CN110057883A - A kind of preparation method of electric chemical formula CO sensor sensing electrode material - Google Patents
A kind of preparation method of electric chemical formula CO sensor sensing electrode material Download PDFInfo
- Publication number
- CN110057883A CN110057883A CN201910183142.9A CN201910183142A CN110057883A CN 110057883 A CN110057883 A CN 110057883A CN 201910183142 A CN201910183142 A CN 201910183142A CN 110057883 A CN110057883 A CN 110057883A
- Authority
- CN
- China
- Prior art keywords
- preparation
- chemical formula
- electrode material
- sensing electrode
- sensor sensing
- 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.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- 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 invention discloses a kind of preparation methods of electric chemical formula CO sensor sensing electrode material, are to solve the problem of prepared by existing electrochemical CO sensor.Specific step is as follows: step 1 by the present invention, prepares the suspension of graphene and water；Step 2, stirred suspension and sequentially adds ruthenic chloride and chloroplatinic acid；Step 3, the pH value for adjusting solution are 8-13 and reducing agent, heating stirring are added thereto；Solution is cooled to room temperature by step 4, then is filtered and dried to get finished product is arrived.Use bigger serface graphene for carrier in the present invention, finished product has the characteristics that highly sensitive, highly selective and stability as sensitive electrode, and the addition of ruthenium improves the utilization rate of pt atom, reduces the dosage of platinum；Preparation method of the invention is easy to operate, low in cost, is suitable for sensor element mass production, and the application for metal nano carbon composite in sensor field provides technical support.
Description
Technical field
The present invention relates to sensor field, the preparation side of specifically a kind of electric chemical formula CO sensor sensing electrode material
Method.
Background technique
CO is a kind of colourless, odorless, toxic and inflammable and explosive gas, the safety of life and property of its presence to people
Bring great threat.The industries such as industrial production coal gas, steel-making, coking, firing, mine operation, mine blasting and chemical industry
Practitioner have an opportunity to touch CO.In daily life, coal stove, chimney blocking, coal gas infra-red heater, gas stove and family
It is possible to generate CO with natural gas range gas leakage etc..The prison of CO is needed in environmentally friendly aspect vehicle exhaust and fuel cell hydrogen fuel
It surveys.
Traditional semiconductor-type CO sensor can cause semiconductor using semiconductor material surface adsorption and desorption gas molecule
The principle of the variation of conductance carrys out the concentration of detection gas.Have the characteristics that high sensitivity, economic and reliable, still, since it is to gas
The poor selectivity of body, stability is poor, cause its report by mistake probability it is big, and if for a long time do not encounter CO will because of oxidation and
Insensitive is become to CO.
In addition to this, the output signal of this quasi-instrument is nonlinear, there is certain difficulty for instrumental calibration.Electrochemistry
Gas sensor has low-power consumption, high sensitivity and selectivity, has good linear relationship etc. between signal and gas concentration
Advantage, therefore be the very important high-end kind that can be used for quantitative detection in gas sensor, it is widely used in petroleum, coal
The on-line checking of the various fields such as charcoal, chemical industry, aerospace, environmental protection, food safety and monitoring.Electrochemical CO sensor
Core material-sensitive electrode material is usually the carbon material of Supported Pt Nanoparticles, but since the catalytic effect of platinum preferably causes to sense
The selectivity of device is poor, and platinum natural resources is rare, expensive, this is just that the preparation of electrochemical CO sensor is brought not
Just.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of electric chemical formula CO sensor sensing electrode material, to solve
The problems mentioned above in the background art.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of electric chemical formula CO sensor sensing electrode material, the specific steps are as follows:
Step 1 prepares the suspension of graphene and water；
Step 2, stirred suspension and sequentially adds ruthenic chloride and chloroplatinic acid, obtains the first mixed solution；
Step 3 adjusts the pH value of the first mixed solution as 8-13 and reducing agent is added thereto, and heating stirring obtains second
Mixed solution；
Second mixed solution is cooled to room temperature by step 4, then is filtered and dried to get nano combined to finished product PtRu/C
Material.
As a further solution of the present invention: in step 1 graphene use bigger serface graphene, graphene and
The mass ratio of water is 1:1000-4000.
As a further solution of the present invention: the mass ratio of ruthenic chloride and graphene is 0.1-20:1, chlorine in step 2
The ratio between mole for changing ruthenium and chloroplatinic acid is 0.1-1:1.
As a further solution of the present invention: reducing agent is in sodium borohydride, hydrazine hydrate and ascorbic acid in step 3
Any one.
As a further solution of the present invention: the mode that the first mixed solution pH value is adjusted in step 3 is to the first mixing
The alkaline matters such as sodium hydroxide or ammonium hydroxide are added in solution.
As a further solution of the present invention: the temperature of heating stirring is 50-150 degrees Celsius in step 3, heating stirring
Time be 4-48 hours.
As a further solution of the present invention: the dry vacuum drying for being 60-120 degrees Celsius, drying time in step 4
It is 4-48 hours.
Compared with prior art, the beneficial effects of the present invention are:
Platinum-ruthenium alloys/the graphene nanocomposite material for using bigger serface graphene to prepare in the present invention for carrier, and pass
The platinum carbon material of system is compared, and is had highly sensitive, highly selective as sensitive electrode in electric chemical formula CO sensor and is stablized
The features such as property, and the addition of ruthenium improves the utilization rate of pt atom, reduces the dosage of platinum；
The present invention uses bigger serface graphene for raw material, so that platinum ruthenium atom is uniformly dispersed on the surface of graphene, rings to CO
It should be rapid；
The preparation method of electric chemical formula CO sensor sensing electrode material, easy to operate in the present invention, low in cost, system of the present invention
Material not only with higher sensitivity, good selectivity of the standby finished product as the sensitive electrode of electrochemical sensor, and
And the dosage of platinum can be reduced, it is suitable for sensor element mass production, is that metal nano carbon composite is led in sensor
The application in domain provides technical support.
Detailed description of the invention
Fig. 1 is the XRD diagram of the finished product of embodiment 1 in the preparation method of electric chemical formula CO sensor sensing electrode material.
Fig. 2 is that the finished product of embodiment 1 in the preparation method of electric chemical formula CO sensor sensing electrode material is in CO concentration
Response current figure under 20-100ppm.
Fig. 3 is that the finished product of embodiment 1 in the preparation method of electric chemical formula CO sensor sensing electrode material is in CO concentration
The relational graph of response current and CO concentration under 20-100ppm.
Fig. 4 is the finished product of embodiment 1 in the preparation method of electric chemical formula CO sensor sensing electrode material in density of hydrogen
For the curent change figure under 1000ppm.
Specific embodiment
The technical solution of the patent is explained in further detail With reference to embodiment.
Embodiment 1
The present embodiment provides a kind of preparation methods of electric chemical formula CO sensor sensing electrode material, specifically includes the following steps:
Accurately weigh 100mg bigger serface graphene, 200ml deionized water be added and stirs 30 minutes in beaker, then plus
Enter 50mg ruthenic chloride and 98mg chloroplatinic acid, adjust pH to 13 to above-mentioned mixed solution and dripping NaOH solution after stirring, is added
0.4g sodium borohydride, 50 degrees Celsius at a temperature of stir 2 hours, be cooled to room temperature and filtered to solution, when suction filtration is distinguished
It is eluted repeatedly 3 times with deionized water and ethyl alcohol, it is small that filtered filter cake is placed in in 120 degrees Celsius of vacuum oven dry 4
When, obtain PtRu/C nanocomposite.
For the characterization of the PtRu/C nanocomposite of preparation as shown in Figure 1, according to XRD test result, PtRu/C is platinum ruthenium
The composite material of alloy and graphene.Fig. 2 and Fig. 3 shows that PtRu/C can respond rapidly to CO, and response sensitivity is
64nA/ppm, carrying out repeatedly test can restore, and restore very fast, and the response current after recovery does not weaken, and shows material
It is with good stability and repeated.As shown in figure 4, the response current of hydrogen that PtRu/C is 1000ppm to concentration is
0.734 μ A, i.e. response sensitivity are about 0.73nA/ppm, far below PtRu/C to the response sensitivity of CO, so the material has
There is good selectivity.
Embodiment 2
The present embodiment provides a kind of preparation methods of electric chemical formula CO sensor sensing electrode material, specifically includes the following steps:
Accurately weigh 100mg bigger serface graphene, 100ml deionized water be added and stirs 30 minutes in beaker, then plus
Enter 10mg ruthenic chloride and 196mg chloroplatinic acid, adjust pH to 9 to above-mentioned mixed solution and dripping ammonium hydroxide after stirring, 10ml water is added
Close hydrazine, 150 degrees Celsius at a temperature of stir 24 hours, be cooled to room temperature and filtered to solution, when suction filtration spend respectively from
Sub- water and ethyl alcohol elute 3 times repeatedly, and filtered filter cake is placed in drying 24 hours in 80 degrees Celsius of vacuum oven, that is, is made
Obtain PtRu/C nanocomposite.
Material made from the PtRu/C nanocomposite and embodiment 1 of preparation has equal performance.
Embodiment 3
The present embodiment provides a kind of preparation methods of electric chemical formula CO sensor sensing electrode material, specifically includes the following steps:
50mg bigger serface graphene is accurately weighed, 200ml deionized water is added and is stirred in beaker 30 minutes, is then added
100mg ruthenic chloride and 98mg chloroplatinic acid adjust PH to 8 to above-mentioned mixed solution and dripping ammonium hydroxide after stirring, and it is anti-bad that 0.6g is added
Hematic acid, 70 degrees Celsius at a temperature of stir 48 hours, be cooled to room temperature and filtered to solution, when suction filtration spends ion respectively
Water and ethyl alcohol elute 3 times repeatedly, and filtered filter cake is placed in drying 48 hours in 60 degrees Celsius of vacuum oven, is obtained
PtRu/C nanocomposite.
Material made from the PtRu/C nanocomposite and embodiment 1 of preparation has equal performance.
The working principle of the invention is: the graphene nanocomposite material of the load platinum ruthenium alloy prepared in the present invention
(PtRu/C) as the not only sensitivity with higher, good selectivity of the material of the sensitive electrode of electrochemical sensor, and
And the dosage of platinum can be reduced.Simultaneously have the characteristics that simple process, it is low in cost, can large-scale industrial production.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.No
It should treat any reference in the claims as limiting the claims involved.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (8)
1. a kind of preparation method of electric chemical formula CO sensor sensing electrode material, which is characterized in that specific step is as follows:
Step 1 prepares the suspension of graphene and water；
Step 2, stirred suspension and sequentially adds ruthenic chloride and chloroplatinic acid, obtains the first mixed solution；
Step 3 adjusts the pH value of the first mixed solution as 8-13 and reducing agent is added thereto, and heating stirring obtains second
Mixed solution；
Second mixed solution is cooled to room temperature by step 4, then is filtered and dried to get finished product is arrived.
2. the preparation method of electric chemical formula CO sensor sensing electrode material according to claim 1, which is characterized in that institute
Stating the mass ratio of graphene and water in step 1 is 1:1000-4000.
3. the preparation method of electric chemical formula CO sensor sensing electrode material according to claim 1 or 2, feature exist
In the mass ratio of ruthenic chloride and graphene is 0.1-20:1 in the step 2, and the ratio between mole of ruthenic chloride and chloroplatinic acid is
0.1-1:1。
4. the preparation method of electric chemical formula CO sensor sensing electrode material according to claim 1, which is characterized in that institute
Stating reducing agent in step 3 is any one in sodium borohydride, hydrazine hydrate and ascorbic acid.
5. the preparation method of electric chemical formula CO sensor sensing electrode material according to claim 1, which is characterized in that institute
Stating and adjusting the mode of the first mixed solution pH value in step 3 is that alkaline matter is added into the first mixed solution.
6. the preparation method of electric chemical formula CO sensor sensing electrode material according to claim 1 or 4, feature exist
In the temperature of heating stirring is 50-150 degrees Celsius in the step 3, and the time of heating stirring is 4-48 hours.
7. the preparation method of electric chemical formula CO sensor sensing electrode material according to claim 1, which is characterized in that institute
Stating the dry vacuum drying for being 60-120 degrees Celsius, drying time in step 4 is 4-48 hours.
8. the preparation method of electric chemical formula CO sensor sensing electrode material according to claim 1, which is characterized in that institute
Ionized water and ethyl alcohol is spent respectively when stating suction filtration in step 4 to elute repeatedly 3 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910183142.9A CN110057883A (en) | 2019-03-12 | 2019-03-12 | A kind of preparation method of electric chemical formula CO sensor sensing electrode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910183142.9A CN110057883A (en) | 2019-03-12 | 2019-03-12 | A kind of preparation method of electric chemical formula CO sensor sensing electrode material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110057883A true CN110057883A (en) | 2019-07-26 |
Family
ID=67316871
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910183142.9A Pending CN110057883A (en) | 2019-03-12 | 2019-03-12 | A kind of preparation method of electric chemical formula CO sensor sensing electrode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110057883A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101740786A (en) * | 2009-12-14 | 2010-06-16 | 浙江大学 | PtRu/graphene nano electro-catalyst and preparation method thereof |
| US20140377790A1 (en) * | 2013-06-19 | 2014-12-25 | Indian Institute Of Technology Madras | Metal nanoparticle decorated carbon nanotubes and methods of preparation and use |
| CN104483365A (en) * | 2014-12-17 | 2015-04-01 | 江西师范大学 | Electrochemical gas sensing device adopting precious metal and graphene composite material as sensing electrode and production method of electrochemical gas sensing device |
| CN107991366A (en) * | 2017-12-01 | 2018-05-04 | 无锡市尚沃医疗电子股份有限公司 | The expiration hydrogen sensor of anti-interference fast-response |
| CN108802138A (en) * | 2018-08-06 | 2018-11-13 | 南京工业大学 | A kind of membrane electrode, electrochemical gas sensor and its application |
-
2019
- 2019-03-12 CN CN201910183142.9A patent/CN110057883A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101740786A (en) * | 2009-12-14 | 2010-06-16 | 浙江大学 | PtRu/graphene nano electro-catalyst and preparation method thereof |
| US20140377790A1 (en) * | 2013-06-19 | 2014-12-25 | Indian Institute Of Technology Madras | Metal nanoparticle decorated carbon nanotubes and methods of preparation and use |
| CN104483365A (en) * | 2014-12-17 | 2015-04-01 | 江西师范大学 | Electrochemical gas sensing device adopting precious metal and graphene composite material as sensing electrode and production method of electrochemical gas sensing device |
| CN107991366A (en) * | 2017-12-01 | 2018-05-04 | 无锡市尚沃医疗电子股份有限公司 | The expiration hydrogen sensor of anti-interference fast-response |
| CN108802138A (en) * | 2018-08-06 | 2018-11-13 | 南京工业大学 | A kind of membrane electrode, electrochemical gas sensor and its application |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Afkhami et al. | Construction of a chemically modified electrode for the selective determination of nitrite and nitrate ions based on a new nanocomposite | |
| Wang et al. | Controlled synthesis and enhanced catalytic and gas‐sensing properties of tin dioxide nanoparticles with exposed high‐energy facets | |
| Ma et al. | Enhanced formaldehyde sensing performance at ppb level with Pt-doped nanosheet-assembled In2O3 hollow microspheres | |
| CN107827150B (en) | Nickel-doped tin oxide nano material, formaldehyde gas sensor and preparation method | |
| Li et al. | Enhanced methanol sensing properties of SnO 2 microspheres in a composite with Pt nanoparticles | |
| CN101251508B (en) | Method for manufacturing gas sensor for testing hydrogen | |
| CN107561133A (en) | A kind of preparation method and application of precious metal doping WO3 base formaldehyde gas sensitive materials | |
| CN108387625B (en) | A kind of double coating methane gas sensors and preparation method thereof of anti-organosilicon poisoning | |
| Karaduman et al. | Green synthesis of γ-Fe 2 O 3 nanoparticles for methane gas sensing | |
| CN112240898B (en) | Photoelectrochemical aptamer sensor and preparation method and application thereof | |
| Wang et al. | PdO/SnO2 hollow nanospheres for carbon monoxide detection | |
| CN110308186A (en) | A kind of preparation method and applications of the electrochemical sensor based on MIL-88-Fe/Ni | |
| CN105973957A (en) | Nafion based current type CO sensor with carbon fiber supported Pt nanoparticles as sensitive material and preparation method thereof | |
| Li et al. | Au@ Pd core–shell nanoparticles: A highly active electrocatalyst for amperometric gaseous ethanol sensors | |
| He et al. | Oxygen vacancy mediated step-scheme heterojunction of WO2. 9/g-C3N4 for efficient electrochemical sensing of 4-nitrophenol | |
| Lee et al. | Novel SnO2-based gas sensors promoted with metal oxides for the detection of dichloromethane | |
| Liu et al. | An electrochemical sensor for selective detection of p-aminophenol using hemin-graphene composites and molecularly imprinted polymer | |
| Liu et al. | Purification of Residual Ni and Co Hydroxides from Fe‐Free Alkaline Electrolyte for Electrocatalysis Studies | |
| Cai et al. | Fabrication of ZnO/Pd@ ZIF-8/Pt hybrid for selective methane detection in the presence of ethanol and NO2 | |
| CN112924498B (en) | Palladium monoatomic modified tin oxide composite material and preparation method and application thereof | |
| CN110057883A (en) | A kind of preparation method of electric chemical formula CO sensor sensing electrode material | |
| Tang et al. | ZnO@ CuO hollow nanosphere-based composites used for the sensitive detection of hydrogen sulfide with long-term stability | |
| Li et al. | Room temperature hydrogen sensor based on Nafion and Pd/CF sensing electrode | |
| Li et al. | Photoactivated oxidase mimetics derived from dicyandiamide and barbituric acid for colorimetric detection of glutathione | |
| CN109557139A (en) | A kind of preparation method of ZnO nanorod compound |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190726 |