CN108298532A - A kind of preparation method of the sensing material of graphene doping - Google Patents
A kind of preparation method of the sensing material of graphene doping Download PDFInfo
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- CN108298532A CN108298532A CN201711412819.9A CN201711412819A CN108298532A CN 108298532 A CN108298532 A CN 108298532A CN 201711412819 A CN201711412819 A CN 201711412819A CN 108298532 A CN108298532 A CN 108298532A
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Abstract
The invention discloses a kind of preparation methods of the sensing material of graphene doping, and the present invention is by three-dimensional grapheme and Fe1.833(OH)0.5O2.5In conjunction with, contribute to improve Fe1.833(OH)0.5O2.5Configuration of surface, give full play to the synergistic effect of three-dimensional grapheme and hetero-junctions, enhance sensor detection sensitivity；This method preparation process avoids cumbersome multicomponent material synthesis step, as long as by routine operations such as simple centrifuge washing, filterings, it is simple for process, it is environmentally protective.
Description
Technical field
The present invention relates to sensor manufacturing fields, and in particular to a kind of preparation method of the sensing material of graphene doping.
Background technology
Nitrite is widely present in human environment, is most common nitrogenous compound in nature, green plants
Nitrogen source, frequently as food additive and preservative in food industry.The pollution of nitrite in drinking water can lead to many diseases
Sick such as methemoglobinemia, blue baby's syndrome also have gastric cancer, these diseases are reacted by nitrite and amine substance
Caused by the nitrosamine generated.Since nitrite is to the adverse effect of environment and human health, for nitrite
Sensitive detection has caused the attention of height.
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.
It is carbon nano-structured（Including fullerene, carbon nanotube and graphene etc.）Possess in terms of Electrochemical Detection a large amount of
Application.Because these materials possess high conductivity, wide electrochemical window, possess good chemical stability in most of electrolyte
And surface the advantages of easily regenerating.In carbon material, graphene（Graphene）, as novel two-dimension nano materials, to seek
Ideal nanostructure is asked to provide important channel.The synergistic effect of graphene and other components can assign material new spy
Property make material that there is different potential applications, such as metal-metallic oxide nano-particle, polymer for different demands
And the binary catalyst systems such as biomolecule.
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 the sensing material of graphene doping, the present invention by three-dimensional grapheme with
Fe1.833(OH)0.5O2.5In conjunction with, contribute to improve Fe1.833(OH)0.5O2.5Configuration of surface, give full play to three-dimensional grapheme and different
The synergistic effect of matter knot enhances the sensitivity of sensor detection；This method preparation process avoids cumbersome multicomponent material and closes
At step, as long as by routine operations such as simple centrifuge washing, filterings, it is simple for process, it is environmentally protective.
To achieve the goals above, the present invention provides a kind of preparation method of the sensing material of graphene doping, the party
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）Under ultrasound, the glycolic suspension of the three-dimensional grapheme is prepared, the ultrasonic time is 15-20 h, described three
The ratio for tieing up graphene and ethylene glycol is 0.5 mg/ml of 1-；
It is added in PDDA to the suspension and stirs evenly, continuously add FeCl2·4H2O is stirred evenly, the three-dimensional grapheme
Ratio with PDDA is 1:5-1:7 mg/μl；The three-dimensional grapheme and FeCl2·4H2The mass ratio of O is 1:2-2:1；
By obtained mixture and NH3·H2Hydro-thermal reaction is carried out immediately after O mixing, wherein the three-dimensional grapheme and NH3·
H2The ratio of O is 1:2 -1:3 mg/μl；Reaction temperature is 200 DEG C of 180-；
The sensing material is obtained after washing, drying.
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.
Under ultrasound, the glycolic suspension of the three-dimensional grapheme is prepared, the ultrasonic time is 15h, the three-dimensional
The ratio of graphene and ethylene glycol is 1mg/ml；It is added in PDDA to the suspension and stirs evenly, continuously add FeCl2·4H2O
It stirs evenly, the ratio of the three-dimensional grapheme and PDDA are 1:5 mg/μl；The three-dimensional grapheme and FeCl2·4H2The quality of O
Than being 1:2.
By obtained mixture and NH3·H2O mixing after carry out hydro-thermal reaction immediately, wherein the three-dimensional grapheme and
NH3·H2The ratio of O is 1:2 mg/μl；Reaction temperature is 180 DEG C；The sensing material is obtained after washing, drying.
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.
Under ultrasound, the glycolic suspension of the three-dimensional grapheme is prepared, the ultrasonic time is 20 h, the three-dimensional
The ratio of graphene and ethylene glycol is 0.5 mg/ml；It is added in PDDA to the suspension and stirs evenly, continuously add FeCl2·
4H2O is stirred evenly, and the ratio of the three-dimensional grapheme and PDDA are 1:7 mg/μl；The three-dimensional grapheme and FeCl2·4H2O's
Mass ratio is 2:1.
By obtained mixture and NH3·H2O mixing after carry out hydro-thermal reaction immediately, wherein the three-dimensional grapheme and
NH3·H2The ratio of O is 1:3 mg/μl；Reaction temperature is 200 DEG C；The sensing material is obtained after washing, drying.
Claims (2)
1. a kind of preparation method of the sensing material of graphene doping, 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）Under ultrasound, the glycolic suspension of the three-dimensional grapheme is prepared, the ultrasonic time is 15-20 h, described three
The ratio for tieing up graphene and ethylene glycol is 0.5 mg/ml of 1-；
It is added in PDDA to the suspension and stirs evenly, continuously add FeCl2·4H2O is stirred evenly, the three-dimensional grapheme
Ratio with PDDA is 1:5-1:7 mg/μl；The three-dimensional grapheme and FeCl2·4H2The mass ratio of O is 1:2-2:1；
By obtained mixture and NH3·H2Hydro-thermal reaction is carried out immediately after O mixing, wherein the three-dimensional grapheme and NH3·
H2The ratio of O is 1:2 -1:3 mg/μl；Reaction temperature is 200 DEG C of 180-；
The sensing material is obtained after washing, drying.
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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| CN201711412819.9A CN108298532A (en) | 2017-12-24 | 2017-12-24 | A kind of preparation method of the sensing material of graphene doping |
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| CN201711412819.9A CN108298532A (en) | 2017-12-24 | 2017-12-24 | A kind of preparation method of the sensing material of graphene doping |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104807861A (en) * | 2015-04-09 | 2015-07-29 | 山东师范大学 | Preparation method of spongy graphene-based stretchable gas sensor |
| CN106243652A (en) * | 2016-08-04 | 2016-12-21 | 苏州锐特捷化工制品有限公司 | A kind of graphene fiber modified Nano adsorbing material and preparation method |
| CN106629685A (en) * | 2016-12-28 | 2017-05-10 | 北京大学 | Three-dimensional graphene foam with multilevel structure and preparation method thereof |
-
2017
- 2017-12-24 CN CN201711412819.9A patent/CN108298532A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104807861A (en) * | 2015-04-09 | 2015-07-29 | 山东师范大学 | Preparation method of spongy graphene-based stretchable gas sensor |
| CN106243652A (en) * | 2016-08-04 | 2016-12-21 | 苏州锐特捷化工制品有限公司 | A kind of graphene fiber modified Nano adsorbing material and preparation method |
| CN106629685A (en) * | 2016-12-28 | 2017-05-10 | 北京大学 | Three-dimensional graphene foam with multilevel structure and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘茂祥: "以廉价铁氧化合物为催化核心的三维墨烯基亚硝酸盐电化学传感材料研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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