CN110095512A - A kind of gallic acid cadmium nano material of PARA FORMALDEHYDE PRILLS(91,95) gas highly selective, low detection limit and quick response - Google Patents
A kind of gallic acid cadmium nano material of PARA FORMALDEHYDE PRILLS(91,95) gas highly selective, low detection limit and quick response Download PDFInfo
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- CN110095512A CN110095512A CN201910464194.3A CN201910464194A CN110095512A CN 110095512 A CN110095512 A CN 110095512A CN 201910464194 A CN201910464194 A CN 201910464194A CN 110095512 A CN110095512 A CN 110095512A
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- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
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Abstract
The gallic acid cadmium nano material of the invention discloses a kind of PARA FORMALDEHYDE PRILLS(91,95) gases highly selective, low detection limit and quick response, belongs to gas sensitive technical field.Nano material composition is gallic acid cadmium nano-powder, and the size of powder granule is 40-60 nanometers；The nano-powder is prepared by co-precipitation and heat-treating methods.Using the nano-powder material as heater-type gas sensor made of gas sensitive, when operating temperature is 150 DEG C, element reaches 50-70 to the sensitivity of 100ppm formaldehyde, and PARA FORMALDEHYDE PRILLS(91,95) detection limit is down to 0.01ppm, and response to 0.01-100ppm formaldehyde gas and recovery time are no more than 20s；The element is below 3.0 at 150 DEG C of operating temperature, to the sensitivity of interior common the polluted gas carbon monoxide, carbon dioxide, nitrogen dioxide, ammonia, benzene, toluene of 100ppm.
Description
Technical field
The invention belongs to gas sensitive technical fields, and in particular to a kind of PARA FORMALDEHYDE PRILLS(91,95) gas is highly selective, low detection limit
With the gallic acid cadmium nano-powder gas sensitive of quick response.
Background technique
Formaldehyde is a kind of colourless, volatile colourless gas, it has strong impulse effect, energy to the eyes and nose of people
Lead to skin allergy and gene mutation, asthma and uncomfortable can be caused when concentration is lower, is chronically exposed to low concentration formaldehyde
Environment in can cause cancer, when concentration of formaldehyde is higher, it is dead immediately to will lead to people.At 2017, world health group
It knits and formaldehyde is just classified as a kind of carcinogenic substance, China just defined the maximum permissible concentration of formaldehyde in indoor air early in 2001
0.08mg/m3 (59.7ppb) should be not higher than.The method of measurement air formaldehyde concentration mainly uses spectrophotometry at present, electricity
Chemical method and the chromatography of ions etc., these methods need instrument and equipment costly, and sampling analysis needs consume a longer time.Gas
For body sensor due to easy to operate, it is convenient to test, low in cost, and is widely used in the detection of various gases.There is text
It offers and once reports a kind of gallic acid cadmium nanofiber that there is PARA FORMALDEHYDE PRILLS(91,95) highly sensitive and low detection limit cadmium oxide to modify
(Well-Tuned Surface Oxygen Chemistry of Cation Off-Stoichiometric Spinel
Oxides for Highly Selective and Sensitive Formaldehyde Detection[J].Chemistry
Of Materials, 2018,30 (6): 2018-2027.), but the actually detected limit of the material PARA FORMALDEHYDE PRILLS(91,95) is reported in article only
For 100ppb, theoretical detection limit is 20-50ppb, while there are cadmium oxide in the material, the substance be it is a kind of it is poisonous and harmful can
Carcinogenic substance, a small amount of cadmium oxide can cause to seriously endanger to water resource, and simultaneous oxidation cadmium can slow-absorbing in air
Carbon dioxide in air and become cadmium carbonate, lead to material modification.In consideration of it, research and develop it is a kind of safely, effectively, it is stable for
Low concentration formaldehyde has the material of preferable sensitive property to have a very important significance.
Summary of the invention
In order to overcome the deficiencies of the prior art, technical problem to be solved by the invention is to provide one kind for detecting in air
The gas sensitive material of highly selective, the low detection limit and quick response of low concentration formaldehyde gas, can be with base to the material
The interference to detection formaldehyde gas such as this elimination carbon monoxide, carbon dioxide, nitrogen dioxide, ammonia, benzene, toluene, provides one kind
The quickly approach of detection formaldehyde in air gas concentration.
The present invention is achieved by the following technical programs.
The present invention provides a kind of PARA FORMALDEHYDE PRILLS(91,95) gas high sensitivity, the gallic acid cadmium nano powder of low detection limit and quick response
Body gas sensitive, material composition are gallic acid cadmium nano-powders, and the size of powder granule is 40-60 nanometers.
The preparation method and process of above-mentioned gallic acid cadmium nano-powder are: by 0.001 mole of Cd (NO3)2·4H2O and 0.002
Mole Ga (NO3)3·XH2O dissolves in deionized water, and the pH with the NaOH of 2mol/L adjusting solution is respectively 7.00-
11.00；Obtained mixture is filtered, and is washed with deionized water and dehydrated alcohol, the sediment after washing is placed on baking
It is dry in case.Presoma after drying is put into Muffle furnace with the heating rate of 2-4 DEG C/min respectively at 500-900 DEG C
4h is calcined, gallic acid cadmium nano-powder is finally obtained.
Material of the invention can be used as the sensitive material of low concentration formaldehyde gas detecting element, be made using the material other
The method of hot type gas sensor is: slurry is made in 0.2 gram of material and 0.1 gram of terpinol mixed grinding, with small brushes by slurry
It is coated onto the surface of alumina ceramic tube；The size of alumina ceramic tube is: it is 6 millimeters long, 1.6 millimeters of internal diameter, and 2 millimeters of outer diameter,
Alumina tube both ends gold paste electrode is welded with spun gold on electrode as lead, and distance is 1 millimeter between electrode；In alumina tube
Interior placement nichrome wire can control oxygen as heater strip, by controlling the electric current for flowing through heater strip and heater strip both end voltage
Change the operating temperature of aluminum tube surfaces sensitive material；The alumina tube for being coated with sensitive material slurry is placed under infrared lamp and is dried, i.e.,
Obtain heater-type gas sensor.Element to the sensitivity of certain gas be at the working temperature, element in air resistance and member
The ratio of part resistance in tested gas.
Compared with prior art, the present invention has following technical effect that
1, the gallic acid cadmium nano-powder material that the present invention obtains utilizes material production when operating temperature is 150 DEG C
Heater-type gas sensor reaches 50-70 to 100ppm formaldehyde sensitivity, and PARA FORMALDEHYDE PRILLS(91,95) detection limit is down to 0.01ppm, to 0.01ppm
The sensitivity of acetic acid gas reaches 1.2-1.5, and response to 0.01-100ppm formaldehyde gas and recovery time do not surpass respectively
Cross 20s.
2, the obtained gallic acid cadmium nano-powder material of the present invention is at 150 DEG C of operating temperature, to the carbon monoxide of 100ppm,
The sensitivity of carbon dioxide, nitrogen dioxide, ammonia, benzene, toluene is below 3.0.
To sum up, gallic acid cadmium nano-powder gas sensitive PARA FORMALDEHYDE PRILLS(91,95) gas of the present invention has high air-sensitive selectivity, lower detection
Limit and the quickly characteristics such as response.
Detailed description of the invention
Fig. 1 is the SEM photograph of gallic acid cadmium nano-powder prepared by the embodiment of the present invention 3.
Fig. 2 is the TEM photo of gallic acid cadmium nano-powder prepared by the embodiment of the present invention 3.
Specific embodiment
The present invention is described in detail below in conjunction with specific embodiment, but the present invention is not limited to following embodiments.
Embodiment 1
By 0.001 mole of Cd (NO3)2·4H2O and 0.002 mole of Ga (NO3)3·XH2O dissolves in deionized water, uses
The pH that the NaOH of 2mol/L adjusts solution is respectively 7.2；Obtained mixture is filtered, and with deionized water and dehydrated alcohol
Sediment after washing is placed in 80 DEG C of baking ovens dry 12h by washing.Presoma after drying is put into Muffle furnace, 2 DEG C/
The heating rate of min calcines 4h at 500 DEG C respectively, finally obtains gallic acid cadmium nano-powder.
Heater-type element is made in material, measure element under 150 DEG C of operating temperatures to 0.01,0.1,1,10,50,
The maximum sensitivity of 100ppm formaldehyde gas is respectively 1.3,2.5,9.0,25.0,45.0,65.0；To 100ppm carbon monoxide,
The sensitivity of carbon dioxide, nitrogen dioxide, ammonia, benzene, toluene is respectively 1.2,1.1,1.8,2.8,1.7,1.6, element pair
The sensitivity of 100ppm formaldehyde with to the ratio between 100ppm ammonia sensitivity be 23.2, show that material has Gao Ling to low concentration formaldehyde gas
Sensitivity, low detection limit and highly selective；The formaldehyde response time of 0.01-100ppm and recovery time are no more than 20 seconds.
Embodiment 2
By 0.001 mole of Cd (NO3)2·4H2O and 0.002 mole of Ga (NO3)3·XH2O dissolves in deionized water, uses
The pH that the NaOH of 2mol/L adjusts solution is respectively 8.5；Obtained mixture is filtered, and with deionized water and dehydrated alcohol
Sediment after washing is placed in 80 DEG C of baking ovens dry 12h by washing.By the presoma after drying be put into Muffle furnace with 3 DEG C/
The heating rate of min calcines 4h at 600 DEG C respectively, finally obtains gallic acid cadmium nano-powder.
Heater-type element is made in material, measure element under 150 DEG C of operating temperatures to 0.02,0.2,2,10,50,
The maximum sensitivity of 100ppm formaldehyde gas is respectively 1.8,3.0,10.0,23.2,47.2,66.6；To 100ppm carbon monoxide,
The sensitivity of carbon dioxide, nitrogen dioxide, ammonia, benzene, toluene is respectively 1.2,1.3,1.8,2.9,1.1,1.3, element pair
The sensitivity of 100ppm formaldehyde with to the ratio between 100ppm ammonia sensitivity be 23.0, show that material has Gao Ling to low concentration formaldehyde gas
Sensitivity, low detection limit and highly selective；20s is no more than to the acetic acid response time of 0.01-100ppm and recovery time.
Embodiment 3
By 0.001 mole of Cd (NO3)2·4H2O and 0.002 mole of Ga (NO3)3·XH2O dissolves in deionized water, uses
The pH that the NaOH of 2mol/L adjusts solution is respectively 9.6；Obtained mixture is filtered, and with deionized water and dehydrated alcohol
Sediment after washing is placed in 80 DEG C of baking ovens dry 12h by washing.By the presoma after drying be put into Muffle furnace with 4 DEG C/
The heating rate of min calcines 4h at 700 DEG C respectively, finally obtains gallic acid cadmium nano-powder.
Heater-type element is made in material, measure element under 130 DEG C of operating temperatures to 0.01,0.2,0.8,8,45,
The maximum sensitivity of 100ppm formaldehyde gas is respectively 1.8,3.0,8.0,21.2,42.6,66.7；To 100ppm carbon monoxide,
The sensitivity of carbon dioxide, nitrogen dioxide, ammonia, benzene, toluene is respectively 1.2,1.4,1.5,2.7,1.2,1.3, element pair
The sensitivity of 100ppm formaldehyde with to the ratio between 100ppm ammonia sensitivity be 24.7, show that material has Gao Ling to low concentration formaldehyde gas
Sensitivity, low detection limit and highly selective；20s is no more than to the acetic acid response time of 0.01-100ppm and recovery time.
Embodiment 4
By 0.001 mole of Cd (NO3)2·4H2O and 0.002 mole of Ga (NO3)3·XH2O dissolves in deionized water, uses
The pH that the NaOH of 2mol/L adjusts solution is respectively 10.3；Obtained mixture is filtered, and with deionized water and anhydrous second
Sediment after washing is placed in 80 DEG C of baking ovens dry 12h by alcohol washing.Presoma after drying is put into Muffle furnace with 2
DEG C/heating rate of min calcines 4h at 800 DEG C respectively, finally obtain gallic acid cadmium nano-powder.
Heater-type element is made in material, measure element under 130 DEG C of operating temperatures to 0.01,0.1,1,10,50,
The maximum sensitivity of 100ppm formaldehyde gas is respectively 1.5,2.5,7.5,28.0,43.0,70.0；To 100ppm carbon monoxide,
The sensitivity of carbon dioxide, nitrogen dioxide, ammonia, benzene, toluene is respectively 1.9,1.6,1.8,2.8,1.6,2.1, element pair
The sensitivity of 100ppm formaldehyde with to the ratio between 100ppm ammonia sensitivity be 25.0, show that material has Gao Ling to low concentration formaldehyde gas
Sensitivity, low detection limit and highly selective；20s is no more than to the acetic acid response time of 0.01-100ppm and recovery time.
Embodiment 5
By 0.001 mole of Cd (NO3)2·4H2O and 0.002 mole of Ga (NO3)3·XH2O dissolves in deionized water, uses
The pH that the NaOH of 2mol/L adjusts solution is respectively 11.00；Obtained mixture is filtered, and with deionized water and anhydrous second
Sediment after washing is placed in 80 DEG C of baking ovens dry 12h by alcohol washing.Presoma after drying is put into Muffle furnace with 3
DEG C/heating rate of min calcines 4h at 900 DEG C respectively, finally obtain gallic acid cadmium nano-powder.
Heater-type element is made in material, measure element under 130 DEG C of operating temperatures to 0.01,0.1,1,10,50,
The maximum sensitivity of 100ppm formaldehyde gas is respectively 13,2.5,7.5,30.0,40.0,67.0；To 100ppm carbon monoxide, two
The sensitivity of carbonoxide, nitrogen dioxide, ammonia, benzene, toluene is respectively 1.2,1.1,1.5,2.9,1.4,1.2, element pair
The sensitivity of 100ppm formaldehyde with to the ratio between 100ppm ammonia sensitivity be 23.1, show that material has Gao Ling to low concentration formaldehyde gas
Sensitivity, low detection limit and highly selective；20s is no more than to the acetic acid response time of 0.01-100ppm and recovery time.
Claims (4)
1. the gallic acid cadmium nano material of a kind of PARA FORMALDEHYDE PRILLS(91,95) gas highly selective, low detection limit and quick response, which is characterized in that should
Nano material composition is gallic acid cadmium nano-powder, and the size of the nano-powder particle is 40~60 nanometers；The nano material passes through
Co-precipitation and heat-treating methods preparation, specific preparation step is:
(1) by 0.001 mole of Cd (NO3)2·4H2O and 0.002 mole of Ga (NO3)3·9H2O dissolves in deionized water, uses
The NaOH of 2mol/L adjusts the pH to 7.00~11.00 of solution；Obtained mixture is filtered, and with deionized water and anhydrous
Ethanol washing puts the sediment after washing into baking oven dry；
(2) presoma of step (1) after dry is put into Muffle furnace with the heating rate of 2~4 DEG C/min at 500~900 DEG C
Lower calcining 4h finally obtains gallic acid cadmium nano-powder.
2. gallic acid cadmium nano material as described in claim 1, which is characterized in that the pH of solution is 9.6 in the step (1).
3. gallic acid cadmium nano material as described in claim 1, which is characterized in that the calcination temperature in the step (2) is 700
DEG C, heating rate is 4 DEG C.
4. the gas sensor that gallic acid cadmium nano material as described in claim 1 makes as formaldehyde gas sensitive material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112362702A (en) * | 2020-11-13 | 2021-02-12 | 安徽工业大学 | Composite gas-sensitive material with high gas-sensitive selectivity and low detection limit for toluene at room temperature |
| CN113358710A (en) * | 2021-06-03 | 2021-09-07 | 吉林大学 | Olivine structure gas-sensitive material for detecting formaldehyde and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109490376A (en) * | 2018-12-03 | 2019-03-19 | 安徽工业大学 | A kind of graphene-ZnGa that PARA FORMALDEHYDE PRILLS(91,95) gas is highly selective2O4Composite air-sensitive material |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109490376A (en) * | 2018-12-03 | 2019-03-19 | 安徽工业大学 | A kind of graphene-ZnGa that PARA FORMALDEHYDE PRILLS(91,95) gas is highly selective2O4Composite air-sensitive material |
Non-Patent Citations (2)
| Title |
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| 张俊: "石墨烯（量子点）—锌锡氧化物复合材料气敏性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 陈辉: "镓基半导体纳米材料的电子结构调控与性能优化", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112362702A (en) * | 2020-11-13 | 2021-02-12 | 安徽工业大学 | Composite gas-sensitive material with high gas-sensitive selectivity and low detection limit for toluene at room temperature |
| CN113358710A (en) * | 2021-06-03 | 2021-09-07 | 吉林大学 | Olivine structure gas-sensitive material for detecting formaldehyde and preparation method thereof |
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Application publication date: 20190806 |