CN108655412A - A kind of preparation method of load nickel particles graphene powder - Google Patents
A kind of preparation method of load nickel particles graphene powder Download PDFInfo
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- CN108655412A CN108655412A CN201810359404.8A CN201810359404A CN108655412A CN 108655412 A CN108655412 A CN 108655412A CN 201810359404 A CN201810359404 A CN 201810359404A CN 108655412 A CN108655412 A CN 108655412A
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
Abstract
The invention discloses a kind of preparation methods of load nickel particles graphene powder, specifically implement in accordance with the following steps：Graphene oxide and nickel ion solution are first configured, two kinds of solution are mixed, adjusts pH value, reducing agent hydrazine hydrate is added to be restored, is then transferred in water-bath and is reacted, after reaction centrifuge washing, it is freeze-dried again to get load nickel particles graphene powder.Pass through the above method, nickel particles can be introduced into graphene sheet layer by the present invention, solve the problems, such as that graphene is easily reunited, nickel particles are made to be evenly distributed on graphene, this method is that basis early period has been established in the preparation that graphene enhances in Metal Substrate block composite material, is had broad application prospects.
Description
Technical field
The invention belongs to graphene preparation method technical field, and in particular to a kind of graphene powder of load nickel particles
Preparation method.
Background technology
Graphene has the hexagonal cell shape structure that is made of with sp2 hybridized orbits single layer of carbon atom, is intensity so far
Highest material, theoretical strength reach 125GPa, and the capacity of heat transmission reaches 5000W/ (mk)；Elasticity modulus is 1TPa, and most thin most
Light material, thickness are only 0.34nm, density 2.2g/cm3.It is wide that the excellent performance of graphene makes it have in various fields
Application prospect.
Graphene can prepare the metal-base composites of excellent combination property as the ideal reinforcement of Metal Substrate.But
It is that the huge specific surface area of graphene and high surface energy cause graphene to be easy to reunite, and it is multiple in Metal Substrate to constrain graphene
Extensive use in condensation material.Therefore, seek a kind of method that solution graphene is easily reunited, realize graphene in metallic matrix
It is evenly dispersed, have important engineering significance and practical value.
Invention content
The object of the present invention is to provide a kind of load nickel particles graphene powders, solve graphene itself and are also easy to produce reunion
The problem of.
The first technical solution of the present invention is a kind of preparation method of load nickel particles graphene powder, tool
Body implementation steps are as follows：.
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 13-40%, nickel nitrate 60-87%,
The sum of above constituent mass percentage is 100%；
Step 2, graphene oxide is added in deionized water, continues the obtained oxygen of ultrasonic disperse 60min after stirring 30min
Graphite alkene solution；
Step 3, the nickel nitrate is dissolved in alcoholic solution, nickel nitrate is 1 with alcohol quality ratio:55-80 is to get to nitre
Sour nickel solution；
Step 4, nickel nitrate solution is added dropwise in graphene oxide solution, dropwise addition process is carried out at the same time stirring, drop
Continue to stir 30min after adding, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, mixed solution pH value is adjusted to 9- using sodium hydroxide solution
11, hydrazine hydrate is then added dropwise, transfers in 90 DEG C of water-baths and keeps the temperature 2-4h, magnetic agitation is carried out in insulating process, protects
It is taken out after temperature, then cooled to room temperature sops up supernatant liquor with suction pipe, wine is used first to remaining black floccule
Essence and deionized water washing, then centrifugal treating is carried out, obtain solid product；
Step 6, the solid product is freeze-dried to get the graphene of load nickel particles.
The features of the present invention also characterized in that
A concentration of the 99.7% of the alcoholic solution of step 3, nickel nitrate are 1 with alcohol quality ratio:55-80.
The hydrazine hydrate mass concentration of step 5 is 85%, and the mass ratio of hydrazine hydrate and mixed solution is 1:10-28.
It is -55 DEG C that step 6, which is freeze-dried temperature, time 9-14h.
The invention has the advantages that a kind of load nickel particles graphene powder of the present invention, by graphene sheet layer
Between introduce the second phase nickel particles, solve the problems, such as graphene itself easily reunite, realize the evenly dispersed of graphene, be graphite
Basis early period has been established in preparation in alkene enhancing Metal Substrate block composite material, is had broad application prospects.
Description of the drawings
Fig. 1 is a kind of load nickel particles graphene powder preparation flow figure of the present invention；
Fig. 2 is a kind of load nickel particles graphene powder stereoscan photograph of the present invention.
Specific implementation mode
It is a kind of load nickel particles graphene powder preparation method detailed process as shown in Figure 1, concrete operation step is as follows：
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 13-40%, nickel nitrate 60-87%,
The sum of above constituent mass percentage is 100%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 60min systems after stirring 30min
Obtain graphene oxide solution；
Step 3, the nickel nitrate is dissolved in the alcoholic solution that mass concentration is 99.7%, the nickel nitrate and alcohol matter
Amount is than being 1:55-80 is to get to nickel nitrate solution；
Step 4, the nickel nitrate solution is added dropwise in the graphene oxide solution, dropwise addition, which is carried out at the same time, stirs
It mixes, continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, are adjusted to the mixed solution pH value using sodium hydroxide solution
Mass concentration is then added dropwise as 85% hydrazine hydrate in 9-11, and the mass ratio of hydrazine hydrate and mixed solution is 1:10-28, then
It is transferred in 90 DEG C of water-baths and keeps the temperature 2-4h, magnetic agitation is carried out in insulating process, is taken out after heat preservation, naturally cools to room
Then temperature sops up supernatant liquor with suction pipe, use alcohol and deionized water to wash first remaining black floccule, then carry out from
Heart processing, obtains solid product；
Step 6, the solid product is freeze-dried, freeze-drying temperature be -55 DEG C, the time be 9-14h to get
Load the graphene of nickel particles.
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 13%, nickel nitrate 87%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 60min systems after stirring 30min
Obtain graphene oxide solution；
Step 3, the nickel nitrate is dissolved in the alcoholic solution that mass concentration is 99.7%, the nickel nitrate and alcohol matter
Amount is than being 1:55 to get to nickel nitrate solution；
Step 4, the nickel nitrate solution is added dropwise in the graphene oxide solution, dropwise addition process is carried out at the same time
Stirring continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, are adjusted to the mixed solution pH value using sodium hydroxide solution
9, mass concentration is then added dropwise as 85% hydrazine hydrate, the mass ratio of hydrazine hydrate and mixed solution is 1:10, it transfers to
2h is kept the temperature in 90 DEG C of water-baths, and magnetic agitation is carried out in insulating process, is taken out after heat preservation, cooled to room temperature, then
Supernatant liquor is sopped up with suction pipe, uses alcohol and deionized water to wash first remaining black floccule, then carry out centrifugal treating,
Obtain solid product；
Step 6, the solid product is freeze-dried, freeze-drying temperature is -55 DEG C, and the time is 9h to get negative
Carry the graphene of nickel particles.
Embodiment 2
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 40%, nickel nitrate 60%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 60min systems after stirring 30min
Obtain graphene oxide solution；
Step 3, the nickel nitrate is dissolved in the alcoholic solution that mass concentration is 99.7%, the nickel nitrate and alcohol matter
Amount is than being 1:80 to get to nickel nitrate solution；
Step 4, the nickel nitrate solution is added dropwise in the graphene oxide solution, dropwise addition process is carried out at the same time
Stirring continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, are adjusted to the mixed solution pH value using sodium hydroxide solution
11, mass concentration is then added dropwise as 85% hydrazine hydrate, the mass ratio of hydrazine hydrate and mixed solution is 1:28, it transfers to
4h is kept the temperature in 90 DEG C of water-baths, and magnetic agitation is carried out in insulating process, is taken out after heat preservation, cooled to room temperature, then
Supernatant liquor is sopped up with suction pipe, uses alcohol and deionized water to wash first remaining black floccule, then carry out centrifugal treating,
Obtain solid product；
Step 6, the solid product is freeze-dried, freeze-drying temperature is -55 DEG C, and the time is 14h to get negative
Carry the graphene of nickel particles.
Embodiment 3
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 26.5%, nickel nitrate 77.5%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 60min systems after stirring 30min
Obtain graphene oxide solution；
Step 3, the nickel nitrate is dissolved in the alcoholic solution that mass concentration is 99.7%, the nickel nitrate and alcohol matter
Amount is than being 1:67.5 to get to nickel nitrate solution；
Step 4, the nickel nitrate solution is added dropwise in the graphene oxide solution, dropwise addition, which is carried out at the same time, stirs
It mixes, continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, are adjusted to the mixed solution pH value using sodium hydroxide solution
10, mass concentration is then added dropwise as 85% hydrazine hydrate, the mass ratio of hydrazine hydrate and mixed solution is 1:19, it transfers to
3h is kept the temperature in 90 DEG C of water-baths, and magnetic agitation is carried out in insulating process, is taken out after heat preservation, cooled to room temperature, then
Supernatant liquor is sopped up with suction pipe, uses alcohol and deionized water to wash first remaining black floccule, then carry out centrifugal treating,
Obtain solid product；
Step 6, the solid product is freeze-dried, freeze-drying temperature be -55 DEG C, the time be 11.5h to get
Load the graphene of nickel particles.
Embodiment 4
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 33%, nickel nitrate 67%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 60min systems after stirring 30min
Obtain graphene oxide solution；
Step 3, the nickel nitrate is dissolved in the alcoholic solution that mass concentration is 99.7%, the nickel nitrate and alcohol matter
Amount is than being 1:60 to get to nickel nitrate solution；
Step 4, the nickel nitrate solution is added dropwise in the graphene oxide solution, dropwise addition, which is carried out at the same time, stirs
It mixes, continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, are adjusted to the mixed solution pH value using sodium hydroxide solution
10, mass concentration is then added dropwise as 85% hydrazine hydrate, the mass ratio of hydrazine hydrate and mixed solution is 1:20, it transfers to
3h is kept the temperature in 90 DEG C of water-baths, and magnetic agitation is carried out in insulating process, is taken out after heat preservation, cooled to room temperature, then
Supernatant liquor is sopped up with suction pipe, uses alcohol and deionized water to wash first remaining black floccule, then carry out centrifugal treating,
Obtain solid product；
Step 6, the solid product is freeze-dried, freeze-drying temperature is -55 DEG C, and the time is 12h to get negative
Carry the graphene of nickel particles.
Embodiment 5
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 30%, nickel nitrate 70%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 60min systems after stirring 30min
Obtain graphene oxide solution；
Step 3, the nickel nitrate is dissolved in the alcoholic solution that mass concentration is 99.7%, the nickel nitrate and alcohol matter
Amount is than being 1:65 to get to nickel nitrate solution；
Step 4, the nickel nitrate solution is added dropwise in the graphene oxide solution, dropwise addition process is carried out at the same time
Stirring continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, are adjusted to the mixed solution pH value using sodium hydroxide solution
10, mass concentration is then added dropwise as 85% hydrazine hydrate, the mass ratio of hydrazine hydrate and mixed solution is 1:15, it transfers to
3h is kept the temperature in 90 DEG C of water-baths, and magnetic agitation is carried out in insulating process, is taken out after heat preservation, cooled to room temperature, then
Supernatant liquor is sopped up with suction pipe, uses alcohol and deionized water to wash first remaining black floccule, then carry out centrifugal treating,
Obtain solid product；
Step 6, the solid product is freeze-dried, freeze-drying temperature is -55 DEG C, and the time is 14h to get negative
Carry the graphene of nickel particles.
Fig. 2 is load nickel particles graphene powder transmission electron microscope photo.From load nickel particles graphene powder scanning electron microscope
It is in very thin transparence that photo, which can be seen that and restore the graphene of acquisition after water-bath, and nickel particles are evenly distributed on graphene
On.
Claims (6)
1. a kind of preparation method of load nickel particles graphene powder, which is characterized in that concrete operation step is as follows：
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 13-40%, nickel nitrate 60-87%, it is above
The sum of constituent mass percentage is 100%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse after stirring for the first time, oxidation is made
Graphene solution；
Step 3, the nickel nitrate is dissolved in alcoholic solution to get to nickel nitrate solution；
Step 4, the nickel nitrate solution is added dropwise in the graphene oxide solution, dropwise addition process, which is carried out at the same time, to be stirred
It mixes, is again stirring for after completion of dropwise addition, is then ultrasonically treated to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, the mixed solution pH value is adjusted to 9- using sodium hydroxide solution
11, hydrazine hydrate is then added dropwise, transfers in 90 DEG C of water-baths and keeps the temperature 2-4h, magnetic agitation is carried out in insulating process, protects
It is taken out after temperature, then cooled to room temperature sops up supernatant liquor with suction pipe, wine is used first to remaining black floccule
Essence and deionized water washing, then centrifugal treating is carried out, obtain solid product；
Step 6, the solid product is freeze-dried to get the graphene of load nickel particles.
2. a kind of preparation method of load nickel particles graphene powder according to claim 1, which is characterized in that step 3
A concentration of the 99.7% of the alcoholic solution.
3. a kind of preparation method of load nickel particles graphene powder according to claim 1, which is characterized in that step 5
The hydrazine hydrate mass concentration is 85%, and the mass ratio of the hydrazine hydrate and mixed solution is 1:10-28.
4. a kind of preparation method of load nickel particles graphene powder according to claim 1, which is characterized in that step 6
The freeze-drying temperature is -55 DEG C, time 9-14h.
5. a kind of preparation method of load nickel particles graphene powder according to claim 1, which is characterized in that step 2
The nickel nitrate is 1 with alcohol quality ratio:55-80, first time mixing time are 30min, ultrasonic disperse time 60min.
6. a kind of preparation method of load nickel particles graphene powder according to claim 1, which is characterized in that step 4
The time that is again stirring for is 30min, sonication treatment time 60min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113755697A (en) * | 2021-09-03 | 2021-12-07 | 湖南众鑫新材料科技股份有限公司 | Vanadium alloy reduction smelting reducing agent and application thereof |
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| CN113755697A (en) * | 2021-09-03 | 2021-12-07 | 湖南众鑫新材料科技股份有限公司 | Vanadium alloy reduction smelting reducing agent and application thereof |
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