CN106744863A - A kind of preparation method of the grapheme modified zinc oxide composites of PDDA - Google Patents
A kind of preparation method of the grapheme modified zinc oxide composites of PDDA Download PDFInfo
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- CN106744863A CN106744863A CN201710186111.XA CN201710186111A CN106744863A CN 106744863 A CN106744863 A CN 106744863A CN 201710186111 A CN201710186111 A CN 201710186111A CN 106744863 A CN106744863 A CN 106744863A
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- pdda
- zinc oxide
- composite
- grapheme modified
- preparation
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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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- C—CHEMISTRY; METALLURGY
- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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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
-
- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The present invention relates to a kind of preparation method of the grapheme modified zinc oxide composites of PDDA.Specific experiment step, prepares graphite oxide using improved Hummers methods first, by the use of hydrazine hydrate as reducing agent, the Graphene zinc oxide composite that PDDA is modified is obtained by reducing zinc nitrate hexahydrate and graphite oxide in a water bath.In experimentation, using FT IR, the means such as SEM, TEM, XRD are characterized to the composite for preparing.
Description
Technical field
The invention belongs to electrochemistry and its preparation field, be related to a kind of PDDA it is grapheme modified-zinc oxide composite
Preparation method.
Background technology
Used as a kind of individual layer carbon material of two dimension, Graphene possesses many excellent physics and chemical property, as high
Mechanical strength, marvellous electron transfer capacity and outstanding pyroconductivity；Due to its this property, Graphene is very
It is multi-field to be developed.Zero band gap yet with original graphite alkene is embedded into sp2In the C atoms of hydridization, cause Graphene
Certain defect is there is in follow-up practical application, additionally, the surface of Graphene does not have activating functional group, is unfavorable for and other materials
The compound of (such as metallic and organic functions small molecule) is expected, so as to hinder its application study in broader field.In order to
Graphene is set preferably to be utilized in every field, people's trial is dilute to graphite to modify, so as to change the knot of Graphene
Structure, improves its electric conductivity and stability, and then expand its application in fields such as sensor, ultracapacitor and batteries.
Zinc oxide has the advantages that simple stable in properties, preparation process, uniform particle sizes, affinity be strong, good biocompatibility,
And easily modified with biomolecule fixation, it is widely used in the field such as diagnosis and treatment of biology sensor and disease.And pass through to change
Different synthetic methods can obtain different shape, various sizes of zinc oxide particles, it is possessed different properties, use extensively
In the every field of analytical chemistry.
In order to further improve the electric conductivity of Graphene, the application field of zinc oxide particles is widened, we take a kind of letter
Single easy method by zinc oxide particles be compound to the Graphene that PDDA is modified together with obtain a kind of new composite-PDDA
Grapheme modified-zinc oxide composite (PDDA-RGO-ZnO).The composite is in electrochemical analysis, catalyst, super electricity
The fields such as container have a wide range of applications.
The content of the invention
The technical problems to be solved by the invention be to provide it is a kind of simple prepare PDDA it is grapheme modified-zinc oxide is combined
The method of material.The method is prepared for graphite oxide using improved Hummers methods first, then with hydrazine hydrate as reduction
Agent, the Graphene-zinc oxide composite of PDDA modifications is obtained using immersion method.Specific experiment process is with graphite oxide as base
Bottom is made into 1mg mL-1Suspension, add certain PDDA solution to stir 30min after ultrasonic disperse 30min, then according still further to one
Fixed ratio adds the zinc nitrate hexahydrate solution ＆ stir 30min of 50mM, and hydration hydrazine reaction 3h is added after being warming up to 95 DEG C, from
Solid is so centrifugally separating to obtain after cooling, and is dried in 60 DEG C of vacuum drying oven.
The present invention relates to prepare PDDA it is grapheme modified-method of zinc oxide composite, including：
(1) graphite oxide is prepared：In this experiment, graphite oxide is prepared using improved Hummers methods：In the control of ice-water bath
Under system, 2g crystalline flake graphites and 2g sodium nitrate are slowly added into the concentrated sulfuric acid of 45mL to be well mixed, be added slowly with stirring
6g KMnO4, and temperature is risen to isothermal reaction 2h in 35 DEG C of water-baths, solution is then moved into 98 DEG C of preprepared
In water-bath, control temperature adds the secondary water of 90mL below 98 DEG C, and now solution is changed into glassy yellow from blackish green, after stirring 1h
400mL secondary waters are continuously added, equitemperature is slowly added to 25mL H when dropping to less than 60 DEG C2O2(30%), it is followed by stirring for 15min
5% HCl/water solution 400mL is added afterwards, and the sediment washing that will finally obtain is smashed standby with agate mortar after drying.
(2) prepare PDDA it is grapheme modified-zinc oxide composite：The graphite oxide of appropriate above-mentioned synthesis is claimed to be dissolved in
1mg mL are made into ionized water-1Solution, ultrasonic disperse 30min, add 0.5% PDDA solution, stirring 30min after add one
The zinc nitrate hexahydrate solution of quantitative 50mM, adds hydration hydrazine reaction 3h under finally being stirred at 95 DEG C, with secondary after natural cooling
Water washing, drying for standby at 60 DEG C.
Brief description of the drawings
The infrared spectrogram of Fig. 1 graphite oxides
Fig. 2 PDDA are grapheme modified-the TEM figures of zinc oxide composite
Fig. 3 PDDA are grapheme modified-the SEM figures of zinc oxide composite
Fig. 4 graphite oxides and PDDA it is grapheme modified-XRD of zinc oxide composite
Specific embodiment
Embodiment 1：
Prepare the sign of graphite oxide and graphite oxide
Prepare graphite oxide：Graphite oxide drying and grinding is prepared using improved Hummers methods and obtains graphite oxide powder,
Resulting solid powder is carried out into infrared and XRD to it respectively to characterize, the data obtained is as depicted in figs. 1 and 2.
Embodiment 2：
By obtained PDDA it is grapheme modified-zinc oxide composite is dispersed in ultrasound 1h in secondary water, takes 5 μ L dispersion liquids
Drop in it is to be dried on copper mesh after sample topography structure is observed in transmission electron microscope, transmission electron microscope picture is as shown in Figure 3.
Embodiment 3：
By obtained PDDA it is grapheme modified-zinc oxide composite be made after sample respectively in SEM and
Characterized under X-ray diffractometer, obtained such as Fig. 3, shown in Fig. 4.
Claims (4)
1.PDDA is grapheme modified-and zinc oxide (PDDA-RGO-Ag) is a kind of composite, observed under transmission electron microscope
It is the zinc oxide material that fusiformis is loaded in thin two-dimensional material, the composite has preferable electric conductivity and compared with Large ratio surface
Product.
2.PDDA is grapheme modified-preparation of zinc oxide composite：Claim appropriate above-mentioned synthesis graphite oxide be dissolved in from
1mg mL are made into sub- water-1Solution, ultrasonic disperse 30min adds 0.5% PDDA solution, added after stirring 30min certain
The zinc nitrate hexahydrate solution of 50mM is measured, hydration hydrazine reaction 3h is added under finally being stirred at 95 DEG C, secondary water is used after natural cooling
Washing, drying for standby at 60 DEG C.
3. according to claim it is grapheme modified to the PDDA that synthesizes-zinc oxide composite be centrifuged when with two
Secondary water.
4. according to claim it is grapheme modified to the PDDA that synthesizes-zinc oxide composite carries out TEM signs, first will before sample preparation
The uniform 1h of sample ultrasonic disperse in secondary water, then take 5 μ L drop on copper mesh dry after carry out transmission electron microscope sign.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710186111.XA CN106744863A (en) | 2017-03-23 | 2017-03-23 | A kind of preparation method of the grapheme modified zinc oxide composites of PDDA |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710186111.XA CN106744863A (en) | 2017-03-23 | 2017-03-23 | A kind of preparation method of the grapheme modified zinc oxide composites of PDDA |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966453A (en) * | 2010-10-28 | 2011-02-09 | 南昌大学 | Method for preparing graphene-loaded platinum nano catalyst |
| CN102658201A (en) * | 2012-05-09 | 2012-09-12 | 福建师范大学 | Preparation method of direct methanol fuel cell anode composite membrane catalyst |
| CN103094540A (en) * | 2013-01-06 | 2013-05-08 | 中物院成都科学技术发展中心 | Method for compounding graphene and metallic oxide/metallic compound and composite material thereof |
| CN103808779A (en) * | 2014-01-22 | 2014-05-21 | 西北师范大学 | Method for detecting p-nitrophenol by using PDDA (Poly Diallyldimethylammonium) functionalized graphene modified glassy carbon electrode |
| CN104701490A (en) * | 2015-04-02 | 2015-06-10 | 北京师范大学 | Preparing method and application of sandwich-structure graphene-based carbon cladding metal oxide |
-
2017
- 2017-03-23 CN CN201710186111.XA patent/CN106744863A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966453A (en) * | 2010-10-28 | 2011-02-09 | 南昌大学 | Method for preparing graphene-loaded platinum nano catalyst |
| CN102658201A (en) * | 2012-05-09 | 2012-09-12 | 福建师范大学 | Preparation method of direct methanol fuel cell anode composite membrane catalyst |
| CN103094540A (en) * | 2013-01-06 | 2013-05-08 | 中物院成都科学技术发展中心 | Method for compounding graphene and metallic oxide/metallic compound and composite material thereof |
| CN103808779A (en) * | 2014-01-22 | 2014-05-21 | 西北师范大学 | Method for detecting p-nitrophenol by using PDDA (Poly Diallyldimethylammonium) functionalized graphene modified glassy carbon electrode |
| CN104701490A (en) * | 2015-04-02 | 2015-06-10 | 北京师范大学 | Preparing method and application of sandwich-structure graphene-based carbon cladding metal oxide |
Non-Patent Citations (3)
| Title |
|---|
| HUICHAO LI ET AL: "Highly sensitive determination of esculetin on TiO2-NPs-coated poly(diallyldimethylammonium chloride)-functionalized graphene modified electrode", 《TALANTA》 * |
| PING LI ET AL: "Enhancement of the interfacial interaction between poly(vinyl chloride) and zinc oxide modified reduced graphene oxide", 《RSC ADV.》 * |
| SITI NUR AKMAR MOHD YAZID ET AL: "A Review of Glucose Biosensors Based on Graphene/Metal Oxide Nanomaterials", 《ANALYTICAL LETTERS》 * |
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