CN108611514A - 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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-powders, which are put into high-temperature tubular atmosphere furnace, is heated to 1250 DEG C, obtains ultra-fine ZrC particles 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 particles ZrB2Stick crystalline substance enhances copper base electrode material.The method of the present invention has the characteristics that at low cost, technique is simple, production efficiency is high, 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 technology
Spot welding is widely used in the industries such as automobile, instrument and aeronautical manufacture, and high temperature and high pressure effect, copper are born 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
One of effective way be to prepare superfine ceramic Reinforced Cu-Base Composites.It is existing studies have shown that nanometer Al2O3Particles Reinforced Cu
Based composites have good mechanical performance, but Al2O3(the resistance coefficient of ceramics almost insulation：1020×10-6Ω·
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 while keeping copper good electric conductivity, improve its mechanicalness
Energy.ZrC-ZrB can be prepared by SHS technology2/ Cu composite materials (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 thereofs.
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.
Invention content
In view of above-mentioned technical problem exists 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, together under the premise of keeping copper good electric conductivity
When efficiently solve the problems, such as that ultra-fine zirconium carbide is expensive with zirconium boride powder price, this method also has that equipment is simple, operation letter
Easily, the advantages such as low, production efficiency is high, 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 particles 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 particles-ZrB containing Cu2Stick crystalline substance composite particles；
Step 2: by ultra-fine ZrC particle-ZrB of the loose state containing Cu2Stick crystalline substance composite particles are ground into powder；
Step 3: by the ultra-fine ZrC particles-ZrB containing Cu2Stick crystalline substance composite granule is put into copper foil in glove box, is then existed
In inert gas environment the ultra-fine ZrC particles-ZrB containing Cu is sealed with copper foil2Stick crystalline substance composite granule；
Step 4: by oxygen-free copper block and the ultra-fine ZrC particles-ZrB containing Cu2Stick crystalline substance composite granule is put into vacuum melting furnace
In, wherein the ultra-fine ZrC particles-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, so that oxygen-free copper block is melted and is covered in the ultra-fine ZrC particles-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 particles-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 ratios are 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-powders；
Step (3), by loose Cu-Zr-B4C mixed-powders are put into ceramic boat, then the ceramic boat equipped with powder
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, waits for that temperature is increased to 1250 DEG C
Afterwards, furnace cooling is to room temperature, you can obtains loose state, the ultra-fine ZrC particles-ZrB containing Cu2Stick crystalline substance composite particles.
The Cu powder, purity>99%, 0.5~75 μm of average grain diameter.
The Zr powder, purity>98%, grain size~45 μm.
The B4C powder, purity>99%, average grain diameter is 14~28 μm.
The oxygen-free copper block, purity>99.97%, oxygen content<0.003%, content of impurities is not more than 0.03%.
The abrading-ball of the ball mill is ZrO2Abrading-ball, ZrO2The weight ratio of a diameter of 8mm of abrading-ball, abrading-ball and powder is 10:
1, the rotating 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 prepared2In ceramic Reinforced Cu base electrode material, ZrC average grain diameters<100nm, ZrB2Stick crystalline substance
A diameter of 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-powders, 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 compounds.
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 is：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-powders are
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 lead to ZrC-ZrB2Ceramics
Synthesis it is incomplete, ZrC-ZrB can be caused slowly excessively2The roughening of ceramics.
In above-mentioned steps two, the ultra-fine ZrC particles-ZrB containing Cu by loose state is needed2Stick crystalline substance is ground into powder, in favor of
ZrC-ZrB in follow-up fusion process2Ceramics being dispersed with stirring in copper liquid.
In above-mentioned steps three, by the nanometer ZrC-ZrB containing Cu2Powder is put into copper foil in glove box, extracts 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 follow-up fusion process, vacuumizing phase, powder is sucked away.
In above-mentioned steps four, the ultra-fine ZrC particles-ZrB2 stick crystalline substance composite granules containing Cu of copper foil sealing are 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 of copper liquid can be caused poor when temperature is too low, stirring action is limited, and temperature is excessively high, is being cast to
In long-time cooling procedure after mold, because proportion is small segregation phenomenon occurs for ultra-fine ZrC, ZrB2；The magnetic stirring electricity of application
Stream is 20-30A, time 5-10min, to ensure ultra-fine ZrC-ZrB2 composite ceramics being uniformly distributed in copper.
In the present invention, Cu flour additive agents are 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 with Zr between 600~660 DEG C by solid-state diffusion10Zr7Etc. compounds, with temperature
Raising, Cu10Zr7Cu-Zr liquid phases are molten at 895 DEG C, liquid phase is ZrC and ZrB2Formation provide shortcut, when Zr powder with
B4C powder dissolves in Cu-Zr liquid phases, Zr and B4C is combined into stable ZrC and ZrB by fast moving2Ceramics, accelerate ZrC and
ZrB2Synthesis, in 1250 DEG C of energy complete synthesis ZrC and ZrB2, low temperature contributes to ZrC and ZrB2The refinement of grain size.The
Two, as ZrC and ZrB2After being formed in liquid, Cu liquid will increase ZrC, ZrB2The distance between particle, to 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
It is long, the ZrC-ZrB in composite material2Meeting 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 advantages that：(1) Cu-Zr-B is utilized4The reaction synthesis of C mixed-powders contains Cu
Ultra-fine ZrC-ZrB2Composite granule, price ZrC, ZrB ultra-fine far below business2Powder, can reduce ultra-fine ZrC particles and
ZrB2Stick crystalline substance enhances composite material manufacturing 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-powders Cu contents can 10~
40wt.% changes, and the variation range of copper powder size is 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 materials is simple, and reinforcement is tiny, is evenly distributed；(5) in addition to particle enhancing effect,
ZrC-ZrB2Ultra-fine ZrC, ZrB in/Cu composite materials2Ceramics 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.
Description of the drawings
Fig. 1 is the ultra-fine ZrC-ZrB containing Cu in the embodiment of the present invention 32The XRD testing results of composite granule；
Fig. 2 is ultra-fine ZrC particles and ZrB in the embodiment of the present invention 32Stick crystalline substance enhances the shape after copper base electrode material corrosion
Looks.
Specific implementation mode
In order to be easier to understand the present invention technological means, workflow and effect, 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：
1, weighing：By the Cu powder of grain size~0.5 μm, the Zr powder of grain size~45 μm, grain size~14 μm B4C powder is in molar ratio
1.28：3：1 weighs raw material, and raw materials are commercial powder.
2, batch mixing：By load weighted Cu powder, Zr powder, B4C powder and abrading-ball, ball grinder are put into vacuum glove box, wait taking out
Argon gas is poured after vacuum to 5~10Pa to normal pressure, 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 10:1, the rotating speed of ball mill is 60 rev/min.
3, it feeds：The Cu-Zr-B that will be mixed4C powder is put into Al2O3In ceramic boat, then the ceramic boat equipped with powder
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 stove), 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, you can obtain ultra-fine ZrC containing Cu and
ZrB2Composite particles.
5, it grinds：By ultra-fine ZrC and ZrB of the loose state containing Cu2Ceramic grinding is at powder.
6, it seals：By the ultra-fine ZrC-ZrB containing Cu2Powder is put into copper foil in 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 by weight 799：1 is put into
In vacuum melting furnace, wherein the ultra-fine ZrC containing Cu and ZrB2Powder 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, oxygen-free copper block is made to melt and is covered in is containing Cu super
The surface of thin ZrC powders；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, you can
Obtain ZrC-ZrB2Total content is the ultra-fine ZrC particles-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-powders4C powder in molar ratio 0.91：3：1 weighs；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 by weight about than 424：1 is put into vacuum melting furnace；
(3) ZrC-ZrB is obtained2Ceramic content is the ultra-fine ZrC-ZrB of 0.2wt.%2/ Cu electrode materials.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 powders diameter is 25 μm in C mixed-powders, B4The grain 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 by weight 79：1 is put into vacuum melting furnace；
(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 materials.The composite material
Tensile strength is 487MPa, conductivity 89%IACS.
Fig. 1 is the ultra-fine ZrC-ZrB containing Cu2The XRD testing results 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 particles and ZrB2Stick crystalline substance enhances the pattern after copper base electrode material corrosion.As shown in Figure 2,
ZrC particles are in Nano grade, and ZrB2A diameter of 50nm~0.2 μm of stick crystalline substance, and ZrC particles and ZrB2Stick crystalline substance is uniformly distributed in
In Cu matrixes, 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 powders diameter is 75 μm in C mixed-powders, B4C powder diameters are 28 μm, Cu, Zr, B4C massages
That ratio 3.42：3：1 weighs.
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-powders4C powder in molar ratio 0.57：3：1 weighs.
Claims (7)
1. a kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhances copper base electrode material, which is characterized in that by oxygen-free copper, ultra-fine
ZrC particles 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.%.
2. a kind of preparation method of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material, step include：
Step 1: with Cu powder, Zr powder and B4C powder is that raw material prepares the ultra-fine ZrC particles-ZrB containing Cu2Stick crystalline substance composite particles；
Step 2: by ultra-fine ZrC particle-ZrB of the loose state containing Cu2Stick crystalline substance composite particles are ground into powder；
Step 3: by the ultra-fine ZrC particles-ZrB containing Cu2Stick crystalline substance composite granule is put into copper foil in glove box, then in indifferent gas
In body environment the ultra-fine ZrC particles-ZrB containing Cu is sealed with copper foil2Stick crystalline substance composite granule；
Step 4: by the ultra-fine ZrC particles-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 particles-ZrB containing Cu of copper foil sealing2Stick crystalline substance composite granule is placed below oxygen-free copper block；It waits taking out
After taking vacuum, smelting furnace is heated to 1200~1250 DEG C, oxygen-free copper block is made to melt and is covered in the ultra-fine ZrC particles-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 particles-ZrB2Stick crystalline substance enhances Cu-base composites.
3. a kind of preparation of ultra-fine zirconium carbide particle according to claim 2-zirconium boride stick crystalline substance enhancing copper base electrode material
Method, which is characterized in that 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 ratios are the additive amount of 3, Cu powder
For 10wt.%~40wt.%；
Step (2), by load weighted Cu powder, Zr powder, B4C powder mixes 10~14 in inert gas environment with tumbling ball mill
Hour, obtain Cu-Zr-B4C mixed-powders；
Step (3), by loose Cu-Zr-B4C mixed-powders are put into Al2O3In ceramic boat, then the ceramic boat equipped with powder
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
Stove is cooled to room temperature, you can obtains loose state, prepares the ultra-fine ZrC particles-ZrB containing Cu2Stick crystalline substance composite particles.
4. a kind of preparation method of nano-zirconium carbide ceramic strengthening copper base electrode material according to claim 3, feature
It is, in step (2), the abrading-ball of the ball mill is ZrO2Abrading-ball, ZrO2A diameter of 8mm of abrading-ball, the weight of abrading-ball and powder
Than being 10:1, the rotating speed of ball mill is 50~70 revs/min.
5. a kind of preparation method of nano-zirconium carbide ceramic strengthening copper base electrode material according to claim 3, feature
It is, in step (3), the placement process of inert gas environment is：After high-temperature atmosphere furnace is first evacuated to 5~10Pa；Then
Ar gas is poured to 0.06~0.08MPa, is evacuated, inflated three times repeatedly；Ar gas finally is poured to normal pressure to high-temperature tubular atmosphere furnace
Afterwards, it is continually fed into the Ar gas that flow is 0.5~0.7L/min.
6. a kind of preparation of ultra-fine zirconium carbide particle according to claim 2-zirconium boride stick crystalline substance enhancing copper base electrode material
Method, which is characterized in that the Cu powder, purity>99%, average grain diameter is 0.5~75 μm, the Zr powder, purity>
98%, grain size is 45 μm, the B4C powder, purity>99%, average grain diameter is 14~28 μm.
7. a kind of preparation of ultra-fine zirconium carbide particle according to claim 2-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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