CN106546650A - A kind of highly sensitive lead ion sensor - Google Patents
A kind of highly sensitive lead ion sensor Download PDFInfo
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- CN106546650A CN106546650A CN201510592917.XA CN201510592917A CN106546650A CN 106546650 A CN106546650 A CN 106546650A CN 201510592917 A CN201510592917 A CN 201510592917A CN 106546650 A CN106546650 A CN 106546650A
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Abstract
The invention discloses in a kind of test solution lead ion simple efficient sensor, manufacturing process mainly includes the following steps that：Prepare certain density graphene oxide solution；Resulting solution blade coating is scratched into into certain thickness on substrate, after being dried, electrode is made on gained sample.This new solid-state devices that the present invention is provided, not only sensitivity and ion selectivity are high, make simple, be easy to mass production, and portability is high, can be widely applied in the testing equipment of heavy metal ion.
Description
Technical field
The present invention relates to environment measuring field, and in particular to a kind of high sensitivity, the making of the graphite oxide thiazolinyl lead ion sensor of process is simple and Detection results.
Background technology
Lead ion is a kind of typical heavy metal ion, in vivo it is difficult to degrade, and top of the mankind in food chain, a lot, once Excess free enthalpy, may result in protein denaturation and cause poisoning, the harm to human body is very big in the lead ion source for touching.Therefore, China's regulation Pb in Drinking Water（Pb）Content must not exceed 0.01mg/L (i.e. 4.826 × 10-8M).Although current many methods that have are detected to lead ion, such as atomic spectroscopy, mass spectrometry, electrochemical methods etc., these methods need to carry out under lab, can not meet the requirement of the ageing and portability of detection of heavy metal ion.The rise of two-dimensional structure material in recent years, provides new thinking to the quick of lead ion, high-sensitivity detection.The present invention relates to a kind of new highly sensitive graphene oxide based sensor, the effective detection range of this sensing material can reach 30nm or so (being approximately 5 times of traditional sensing material), so detection of this sensor to lead ion has very high sensitivity, and be easy to carry, can realize sampling real-time monitoring on the spot in environment measuring.
The content of the invention
It is an object of the invention to utilize the highly dissoluble and long detection range of graphene oxide, a kind of heavy metal ion sensor of new type of high sensitivity is made.This will solve the problems, such as the sensitivity of current heavy metal analysis, ageing and portability.
The technical solution of the present invention is comprised the following steps：
1st, by certain density graphene oxide powder, in appropriate solvent, ultrasonic disperse is uniform;
2nd, scraper height and speed are adjusted, certain thickness graphene oxide solution is scratched in target substrate；
3rd, after Graphene to be oxidized is dried, two-stage spacing is controlled, makes electrode；
4th, the lead ion solution of variable concentrations is detected.
It is an advantage of the invention that having selective and high sensitivity, process is simple well to lead ion, it is easy to mass production, and portability is high, can realize sampling real-time monitoring on the spot in environment measuring.
Description of the drawings
Figure
1
Example
1
Result of detection figure.
Figure
2
Example
2
Result of detection figure.
Figure
3
Example
3
Result of detection figure.
Specific embodiment
1st, by graphene oxide powder in electrical conductivity >=18.25 Ω cm-1Ultrasonic disperse in the mixed solution of deionized water, ethanol or both, prepares the graphene oxide solution of 1-20mg/mL;
2nd, scraper height is adjusted, the graphene oxide solution of 1 μm -4mm of thickness is scratched in target substrate, blade coating speed is 1-20mm/s；
3rd, after Graphene to be oxidized is dried, control two-stage spacing makes electrode in 3-15mm；
4th, the lead ion solution of variable concentrations is detected, tests the detection of device.
Example
1
By graphene oxide powder in electrical conductivity >=18.25 Ω cm-1Ultrasonic disperse in deionized water, prepares the graphene oxide solution of 1mg/mL;Scraper height is adjusted, in printed circuit board（PCB）The graphene oxide solution of upper 1 μm of thickness of blade coating, blade coating speed is 8mm/s；After Graphene to be oxidized is spontaneously dried at room temperature, control two-stage spacing makes electrode in 3mm；Prepare 1 × 10-3M, 1×10-4M, 1×10-5M, 1×10-6M, 1×10-7M, 1×10-8M, 1×10-9Pb (the NO of M3)2Solution；Test the resistance of pure device and same volume variable concentrations Pb (NO are added dropwise3)2The resistance of solution-stabilized rear device.
Experimental result such as Fig. 1, wherein square represents the resistance R of pure device, round dot represents dropwise addition same volume variable concentrations Pb (NO3)2The resistance R ' of device after solution, five-pointed star represent dropwise addition Pb (NO3)2In front and back the rate of change of device resistance, i.e. η=（R-R '）/R.As can be seen from the figure η >=92%, illustrates that device has good Effect on Detecting, and the rate of change of this resistance and Pb (NO to be measured to lead ion3)2The concentration of solution is relevant.
Example
2
By graphene oxide powder in electrical conductivity >=18.25 Ω cm-1Deionized water and alcohol by volume ratio are 1:Ultrasonic disperse in 1 mixed solution, prepares the graphene oxide solution of 20mg/mL;Scraper height is adjusted, graphene oxide solution of the thickness for 2mm is scratched on silicon chip, blade coating speed is 20mm/s；After 50 DEG C of dryings, control two-stage spacing makes electrode in 15mm to Graphene to be oxidized；Prepare 1 × 10-3M, 1×10-4M, 1×10-5M, 1×10-6M, 1×10-7M, 1×10-8M, 1×10-9M, 1×10-10Pb (the NO of M3)2Solution；Test the resistance of pure device and same volume variable concentrations Pb (NO are added dropwise3)2The resistance of solution-stabilized rear device.
Experimental result such as Fig. 2, wherein square represents the resistance R of pure device, round dot represents dropwise addition variable concentrations Pb (NO3)2The resistance R ' of device after solution, five-pointed star represent dropwise addition Pb (NO3)2In front and back the rate of change of device resistance, i.e. η=（R-R '）/R.Even if as can be seen from the figure working as Pb (NO3)2Solution reaches 1 × 10-10During M, η >=94% illustrates that device has good Effect on Detecting, and the rate of change of this resistance and Pb (NO to be measured to lead ion3)2The concentration of solution is relevant.
Example
3
By graphene oxide powder in alcoholic solution ultrasonic disperse, prepare 10mg/mL graphene oxide solution;Scraper height is adjusted, in PET（PET）The graphene oxide solution of upper blade coating thickness 4mm, blade coating speed are 10mm/s；After Graphene to be oxidized is dried at 80 DEG C, control two-stage spacing makes electrode in 10mm；Prepare 1 × 10-3M, 1×10-4M, 1×10-5M, 1×10-6M, 1×10-7M, 1×10-8Pb (the NO of M3)2Solution；Test the resistance of pure device and same volume variable concentrations Pb (NO are added dropwise3)2The resistance of solution-stabilized rear device.
Experimental result such as Fig. 3, wherein square represents the resistance R of pure device, round dot represents dropwise addition variable concentrations Pb (NO3)2The resistance R ' of device after solution, five-pointed star represent dropwise addition Pb (NO3)2In front and back the rate of change of device resistance, i.e. η=（R-R '）/R.As can be seen from the figure η >=92%, illustrates that device has good Effect on Detecting, and the rate of change of this resistance and Pb (NO to be measured to lead ion3)2The concentration of solution is relevant.
Claims (7)
1. a kind of highly sensitive lead ion sensor, it is characterised in that methods described is to be coated in after graphene oxide powder ultrasonic disperse in target substrate, does electrode on graphene oxide sample after being dried, make sensor.
2. high sensitivity graphene oxide based sensor as claimed in claim 1, it is characterised in that detecting concentration<10-8M, resistance change rate>90%.
3. the sensor as described in claim 1 and 2, it is characterised in that to lead ion（Pb2+）There is good Effect on Detecting, and to copper ion（Cu2+）, zinc ion（Zn2+）, bismuth ion（Bi2+）, iron ion（Fe2+）, manganese ion（Mn2+）Deng other responding heavy metal ion very littles（Detecting concentration is 10-3M or so）.
4. the sensor as described in claim 1, it is characterised in that the dispersant of the graphene oxide powder can select the mixed solution of deionized water, ethanol or both, wherein deionization electrical conductivity of water >=18.25 Ω cm-1。
5. the sensor as described in claim 1 and 4, it is characterised in that concentration of the graphene oxide in dispersion liquid is 1-20mg/mL, and blade coating thickness is 1 μm -4mm, and speed 1-20mm/s, drying can be carried out in the range of 20-80 DEG C.
6. the method as described in claim 1-5, it is characterised in that substrate used by device can be printed circuit board（PCB）, silicon chip, the rigid substrate such as sapphire, it is also possible to select PET（PET）, polyvinyl chloride（PVC）Etc. flexible substrate.
7. the method as described in claim 1-6, it is characterised in that in 3-15mm, resistance is 10 for the electrode spacing of the high sensor8-1011Ω。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108318543A (en) * | 2018-01-30 | 2018-07-24 | 河海大学常州校区 | A kind of heavy metal ion sensor and its operating method based on grapheme material |
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| JP2014227304A (en) * | 2013-05-17 | 2014-12-08 | 国立大学法人大阪大学 | Method for producing graphene thin film, electronic element equipped with graphene thin film, sensor, array device and sensing method |
| CN104502412A (en) * | 2014-12-08 | 2015-04-08 | 中国石油大学(华东) | Graphene-based ammonia sensitive material and preparation method thereof |
| CN104569079A (en) * | 2015-01-29 | 2015-04-29 | 重庆墨希科技有限公司 | Graphene nano wall resistance-type humidity sensor and preparation method thereof |
| CN104569052A (en) * | 2014-12-17 | 2015-04-29 | 东南大学 | Method for preparing graphene oxide sensor |
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- 2015-09-17 CN CN201510592917.XA patent/CN106546650A/en active Pending
Patent Citations (4)
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| JP2014227304A (en) * | 2013-05-17 | 2014-12-08 | 国立大学法人大阪大学 | Method for producing graphene thin film, electronic element equipped with graphene thin film, sensor, array device and sensing method |
| CN104502412A (en) * | 2014-12-08 | 2015-04-08 | 中国石油大学(华东) | Graphene-based ammonia sensitive material and preparation method thereof |
| CN104569052A (en) * | 2014-12-17 | 2015-04-29 | 东南大学 | Method for preparing graphene oxide sensor |
| CN104569079A (en) * | 2015-01-29 | 2015-04-29 | 重庆墨希科技有限公司 | Graphene nano wall resistance-type humidity sensor and preparation method thereof |
Non-Patent Citations (1)
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| XUEZHONG GONG ET.AL: "Graphene oxide-based electrochemical sensor：a platform for ultrasensitive detection of heavy metal ions", 《RSC ADVANCES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108318543A (en) * | 2018-01-30 | 2018-07-24 | 河海大学常州校区 | A kind of heavy metal ion sensor and its operating method based on grapheme material |
| CN108318543B (en) * | 2018-01-30 | 2020-12-25 | 河海大学常州校区 | Heavy metal ion sensor based on graphene material and operation method thereof |
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