CN106363190B - A kind of silver-nickel-graphite alkene alloy material and preparation method thereof - Google Patents
A kind of silver-nickel-graphite alkene alloy material and preparation method thereof Download PDFInfo
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- CN106363190B CN106363190B CN201610827041.7A CN201610827041A CN106363190B CN 106363190 B CN106363190 B CN 106363190B CN 201610827041 A CN201610827041 A CN 201610827041A CN 106363190 B CN106363190 B CN 106363190B
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Abstract
The present invention relates to technical field of alloy material, and in particular to a kind of silver nickel graphene alloy material and preparation method thereof, the preparation method of the silver nickel graphene alloy material includes the following steps：Step 1: the preparation of silver-colored graphene composite powder：Including（1）The preparation of each solution,（2）The preparation of silver-colored graphene composite powder and（3）Cleaning, dry and screening, Step 2: the recombination reaction of nickel and silver-colored graphene composite powder：Including（1）Dry,（2）Mixed powder,（3）Isostatic pressing,（4）Sintering processes and（5）Extrusion forming, the preparation method have simple for process, the high advantage of production efficiency；In addition, silver-colored nickel graphene alloy material made from the preparation method is uniformly dispersed, stability is high, have the advantages that good heat conductivity, erosion property can be got well and hardness is strong.
Description
Technical field
The present invention relates to technical field of alloy material, and in particular to a kind of silver-nickel-graphite alkene alloy material and its preparation side
Method.
Background technology
Silver metal is a kind of metal material with excellent conductive performance, however silver metal is few in nature storage, valence
Lattice are also relatively expensive, and in practical application, silver metal can't be widely used in conductive production field.Further, since silver metal is hard
It spends poor, so that the tensile strength of silver wire is also poor, further limits application of the silver metal in conductive field in this way.
The prior art uses that unlike material is compound with silver metal, to enhance the performance of silver metal, wherein nickel material has
Preferable ductility, medium hardness and good corrosion resistance, and nickel derives from a wealth of sources, it is cheap, by nickel and silver metal
The performance that alloy material is greatly improved silver metal is made, which has good electric conductivity, thermal conductivity, electrical arc erosion
Property, electroerosion, wearability and improve silver metal intensity, and then expand the use scope of silver, and the silver-nickel is made
It is widely used in all kinds of switches, controller, voltage regulator, breaker, electrical apparatus for vehicle use, magnetic starter etc. for contact material.
However the silver-nickel material prepared in the prior art has that dispersion is uneven, stability is poor, so that
The problem that silver-nickel heat conductivility is poor, electroerosion poor performance and hardness are weak cannot preferably be applied to all kinds of switches, control
Device, voltage regulator, breaker, electrical apparatus for vehicle use, magnetic starter etc..In addition, the method for preparing silver-nickel material is also deposited
In complex process, the defect of low production efficiency, the popularization of silver-nickel material is hindered in this way, and therefore, it is a kind of new that there is an urgent need for developings
Technique is to optimize the performance of silver-nickel.
Invention content
For the prior art, there are above-mentioned technical problems, and it is an object of the present invention to provide a kind of silver-nickel-graphite alkene to close
The preparation method of golden material, this method have the advantages that simple for process, production efficiency is high.
For the prior art there are above-mentioned technical problem, the second purpose of the present invention is to provide one kind to be uniformly dispersed, stablizes
Property high silver-nickel-graphite alkene alloy material, which has good heat conductivity, erosion property can well and strong excellent of hardness
Point.
One of to achieve the above object, the present invention provides following technical scheme：
A kind of preparation method of silver-nickel-graphite alkene alloy material is provided, it is characterized in that：Include the following steps：
Step 1, the preparation of silver-colored graphene composite powder
(1) preparation of each solution
The preparation of silver ammino solution：Pure water is weighed, silver nitrate is added into pure water, is then added ammonium hydroxide, agitating solution is to clear
It is clear well-illuminated, silver ammino solution is made；
The preparation of reducing agent solution：Reducing agent solution is weighed, and is diluted with pure water, required reducing agent solution is made；
The preparation of graphene solution：Pure water is weighed, graphene powder is added into pure water, is dispersed with stirring certain time, makes
Graphene powder is uniformly suspended in pure water, and graphene solution is made；
(2) preparation of silver-colored graphene composite powder：Step 1 (1) is added in silver ammino solution made from step 1 (1) to be made
Graphene solution in, stir certain time, then instill step 1 (1) prepare reducing agent solution, silver-colored graphite is obtained by the reaction
Alkene composite granule；
(3) it cleans, dry and screening：
A) it cleans：Silver-colored graphene composite powder made from (2) in step 1 is filtered into cleaning so that silver-colored graphene is compound
Powder is loose, no ammonia taste；
B) dry：By the silver-colored graphene composite powder drying after cleaning, calcined after drying；
C) it sieves：Silver-colored graphene composite powder ball milling after calcining is answered the silver-colored graphene after ball milling after removing ball material
Fine powder, as finished product silver graphene composite powder are obtained after closing powder sieving；
Step 2, the recombination reaction of nickel and silver-colored graphene composite powder
(1) dry：By silver powder, nickel powder, finished product silver graphene composite powder made from step 1 is respectively dried, for use；
(2) powder is mixed：Nickel powder after drying is sufficiently mixed uniformly with finished product silver-nickel graphene alloy powder, is then added
Silver powder continues to be sufficiently mixed uniformly, and mixed powder is made；
(3) isostatic pressing：Mixed powder made from step 2 (2) is subjected to pressurized treatments, silver-nickel-graphite alkene is made
Silver ingot；
(4) sintering processes：Silver made from step 2 (3)-nickel-graphite alkene silver ingot is sintered, the silver-sintered
Nickel-graphite alkene silver ingot；
(5) extrusion forming：The silver that step 2 (4) is obtained-nickel-graphite alkene silver ingot the pre-heat treatment, then extrusion process, obtains
To silver-nickel-graphite alkene alloy material.
Wherein, in the preparation process of (1) silver ammino solution in the step 1, the silver nitrate, the ammonium hydroxide with it is described
The mass ratio of pure water is 1:0.5~5:1.5~10, a concentration of the 5%~30% of the ammonium hydroxide；
In the preparation process of (1) reducing solution in the step 1, the reducing agent be hydrazine hydrate, the hydrazine hydrate with
The mass ratio of pure water is 1:1~8；
In the preparation process of (1) graphene solution in the step 1, the mass ratio of the Graphene powder and pure water is
1:10~100, and 1h~3h is dispersed with stirring by ultrasonic vibration.
Wherein, the silver ammino solution, described in the preparation process of (2) in the step 1 silver-colored graphene composite powder
Mass ratio between reducing agent solution and the graphene solution is 1:10:50.
Wherein, in (3) cleaning, drying and the screening step in the step 1, the drying temperature in the b) drying steps
Degree is 100 DEG C~400 DEG C, and drying time is 3h~6h, and calcination temperature is 400 DEG C~700 DEG C, and calcination time is 2h~4h；Institute
It is 0.5h~2h, ratio of grinding media to material 2 to state the Ball-milling Time during c) screening is rapid:1, the mesh number of sieving is the mesh of 80 mesh~200.
Wherein, in (1) drying steps in the step 2, drying temperature is 60 DEG C~100 DEG C, drying time 0.5h
~1.5h.
Wherein, (2) in the step 2 are mixed in powder step, the nickel powder, the silver-colored graphene composite powder with it is described
The mass ratio of silver powder is 1:0.5~1:0.5~3, the nickel powder and the finished product silver graphene composite powder are mixed by plough type
Powder machine is sufficiently mixed uniformly, after the well-mixed nickel powder and the finished product silver graphene composite powder is added in the silver powder,
It is uniform to first pass through manual mixing, then powder machine is mixed by plough type and is sufficiently mixed uniformly.
Wherein, in (3) isostatic pressing step in the step 2, the mixed powder is placed in isostatic pressing machine and is added
Pressure processing, input amount are 10kg~30kg, and pressure is 50MPa~300MPa, and it is 1min~10min to be kept for the time of pressurization.
Wherein, in (4) sintering processes step in the step 2, by silver made from step 2 (3)-nickel-graphite alkene silver
Ingot is put into pit furnace, first with 200 DEG C~500 DEG C heat preservation 0.5h~2h, then heats to 500 DEG C~800 DEG C heat preservation 0.5h~2h, then
800 DEG C~900 DEG C heat preservation 2h~4h are warming up to, after furnace temperature is finally down to 25 DEG C~200 DEG C, take out silver ingot.
Wherein, in (5) extrusion forming step in the step 2, it is with temperature by the silver ingot that step 2 (4) sinters
800 DEG C~900 DEG C the pre-heat treatment 1h~3h recycle extruder to be squeezed, obtain the silver-of a diameter of 4mm~5.5mm
Nickel-graphite alkene alloy material.
To achieve the above object two, the present invention provides following technical scheme：
A kind of silver-nickel-graphite alkene alloy material is provided, using the silver described in claim 1 to 9-nickel-graphite alkene alloy material
Silver made of the preparation method of material-nickel-graphite alkene alloy material.
Beneficial effects of the present invention：
(1) preparation method of a kind of silver-nickel-graphite alkene alloy material of the invention, this method pass through silver ammino solution, reduction
Agent solution and graphene solution hybrid reaction are made silver-colored graphene composite powder, then by silver-colored graphene composite powder obtained and nickel
Powder, silver powder are through overmulling powder, heating and extrusion process, you can silver-nickel-graphite alkene alloy material is obtained, it compared with prior art, should
The reagent source of preparation method is extensive, is not required to add any coating material and operational sequence is simple, has simple for process, production
Efficient advantage.
(2) a kind of silver-nickel-graphite alkene alloy material of the invention, which is that graphite is added in silver-nickel
Alkene material, due to graphene by hexa-atomic ring carbon atom form only one layer of atomic thickness two dimensional crystal, can with metal from
Sub- stable bond, therefore silver-nickel and graphene are compound, graphene can steadily combine silver-nickel, and graphene has
There are the performance of high ductibility, high rigidity and high conductivity, silver-colored nickel graphene to combine thermal conductivity, the electricity that not only ensure that silver-nickel
Aggressivity and hardness, while silver-preferable ductility of nickel-graphite alkene alloy material and electric conductivity are assigned, and further improve
Its electric conductivity；In addition, it is that graphene solution reaction, stirring first is added by silver ammino solution to prepare silver-nickel-graphite alkene alloy material
Afterwards, then reducing agent solution is added dropwise, the silver-colored ammonium ion of reducing agent solution reduction of dropwise addition simultaneously makes silver ion and graphite after reduction in time
Alkene combine, and then silver with graphene stable bond, nickel powder is then added, then using mix powder, isostatic pressing, repeatedly heating and
Pressing steps so that nickel powder can preferably mix silver-graphene alloyed powder, and then make silver obtained-nickel-graphite alkene alloy material
In a variety of materials be uniformly dispersed and stable bond, compared with prior art, the silver-nickel-graphite alkene alloy material makes full use of
The performance of graphene stable bond power and deep drawing quality, high intensity and high conductivity, makes silver metal and the nickel metal in graphene
It is uniformly dispersed in and stable bond, so that silver-nickel-graphite alkene alloy material has good heat conductivity, erosion property energy
Good and strong hardness advantage promotes application of the silver metal in conductor wire production.
(3) offer silver provided by the invention-nickel-graphite alkene alloy material and preparation method thereof, simple with preparation method,
Production cost it is low and can be suitable for large-scale production the characteristics of.
Specific implementation mode
Embodiment 1.
A kind of preparation method of silver-nickel-graphite alkene alloy material in the present embodiment, includes the following steps：
Step 1, the preparation of silver-colored graphene composite powder
(1) preparation of each solution
The preparation of silver ammino solution：Pure water is weighed, silver nitrate is added into pure water, is then added ammonium hydroxide, agitating solution is to clear
It is clear well-illuminated, silver ammino solution is made；
The preparation of reducing agent solution：Reducing agent solution is weighed, and is diluted with pure water, required reducing agent solution is made；
The preparation of graphene solution：Pure water is weighed, graphene powder is added into pure water, is dispersed with stirring certain time, makes
Graphene powder is uniformly suspended in pure water, and graphene solution is made；
(2) preparation of silver-colored graphene composite powder：Step 1 (1) is added in silver ammino solution made from step 1 (1) to be made
Graphene solution in, stir certain time, then instill reducing agent solution prepared by step 1 (1), it is multiple that silver graphene is made
Close powder；
(3) it cleans, dry and screening：
A) it cleans：Silver-colored graphene composite powder made from step 2 is filtered into cleaning so that silver-graphene powder is loose,
Without ammonia taste；
B) dry：By the silver-colored graphene composite powder drying after cleaning, calcined after drying；
C) it sieves：By the silver-colored graphene composite powder ball milling after drying, after removing ball material, the silver-colored graphene after screen analysis ball milling
The fine powder of composite granule, sieving is finished product silver graphene composite powder；
Step 2, the recombination reaction of nickel and silver-colored graphene composite powder
(1) dry：By silver powder, nickel powder, finished product silver graphene composite powder made from step 1 is respectively dried, for use；
(2) powder is mixed：The nickel powder of step 2 (1) and finished product silver-nickel graphene alloy powder of step 2 (1) are sufficiently mixed
Uniformly, the silver powder that step 2 (1) is then added continues to be sufficiently mixed uniformly, and mixed powder is made；
(3) isostatic pressing：Mixed powder made from step 2 (2) is placed in pressurized treatments in isostatic pressing machine, silver-is made
Nickel-graphite alkene silver ingot；
(4) sintering processes：Silver made from step 2 (3)-nickel-graphite alkene silver ingot is sintered, the silver-sintered
Nickel-graphite alkene silver ingot；
(5) extrusion forming：The silver that step 2 (4) is obtained-nickel-graphite alkene silver ingot elder generation the pre-heat treatment, then passes through extruding
Machine extrusion process obtains silver-nickel-graphite alkene alloy wire of certain diameter.
In the present embodiment, in the preparation process of (1) silver ammino solution in the step 1, the silver nitrate, the ammonium hydroxide
Mass ratio with the pure water is 1:0.5:1.5, a concentration of the 5% of the ammonium hydroxide；
In the preparation process of (1) reducing solution in the step 1, the reducing agent be hydrazine hydrate, the hydrazine hydrate with
The mass ratio of pure water is 1:1；
In the preparation process of (1) graphene solution in the step 1, the mass ratio of the Graphene powder and pure water is
1:10, and water 1h is dispersed with stirring by ultrasonic vibration.
In the present embodiment, in the preparation process of (2) silver-colored graphene composite powder in the step 1, the silver ammonia is molten
Mass ratio between liquid, the reducing agent solution and the graphene solution is 1:10:50.
It is described in the drying steps in (3) cleaning, dry and screening step in the step 1 in the present embodiment
Drying temperature is 100 DEG C, and the drying time is 3h, and the calcination temperature is 400 DEG C, and the calcination time is 2h；
In the screening step, the Ball-milling Time is 0.5h, ratio of grinding media to material 2:1, after 80 mesh sieve screen analysis ball millings
Silver-colored graphene composite powder.
In the present embodiment, in (1) baking step in the step 2, the drying temperature is 60 DEG C, when the drying
Between be 0.5h.
In the present embodiment, (2) in the step 2 are mixed in powder step, the nickel powder, the silver-colored graphene composite powder
Mass ratio with the silver powder is：1:0.5:0.5, the nickel powder and the silver-colored graphene composite powder mix powder machine by plough type
It is sufficiently mixed uniformly, it is first mixed by hand after the well-mixed nickel powder and the silver-colored graphene composite powder is added in the silver powder
It closes uniformly, then powder machine is mixed by plough type and is sufficiently mixed uniformly.
In the present embodiment, in (3) isostatic pressing step in the step 2, the input amount of mixed powder is 10kg,
The pressure of isostatic pressed is 50MPa, and the time of isostatic pressing is 1min.
In the present embodiment, in the sintering processes step of the step 2 (4), by silver-nickel-graphite made from step 2 (3)
Alkene silver ingot is put into pit furnace with 200 DEG C of heat preservation 0.5h, with 500 DEG C of heat preservation 0.5h, with 800 DEG C of heat preservation 2h, after the completion of sintering, by furnace temperature
To after 25 DEG C, silver ingot is taken out.
In the present embodiment, in step 2 (5) the extrusion forming step, the silver ingot that step 2 (4) is sintered is with temperature
For 800 DEG C of the pre-heat treatment 1h, recycles extruder to be squeezed, obtains silver-nickel-graphite alkene alloy material of a diameter of 4mm,
Wherein, by wire drawing after the silver of a diameter of 4mm-nickel-graphite alkene alloy material annealing, silver-nickel-graphite of a diameter of 1.4mm is made
Alkene alloy wire.
Silver-colored graphene composite powder is made by silver ammino solution, reducing agent solution and graphene solution hybrid reaction in this method
Body, then by silver-graphene powder obtained and nickel powder, silver powder through overmulling powder, heating and extrusion process, you can obtain silver-nickel-stone
Black alkene alloy material, compared with prior art, the reagent source of the preparation method is extensive, be not required to add any coating material and
Process is easily operated, has the advantages that simple for process, production efficiency is high.
Embodiment 2.
A kind of preparation method of silver-nickel-graphite alkene alloy material in the present embodiment, includes the following steps：
Step 1, the preparation of silver-colored graphene composite powder
(1) preparation of each solution
The preparation of silver ammino solution：Pure water is weighed, silver nitrate is added into pure water, is then added ammonium hydroxide, agitating solution is to clear
It is clear well-illuminated, silver ammino solution is made；
The preparation of reducing agent solution：Reducing agent solution is weighed, and is diluted with pure water, required reducing agent solution is made；
The preparation of graphene solution：Pure water is weighed, graphene powder is added into pure water, is dispersed with stirring certain time, makes
Graphene powder is uniformly suspended in pure water, and graphene solution is made；
(2) preparation of silver-colored graphene composite powder：Step 1 (1) is added in silver ammino solution made from step 1 (1) to be made
Graphene solution in, stir certain time, then instill reducing agent solution prepared by step 1 (1), it is multiple that silver graphene is made
Close powder；
(3) it cleans, dry and screening：
A) it cleans：Silver-colored graphene composite powder made from step 2 is filtered into cleaning so that silver-graphene powder is loose,
Without ammonia taste；
B) dry：By the silver-colored graphene composite powder drying after cleaning, calcined after drying；
C) it sieves：By the silver-colored graphene composite powder ball milling after drying, after removing ball material, the silver-colored graphene after screen analysis ball milling
The fine powder of composite granule, sieving is finished product silver graphene composite powder；
Step 2, the recombination reaction of nickel and silver-colored graphene composite powder
(1) dry：By silver powder, nickel powder, finished product silver graphene composite powder made from step 1 is respectively dried, for use；
(2) powder is mixed：The nickel powder of step 2 (1) and finished product silver-nickel graphene alloy powder of step 2 (1) are sufficiently mixed
Uniformly, the silver powder that step 2 (1) is then added continues to be sufficiently mixed uniformly, and mixed powder is made；
(3) isostatic pressing：Mixed powder made from step 2 (2) is placed in pressurized treatments in isostatic pressing machine, silver-is made
Nickel-graphite alkene silver ingot；
(4) sintering processes：Silver made from step 2 (3)-nickel-graphite alkene silver ingot is sintered, the silver-sintered
Nickel-graphite alkene silver ingot；
(5) extrusion forming：The silver that step 2 (4) is obtained-nickel-graphite alkene silver ingot elder generation the pre-heat treatment, then passes through extruding
Machine extrusion process obtains silver-nickel-graphite alkene alloy wire of certain diameter.
In the present embodiment, in the preparation process of (1) silver ammino solution in the step 1, the silver nitrate, the ammonium hydroxide
Mass ratio with the pure water is 1:5:10, a concentration of the 30% of the ammonium hydroxide；
In the preparation process of (1) reducing solution in the step 1, the reducing agent be hydrazine hydrate, the hydrazine hydrate with
The mass ratio of pure water is 1:8；
In the preparation process of (1) graphene solution in the step 1, the mass ratio of the Graphene powder and pure water is
1:100, and water 3h is dispersed with stirring by ultrasonic vibration.
In the present embodiment, in the preparation process of (2) silver-colored graphene composite powder in the step 1, the silver ammonia is molten
Mass ratio between liquid, the reducing agent solution and the graphene solution is 1:10:50.
It is described in the drying steps in (3) cleaning, dry and screening step in the step 1 in the present embodiment
Drying temperature is 400 DEG C, and the drying time is 6h, and the calcination temperature is 700 DEG C, and the calcination time is 4h；
In the screening step, the Ball-milling Time is 2h, ratio of grinding media to material 2:1, after 200 mesh sieve screen analysis ball millings
Silver-colored graphene composite powder.
In the present embodiment, in (1) baking step in the step 2, the drying temperature is 100 DEG C, when the drying
Between be 1.5h.
In the present embodiment, (2) in the step 2 are mixed in powder step, the nickel powder, the silver-colored graphene composite powder
Mass ratio with the silver powder is：1:1:3, it is abundant that the nickel powder and the silver-colored graphene composite powder by plough type mix powder machine
It is uniformly mixed, the well-mixed nickel powder is added with after the silver-colored graphene composite powder in the silver powder, and first manual mixing is equal
It is even, then powder machine is mixed by plough type and is sufficiently mixed uniformly.
In the present embodiment, in (3) isostatic pressing step in the step 2, the input amount of mixed powder is 30kg,
The pressure of isostatic pressed is 300MPa, and the time of isostatic pressing is 10min.
In the present embodiment, in the sintering processes step of the step 2 (4), by silver-nickel-graphite made from step 2 (3)
Alkene silver ingot is put into pit furnace with 500 DEG C of heat preservation 2h, with 800 DEG C of heat preservation 2h, with 900 DEG C of heat preservation 4h, after the completion of sintering, extremely by furnace temperature
After 200 DEG C, silver ingot is taken out.
In the present embodiment, in step 2 (5) the extrusion forming step, the silver ingot that step 2 (4) is sintered is with temperature
For 900 DEG C of the pre-heat treatment 3h, recycles extruder to be squeezed, obtain silver-nickel-graphite alkene alloy material of a diameter of 5.5mm
Material, wherein by wire drawing after the silver of a diameter of 5mm-nickel-graphite alkene alloy material annealing, silver-nickel-stone of a diameter of 1.4mm is made
Black alkene alloy wire.
Silver-colored graphene composite powder is made by silver ammino solution, reducing agent solution and graphene solution hybrid reaction in this method
Body, then by silver-graphene powder obtained and nickel powder, silver powder through overmulling powder, heating and extrusion process, you can obtain silver-nickel-stone
Black alkene alloy material, compared with prior art, the reagent source of the preparation method is extensive, be not required to add any coating material and
Process is easily operated, has the advantages that simple for process, production efficiency is high.
The present embodiment 3.
A kind of preparation method of silver-nickel-graphite alkene alloy material in the present embodiment, includes the following steps：
Step 1, the preparation of silver-colored graphene composite powder
(1) preparation of each solution
The preparation of silver ammino solution：Pure water is weighed, silver nitrate is added into pure water, is then added ammonium hydroxide, agitating solution is to clear
It is clear well-illuminated, silver ammino solution is made；
The preparation of reducing agent solution：Reducing agent solution is weighed, and is diluted with pure water, required reducing agent solution is made；
The preparation of graphene solution：Pure water is weighed, graphene powder is added into pure water, is dispersed with stirring certain time, makes
Graphene powder is uniformly suspended in pure water, and graphene solution is made；
(2) preparation of silver-colored graphene composite powder：Step 1 (1) is added in silver ammino solution made from step 1 (1) to be made
Graphene solution in, stir certain time, then instill reducing agent solution prepared by step 1 (1), it is multiple that silver graphene is made
Close powder；
(3) it cleans, dry and screening：
A) it cleans：Silver-colored graphene composite powder made from step 2 is filtered into cleaning so that silver-graphene powder is loose,
Without ammonia taste；
B) dry：By the silver-colored graphene composite powder drying after cleaning, calcined after drying；
C) it sieves：By the silver-colored graphene composite powder ball milling after drying, after removing ball material, the silver-colored graphene after screen analysis ball milling
The fine powder of composite granule, sieving is finished product silver graphene composite powder；
Step 2, the recombination reaction of nickel and silver-colored graphene composite powder
(1) dry：By silver powder, nickel powder, finished product silver graphene composite powder made from step 1 is respectively dried, for use；
(2) powder is mixed：The nickel powder of step 2 (1) and finished product silver-nickel graphene alloy powder of step 2 (1) are sufficiently mixed
Uniformly, the silver powder that step 2 (1) is then added continues to be sufficiently mixed uniformly, and mixed powder is made；
(3) isostatic pressing：Mixed powder made from step 2 (2) is placed in pressurized treatments in isostatic pressing machine, silver-is made
Nickel-graphite alkene silver ingot；
(4) sintering processes：Silver made from step 2 (3)-nickel-graphite alkene silver ingot is sintered, the silver-sintered
Nickel-graphite alkene silver ingot；
(5) extrusion forming：The silver that step 2 (4) is obtained-nickel-graphite alkene silver ingot elder generation the pre-heat treatment, then passes through extruding
Machine extrusion process obtains silver-nickel-graphite alkene alloy wire of certain diameter.
In the present embodiment, in the preparation process of (1) silver ammino solution in the step 1, the silver nitrate, the ammonium hydroxide
Mass ratio with the pure water is 1:3:6, a concentration of the 18% of the ammonium hydroxide；
In the preparation process of (1) reducing solution in the step 1, the reducing agent be hydrazine hydrate, the hydrazine hydrate with
The mass ratio of pure water is 1:4；
In the preparation process of (1) graphene solution in the step 1, the mass ratio of the Graphene powder and pure water is
1:50, and water 2h is dispersed with stirring by ultrasonic vibration.
In the present embodiment, in the preparation process of (2) silver-colored graphene composite powder in the step 1, the silver ammonia is molten
Mass ratio between liquid, the reducing agent solution and the graphene solution is 1:30.
It is described in the drying steps in (3) cleaning, dry and screening step in the step 1 in the present embodiment
Drying temperature is 200 DEG C, and the drying time is 5h, and the calcination temperature is 500 DEG C, and the calcination time is 3h；
In the screening step, the Ball-milling Time is 1.5h, ratio of grinding media to material 2:1, after 100 mesh sieve screen analysis ball millings
Silver-colored graphene composite powder.
In the present embodiment, in (1) baking step in the step 2, the drying temperature is 80 DEG C, when the drying
Between be 1h.
In the present embodiment, (2) in the step 2 are mixed in powder step, the nickel powder, the silver-colored graphene composite powder
Mass ratio with the silver powder is：1:0.7:1.5, the nickel powder and the silver-colored graphene composite powder mix powder machine by plough type
It is sufficiently mixed uniformly, it is first mixed by hand after the well-mixed nickel powder and the silver-colored graphene composite powder is added in the silver powder
It closes uniformly, then powder machine is mixed by plough type and is sufficiently mixed uniformly.
In the present embodiment, in (3) isostatic pressing step in the step 2, the input amount of mixed powder is 15kg,
The pressure of isostatic pressed is 210MPa, and the time of isostatic pressing is 5min.
In the present embodiment, in the sintering processes step of the step 2 (4), by silver-nickel-graphite made from step 2 (3)
Alkene silver ingot is put into pit furnace with 400 DEG C of heat preservation 1h, with 650 DEG C of heat preservation 1h, with 880 DEG C of heat preservation 3h, after the completion of sintering, extremely by furnace temperature
After 150 DEG C, silver ingot is taken out.
In the present embodiment, in step 2 (5) the extrusion forming step, the silver ingot that step 2 (4) is sintered is with temperature
For 830 DEG C of the pre-heat treatment 2h, 880 tons of extruder is recycled to be squeezed, the silver-nickel-graphite alkene for obtaining a diameter of 5mm closes
Golden material, wherein by wire drawing after the silver of a diameter of 5mm-nickel-graphite alkene alloy material annealing, the silver-of a diameter of 1.4mm is made
Nickel-graphite alkene alloy wire.
Silver-colored graphene composite powder is made by silver ammino solution, reducing agent solution and graphene solution hybrid reaction in this method
Body, then by silver-graphene powder obtained and nickel powder, silver powder through overmulling powder, heating and extrusion process, you can obtain silver-nickel-stone
Black alkene alloy material, compared with prior art, the reagent source of the preparation method is extensive, be not required to add any coating material and
Process is easily operated, has the advantages that simple for process, production efficiency is high.
Embodiment 4.
A kind of silver of the present embodiment-nickel-graphite alkene alloy material, the silver-nickel-graphite alkene alloy material by embodiment 1,
The preparation method of any one silver-nickel-graphite alkene alloy material in embodiment 2, embodiment 3 or embodiment 4 is made, the alloy
Material is that grapheme material is added in silver-nickel, the only one layer of atom being made of hexa-atomic ring carbon atom due to graphene
The two dimensional crystal of thickness, can be with metal ion stable bond, therefore silver-nickel and graphene are compound, and graphene can close silver-colored nickel
Gold steadily combines, and performance of the graphene with high ductibility, high rigidity and high conductivity, silver-colored nickel graphene combine not only
It ensure that thermal conductivity, erosion property and the hardness of silver-nickel, while assigning silver-nickel-graphite alkene alloy material and preferably extending
Property and electric conductivity, and further improve its electric conductivity；In addition, it is first by silver ammino solution to prepare silver-nickel-graphite alkene alloy material
Graphene solution reaction is added, after stirring, then reducing agent solution is added dropwise, the silver-colored ammonium ion of reducing agent solution reduction of dropwise addition is simultaneously timely
So that the silver ion after reduction is combined with graphene, and then silver and graphene stable bond, nickel powder is then added, then using mixed
Powder, isostatic pressing, repeatedly heating and pressing steps so that nickel powder can preferably mix silver-graphene alloyed powder, and then make system
A variety of materials in the silver-nickel-graphite alkene alloy material obtained are uniformly dispersed and stable bond, compared with prior art, the silver-
Nickel-graphite alkene alloy material take full advantage of graphene stable bond power and deep drawing quality, high intensity and high conductivity performance,
Silver metal and nickel metal is set to be uniformly dispersed in and stable bond in graphene, so that silver-nickel-graphite alkene alloy material
Have the advantages that good heat conductivity, erosion property can be got well and hardness is strong, promotes application of the silver metal in conductor wire production.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than the present invention is protected
The limitation of range is protected, although being explained in detail to the present invention with reference to preferred embodiment, those skilled in the art answer
Work as understanding, technical scheme of the present invention can be modified or replaced equivalently, without departing from the reality of technical solution of the present invention
Matter and range.
Claims (10)
1. a kind of preparation method of silver-nickel-graphite alkene alloy material, it is characterized in that：Include the following steps：
Step 1, the preparation of silver-colored graphene composite powder
（1）The preparation of each solution
The preparation of silver ammino solution：Pure water is weighed, silver nitrate is added into pure water, ammonium hydroxide is then added, agitating solution leads to limpid
It is bright, silver ammino solution is made；
The preparation of reducing agent solution：Reducing agent solution is weighed, and is diluted with pure water, required reducing agent solution is made；
The preparation of graphene solution：Pure water is weighed, graphene powder is added into pure water, is dispersed with stirring certain time, makes graphite
Alkene powder is uniformly suspended in pure water, and graphene solution is made；
（2）The preparation of silver-colored graphene composite powder：By step 1（1）Step 1 is added in silver ammino solution obtained（1）Stone obtained
In black alkene solution, certain time is stirred, step 1 is then instilled（1）It is multiple that silver-colored graphene is obtained by the reaction in the reducing agent solution of preparation
Close powder；
（3）Cleaning, dry and screening：
Cleaning：It will be in step 1（2）Silver graphene composite powder obtained filters cleaning so that silver-colored graphene composite powder pine
It dissipates, no ammonia taste；
It is dry：By the silver-colored graphene composite powder drying after cleaning, calcined after drying；
Screening：By the silver-colored graphene composite powder ball milling after calcining, after removing ball material, by the silver-colored graphene composite powder after ball milling
Fine powder, as finished product silver graphene composite powder are obtained after sieving；
Step 2, the recombination reaction of nickel and silver-colored graphene composite powder
（1）It is dry：By silver powder, nickel powder, finished product silver graphene composite powder made from step 1 is respectively dried, for use；
（2）Mixed powder：Nickel powder after drying is sufficiently mixed uniformly with finished product silver-nickel graphene alloy powder, silver powder is then added
Continue to be sufficiently mixed uniformly, mixed powder is made；
（3）Isostatic pressing：By step 2（2）Mixed powder obtained carries out pressurized treatments, and silver-nickel-graphite alkene silver ingot is made；
（4）Sintering processes：By step 2（3）Silver obtained-nickel-graphite alkene silver ingot is sintered, the silver-nickel-sintered
Graphene silver ingot；
（5）Extrusion forming：By step 2（4）Obtained silver-nickel-graphite alkene silver ingot the pre-heat treatment, then extrusion process, obtains
Silver-nickel-graphite alkene alloy material.
2. a kind of preparation method of silver according to claim 1-nickel-graphite alkene alloy material, it is characterized in that：The step
In one（1）In the preparation process of silver ammino solution, the mass ratio of the silver nitrate, the ammonium hydroxide and the pure water is 1:0.5~
5:1.5 ~ 10, a concentration of the 5% ~ 30% of the ammonium hydroxide；
In the step 1（1）In the preparation process of reducing solution, the reducing agent is hydrazine hydrate, the hydrazine hydrate and pure water
Mass ratio be 1:1~8；
In the step 1（1）In the preparation process of graphene solution, the mass ratio of the Graphene powder and pure water is 1:10~
100, and 1h ~ 3h is dispersed with stirring by ultrasonic vibration.
3. a kind of preparation method of silver according to claim 1-nickel-graphite alkene alloy material, it is characterized in that：The step
In one（2）In the preparation process of silver-colored graphene composite powder, the silver ammino solution, the reducing agent solution and the graphene
Mass ratio between solution is 1:10:50.
4. a kind of preparation method of silver according to claim 1-nickel-graphite alkene alloy material, it is characterized in that：The step
In one（3）In cleaning, dry and screening step, the drying temperature in the drying steps is 100 DEG C ~ 400 DEG C, drying time
For 3h ~ 6h, calcination temperature is 400 DEG C ~ 700 DEG C, and calcination time is the h of 2 h ~ 4；
Ball-milling Time in the screening step is 0.5h ~ 2h, ratio of grinding media to material 2:1, the mesh number of sieving is the mesh of 80 mesh ~ 200.
5. a kind of preparation method of silver according to claim 1-nickel-graphite alkene alloy material, it is characterized in that：The step
In two（1）In drying steps, drying temperature is 60 DEG C ~ 100 DEG C, and drying time is 0.5h ~ 1.5h.
6. a kind of preparation method of silver according to claim 1-nickel-graphite alkene alloy material, it is characterized in that：The step
In two（2）In mixed powder step, the mass ratio of the nickel powder, the silver-colored graphene composite powder and the silver powder is 1:0.5~1:
0.5 ~ 3, the nickel powder and the finished product silver graphene composite powder mix powder machine by plough type and are sufficiently mixed uniformly, the silver powder
After the well-mixed nickel powder and the finished product silver graphene composite powder is added, it is uniform to first pass through manual mixing, then passes through
Plough type mixes powder machine and is sufficiently mixed uniformly.
7. a kind of preparation method of silver according to claim 1-nickel-graphite alkene alloy material, it is characterized in that：The step
In two（3）In isostatic pressing step, the mixed powder be placed in isostatic pressing machine carry out pressurized treatments, input amount be 10kg ~
30kg, pressure are 50MPa ~ 300MPa, and it is 1min ~ 10min to be kept for the time of pressurization.
8. a kind of preparation method of silver according to claim 1-nickel-graphite alkene alloy material, it is characterized in that：The step
In two（4）In sintering processes step, by step 2（3）Silver obtained-nickel-graphite alkene silver ingot is put into pit furnace, first with 200 DEG C ~
500 DEG C heat preservation 0.5h ~ 2h, then heat to 500 DEG C ~ 800 DEG C heat preservation 0.5h ~ 2h, then be warming up to 800 DEG C ~ 900 DEG C heat preservation 2h ~
4h after furnace temperature is finally down to 25 DEG C ~ 200 DEG C, takes out silver ingot.
9. a kind of preparation method of silver according to claim 1-nickel-graphite alkene alloy material, it is characterized in that：The step
In two（5）In extrusion forming step, by step 2（4）The silver ingot sintered with temperature be 800 DEG C ~ 900 DEG C the pre-heat treatment 1h ~
3h recycles extruder to be squeezed, obtains silver-nickel-graphite alkene alloy material of a diameter of 4mm ~ 5.5mm.
10. a kind of silver-nickel-graphite alkene alloy material, it is characterised in that：Using the silver described in claim 1 to 9-nickel-graphite alkene
Silver made of the preparation method of alloy material-nickel-graphite alkene alloy material.
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