CN102980926A - Preparation method of flexible double-faced full-solid ion concentration detection sensor - Google Patents
Preparation method of flexible double-faced full-solid ion concentration detection sensor Download PDFInfo
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Abstract
The invention relates to a preparation method of a flexible double-faced full-solid ion concentration detection sensor and belongs to the technical field of preparation of an electrochemical sensor. The preparation method comprises the following steps of: firstly, machining a flexible substrate by utilizing a flexible material; forming an electrolyte layer on the flexible substrate; respectively forming an ion selectivity film, a reference film and an electrode layer on a surface of a junction part of the flexible substrate and the electrolyte layer; and finally, coating an insulating coating on a naked part on the flexible substrate except the ion selectivity film, the reference film and the electrode layer to form an insulating layer. The detection sensor prepared by the method disclosed by the invention is simple to manufacture, low in cost and strong in stability, and is suitable for large-scale production and manufacturing; and the flexible substrate has the characteristic of easiness of being bent and folded, thus the volume is greatly saved, and the detection sensor is convenient to carry and store.
Description
Technical field
The present invention relates to the preparation method of all solid state ion concentration detecting sensor of a kind of flexible double-sided, belong to the electrochemical sensor preparing technical field.
Background technology
Present stage, the detection of various ions is having a wide range of applications aspect medical science, environmental protection, food, chemical industry, the pharmacy.For example, the heavy metal ion (Zn in the soil
2+, Pb
2+, Cu
2+, Hg
2+) exceed standard after, can produce harm to human body, entail dangers to life is gone back in the impact that is subject to for a long time heavy metal ion; In addition, as potassium ion, sodion etc., be to consist of the indispensable kation of human body fluid, the detection of these ion concentrations has great significance for the medical science aspect.
Ion detection method commonly used mainly contains optical spectroscopy, mass spectroscopy, electrolyte analysis method etc. at present.
Front two kinds of method equipment are huge, expensive, and need complicated pre-service, and the operating personnel that need specialty, and this exists serious drawback aspect portable application.
And the electrolyte analysis method adopts ion-selective electrode and contrast electrode to consist of electrochemical cell, by the relation between ion concentration and the current potential, utilizes the ion concentration in the Nernst equation release solution.But fill electrolyte solution in existing commercial ion-selective electrode and the contrast electrode, this makes it receive great restriction aspect preservation, the transportation; And use complex operation complicated ion-selective electrode and contrast electrode pairing, poor stability can't well provide higher precision; In addition, the various ion-selective electrode of present stage all are the rigidity parallel constructions, can't be crooked, and area occupied is large, can't satisfy portable requirement.
Summary of the invention
The objective of the invention is to propose the preparation method of all solid state ion concentration detecting sensor of a kind of flexible double-sided, make the preparation technology of sensor simple, with low cost, and ion-selective electrode and contrast electrode are integrated in the cavity of pros and cons, to realize the microminiaturization of sensor, be easy to carry.
The preparation method of all solid state ion concentration detecting sensor of flexible double-sided that the present invention proposes may further comprise the steps:
(1) with reeded flexible substrates of both sides tool of flexible material processing;
(2) conducting polymer PEDOT/PSS is mixed according to the ratio of volume ratio 5:1 with dimethyl sulfoxide (DMSO), obtain mixed liquor, mixed liquor is dripped in the groove of flexible substrate, be full of groove after mixed liquor is solidified, obtain dielectric substrate;
(3) with ionophore, lipophilicity macromolecular compound, plastifier and non-conductive polymer polymer mixed, the mass percent of mixing is:
The potpourri that obtains is joined in the organic solvent tetrahydrofuran, the mass percent that adds is: potpourri: organic solvent tetrahydrofuran=1:6, form viscous solution, viscous solution is topped to step (1) and the flexible substrates of step (2) formation and the below of dielectric substrate intersection one side, form ion selective membrane;
(4) with lipophilicity negative ion macromolecular compound, lipophilicity negative ion macromolecular compound, plastifier and non-conductive polymer polymer mixed, the mass percent of mixing is:
The potpourri that obtains is joined in the organic solvent tetrahydrofuran, the mass percent that adds is: potpourri: organic solvent tetrahydrofuran=1:6, form viscous solution, viscous solution is topped to step (1) and the flexible substrates of step (2) formation and the below of dielectric substrate intersection opposite side, form reference film;
(5) flexible substrates that forms in step (1) and step (2) is coated respectively carbon paste with the top of dielectric substrate intersection both sides, the formation electrode layer;
(6) exposed part beyond ion selective membrane, reference film and electrode layer on the flexible substrates that step (2) forms applies coatings, forms insulation course.
Among the above-mentioned preparation method, described flexible material is any in dimethyl silicone polymer, polyurethane or the silica gel.
Among the above-mentioned preparation method, described ionophore is corresponding with the kind of detected ion.
Among the above-mentioned preparation method, described lipophilicity negative ion macromolecular compound is tetraphenylboron sodium, tetrachlorobenzene potassium borate or four [3,5-two (trifluoromethyl) phenyl] any in the potassium borate, and the lipophilic cation macromolecular compound is three (dodecyl) ammonio methacrylate.
Among the above-mentioned preparation method, described plastifier is any in decanedioic acid dibutylester, hexane diacid dibutyl ester or the decanedioic acid di-sec-octyl.
Among the above-mentioned preparation method, described non-conductive polymer polymkeric substance is any in Polyvinylchloride (PVC), polyurethane (PU) or the polymethyl methacrylate (PMMA).
The preparation method of all solid state ion concentration detecting sensor of flexible double-sided that the present invention proposes, its advantage is:
1, the ion concentration detecting sensor of the inventive method preparation, can be maximum utilize Substrate Area, the double integrated level that improves ion transducer.
2, the ion concentration detecting sensor of the inventive method preparation adopts structure of whole solid state, has thoroughly changed the idea of filling electrolyte solution in conventional ion electrodes selective and the contrast electrode needs, the sensor of preparation is easy to carry, storage and transport.
3, the ion concentration detecting sensor of the inventive method preparation, flexible substrate wherein can fold, improved to a certain extent the ability that sensor adapts to varying environment, and ion selective membrane and reference film and substrate there is better adhesive capacity, guaranteed the reliability of working sensor.
4, transducer production method of the present invention, manufacturing process is simple, and preparation cost is cheap, and the sensor stability of preparation is strong, and is low to preparation technology's precision prescribed, is fit to produce in enormous quantities.
Description of drawings
Fig. 1 is the cut-open view of the flexible substrates for preparing among the preparation method of the present invention.
Fig. 2 fills the cut-open view that mixed liquor obtains dielectric substrate in the groove of flexible substrates shown in Figure 1.
Fig. 3 is at dielectric substrate difference topped ion selective membrane, reference film and the later cut-open view of electrode layer shown in Figure 2.
Fig. 4 is that the exposed part beyond deionization selective membrane, reference film and the electrode layer applies coatings on dielectric substrate shown in Figure 3, forms the cut-open view of insulation course.
Fig. 5 is the front elevation of the sensor of the inventive method preparation.
Fig. 6 is the potential response curves of embodiments of the invention 1 in the KCL of variable concentrations solution.
Fig. 7 potential response curve in the KCL of variable concentrations solution that is embodiments of the invention 1 after folding.
Among Fig. 1-Fig. 4, the 1st, flexible substrates, the 2nd, dielectric substrate, the 3rd, ion selective membrane, the 4th, reference film, the 5th, electrode layer, the 6th, insulation course.
Embodiment
The preparation method of all solid state ion concentration detecting sensor of flexible double-sided that the present invention proposes may further comprise the steps:
(1) with reeded flexible substrates 1 of both sides tool of flexible material processing, as shown in Figure 1.
(2) conducting polymer PEDOT/PSS is mixed according to the ratio of volume ratio 5:1 with dimethyl sulfoxide (DMSO), obtain mixed liquor, mixed liquor is dripped in the groove of flexible substrate, be full of groove after mixed liquor is solidified, obtain dielectric substrate 2, as shown in Figure 2.
(3) with ionophore, lipophilicity macromolecular compound, plastifier and non-conductive polymer polymer mixed, the mass percent of mixing is:
The potpourri that obtains is joined in the organic solvent tetrahydrofuran, the mass percent that adds is: potpourri: organic solvent tetrahydrofuran=1:6, form viscous solution, viscous solution is topped to step (1) and the flexible substrates of step (2) formation and the below of dielectric substrate intersection one side, form ion selective membrane 3, as shown in Figure 3.
(4) with lipophilicity negative ion macromolecular compound, lipophilicity negative ion macromolecular compound, plastifier and non-conductive polymer polymer mixed, the mass percent of mixing is:
The potpourri that obtains is joined in the organic solvent tetrahydrofuran, the mass percent that adds is: potpourri: organic solvent tetrahydrofuran=1:6, form viscous solution, viscous solution is topped to step (1) and the flexible substrates of step (2) formation and the below of dielectric substrate intersection opposite side, form reference film 4, as shown in Figure 3.
(5) flexible substrates that forms in step (1) and step (2) is coated respectively carbon paste with the top of dielectric substrate intersection both sides, formation electrode layer 5, as shown in Figure 3.
(6) exposed part beyond ion selective membrane, reference film and electrode layer on the flexible substrates that step (2) forms applies coatings, forms insulation course 6, as shown in Figure 4 and Figure 5.
Among the above-mentioned preparation method, described flexible material is any in dimethyl silicone polymer, polyurethane or the silica gel.
Among the above-mentioned preparation method, described ionophore is corresponding with the kind of detected ion.
Among the above-mentioned preparation method, described lipophilicity negative ion macromolecular compound is tetraphenylboron sodium, tetrachlorobenzene potassium borate or four [3,5-two (trifluoromethyl) phenyl] any in the potassium borate, and the lipophilic cation macromolecular compound is three (dodecyl) ammonio methacrylate.
Among the above-mentioned preparation method, described plastifier is any in decanedioic acid dibutylester, hexane diacid dibutyl ester or the decanedioic acid di-sec-octyl.
Among the above-mentioned preparation method, described non-conductive polymer polymkeric substance is any in Polyvinylchloride (PVC), polyurethane (PU) or the polymethyl methacrylate (PMMA).
When using the present invention to prepare all solid state ion concentration detecting sensor measurement of flexible double-sided, the electrode bottom is immersed in the solution to be measured, ion selective membrane and reference film contact concurrent looks with solution to be measured respectively and should react, ionophore in the ion selective membrane can with solution to be measured in corresponding ion ion complexation, thereby change the current potential of ion selective membrane.And the conducting polymer current potential under the reference film can keep constant, so two electrodes of electrode layer can pick out potential change by external lead wire.According to Nernst equation, can from potential change, read the ion concentration in the solution.
Among the preparation method of the present invention, the conducting polymer PEDOT/PSS of use is provided by Heraeus Inc., and product type is PH1000; Valinomycins, tetrachlorobenzene potassium borate, three (dodecyl) ammonio methacrylate, decanedioic acid dibutylester, Polyvinylchloride (PVC) are provided by Sigma aldrich company.
Utilize the inventive method can prepare the sensor that detects different kinds of ions concentration, for example, potassium concentration sensor, Na ion concentration sensor, calcium ion concentration sensor, magnesium ion concentration sensor, ion concentration of mercury sensor etc.
Below introduce preparation method's of the present invention embodiment:
Sensor for the preparation of the detection potassium concentration:
(1) with reeded flexible substrates of both sides tool of dimethyl silicone polymer processing, as shown in Figure 1;
(2) conducting polymer PEDOT/PSS is mixed according to the ratio of volume ratio 5:1 with dimethyl sulfoxide (DMSO), obtain mixed liquor, mixed liquor is dripped in the groove of flexible substrate, be full of groove after mixed liquor is solidified, obtain dielectric substrate, as shown in Figure 2;
(3) 3mg valinomycins, 1mg tetrachlorobenzene potassium borate, 60ul decanedioic acid dibutylester and 36mg Polyvinylchloride (PVC) are mixed,
The potpourri that obtains is joined in the 600ul organic solvent tetrahydrofuran, mix, form viscous solution, viscous solution is topped to step (1) and the flexible substrates of step (2) formation and the below of dielectric substrate intersection one side, form ion selective membrane;
(4) 1mg tetrachlorobenzene potassium borate, 1mg three (dodecyl) ammonio methacrylate, 60ml decanedioic acid dibutylester and 38mg Polyvinylchloride are mixed, the potpourri that obtains is joined in the 600ml tetrahydrofuran, form viscous solution, viscous solution is topped to step (1) and the flexible substrates of step (2) formation and the below of dielectric substrate intersection opposite side, form reference film;
(5) flexible substrates that forms in step (1) and step (2) is coated respectively carbon paste with the top of dielectric substrate intersection both sides, the formation electrode layer, as shown in Figure 3;
(6) the exposed part coated with paraffin beyond ion selective membrane, reference film and electrode layer on the flexible substrates that step (2) forms, form insulation course, as shown in Figure 4, namely obtained can be used for detecting the two-sided full-solid-state minisize ion concentration detecting sensor based on flexible substrate of potassium concentration, as shown in Figure 5.
The sensor of preparation is immersed in 0.0001mol/L, 0.001mol/L, 0.01mol/L, 0.1mol/L, in the solution to be measured of 1mol/L, the potential response curve that obtains satisfies the log-linear relation as shown in Figure 6.With folding 100 times of ion electrode, again be immersed in the solution to be measured, the potential response curve that obtains as can be seen from the figure, on not impact of sensor performance, illustrates that its job stability is good as shown in Figure 7 substantially.
Sensor for the preparation of the detection potassium concentration:
(1) with reeded flexible substrates of both sides tool of polyurethane processing;
(2) conducting polymer PEDOT/PSS is mixed according to the ratio of volume ratio 5:1 with dimethyl sulfoxide (DMSO), obtain mixed liquor, mixed liquor is dripped in the groove of flexible substrate, be full of groove after mixed liquor is solidified, obtain dielectric substrate;
(3) 40mg valinomycins, 15mg tetraphenylboron sodium, 700ul hexane diacid dibutyl ester and 345mg polymethyl methacrylate are mixed, the potpourri that obtains is joined in the 6.6ml organic solvent tetrahydrofuran, mix, form viscous solution, viscous solution is topped to step (1) and the flexible substrates of step (2) formation and the below of dielectric substrate intersection one side, form ion selective membrane;
(4) 20mg tetraphenylboron sodium, 20mg three (dodecyl) ammonio methacrylate, 700ul hexane diacid dibutyl ester and 360mg polymethyl methacrylate are mixed, the potpourri that obtains is joined in the 6ml tetrahydrofuran, form viscous solution, viscous solution is topped to step (1) and the flexible substrates of step (2) formation and the below of dielectric substrate intersection opposite side, form reference film;
(5) flexible substrates that forms in step (1) and step (2) is coated respectively carbon paste with the top of dielectric substrate intersection both sides, the formation electrode layer, as shown in Figure 3;
(6) the exposed part coated with paraffin beyond ion selective membrane, reference film and electrode layer on the flexible substrates that step (2) forms, form insulation course, as shown in Figure 4, obtain can be used for detecting the two-sided full-solid-state minisize ion concentration detecting sensor based on flexible substrate of potassium concentration.
Sensor for the preparation of the detection potassium concentration:
(1) with reeded flexible substrates of both sides tool of silica gel processing;
(2) conducting polymer PEDOT/PSS is mixed according to the ratio of volume ratio 5:1 with dimethyl sulfoxide (DMSO), obtain mixed liquor, mixed liquor is dripped in the groove of flexible substrate, be full of groove after mixed liquor is solidified, obtain dielectric substrate;
(3) with 5mg valinomycins, 2mg four [3,5-two (trifluoromethyl) phenyl] potassium borate, 65ul decanedioic acid di-sec-octyl and 28mg polyurethane mixes, the potpourri that obtains is joined in the 600ul organic solvent tetrahydrofuran, mix, form viscous solution, viscous solution is topped to step (1) and the flexible substrates of step (2) formation and the below of dielectric substrate intersection one side, form ion selective membrane;
(4) with 3mg four [3,5-two (trifluoromethyl) phenyl] potassium borate, 3mg three (dodecyl) ammonio methacrylate, 65ul decanedioic acid di-sec-octyl and 29mg polyurethane mixes, the potpourri that obtains is joined in the 600ul tetrahydrofuran, form viscous solution, viscous solution is topped to step (1) and the flexible substrates of step (2) formation and the below of dielectric substrate intersection opposite side, form reference film;
(5) flexible substrates that forms in step (1) and step (2) is coated respectively carbon paste with the top of dielectric substrate intersection both sides, the formation electrode layer, as shown in Figure 3;
(6) the exposed part coated with paraffin beyond ion selective membrane, reference film and electrode layer on the flexible substrates that step (2) forms, form insulation course, as shown in Figure 4, namely obtain can be used for detecting the two-sided full-solid-state minisize ion concentration detecting sensor based on flexible substrate of potassium concentration.
Claims (6)
1. the preparation method of all solid state ion concentration detecting sensor of flexible double-sided is characterized in that the method may further comprise the steps:
(1) with reeded flexible substrates of both sides tool of flexible material processing;
(2) conducting polymer PEDOT/PSS is mixed according to the ratio of volume ratio 5:1 with dimethyl sulfoxide (DMSO), obtain mixed liquor, mixed liquor is dripped in the groove of flexible substrate, be full of groove after mixed liquor is solidified, obtain dielectric substrate;
(3) with ionophore, lipophilicity macromolecular compound, plastifier and non-conductive polymer polymer mixed, the mass percent of mixing is:
The potpourri that obtains is joined in the organic solvent tetrahydrofuran, the mass percent that adds is: potpourri: organic solvent tetrahydrofuran=1:6, form viscous solution, viscous solution is topped to step (1) and the flexible substrates of step (2) formation and the below of dielectric substrate intersection one side, form ion selective membrane;
(4) with lipophilicity negative ion macromolecular compound, lipophilicity negative ion macromolecular compound, plastifier and non-conductive polymer polymer mixed, the mass percent of mixing is:
The potpourri that obtains is joined in the organic solvent tetrahydrofuran, the mass percent that adds is: potpourri: organic solvent tetrahydrofuran=1:6, form viscous solution, viscous solution is topped to step (1) and the flexible substrates of step (2) formation and the below of dielectric substrate intersection opposite side, form reference film;
(5) flexible substrates that forms in step (1) and step (2) is coated respectively carbon paste with the top of dielectric substrate intersection both sides, the formation electrode layer;
(6) exposed part beyond ion selective membrane, reference film and electrode layer on the flexible substrates that step (2) forms applies coatings, forms insulation course.
2. preparation method as claimed in claim 1 is characterized in that wherein said flexible material is any in dimethyl silicone polymer, polyurethane or the silica gel.
3. preparation method as claimed in claim 1 is characterized in that wherein said ionophore is corresponding with the kind of detected ion.
4. preparation method as claimed in claim 1, it is characterized in that wherein said lipophilicity negative ion macromolecular compound is tetraphenylboron sodium, tetrachlorobenzene potassium borate or four [3,5-two (trifluoromethyl) phenyl] any in the potassium borate, and the lipophilic cation macromolecular compound is three (dodecyl) ammonio methacrylate.
5. preparation method as claimed in claim 1 is characterized in that wherein said plastifier is any in decanedioic acid dibutylester, hexane diacid dibutyl ester or the decanedioic acid di-sec-octyl.
6. preparation method as claimed in claim 1 is characterized in that wherein said non-conductive polymer polymkeric substance is any in Polyvinylchloride, polyurethane or the polymethyl methacrylate.
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| CN108120751A (en) * | 2017-12-20 | 2018-06-05 | 南京航空航天大学 | A kind of all solid state PH sensor |
| CN108398474A (en) * | 2018-02-13 | 2018-08-14 | 中国科学院烟台海岸带研究所 | It is a kind of to can be used for the electric potential type microelectrode sensors and its application that deposit intermediate ion detects |
| CN110658243A (en) * | 2019-09-10 | 2020-01-07 | 华东师范大学 | Flexible ion detection sensor, preparation method and application |
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| CN106018524A (en) * | 2016-05-20 | 2016-10-12 | 浙江刚竹网络科技有限公司 | High-sensitivity nitrite ion electrode based on poly(3,4-ethylenedioxythiophene) and preparation method thereof |
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| WO2022102649A1 (en) * | 2020-11-12 | 2022-05-19 | オムロンヘルスケア株式会社 | Electrolyte analysis test strip and electrolyte analysis device |
| CN114252491A (en) * | 2021-12-07 | 2022-03-29 | 中国科学院海洋研究所 | Marine steel corrosion hydrogen permeation monitoring sensor and monitoring method in ocean tidal range area |
| CN115211995A (en) * | 2022-07-18 | 2022-10-21 | 天津大学 | Flexible intelligent sensing tooth socket |
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