CN107703196A - A kind of application of the preparation method of graphene filter paper and its flexible electrode as self-supporting - Google Patents
A kind of application of the preparation method of graphene filter paper and its flexible electrode as self-supporting Download PDFInfo
- Publication number
- CN107703196A CN107703196A CN201710863994.3A CN201710863994A CN107703196A CN 107703196 A CN107703196 A CN 107703196A CN 201710863994 A CN201710863994 A CN 201710863994A CN 107703196 A CN107703196 A CN 107703196A
- Authority
- CN
- China
- Prior art keywords
- filter paper
- graphene
- electrode
- preparation
- graphene oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
Abstract
The application of flexible electrode the invention discloses a kind of preparation method of graphene filter paper and its as self-supporting, the present invention are by the use of filter paper as substrate, pass through the integrated artistic design to its crucial preparation technology, the reaction condition of each step（Such as reactant concentration, reaction temperature, reaction time）Etc. being improved, flexible electrode is prepared by modifying graphene sheet layer in its surface, can also preferably continue to load Pd nano particle on graphene modified filter paper, palladium granular graphite alkene filter paper is made；The graphene filter paper has good specific surface area, and this can be as the flexible electrode of self-supporting；Obtained flexible electrical extremely size can easily be regulated and controled according to demand, can be used as self-supporting application of electrode in hydrogen peroxide sensor（Such as concentration sensor）, it is highly suitable for detecting hydrogen peroxide（The concentration of such as hydrogen peroxide）, there is the advantages of high sensitivity.
Description
Technical field
The invention belongs to material electrochemical field, more particularly, to a kind of preparation method and its work of graphene-filter paper
For the application of the flexible electrode of self-supporting.
Background technology
Electrochemical sensor has the advantages such as analysis rapid sensitive, instrumentation simplicity and low cost.And with nanometer
Material and electronic technology are developed rapidly, and material preparation technology is just gradually dissolved into electrochemical analysis, has promoted electrochemistry biography
Sense technology obtains further breakthrough.In the last few years, the research in terms of electrochemical sensor emerged in an endless stream, especially will be new
Functional material is combined with traditional electrochemical sensor, builds the core parts of sensor --- new functional electrode, and open
Send the high-performance electric chemistry sensor of a new generation.Novel electrochemical sensor based on functional electrode material structure shows sound
Should faster, the excellent performance such as sensitivity is higher and stability is more preferable.
Graphene has mechanical strength and pliability, the huge theoretical specific surface area and excellent conductivity of superelevation,
And significant chemical property, such as larger potential window, relatively low charge transfer resistance and quick electron transport rate
Deng.Based on its above-mentioned special physical property and excellent chemical property, grapheme material obtains in electrochemical sensor field
To being widely applied.Pi-pi accumulation and van der Waals interaction between the carbon atomic layer of graphene sheet layer so that graphene possesses good
Good film forming, can be prepared into graphene film/paper.Two-dimensional graphene film/paper-like functional material typically have self-supporting,
The advantage of flexible, low-density and high conductivity, it is multi-field in flexible energy storage device, multifunctional membrane material and portable detector etc.
Show huge potential application.Therefore, graphite film/paper electrode material of high-quality is prepared to promoting electrochemical sensor
Develop most important.Hydrogen peroxide is a kind of important small molecule present in biosystem, and weight is played in many physiology courses
Act on.Hydrogen peroxide and the physiological status of plant or animal are closely bound up, therefore the detection of content of hydrogen peroxide is to us
The contact of solution organism and environment is significant.
In addition, with the development of material electrochemical technology, using interfacial effect of nano material etc., by graphene nano material
Material introduces flexible electrode surface, the characteristic such as one side combination electrode the flexibility that can inherit substrate in itself, low-density, on the other hand
Also possess the advantages such as the high conductivity of graphene, big specific surface area, it is peculiar so as to be produced to the performance of electrochemical sensor
Facilitation.Flexible electrode is from self-supporting substrate and is loaded with having special construction and the grapheme material of function, this
A little design features impart the advantages that its specific surface area is big, density is low, raw material is cheap so that it is in electrochemical sensor field
Using very it is simple effectively, be particularly suited for the detection of hydrogen peroxide.
The content of the invention
Above current situation for prior art improves trend, it is an object of the invention to provide a kind of graphene-
The preparation method and applications of filter paper, the graphene-filter paper being prepared（Including palladium particle-graphene-filter paper）With good
Specific surface area, and the graphene-filter paper can be as the flexible micro-electrode of self-supporting, for detecting peroxidating in physiological systems
Hydrogen（The concentration of such as hydrogen peroxide）, there is higher high sensitivity.
To achieve the above object, according to one aspect of the present invention, there is provided a kind of preparation method of graphene-filter paper,
Comprise the following steps：
（1）Graphene oxide water solution is prepared, filter paper uses use for laboratory qualitative filter paper, wherein：
The concentration of the graphene oxide water solution is the mg/mL of 2 mg/mL~10；
The cm of a diameter of 4 cm of the filter paper~16；
（2）By the step（1）In filter paper be immersed in step（1）It is middle to prepare in the obtained graphene oxide water solution,
Then, lifting is out dried in an oven, is repeated for several times, graphene oxide-filter paper is prepared；
（3）By the step（2）In obtained graphene oxide-filter paper carry out reduction treatment with hydrazine hydrate steam, that is, obtain stone
Black alkene-filter paper.
As present invention further optimization, the preparation method of above-mentioned graphene-filter paper is further comprising the steps of：
（4）With the step（3）In the obtained graphene-filter paper be working electrode, be placed in dissolved with potassium chloropalladite
In precursor solution, graphene-filter paper that electro-deposition obtains loading Pd nano particle is carried out.
As present invention further optimization, the step（2）Filter paper is totally submerged graphite oxide during middle filter paper immersion
In aqueous solution；The soak time is the s of 10 s~30.
As present invention further optimization, the step（2）The temperature of middle drying is 20 DEG C~45 DEG C.
As present invention further optimization, the step（2）In soak repeatedly lifting number be 5~20 times.
As present invention further optimization, the step（3）The mass concentration of middle hydrazine hydrate is 40%-70%, is preferably
50%；The vapor (steam) temperature is 120 DEG C~180 DEG C；The reduction reaction time is the h of 6 h~24.
As present invention further optimization, the step（4）In electro-deposition be using three-electrode system in constant potential
Under conditions of carry out, sedimentation potential is the V of -0.1 V~-0.5, and sedimentation time is the s of 30 s~300.
As present invention further optimization, the step（4）In precursor solution be containing 5 mM H2PtCl6With 0.2
M H2SO4Mixed liquor.
As the most preferably scheme of the present invention, the preparation method of graphene-filter paper comprises the following steps：
（1）Compound concentration is 8 mg/mL graphene oxide water solution, and filter paper uses the qualitative filter paper that laboratory is commonly used, diameter
For 10 cm；
（2）Modify graphene oxide：Filter paper is immersed in step（1）The graphene oxide for 8 mg/mL that middle preparation obtains is water-soluble
Liquid, soak time are 30 s, and then, lifting is out dried in 25 DEG C of baking oven, is repeated 12 times, that is, is prepared oxidation stone
Black alkene-filter paper；
（3）Redox graphene：By step（2）In obtained graphene oxide-filter paper it is dense with quality under the conditions of 160 DEG C
The hydrazine hydrate steam of degree 50% carries out the h of reduction treatment 12, obtains graphene-filter paper；
（4）Electro-deposition active component Pd nano particles：Using graphene-filter paper as working electrode, gauze platinum electrode is as auxiliary electricity
Pole, for saturated calomel electrode as reference electrode, be placed in 50 ml contains 5 mM H2PtCl6With 0.2 M H2SO4Mixed liquor in,
The s of electro-deposition 200 under conditions of the V of constant potential -0.15, Pd- graphenes-filter paper is made.
It is another aspect of this invention to provide that the application process for graphene-filter paper that above-mentioned preparation method obtains is provided, i.e.,
Application as the flexible electrode of self-supporting.
As present invention further optimization, the graphene-filter paper as self-supporting flexible electrode in hydrogen peroxide
Application in content detection.
As present invention further optimization, the graphene-filter paper as self-supporting flexible electrode in hydrogen peroxide
Application in electrochemical sensor
The present invention is by the use of filter paper as substrate, passes through the integrated artistic design to its crucial preparation technology, the reaction bar of each step
Part（Such as reactant concentration, reaction temperature, reaction time）Etc. being improved, by modified in its surface graphene sheet layer come
Flexible electrode is prepared, can also preferably continue to load Pd nano particle on graphene modified filter paper, palladium particle-graphite is made
Alkene-filter paper；Graphene-the filter paper has good specific surface area, and this can be as the flexible electrode of self-supporting；It is obtained soft
Property electrode its size can easily be regulated and controled according to demand, self-supporting application of electrode can be used as to be sensed in hydrogen peroxide
Device（Such as concentration sensor）, it is highly suitable for detecting hydrogen peroxide（The concentration of such as hydrogen peroxide）, there is the excellent of high sensitivity
Point.
Condition of the invention by reacting every step（The concentration of such as reactant, the parameter of reaction temperature, reaction time）
It is controlled, obtained product can be greatly improved（That is graphene-filter paper）Specific surface area, especially make when using these products
For combination electrode in use, because these combination electrodes have larger specific surface area and high conductivity, can be carried for catalytic reaction
Good catalytic effect and excellent selectivity are shown for more avtive spots, during as hydrogen peroxide sensor.
The method for modifying upper graphene sheet layer in the present invention by the use of filter paper as substrate, the raw material of reaction is easy to get, and is inhaling
Due to the aperture adsorption rate that filter paper is big during attached, can modify substantial amounts of graphene sheet layer enhancing paper electrode specific surface area and
Electric conductivity, and it is that spontaneous progress, energy consumption are low to adsorb modification.In addition, the graphene sheet layer of absorption is to follow-up active palladium
The load of particle also has the function that to promote, and can further improve the specific surface area parameter of product.
To sum up, compared with prior art, its is easy to operate for preparation method of the present invention, and synthesis cost is low（Filter paper substrate raw material
It is easy to get）, and the microscopic appearance of product（Such as nanotopography）It is good controllable；Prepared self-supporting flexible electrode has big ratio table
Area, excellent performance is showed as hydrogen peroxide electrochemical sensor material.
Brief description of the drawings
In Fig. 1, Fig. 1 a and Fig. 1 b are the scanning electron microscope (SEM) photographs of filter paper, and Fig. 1 c, Fig. 1 d are the steps of example 3（3）Obtained graphene-
The scanning electron microscope (SEM) photograph of filter paper；
In Fig. 2, Fig. 2 a, Fig. 2 b are the steps of embodiment 3（4）The scanning electron microscope (SEM) photograph of obtained Pd- graphenes-filter paper；
In Fig. 3, Fig. 3 a, Fig. 3 b and Fig. 3 c are embodiment 1, embodiment 3 and the step of embodiment 5（4）Obtained Pd- graphenes-filter
The scanning electron microscope (SEM) photograph of paper；
Fig. 4 be embodiment 1-5 prepare Pd- graphenes-filter paper electrode as hydrogen peroxide sensor 3 mM hydrogen peroxide
Physiological systems be disodium hydrogen phosphate/sodium dihydrogen phosphate（PBS）Buffer solution（PH about 7.2）In cyclic voltammetric（CV）Figure；
Fig. 5 be embodiment 3 prepare Pd- graphenes-filter paper electrode as hydrogen peroxide sensor in the peroxide containing various concentrations
The physiological systems for changing hydrogen are disodium hydrogen phosphate/sodium dihydrogen phosphate（PBS）Buffer solution（PH about 7.2）In cyclic voltammetric（CV）Figure；
Fig. 6 be Pd- graphenes-filter paper application of electrode prepared by embodiment 3 in hydrogen peroxide sensor, apply current potential in -0.18V
The lower PBS to 20ml（PH about 7.2）It is continuously added to the timing ampere response curve of various concentrations hydrogen peroxide
（Amperometric i-t Curve）With corresponding linear fit curve map；
Fig. 7 is the pictorial diagram of 3 graphenes of embodiment-filter paper.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, not
For limiting the present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below that
Conflict can is not formed between this to be mutually combined.
Embodiment 1
A kind of preparation method of Pd- graphenes-filter paper, comprises the following steps：
（1）Compound concentration is 2 mg/mL graphene oxide water solution, and filter paper uses the qualitative filter paper that laboratory is commonly used, diameter
For 6 cm.
（2）Modify graphene oxide：Filter paper is immersed in step（1）The middle graphene oxide for preparing 2 obtained mg/mL
The aqueous solution, soak time are 10 s, and then, lifting is out dried in 30 DEG C of baking oven, is repeated 8 times, that is, is prepared oxidation
Graphene-filter paper.
（3）Redox graphene：By step（2）In obtained graphene oxide-filter paper graphene oxide-filter paper exist
The h of reduction treatment 6 is carried out with the hydrazine hydrate steam that mass concentration is 50% under the conditions of 120 DEG C, prepares graphene-filter paper.
（4）Electro-deposition active component Pd nano particles：Using graphene-filter paper as working electrode, gauze platinum electrode is as auxiliary
Electrode is helped, for saturated calomel electrode as reference electrode, be placed in 50 ml contains 5 mM H2PtCl6With 0.2 M H2SO4Mixed liquor
In, the s of electro-deposition 100 under conditions of the V of constant potential -0.1, Pd- graphenes-filter paper electrode is made.
Electrochemical sensing application：By Pd- graphenes-filter paper electrode of preparation, as the flexible electrode of self-supporting, it is applied to
In hydrogen peroxide electrochemical sensor.
Embodiment 2
A kind of preparation method of Pd- graphenes-filter paper, comprises the following steps：
（1）Compound concentration is 4 mg/mL graphene oxide water solution, and filter paper uses the qualitative filter paper that laboratory is commonly used, diameter
For 8 cm.
（2）Modify graphene oxide：Filter paper is immersed in step（1）The middle graphene oxide for preparing 4 obtained mg/mL
The aqueous solution, soak time are 20 s, and then, lifting is out dried in 20 DEG C of baking oven, is repeated 6 times, that is, is prepared oxidation
Graphene-filter paper.
（3）Redox graphene：By step（2）In obtained graphene oxide-filter paper graphene oxide-filter paper exist
The h of reduction treatment 8 is carried out with the hydrazine hydrate steam that mass concentration is 50% under the conditions of 140 DEG C, prepares graphene-filter paper.
（4）Electro-deposition active component Pd nano particles：Using graphene-filter paper as working electrode, gauze platinum electrode is as auxiliary
Electrode is helped, for saturated calomel electrode as reference electrode, be placed in 50 ml contains 5 mM H2PtCl6With 0.2 M H2SO4Mixed liquor
In, the s of electro-deposition 50 under conditions of the V of constant potential -0.1, Pd- graphenes-filter paper electrode is made.
Electrochemical sensing application：By Pd- graphenes-filter paper electrode of preparation, as the flexible electrode of self-supporting, it is applied to
In hydrogen peroxide electrochemical sensor.
Embodiment 3
A kind of preparation method of Pd- graphenes-filter paper, comprises the following steps：
（1）Compound concentration is 8 mg/mL graphene oxide water solution, and filter paper uses the qualitative filter paper that laboratory is commonly used, diameter
For 10 cm.
（2）Modify graphene oxide：Filter paper is immersed in step（1）The middle graphene oxide for preparing 8 obtained mg/mL
The aqueous solution, soak time are 30 s, and then, lifting is out dried in 25 DEG C of baking oven, is repeated 12 times, that is, is prepared oxygen
Graphite alkene-filter paper.
（3）Redox graphene：By step（2）In obtained graphene oxide-filter paper graphene oxide-filter paper exist
The h of reduction treatment 12 is carried out with the hydrazine hydrate steam that mass concentration is 50% under the conditions of 160 DEG C, prepares graphene-filter paper.
（4）Electro-deposition active component Pd nano particles：Using graphene-filter paper as working electrode, gauze platinum electrode is as auxiliary
Electrode is helped, for saturated calomel electrode as reference electrode, be placed in 50 ml contains 5 mM H2PtCl6With 0.2 M H2SO4Mixed liquor
In, the s of electro-deposition 200 under conditions of the V of constant potential -0.15, Pd- graphenes-filter paper electrode is made.
Electrochemical sensing application：By Pd- graphenes-filter paper electrode of preparation, as the flexible electrode of self-supporting, it is applied to
In hydrogen peroxide electrochemical sensor.
Embodiment 4
A kind of preparation method of Pd- graphenes-filter paper, comprises the following steps：
（1）Compound concentration is 10 mg/mL graphene oxide water solution, and filter paper uses the qualitative filter paper that laboratory is commonly used, diameter
For 16 cm.
（2）Modify graphene oxide：Filter paper is immersed in step（1）The middle graphene oxide for preparing 10 obtained mg/mL
The aqueous solution, soak time are 30 s, and then, lifting is out dried in 45 DEG C of baking oven, is repeated 16 times, that is, is prepared oxygen
Graphite alkene-filter paper.
（3）Redox graphene：By step（2）In obtained graphene oxide-filter paper graphene oxide-filter paper exist
The h of reduction treatment 24 is carried out with the hydrazine hydrate steam that mass concentration is 50% under the conditions of 180 DEG C, prepares graphene-filter paper.
（4）Electro-deposition active component Pd nano particles：Using graphene-filter paper as working electrode, gauze platinum electrode is as auxiliary
Electrode is helped, for saturated calomel electrode as reference electrode, be placed in 50 ml contains 5 mM H2PtCl6With 0.2 M H2SO4Mixed liquor
In, the s of electro-deposition 300 under conditions of the V of constant potential -0.20, Pd- graphenes-filter paper electrode is made.
Electrochemical sensing application：By Pd- graphenes-filter paper electrode of preparation, as the flexible electrode of self-supporting, it is applied to
In hydrogen peroxide electrochemical sensor.
Embodiment 5
A kind of preparation method of Pd- graphenes-filter paper, comprises the following steps：
（1）Compound concentration is 10 mg/mL graphene oxide water solution, and filter paper uses the qualitative filter paper that laboratory is commonly used, diameter
For 14 cm.
（2）Modify graphene oxide：Filter paper is immersed in step（1）The middle graphene oxide for preparing 10 obtained mg/mL
The aqueous solution, soak time are 25 s, and then, lifting is out dried in 35 DEG C of baking oven, is repeated 10 times, that is, is prepared oxygen
Graphite alkene-filter paper.
（3）Redox graphene：By step（2）In obtained graphene oxide-filter paper graphene oxide-filter paper exist
The h of reduction treatment 12 is carried out with the hydrazine hydrate steam that mass concentration is 50% under the conditions of 180 DEG C, prepares graphene-filter paper.
（4）Electro-deposition active component Pd nano particles：Using graphene-filter paper as working electrode, gauze platinum electrode is as auxiliary
Electrode is helped, for saturated calomel electrode as reference electrode, be placed in 50 ml contains 5 mM H2PtCl6With 0.2 M H2SO4Mixed liquor
In, the s of electro-deposition 50 under conditions of the V of constant potential -0.20, Pd- graphenes-filter paper electrode is made.
Electrochemical sensing application：By Pd- graphenes-filter paper electrode of preparation, as the flexible electrode of self-supporting, it is applied to
In hydrogen peroxide electrochemical sensor.
The exemplary embodiments that it is the present invention that embodiment 1-5, which is, its Pd- being prepared graphenes-filter paper electrode have
Larger specific surface area and high conductivity, more avtive spots can be provided for catalytic reaction, during as hydrogen peroxide sensor
Show good catalytic effect and excellent selectivity；Pd- graphenes-filter paper electrode effect that wherein prepared by embodiment 3 is most
It is good, in Fig. 3 paired observation show that the aperture of the Pd- graphenes-filter paper electrode prepared in embodiment 3 is the most obvious, electricity can be promoted
Proton transport in catalytic process.Contrast is drawn in Fig. 4, and Pd/ graphenes/filter paper electrode prepared by embodiment 1-5 is as peroxide
It is disodium hydrogen phosphate/sodium dihydrogen phosphate to change hydrogen sensor in the physiological systems of the hydrogen peroxide containing 5 mM（PBS）Buffer solution（PH is about
7.2）In cyclic voltammetric（CV）Figure, it is seen then that the response for the electrode that the electrode is prepared in embodiment 3 is the most obvious.
Below by taking embodiment 3 as an example, Pd- graphenes-filter paper electrode that it is prepared is analyzed：
From Figure 2 it can be seen that Pd particles are densely distributed uniform on graphene sheet layer.
As seen from Figure 5, Pd/ graphenes/filter paper electrode that prepared by embodiment 3 is as hydrogen peroxide sensor containing different dense
The physiological systems of the hydrogen peroxide of degree are disodium hydrogen phosphate/sodium dihydrogen phosphate（PBS）Buffer solution（PH about 7.2）In cyclic voltammetric
（CV）Figure, the 0, hydrogenperoxide steam generator of 2mM, 5mM and 10mM concentration is corresponded to respectively；It can be seen that sound of the electrode in -0.18V current potentials
Should be the most obvious.
As seen from Figure 6, Pd/ graphenes/filter paper electrode that prepared by embodiment 3 is as hydrogen peroxide sensor, in -0.18V
Apply under current potential to 20ml PBS（PH about 7.2）The timing ampere for being continuously added to various concentrations hydrogen peroxide is accordingly bent
Line（Amperometric i-t Curve）With corresponding linear fit curve；The curve shows stepped, the explanation of rule
The response quickly of the electrode pair hydrogen peroxide（Response time is less than 5s）, it is sensitive high to 105.4 μ A cm-2 mM-1。
It is visible by analysis below, the present invention in Pd- graphenes-filter paper electrode for hydrogen peroxide fast response time,
High sensitivity, it is highly suitable for detecting the concentration of hydrogen peroxide：Therefore the present invention can prepare high performance self-supporting flexible electrical
Pole material, the graphene-filter paper obtained using preparation method of the present invention（Including palladium particle/graphene-filter paper）Flexibility can be used as
Electrode, applied in hydrogen peroxide electrochemical sensor, for detecting such as the concentration of hydrogen peroxide；The flexible electrode can
Self-supporting, further, since the size of graphene-filter paper can very easily regulate and control according to demand, it is kind of a flexible electrode.Due to
Graphene has mechanical strength and pliability, the huge theoretical specific surface area and excellent conductivity of superelevation, and significantly
Chemical property, such as larger potential window, relatively low charge transfer resistance and the advantages that quick electron transport rate, by
The electrode material that grapheme material is formed, and its microstructure and properties is very superior；Method provided by the invention is on filter paper
It is grapheme modified to obtain porous structure, increase the specific surface area and electrical conductivity of filter paper；Also, by the use of filter paper as substrate,
The characteristics of raw material is cheap and easy to get, green non-pollution, and this life of filter paper is with flexible and high aperture adsorption rate, it can pass through simple high
Effect, the upper grapheme material of the immersion adsorption process of low energy consumption modification.This method stabilization simple to operate, raw material are easy to get pollution-free, anti-
Simple and efficient is answered, the preparation to flexible electrode simultaneously has great innovative significance applied to hydrogen peroxide sensor.
Above embodiment selects when being the concrete operations in the condition range of choice of scheme provided by the invention
Data, and the above raw material enumerated of the present invention, reaction condition such as graphene concentration, soak time and drying temperature, steam
Citing and high-low limit value in reduction temperature and time, electro-deposition current potential and time etc. can be realized to be proposed to the present invention
Microelectrode preparation, therefore just no longer repeat one by one.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included
Within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of graphene-filter paper, it is characterised in that comprise the following steps：
（1）Graphene oxide water solution is prepared, filter paper uses use for laboratory qualitative filter paper, wherein：
The concentration of the graphene oxide water solution is the mg/mL of 2 mg/mL~10；
The cm of a diameter of 4 cm of the filter paper~16；
（2）By the step（1）In filter paper be immersed in step（1）It is middle to prepare in the obtained graphene oxide water solution,
Then, lifting is out dried in an oven, is repeated for several times, graphene oxide-filter paper is prepared；
（3）By the step（2）In obtained graphene oxide-filter paper carry out reduction treatment with hydrazine hydrate steam, that is, obtain stone
Black alkene-filter paper.
2. the preparation method of graphene-filter paper as claimed in claim 1, it is characterised in that further comprising the steps of：
（4）With the step（3）In the obtained graphene-filter paper be working electrode, be placed in dissolved with potassium chloropalladite
In precursor solution, graphene-filter paper that electro-deposition obtains loading Pd nano particle is carried out.
3. the preparation method of graphene-filter paper as claimed in claim 1, it is characterised in that
The step（2）Filter paper is totally submerged in graphene oxide water solution during middle filter paper immersion；The soak time is 10
The s of s~30；
The step（2）The temperature of middle drying is 20 DEG C~45 DEG C；
The step（2）In soak repeatedly lifting number be 5~20 times.
4. the preparation method of graphene-filter paper as claimed in claim 1, it is characterised in that the step（3）Middle hydrazine hydrate it is dense
Degree is not less than 40%；The vapor (steam) temperature is 120 DEG C~180 DEG C；The reduction reaction time is the h of 6 h~24.
5. the preparation method of graphene-filter paper as claimed in claim 2, it is characterised in that the step（4）In electro-deposition be
Carried out using three-electrode system under conditions of constant potential, sedimentation potential is the V of -0.1 V~-0.5, and sedimentation time is 30 s
~300 s.
6. the preparation method of graphene-filter paper as claimed in claim 2, it is characterised in that the step（4）In presoma it is molten
Liquid is containing 5 mM H2PtCl6With 0.2 M H2SO4Solution.
7. the preparation method of graphene-filter paper as claimed in claim 2, it is characterised in that comprise the following steps：
（1）Compound concentration is 8 mg/mL graphene oxide water solution, and filter paper uses the qualitative filter paper that laboratory is commonly used, diameter
For 10 cm；
（2）Modify graphene oxide：Filter paper is immersed in step（1）The graphene oxide for 8 mg/mL that middle preparation obtains is water-soluble
Liquid, soak time are 30 s, and then, lifting is out dried in 25 DEG C of baking oven, is repeated 12 times, that is, is prepared oxidation stone
Black alkene-filter paper；
（3）Redox graphene：By step（2）In obtained graphene oxide-filter paper it is dense with quality under the conditions of 160 DEG C
The hydrazine hydrate steam of degree 50% carries out the h of reduction treatment 12, obtains graphene-filter paper；
（4）Electro-deposition active component Pd nano particles：Using graphene-filter paper as working electrode, gauze platinum electrode is as auxiliary electricity
Pole, for saturated calomel electrode as reference electrode, be placed in 50 ml contains 5 mM H2PtCl6With 0.2 M H2SO4Mixed liquor in,
The s of electro-deposition 200 under conditions of the V of constant potential -0.15, Pd- graphenes-filter paper is made.
8. the preparation method as described in claim 1-7 any one obtains graphene-filter paper as the flexible electrode of self-supporting
Using.
9. application as claimed in claim 8, it is characterised in that：Graphene-the filter paper exists as the flexible electrode of self-supporting
Application in content of hydrogen peroxide detection.
10. application as claimed in claim 9, it is characterised in that：Graphene-the filter paper exists as the flexible electrode of self-supporting
Application in hydrogen peroxide electrochemical sensor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710863994.3A CN107703196B (en) | 2017-09-22 | 2017-09-22 | Preparation method of graphene-filter paper and application of graphene-filter paper as self-supporting flexible electrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710863994.3A CN107703196B (en) | 2017-09-22 | 2017-09-22 | Preparation method of graphene-filter paper and application of graphene-filter paper as self-supporting flexible electrode |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107703196A true CN107703196A (en) | 2018-02-16 |
| CN107703196B CN107703196B (en) | 2020-05-22 |
Family
ID=61171887
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710863994.3A Active CN107703196B (en) | 2017-09-22 | 2017-09-22 | Preparation method of graphene-filter paper and application of graphene-filter paper as self-supporting flexible electrode |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107703196B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108845007A (en) * | 2018-04-25 | 2018-11-20 | 上海第二工业大学 | A kind of platinum/graphen paper nanometer combined electrode material and preparation method thereof for detecting hydrogen peroxide |
| CN109518530A (en) * | 2018-11-02 | 2019-03-26 | 杭州特种纸业有限公司 | Thick vulcan fibre of a kind of lamination and preparation method thereof |
| CN110687169A (en) * | 2019-11-01 | 2020-01-14 | 电子科技大学 | Humidity-sensitive carbon nanotube/graphene/organic composite flexible material, humidity sensor and preparation method thereof |
| CN110865115A (en) * | 2019-11-07 | 2020-03-06 | 杭州电子科技大学 | HA-graphene flexible electrode and preparation method and application thereof |
| CN113030204A (en) * | 2019-12-25 | 2021-06-25 | 大连大学 | Paper plastic electrode for detecting hydrogen peroxide and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265017A (en) * | 2013-05-17 | 2013-08-28 | 山西大学 | Preparation method of flexible self-supported paper graphene membrane and composite membrane thereof |
| CN104502412A (en) * | 2014-12-08 | 2015-04-08 | 中国石油大学(华东) | Graphene-based ammonia sensitive material and preparation method thereof |
| CN106483172A (en) * | 2016-09-22 | 2017-03-08 | 华中科技大学 | Method and product and application using ionic liquid electrodeposition graphene/carbon fiber |
-
2017
- 2017-09-22 CN CN201710863994.3A patent/CN107703196B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265017A (en) * | 2013-05-17 | 2013-08-28 | 山西大学 | Preparation method of flexible self-supported paper graphene membrane and composite membrane thereof |
| CN104502412A (en) * | 2014-12-08 | 2015-04-08 | 中国石油大学(华东) | Graphene-based ammonia sensitive material and preparation method thereof |
| CN106483172A (en) * | 2016-09-22 | 2017-03-08 | 华中科技大学 | Method and product and application using ionic liquid electrodeposition graphene/carbon fiber |
Non-Patent Citations (2)
| Title |
|---|
| YINSHUANG ZHAO 等: "Promotion effect of oxygen-containing functional groups and Fe species on Pd@graphene for CO catalytic oxidation", 《NEW JOURNAL OF CHEMISTRY》 * |
| 高玉荣 等: "石墨烯/纤维素复合材料的制备及应用", 《化学进展》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108845007A (en) * | 2018-04-25 | 2018-11-20 | 上海第二工业大学 | A kind of platinum/graphen paper nanometer combined electrode material and preparation method thereof for detecting hydrogen peroxide |
| CN109518530A (en) * | 2018-11-02 | 2019-03-26 | 杭州特种纸业有限公司 | Thick vulcan fibre of a kind of lamination and preparation method thereof |
| CN110687169A (en) * | 2019-11-01 | 2020-01-14 | 电子科技大学 | Humidity-sensitive carbon nanotube/graphene/organic composite flexible material, humidity sensor and preparation method thereof |
| CN110687169B (en) * | 2019-11-01 | 2022-06-10 | 电子科技大学 | Humidity-sensitive carbon nano tube/graphene/organic composite flexible material, humidity sensor and preparation method thereof |
| CN110865115A (en) * | 2019-11-07 | 2020-03-06 | 杭州电子科技大学 | HA-graphene flexible electrode and preparation method and application thereof |
| CN113030204A (en) * | 2019-12-25 | 2021-06-25 | 大连大学 | Paper plastic electrode for detecting hydrogen peroxide and preparation method thereof |
| CN113030204B (en) * | 2019-12-25 | 2022-08-02 | 大连大学 | Paper plastic electrode for detecting hydrogen peroxide and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107703196B (en) | 2020-05-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107703196A (en) | A kind of application of the preparation method of graphene filter paper and its flexible electrode as self-supporting | |
| Chen et al. | Preparation of highly sensitive Pt nanoparticles-carbon quantum dots/ionic liquid functionalized graphene oxide nanocomposites and application for H2O2 detection | |
| Zhang et al. | Direct electrochemistry of cytochrome c immobilized on one dimensional Au nanoparticles functionalized magnetic N-doped carbon nanotubes and its application for the detection of H2O2 | |
| Li et al. | Electrochemical biosensor based on one-dimensional MgO nanostructures for the simultaneous determination of ascorbic acid, dopamine, and uric acid | |
| Han et al. | Leaf-templated synthesis of 3D hierarchical porous cobalt oxide nanostructure as direct electrochemical biosensing interface with enhanced electrocatalysis | |
| Luo et al. | Reduced graphene oxide/PAMAM–silver nanoparticles nanocomposite modified electrode for direct electrochemistry of glucose oxidase and glucose sensing | |
| Ensafi et al. | A new non-enzymatic glucose sensor based on copper/porous silicon nanocomposite | |
| Liu et al. | Three-dimensional porous NiO nanosheets vertically grown on graphite disks for enhanced performance non-enzymatic glucose sensor | |
| Li et al. | Electrochemical behavior of graphene doped carbon paste electrode and its application for sensitive determination of ascorbic acid | |
| Sun et al. | Direct electrochemistry with enhanced electrocatalytic activity of hemoglobin in hybrid modified electrodes composed of graphene and multi-walled carbon nanotubes | |
| Niu et al. | Platinum nanoparticle-decorated carbon nanotube clusters on screen-printed gold nanofilm electrode for enhanced electrocatalytic reduction of hydrogen peroxide | |
| Rashed et al. | rGO/ZnO/Nafion nanocomposite as highly sensitive and selective amperometric sensor for detecting nitrite ions (NO2−) | |
| Ho Yang et al. | Directed Self‐Assembly of Gold Nanoparticles on Graphene‐Ionic Liquid Hybrid for Enhancing Electrocatalytic Activity | |
| Li et al. | Nonenzymatic glucose sensor based on a glassy carbon electrode modified with chains of platinum hollow nanoparticles and porous gold nanoparticles in a chitosan membrane | |
| Mani et al. | Iron nanoparticles decorated graphene-multiwalled carbon nanotubes nanocomposite-modified glassy carbon electrode for the sensitive determination of nitrite | |
| Ning et al. | A novel strategy to synthesize Au nanoplates and their application for enzymeless H2O2 detection | |
| Sun et al. | Electrochemical biosensor based on graphene, Mg2Al layered double hydroxide and hemoglobin composite | |
| Chen et al. | Dispersed Nickel Nanoparticles on Flower‐like Layered Nickel‐Cobalt Double Hydroxides for Non‐enzymic Amperometric Sensing of Glucose | |
| Zhao et al. | Enhancing direct electron transfer of glucose oxidase using a gold nanoparticle| titanate nanotube nanocomposite on a biosensor | |
| Peng et al. | One pot synthesis of nitrogen-doped hollow carbon spheres with improved electrocatalytic properties for sensitive H2O2 sensing in human serum | |
| Huang et al. | Direct electrochemistry of hemoglobin based on chitosan–ionic liquid–ferrocene/graphene composite film | |
| Chen et al. | Selective electrochemical detection of dopamine using nitrogen-doped graphene/manganese monoxide composites | |
| Li et al. | Electrodeposited nanogold decorated graphene modified carbon ionic liquid electrode for the electrochemical myoglobin biosensor | |
| Wang et al. | Direct electrochemistry and electrocatalysis of myoglobin using an ionic liquid-modified carbon paste electrode coated with Co 3 O 4 nanorods and gold nanoparticles | |
| Li et al. | An electrochemical sensor based on platinum nanoparticles and mesoporous carbon composites for selective analysis of dopamine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |