CN108284223A - A method of preparing high strength heat resistant copper alloy powder - Google Patents
A method of preparing high strength heat resistant copper alloy powder Download PDFInfo
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- CN108284223A CN108284223A CN201710756694.5A CN201710756694A CN108284223A CN 108284223 A CN108284223 A CN 108284223A CN 201710756694 A CN201710756694 A CN 201710756694A CN 108284223 A CN108284223 A CN 108284223A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
Include that the oxide for adding phase as dispersion-strengtherning is provided using soluble salt solutions this application discloses a kind of method preparing high strength heat resistant copper alloy powder, copper alloy powder is formed in the oxide particle surface coated copper of precipitation.Method provided by the present application can ensure the full and uniform mixing of solution, and the reaction was complete, and mixing power is strong, and temperature, flow velocity are controllable.Obtain the subsphaeroidal powder of even particle size distribution.By copper clad oxide composite end filtering means dehydration, vacuum drying.Screening obtains 73um product powder below.Recovery rate can reach 95%.
Description
Technical field
This application involves a kind of methods preparing copper alloy powder, and in particular to a kind of to prepare high strength heat resistant copper alloy powder
The method at end.
Background technology
Metallic copper is widely used due to its high heat-conductivity conducting in military-civil industrial production.But the high annealing of copper
Softening properties limit Enlargement and the performance boost of copper.The annealing temperature for being improved copper using alloyage process at present, is such as welded
Connect the Cr-Zr-Cu alloys generally used in industry.But beginning softening temperature is still relatively low, cannot meet demand of industrial production.
High strength heat resistant copper alloy is a kind of dispersion strengthening composites, the even dispersion superfine oxide in Copper substrate
Grain comes the movement of pinning dislocation and limitation micro-crack development.It has very excellent high temperature resistance softening properties, while having concurrently good
Conduction, heat conductivility, be one kind best in current all heat-resisting high-conductivity copper alloys.
High-conductive heat-resistant copper alloy be manufacture welding profession in resistance welding electrode and robot welding system ignition tip it is new
Proximate matter material.Because resistance welding electrode needs are continually contacted with workpiece under high temperature, high pressure, therefore abrasion is very fast, needs
It is frequently replaced in use.Such as the chrome zirconium copper alloy (Cu-Cr-Zr series) largely used at present starts at 500 DEG C or so
Softening, therefore well damage when use, need frequently to replace, welding cost are made to greatly improve, and have also seriously affected welding and have set
Standby service efficiency.In addition, with the development of automobile industry in recent years, the galvanized sheet of excellent corrosion resistance has obtained widely answering
With.However when the progress spot welding of chrome zirconium copper alloy material electrodes, the zinc in steel plate coating is easy in infiltration to electrode material, is made
Electrode bonds together with steel plate, influences bond quality and automatic assembly line can be caused to interrupt, productivity is caused to decline.High intensity
Softening temperature can be increased to 900 degree by heat resistant copper alloy, simultaneously because disperse oxide has the infiltration for limiting zinc, be had anti-
The effect of bonding.And conductivity > 80%IACS.2~5 times of electrode life can be improved.
The powder properties of high strength heat resistant copper alloy obtained by the preparation method of existing high strength heat resistant copper alloy are unstable,
Quality can not accurately control, and lead to the unstable quality of final high strength heat resistant copper alloy, cannot be satisfied domestic and international market needs.
Invention content
In view of drawbacks described above in the prior art or deficiency, it is intended to provide a kind of high strength heat resistant copper alloy powder for preparing
Method.
In a first aspect, the application provides a kind of method preparing high strength heat resistant copper alloy powder, including with soluble-salt
Solution provides the oxide that phase is added as dispersion-strengtherning, and copper alloy powder is formed in the oxide particle surface coated copper of precipitation
End.Copper clad nano-oxide powder obtained by the application is submicron order, and impurity content is low, epigranular, and granule-morphology is close
The oxide powder of spherical shape, granular core is nano particle, and dispersion-strengtherning phase still keeps nano-scale after ensure that sintering.
Preferably, the above method includes the following steps:
Step 1:The oxide powder that phase is added as dispersion-strengtherning is dissolved in sodium hydroxide solution, being prepared into can
Dissolubility salting liquid;
Step 2:The soluble salt solutions input channel synthesizer that step 1 is obtained, it is defeated into the pipeline synthesizer
Enter copper ion source solution and reducing agent;Make the oxide that phase is added as dispersion-strengtherning using pH adjusting agent to reduce system pH
Particle is precipitated;Copper ion is reduced agent reduction, and cladding is precipitated in the oxide particle surface for adding phase as dispersion-strengtherning, is formed
Copper alloy powder suspension;Suspension obtains finished product copper alloy powder crude product after filtration washing is dried and is sieved;
Step 3:Copper alloy powder crude product obtained by step 2 anneal at 400-800 DEG C restore 1.5-2.5h to get at
Product.
Preferably, the oxide for adding phase described in step 1 as dispersion-strengtherning is aluminium oxide, yttrium oxide, titanium dioxide
Silicon, boron oxide, cerium oxide are one or more in lanthana.
Preferably, sodium hydroxide mass concentration is 50% in sodium hydroxide solution described in step 1.
Preferably, pipeline synthesizer includes the interior strong rotational flow pipeline for being equipped with strong mixer in step 2;Strong mixer
Including the helicoidal gear and screw rod being connected;The motor being arranged on pipeline synthesizer is connect with helicoidal gear;
Helicoidal gear is connect with one end of strong rotational flow pipeline, and strong another end of rotational flow pipeline is material outlet;Screw rod is located at strong
In rotational flow pipeline;Strong rotational flow pipeline is equipped with liquid-inlet and sample tap;The liquid synthesis stage of strong rotational flow pipeline is equipped with heat preservation
Layer, insulating layer are equipped with heating agent outlet and Heating medium.It is designed with 2 advantages in this way:(1) increase turbulent extent, material mixing
Strongly, strengthen alternate transmission significantly;(2) it can provide bigger than traditional reaction kettle than volumetric heat transfer area, avoid to reactant
There is temperature gradient in reacting fluid, to control the growth rate of crystal, reduce the generation of agglomeration in the reactor.Pipeline
The advantage of synthetic method is to ensure the full and uniform mixing of solution, and the reaction was complete, and mixing power is strong, and temperature, flow velocity are controllable.It obtains
The subsphaeroidal powder of even particle size distribution.
Preferably, the soluble salt solutions a concentration of 15-25g/L, input speed 20-50mL/ in step 2
min.Soluble salt solutions excessive concentration is too low and input speed is too fast can cause the copper particle generated coarse slowly excessively, spherical
Degree is poor.Copper particle fine uniform when experiment shows to select above-mentioned concentration and speed, sphericity are high.
Preferably, copper ion source solution described in step 2 is the copper-bath of 0.25-0.75mol/L, input speed
For 100-250mL/min.Copper ion source solution concentration is excessively high too low and input speed is too fast can lead to the copper generated slowly excessively
Grain is coarse, and sphericity is poor.Copper particle fine uniform when experiment shows to select above-mentioned concentration and speed, sphericity are high.
Preferably, reducing agent described in step 2 is hydrazine hydrate, input speed 120-300mL/min.Hydrazine hydrate is liquid
Body reducing agent, reproducibility is strong, and is in alkalescence conducive to control input speed and flow, and effect on environment is born very little, do not pierced
Swash property, it is environmental-friendly to industrialized production.
Preferably, pH adjusting agent described in step 2 is the ammonium hydroxide of concentration 0.25-8.0mol/L, input speed 25-
50mL/min.PH adjusting agent excessive concentration is too low and input speed is too fast can cause the copper particle generated coarse slowly excessively, spherical
Degree is poor.Copper particle fine uniform when experiment shows to select above-mentioned concentration and speed, sphericity are high.
Preferably, the soluble salt solutions, copper ion source solution, reducing agent and pH adjusting agent input the pipeline simultaneously
Synthesizer stops the input of the pH adjusting agent when pH value is down to 10-13 in the pipeline synthesizer.
Preferably, strong mixer is equipped in the pipeline synthesizer;The strong mixer is molten in the soluble-salt
Liquid starts while input, mixing speed 100-240r/min..
Preferably, the pipeline synthesizer temperature is 60-80 DEG C.
Preferably, the oxide powder for adding phase described in step 1 as dispersion-strengtherning accounts for copper alloy powder obtained by step 2
Last finished weight percentage is 0.1%-6.0%.
Second aspect, the application a kind of copper alloy powder obtained by the above method and copper alloy powder processing is also provided and
At other form copper alloys, as copper alloy block, copper alloy tube, copper alloy plate, copper alloy column and copper alloy powder processing and
At product, such as resistance welding electrode.
The application has the advantages and positive effects of:Since the application uses technical solution as above, it is ensured that solution
Full and uniform mixing, the reaction was complete, and mixing power is strong, and temperature, flow velocity are controllable.Obtain the subsphaeroidal powder of even particle size distribution.It will
Copper clad oxide composite end filtering means dehydration, vacuum drying.Screening obtains 73um product powder below.Recovery rate can reach
To 95%.
The technical issues of being solved in addition to the application described above, constitute technical solution technical characteristic and by these
Except advantage caused by the technical characteristic of technical solution, wrapped in other technologies problem that the application can solve, technical solution
Advantage caused by the other technical characteristics contained and these technical characteristics, makees further details of hereinafter in conjunction with attached drawing
Explanation.
Description of the drawings
By reading a detailed description of non-restrictive embodiments in the light of the attached drawings below, the application's is other
Feature, objects and advantages will become more apparent upon:
Fig. 1 is pipeline synthesizer structural schematic diagram provided by the embodiments of the present application.
In figure:1, motor;2, helicoidal gear;3, sample tap;4, inlet;5, heating agent exports;6, strong rotational flow pipeline;
7, insulating layer;8, Heating medium;9, analytical sampling mouth.
Specific implementation mode
The application is described in further detail with reference to the accompanying drawings and examples.It is understood that this place is retouched
The specific embodiment stated is used only for explaining related invention, rather than the restriction to the invention.It also should be noted that in order to
Convenient for description, is illustrated only in attached drawing and invent relevant part.
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The application is described in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
Embodiment 1:
Alumina powder by the ultra-fine purity of 125g more than 99.99 is put into the sodium hydroxide solution that mass concentration is 50%
In, it is configured to the solution of 25g/L.The anhydrous cupric sulfate of 25.0kg is dissolved in 250L water, copper-bath is configured to.
By oxide soluble salt solutions input channel synthesizer, the speed 20mL/min of control input liquid.Simultaneously will
In copper-bath input channel synthesizer, the speed 250mL/min of control input liquid.By hydrazine hydrate input channel synthesizer
In, the speed of control input liquid is 280mL/min.Start strong mixer, mixing speed 120r/min simultaneously.Keep pipe
80 DEG C of road synthesizer temperature.By in ammonia spirit (a concentration of 0.5mol/L) input channel synthesizer, control inputs the speed of liquid
Degree is 50mL/min.It waits for and closes ammonium hydroxide valve when pH value is 12 in pipeline synthesizer.The copper clad nano-oxide powder of generation
Last suspension is flowed out from material outlet.Suspension is filtered washing, then 80 DEG C of vacuum dryings, the time is 4 hours, is used
Powder sample 9.8kg is obtained after the screening of 200 mesh screens.
Base is made in copper clad oxide composite end progress isostatic cool pressing, cause is sintered into hydrogen shield sintering furnace
Densification.The high strength heat resistant copper alloy bar of φ 15mm is hot extruded into after sintering.Carry out hardness determination and conductivity detection.Measure Lip river
Family name's hardness HRB values are 82, use International Annealed Copper Standard conductivity for 95%IACS.
High annealing hardness test, after 900 DEG C keep the temperature 0.5 hour, measurement surface hardness is 76, and high annealing softens amplitude
It is 7.3%.
Embodiment 2:
Alumina powder and the ultra-fine purity of 62.5g by the ultra-fine purity of 62.5g more than 99.99 are more than 99.99 yttrium oxide
Powder is put into sodium hydroxide solution (50%), is configured to the solution of 25g/L.The anhydrous cupric sulfate of 30.0kg is dissolved in 250L
In water, it is configured to copper-bath.By oxide soluble salt solutions input channel synthesizer, the speed of control input liquid
25mL/min.Simultaneously by copper-bath input channel synthesizer, control inputs the speed 230mL/min of liquid.It will hydration
In hydrazine input channel synthesizer, the speed of control input liquid is 300mL/min.Start strong mixer, mixing speed simultaneously
For 120r/min.Keep 80 DEG C of pipeline synthesizer temperature.By in ammonia spirit (a concentration of 0.5mol/L) input channel synthesizer,
The speed of control input liquid is 50mL/min.It waits for and closes ammonium hydroxide valve when pH value is 11.6 in pipeline synthesizer.It generates
Copper clad nano-oxide powder suspension is flowed out from material outlet.Suspension is filtered washing, then 80 DEG C of vacuum are dried
Dry, the time is 4 hours, and powder sample 9.7kg is obtained after being sieved with 200 mesh screens.
Base is made in copper clad oxide composite end progress isostatic cool pressing, cause is sintered into hydrogen shield sintering furnace
Densification.The high strength heat resistant copper alloy bar of φ 15mm is hot extruded into after sintering.Carry out hardness determination and conductivity detection.It measures hard
It is 85 to spend HRB values, conductivity 90%IACS.High annealing hardness test, after 900 DEG C keep the temperature 0.5 hour, measurement surface hardness
It is 79, it is 7.1% that high annealing, which softens amplitude,.
Embodiment 3
SiO 2 powder by the ultra-fine purity of 10g more than 99.99 is put into sodium hydroxide solution (50%), is configured to
The solution of 15g/L.The anhydrous cupric sulfate of 25.0kg is dissolved in 625L water, copper-bath is configured to.Oxide is solvable
Property salting liquid input channel synthesizer, control input liquid speed 50mL/min.Copper-bath input channel is closed simultaneously
In growing up to be a useful person, the speed 100mL/min of control input liquid.By in hydrazine hydrate input channel synthesizer, control inputs the speed of liquid
Degree is 120mL/min.Start strong mixer, mixing speed 100r/min simultaneously.Keep 80 DEG C of pipeline synthesizer temperature.It will
In ammonia spirit (a concentration of 0.25mol/L) input channel synthesizer, the speed of control input liquid is 25mL/min.Wait for pipe
Ammonium hydroxide valve is closed when pH value is 13 in road synthesizer.The copper clad nano-oxide powder suspension of generation is from material outlet stream
Go out.Suspension is filtered washing, then 60 DEG C of vacuum dryings, the time is 5 hours, and powder is obtained after being sieved with 200 mesh screens
Last sample 9.6kg.
Base is made in copper clad oxide composite end progress isostatic cool pressing, cause is sintered into hydrogen shield sintering furnace
Densification.The high strength heat resistant copper alloy bar of φ 15mm is hot extruded into after sintering.Carry out hardness determination and conductivity detection.It measures hard
It is 83 to spend HRB values, conductivity 92%IACS.High annealing hardness test, after 900 DEG C keep the temperature 0.5 hour, measurement surface hardness
It is 77, it is 7.2% that high annealing, which softens amplitude,.
Embodiment 4
Boron oxide powder, the ultra-fine purity of 200g by the ultra-fine purity of 200g more than 99.99 are more than 99.99 ceria oxide powder
Lanthana with the ultra-fine purity of 150g more than 99.99 is put into sodium hydroxide solution (50%), is configured to the solution of 20g/L.It will
The anhydrous cupric sulfate of 25.0kg is dissolved in 250L water, is configured to copper-bath.By oxide soluble salt solutions input pipe
Road synthesizer, the speed 25mL/min of control input liquid.Simultaneously by copper-bath input channel synthesizer, control inputs
The speed 200mL/min of liquid.By in hydrazine hydrate input channel synthesizer, the speed of control input liquid is 200mL/min.Together
Shi Qidong strong mixers, mixing speed 240r/min.Keep 80 DEG C of pipeline synthesizer temperature.Ammonia spirit is (a concentration of
8mol/L) in input channel synthesizer, the speed of control input liquid is 30mL/min.It is 10 to wait for pH value in pipeline synthesizer
When close ammonium hydroxide valve.The copper clad nano-oxide powder suspension of generation is flowed out from material outlet.Suspension was carried out
Filter washing, then 80 DEG C of vacuum dryings, time are 3 hours, and powder sample 9.8kg is obtained after being sieved with 200 mesh screens.
Base is made in copper clad oxide composite end progress isostatic cool pressing, cause is sintered into hydrogen shield sintering furnace
Densification.The high strength heat resistant copper alloy bar of φ 15mm is hot extruded into after sintering.Carry out hardness determination and conductivity detection.It measures hard
It is 85 to spend HRB values, conductivity 91%IACS.High annealing hardness test, after 900 DEG C keep the temperature 0.5 hour, measurement surface hardness
It is 78, it is 8.2% that high annealing, which softens amplitude,.
The application also provides the pipeline synthesizer used in a kind of above-described embodiment, and structure is as shown in Figure 1.
As shown in Figure 1, pipeline synthesizer includes sequentially connected initial segment, interlude and latter end.Per segment pipe synthesizer
Including the interior strong rotational flow pipeline 6 equipped with strong mixer;Strong mixer includes the helicoidal gear 2 and screw rod being connected
(not shown);The motor 1 being arranged on pipeline synthesizer is connect with helicoidal gear 2;Helicoidal gear 2 and strong cyclone pipe
6 one end of road connects, and 6 another end of strong rotational flow pipeline is material outlet;Screw rod is located in strong rotational flow pipeline 6.By liquid flow
The initial end of dynamic direction description, the strong rotational flow pipeline of initial segment 6 is provided with multiple inlets 4 and a sample tap 3, interlude and end
Analytical sampling mouth 9 is equipped on the strong rotational flow pipeline of section, after the completion of the material outlet of the end of the strong rotational flow pipeline of latter end 6 is for reacting
Discharging.The strong rotational flow pipeline of the material outlet of the strong rotational flow pipeline of initial segment 6 and interlude 6 is at interlude helicoidal gear
Connection, the strong rotational flow pipeline of the material outlet of the strong rotational flow pipeline of interlude 6 and latter end 6 are connect at latter end helicoidal gear.
The liquid synthesis stage (remove inlet part and interconnecting piece grades) of strong rotational flow pipeline 6 is equipped with insulating layer 7, is set on insulating layer 7
There are heating agent outlet 5 and Heating medium 8, to ensure 6 temperature of strong rotational flow pipeline.Soluble salt solutions, copper-bath, hydrazine hydrate and
Ammonium hydroxide starts strong mixer simultaneously from different inlet input channel synthesizers, increases turbulent extent, and material mixing is strong
It is strong, strengthen alternate transmission significantly;It can be provided to reactant bigger than traditional reaction kettle than volumetric heat transfer area, avoid reaction stream
There is temperature gradient in body, to control the growth rate of crystal, reduce the generation of agglomeration in the reactor.Pipeline synthetic method
Advantage be to ensure the full and uniform mixing of solution, the reaction was complete, and mixing power is strong, and temperature, flow velocity are controllable;It is anti-in input
Ying Bianxiang latter end material outlets flow, and mixing evenly, reacts more abundant, products obtained therefrom grain size smaller, sphericity higher.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.People in the art
Member should be appreciated that invention scope involved in the application, however it is not limited to technology made of the specific combination of above-mentioned technical characteristic
Scheme, while should also cover in the case where not departing from the inventive concept, it is carried out by above-mentioned technical characteristic or its equivalent feature
Other technical solutions of arbitrary combination and formation.Such as features described above has similar work(with (but not limited to) disclosed herein
Can technical characteristic replaced mutually and the technical solution that is formed.
Claims (11)
1. a kind of method preparing high strength heat resistant copper alloy powder, which is characterized in that including providing work with soluble salt solutions
The oxide that phase is added for dispersion-strengtherning forms copper alloy powder in the oxide particle surface coated copper of precipitation.
2. the method according to claim 1 for preparing high strength heat resistant copper alloy powder, which is characterized in that including following step
Suddenly:
Step 1:The oxide powder for adding phase as dispersion-strengtherning is dissolved in sodium hydroxide solution, solubility is prepared into
Salting liquid;
Step 2:The soluble salt solutions input channel synthesizer that step 1 is obtained, copper is inputted into the pipeline synthesizer
Ion source solution and reducing agent;Make the oxide particle that phase is added as dispersion-strengtherning using pH adjusting agent to reduce system pH
It is precipitated;Copper ion is reduced agent reduction, and cladding is precipitated in the oxide particle surface for adding phase as dispersion-strengtherning, forms copper and closes
Bronze end suspension;Suspension obtains copper alloy powder crude product after filtration washing is dried and is sieved;
Step 3:Copper alloy powder crude product obtained by step 2 is annealed into reduction 1.5-2.5h to get finished product at 400-800 DEG C.
3. the method according to claim 2 for preparing high strength heat resistant copper alloy powder, which is characterized in that institute in step 1
It is aluminium oxide, yttrium oxide, silica, boron oxide, cerium oxide, in lanthana to state and add the oxide of phase as dispersion-strengtherning
It is one or more.
4. the method according to claim 2 for preparing high strength heat resistant copper alloy powder, which is characterized in that institute in step 2
It includes the interior strong rotational flow pipeline for being equipped with strong mixer to state pipeline synthesizer;The strong mixer includes that the spiral being connected passes
Dynamic device and screw rod;The motor being arranged on the pipeline synthesizer is connect with the helicoidal gear;The spiral passes
Dynamic device is connect with one end of strong rotational flow pipeline, and strong another end of rotational flow pipeline is material outlet;The screw rod
In the strong rotational flow pipeline;The strong rotational flow pipeline is equipped with liquid-inlet and sample tap;The liquid of the strong rotational flow pipeline
Body synthesis stage is equipped with insulating layer, and insulating layer is equipped with heating agent outlet and Heating medium.
5. the method according to claim 2 for preparing high strength heat resistant copper alloy powder, which is characterized in that in step 2
A concentration of 15-25g/L of soluble salt solutions, input speed 20-50mL/min.
6. the method according to claim 2 for preparing high strength heat resistant copper alloy powder, which is characterized in that institute in step 2
State the copper-bath that copper ion source solution is 0.25-0.75mol/L, input speed 100-250mL/min.
7. the method according to claim 2 for preparing high strength heat resistant copper alloy powder, which is characterized in that institute in step 2
It is hydrazine hydrate, input speed 120-300mL/min to state reducing agent.
8. the method according to claim 2 for preparing high strength heat resistant copper alloy powder, which is characterized in that institute in step 2
State the ammonium hydroxide that pH adjusting agent is concentration 0.25-8.0mol/L, input speed 25-50mL/min.
9. the method according to claim 2 for preparing high strength heat resistant copper alloy powder, which is characterized in that the solubility
Salting liquid, copper ion source solution, reducing agent and pH adjusting agent input the pipeline synthesizer simultaneously, wait in the pipeline synthesizer
PH value stops the input of the pH adjusting agent when being down to 10-13.
10. the method according to claim 2 for preparing high strength heat resistant copper alloy powder, which is characterized in that in step 1
The oxide powder that phase is added as dispersion-strengtherning accounts for copper alloy powder finished weight percentage obtained by step 2
0.1%-6.0%.
11. the copper alloy powder and copper alloy powder obtained by a kind of claim 1-12 any one of them methods are process
Copper alloy block, copper alloy tube, copper alloy plate, copper alloy column.
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