CN103151501B - A kind of preparation method of chromium oxide-graphene nanometer sheet and obtained chromium oxide-graphene nano sheet material thereof - Google Patents
A kind of preparation method of chromium oxide-graphene nanometer sheet and obtained chromium oxide-graphene nano sheet material thereof Download PDFInfo
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- CN103151501B CN103151501B CN201310043761.0A CN201310043761A CN103151501B CN 103151501 B CN103151501 B CN 103151501B CN 201310043761 A CN201310043761 A CN 201310043761A CN 103151501 B CN103151501 B CN 103151501B
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- graphene
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Abstract
The object of this invention is to provide the preparation method of a kind of chromium oxide-graphene nano sheet material, mainly Graphene is template, chromate is chromium source, chromate obtains hydrated chromium oxide-graphene nanometer sheet in Graphene original position by carbonoxide atom under hydrothermal conditions, then carries out chromium oxide-graphene nanometer sheet that thermal bake-out process obtains crystallization.This method production technology is simple, and environmental protection, is easy to industrialization large-scale production.Standby chromium oxide-graphene nanometer sheet the purity of this legal system is high, and specific area is large.Can be used for catalyzing and synthesizing and the fields such as functional material, particularly lithium electric material field has broad application prospects.
Description
Technical field
The present invention relates to inorganic material synthesis field, particularly a kind of preparation method of chromium oxide-graphene nanometer sheet and obtained chromium oxide-graphene nano sheet material thereof.
Background technology
Nano chromium oxide be a kind of developing and have broad prospect of application inorganic functional material, be widely used in the fields such as catalysis, functional paint, photoelectric material and organic synthesis.It is huge at the application potential of lithium electrical domain, and people's theoretical prediction chromium oxide lithium battery peak capacities such as Grugeon, S can reach 1058mAhg
-1(Chem.Mater.
2005,
17, 5041.).For many years, scientist studies the novel oxidized chromium material for lithium electricity always.The people such as Liu have prepared porous oxidation chromium nano particle by hard template method, and its reversible capacity under 0.1C is about 500mAhg
-1(Chem.Commun.
2012,
48, 865).The people such as Jiang have synthesized the chromium oxide-carbon complex of nucleocapsid structure, and its reversible capacity under 0.2C is about 600mAhg
-1.（J.Mater.Chem
. 2010,
20,7565）。Also do not prepare the chromium oxide material of more high reversible capacity so far.
Graphene is a kind of brand-new sequential 2 D material with carbon element in being, has unique physicochemical properties.Its distinctive bigger serface and good electric property thereof determine its great potential in field of lithium.Graphene is made up of monolayer carbon atom close-packed arrays, and lithium not only can be stored in the both sides of graphene sheet layer, can also store in the edge of graphene sheet layer and hole, and its theoretical capacity is more than several times of conventional graphite material.To greatly improve battery lithium storage content with grapheme material as lithium cell cathode material, and then improve energy density.Therefore, there are some graphene nanocomposite materials for the research of lithium electricity, a lot of report as existing in composite materials such as cobalt/cobalt oxide, ferriferous oxide, Mn oxides, but seldom report about chromated oxide-graphene composite material.Only have at present an example be chromium oxide and Graphene physical mixed synthesize report (J.Mater.Chem.,
2012,
22, 16318), because its fault of construction causes lithium electrical property poor.Its capacity is 77mAhg under 0.1C
-1, best sample capacity is 526mAhg
-1, and capacity under higher electric current is low and unstable.
Be template with Graphene and prepare chromium oxide-graphene nanometer sheet composite material by chromate reduction, because chromium oxide grows at Graphene in-situ oxidation carbon atom, and form the nanometer sheet structure of mesh structural porous two dimension, the structure of this uniqueness not only effectively improves conductance and the energy density thereof of chromium oxide composite material, more improves the stability of chromium oxide lithium ion battery.
Summary of the invention
The present invention aims to provide a kind of preparation method and obtained chromium oxide nanometer sheet, the chromium oxide-graphene nano sheet material with the chromium oxide-graphene nano sheet material of good electric chemical property.Cardinal principle is: chromate grows into hydrated chromium oxide at Graphene in-situ oxidation carbon atom and forms the nanometer sheet of two-dimension netted porous, then obtains chromium oxide nanometer sheet material through Overheating Treatment.
Technical solution of the present invention is as follows:
A kind of preparation method of chromium oxide-graphene nanometer sheet, it is characterized in that: take Graphene as template, chromate is chromium source, chromate obtains hydrated chromium oxide-graphene nanometer sheet in Graphene original position by carbonoxide atom under hydrothermal conditions, then carry out chromium oxide-graphene nanometer sheet that thermal bake-out process obtains crystallization, specifically comprise the steps:
(1) be dispersed in 1000-5000 part pure water or water-alcohol solution by portion (being mass ratio) Graphene and 0.2-10 part chromate, ultrasonic or stirring 0.5-24 hour, obtain uniform solution, adjust ph is 1.0-8.0, stirs;
(2) above-mentioned mixed liquor is transferred in hydrothermal reaction kettle, at 110-300 DEG C, react 1-100 hour, by product filtration, washing, drying, obtain chromium oxide hydrate nanometer sheet;
(3) by chromium oxide hydrate nanometer sheet 200-1000 DEG C of calcining 0.1-10 hour under argon gas (nitrogen or other inert gas) protection, final chromium oxide or chromium oxide-graphene nano sheet material can be obtained;
Described chromate is Na
2crO
4, Na
2cr
2o
7, K
2crO
4, K
2cr
2o
7, Li
2crO
4, Li
2cr
2o
7, MgCrO
4, MgCr
2o
7in one, described alcohol is the one in ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutanol;
Described in step (1), the mass ratio of Graphene and chromate is 1:(1-10), in described water-alcohol solution, water and alcohol volume ratio are 100:(1-50);
Described in step (1), the mass ratio of Graphene and chromate is 1:(1-8);
The pure zirconia chromium nanometer sheet obtained by preparation method of described chromium oxide-graphene nanometer sheet or chromium oxide-graphene nano sheet material;
Described chromium oxide-graphene nano sheet material, in porous nano-sheet composite construction, Graphene mass fraction is 0-95%;
The present invention compared with prior art tool has the following advantages:
At present for the inorganic oxide-graphene composite material of lithium electric material, if cobalt oxide, iron oxide etc. are all that coprecipitation is attached directly to graphenic surface or graphene coated to oxide particle surface.Nano particle can not fully mix with the Graphene skeleton with strong conductivity, the present invention is then that chromate is at graphene edge and vacancy in-situ oxidation carbon atom growth chromated oxide, the nanometer sheet structure of mesh structural porous two dimension is formed gradually in Graphene, the structure of this uniqueness not only effectively improves conductance and the energy density thereof of chromium oxide composite material, also improves the stability of chromium oxide lithium ion battery.
Raw material of the present invention only needs Graphene and chromate, and chromium oxide is at Graphene in-situ preparation and obtain the mesh nano sheet composite material of structure uniqueness.Its preparation technology is simple to operation, and environmental protection is easy to suitability for industrialized production.The chromium oxide of preparation be nano-sheet pattern, good dispersion, specific area greatly, and chromium oxide-Graphene to be G-Cr oxide replace network structure, have and show electrochemical properties excellent especially, at high-performance lithium electrical domain, there is broad prospect of application.
accompanying drawing illustrates:
Fig. 1 a crystallization chromium oxide nanometer sheet TEM prepared by the embodiment of the present invention 1 schemes, Fig. 1 b crystallization chromium oxide nanometer sheet HRTEM prepared by the embodiment of the present invention 1 schemes, Fig. 1 c schemes for the present invention executes chromium oxide hydrate-graphene nanometer sheet SEM prepared by example 4, Fig. 1 d schemes for the present invention executes chromium oxide hydrate-graphene nanometer sheet TEM prepared by example 4, Fig. 1 e schemes for the present invention executes crystallization chromium oxide-graphene nanometer sheet TEM prepared by example 4, and Fig. 1 f schemes for the present invention executes crystallization chromium oxide-graphene nanometer sheet HRTEM prepared by example 4.
Fig. 2 a is the embodiment of the present invention 1, the XPS phenogram of chromium oxide prepared by 4 (pitch black line) and chromium oxide-graphene nanometer sheet (light gray), the TGA phenogram of Fig. 2 b chromium oxide (pitch black line) and chromium oxide-graphene nanometer sheet (light gray line) prepared by embodiment Isosorbide-5-Nitrae.The XRD phenogram of Fig. 2 c chromium oxide (black line) prepared by embodiment 1, Fig. 2 d is embodiment Isosorbide-5-Nitrae, the Ramman phenogram of chromium oxide prepared by 6 (pitch black line) and chromium oxide-graphene nanometer sheet (light gray line GCN1,3).
Fig. 3 a is the embodiment of the present invention 1,4, the chemical property figure of chromium oxide prepared by 6 (aterrimus) and chromium oxide-graphene nanometer sheet (light gray line), Fig. 3 b is the embodiment of the present invention 1,4, chromium oxide prepared by 6 (aterrimus) and chromium oxide-graphene nanometer sheet (light grey GCN1,3) constant current charge-discharge curve, cycle performance and the coulombic efficiency figure of Fig. 3 c to be the cycle performance of the made chromium oxide-graphene nanometer sheet of the embodiment of the present invention 6 and coulombic efficiency figure, Fig. 3 d be made chromium oxide-graphene nanometer sheet of the embodiment of the present invention 1.
embodiment:
embodiment 1
By 0.2g Graphene and 1.6gNa
2crO
4(mass ratio 1:8) evenly spreads in deionized water, ultrasonic 2 hours.With acid for adjusting pH to 5.0, stir 30 minutes, transfer in autoclave and seal, react 12 hours at 150 DEG C, filtration washing drying obtains hydrated chromium oxide nanometer sheet product, and then under argon shield, 700 DEG C of calcinings obtain final chromium oxide nanometer sheet for 3 hours.XRD shows the crystalline form that final chromium oxide has had.Electron microscope picture shows that hydrated chromium oxide is micron flakes loose structure, and chromium oxide is the sheet-like particle of 20-30nm and even particle distribution.The test of lithium electrical property shows that its capacity is at 200mAg
-1be down 250mAhg
-1.
embodiment 2
Take step identical in embodiment 1, temperature is different, and react 5 hours at 200 DEG C, filtration washing drying obtains hydrated chromium oxide nanometer sheet product, and then under argon shield, 800 DEG C of calcinings obtain final chromium oxide nanometer sheet for 1 hour.XRD shows the crystalline form that final chromium oxide has had.Electron microscope picture shows that hydrated chromium oxide is micron flakes loose structure, and chromium oxide is the sheet-like particle of 20-30nm.The test of lithium electrical property shows that its capacity is at 200mAg
-1under be about 230mAhg
-1.
embodiment 3
Take step identical in embodiment 1, by 0.2g Graphene and 1.6gNa
2cr
2o
7(mass ratio 1:8) evenly spreads in deionized water.The material structure pattern obtained is identical with embodiment 1, and the test of lithium electrical property shows that its capacity is at 200mAg
-1under be about 255mAhg
-1.
embodiment 4
Take step identical in embodiment 1, unlike by Na
2crO
4addition change 0.6g into, namely Graphene and chromate mass ratio are 1:3.XRD and TEM shows that final product is chromium oxide-graphene composite material.Electron microscope picture shows that hydrated chromium oxide-Graphene is micron flakes loose structure, and final chromium oxide-graphene composite material is the sheet porous structural of tens to hundreds of nanometer.Graphene content is about 38%, and its capacity of chromium oxide-graphene nano sheet material is at 200mAg
-1under up to being 700mAhg
-1.
embodiment 5
Take step identical in embodiment 4, unlike by Na
2crO
4replace with Na
2cr
2o
7addition is constant.The material structure pattern obtained is similar to Example 4, and Graphene content is about 35%, and the test of lithium electrical property shows that its capacity is at 200mAg
-1under be about 685mAhg
-1.
embodiment 6
Take step identical in embodiment 1, unlike Na
2crO
4addition be 0.2g, namely Graphene and chromate mass ratio are 1:1.XRD and TEM shows that final product is chromium oxide-graphene composite material.Electron microscope picture shows that hydrated chromium oxide-Graphene is micron flakes loose structure, and final chromium oxide-graphene composite material is the sheet porous structural of hundred nanometers.Graphene content is about 52%, and its capacity of chromium oxide-graphene nano sheet material is at 200mAg
-1under up to being 990mAhg
-1.
embodiment 7
Take step identical in embodiment 6, unlike by Na
2crO
4replace with K
2crO
4.The material structure pattern obtained is identical with embodiment 6, and the test of lithium electrical property shows that its capacity is at 200mAg
-1under be about 970mAhg
-1.
embodiment 8
Take step identical in embodiment 6, unlike by Na
2crO
4replace with K
2cr
2o
7.The material structure pattern obtained is identical with embodiment 6, and the test of lithium electrical property shows that its reversible capacity is at 200mAg
-1be down 970mAhg
-1.
embodiment 9
Take step identical in embodiment 1, being dispersed in concentration unlike Graphene and chromate is in the ethanol water of 5%, and the material structure obtained is identical with embodiment 1, is of a size of the sheet-like particle of 15-25nm.The test of lithium electrical property shows that its reversible capacity is at 200mAg
-1under be about 255mAhg
-1.
embodiment 10
Take step identical in embodiment 6, being dispersed in concentration unlike Graphene and chromate is in the ethanol water of 20%.The material structure pattern obtained is similar to Example 6, and the pattern of final products is the sheet porous structural of hundred nanometers.The test of lithium electrical property shows that its reversible capacity is at 200mAg
-1under be about 980mAhg
-1.
Graphene content in chromium oxide hydrate-graphene nanometer sheet prepared by the present invention and chromium oxide-graphene nanometer sheet with Graphene and chromate ratio raising and increase.
Claims (9)
1. the preparation method of chromium oxide-graphene nanometer sheet, it is characterized in that: take Graphene as template, chromate is chromium source, chromate obtains hydrated chromium oxide-graphene nanometer sheet in Graphene original position by carbonoxide atom under hydrothermal conditions, then carry out chromium oxide-graphene nanometer sheet that thermal bake-out process obtains crystallization, specifically comprise the steps:
(1) be dispersed in 1000-5000 part pure water or water-alcohol solution by the 1 part of Graphene and 0.2-3 part chromate that are mass ratio, ultrasonic or stirring 0.5-24 hour, obtain uniform solution, adjust ph is 1.0-8.0, stirs;
(2) above-mentioned mixed liquor is transferred in hydrothermal reaction kettle, at 110-300 DEG C, react 1-100 hour, by product filtration, washing, drying, obtain hydrated chromium oxide-Graphene;
(3) hydrated chromium oxide-Graphene 200-1000 DEG C of calcining 0.1-10 hour under argon gas, nitrogen or other inert gas shielding, can obtain chromium oxide-graphene nano sheet material.
2. the preparation method of chromium oxide-graphene nanometer sheet according to claim 1, is characterized in that: described chromate is Na
2crO
4, Na
2cr
2o
7, K
2crO
4, K
2cr
2o
7, Li
2crO
4, Li
2cr
2o
7, MgCrO
4, MgCr
2o
7in one, described alcohol is the one in ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutanol.
3. the preparation method of chromium oxide-graphene nanometer sheet according to claim 1, it is characterized in that: described in step (1), the mass ratio of Graphene and chromate is 1:(0.2-3), in described water-alcohol solution, water and alcohol volume ratio are 100:(1-50).
4. chromium oxide-graphene nano sheet material obtained by the preparation method of chromium oxide-graphene nanometer sheet as claimed in claim 1.
5. the chromium oxide obtained by the preparation method-graphene nano sheet material of chromium oxide-graphene nanometer sheet as claimed in claim 4, it is characterized in that: described chromium oxide-graphene nano sheet material, in porous nano-sheet composite construction, Graphene mass fraction is 0-95%, does not comprise the value of 0.
6. the preparation method of a pure zirconia chromium nanometer sheet, it is characterized in that: take Graphene as template, chromate is chromium source, chromate obtains chromium oxide hydrate nanometer sheet in Graphene original position by carbonoxide atom under hydrothermal conditions, then carry out the pure zirconia chromium nanometer sheet that thermal bake-out process obtains crystallization, specifically comprise the steps:
(1) be dispersed in 1000-5000 part pure water or water-alcohol solution by the 1 part of Graphene and 8-10 part chromate that are mass ratio, ultrasonic or stirring 0.5-24 hour, obtain uniform solution, adjust ph is 1.0-8.0, stirs;
(2) above-mentioned mixed liquor is transferred in hydrothermal reaction kettle, at 110-300 DEG C, react 1-100 hour, by product filtration, washing, drying, obtain chromium oxide hydrate nanometer sheet;
(3) by chromium oxide hydrate nanometer sheet 200-1000 DEG C of calcining 0.1-10 hour under argon gas, nitrogen or other inert gas shielding, final pure zirconia chromium nanometer sheet can be obtained.
7. the preparation method of pure zirconia chromium nanometer sheet according to claim 6, is characterized in that: described chromate is Na
2crO
4, Na
2cr
2o
7, K
2crO
4, K
2cr
2o
7, Li
2crO
4, Li
2cr
2o
7, MgCrO
4, MgCr
2o
7in one, described alcohol is the one in ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutanol.
8. the preparation method of pure zirconia chromium nanometer sheet according to claim 6, it is characterized in that: described in step (1), the mass ratio of Graphene and chromate is 1:(8-10), in described water-alcohol solution, water and alcohol volume ratio are 100:(1-50).
9. the pure zirconia chromium nanometer sheet obtained by preparation method of pure zirconia chromium nanometer sheet as claimed in claim 6.
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| CN108428886A (en) * | 2018-03-26 | 2018-08-21 | 济南大学 | A kind of chrome green load redox graphene lithium cell cathode material and preparation method |
| CN114774043B (en) * | 2022-04-11 | 2023-08-04 | 中国航发北京航空材料研究院 | Corrosion-inhibiting primer for structural adhesive bonding and preparation method thereof |
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