CN110006978A - A kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water - Google Patents
A kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water Download PDFInfo
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- CN110006978A CN110006978A CN201810010842.3A CN201810010842A CN110006978A CN 110006978 A CN110006978 A CN 110006978A CN 201810010842 A CN201810010842 A CN 201810010842A CN 110006978 A CN110006978 A CN 110006978A
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Abstract
The present invention relates to water quality detection sensor fields, and in particular to a kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water, including interdigital electrode, ion-selective membrane；Ion-selective membrane directly overlays interdigital electrode surface in sensor；The interdigital electrode is that two groups of parallel metal electrod-arrays are staggered to form；Ion-selective membrane selectively reacts with the hypochlorite in water, and converts electric potential signal for chemical signal by sensor.Compared with existing chlorine residue detection method, the present invention is detected using interdigital electrode sensor, and the signal noise ratio of miniature arrays of interdigitated electrodes improves a lot relative to voltage, the current signal of traditional electrode, thus detection accuracy is higher, and be not susceptible to drift about, it can monitor on-line for a long time.Secondly because there is the presence of ion selective membrane, sensor is made to be not easy to be improved the stability and accuracy of sensor by other ion interferences and pollution.
Description
Technical field
The present invention relates to water quality detection sensor fields, and in particular to a kind of to use arrays of interdigitated electrodes and pass through potential
Signal carrys out the microsensor of chlorine residue in quantitative detection water.
Background technique
Chlorine residue is one of the important parameter for measuring water quality, refers to water by chlorination, after contacting a period of time, in water body
The effective chlorine remained.Chlorine residue and existence content in water outlet are accurately measured in real time, for the prison of potable water network system
Residual concentration in survey, the sterilization process monitoring of swimming-pool water quality detection, boiler of power plant control box cooling system and wastewater treatment
Monitoring have important economic and social benefit.
Chlorine residual measurement method is generally divided into chemical analysis, spectrophotometry, ion chromatography method and electricity in water at present
Chemical sensor detection method.DPD spectrophotometry is the standard method of chlorine residue detection, and the colour developing using chemical reagent and chlorine residue is anti-
It answers, measures its absorbance using photoelectric sensor, obtain contents of residual chlorine, but spectrophotometry operation is poor, operation interface is not friendly
It is good, it is not able to satisfy the requirement of on-line monitoring.Oxidation-reduction electrode method in electrochemical sensor detection method is needed in yin, yang electrode
Between apply very low voltage, have electric current flowing in oxidation-reduction process, the stability of voltage when work caused to be difficult to control；
Although " electric current " electrode method does not need to apply any voltage at electrode both ends, but two electrodes are exposed easy by dirt in water
Dye, leads to have biggish difference between detected value and true value.Although recent years, there are many chlorine residue on-line measuring devices to occur,
But its detection method not can avoid the above problem substantially or using traditional electrode detection method.Such as application No. is
201310571788.7, using the residual chlorine sensor in overlay film containing electrolyte solution and three electrode detection heads, detection essence is still
Traditional three-electrode method is so used, accuracy and service life not can guarantee；Application No. is 201511030796.6, devise
A kind of online residual chlorine sensor, structure is complicated, still uses traditional electrode, needs that hydrochloric acid is added in test process to electrode progress clearly
It washes, though test accuracy is promoted, the defect of traditional electrode itself can not be eliminated.
Summary of the invention
In view of the deficienciess of the prior art, the present invention provide a kind of structure it is simple, to chlorine residue ClO-Have it is specific selectivity,
The microsensor of accuracy and high sensitivity, and more than being detected in tap water by converting electric potential signal for chemical signal
Chlorine.
In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention are as follows:
A kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water, the electrode array sensor include one
Interdigital electrode, ion-selective membrane.Ion-selective membrane directly overlays interdigital electrode surface in sensor.
A kind of structure of interdigital electrode sensor are as follows: have two arrays of electrodes on an insulating substrate, two arrays of electrodes is first flat
Row metal electrod-array electrode and the second parallel metal electrod-array electrode, every group of electrode respectively by more 1-100 microns wides,
1-100 micron pitch, 100 microns~5 millimeters long parallel metal electrodes are staggered to form the bipolar electrode structure of pectination；Bipolar electrode knot
One layer of ion-selective membrane is deposited on structure；Bipolar electrode both ends are equipped with pad to connect external circuit.
Preferably, the insulating substrate is glass, oxide, plastics, the insulators such as ceramics.
Preferably, the metal is aluminium, copper, gold, silver, stainless steel etc..
Preferably, the electrode has at least 2 to 1000.
Preferably, first deposited layer protecting film (such as HfO2 hafnium oxide) above electrode prevents electrode by solution corruption
Erosion, redeposited one layer of ion-selective membrane.
Preferably, ion-selective membrane is the mixture of multiple components, including polyethylene ferrocene resin doping
(PVFc), dopant is myristyl benzyl dimethyl ammonium chloride (ZephCl), polyethylene ferrocene resin and polystyrene
(PS), wherein polyethylene ferrocene resin, myristyl benzyl dimethyl ammonium chloride play selectively acting, and polystyrene is mainly auxiliary
Furtherance film；
Preferably, in electrode surface, one layer of very thin coupling agent, such as Hexamethyldisilazane(HMDS are coated) molecule
Layer, the binding force of enhanced film and sensor prevent falling off for film.Interdigital electrode surface is coated with coupling agent layer to increase ion
The surface bonding degree of optional membrane, falls to prevent anti-avulsion；When using electrode with protective layer, coupling agent layer protective layer it
Under upper, ion-selective membrane.
Preferably, coupling agent is adulterated in ion-selective membrane, the binding force of enhanced film and sensor prevents film
It falls off.
Preferably, adulterate plasticizer in ion-selective membrane, the degree of adhesion of enhanced film, prevent film cracking and
It falls off.
Preferably, coupling agent is one kind or several of HMDS, KH792, KH550, KH570, KH580, KH590, KBM602 etc.
The mixture of kind.
Preferably, plasticizer is one or more of mixtures of A608, A618, OP-10, PEG, white oil etc..
Preferably, the proportional region of the multiple component are as follows: PVFc mass fraction: 0.1%-9%；PS mass fraction: 0-3%；
ZephCl mass fraction: 0-3%；The mass fraction of coupling agent: 0-2%；Toughener mass fraction: 0-1%.
Ion-selective membrane can selectively react with the hypochlorite in water, and be believed chemistry by sensor
Number it is converted into electric potential signal, the size of electric potential signal is measured by electrochemical workstation or milivoltmeter.
Preferably, the preparation process of ion-selective membrane is to dissolve the material in solvent in glove box nitrogen atmosphere
After middle stirring, filtering, then by mixed liquor dropwise addition behind the surface of sensor, equal solvent volatilization, drying and forming-film；
Preferably, the solvent is THF(Tetrahydrofuran) tetrahydrofuran, Dimethylformamide (DMF), chlorine
One or more mixed solutions of benzene etc..
Preferably, the drying mode of ion selective membrane is dry in glove box nitrogen atmosphere or using freeze drier
It is freeze-dried or dry using supercritical drying.
Compared with existing chlorine residue detection method, the superior effect of the microsensor of the present invention applied to chlorine residue detection exists
In: it is detected using interdigital electrode sensor, the electric potential signal that chlorine residue generates is mostly derived from the thin of 10 microns of surface
In film layer, the signal noise ratio of miniature arrays of interdigitated electrodes improves a lot relative to voltage, the current signal of traditional electrode,
Detection accuracy is higher, and is not susceptible to drift about, and can monitor on-line for a long time.Secondly because there is depositing for ion selective membrane
Sensor is set to be not easy to be improved the stability and accuracy of sensor by other ion interferences and pollution.Third, sensor
Be it is flat and smooth, be conducive to make stable film；4th, sensor is miniature, and finished product size is generally 3-5mm, can
It is welded with the printed circuit board of standard, forms miniature water quality detection system, system cost reduces, and is more advantageous to and is applied to big rule
The application in the fields such as mould distribution water quality monitoring, such as environment, agricultural, smart home Internet of Things.
Detailed description of the invention
Fig. 1-Fig. 3 is the structural schematic diagram for the interdigital electrode residual chlorine sensor that the present invention is implemented；
Fig. 4 is the test device figure of the residual chlorine sensor of the ion selective membrane that the present invention is implemented and sensor composition；
Fig. 5 is the test result figure of the embodiment 3 of invention；
Fig. 6 is the test result figure of the embodiment 4 of invention；
Fig. 7 is the test result figure of the embodiment 5 of invention.
Specific embodiment
Below according to Figure of description and specific embodiment, technical solution of the present invention is illustrated.
Embodiment 1A
A kind of structure of rectangular interdigital electrode sensor as shown in attached drawing 1-2 are as follows: have two arrays of electrodes in insulating substrate 1 (i.e.
First parallel metal electrod-array electrode 2 and the second parallel metal electrod-array electrode 3), every group of electrode is respectively by more 1-100
Microns wide, 1-100 micron pitch, 100 microns~5 millimeters long parallel metal electrodes 4 are staggered to form the bipolar electrode knot of pectination
Structure；The comb teeth of two arrays of electrodes is mutually inserted in the gap of the adjacent fingers of other side, forms square-shaped electrode；Bipolar electrode structure (i.e. by
Two arrays of electrodes composition structure) on deposit one layer of ion-selective membrane 5；Bipolar electrode both ends respectively have pad 6 to connect external electrical
Road;The length and width range of square-shaped electrode can be 1 to 10 millimeters.
Embodiment 1B
The structure of another round interdigital electrode as shown in Figure 3 are as follows: have two groups 100 microns wide concentric in insulating substrate 1
Circle metal electrode 7, two arrays of electrodes be the first parallel metal electrod-array electrode 2 and the second parallel metal electrod-array electrode 3,
The interlaced formation bipolar electrode structure with 100 microns of lines spacing；The diameter of circular electrode is 1 to 10 millimeters；Bipolar electrode two
Head respectively has pad 6 to connect external circuit；One layer of ion-selective membrane 5 is deposited in bipolar electrode structure.
Embodiment 2
As shown in Fig. 4, ion-selective membrane is by certain chemical bonds in sensor surface；On two electrode of sensor
Two pins are welded with, pin is directly connected with circuit for testing voltage or electrochemical workstation；This sensor is put into
In solution to be measured, occurring with the hypochlorite in solution to be measured for the chemical substance property of can choose in ion-selective membrane is anti-
It answers, directly surveys its potential with milivoltmeter, millivolt circuit or electrochemical workstation.
Embodiment 3
In glove box nitrogen atmosphere, dehydrated alcohol is that solvent dissolves coupling agent and shaking up makes it be uniformly dispersed, spare；Anhydrous second
After alcohol repeatedly embathes electrode sensor, sensor is immersed in the solution of coupling agent (such as HMDS hexamethyldisilazane) 1%
After 8 hours, it is dried for standby；By weight by polystyrene, myristyl benzyl dimethyl ammonium chloride, polyethylene ferrocene resin
It is dissolved in 10mL THF solvent for the proportion of 1:1:1, is A608 by 1% specific gravity addition solvent by plasticizer, stirs evenly
(such as 20 minutes ultrasonic), forms uniform mother liquor；Mother liquor drop is taken to do naturally in ready sensor surface, glove box
It is dry；The sensor for being covered with ion selective membrane is put into containing different hypochlorite ion ClO-Solution electricity is tested in the water of concentration
Gesture is with ClO-The variation of concentration, as shown in Figure 5.
Embodiment 4
In glove box nitrogen atmosphere, dehydrated alcohol is that solvent dissolves coupling agent and shaking up makes it be uniformly dispersed, spare；Anhydrous second
After alcohol repeatedly embathes sensor, sensor was immersed in coupling agent solution after 10 hours, is dried for standby；By polystyrene, ten
It is molten that tetraalkyl dimethyl benzyl ammonium chloride, polyethylene ferrocene resin are that the proportion of 1:1:1 is dissolved in 10mL THF by weight
In agent, stir evenly (such as ultrasound 20 minutes), keep its evenly dispersed mother liquor；Take mother liquor drop in ready sensor sheet
Face is put into freeze-drying 3 hours in freeze drier；The sensor for being covered with ion selective membrane is put into containing different hypochlorous acid
Radical ion ClO-Solution potential is tested in the water of concentration with ClO-The variation of concentration, as shown in Figure 6.
Embodiment 5
Sensor with practical value needs to have chlorine residue ion/molecular to be measured selectivity well, i.e., only to hypochlorous acid
Radical ion has response signal, does not respond to but to main ions other in water.This requirement is selected by intermediate ion of the present invention
Property film is completed.Lower Fig. 7 is the letter that sensor compares a large amount of (1000ppm) other ions to the potential response of hypochlorite ion
Number response, such as Na+、K+、Ca2+、Cl-、SO4 2-、H2PO4 -Deng.As a result surface sensor of the invention is equal to these interfering ions
Nothing obvious responses to, and the selectivity of sensor is good.
Above-described embodiment is only the preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill of the art
For personnel, without departing from the principle of the present invention, several improvement and equivalent replacement can also be made, these are to the present invention
Power require improve with the technical solution after equivalent replacement, each fall within protection scope of the present invention.
Claims (10)
1. a kind of interdigital electrode sensor applied to chlorine residue in quantitative detection water, which is characterized in that the interdigital electrode battle array
Sensor includes interdigital electrode, ion-selective membrane；Ion-selective membrane directly overlays interdigital in sensor
Electrode surface；The interdigital electrode is staggered to form by two groups of parallel metal electrod-arrays；Ion-selective membrane's selectivity
It reacts with the hypochlorite in water, and electric potential signal is converted for chemical signal by sensor.
2. a kind of interdigital electrode sensor applied to chlorine residue in quantitative detection water according to claim 1, feature
It is there is two arrays of electrodes on insulating substrate (1), two arrays of electrodes is that the first parallel metal electrod-array electrode (2) and second are flat
Row metal electrod-array electrode (3), every group of electrode respectively by more 1-100 microns wides, 1-100 micron pitch, 100 microns~
10 millimeters long of parallel metal electrode (4) is staggered to form the bipolar electrode structure of pectination；Leafing choosing is deposited in bipolar electrode structure
Selecting property film (5)；Bipolar electrode both ends are equipped with pad (6) to connect external circuit.
3. a kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water according to claim 1,
It is characterized in that, the protective layer of one layer of water corrosion resistant, redeposited one layer of ion-selective membrane is first deposited on interdigital electrode.
4. a kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water according to claim 1,
It is characterized in that, ion-selective membrane is polyethylene ferrocene resin doping (PVFc), and dopant includes dodecyldimethylamine
Base benzyl ammonium chloride (ZephCl), polyethylene ferrocene resin and polystyrene (PS), wherein polyethylene ferrocene resin, 14
Zephiran plays selectively acting, and polystyrene is for assisting film forming.
5. a kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water according to claim 3,
It is characterized in that, interdigital electrode surface is coated with coupling agent layer to increase the surface bonding degree of ion-selective membrane；Using having
When the electrode of protective layer, coupling agent layer is on protective layer, under ion-selective membrane.
6. a kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water according to claim 1,
It is characterized in that, coupling agent is adulterated in ion-selective membrane.
7. a kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water according to claim 1,
It is characterized in that, plasticizer is adulterated in ion-selective membrane.
8. a kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water according to claim 1,
It being characterized in that, ion-selective membrane in the preparation, in nitrogen atmosphere, dissolves the material in solvent, after stirring, filtering,
Mixed liquor is added dropwise behind the surface of sensor, equal solvent volatilization again, drying and forming-film.
9. a kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water according to claim 1,
It is characterized in that, the drying mode of ion selective membrane is dry in glove box nitrogen atmosphere, or cold using freeze drier progress
It is lyophilized dry or dry using supercritical drying.
10. a kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water according to claim 3,
It is characterized in that, the protective layer is HfO2 hafnium oxide, organic matter or paraffin or their mixture.
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| CN112649573A (en) * | 2020-12-17 | 2021-04-13 | 北京交通大学 | Dual-signal response residual chlorine sensor and preparation method and detection system thereof |
| WO2021231073A1 (en) * | 2020-05-12 | 2021-11-18 | University Of Washington | Apparatus and method for measurement of halogens in samples |
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