CN108147399A - A kind of preparation method of three-dimensional grapheme nickel oxide sensor material - Google Patents
A kind of preparation method of three-dimensional grapheme nickel oxide sensor material Download PDFInfo
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- CN108147399A CN108147399A CN201711488710.3A CN201711488710A CN108147399A CN 108147399 A CN108147399 A CN 108147399A CN 201711488710 A CN201711488710 A CN 201711488710A CN 108147399 A CN108147399 A CN 108147399A
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- dimensional grapheme
- foamed aluminium
- nickel
- graphene
- temperature
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
Abstract
The invention discloses a kind of preparation method of three-dimensional grapheme nickel oxide sensor material, the present invention is combined three-dimensional grapheme with nickel oxide, is helped to improve the configuration of surface of nickel oxide, is enhanced the sensitivity of sensor detection；This method preparation process is simple, improves response efficiency by improving material specific surface area and surface-active vacancy, reduces response temperature, makes application of the semi-conducting material in terms of gas sensor simpler.
Description
Technical field
The present invention relates to sensor manufacturing fields, and in particular to a kind of preparation of three-dimensional grapheme nickel oxide sensor material
Method.
Background technology
While science and technology and social economy's rapid development, white elephant is also brought to natural environment, air is dirty
Dye seriously restricts the sustainable development of the mankind.Industrial production produces a large amount of toxic, pernicious gas, not only pollute environment,
Ecology is destroyed, and jeopardizes health and life security.Therefore, the ingredient of toxic gas and concentration meaning weight in environment are detected
Greatly.
So far, 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.
Nickel oxide hollow ball is due to adjustable pore passage structure, high-specific surface area and stronger ion-exchange performance, having
It is reacted in catalytic process in active sites conducive to reactant, the detection aspect of the gases such as ethyl alcohol, acetone, formaldehyde is shown
Greatly application prospect, however study all be not so good as people's will in terms of operating temperature, detection limit, anti-interference earlier.In porous
Empty spherical structure is compared with other nanostructureds, the specific surface area with bigger and more diffusion admittances under same volume, from
And possess higher sensibility and capability of fast response.
Three-dimensional grapheme material has the excellent chemical property of two-dimensional graphene, while has the specific surface area and more of bigger
Add excellent flexibility, the distortion of general level does not interfere with the property and characteristic of material, is conducive to prepare stretchable, stable
The good sensor of property.
Invention content
The present invention provides a kind of preparation method of three-dimensional grapheme nickel oxide sensor material, of the invention by three-dimensional grapheme
It is combined with nickel oxide, helps to improve the configuration of surface of nickel oxide, enhance the sensitivity of sensor detection；This method prepares work
Skill is simple, improves response efficiency by improving material specific surface area and surface-active vacancy, reduces response temperature, make partly to lead
Application of the body material in terms of gas sensor is simpler.
To achieve these goals, the present invention provides a kind of preparation sides of three-dimensional grapheme nickel oxide sensor material
Method, 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）The three-dimensional grapheme material is scattered in deionized water in the mixed solution of dispersant, adding after being completely dispersed
Enter nickel presoma and slow release precipitator pregnancy urotropine, it is permanent at a temperature of 70-95 DEG C that the beaker for filling solution is put into drying box
Temperature heating, reaction time 10-15h obtain being put into crucible high-temperature calcination after precipitating cleaned drying, by the green powder of precipitation
It being put into Muffle furnace, 5-10h is calcined under air conditions, heating rate is 10-15 DEG C/min, and heated perimeter is 600-700 DEG C,
Obtain three-dimensional grapheme nickel oxide sensor material；
Wherein, nickel presoma is one kind of nickel sulfate, nickel chloride, Nickelous nitrate hexahydrate or nickel oxalate；
In mixed liquor, according to molar ratio Ni：Hexa（HMTA）=（2-1）：1；
Wherein, dispersant is dimethyl sulfoxide (DMSO)（DMSO）, dimethylformamide (DMF), one in dimethylacetylamide (DMAC)
Kind；
The method of dispersion is stirred for magnetic stirring apparatus, mixing time 25-30min, the matter of the three-dimensional grapheme material
Measure score 7-10%.
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, be 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 keep hydrogen flowing quantity constant, growth closes gas after 50-100 minutes and is down to room temperature, you can obtains
The substrate of Direct precipitation graphene, i.e. graphene/foamed aluminium composite material.
Specific embodiment
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 keep hydrogen stream
Measure constant, growth closes gas and is down to room temperature after 50 minutes, 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.
The three-dimensional grapheme material is scattered in deionized water in the mixed solution of dispersant, adding after being completely dispersed
Enter nickel presoma and slow release precipitator pregnancy urotropine, wherein, dispersant is dimethyl sulfoxide (DMSO)（DMSO）；The method of dispersion is magnetic
Power blender is stirred, mixing time 25min, the mass fraction 7% of the three-dimensional grapheme material.
The beaker for filling solution is put into drying box heated at constant temperature at a temperature of 70 DEG C, reaction time 10h is precipitated
Crucible high-temperature calcination is put into after cleaned drying, the green powder of precipitation is put into Muffle furnace, 5h is calcined under air conditions,
Heating rate is 10 DEG C/min, and heated perimeter is 600 DEG C, obtains three-dimensional grapheme nickel oxide sensor material；Wherein, nickel forerunner
Body is nickel sulfate；In mixed liquor, according to molar ratio Ni：Hexa（HMTA）=2：1.
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 keep hydrogen
Flow is constant, and growth closes gas after 100 minutes and is down to room temperature, you can obtains 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.
The three-dimensional grapheme material is scattered in deionized water in the mixed solution of dispersant, adding after being completely dispersed
Enter nickel presoma and slow release precipitator pregnancy urotropine, wherein, dispersant is dimethylacetylamide (DMAC)；The method of dispersion is
Magnetic stirring apparatus is stirred, mixing time 30min, the mass fraction 10% of the three-dimensional grapheme material.
The beaker for filling solution is put into drying box heated at constant temperature at a temperature of 95 DEG C, reaction time 15h is precipitated
Crucible high-temperature calcination is put into after cleaned drying, the green powder of precipitation is put into Muffle furnace, is calcined under air conditions
10h, heating rate are 15 DEG C/min, and heated perimeter is 700 DEG C, obtains three-dimensional grapheme nickel oxide sensor material；Wherein, nickel
Presoma is one kind of Nickelous nitrate hexahydrate；In mixed liquor, according to molar ratio Ni：Hexa（HMTA）=1：1.
Claims (2)
1. a kind of preparation method of three-dimensional grapheme nickel oxide 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）The three-dimensional grapheme material is scattered in deionized water in the mixed solution of dispersant, adding after being completely dispersed
Enter nickel presoma and slow release precipitator pregnancy urotropine, it is permanent at a temperature of 70-95 DEG C that the beaker for filling solution is put into drying box
Temperature heating, reaction time 10-15h obtain being put into crucible high-temperature calcination after precipitating cleaned drying, by the green powder of precipitation
It being put into Muffle furnace, 5-10h is calcined under air conditions, heating rate is 10-15 DEG C/min, and heated perimeter is 600-700 DEG C,
Obtain three-dimensional grapheme nickel oxide sensor material；
Wherein, nickel presoma is one kind of nickel sulfate, nickel chloride, Nickelous nitrate hexahydrate or nickel oxalate；
In mixed liquor, according to molar ratio Ni：Hexa（HMTA）=（2-1）：1；
Wherein, dispersant is dimethyl sulfoxide (DMSO)（DMSO）, dimethylformamide (DMF), one in dimethylacetylamide (DMAC)
Kind；
The method of dispersion is stirred for magnetic stirring apparatus, mixing time 25-30min, the matter of the three-dimensional grapheme material
Measure score 7-10%.
2. the method as described in claim 1, which is characterized in that using 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 keep 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 |
|---|---|---|---|---|
| CN109851284A (en) * | 2019-04-15 | 2019-06-07 | 福建农林大学 | Multiple elements design aerogel material and its preparation and its application in electro-magnetic wave absorption |
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| CN102583337A (en) * | 2012-01-20 | 2012-07-18 | 中国科学院上海硅酸盐研究所 | Preparation method for graphene material with porous structure |
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| 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 |
| CN106241782A (en) * | 2016-07-27 | 2016-12-21 | 安徽理工大学 | The preparation method of Graphene/carbon nanotube composite material |
| CN106587173A (en) * | 2016-12-08 | 2017-04-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Micro-porous hollow nickel oxide gas-sensitive material for selectively adsorbing formaldehyde as well as preparation method and application of micro-porous hollow nickel oxide gas-sensitive material |
-
2017
- 2017-12-29 CN CN201711488710.3A patent/CN108147399A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583337A (en) * | 2012-01-20 | 2012-07-18 | 中国科学院上海硅酸盐研究所 | Preparation method for graphene material with porous structure |
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| 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 |
| CN106241782A (en) * | 2016-07-27 | 2016-12-21 | 安徽理工大学 | The preparation method of Graphene/carbon nanotube composite material |
| CN106587173A (en) * | 2016-12-08 | 2017-04-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Micro-porous hollow nickel oxide gas-sensitive material for selectively adsorbing formaldehyde as well as preparation method and application of micro-porous hollow nickel oxide gas-sensitive material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109851284A (en) * | 2019-04-15 | 2019-06-07 | 福建农林大学 | Multiple elements design aerogel material and its preparation and its application in electro-magnetic wave absorption |
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