CN106363190A - Silver-nickel-graphene alloy material and preparation method thereof - Google Patents
Silver-nickel-graphene alloy material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of alloy materials, in particular to a silver-nickel-graphene alloy material and a preparation method thereof. The preparation method of the silver-nickel-graphene alloy material includes the following steps that firstly, preparation of silver and graphene compound powder includes the first step of preparation of all solutions, the second step of preparation of the silver and graphene compound powder and the third step of cleaning, drying and screening; and secondly, the compound reaction of nickel and the silver and graphene compound powder includes the first step of drying, the second step of powder mixing, the third step of isostatic pressing processing, the fourth step of sintering processing and the fifth step of extrusion forming. The preparation method has the beneficial effects of being simple in process and high in production efficiency. In addition, the silver-nickel-graphene alloy material prepared through the preparation method is uniform in dispersion and high in stability and has the beneficial effects of being good in heat conduction performance, good in electric erosion performance and high in hardness.
Description
Technical field
The present invention relates to technical field of alloy material is 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, but silver metal is few in nature storage, valency
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
Degree is poor, so that the tensile strength of silver wire is also poor, so further limit the application in conductive field for the silver metal.
Prior art is employed unlike material and is combined with silver metal, and to strengthen the performance of silver metal, wherein, nickel material has
Preferably ductility, medium hardness and good corrosion resistance, and nickel wide material sources, cheap, by nickel and silver metal
Make the performance that alloy material is greatly improved silver metal, this silver-nickel has good electric conductivity, heat conductivity, electrical arc erosion
Property, electroerosion, wearability and improve silver metal intensity, and then expand the range of silver, and this silver-nickel made
It is widely used in all kinds of switches, controller, voltage regulator, chopper, electrical apparatus for vehicle use, magnetic starter etc. for contact material.
But the silver-nickel material of preparation there is a problem of disperseing uneven, less stable in prior art, so that
Silver-nickel heat conductivility is poor, electroerosion poor performance and the weak problem of hardness are it is impossible to preferably be applied to all kinds of switches, control
Device, voltage regulator, chopper, electrical apparatus for vehicle use, magnetic starter etc..Additionally, the method preparing silver-nickel material is also deposited
In the defect of complex process, low production efficiency, so hinder the popularization of silver-nickel material, therefore, need developing badly a kind of new
Technique is to optimize the performance of silver-nickel.
Content of the invention
There is above-mentioned technical problem for prior art, one of the object of the invention is to provide a kind of silver-nickel-graphite alkene to close
The preparation method of golden material, the method has the advantages that process is simple, production efficiency are high.
There is above-mentioned technical problem for prior art, the two of the object of the invention is to provide one kind to be uniformly dispersed, stablizes
High silver-nickel-graphite alkene the alloy material of property, this alloy material has that good heat conductivity, electroerosion performance be good and that hardness is strong is excellent
Point.
One of for achieving the above object, present invention offer technical scheme below:
A kind of preparation method of silver-nickel-graphite alkene alloy material is provided, it is characterized in that: comprise the following steps:
Step one, the preparation of silver-colored graphene composite powder
(1) preparation of each solution
The preparation of silver ammino solution: weigh pure water, add silver nitrate toward in pure water, be subsequently adding ammonia, agitating solution leads to limpid
Bright, prepared silver ammino solution；
The preparation of reductant solution: weigh reductant solution, and with pure water dilution, required reductant solution is obtained；
The preparation of graphene solution: weigh pure water, add graphene powder toward in pure water, dispersed with stirring certain time, make graphite
Alkene powder body is uniformly suspended in pure water, prepared graphene solution；
(2) preparation of silver-colored graphene composite powder: the silver ammino solution that step one (1) is obtained adds the stone that step one (1) is obtained
In black alkene solution, stir certain time, then instill reductant solution prepared by step one (1), it is multiple that reaction obtains silver-colored Graphene
Close powder body；
(3) cleaning, dry and screening:
A) clean: the silver-colored graphene composite powder sucking filtration cleaning that is obtained (2) in step one is so that silver graphene composite powder
Loose, no ammonia taste；
B) it is dried: the silver-colored graphene composite powder after cleaning is dried, is calcined after drying；
C) sieve: 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
Body obtains fine powder, as finished product silver graphene composite powder after sieving；
Step 2, the compound reaction of nickel and silver-colored graphene composite powder
(1) it is dried: by argentum powder, nikel powder, the finished product silver graphene composite powder that step one is obtained is respectively dried, stand-by；
(2) mix powder: the nikel powder after drying is sufficiently mixed uniformly with finished product silver-nickel Graphene alloy powder, is subsequently adding argentum powder
Continue to be sufficiently mixed uniformly, prepared mixed powder；
(3) isostatic pressed is processed: the mixed powder that step 2 (2) is obtained carries out pressurized treatments, prepared silver-nickel-graphite alkene silver ingot；
(4) sintering processes: silver-nickel-graphite alkene silver ingot that step 2 (3) is obtained is sintered, obtain silver-nickel of sintering-
Graphene silver ingot；
(5) extrusion molding: the silver that step 2 (4) is obtained-nickel-graphite alkene silver ingot the pre-heat treatment, then extrusion process, obtain
Silver-nickel-graphite alkene alloy material.
Wherein, in the preparation process of (1) silver ammino solution in described step one, described silver nitrate, described ammonia with described
The mass ratio of pure water is 1:0.5 ~ 5:1.5 ~ 10, and the concentration of described ammonia is 5% ~ 30%；
In the preparation process of (1) reducing solution in described step one, described reducing agent is hydrazine hydrate, described hydrazine hydrate and pure water
Mass ratio be 1:1 ~ 8；
In the preparation process of (1) graphene solution in described step one, the mass ratio of described Graphene powder and pure water be 1:10 ~
100, and pass through ultrasonic vibration dispersed with stirring 1h ~ 3h.
Wherein, in the preparation process of (2) silver graphene composite powder in described step one, described silver ammino solution, described
Mass ratio between reductant solution and described graphene solution is 1:10:50.
Wherein, the drying temperature in (3) cleaning in described step one, drying and screening step, in described b) drying steps
Spend for 100 DEG C ~ 400 DEG C, drying time is 3h ~ 6h, calcining heat is 400 DEG C ~ 700 DEG C, calcination time is 2 h ~ 4 h；Described
C) Ball-milling Time in sieving suddenly is 0.5h ~ 2h, and ratio of grinding media to material is 2:1, and the mesh number sieved is 80 mesh ~ 200 mesh.
Wherein, in (1) drying steps in described step 2, drying temperature be 60 DEG C ~ 100 DEG C, drying time be 0.5h ~
1.5h.
Wherein, (2) in described step 2 mix powder step in, described nikel powder, described silver graphene composite powder with described
The mass ratio of argentum powder is 1:0.5 ~ 1:0.5 ~ 3, and described nikel powder and described finished product silver graphene composite powder mix powder by plough type
Machine is sufficiently mixed uniformly, after described argentum powder adds the silver-colored graphene composite powder of well-mixed described nikel powder and described finished product, first
By manual mixing uniformly, then mix powder machine by plough type to be sufficiently mixed uniformly.
Wherein, in (3) the isostatic pressed process step in described step 2, described mixed powder is placed in isostatic pressing machine to carry out adding
Pressure is processed, and input amount is 10kg ~ 30kg, and pressure is 50mpa ~ 300mpa, and the time keeping pressurization is 1min ~ 10min.
Wherein, in (4) the sintering processes step in described step 2, silver-nickel-graphite alkene that step 2 (3) is obtained is silver-colored
Pit furnace put into by ingot, first with 200 DEG C ~ 500 DEG C insulation 0.5h ~ 2h, then heats to 500 DEG C ~ 800 DEG C insulation 0.5h ~ 2h, then heats up
To 800 DEG C ~ 900 DEG C insulation 2h ~ 4h, finally furnace temperature is down to after 25 DEG C ~ 200 DEG C, takes out silver ingot.
Wherein, in (5) the extrusion molding step in described step 2, the silver ingot that step 2 (4) is sintered with temperature is
800 DEG C ~ 900 DEG C the pre-heat treatment 1h ~ 3h, recycle extruder to be extruded, that is, the silver-nickel-stone of a diameter of 4mm ~ 5.5mm are obtained
Black alkene alloy material.
Two for achieving the above object, present invention offer technical scheme below:
There is provided a kind of silver-nickel-graphite alkene alloy material, using the silver described in claim 1 to 9-nickel-graphite alkene alloy material
The silver that preparation method is made-nickel-graphite alkene alloy material.
Beneficial effects of the present invention:
(1) preparation method of a kind of silver of the present invention-nickel-graphite alkene alloy material, the method is molten by silver ammino solution, reducing agent
Liquid and graphene solution hybrid reaction are obtained silver graphene composite powder, then by the silver-colored graphene composite powder being obtained and nikel powder,
Argentum powder is through overmulling powder, heating and extrusion process, you can obtain silver-nickel-graphite alkene alloy material, compared with prior art, this system
The reagent source of Preparation Method extensively, is not required to add any coating material and operation sequence is simple, have process is simple, produce effect
The high advantage of rate.
(2) a kind of silver of the present invention-nickel-graphite alkene alloy material, this alloy material is addition graphite in silver-nickel
Alkene material, due to the two dimensional crystal of only one layer of atomic thickness that Graphene is made up of hexa-atomic ring carbon atom, can with metal from
Sub- stable bond, therefore silver-nickel are combined with Graphene, and Graphene can stably combine silver-nickel, and Graphene tool
There is the performance of high ductibility, high rigidity and high conductivity, silver-colored nickel Graphene combines heat conductivity, the electricity that not only ensure that silver-nickel
Aggressivity and hardness, give silver-preferable ductility of nickel-graphite alkene alloy material and electric conductivity simultaneously, and further increase
Its electric conductivity；In addition, preparing silver-nickel-graphite alkene alloy material is first to add graphene solution reaction, stirring by silver ammino solution
Afterwards, then Deca reductant solution, the silver-colored ammonium ion of reductant solution reduction of Deca simultaneously makes the silver ion after reduction and graphite in time
Alkene combines, and then silver and Graphene stable bond, is subsequently adding nikel powder, then processed using mixed powder, isostatic pressed, repeatedly heating and
Pressing steps are so that nikel powder can preferably mix silver-graphene alloyed powder, and then make prepared silver-nickel-graphite alkene alloy material
In various materials be uniformly dispersed and stable bond, compared with prior art, this 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 nickel metal in Graphene
In be uniformly dispersed and stable bond, and then make silver-nickel-graphite alkene alloy material have good heat conductivity, electroerosion performance
Advantage good and that hardness is strong, promotes application in conductor wire production for the silver metal.
(3) offer silver-nickel-graphite alkene alloy material and preparation method thereof that the present invention provides, have preparation method simple,
Low production cost simultaneously can be applied to the feature of large-scale production.
Specific embodiment
Embodiment 1.
The preparation method of one of the present embodiment silver-nickel-graphite alkene alloy material, comprises the following steps:
Step one, the preparation of silver-colored graphene composite powder
(1) preparation of each solution
The preparation of silver ammino solution: weigh pure water, add silver nitrate toward in pure water, be subsequently adding ammonia, agitating solution leads to limpid
Bright, prepared silver ammino solution；
The preparation of reductant solution: weigh reductant solution, and with pure water dilution, required reductant solution is obtained；
The preparation of graphene solution: weigh pure water, add graphene powder toward in pure water, dispersed with stirring certain time, make graphite
Alkene powder body is uniformly suspended in pure water, prepared graphene solution；
(2) preparation of silver-colored graphene composite powder: the silver ammino solution that step one (1) is obtained adds the stone that step one (1) is obtained
In black alkene solution, stir certain time, then instill reductant solution prepared by step one (1), silver Graphene composite powder is obtained
Body；
(3) cleaning, dry and screening:
A) clean: the silver-colored graphene composite powder sucking filtration that step 2 is obtained cleans so that silver-graphene powder body is loose, no ammonia
Taste；
B) it is dried: the silver-colored graphene composite powder after cleaning is dried, is calcined after drying；
C) sieve: by dried silver graphene composite powder ball milling, after removing ball material, the silver-colored Graphene after screen analysis ball milling is combined
Powder body, the fine powder sieving is finished product silver graphene composite powder；
Step 2, the compound reaction of nickel and silver-colored graphene composite powder
(1) it is dried: by argentum powder, nikel powder, the finished product silver graphene composite powder that step one is obtained is respectively dried, stand-by；
(2) mix powder: the finished product silver-nickel Graphene alloy powder of the nikel powder of step 2 (1) and step 2 (1) is sufficiently mixed all
Even, the argentum powder being subsequently adding step 2 (1) continues to be sufficiently mixed uniformly, prepared mixed powder；
(3) isostatic pressed is processed: the mixed powder that step 2 (2) is obtained is placed in pressurized treatments in isostatic pressing machine, and prepared silver-nickel-
Graphene silver ingot；
(4) sintering processes: silver-nickel-graphite alkene silver ingot that step 2 (3) is obtained is sintered, obtain silver-nickel of sintering-
Graphene silver ingot；
(5) extrusion molding: the silver that step 2 (4) is obtained-nickel-graphite alkene silver ingot elder generation the pre-heat treatment, then passes through extruder and squeezes
Pressure is processed, and obtains the silver-nickel-graphite alkene alloy wire of certain diameter.
In the present embodiment, in the preparation process of (1) silver ammino solution in described step one, described silver nitrate, described ammonia
Mass ratio with described pure water is 1:0.5:1.5, and the concentration of described ammonia is 5%；
In the preparation process of (1) reducing solution in described step one, described reducing agent is hydrazine hydrate, described hydrazine hydrate and pure water
Mass ratio be 1:1；
In the preparation process of (1) graphene solution in described step one, described Graphene powder is 1:10 with the mass ratio of pure water,
And pass through ultrasonic vibration dispersed with stirring water 1h.
In the present embodiment, in the preparation process of (2) silver graphene composite powder in described step one, described silver ammonia is molten
Mass ratio between liquid, described reductant solution and described graphene solution is 1:10:50.
In the present embodiment, (3) in described step one cleaning, be dried and screening step in, in described drying steps, described
Drying temperature is 100 DEG C, and described drying time is 3h, and described calcining heat is 400 DEG C, and described calcination time is 2 h；
In described screening step, described Ball-milling Time is 0.5h, and ratio of grinding media to material is 2:1, using the silver after 80 mesh sieve screen analysis ball millings
Graphene composite powder.
In the present embodiment, in (1) baking step in described step 2, described drying temperature is 60 DEG C, during described drying
Between be 0.5h.
In the present embodiment, (2) in described step 2 mix in powder step, described nikel powder, described silver graphene composite powder
Mass ratio with described argentum powder is: 1:0.5:0.5, and described nikel powder and described silver graphene composite powder mix powder machine by plough type
It is sufficiently mixed uniformly, after described argentum powder adds well-mixed described nikel powder and described silver graphene composite powder, first manual mixed
Close uniformly, then powder machine is mixed by plough type and be sufficiently mixed uniformly.
In the present embodiment, in (3) the isostatic pressed process step in described step 2, the input amount of mixed powder is 10kg,
The pressure of isostatic pressed is 50mpa, and the time that isostatic pressed is processed is 1min.
In the present embodiment, in the sintering processes step of described step 2 (4), by the prepared silver-nickel-graphite of step 2 (3)
Alkene silver ingot puts into pit furnace with 200 DEG C of insulation 0.5h, with 500 DEG C of insulation 0.5h, with 800 DEG C of insulation 2h, after the completion of sintering, by furnace temperature
To after 25 DEG C, take out silver ingot.
In the present embodiment, in described step 2 (5) extrusion molding step, the silver ingot that step 2 (4) is sintered is with temperature
For 800 DEG C of the pre-heat treatment 1h, recycle extruder to be extruded, that is, the silver-nickel-graphite alkene alloy material of a diameter of 4mm be obtained,
Wherein, by wire drawing after the silver of a diameter of 4mm-nickel-graphite alkene alloy material annealing, the silver-nickel-graphite of a diameter of 1.4mm is obtained
Alkene alloy wire.
The method is passed through silver ammino solution, reductant solution and graphene solution hybrid reaction and silver Graphene composite powder is obtained
Body, then by the silver-graphene powder body being obtained and nikel powder, argentum 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 this preparation method extensively, be not required to add any coating material and
Operation is easily operated, has the advantages that process is simple, production efficiency are high.
Embodiment 2.
The preparation method of one of the present embodiment silver-nickel-graphite alkene alloy material, comprises the following steps:
Step one, the preparation of silver-colored graphene composite powder
(1) preparation of each solution
The preparation of silver ammino solution: weigh pure water, add silver nitrate toward in pure water, be subsequently adding ammonia, agitating solution leads to limpid
Bright, prepared silver ammino solution；
The preparation of reductant solution: weigh reductant solution, and with pure water dilution, required reductant solution is obtained；
The preparation of graphene solution: weigh pure water, add graphene powder toward in pure water, dispersed with stirring certain time, make graphite
Alkene powder body is uniformly suspended in pure water, prepared graphene solution；
(2) preparation of silver-colored graphene composite powder: the silver ammino solution that step one (1) is obtained adds the stone that step one (1) is obtained
In black alkene solution, stir certain time, then instill reductant solution prepared by step one (1), silver Graphene composite powder is obtained
Body；
(3) cleaning, dry and screening:
A) clean: the silver-colored graphene composite powder sucking filtration that step 2 is obtained cleans so that silver-graphene powder body is loose, no ammonia
Taste；
B) it is dried: the silver-colored graphene composite powder after cleaning is dried, is calcined after drying；
C) sieve: by dried silver graphene composite powder ball milling, after removing ball material, the silver-colored Graphene after screen analysis ball milling is combined
Powder body, the fine powder sieving is finished product silver graphene composite powder；
Step 2, the compound reaction of nickel and silver-colored graphene composite powder
(1) it is dried: by argentum powder, nikel powder, the finished product silver graphene composite powder that step one is obtained is respectively dried, stand-by；
(2) mix powder: the finished product silver-nickel Graphene alloy powder of the nikel powder of step 2 (1) and step 2 (1) is sufficiently mixed all
Even, the argentum powder being subsequently adding step 2 (1) continues to be sufficiently mixed uniformly, prepared mixed powder；
(3) isostatic pressed is processed: the mixed powder that step 2 (2) is obtained is placed in pressurized treatments in isostatic pressing machine, and prepared silver-nickel-
Graphene silver ingot；
(4) sintering processes: silver-nickel-graphite alkene silver ingot that step 2 (3) is obtained is sintered, obtain silver-nickel of sintering-
Graphene silver ingot；
(5) extrusion molding: the silver that step 2 (4) is obtained-nickel-graphite alkene silver ingot elder generation the pre-heat treatment, then passes through extruder and squeezes
Pressure is processed, and obtains the silver-nickel-graphite alkene alloy wire of certain diameter.
In the present embodiment, in the preparation process of (1) silver ammino solution in described step one, described silver nitrate, described ammonia
Mass ratio with described pure water is 1:5:10, and the concentration of described ammonia is 30%；
In the preparation process of (1) reducing solution in described step one, described reducing agent is hydrazine hydrate, described hydrazine hydrate and pure water
Mass ratio be 1:8；
In the preparation process of (1) graphene solution in described step one, described Graphene powder is 1 with the mass ratio of pure water:
100, and pass through ultrasonic vibration dispersed with stirring water 3h.
In the present embodiment, in the preparation process of (2) silver graphene composite powder in described step one, described silver ammonia is molten
Mass ratio between liquid, described reductant solution and described graphene solution is 1:10:50.
In the present embodiment, (3) in described step one cleaning, be dried and screening step in, in described drying steps, described
Drying temperature is 400 DEG C, and described drying time is 6h, and described calcining heat is 700 DEG C, and described calcination time is 4 h；
In described screening step, described Ball-milling Time is 2h, and ratio of grinding media to material is 2:1, using the silver-colored stone after 200 mesh sieve screen analysis ball millings
Black alkene composite granule.
In the present embodiment, in (1) baking step in described step 2, described drying temperature is 100 DEG C, during described drying
Between be 1.5h.
In the present embodiment, (2) in described step 2 mix in powder step, described nikel powder, described silver graphene composite powder
Mass ratio with described argentum powder is: 1:1:3, and described nikel powder and described silver graphene composite powder mix powder machine by plough type and fill
Divide mix homogeneously, after described argentum powder adds well-mixed described nikel powder and described silver graphene composite powder, first manual mixing
Uniformly, then mix powder machine by plough type to be sufficiently mixed uniformly.
In the present embodiment, in (3) the isostatic pressed process step in described step 2, the input amount of mixed powder is 30kg,
The pressure of isostatic pressed is 300mpa, and the time that isostatic pressed is processed is 10min.
In the present embodiment, in the sintering processes step of described step 2 (4), by the prepared silver-nickel-graphite of step 2 (3)
Alkene silver ingot puts into pit furnace with 500 DEG C of insulation 2h, with 800 DEG C of insulation 2h, is incubated 4h with 900 DEG C, after the completion of sintering, by furnace temperature extremely
After 200 DEG C, take out silver ingot.
In the present embodiment, in described step 2 (5) extrusion molding step, the silver ingot that step 2 (4) is sintered is with temperature
For 900 DEG C of the pre-heat treatment 3h, recycle extruder to be extruded, that is, the silver-nickel-graphite alkene alloy material of a diameter of 5.5mm is obtained
Material, wherein, wire drawing after the silver of a diameter of 5mm-nickel-graphite alkene alloy material annealing is obtained the silver-nickel-stone of a diameter of 1.4mm
Black alkene alloy wire.
The method is passed through silver ammino solution, reductant solution and graphene solution hybrid reaction and silver Graphene composite powder is obtained
Body, then by the silver-graphene powder body being obtained and nikel powder, argentum 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 this preparation method extensively, be not required to add any coating material and
Operation is easily operated, has the advantages that process is simple, production efficiency are high.
The present embodiment 3.
The preparation method of one of the present embodiment silver-nickel-graphite alkene alloy material, comprises the following steps:
Step one, the preparation of silver-colored graphene composite powder
(1) preparation of each solution
The preparation of silver ammino solution: weigh pure water, add silver nitrate toward in pure water, be subsequently adding ammonia, agitating solution leads to limpid
Bright, prepared silver ammino solution；
The preparation of reductant solution: weigh reductant solution, and with pure water dilution, required reductant solution is obtained；
The preparation of graphene solution: weigh pure water, add graphene powder toward in pure water, dispersed with stirring certain time, make graphite
Alkene powder body is uniformly suspended in pure water, prepared graphene solution；
(2) preparation of silver-colored graphene composite powder: the silver ammino solution that step one (1) is obtained adds the stone that step one (1) is obtained
In black alkene solution, stir certain time, then instill reductant solution prepared by step one (1), silver Graphene composite powder is obtained
Body；
(3) cleaning, dry and screening:
A) clean: the silver-colored graphene composite powder sucking filtration that step 2 is obtained cleans so that silver-graphene powder body is loose, no ammonia
Taste；
B) it is dried: the silver-colored graphene composite powder after cleaning is dried, is calcined after drying；
C) sieve: by dried silver graphene composite powder ball milling, after removing ball material, the silver-colored Graphene after screen analysis ball milling is combined
Powder body, the fine powder sieving is finished product silver graphene composite powder；
Step 2, the compound reaction of nickel and silver-colored graphene composite powder
(1) it is dried: by argentum powder, nikel powder, the finished product silver graphene composite powder that step one is obtained is respectively dried, stand-by；
(2) mix powder: the finished product silver-nickel Graphene alloy powder of the nikel powder of step 2 (1) and step 2 (1) is sufficiently mixed all
Even, the argentum powder being subsequently adding step 2 (1) continues to be sufficiently mixed uniformly, prepared mixed powder；
(3) isostatic pressed is processed: the mixed powder that step 2 (2) is obtained is placed in pressurized treatments in isostatic pressing machine, and prepared silver-nickel-
Graphene silver ingot；
(4) sintering processes: silver-nickel-graphite alkene silver ingot that step 2 (3) is obtained is sintered, obtain silver-nickel of sintering-
Graphene silver ingot；
(5) extrusion molding: the silver that step 2 (4) is obtained-nickel-graphite alkene silver ingot elder generation the pre-heat treatment, then passes through extruder and squeezes
Pressure is processed, and obtains the silver-nickel-graphite alkene alloy wire of certain diameter.
In the present embodiment, in the preparation process of (1) silver ammino solution in described step one, described silver nitrate, described ammonia
Mass ratio with described pure water is 1:3:6, and the concentration of described ammonia is 18%；
In the preparation process of (1) reducing solution in described step one, described reducing agent is hydrazine hydrate, described hydrazine hydrate and pure water
Mass ratio be 1:4；
In the preparation process of (1) graphene solution in described step one, described Graphene powder is 1:50 with the mass ratio of pure water,
And pass through ultrasonic vibration dispersed with stirring water 2h.
In the present embodiment, in the preparation process of (2) silver graphene composite powder in described step one, described silver ammonia is molten
Mass ratio between liquid, described reductant solution and described graphene solution is 1:30.
In the present embodiment, (3) in described step one cleaning, be dried and screening step in, in described drying steps, described
Drying temperature is 200 DEG C, and described drying time is 5h, and described calcining heat is 500 DEG C, and described calcination time is 3 h；
In described screening step, described Ball-milling Time is 1.5h, and ratio of grinding media to material is 2:1, using the silver after 100 mesh sieve screen analysis ball millings
Graphene composite powder.
In the present embodiment, in (1) baking step in described step 2, described drying temperature is 80 DEG C, during described drying
Between be 1h.
In the present embodiment, (2) in described step 2 mix in powder step, described nikel powder, described silver graphene composite powder
Mass ratio with described argentum powder is: 1:0.7:1.5, and described nikel powder and described silver graphene composite powder mix powder machine by plough type
It is sufficiently mixed uniformly, after described argentum powder adds well-mixed described nikel powder and described silver graphene composite powder, first manual mixed
Close uniformly, then powder machine is mixed by plough type and be sufficiently mixed uniformly.
In the present embodiment, in (3) the isostatic pressed process step in described step 2, the input amount of mixed powder is 15kg,
The pressure of isostatic pressed is 210mpa, and the time that isostatic pressed is processed is 5min.
In the present embodiment, in the sintering processes step of described step 2 (4), by the prepared silver-nickel-graphite of step 2 (3)
Alkene silver ingot puts into pit furnace with 400 DEG C of insulation 1h, with 650 DEG C of insulation 1h, is incubated 3h with 880 DEG C, after the completion of sintering, by furnace temperature extremely
After 150 DEG C, take out silver ingot.
In the present embodiment, in described step 2 (5) extrusion molding 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 extruded, that is, silver-nickel-graphite alkene that a diameter of 5mm is obtained closes
Golden material, wherein, by wire drawing after the annealing of the silver of a diameter of 5mm-nickel-graphite alkene alloy material, be obtained the silver of a diameter of 1.4mm-
Nickel-graphite alkene alloy wire.
The method is passed through silver ammino solution, reductant solution and graphene solution hybrid reaction and silver Graphene composite powder is obtained
Body, then by the silver-graphene powder body being obtained and nikel powder, argentum 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 this preparation method extensively, be not required to add any coating material and
Operation is easily operated, has the advantages that process is simple, production efficiency are high.
Embodiment 4.
A kind of silver of the present embodiment-nickel-graphite alkene alloy material, described silver-nickel-graphite alkene alloy material by embodiment 1,
The preparation method of any one silver in embodiment 2, embodiment 3 or embodiment 4-nickel-graphite alkene alloy material is made, this alloy
Material is addition grapheme material in silver-nickel, the only one layer of atom being made up of hexa-atomic ring carbon atom due to Graphene
The two dimensional crystal of thickness, can be with metal ion stable bond, and therefore silver-nickel and Graphene are combined, and Graphene can close silver-colored nickel
Gold stably combines, and Graphene has the performance of high ductibility, high rigidity and high conductivity, and silver-colored nickel Graphene combines not only
Ensure that heat conductivity, erosion property and the hardness of silver-nickel, give silver-nickel-graphite alkene alloy material simultaneously and preferably extend
Property and electric conductivity, and further increase its electric conductivity；In addition, preparing silver-nickel-graphite alkene alloy material is first by silver ammino solution
Add graphene solution reaction, after stirring, then Deca reductant solution, the silver-colored ammonium ion of reductant solution reduction of Deca is simultaneously in time
The silver ion after reduction is made to be combined with Graphene, and then silver and Graphene stable bond, it is subsequently adding nikel powder, then using mixed
Powder, isostatic pressed are processed, heating and pressing steps, so that nikel powder can preferably mix silver-graphene alloyed powder, and then make system repeatedly
Various materials in the silver-nickel-graphite alkene alloy material obtaining are uniformly dispersed and stable bond, compared with prior art, this silver-
Nickel-graphite alkene alloy material takes full advantage of the performance of Graphene stable bond power and deep drawing quality, high intensity and high conductivity,
Make silver metal and nickel metal Graphene in be uniformly dispersed and stable bond, and then make silver-nickel-graphite alkene alloy material
Have the advantages that good heat conductivity, electroerosion performance are good and hardness is strong, promote application in conductor wire production for the silver metal.
Finally it should be noted that above example is only in order to illustrating technical scheme, rather than the present invention is protected
The restriction of shield scope, although having made to explain to the present invention with reference to preferred embodiment, those of ordinary skill in the art should
Work as understanding, technical scheme can be modified or equivalent, without deviating from the reality of technical solution of the present invention
Matter and scope.
Claims (10)
1. the preparation method of a kind of silver-nickel-graphite alkene alloy material, is characterized in that: comprise the following steps:
Step one, the preparation of silver-colored graphene composite powder
(1) preparation of each solution
The preparation of silver ammino solution: weigh pure water, add silver nitrate toward in pure water, be subsequently adding ammonia, agitating solution leads to limpid
Bright, prepared silver ammino solution；
The preparation of reductant solution: weigh reductant solution, and with pure water dilution, required reductant solution is obtained；
The preparation of graphene solution: weigh pure water, add graphene powder toward in pure water, dispersed with stirring certain time, make graphite
Alkene powder body is uniformly suspended in pure water, prepared graphene solution；
(2) preparation of silver-colored graphene composite powder: the silver ammino solution that step one (1) is obtained adds the stone that step one (1) is obtained
In black alkene solution, stir certain time, then instill reductant solution prepared by step one (1), it is multiple that reaction obtains silver-colored Graphene
Close powder body；
(3) cleaning, dry and screening:
Cleaning: the silver-colored graphene composite powder sucking filtration that (2) in step one are obtained cleans so that silver-colored graphene composite powder is loose
Dissipate, no ammonia taste；
It is dried: the silver-colored graphene composite powder after cleaning is dried, is 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 is obtained after sieving；
Step 2, the compound reaction of nickel and silver-colored graphene composite powder
(1) it is dried: by argentum powder, nikel powder, the finished product silver graphene composite powder that step one is obtained is respectively dried, stand-by；
(2) mix powder: the nikel powder after drying is sufficiently mixed uniformly with finished product silver-nickel Graphene alloy powder, is subsequently adding argentum powder
Continue to be sufficiently mixed uniformly, prepared mixed powder；
(3) isostatic pressed is processed: the mixed powder that step 2 (2) is obtained carries out pressurized treatments, prepared silver-nickel-graphite alkene silver ingot；
(4) sintering processes: silver-nickel-graphite alkene silver ingot that step 2 (3) is obtained is sintered, obtain silver-nickel of sintering-
Graphene silver ingot；
(5) extrusion molding: the silver that step 2 (4) is obtained-nickel-graphite alkene silver ingot the pre-heat treatment, then extrusion process, obtain
Silver-nickel-graphite alkene alloy material.
2. a kind of preparation method of silver according to claim 1-nickel-graphite alkene alloy material, is characterized in that: described step
In the preparation process of (1) silver ammino solution in one, the mass ratio of described silver nitrate, described ammonia and described pure water be 1:0.5 ~
5:1.5 ~ 10, the concentration of described ammonia is 5% ~ 30%；
In the preparation process of (1) reducing solution in described step one, described reducing agent is hydrazine hydrate, described hydrazine hydrate and pure water
Mass ratio be 1:1 ~ 8；
In the preparation process of (1) graphene solution in described step one, the mass ratio of described Graphene powder and pure water be 1:10 ~
100, and pass through ultrasonic vibration dispersed with stirring 1h ~ 3h.
3. a kind of preparation method of silver according to claim 1-nickel-graphite alkene alloy material, is characterized in that: described step
In the preparation process of (2) silver graphene composite powder in one, described silver ammino solution, described reductant solution and described 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, is characterized in that: described step
In (3) cleaning in one, drying and screening step, the drying temperature in described b) drying steps is 100 DEG C ~ 400 DEG C, during drying
Between be 3h ~ 6h, calcining heat be 400 DEG C ~ 700 DEG C, calcination time be 2 h ~ 4 h；
Ball-milling Time in described c) screening suddenly is 0.5h ~ 2h, and ratio of grinding media to material is 2:1, and the mesh number sieved is 80 mesh ~ 200 mesh.
5. a kind of preparation method of silver according to claim 1-nickel-graphite alkene alloy material, is characterized in that: described step
In (1) drying steps in two, 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, is characterized in that: described step
(2) in two are mixed in powder step, and described nikel powder, described silver graphene composite powder and the mass ratio of described argentum powder are 1:0.5 ~ 1:
0.5 ~ 3, described nikel powder and described finished product silver graphene composite powder pass through the mixed powder machine of plough type and are sufficiently mixed uniformly, described argentum powder
After adding the silver-colored graphene composite powder of well-mixed described nikel powder and described finished product, first pass through manual mixing uniformly, then pass 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, is characterized in that: described step
In (3) isostatic pressed process step in two, described mixed powder is placed in isostatic pressing machine and carries out pressurized treatments, input amount be 10kg ~
30kg, pressure is 50mpa ~ 300mpa, and the time keeping pressurization is 1min ~ 10min.
8. a kind of preparation method of silver according to claim 1-nickel-graphite alkene alloy material, is characterized in that: described step
In (4) sintering processes step in two, pit furnace put into by silver-nickel-graphite alkene silver ingot that step 2 (3) is obtained, first with 200 DEG C ~
500 DEG C insulation 0.5h ~ 2h, then heat to 500 DEG C ~ 800 DEG C insulation 0.5h ~ 2h, then be warming up to 800 DEG C ~ 900 DEG C insulation 2h ~
4h, finally furnace temperature is down to after 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, is characterized in that: described step
In (5) extrusion molding step in two, silver ingot that step 2 (4) is sintered with temperature for 800 DEG C ~ 900 DEG C the pre-heat treatment 1h ~
3h, recycles extruder to be extruded, that is, the silver-nickel-graphite alkene alloy material of a diameter of 4mm ~ 5.5mm is obtained.
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
The silver that the preparation method of alloy material is made-nickel-graphite alkene alloy material.
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