CN107755686A - A kind of nanometer silver carbon composite and preparation method thereof - Google Patents
A kind of nanometer silver carbon composite and preparation method thereof Download PDFInfo
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- CN107755686A CN107755686A CN201710949200.5A CN201710949200A CN107755686A CN 107755686 A CN107755686 A CN 107755686A CN 201710949200 A CN201710949200 A CN 201710949200A CN 107755686 A CN107755686 A CN 107755686A
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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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/027—Composite material containing carbon particles or fibres
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
- B22F2003/208—Warm or hot extruding
-
- 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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- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention provides a kind of nanometer silver carbon composite and one kind to combine high-energy ball milling, is cold-pressed the method for preparing nanometer silver carbon composite with the powder metallurgy of hot extrusion.Present invention employs following technical scheme, including step 1) to prepare silver powder and graphite powder；2) high-energy ball milling；3) Passivation Treatment；4) cold pressing treatment；5) hot extrusion.Technique provided by the invention is simple, and using common PM technique, high-energy ball milling is introduced into preparation process, using cold pressing and hot extrusion technique, simplifies technological process, shortens preparation time, reduces material cost.The microstructure of nanometer silver carbon composite prepared by the present invention is evenly distributed on inside silver matrix for the carbon particle of nano-scale；ESEM and transmission electron microscope results are shown：Nano carbon particle size is between 3~300 nanometers；Between composite consistency is 99.5~100%, hardness is between 55~68Hv, and resistivity is between 1.7~2.5u Ω .cm.
Description
Technical field
The present invention relates to powder metallurgical technology, more particularly to a kind of nanometer silver carbon composite and preparation method thereof.
Background technology
Electrical contact is the core parts of electric switch, instrument and meter etc., mainly undertakes on-off circuit and load current
Effect, be widely used in various AC, DC contactors in the dual-use industrial circle such as Aeronautics and Astronautics, navigation, open circuit
In device, relay, change-over switch, its performance plays certainly to break-make capacity, service life and the operational reliability of whole electrical equipment
Qualitative effect.Electrical contact caused phenomenon numerous and complicated in the course of the work, influence factor is numerous, and this is just to the comprehensive of material
High request can be proposed.Preferable electrical contact material must possess good physical property, mechanical property, electrical contact performance, change
Learn performance, processing and manufacturing performance etc..
Ag-based electrical contact material is because it has preferable resistance to electrical wear, anti-melting welding and electric conductivity, contact resistance low and steady
Fixed and certain mechanical strength, be widely used in various relays, contactor, combination switch, Low Voltage Circuit Breaker and
It is the product being had a large capacity and a wide range the most in Electrical Contact Industry in the switching devices such as household electrical appliance.It is particularly low with process of industrialization
It is press-fitted electric system and control system continues to develop and the update of electronic industrial products, the research to Ag-based electrical contact material
Exploitation proposes higher and higher requirement.Due to the superior combination property of Ag-based electrical contact material, for quite a long time
Interior, it will be the important composition of contact material.
The good conductivity of silver-colored carbon composite, contact resistance are low and stablize, resistance fusion welding height, and self lubricity is good, low-temperature-rise
Excellent, in arcing contact and the existing very long history of slider application.But its arc extinction performance is poor, electric deterioration amount is big, and
Galvanic corrosion amount increases and increased with content of graphite.In order to improve constantly the quality of electrical contact, some high-tech raw materials, as carbon is fine
Dimension, CNT etc., also begin to suitable for manufacturing.Due to the infiltration sex-intergrade of carbon fiber, CNT and metal, therefore
Need first to carry out silver-plated process, then mixed by a certain percentage with silver powder, graphite powder, suppress and sinter, cause complex process,
Material cost raises.
The content of the invention
In view of the drawbacks described above of prior art, the technical problems to be solved by the invention are that how to reduce nanometer silver carbon compound
Material manufacture process, reduces cost, enhances product performance.
To achieve these goals, object of the present invention is to provide a kind of nanometer silver carbon composite, meanwhile, this hair
The bright one kind that additionally provides combines high-energy ball milling, is cold-pressed the method for preparing nanometer silver carbon composite with the powder metallurgy of hot extrusion.
The technical scheme that the present invention takes is a kind of preparation method of nanometer silver carbon composite, is comprised the following steps：
1) silver powder and graphite powder are prepared：Weigh silver powder and graphite powder, wherein the mass percent of silver powder be 90wt.%~
99wt.%, the mass percent of graphite powder is 1wt.%~10wt.%, is dried in vacuo, and silver powder and powdered graphite are averaged
Particle diameter is between 10~100 microns；
2) mix and grind：The dried silver powder and graphite powder that are obtained in step 1) are subjected to premixing flour, then carried out
High-energy ball milling, obtain the good silver-colored carbon composite powder of ball milling；
3) Passivation Treatment：The Passivation Treatment that the good silver-colored carbon composite powder of ball milling in step 2) is carried out 1~3 hour is obtained blunt
Composite powder after change processing；
4) cold pressing treatment：Silver-colored carbon composite powder after Passivation Treatment in step 3) is cold-pressed at room temperature, obtains silver
Carbon composite prefabricated section；
5) hot extrusion：Silver-colored carbon composite prefabricated section in step 4) is subjected to hot extrusion under inert gas shielding,
Obtain nanometer silver carbon composite extruded rod.
Further, the vacuum drying time in step 1) is 1~6 hour, and temperature is 50~80 DEG C.
Further, the premixing flour mode in step 2) is ball milling, ratio of grinding media to material 5：1, rotating speed 200r/min.
Further, the high-energy ball milling parameter in step 2) is：Ratio of grinding media to material 5：1~20：1,400~550r/min of rotating speed,
Ball-milling Time is 6~12 hours.
Further, the Passivation Treatment in step 3) is carried out in glove box, and the oxygen content in glove box need to control
Below 200ppm.
Further, the cold pressing treatment in step 4) is carried out at room temperature, and between 100~1000Mpa, the time is pressure
1~30 minute.
Further, hot extrusion in step 5), silver-colored carbon composite prefabricated section is pre-processed before extruding, passed through
Sensing heating quickly heats up to 700~1000 DEG C, and sensing heating speed is 150 DEG C/min, be heated to insulation 2 after extrusion temperature~
Make temperature uniform within 30 minutes.
Further, hot extrusion will be carried out in pretreated silver-colored carbon composite prefabricated section fast transfer to recipient,
Extrusion ratio is 9：1~100：1, recipient temperature is 400~500 DEG C.
Further, hot extrusion is carried out in closed glove box in step 5), is passed through argon gas in glove box in advance
Or nitrogen, oxygen content is less than 1000ppm in atmosphere.
According to the nanometer silver carbon composite prepared by any one above-mentioned nanometer silver carbon composite material and preparation method thereof.
The microstructure of nanometer silver carbon composite made from above method is dispersed in for the carbon particle of nano-scale
Inside silver matrix；ESEM and transmission electron microscope results show that nano carbon particle size is between 3~300 nanometers；Composite
Between consistency is 99.5~100%, hardness is between 55~68Hv, and resistivity is between 1.7~2.5u Ω .cm.
Beneficial effects of the present invention are：
Present invention process is simple, and using common PM technique, preparation has higher-density and hardness, relatively low electricity
The nanometer silver carbon composite of resistance rate, high-energy ball milling is introduced into preparation process, graphite particle is refine to nanoscale, is utilized
It is cold-pressed and without Canned Hot technique, simplifies technological process, shorten preparation time, reduce material cost.
Compared with prior art, graphite particle can refine to nanoscale by the present invention by high-energy ball milling, improve material
Expect performance；Meanwhile extrusion billet is prepared using cold-press process, avoid isostatic pressing process and powder jacket and the degasification of costliness
Journey, shorten preparation time, reduce material cost；In addition, heating sample using the mode of sensing heating, programming rate is fast, sintering
Efficiency high；And sample is heated and extrusion process is carried out under inert atmosphere protection, avoids sample from aoxidizing.
Nanometer silver carbon composite produced by the present invention, good combination property, technological process is short, and the cost of material is low.
Design, concrete structure and the caused technique effect of the present invention are described further below with reference to accompanying drawing, with
It is fully understood from the purpose of the present invention, feature and effect.
Brief description of the drawings
Fig. 1 is the nanometer silver carbon composite scanning electron microscopic picture that powder metallurgical technique is prepared in embodiment 1；
Fig. 2 is the nanometer silver carbon composite transmission electron microscope picture that powder metallurgical technique is prepared in embodiment 2.
Embodiment
With reference to embodiment, the invention will be further described：
Embodiment 1：
Step 1：Respectively by silver powder and graphite powder according to quality proportioning：Silver-colored 95wt.%, graphite 5wt.%, it is weighted and put
Enter ball grinder.
Step 2：Ball grinder is put into vacuum drying chamber, is dried in vacuo 6 hours under the conditions of being 50 DEG C in temperature.
Step 3：The premixing flour of 2 hours is first carried out, rotating speed 200r/min, carries out high-energy ball milling again after mixing powder, parameter is
450r/min, ratio of grinding media to material 5：1, Ball-milling Time 6 hours, every ball milling 3 hours, 0.5 hour out of service.
Step 4：The good nanometer silver carbon composite powder of ball milling in step 3 is taken out from ball grinder, is placed in glove box
The row Passivation Treatment of 2 hours, the oxygen content of glove box should be controlled in below 200ppm.
Step 5：Powder after Passivation Treatment in step 4 is cold-pressed, parameter is：Pressure 500Mpa, dwell time be
10 minutes, prepare silver-colored carbon composite prefabricated section.
Step 6：Prefabricated section sample in step 5 is subjected to sensing heating and hot extrusion, parameter are：Induction heating temperature is
850 DEG C, heating rate is 150 DEG C/min, and hot extrusion, extrusion ratio are carried out in fast transfer to recipient after sample is incubated 2 minutes
For 25：1, recipient temperature is 500 DEG C.Hot extrusion is carried out in closed glove box, is passed through argon gas, atmosphere in glove box in advance
Middle oxygen content is less than 1000ppm.
Fig. 1 is the nanometer silver carbon composite scanning electron microscopic picture that powder metallurgical technique is prepared in embodiment 1.It can see
The carbon particle for going out nano-scale is dispersed in inside silver matrix；Carbon particle size is less than 300 nanometers.Table 1 is powder metallurgy work
The nanometer silver carbon composite property list that skill is prepared, composite consistency are 99.6%, hardness 58Hv, and resistivity is
1.8uΩ.cm。
| Composition | Consistency (%) | Resistivity (u Ω .cm) | Microhardness (HV) |
| Ag~5wt.%C | 99.6 | 1.8 | 58 |
The nanometer silver carbon composite property list that powder metallurgical technique is prepared in the embodiment 1 of table 1.
Embodiment 2：
Step 1：Respectively by silver powder and graphite powder according to quality proportioning：Silver-colored 96.4wt.%, graphite 3.6wt.%, it is weighted
And it is put into ball grinder.
Step 2：Ball grinder is put into vacuum drying chamber, is dried in vacuo 4 hours under the conditions of being 60 DEG C in temperature.
Step 3：The premixing flour of 2 hours is first carried out, rotating speed 200r/min, carries out high-energy ball milling again after mixing powder, parameter is
500r/min, ratio of grinding media to material 10：1, Ball-milling Time 12 hours, every ball milling 3 hours, 0.5 hour out of service.
Step 4：The good nanometer silver carbon composite powder of ball milling in step 3 is taken out from ball grinder, is placed in glove box
The row Passivation Treatment of 2 hours, the oxygen content of glove box should be controlled in below 200ppm.
Step 5：Powder after Passivation Treatment in step 4 is cold-pressed, parameter is：Pressure 800Mpa, dwell time 5
Minute, prepare silver-colored carbon composite prefabricated section.
Step 6：Prefabricated section sample in step 5 is subjected to sensing heating and hot extrusion, parameter are：Induction heating temperature
950 DEG C, heating rate is 150 DEG C/min, and hot extrusion, extrusion ratio are carried out in fast transfer to recipient after sample is incubated 5 minutes
For 50：1, recipient temperature is 500 DEG C.Hot extrusion is carried out in closed glove box, is passed through argon gas, atmosphere in glove box in advance
Middle oxygen content is less than 1000ppm.
Fig. 2 is the nanometer silver carbon composite transmission electron microscope picture that powder metallurgical technique is prepared in embodiment 2.It can see
The carbon particle for going out nano-scale is dispersed in inside silver matrix；Carbon particle size is between 3~10 nanometers.Table 2 is powder smelting
The nanometer silver carbon composite property list that gold process is prepared, composite consistency are 99.9%, hardness 62Hv, resistance
Rate is 2.3u Ω .cm.
| Composition | Consistency (%) | Resistivity (u Ω .cm) | Microhardness (HV) |
| Ag~3.6wt%C | 99.9 | 2.3 | 62 |
The nanometer silver carbon composite property list that powder metallurgical technique is prepared in the embodiment 2 of table 2
Preferred embodiment of the invention described in detail above.It should be appreciated that one of ordinary skill in the art without
Creative work can is needed to make many modifications and variations according to the design of the present invention.Therefore, all technologies in the art
Personnel are available by logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Technical scheme, all should be in the protection domain being defined in the patent claims.
Claims (10)
1. a kind of preparation method of nanometer silver carbon composite, it is characterised in that comprise the following steps：
1) silver powder and graphite powder are prepared：Weigh silver powder and graphite powder, wherein the mass percent of the silver powder be 90wt.%~
99wt.%, the mass percent of the graphite powder is 1wt.%~10wt.%, is dried in vacuo, the silver powder and graphite powder
The average grain diameter at end is between 10~100 microns；
2) mix and grind：The dried silver powder and graphite powder that are obtained in step 1) are subjected to premixing flour, then carry out high energy
Ball milling, obtain the good silver-colored carbon composite powder of ball milling；
3) Passivation Treatment：The Passivation Treatment that the good silver-colored carbon composite powder of ball milling in step 2) is carried out 1~3 hour is obtained at passivation
Composite powder after reason；
4) cold pressing treatment：Silver-colored carbon composite powder after Passivation Treatment in step 3) is cold-pressed at room temperature, silver-colored carbon is obtained and answers
Condensation material prefabricated section；
5) hot extrusion：Silver-colored carbon composite prefabricated section in step 4) is subjected to hot extrusion under inert gas shielding, obtained
Nanometer silver carbon composite extruded rod.
2. according to the preparation method of the nanometer silver carbon composite described in claim 1, it is characterised in that in the step 1)
The vacuum drying time be 1~6 hour, temperature be 50~80 DEG C.
3. according to the preparation method of the nanometer silver carbon composite described in claim 1, it is characterised in that in the step 2)
Premixing flour mode be ball milling, ratio of grinding media to material 5：1, rotating speed 200r/min.
4. according to the preparation method of the nanometer silver carbon composite described in claim 1, it is characterised in that in the step 2)
High-energy ball milling parameter be：Ratio of grinding media to material 5：1~20：1,400~550r/min of rotating speed, Ball-milling Time are 6~12 hours.
5. according to the preparation method of the nanometer silver carbon composite described in claim 1, it is characterised in that in the step 3)
Passivation Treatment carried out in glove box, the oxygen content in glove box need to be controlled in below 200ppm.
6. according to the preparation method of the nanometer silver carbon composite described in claim 1, it is characterised in that in the step 4)
Cold pressing treatment carry out at room temperature, pressure between 100~1000Mpa, the time be 1~30 minute.
7. according to the preparation method of the nanometer silver carbon composite described in claim 1, it is characterised in that in the step 5)
Hot extrusion, the silver-colored carbon composite prefabricated section is pre-processed before extruding, 700 are quickly heated up to by sensing heating
~1000 DEG C, sensing heating speed is 150 DEG C/min, and being heated to being incubated 2~30 minutes after extrusion temperature makes temperature uniform.
8. according to the preparation method of the nanometer silver carbon composite described in claim 7, it is characterised in that will be pretreated
Hot extrusion, extrusion ratio 9 are carried out in silver-colored carbon composite prefabricated section fast transfer to recipient：1~100：1, recipient temperature
For 400~500 DEG C.
9. according to the preparation method of the nanometer silver carbon composite described in claim 1, it is characterised in that in the step 5)
Hot extrusion is carried out in closed glove box, is passed through argon gas or nitrogen in glove box in advance, and oxygen content is less than in atmosphere
1000ppm。
A kind of 10. receiving prepared by nanometer silver carbon composite material and preparation method thereof according to any one in claim 1~9
The silver-colored carbon composite of rice.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111218581A (en) * | 2020-02-24 | 2020-06-02 | 昆明贵金属研究所 | High-density high-strength silver-carbon composite electric contact material and preparation method thereof |
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