valve, tube-type atmosphere furnace is evacuated to 5 with mechanical pump~
10Pa then shuts extraction valve, opens charge valve, pours Ar gas to 0.06~0.08MPa；Repeatedly pumping, qi of chong channel ascending adversely three times.
4, it heats: to normal pressure (or air pressure high point slightly than normal pressure in furnace), then Ar gas is poured to high-temperature tubular atmosphere furnace
It opens air outlet valve, be continually fed into the Ar gas that flow is 0.5~0.7L/min；Heating rate, maximum temperature are set, tube furnace is pressed
After the heating rate of 30 DEG C/min is heated to 1250 DEG C, then furnace cooling to room temperature, can be obtained ultra-fine ZrC containing Cu and
ZrB2Composite particles.
5, it grinds: ultra-fine ZrC and ZrB by loose state containing Cu2Ceramic grinding is at powder.
6, it seals: by the ultra-fine ZrC-ZrB containing Cu2Powder and copper foil are put into glove box, after extracting vacuum to 5~10Pa
Argon gas is poured to normal pressure, then seals the ZrC-ZrB containing Cu with copper foil2Powder.
7, melting: by the ultra-fine ZrC and ZrB containing Cu of oxygen-free copper block and copper foil sealing2Powder is put by weight 799:1
In vacuum melting furnace, wherein ultra-fine ZrC and ZrB containing Cu2Powder is placed below oxygen-free copper block；Smelting furnace is taken out with mechanical pump
After taking vacuum to about 5Pa, smelting furnace is then heated to 1200~1250 DEG C, melt oxygen-free copper block and is covered in is containing Cu super
The surface of thin ZrC powder；Then 5min is kept the temperature, magnetic stirring is opened, applies the stir current of 20A, make ultra-fine ZrC and ZrB2Powder
5min is rotated jointly with copper liquid；Heating power supply, magnetic stirring power supply are closed, is cast in metal die, is cooled to room temperature
Obtain ZrC-ZrB2Total content is the ultra-fine ZrC particle-ZrB of 0.1wt.%2Stick crystalline substance enhances copper base electrode material.The composite material
Tensile strength be 304MPa, conductivity 96%IACS.
Embodiment 2
A kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material and preparation method thereof, in addition to following,
It is remaining same as Example 1.
In the present embodiment:
(1)Cu-Zr-B4Cu powder, Zr powder, B in C mixed-powder40.91:3:1 is weighed C powder in molar ratio；And mixed-powder exists
It is mixed 14 hours in ball mill, drum's speed of rotation is 50 revs/min；Tube furnace heating rate is 20 DEG C/min；
(2) oxygen-free copper block and the ultra-fine ZrC-ZrB containing Cu2Powder is about put into vacuum melting furnace than 424:1 by weight；
(3) ZrC-ZrB is obtained2Ceramic content is the ultra-fine ZrC-ZrB of 0.2wt.%2/ Cu electrode material.The composite material
Tensile strength be 365MPa, conductivity 92%IACS.
Embodiment 3
A kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material and preparation method thereof, in addition to following,
It is remaining same as Example 1.
In the present embodiment:
(1)Cu-Zr-B4Cu powder diameter is 25 μm in C mixed-powder, B4The partial size of C powder is about 28 μm；Drum's speed of rotation is
70 revs/min；
(2) oxygen-free copper block and the ultra-fine ZrC-ZrB containing Cu2Powder is put into vacuum melting furnace by weight 79:1；
(3) soaking time is 10min, and magnetic stir current is 30A；
(4) ZrC-ZrB is obtained2Ceramic content is the ultra-fine ZrC-ZrB of 1wt.%2/ Cu electrode material.The composite material
Tensile strength is 487MPa, conductivity 89%IACS.
Fig. 1 is the ultra-fine ZrC-ZrB containing Cu2The XRD testing result of composite granule.It will be seen from figure 1 that containing the ultra-fine of Cu
ZrC-ZrB2Only by ZrB in composite granule2, tri- phase composition of ZrC and Cu, do not check zirconium oxide, unreacted Zr or B4C, explanation
Zr and B4C completes conversion for ZrC and ZrB2。
(5) Fig. 2 is ultra-fine ZrC particle and ZrB2Stick crystalline substance enhances the pattern after copper base electrode material corrosion.As shown in Figure 2,
ZrC particle is in Nano grade, and ZrB2The diameter of stick crystalline substance is 50nm~0.2 μm, and ZrC particle and ZrB2Stick crystalline substance is uniformly distributed in
In Cu matrix, apparent agglomeration is not observed.
Embodiment 4
A kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material and preparation method thereof, in addition to following,
It is remaining same as Example 1.
In the present embodiment:
(1)Cu-Zr-B4Cu powder diameter is 75 μm in C mixed-powder, B4C powder diameter is 28 μm, Cu, Zr, B4C massage
You weigh than 3.42:3:1.
Embodiment 5
A kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material and preparation method thereof, in addition to following,
It is remaining same as Example 1.
In the present embodiment:
(1)Cu-Zr-B4Cu powder, Zr powder, B in C mixed-powder40.57:3:1 is weighed C powder in molar ratio.
Claims (5)
1. a kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material preparation method, which is characterized in that described
Ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material is by oxygen-free copper, ultra-fine ZrC particle and ZrB2Stick crystalline substance is constituted,
Wherein, copper content is 99.0~99.9wt.%, ultra-fine ZrC and ZrB2Total content be 0.1~1.0wt.%；
Its step includes:
Step 1: with Cu powder, Zr powder and B4C powder is that raw material prepares the ultra-fine ZrC particle-ZrB containing Cu2Stick crystalline substance composite particles；
Step 2: the ultra-fine ZrC particle-ZrB by loose state containing Cu2Stick crystalline substance composite particles are ground into powder；
Step 3: by the ultra-fine ZrC particle-ZrB containing Cu2Stick crystalline substance composite granule and copper foil are put into glove box, then in indifferent gas
The ultra-fine ZrC particle-ZrB containing Cu is sealed with copper foil in body environment2Stick crystalline substance composite granule；
Step 4: by the ultra-fine ZrC particle-ZrB containing Cu of oxygen-free copper block and copper foil sealing2It is molten that stick crystalline substance composite granule is put into vacuum
In furnace, wherein the ultra-fine ZrC particle-ZrB containing Cu of copper foil sealing2Stick crystalline substance composite granule is placed below oxygen-free copper block；Wait take out
After taking vacuum, smelting furnace is heated to 1200~1250 DEG C, melt oxygen-free copper block and is covered on the ultra-fine ZrC particle-containing Cu
ZrB2The surface of stick crystalline substance composite granule；Then keeping the temperature 5~10min and applying magnetic stirring makes ZrC and ZrB2It is uniformly distributed in Cu liquid
It is interior, it is finally cast in metal die and obtains ultra-fine ZrC particle-ZrB2Stick crystalline substance enhances Cu-base composites；
Wherein, the specific preparation process of step 1 includes the following steps,
Step (1), with Cu powder, Zr powder and B4C powder is raw material, wherein Zr powder and B4C powder molar ratio is the additive amount of 3, Cu powder
For 10wt.%~40wt.%；
Step (2), by load weighted Cu powder, Zr powder, B4C powder, with tumbling ball mill mixing 10~14 in inert gas environment
Hour, obtain Cu-Zr-B4C mixed-powder；
Step (3), by loose Cu-Zr-B4C mixed-powder is put into Al2O3In ceramic boat, then the ceramic boat that powder is housed
It is put into high-temperature tubular atmosphere furnace, then is arranged as inert gas environment；
Step (4) is heated high temperature process furnances by the heating rate of 20~30 DEG C/min, after temperature is increased to 1250 DEG C, with
Furnace is cooled to room temperature, and loose state, ultra-fine ZrC particle-ZrB of the preparation containing Cu can be obtained2Stick crystalline substance composite particles.
2. a kind of preparation of ultra-fine zirconium carbide particle according to claim 1-zirconium boride stick crystalline substance enhancing copper base electrode material
Method, which is characterized in that in step (2), the abrading-ball of the ball mill is ZrO2Abrading-ball, ZrO2The diameter of abrading-ball is 8mm, abrading-ball
Weight ratio with powder is 10:1, and the revolving speed of ball mill is 50~70 revs/min.
3. a kind of preparation of ultra-fine zirconium carbide particle according to claim 1-zirconium boride stick crystalline substance enhancing copper base electrode material
Method, which is characterized in that in step (3), the placement process of inert gas environment are as follows: high-temperature atmosphere furnace is first evacuated to 5~
After 10Pa；Then Ar gas is poured to 0.06~0.08MPa, is evacuated, is inflated three times repeatedly；Finally high-temperature tubular atmosphere furnace is poured
After Ar gas to normal pressure, it is continually fed into the Ar gas that flow is 0.5~0.7L/min.
4. a kind of preparation of ultra-fine zirconium carbide particle according to claim 1-zirconium boride stick crystalline substance enhancing copper base electrode material
Method, which is characterized in that the Cu powder, purity > 99%, average grain diameter are 0.5~75 μm, the Zr powder, purity >
98%, partial size is 45 μm, the B4C powder, purity > 99%, average grain diameter are 14~28 μm.
5. a kind of preparation of ultra-fine zirconium carbide particle according to claim 1-zirconium boride stick crystalline substance enhancing copper base electrode material
Method, which is characterized in that in step 4, the magnetic stir current of application is 20-30A, time 5-10min.
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| JP2552679B2 (en) * | 1987-09-07 | 1996-11-13 | 福田金属箔粉工業株式会社 | Method for manufacturing high hardness composite copper alloy |
| CN102190495B (en) * | 2010-03-18 | 2013-10-30 | 中国科学院上海硅酸盐研究所 | Preparation method for promoting to sinter zirconium boride or zirconium carbide ceramics by using reaction aids |
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| CN103466620B (en) * | 2013-08-20 | 2015-03-25 | 西北农林科技大学 | Method for preparing zirconium carbide/zirconium boride composite powder by solid phase reaction diffusion method |
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| CN105441767B (en) * | 2015-11-17 | 2017-08-11 | 中国工程物理研究院激光聚变研究中心 | A kind of resistance to high temperature oxidation damages ZrB2The preparation method of SiC ZrC W complex phase ceramics |
| CN106904976A (en) * | 2015-12-23 | 2017-06-30 | 雅安百图高新材料有限公司 | The method of preparing aluminum nitride/boron nitride composite ceramic through combustion synthesis |
| CN106431416A (en) * | 2016-09-22 | 2017-02-22 | 铜仁学院 | Zirconium carbide-zirconium diboride complex-phase ceramic powder synthesized through thermal explosion and preparation method thereof |
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