CN108318556A - A kind of preparation method of graphene cobalt acid nickel sensor material - Google Patents
A kind of preparation method of graphene cobalt acid nickel sensor material Download PDFInfo
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- CN108318556A CN108318556A CN201711412810.8A CN201711412810A CN108318556A CN 108318556 A CN108318556 A CN 108318556A CN 201711412810 A CN201711412810 A CN 201711412810A CN 108318556 A CN108318556 A CN 108318556A
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Abstract
The invention discloses a kind of preparation method of graphene cobalt acid nickel sensor material, the present invention is by three-dimensional grapheme and NiCo2O4In conjunction with, contribute to improve NiCo2O4Configuration of surface, give full play to the synergistic effect of three-dimensional grapheme and hetero-junctions, enhance sensor detection sensitivity；In the application of electrode to ascorbic acid non-enzymatic electrochemical sensor for the material modification that this method preparation process obtains, Ascorbic Acid has preferable detectable limit, linearly related system, linear detection range, high sensitivity.
Description
Technical field
The present invention relates to sensor manufacturing fields, and in particular to a kind of preparation side of graphene cobalt acid nickel sensor material
Method.
Background technology
Now, there are many method for measuring ascorbic acid, including titrimetry method, fluorescer method, voltammetry, flow injection point
Analysis method, spectrophotometry de termination, ultra-performance liquid chromatography and electrochemical sensor etc., wherein electrochemical sensor method has
The advantages that analyze speed is fast, and reagent dosage is few and detection sensitivity is high, so having in the detection of detection ascorbic acid preferable
Foreground.Electrochemical sensor is based primarily upon target detection thing and the redox of material surface, easy to operation, by
The concern of more and more researchers.
So far, be based on nickel oxide (NiO), cobalt oxide (Co3O4), cuprous oxide (Cu2O), zinc oxide (ZnO), two
The transition metal oxides such as manganese oxide (MnO2) and cobalt acid nickel (NiCo2O4) are the sensitive material of modified electrode in sensor
Field has carried out certain research.Wherein in these oxides, since ternary transition oxide NiCo2O4 contains different prices
Nickel ion and cobalt ions, show the electron conduction of superelevation and excellent electro catalytic activity.According to research reports, with NiO,
Co3O4 is compared, and the electron conduction of hybrid transition metal NiCo2O4 is at least their twice or more, these characteristics are to test
High performance electrochemical sensor electrodes material is highly beneficial.
Graphene（Graphene）, as novel two-dimension nano materials, weight is provided to seek ideal nanostructure
The channel wanted.The synergistic effect of graphene and other components can assign material new characteristic and material is had for different demands
There are the binary catalysts bodies such as different potential application, such as metal-metallic oxide nano-particle, polymer and biomolecule
System.
The chemical property and electric conductivity that three-dimensional grapheme material has two-dimensional graphene excellent, while having the ratio table of bigger
Area and more excellent flexibility, the distortion of general level do not interfere with the property and characteristic of material, are conducive to prepare
Sensor stretchable, stability is good.
Invention content
The present invention provides a kind of preparation method of graphene cobalt acid nickel sensor material, the present invention by three-dimensional grapheme with
NiCo2O4In conjunction with, contribute to improve NiCo2O4Configuration of surface, give full play to the synergistic effect of three-dimensional grapheme and hetero-junctions,
Enhance the sensitivity of sensor detection；The application of electrode of material that this method preparation process obtains modification is to ascorbic acid non-enzymatic
In electrochemical sensor, Ascorbic Acid has preferable detectable limit, linearly related system, linear detection range, sensitivity
It is high.
To achieve the goals above, the present invention provides a kind of preparation methods of graphene cobalt acid nickel sensor material, should
Method includes the following steps：
（1）Prepare three-dimensional grapheme material
Three-dimensional grapheme is prepared on foamed aluminium substrate, obtains graphene/foamed aluminium composite material；
Graphene/foamed aluminium composite material is immersed in etching solution, after the dissolving completely of foamed aluminium substrate, obtains three-dimensional graphite
Alkene material；The etching solution is iron chloride or iron nitrate solution, and the solution concentration is 0.5-5mol/L
（2）It is 1 to take ethylene glycol and water by volume:The ratio of 1-2 is mixed to get mixed liquor, weighs 1-2 respectively in parts by weight
PVP, is first dissolved in 400-450 portions of mixed liquors by part described three-dimensional grapheme material, 35-38 parts of PVP, then by the three-dimensional graphite
Alkene material is scattered in mixed liquor, and NiCl is added after being stirred by ultrasonic uniformly2·6H2O and CoCl2·6H2O, stirring keep it final dense
Degree is respectively 0.002-0.004mg/L, 0.001-0.003mg/L；Then 0.003 is added dropwise into above-mentioned solution by volume
Part Na2S2O3, distilled water and ethylene glycol centrifuge washing are used after colour stable immediately, 250- in air after being dried at 50-60 DEG C
300 DEG C of calcining 2-3h, collection obtain the sensor electrode material.
Preferably, using chemical vapour deposition technique graphene/foamed aluminium composite material, the specific steps are：Foamed aluminium is put
Enter in vacuum reaction stove heating region, vacuumize, heat simultaneously, by hydrogen injection vacuum reaction stove, is heated to predetermined temperature
After 100-500 DEG C, then constant temperature 10-30 minutes anneals, after being heated to 900-1100 DEG C of predetermined temperature, carbon source is led to
Enter vacuum reaction stove, while keeping hydrogen flowing quantity constant, growth closes gas and is down to room temperature after 50-100 minutes, you can obtain
The substrate of Direct precipitation graphene, i.e. graphene/foamed aluminium composite material.
Specific implementation mode
Embodiment one
Using chemical vapour deposition technique graphene/foamed aluminium composite material, the specific steps are：Foamed aluminium is put into vacuum reaction stove
It in heating region, vacuumizes, heats simultaneously, by hydrogen injection vacuum reaction stove, after being heated to 100 DEG C of predetermined temperature, constant temperature 10
Minute, it then anneals, after being heated to 900 DEG C of predetermined temperature, carbon source is passed through vacuum reaction stove, while keeping hydrogen stream
Measure constant, growth closes after 50 minutes and gas and is down to room temperature, you can obtain the substrate of Direct precipitation graphene, i.e., graphene/
Foamed aluminium composite material.
Graphene/foamed aluminium composite material is immersed in etching solution, after the dissolving completely of foamed aluminium substrate, obtains three-dimensional
Grapheme material；The etching solution is iron chloride or iron nitrate solution, and the solution concentration is 0.5mol/L.
It is 1 to take ethylene glycol and water by volume:1 ratio is mixed to get mixed liquor, weighs 1 part of institute respectively in parts by weight
Three-dimensional grapheme material, 35 parts of PVP are stated, first PVP is dissolved in 400 portions of mixed liquors, then the three-dimensional grapheme material is disperseed
In mixed liquor, NiCl is added after being stirred by ultrasonic uniformly2·6H2O and CoCl2·6H2O, stirring make its ultimate density be respectively
0.002mg/L、0.001mg/L；0.003 part of Na is then added dropwise into above-mentioned solution by volume2S2O3, after colour stable
Distilled water and ethylene glycol centrifuge washing are used immediately, and 250 DEG C of calcining 2h, collection obtain the sensing in air after being dried at 50 DEG C
Device electrode material.
Embodiment two
Using chemical vapour deposition technique graphene/foamed aluminium composite material, the specific steps are：Foamed aluminium is put into vacuum reaction stove
It in heating region, vacuumizes, heats simultaneously, by hydrogen injection vacuum reaction stove, after being heated to 500 DEG C of predetermined temperature, constant temperature 30
Minute, it then anneals, after being heated to 1100 DEG C of predetermined temperature, carbon source is passed through vacuum reaction stove, while keeping hydrogen
Flow is constant, and growth closes gas and is down to room temperature after 100 minutes, you can obtain the substrate of Direct precipitation graphene, i.e. graphite
Alkene/foamed aluminium composite material.
Graphene/foamed aluminium composite material is immersed in etching solution, after the dissolving completely of foamed aluminium substrate, obtains three-dimensional
Grapheme material；The etching solution is iron nitrate solution, and the solution concentration is 5mol/L.
It is 1 to take ethylene glycol and water by volume:2 ratio is mixed to get mixed liquor, weighs 2 parts of institutes respectively in parts by weight
Three-dimensional grapheme material, 38 parts of PVP are stated, first PVP is dissolved in 450 portions of mixed liquors, then the three-dimensional grapheme material is disperseed
In mixed liquor, NiCl is added after being stirred by ultrasonic uniformly2·6H2O and CoCl2·6H2O, stirring make its ultimate density be respectively
0.002-0.004mg/L、0.003mg/L；0.003 part of Na is then added dropwise into above-mentioned solution by volume2S2O3, color
Distilled water and ethylene glycol centrifuge washing are used after stabilization immediately, 300 DEG C of calcining 3h, collection obtain institute in air after being dried at 60 DEG C
State sensor electrode material.
Claims (2)
1. a kind of preparation method of graphene cobalt acid nickel sensor material, this method comprises the following steps：
（1）Prepare three-dimensional grapheme material
Three-dimensional grapheme is prepared on foamed aluminium substrate, obtains graphene/foamed aluminium composite material；
Graphene/foamed aluminium composite material is immersed in etching solution, after the dissolving completely of foamed aluminium substrate, obtains three-dimensional graphite
Alkene material；The etching solution is iron chloride or iron nitrate solution, and the solution concentration is 0.5-5mol/L
（2）It is 1 to take ethylene glycol and water by volume:The ratio of 1-2 is mixed to get mixed liquor, weighs 1-2 respectively in parts by weight
PVP, is first dissolved in 400-450 portions of mixed liquors by part described three-dimensional grapheme material, 35-38 parts of PVP, then by the three-dimensional graphite
Alkene material is scattered in mixed liquor, and NiCl is added after being stirred by ultrasonic uniformly2·6H2O and CoCl2·6H2O, stirring keep it final dense
Degree is respectively 0.002-0.004mg/L, 0.001-0.003mg/L；Then 0.003 is added dropwise into above-mentioned solution by volume
Part Na2S2O3, distilled water and ethylene glycol centrifuge washing are used after colour stable immediately, 250- in air after being dried at 50-60 DEG C
300 DEG C of calcining 2-3h, collection obtain the sensor electrode material.
2. the method as described in claim 1, which is characterized in that use chemical vapour deposition technique graphene/foamed aluminium composite wood
Material, the specific steps are：Foamed aluminium is put into vacuum reaction stove heating region, vacuumizes, heats simultaneously, hydrogen injection vacuum is anti-
It answers in stove, after being heated to 100-500 DEG C of predetermined temperature, then constant temperature 10-30 minutes anneals, is heated to predetermined temperature
After 900-1100 DEG C, carbon source is passed through vacuum reaction stove, while keeping hydrogen flowing quantity constant, growth closes gas after 50-100 minutes
Body is simultaneously down to room temperature, you can obtains the substrate of Direct precipitation graphene, i.e. graphene/foamed aluminium composite material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112946035A (en) * | 2021-01-29 | 2021-06-11 | 华中科技大学 | Long-acting reference electrode for monitoring corrosion of steel bar and preparation method thereof |
Citations (4)
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|---|---|---|---|---|
| CN102826545A (en) * | 2012-09-24 | 2012-12-19 | 吴敏 | Magnetic graphene material for detecting phthalic acid ester, and preparation and application thereof |
| CN104764779A (en) * | 2015-04-09 | 2015-07-08 | 山东师范大学 | Preparation method of flexible gas-sensitive sensor with spongy graphene/zinc oxide mixed structure |
| CN106770547A (en) * | 2016-12-07 | 2017-05-31 | 海南大学 | A kind of synthetic method of cobalt acid nickel hollow ball non-enzymatic biological sensor sensing material |
| CN107176595A (en) * | 2017-05-24 | 2017-09-19 | 北京石油化工学院 | A kind of phosphorus alkene graphene composite material and preparation method thereof |
-
2017
- 2017-12-24 CN CN201711412810.8A patent/CN108318556A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826545A (en) * | 2012-09-24 | 2012-12-19 | 吴敏 | Magnetic graphene material for detecting phthalic acid ester, and preparation and application thereof |
| CN104764779A (en) * | 2015-04-09 | 2015-07-08 | 山东师范大学 | Preparation method of flexible gas-sensitive sensor with spongy graphene/zinc oxide mixed structure |
| CN106770547A (en) * | 2016-12-07 | 2017-05-31 | 海南大学 | A kind of synthetic method of cobalt acid nickel hollow ball non-enzymatic biological sensor sensing material |
| CN107176595A (en) * | 2017-05-24 | 2017-09-19 | 北京石油化工学院 | A kind of phosphorus alkene graphene composite material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112946035A (en) * | 2021-01-29 | 2021-06-11 | 华中科技大学 | Long-acting reference electrode for monitoring corrosion of steel bar and preparation method thereof |
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