CN107188164A - A kind of preparation method of rGO/ZnO tiny balloons - Google Patents
A kind of preparation method of rGO/ZnO tiny balloons Download PDFInfo
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- CN107188164A CN107188164A CN201710559365.1A CN201710559365A CN107188164A CN 107188164 A CN107188164 A CN 107188164A CN 201710559365 A CN201710559365 A CN 201710559365A CN 107188164 A CN107188164 A CN 107188164A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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Abstract
The invention provides the preparation method that a kind of GO parcels are mutually overlapped the zinc oxide for growing into tiny balloon by single hexagonal flake zinc oxide.The preparation method is specifically included：With graphene oxide GO, zinc acetate dihydrate is raw material, monoethanolamine（MEA）For surfactant, aminopropyl triethoxysilane (APTES) is coupling agent, through hydro-thermal method, calcination processing, obtains rGO parcels and the zinc oxide for growing into tiny balloon is mutually overlapped by single hexagonal flake zinc oxide；The composite of rGO/ZnO tiny balloon patterns is made.This method simple production process, by the effect of APTES coupling agents be made it is a kind of hexagonal flake wrapped up by rGO mutually overlapped grow into the zinc oxide composite of tiny balloon.
Description
Technical field
The present invention relates to a kind of preparation method of rGO/ZnO tiny balloons, belong to advanced nano material fabricating technology
Field.
Background technology
The metal oxide nano-material gas sensitization superior due to possessing, optical characteristics, it is with low cost the advantages of
Obtain extensively and in-depth study, its application has come into the multiple fields of human being's production life, promotes a large amount of industries
Development.In types of functionality metal oxide nano-material, good stability that zinc oxide has due to it, high electronics are moved
The advantages of shifting rate and abundant nanotopography, have been widely used in photoelectric device, solar cell, feds with
And the field such as chemical sensor.At present, the preparation research method for forming zinc oxide nanowire is varied.And by six square pieces
The research of the Zinc oxide hollow microsphere of shape composition is also very fresh few.Therefore, the preparation of the zinc oxide of this tiny balloon nanostructured
Technology is also to be developed.On the other hand, for the sensor using zinc oxide as sensitive material, contacted with each other between its hexagonal flake
What is constituted is electrically connected the conduction that ensure that chemically sensitive resistor signal.With the zinc oxide hollow overlapped by laminated structure
Contacting with each other between micro-sphere structure is more close, with bigger specific surface area and more excellent sensitive property.
Graphene possesses huge ratio table as a kind of carbon material with bi-dimensional cellular shape structure of monoatomic layer thickness
Area and superior electron mobility and property stabilization, are widely used in the fields such as electronics, sensor, medicine and catalysis, are
The wider research of nano composite material provides new thinking and direction.Various countries expert is become since being found from graphene
The focus of scholar's research, while being also considered as improving the new material in the fields such as the son that conducts electricity, sensor, medicine and catalysis.I
State is graphite resource most abundant country, is also big producer, but the deep processing of its high-tech is probed into still is in the junior stage.
The research of graphene composite material is concentrated mainly on last decade, and also many problems need research.Therefore, rGO parcels are explored
The preparation method of zinc oxide nanometer composite material be one still need to solution the problem of.
The content of the invention
It is an object of the present invention to overcome the deficiencies in the prior art to be aoxidized there is provided a kind of rGO parcels by single hexagonal flake
Zinc mutually overlaps the preparation method for the zinc oxide nanometer composite material for growing into tiny balloon.With simple production process, yield
The characteristics of height, non-environmental-pollution.The nano composite material of gained rGO/ZnO hollow microsphere structures available for improvement conduct electricity son, pass
The new material in the fields such as sensor, medicine and catalysis.Realizing the object of the invention technical scheme is：A kind of rGO/ZnO tiny balloons
Preparation method, it is characterised in that：With graphene oxide GO, zinc acetate dihydrate is raw material, monoethanolamine（MEA）For surface-active
Agent, aminopropyl triethoxysilane (APTES) is coupling agent, through hydro-thermal method, calcination processing, obtains rGO parcels by single six side
Sheet zinc oxide mutually overlaps the zinc oxide for growing into tiny balloon；The composite of rGO/ZnO tiny balloon patterns is made.This
Method simple production process, gained nano composite material can be used for improving the new of the fields such as the son that conducts electricity, sensor, medicine and catalysis
Section bar material.Specific synthesis step is as follows：
（1）Weigh a certain amount of two water zinc acetate to be dissolved in 10-100ml absolute ethyl alcohol, after stirring certain time, add one
Quantitative monoethanolamine（MEA）After be stirred for 1h, resulting solution is placed in reactor at 150-180 DEG C after stirring
24-38h is reacted, gained solid product is collected by centrifugation, and is washed for several times with deionized water and absolute ethyl alcohol, is placed in drying box,
60 DEG C of dryings 24 hours, then in groom's stove, carry out high-temperature calcination, calcining heat is 400-600 DEG C, and soaking time is 2-5
It can obtain hexagonal flake after hour and mutually overlap the Zinc oxide hollow microsphere of growth, and control the two water acetic acid zinc concentrations to be：
0.05-0.2mol/l, MEA volume are 20-50ml, and control two water zinc acetates：MEA mass ratio is 1：0.01-0.1；
（2）Weigh certain mass step（1）Obtained ZnO, ultrasound is dispersed in 10-100ml ethanol solutions, is added
A certain amount of aminopropyl triethoxysilane（APTES）, 4-6h is stirred at 60-80 DEG C, after cooling by solid ethanol
Washing for several times, is dried overnight, the concentration for controlling ZnO is in 60 DEG C of drying boxes：0.01-0.1mol/l, APTES volume is：
0.5-1ml, and control ZnO：APTES mol ratio is 1：0.001-0.01；
（3）Graphene oxide GO prepared by a certain amount of improvement Hummers methods is weighed, by its ultrasonic disperse in 10-100 mL water
In, GO colloidal solution is obtained, wherein GO concentration is 0.1-1 mg/mL, with step（2）Gained sample is dispersed in GO colloids together
In solution, then ultrasonic disperse 30min.Resulting solution is transferred in reactor in 120-160 DEG C of constant temperature 14-20h, reacted
Washed after complete with deionized water and absolute ethyl alcohol, 24h is dried at -50 DEG C with freeze drier, rGO parcel hexagonal flakes are made
The ZnO microsphere of mutually overlap joint growth obtains composite.
Brief description of the drawings
Fig. 1 schemes for the FESEM of rGO/ZnO nano composite materials.
Fig. 2 schemes for the FESEM of rGO/ZnO nano composite materials.
Fig. 3 schemes for the FESEM of rGO/ZnO nano composite materials.
Fig. 4 is the XRD spectrum of rGO/ZnO nano composite materials.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementations
Example.
Embodiment 1
（1）The two water zinc acetates for weighing 0.1mol/l are dissolved in 40ml absolute ethyl alcohol, after stirring certain time, add 30ml
Monoethanolamine（MEA）After be stirred for 1h, resulting solution is placed in reactor after stirring and reacts 24h at 160 DEG C,
Gained solid product is collected by centrifugation, and is washed for several times with deionized water and absolute ethyl alcohol, is placed in drying box, 60 DEG C of dryings 24 are small
When, then in groom's stove, high-temperature calcination is carried out, calcining heat is 500 DEG C, soaking time is i.e. available six sides after 2 hours
Sheet mutually overlaps the Zinc oxide hollow microsphere of growth, and two water zinc acetates of control：MEA mass ratio is 1：0.034；
（2）Weigh 55mg quality steps（1）Obtained ZnO, ultrasound is dispersed in 55ml ethanol solutions, is added
0.55ml aminopropyl triethoxysilane（APTES）, 4h is stirred at 60 DEG C, after cooling by solid with ethanol wash number
It is secondary, it is dried overnight in 60 DEG C of drying boxes, controls ZnO：APTES mol ratio is 1：0.0036；
（3）Graphene oxide GO prepared by 10mg improvement Hummers methods is weighed, by its ultrasonic disperse in 80mL water, is obtained
The concentration of GO colloidal solution, wherein GO is 0.125 mg/mL, with step（2）Gained sample is dispersed in GO colloidal solution together,
Then ultrasonic disperse 30min.Resulting solution is transferred in reactor in 120 DEG C of constant temperature 14h, deionized water is used after reaction completely
With absolute ethyl alcohol washing, 24h is dried at -50 DEG C with freeze drier, rGO parcel hexagonal flakes are made and mutually overlap growth
ZnO microsphere obtains composite.
Embodiment 2
（1）The two water zinc acetates for weighing 0.15mol/l are dissolved in 50ml absolute ethyl alcohol, after stirring certain time, are added
40ml monoethanolamine（MEA）After be stirred for 1h, after stirring by resulting solution be placed in reactor at 165 DEG C react
26h, is collected by centrifugation gained solid product, and is washed for several times with deionized water and absolute ethyl alcohol, is placed in drying box, 60 DEG C of dryings
24 hours, then in groom's stove, high-temperature calcination is carried out, calcining heat is 600 DEG C, soaking time is i.e. available after 2 hours
Hexagonal flake mutually overlaps the Zinc oxide hollow microsphere of growth, and two water zinc acetates of control：MEA mass ratio is 1：0.036；
（2）Weigh 55mg quality steps（1）Obtained ZnO, ultrasound is dispersed in 55ml ethanol solutions, is added
0.55ml aminopropyl triethoxysilane（APTES）, 4h is stirred at 60 DEG C, after cooling by solid with ethanol wash number
It is secondary, it is dried overnight in 60 DEG C of drying boxes, controls ZnO：APTES mol ratio is 1：0.0037；
（3）Graphene oxide GO prepared by 15mg improvement Hummers methods is weighed, by its ultrasonic disperse in 85mL water, is obtained
The concentration of GO colloidal solution, wherein GO is 0.175 mg/mL, with step（2）Gained sample is dispersed in GO colloidal solution together,
Then ultrasonic disperse 30min.Resulting solution is transferred in reactor in 130 DEG C of constant temperature 14h, deionized water is used after reaction completely
With absolute ethyl alcohol washing, 24h is dried at -50 DEG C with freeze drier, rGO parcel hexagonal flakes are made and mutually overlap growth
ZnO microsphere obtains composite.
Embodiment 3
（1）The two water zinc acetates for weighing 0.125mol/l are dissolved in 52ml absolute ethyl alcohol, after stirring certain time, are added
35ml monoethanolamine（MEA）After be stirred for 1h, after stirring by resulting solution be placed in reactor at 175 DEG C react
28h, is collected by centrifugation gained solid product, and is washed for several times with deionized water and absolute ethyl alcohol, is placed in drying box, 60 DEG C of dryings
24 hours, then in groom's stove, high-temperature calcination is carried out, calcining heat is 600 DEG C, soaking time is i.e. available after 2 hours
Hexagonal flake mutually overlaps the Zinc oxide hollow microsphere of growth, and two water zinc acetates of control：MEA mass ratio is 1：0.025；
（2）Weigh 60mg quality steps（1）Obtained ZnO, ultrasound is dispersed in 60ml ethanol solutions, is added
0.65ml aminopropyl triethoxysilane（APTES）, 4h is stirred at 60 DEG C, after cooling by solid with ethanol wash number
It is secondary, it is dried overnight in 60 DEG C of drying boxes, controls ZnO：APTES mol ratio is 1：0.0039；
（3）Graphene oxide GO prepared by 8mg improvement Hummers methods is weighed, by its ultrasonic disperse in 80mL water, GO is obtained
The concentration of colloidal solution, wherein GO is 0.1 mg/mL, with step（2）Gained sample is dispersed in GO colloidal solution together, then
Ultrasonic disperse 30min.Resulting solution is transferred in reactor in 120 DEG C of constant temperature 14h, deionized water and nothing are used after reaction completely
Water-ethanol is washed, and 24h is dried at -50 DEG C with freeze drier, and the oxidation that rGO parcel hexagonal flakes mutually overlap growth is made
Zinc microballoon obtains composite.
Claims (1)
1. a kind of preparation method of rGO/ZnO tiny balloons：Specific synthesis step is as follows：
（1）Weigh a certain amount of two water zinc acetate to be dissolved in 10-100ml absolute ethyl alcohol, after stirring certain time, add one
Quantitative monoethanolamine（MEA）After be stirred for 1h, resulting solution is placed in reactor at 150-180 DEG C after stirring
24-38h is reacted, gained solid product is collected by centrifugation, and is washed for several times with deionized water and absolute ethyl alcohol, is placed in drying box,
60 DEG C of dryings 24 hours, then in groom's stove, carry out high-temperature calcination, calcining heat is 400-600 DEG C, and soaking time is 2-5
It can obtain hexagonal flake after hour and mutually overlap the Zinc oxide hollow microsphere of growth, and control the two water acetic acid zinc concentrations to be：
0.01-0.1mol/l, MEA volume are 20-50ml, and control two water zinc acetates：MEA mass ratio is 1：0.01-0.1；
（2）Weigh certain mass step（1）Obtained ZnO, ultrasound is dispersed in 10-100ml ethanol solutions, is added
A certain amount of aminopropyl triethoxysilane（APTES）, 4-6h is stirred at 60-80 DEG C, after cooling by solid ethanol
Washing for several times, is dried overnight, the concentration for controlling ZnO is in 60 DEG C of drying boxes：0.01-0.1mol/l, APTES volume is：
0.5-1ml, and control ZnO：APTES mol ratio is 1：0.001-0.01；
（3）Graphene oxide GO prepared by a certain amount of improvement Hummers methods is weighed, by its ultrasonic disperse in 10-100 mL water
In, GO colloidal solution is obtained, wherein GO concentration is 0.1-1 mg/mL, with step（4）Gained sample is dispersed in GO colloids together
In solution, then ultrasonic disperse 30min；
（4）Resulting solution is transferred in reactor in 120-160 DEG C of constant temperature 14-20h, deionized water and nothing are used after reaction completely
Water-ethanol is washed, and 24h is dried at -50 DEG C with freeze drier, and the oxidation that rGO parcel hexagonal flakes mutually overlap growth is made
Zinc microballoon obtains composite.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109860730A (en) * | 2018-12-25 | 2019-06-07 | 华南师范大学 | A kind of preparation method of lead-acid battery cathode composite additives |
| CN113372131A (en) * | 2021-04-26 | 2021-09-10 | 西安理工大学 | Micro-nano pore channel structure tetragonal phase BaTiO3Preparation method of/HA hollow microspheres |
| CN114784242A (en) * | 2022-04-13 | 2022-07-22 | 内蒙古欣源石墨烯科技股份有限公司 | Preparation method of nano-carbon coated lithium battery negative electrode material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109860730A (en) * | 2018-12-25 | 2019-06-07 | 华南师范大学 | A kind of preparation method of lead-acid battery cathode composite additives |
| CN109860730B (en) * | 2018-12-25 | 2021-09-21 | 华南师范大学 | Preparation method of lead-acid battery negative electrode composite material additive |
| CN113372131A (en) * | 2021-04-26 | 2021-09-10 | 西安理工大学 | Micro-nano pore channel structure tetragonal phase BaTiO3Preparation method of/HA hollow microspheres |
| CN114784242A (en) * | 2022-04-13 | 2022-07-22 | 内蒙古欣源石墨烯科技股份有限公司 | Preparation method of nano-carbon coated lithium battery negative electrode material |
| CN114784242B (en) * | 2022-04-13 | 2024-06-07 | 内蒙古欣源石墨烯科技股份有限公司 | Preparation method of nano-carbon coated lithium battery anode material |
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