CN106670501A - Preparing method for graphene-metal base composite powder - Google Patents
Preparing method for graphene-metal base composite powder Download PDFInfo
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- CN106670501A CN106670501A CN201611241794.6A CN201611241794A CN106670501A CN 106670501 A CN106670501 A CN 106670501A CN 201611241794 A CN201611241794 A CN 201611241794A CN 106670501 A CN106670501 A CN 106670501A
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Abstract
The invention discloses a preparing method for graphene-metal base composite powder. Oxidized graphene and deionized water are mixed, subjected to ultrasounds and dispersed evenly; meanwhile silver nitrate or copper sulfate is subjected to ultrasounds in absolute ethyl alcohol; then a silver nitrate or copper sulfate solution is poured into a graphene dispersion solution, stirring is conducted under the water bath condition, hydrazine hydrate is added for a reaction, washing, filtering and drying are conducted after the reaction is completed, and the graphene load metal composite powder is obtained; the graphene load metal composite powder and the absolute ethyl alcohol are mixed, dispersed and homogenized, then silver powder or copper powder is added for ultrasound mixing, drying is conducted, and the graphene-metal base composite powder is obtained. Little graphene in the obtained graphene-metal base composite powder is agglomerated and is not oxidized, the powder mixing time is short, efficiency is high, the graphene-metal base composite powder can be directly used for preparing block graphene-metal base composite powder, and raw materials are provided for the subsequent technology.
Description
Technical field
The invention belongs to the preparing technical field of composite, and in particular to a kind of Graphene-metal-based compound powder body
Preparation method.
Background technology
Graphene be one kind by carbon atom with sp2The similar cellular two-dimensional crystal lattice flat thin that hybrid orbital is arranged in
Film.It is material most thin in the world that thickness is about 0.335nm, the specific surface area with super large.Each of which C atom has four valency electricity
Son, is connected between each carbon atom by the very strong σ keys of polarity, after σ keys are formed, each carbon atom there remains one not into
The pi-electron of key, these electronics random in crystal can be moved freely, therefore its electric conductivity is superpower, can be good as one
Carrier is incorporated in composite.
Metallic copper and argent have high heat conduction, conductive and forming property, are the important matrixes for preparing above-mentioned composite
Material, prepares in pertinent literature report in current relevant Graphene cuprio or silver-based composite powder material, and majority is confined to copper
Graphene is directly added in powder or argentum powder, more mixed powder, Graphene in powder body after mixing is carried out using high energy spheroidal graphite method, homogenizer etc.
Easily occur agglomeration in powder body, the performance of material greatly reduces.
The content of the invention
It is an object of the invention to provide a kind of Graphene-metal-based compound raw powder's production technology, solves existing preparation
The problem that method Graphene is easily reunited in powder body.
The technical solution adopted in the present invention is, a kind of Graphene-metal-based compound raw powder's production technology, specifically according to
Following steps are implemented：
Step 1, graphene oxide is uniform with deionized water mixing ultrasonic disperse, obtain graphene dispersing solution；By nitric acid
The silver or copper sulfate ultrasound in dehydrated alcohol, obtains silver nitrate solution or copper-bath；
Step 2, then pours silver nitrate solution or copper-bath in graphene dispersing solution into, stirs simultaneously under water bath condition
Hydration hydrazine reaction is added, washed after the completion of reaction, filter, be dried, obtain graphene-supported argentum composite powder body or graphene-supported
Copper composite powders；
Step 3, the composite granule that step 2 is obtained is scattered in dehydrated alcohol, in ultrasonic power for 1800-2500W's
Crushed in cell disruptor, decentralized processing 10-30 minute, then add composite granule quality 50-100 times argentum powder or
Copper powder, continues ultrasonic disperse 10-30 minutes, is dried, and obtains Graphene-silver-based composite granule or Graphene-cuprio composite granule.
Of the invention the characteristics of, also resides in,
Silver nitrate solution is 1 with the mass ratio of silver nitrate with graphene oxide in graphene dispersing solution in step 2：2.5-
16, use 1ml hydrazine hydrates per 5-16mg silver nitrate correspondence.
Copper-bath is 1 with the mass ratio of copper sulfate with graphene oxide in graphene dispersing solution in step 2：1.5-5,
1ml hydrazine hydrates are used per 15-25mg copper sulfate correspondence.
Bath temperature is 70 DEG C -90 DEG C in step 2, adds hydration hydrazine reaction 1-2h.
The particle diameter of argentum powder or copper powder is 200-500nm in step 3.
The invention has the beneficial effects as follows, Graphene of the present invention-metal-based compound raw powder's production technology, with graphite oxide
Alkene, silver nitrate or copper sulfate be raw material, by add reducing agent hydrazine hydrate carry out reduction reaction be obtained graphene-supported metal from
The composite of son, has blended the Graphene-metal-based compound powder body of few soilless sticking, greatly using the principle of ultrasonic disperse
Improve and Graphene reunion during powder is mixed present in research at present, disperses uneven phenomenon, while using simplest
Drying meanss, reduce cost, it is therefore prevented that oxidation.The process stabilizing, solves the problems, such as that well Graphene is easily reunited, technique behaviour
Make simple, equipment investment low, reliable in quality is adapted to industrialization large-scale production.
Description of the drawings
Fig. 1 is that scale is 1 μm of scanning electron microscope (SEM) photograph under Graphene-silver-based composite granule microcosmic prepared by embodiment 3；
Fig. 2 is the Graphene-silver-based composite granule energy spectrum diagram prepared by embodiment 3；
Fig. 3 be under Graphene-silver-based composite granule microcosmic prepared by embodiment 3 scale for 100nm transmission electron microscope picture；
Fig. 4 is the X-ray diffractogram of the Graphene-silver-based composite granule prepared by embodiment 3；
Fig. 5 is that scale is 2 μm of stereoscan photograph under Graphene-cuprio composite granule microcosmic that embodiment 4 is obtained；
Fig. 6 is Graphene-cuprio composite granule energy spectrum diagram that embodiment 4 is obtained；
Fig. 7 is Graphene-cuprio composite granule X-ray diffractogram that embodiment 4 is obtained.
Specific embodiment
With reference to the accompanying drawings and detailed description the present invention is described in detail.
Graphene of the present invention-metal-based compound raw powder's production technology, specifically implements according to following steps：
Step 1, graphene oxide is uniform with deionized water mixing ultrasonic disperse, obtain graphene dispersing solution；By nitric acid
The silver or copper sulfate ultrasound in dehydrated alcohol, obtains silver nitrate solution or copper-bath；
Step 2, is 1 according to the mass ratio of graphene oxide and copper sulfate：The ratio of 2.5-16, by graphene oxide solution
Mix with copper-bath, or, it is 1 according to the mass ratio of graphene oxide and copper sulfate：The ratio of 1.5-5, will aoxidize stone
Black alkene solution and copper-bath mix, and hydration hydrazine reaction is stirred and added under 70 DEG C of -90 DEG C of water bath conditions (per 5-16mg nitric acid
Silver is corresponding to use 1ml hydrazine hydrates using 1ml hydrazine hydrates or per 15-25mg copper sulfate correspondence), wash after the completion of reaction, filter,
It is dried, obtains graphene-supported argentum composite powder body or graphene-supported copper composite powders；
Step 3, the composite granule that step 2 is obtained is scattered in dehydrated alcohol, in ultrasonic power for 1800-2500W's
Crushed in cell disruptor, decentralized processing 10-30 minute, then add composite granule quality 50-100 times argentum powder or
Copper powder (particle diameter of argentum powder or copper powder is 200-500nm), continues ultrasonic disperse 10-30 minutes, is dried, and obtains Graphene-silver-based
Composite granule or Graphene-cuprio composite granule.
It is of the invention mainly to reach the purpose that graphene uniform disperses and reduces Graphene thickness using ultrasound.Ultrasonic powder
Broken is, when supersonic vibration is delivered in liquid, because the sound intensity is very big, in a liquid to excite very strong cavitation effect, so as to
Substantial amounts of cavitation bubble is produced in liquid.As these cavitation bubbles are produced and explosion, microjet will be produced, and then by liquid
Solid particle smash.Simultaneously because the vibration of ultrasound wave, makes solid-liquid more fully dispersion mixing uniform.In ultrasonic explosion point
Copper ion, silver ion is set to enter wherein while opening graphene layer again, it is possible to pull open Graphene interfloor distance, reach Graphene
Dispersed and load upper copper, the purpose of silver ion.
Compared with the mixed powder of existing high-energy ball milling, the graphite in Graphene-metal-base composites powder body that the present invention is obtained
Alkene is reunited few, and without being oxidized, mixes that the powder used time is short, efficiency high, can be directly used for preparing the Graphene-metal-based compound of block
Material powder, for subsequent technique raw material is provided.The process stabilizing, solves the problems, such as that well Graphene is easily reunited, technique
Simple to operate, equipment investment is low, powder quality reliability, is adapted to industrialization large-scale production.
Embodiment 1
Step 1,50mg graphene oxides are dispersed in 100mg deionized waters, are disperseed under 40KHz ultrasonic environments
2h；Obtain graphene oxide dispersion；Silver nitrate 125mg and 10ml dehydrated alcohol are disperseed into 2h under 40KHz ultrasonic environments,
Obtain silver nitrate solution；
Step 2, silver nitrate solution is poured in graphene dispersing solution in the thermostat water bath for proceeding to 80 DEG C carries out electromagnetism and stirs
Mix, while adding 5ml, the hydration hydrazine reaction 2h that concentration is 75%, be cooled to room temperature, distinguished using deionized water and dehydrated alcohol
Centrifugal treating 3 times, is dried using electric heating cover to the precipitate after centrifugation at less than 60 DEG C, and the Graphene for obtaining non-oxidation is born
Carry the composite granule of silver；
Step 3, the graphene-supported argentum composite powder body 0.5g that step 2 is obtained and dehydrated alcohol 300ml mix, in ultrasound
Power in the cell disruptor of 2200W to be crushed, decentralized processing 20min, adds the silver that 30g, mean diameter are 400nm
Powder carries out ultrasonication, dispersion, mixing 20min, obtains that layer is thin and finely dispersed Graphene-silver-based composite material；
Step 4, Graphene-silver-based composite material that step 3 is obtained is dried at 60 DEG C using electric heating cover, i.e.,
Obtain being directly used in the Graphene for preparing block-silver-based composite granule.
Embodiment 2
Step 1,50mg graphene oxides are dispersed in 75mg deionized waters, and under 40KHz ultrasonic environments 2h is disperseed,
Obtain graphene oxide dispersion；500mg silver nitrate and 10ml dehydrated alcohol are disperseed into 2h under 40KHz ultrasonic environments, is obtained
To silver nitrate solution；
Step 2, silver nitrate solution is poured in graphene dispersing solution in the thermostat water bath for proceeding to 70 DEG C carries out electromagnetism and stirs
Mix, while adding 5ml, the hydration hydrazine reaction 1.5h that concentration is 75%, be cooled to room temperature, using deionized water and dehydrated alcohol point
Other centrifugal treating 3 times, is dried using electric heating cover to the precipitate after centrifugation at less than 60 DEG C, obtains the Graphene of non-oxidation
The composite granule of load silver；
Step 3, the graphene-supported argentum composite powder body 0.5g that step 2 is obtained and dehydrated alcohol 300ml mix, in ultrasound
Power in the cell disruptor of 2200W to be crushed, decentralized processing 10min, adds the silver that 30g, mean diameter are 400nm
Powder carries out ultrasonication, dispersion, mixing 15min, obtains that layer is thin and finely dispersed Graphene-silver-based composite material；
Step 4, Graphene-silver-based composite material that step 3 is obtained is dried at 60 DEG C using electric heating cover, i.e.,
Obtain being directly used in the Graphene for preparing block-silver-based composite granule.
Embodiment 3
Step 1,50mg graphene oxides are dispersed in 50mg deionized waters, and under 40KHz ultrasonic environments 2h is disperseed,
Obtain graphene oxide dispersion；800mg silver nitrate and 10ml dehydrated alcohol are disperseed into 2h under 40KHz ultrasonic environments；
Step 2, silver nitrate solution is poured in graphene dispersing solution in the thermostat water bath for proceeding to 90 DEG C carries out electromagnetism and stirs
Mix, while adding 5ml, the hydration hydrazine reaction 1h that concentration is 75%, be cooled to room temperature, distinguished using deionized water and dehydrated alcohol
Centrifugal treating 3 times, is dried using electric heating cover at less than 60 DEG C, obtains the composite granule of the graphene-supported silver of non-oxidation；
Step 3, the graphene-supported argentum composite powder body 0.5g that step 2 is obtained and dehydrated alcohol 300ml mix, in ultrasound
Power in the cell disruptor of 2200W to be crushed, decentralized processing 30min, adds the silver that 30g, mean diameter are 400nm
Powder carries out ultrasonication, dispersion, mixing 30min, obtains that layer is thin and finely dispersed Graphene-silver-based composite material；
Step 4, Graphene-silver-based composite material that step 3 is obtained is dried at 60 DEG C using electric heating cover, i.e.,
Obtain being directly used in the Graphene for preparing block-silver-based composite granule.
The structure and performance of the Graphene obtained to embodiment 3-silver-based composite granule detect, its pattern such as Fig. 1 institutes
Show, from Fig. 1 it can clearly be seen that thin graphene is wrapped up, is wrapped between Argent grain, Fig. 2 shows that Graphene silver-based is combined
The content situation of powder body selected areas, hence it is evident that it can be seen that composition is essentially carbon and silver, illustrate the powder body prepared not by oxygen
Change.Fig. 3 illustrates graphene layer than relatively thin.From the XRD figure of Fig. 4, the diffraction maximum of four silver is found that in the composite granule
(111), (200), (220), (311), in addition to this four diffraction maximums other diffraction maximums are not found, illustrate mixed powder
In silver do not aoxidize；Because Graphene addition is less in mixed powder, fail the diffraction maximum for finding carbon.
Embodiment 4
Step 1,50mg graphene oxides are dispersed in 100ml deionized waters, in the ultrasound wave ring of ultrasonic power 40KHz
Disperse under border, 75mg copper sulfate is scattered in 10ml dehydrated alcohol, and disperse under 40KHz ultrasonic environments.
Step 2, above-mentioned copper-bath is mixed with graphene oxide solution, and proceeds to enter in 90 DEG C of thermostat water bath
Row electromagnetic agitation, at the same add 5ml hydrazine hydrates (mass ratio is 75%), react 1 hour, be cooled to room temperature, by solid product according to
Secondary deionized water and each centrifugal treating of dehydrated alcohol three times, by the precipitate after centrifugation using electric heating cover at less than 60 DEG C
It is dried, obtains the composite granule of the graphene-supported copper of non-oxidation.
Step 3, takes the graphene-supported copper composite powders 0.5g for preparing, and the dehydrated alcohol of 300ml burns in 500ml
Mixed in cup, crushed in ultrasonic power is for the cell disruptor of 2200W, decentralized processing 20 minutes, added 30g
Copper powder (particle diameter 500nm), carry out again under same ultrasound condition ultrasonication, dispersion, mixing 20 minutes, you can obtain layer it is thin and point
Dissipate uniform Graphene-Cu-base composites.
Step 4, the powder body after dispersion is dried at 60 DEG C using electric heating cover, you can.
The structure and performance of the Graphene obtained to embodiment 4-cuprio composite granule detect, its pattern such as Fig. 5 institutes
Show, from Fig. 5 it can clearly be seen that thin graphene is wrapped up, is wrapped between copper granule, Fig. 6 shows that Graphene cuprio is combined
The content situation of split selected areas, hence it is evident that it can be seen that composition is essentially carbon, copper and minimal amount of oxygen, the content of oxygen almost may be used
To ignore, illustrate that the powder body prepared almost is not oxidized.From the XRD figure of Fig. 7, three are found that in the composite granule
The diffraction maximum (111) of copper, (200), (220), do not find other diffraction maximums in addition to these three diffraction maximums, illustrate mixed
The copper closed in powder body is not aoxidized；Because Graphene addition is less in mixed powder, fail the diffraction maximum for finding carbon.
Embodiment 5
Step 1,30mg graphene oxides are dispersed in 15ml deionized waters, in the ultrasound wave ring of ultrasonic power 40KHz
Disperse under border, 150mg copper sulfate is scattered in 10ml dehydrated alcohol, and disperse under 40KHz ultrasonic environments.
Step 2, above-mentioned copper-bath is mixed with graphene oxide solution, and proceeds to enter in 80 DEG C of thermostat water bath
Row electromagnetic agitation, at the same add 6ml hydrazine hydrates (mass ratio is 75%), react 2 hours, be cooled to room temperature, by solid product according to
Secondary deionized water and each centrifugal treating of dehydrated alcohol three times, and be dried at less than 60 DEG C using electric heating cover, obtain anaerobic
The composite granule of the graphene-supported copper changed.
Step 3, takes the graphene-supported copper composite powders 0.3g that step 2 is prepared, and the dehydrated alcohol of 300ml exists
Mixed in 500ml beakers, crushed in ultrasonic power is for the cell disruptor of 1800W, decentralized processing 30 minutes, then
30g copper powders (particle diameter 200nm) are added, ultrasonication, dispersion is carried out under same ultrasound condition again, is mixed 30 minutes, you can obtain
Layer is thin and finely dispersed Graphene-Cu-base composites.
Step 4, the powder body after dispersion is dried at 60 DEG C using electric heating cover, you can.
Embodiment 6
Step 1,100mg graphene oxides is dispersed in 100ml deionized waters, in the ultrasound wave of ultrasonic power 40KHz
Disperse under environment, 200mg copper sulfate is scattered in 10ml dehydrated alcohol, and disperse under 40KHz ultrasonic environments.
Step 2, above-mentioned copper-bath is mixed with graphene oxide solution, and proceeds to enter in 60 DEG C of thermostat water bath
Row electromagnetic agitation, at the same add 8ml hydrazine hydrates (mass ratio is 75%), react 3 hours, be cooled to room temperature, by solid product according to
Secondary deionized water and each centrifugal treating of dehydrated alcohol three times, and be dried at less than 60 DEG C using electric heating cover, obtain anaerobic
The composite granule of the graphene-supported copper changed.
Step 3, takes the graphene-supported copper composite powders 0.6g that step 2 is prepared, and the dehydrated alcohol of 300ml exists
Mixed in 500ml beakers, crushed in ultrasonic power is for the cell disruptor of 2500W, decentralized processing 10 minutes, then
30g copper powders (particle diameter 300nm) are added, ultrasonication, dispersion is carried out under same ultrasound condition again, is mixed 10 minutes, you can obtain
Layer is thin and finely dispersed Graphene-Cu-base composites.
Step 4, the powder body after dispersion is dried at 60 DEG C using electric heating cover, you can.
Claims (5)
1. a kind of Graphene-metal-based compound raw powder's production technology, it is characterised in that specifically implement according to following steps：
Step 1, graphene oxide is uniform with deionized water mixing ultrasonic disperse, obtain graphene dispersing solution；By silver nitrate or
Copper sulfate ultrasound in dehydrated alcohol, obtains silver nitrate solution or copper-bath；
Step 2, then pours silver nitrate solution or copper-bath in graphene dispersing solution into, stirs and adds under water bath condition
Hydration hydrazine reaction, washs after the completion of reaction, filters, is dried, and obtains graphene-supported argentum composite powder body or graphene-supported copper is multiple
Close powder body；
Step 3, the composite granule that step 2 is obtained is scattered in dehydrated alcohol, in the cell that ultrasonic power is 1800-2500W
Crushed in pulverizer, decentralized processing 10-30 minute, then add the argentum powder or copper of composite granule quality 50-100 times
Powder, continues ultrasonic disperse 10-30 minutes, is dried, and obtains Graphene-silver-based composite granule or Graphene-cuprio composite granule.
2. Graphene according to claim 1-metal-based compound raw powder's production technology, it is characterised in that nitre in step 2
Sour silver solution is 1 with the mass ratio of silver nitrate with graphene oxide in graphene dispersing solution：2.5-16, per 5-16mg silver nitrate pair
1ml hydrazine hydrates should be used.
3. Graphene according to claim 1-metal-based compound raw powder's production technology, it is characterised in that sulfur in step 2
Sour copper solution is 1 with the mass ratio of copper sulfate with graphene oxide in graphene dispersing solution：1.5-5, per 15-25mg copper sulfate pair
1ml hydrazine hydrates should be used.
4. according to the arbitrary described Graphene-metal-based compound raw powder's production technology of claims 1 to 3, it is characterised in that step
Bath temperature is 70 DEG C -90 DEG C in rapid 2, adds hydration hydrazine reaction 1-2h.
5. Graphene according to claim 1-metal-based compound raw powder's production technology, it is characterised in that silver in step 3
The particle diameter of powder or copper powder is 200-500nm.
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| CN108127112A (en) * | 2017-12-28 | 2018-06-08 | 宁波丞材金属表面处理有限公司 | A kind of copper-based composite granule and its preparation method and application |
| CN108677172A (en) * | 2018-04-18 | 2018-10-19 | 重庆材料研究院有限公司 | A kind of Zero-discharge non-pollution graphene electroless copper plating method |
| KR102361553B1 (en) * | 2020-11-18 | 2022-02-14 | 주식회사 케이비엘러먼트 | Manufacturing method of graphene coated inorganic particle and graphene coated inorganic manufactured by the same |
| CN113512662A (en) * | 2021-07-16 | 2021-10-19 | 陕西科技大学 | Silver-loaded graphene/copper self-lubricating material and preparation method thereof |
| CN114464369A (en) * | 2021-12-31 | 2022-05-10 | 上海匡宇科技股份有限公司 | Preparation method of solar cell conductive silver paste |
| CN114535594A (en) * | 2021-12-31 | 2022-05-27 | 嘉兴辰昊新材料科技有限公司 | Preparation method of nano reduced graphene oxide silver powder and graphene silver powder |
| CN115301941A (en) * | 2022-08-12 | 2022-11-08 | 大连大学 | Brake copper-iron-based composite friction material and preparation method thereof |
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