CN110146563A - It is a kind of based on Prussian blue no enzymuria acid sensor - Google Patents
It is a kind of based on Prussian blue no enzymuria acid sensor Download PDFInfo
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- CN110146563A CN110146563A CN201811539838.2A CN201811539838A CN110146563A CN 110146563 A CN110146563 A CN 110146563A CN 201811539838 A CN201811539838 A CN 201811539838A CN 110146563 A CN110146563 A CN 110146563A
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- prussian blue
- electrode
- enzymuria
- carbon slurry
- acid sensor
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- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 title claims abstract description 163
- 239000013225 prussian blue Substances 0.000 title claims abstract description 163
- 229960003351 prussian blue Drugs 0.000 title claims abstract description 163
- 239000002253 acid Substances 0.000 title claims abstract description 77
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 137
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 137
- 239000002002 slurry Substances 0.000 claims abstract description 69
- 239000000758 substrate Substances 0.000 claims abstract description 45
- 238000007581 slurry coating method Methods 0.000 claims abstract description 39
- 238000000576 coating method Methods 0.000 claims abstract description 29
- 239000004020 conductor Substances 0.000 claims abstract description 29
- 239000011248 coating agent Substances 0.000 claims abstract description 28
- AILDTIZEPVHXBF-UHFFFAOYSA-N Argentine Natural products C1C(C2)C3=CC=CC(=O)N3CC1CN2C(=O)N1CC(C=2N(C(=O)C=CC=2)C2)CC2C1 AILDTIZEPVHXBF-UHFFFAOYSA-N 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 20
- 235000016594 Potentilla anserina Nutrition 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims description 23
- 229920002472 Starch Polymers 0.000 claims description 20
- 235000019698 starch Nutrition 0.000 claims description 20
- 239000012528 membrane Substances 0.000 claims description 19
- 244000308495 Potentilla anserina Species 0.000 claims description 18
- 241001062009 Indigofera Species 0.000 claims description 15
- 230000010355 oscillation Effects 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000005611 electricity Effects 0.000 claims description 4
- 238000009738 saturating Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 23
- 239000006255 coating slurry Substances 0.000 abstract description 3
- 241000412565 Argentina sphyraena Species 0.000 abstract 2
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 description 46
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 description 46
- 229940116269 uric acid Drugs 0.000 description 46
- 238000001035 drying Methods 0.000 description 27
- 239000000853 adhesive Substances 0.000 description 26
- 230000001070 adhesive effect Effects 0.000 description 26
- 239000003960 organic solvent Substances 0.000 description 25
- 230000000052 comparative effect Effects 0.000 description 19
- 239000003822 epoxy resin Substances 0.000 description 18
- 229920000647 polyepoxide Polymers 0.000 description 18
- 239000002390 adhesive tape Substances 0.000 description 16
- 238000000034 method Methods 0.000 description 14
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 13
- 239000004332 silver Substances 0.000 description 13
- 229910052709 silver Inorganic materials 0.000 description 13
- 239000008107 starch Substances 0.000 description 13
- 238000005660 chlorination reaction Methods 0.000 description 9
- 238000007639 printing Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 238000004090 dissolution Methods 0.000 description 8
- 239000003292 glue Substances 0.000 description 8
- 108090000790 Enzymes Proteins 0.000 description 7
- 102000004190 Enzymes Human genes 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- 239000002114 nanocomposite Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 230000002485 urinary effect Effects 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 240000001973 Ficus microcarpa Species 0.000 description 1
- 108010092464 Urate Oxidase Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000009144 enzymatic modification Effects 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
Classifications
-
- 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
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
The present invention provides that a kind of detection accuracy is high, speed is fast, performance is stable based on Prussian blue no enzymuria acid sensor.This is without enzymuria acid sensor, and including the substrate, conductor layer and electrode layer successively to splice, electrode layer includes to electrode and working electrode, and working electrode is the Prussian blue carbon slurry coating on substrate, and Prussian blue carbon slurry is mixed by prussian blue powder and carbon slurry.There is respective electrode terminal to electrode and working electrode, pass through the first conducting wire respectively to electrode and working electrode to connect with respective electrode terminal, electrode terminal and the first conducting wire are respectively positioned on conductor layer, and the first conducting wire includes argentine chloride coating and the Prussian blue carbon being covered on argentine chloride coating slurry coating.
Description
Technical field
The present invention relates to electrochemical fields, more particularly to a kind of based on Prussian blue no enzymuria acid sensor.
Background technique
Following background technique is used to help reader and understands the present invention, and is not construed as the prior art.
The testing principle of electrode is to pass through enzymatic reaction on enzyme modification to working electrode corresponding to substrate mostly at present
Measure electric signal, therefore uric acid sensor generally uses urinary acidification.But the rigid condition of enzyme on the working electrode (s compares
Harshness needs to keep in immobilization process the activity of enzyme unaffected, and temperature and humidity requires to consider when enzyme is fixed.This
Outside, the price of uricase is generally all more expensive, limits its use scope, increases the production cost of electrode test piece.It is general
Shandong scholar's indigo plant have excellent electrochemical reversibility, stability, with Prussian blue preparation can be effective without enzyme type uric acid sensor
The various drawbacks for avoiding urinary acidification from detecting.
Chinese patent 201510605173.0 disclose a kind of Prussian blue/N- doping carbon nano-composite material preparation and
Using, take 2 μ L it is Prussian blue/working electrode in screen printing electrode is added dropwise in N- doped carbon Nanocomposite solution
On, room temperature is dried;Add dehydrated alcohol dilute solution on the surface that material was added dropwise after drying, up to no enzyme type uric acid biography after drying
Sensor.The shortcomings that patent, is: 1, needing to form working electrode first on substrate, then coats general Shandong on the working electrode (s
Scholar's indigo plant/N- adulterates carbon nano-composite material, complex process;And Prussian blue/N- doping carbon nano-composite material is easy from work
It falls off as electrode surface, leads to the failure of electrode slice.2, the preparation step of Prussian blue/N- doping carbon nano-composite material is multiple
It is miscellaneous, increase production cost.
Summary of the invention
The purpose of the present invention is to provide a kind of detection accuracy height, speed is fast, performance is stable based on Prussian blue nothing
Enzymuria acid sensor.
It is industrial based on Prussian blue no enzymuria suitable for high-volume that the object of the invention is also to provide a kind of
The preparation method of acid sensor.
It is a kind of based on Prussian blue no enzymuria acid sensor, including the substrate, conductor layer and electrode layer successively to splice, electricity
Pole layer includes to electrode and working electrode, and working electrode is starched with Prussian blue carbon, and Prussian blue carbon slurry is by prussian blue powder
It is mixed with carbon slurry.Preferably, the mixture that electrode is silver coating, argentine chloride coating or silver and silver chlorate on substrate is applied
Layer.
Further, working electrode is the Prussian blue carbon slurry coating on substrate;Alternatively, working electrode includes being printed on substrate
On carbon starch coating, have Prussian blue carbon slurry coating on carbon slurry coating.
Further, mass fraction Prussian blue in Prussian blue carbon slurry is 0.5%~5%.
Further, there is respective electrode terminal to electrode and working electrode, the is passed through respectively to electrode and working electrode
One conducting wire is connect with respective electrode terminal, and electrode terminal and the first conducting wire are respectively positioned on conductor layer, and the first conducting wire includes silver chlorate
Coating and the Prussian blue carbon being covered on argentine chloride coating starch coating.Argentine chloride coating is clipped in substrate and Prussian blue carbon slurry applies
Between layer.Preferably, electrode terminal is printed on substrate by chlorination silver paste and is formed.
Further, conductor layer includes two recognition terminals and the second conducting wire for connecting two recognition terminals, identifies end
Son and the second conducting wire include argentine chloride coating and the Prussian blue carbon being covered on argentine chloride coating slurry coating.
Further, this further includes the insulating layer successively to splice, layers of two-sided and hydrophilic membrane, insulation without enzymuria acid sensor
Stacking is connected on electrode layer, and insulating layer and layers of two-sided are all provided with jagged, and notch intersects with to electrode and working electrode, base
Plate, insulating layer notch, layers of two-sided notch and hydrophilic membrane are collectively formed for sample to be tested to be drained to working electrode and right
The siphon passage of electrode.Preferably, insulating layer notch and layers of two-sided notch are overlapped.Preferably, the shape of notch be rectangle,
Square, ellipse or round.Preferably, insulating layer is prepared by hydrophobic material.For example, insulating layer can be with dissolved with
The organic solvent of epoxy resin prints.
Further, hydrophilic membrane has air hole, and air hole is provided at the through-hole on hydrophilic membrane, and air hole and siphon are logical
Road is connected close to one end of substrate center.
Further, Prussian blue carbon slurry is Prussia's blue powder to be added in carbon slurry, stir 200~500 with machine mixer
Turn, the slurry that 10~60min is formed then is stirred by ultrasonic with ultrasonic oscillation instrument.Preferably, machine mixer stirs 300 turns,
Then 30min is stirred by ultrasonic with ultrasonic oscillation instrument.
A kind of the case where working electrode is Prussian blue carbon slurry coating: system based on Prussian blue no enzymuria acid sensor
Preparation Method, successively the following steps are included:
1) prussian blue powder, which is added in carbon slurry, is mixed, prepares Prussian blue carbon slurry, general Shandong in Prussian blue carbon slurry
The mass fraction of scholar's indigo plant is 0.5%~5%;
2) it prints Prussian blue carbon on substrate to starch to form Prussian blue carbon slurry coating, Prussian blue carbon slurry coating is as work
Make electrode;
3) it dries, drying temperature is 80 DEG C~100 DEG C, and drying time is 8~15min.
In some cases, step 2) is substituted for: Prussian blue carbon is added dropwise on substrate and starches to form Prussian blue carbon slurry
Coating, Prussian blue carbon slurry coating is as working electrode.
Further, after the step 3) also successively the following steps are included:
4) it in organic solvent by epoxy resin dissolution, is printed on electrode layer with the organic solvent dissolved with epoxy resin absolutely
Edge layer dries, organic solvent is made to volatilize, and insulating layer has the notch intersected with to electrode and working electrode;
5) notch is made on double-sided adhesive, on the insulating layer by sticking double faced adhesive tape, sticking double faced adhesive tape in insulating layer, it is two-sided
Glue notch is overlapped with insulating layer notch, double-sided adhesive with a thickness of 0.1~0.2mm;
6) hydrophilic membrane is covered on double-sided adhesive.
Working electrode includes the case where carbon slurry coating and Prussian blue carbon slurry coating: a kind of based on Prussian blue no enzymuria
The preparation method of acid sensor, successively the following steps are included:
1) carbon is printed on substrate to starch to form carbon slurry coating, drying;
2) prussian blue powder, which is added in carbon slurry, is mixed, prepares Prussian blue carbon slurry, general Shandong in Prussian blue carbon slurry
The mass fraction of scholar's indigo plant is 0.5%~5%;
3) Prussian blue carbon is printed on carbon slurry coating to starch to form Prussian blue carbon slurry coating;
4) it dries, drying temperature is 80 DEG C~100 DEG C, and drying time is 8~15min.
In some cases, step 3) is substituted for: carbon slurry coating on be added dropwise Prussian blue carbon starch to be formed it is Prussian blue
Carbon starches coating.
Further, after the step 4) also successively the following steps are included:
5) it in organic solvent by epoxy resin dissolution, is printed on electrode layer with the organic solvent dissolved with epoxy resin absolutely
Edge layer dries, organic solvent is made to volatilize, and insulating layer has the notch intersected with to electrode and working electrode;
6) notch is made on double-sided adhesive, on the insulating layer by sticking double faced adhesive tape, sticking double faced adhesive tape in insulating layer, it is two-sided
Glue notch is overlapped with insulating layer notch, double-sided adhesive with a thickness of 0.1~0.2mm;
7) hydrophilic membrane is covered on double-sided adhesive.
Further, substrate is placed in pure water before step 1) and is cleaned by ultrasonic, dries.
Beneficial effects of the present invention:
1, the Prussian blue mass fraction in Prussian blue carbon slurry is 0.5%~5%, realizes detecting without enzyme for uric acid, and
And sensor detection signal is strong, performance is stable, high sensitivity, accuracy is high, detection speed is fast, uric acid concentration model that can be detected
It encloses big.
2, the Prussian blue carbon slurry coating on substrate can directly form working electrode, and preparation process is simple, save the cost.
3, the first conducting wire of conductor layer, the second conducting wire and recognition terminal include that argentine chloride coating and Prussian blue carbon slurry apply
Layer, double coatings can preferably avoid argentine chloride coating width is smaller, conducting wire be easy open circuit problem;And work is prepared in printing
When making electrode, only need to improve printing stencil;It is needed when preparation work electrode, only in a manner of being added dropwise corresponding in conductor layer
Prussian blue carbon slurry is added dropwise in region, and Prussian blue carbon slurry coating can be made to be covered on conductor layer while preparation work electrode
On argentine chloride coating, simple process.
4, Prussian blue carbon slurry is printed on preparation work electrode on substrate, is suitable for large-scale industrial production, the work of preparation
It is uniform, not easily to fall off to make thickness of electrode, either liquid wash or foreign object friction will not all have an impact working electrode.
Detailed description of the invention
Fig. 1 is the appearance diagram without enzymuria acid sensor in one embodiment of the invention.
Fig. 2 is substrate without enzymuria acid sensor in one embodiment of the invention, conductor layer, electrode layer, insulating layer, two-sided
The schematic diagram of glue-line and hydrophilic membrane.
Fig. 3 is in the embodiment of the present invention 1 without the time current curve under enzymuria acid sensor difference uric acid concentration.
Fig. 4 is uric acid concentration-electric current Linear Fit Chart in the embodiment of the present invention 1 without enzymuria acid sensor.
Fig. 5 be in the embodiment of the present invention 2 without enzymuria acid sensor in various concentration uric acid solution cyclic voltammogram.
Fig. 6 is in the embodiment of the present invention 2 without the time current curve under enzymuria acid sensor difference uric acid concentration.
Fig. 7 is uric acid concentration-electric current Linear Fit Chart in the embodiment of the present invention 2 without enzymuria acid sensor.
Fig. 8 is in the embodiment of the present invention 3 without the time current curve under enzymuria acid sensor difference uric acid concentration.
Fig. 9 is uric acid concentration-electric current Linear Fit Chart in the embodiment of the present invention 3 without enzymuria acid sensor.
Figure 10 is in the embodiment of the present invention 4 without the time current curve under enzymuria acid sensor difference uric acid concentration.
Figure 11 is uric acid concentration-electric current Linear Fit Chart in the embodiment of the present invention 4 without enzymuria acid sensor.
Figure 12 is in the embodiment of the present invention 5 without the time current curve under enzymuria acid sensor difference uric acid concentration.
Figure 13 is uric acid concentration-electric current Linear Fit Chart in the embodiment of the present invention 5 without enzymuria acid sensor.
Figure 14 is in the embodiment of the present invention 6 without the time current curve under enzymuria acid sensor difference uric acid concentration.
Figure 15 is uric acid concentration-electric current Linear Fit Chart in the embodiment of the present invention 6 without enzymuria acid sensor.
Figure 16 is in comparative example 1 of the present invention without the time current curve under enzymuria acid sensor difference uric acid concentration.
Figure 17 is uric acid concentration-electric current Linear Fit Chart in comparative example 1 of the present invention without enzymuria acid sensor.
Figure 18 is in comparative example 2 of the present invention without the time current curve under enzymuria acid sensor difference uric acid concentration.
Figure 19 is uric acid concentration-electric current Linear Fit Chart in comparative example 2 of the present invention without enzymuria acid sensor.
Specific embodiment
The present invention is further described in detail combined with specific embodiments below.
Embodiment 1
As depicted in figs. 1 and 2, a kind of based on Prussian blue no enzymuria acid sensor, including successively splice substrate 1,
Conductor layer 2, electrode layer 3, insulating layer 4, layers of two-sided 5 and hydrophilic membrane 6.Electrode layer include to electrode 31 and working electrode 32,
Working electrode 32 is the Prussian blue carbon slurry coating on substrate, and Prussian blue carbon slurry is mixed by Prussian blue (PB) powder with carbon slurry
It forms.Prussian blue mass fraction is 0.5% in Prussian blue carbon slurry.It is Prussian blue to be used to detect uric acid.It is to electrode 31
Argentine chloride coating on substrate.Prussian blue mass fraction refers to that Prussian blue quality accounts for Prussian blue carbon slurry gross mass
Percentage.It is parallel with working electrode to electrode, it is vertical with substrate axis to electrode and working electrode.
It in some embodiments, is the mixture coating of silver coating or silver and silver chlorate on substrate to electrode.
As shown in Fig. 2, there is respective electrode terminal to electrode 31 and working electrode 32, have to electrode corresponding
Have to electrode terminal 21, working electrode corresponding to working electrode terminal 22.Electrode 31 and working electrode are led to respectively
It crosses the first conducting wire to connect with respective electrode terminal, electrode 31 is connect by the first conducting wire 201 with to electrode terminal 21, is worked
Electrode 32 is connect by the first conducting wire 202 with working electrode terminal 31.Electrode cross-talk 21, working electrode terminal 31, first are led
Line 201, the first conducting wire 202 are respectively positioned on conductor layer, and the first conducting wire includes argentine chloride coating and is covered on general on argentine chloride coating
Shandong scholar's indigo plant carbon starches coating.Argentine chloride coating is clipped between substrate and Prussian blue carbon slurry coating.Electrode terminal is by chlorination silver paste
It is printed on substrate and is formed.It only is easy to appear conductive bad or even broken string with conducting wire prepared by chlorination silver paste, in silver chlorate
Prussian blue carbon slurry coating is covered on coating, reduces the conductive bad situation of conducting wire.
As shown in Fig. 2, conductor layer includes two recognition terminals 23 and the second conducting wire for connecting two recognition terminals
203, recognition terminal 23 and the second conducting wire 203 include argentine chloride coating and the Prussian blue carbon being covered on argentine chloride coating slurry
Coating.Recognition terminal judges whether sensor is inserted into for detecting instrument: detecting instrument to two recognition terminals one of them
Output voltage, if another recognition terminal can detect that voltage, detecting instrument judge that sensor is already inserted into, starts to telecommunications
It number is detected;If another recognition terminal cannot detect that voltage, detecting instrument judge that sensor is not inserted into.
As shown in Fig. 2, insulating layer 4 is equipped with notch 41, layers of two-sided 5 is equipped with notch 51, insulating layer notch 41 and double-sided adhesive
Break mouth 51 intersects with to electrode 31 and working electrode 32, substrate 1, insulating layer notch 41, layers of two-sided notch 51 and hydrophilic film
Layer 6 is collectively formed for sample to be tested to be drained to working electrode and to the siphon passage of electrode.Insulating layer notch and double-sided adhesive
The salty conjunction of break.The shape of notch is rectangle.Insulating layer is prepared by hydrophobic material.Insulating layer notch, layers of two-sided
Notch is respectively positioned on working electrode and the surface to electrode.Siphon passage has siphon port, and siphon passage will using capillarity
Sample to be tested sucks siphon passage from siphon port, and sample to be tested is guided to working electrode and to electrode by siphon passage.
In some embodiments, the shape of notch is square, ellipse or round.
In the present embodiment, insulating layer epoxy resin is prepared.
As shown in Fig. 2, hydrophilic membrane 6 has air hole 61, air hole 61 is provided at the through-hole on hydrophilic membrane 6, breathes freely
Hole and siphon passage are connected close to one end of substrate center.Air hole prevents remaining gas in siphon passage from producing for breathing freely
Anger pressure hinders sample to be tested from siphon passage to be drained to working electrode and to electrode.
A kind of preparation method based on Prussian blue no enzymuria acid sensor, successively the following steps are included:
1) pet substrate is placed in pure water and is cleaned by ultrasonic 15min, be put into baking oven 90 DEG C, 30min drying.
2) with chlorination silver paste in substrate surface printed circuit cable layer and to electrode, 120 DEG C, 15min baking are put into baking oven
It is dry;Conductor layer includes electrode terminal, two recognition terminals, the first conducting wire and the second conducting wire.
3) prussian blue powder, which is added in carbon slurry, is mixed, prepares Prussian blue carbon slurry, general Shandong in Prussian blue carbon slurry
The mass fraction of scholar's indigo plant is 0.5%;The method for mixing Prussian blue and carbon slurry is Prussia's blue powder to be added in carbon slurry, with machinery
Blender stirs 500 turns, and 60min then is stirred by ultrasonic with ultrasonic oscillation instrument.
4) it prints Prussian blue carbon on substrate to starch to form Prussian blue carbon slurry coating, Prussian blue carbon slurry coating is as work
Make electrode;And conducting wire and recognition terminal in printing covering conductor layer are starched with Prussian blue carbon.
5) 80 DEG C, 15min drying are put into baking oven.
6) it in organic solvent by epoxy resin dissolution, is printed on electrode layer with the organic solvent dissolved with epoxy resin absolutely
Edge layer is put into baking oven 90 DEG C, 15min drying, organic solvent is made to volatilize, and insulating layer has to intersect with to electrode and working electrode
Notch.The organic solvent of dissolved epoxy can be acetone, dimethylbenzene or n-butanol.
7) notch is made on double-sided adhesive, on the insulating layer by sticking double faced adhesive tape, sticking double faced adhesive tape in insulating layer, it is two-sided
Glue notch is overlapped with insulating layer notch, double-sided adhesive with a thickness of 0.1mm.
8) hydrophilic membrane is covered on double-sided adhesive.
Embodiment 2
Prepared in the present embodiment based on Prussian blue no enzymuria acid sensor, except the Prussia in Prussian blue carbon slurry
Blue mass fraction is except 3.5%, remaining structure is identical without enzymuria acid sensor as in embodiment 1.
Preparation method based on Prussian blue no enzymuria acid sensor in the present embodiment, successively the following steps are included:
1) pet substrate is placed in pure water and is cleaned by ultrasonic 15min, be put into baking oven 90 DEG C, 30min drying.
2) with chlorination silver paste in substrate surface printed circuit cable layer and to electrode, 120 DEG C, 15min baking are put into baking oven
It is dry;Conductor layer includes electrode terminal, two recognition terminals, the first conducting wire and the second conducting wire.
3) prussian blue powder, which is added in carbon slurry, is mixed, prepares Prussian blue carbon slurry, general Shandong in Prussian blue carbon slurry
The mass fraction of scholar's indigo plant is 3.5%;The method for mixing Prussian blue and carbon slurry is Prussia's blue powder to be added in carbon slurry, with machinery
Blender stirs 300 turns, and 30min then is stirred by ultrasonic with ultrasonic oscillation instrument.
4) it prints Prussian blue carbon on substrate to starch to form Prussian blue carbon slurry coating, Prussian blue carbon slurry coating is as work
Make electrode;And conducting wire and recognition terminal in printing covering conductor layer are starched with Prussian blue carbon.
5) 90 DEG C, 10min drying are put into baking oven.
6) it in organic solvent by epoxy resin dissolution, is printed on electrode layer with the organic solvent dissolved with epoxy resin absolutely
Edge layer is put into baking oven 90 DEG C, 15min drying, organic solvent is made to volatilize, and insulating layer has to intersect with to electrode and working electrode
Notch.
7) notch is made on double-sided adhesive, on the insulating layer by sticking double faced adhesive tape, sticking double faced adhesive tape in insulating layer, it is two-sided
Glue notch is overlapped with insulating layer notch, double-sided adhesive with a thickness of 0.15mm.
8) hydrophilic membrane is covered on double-sided adhesive.
Embodiment 3
Prepared in the present embodiment based on Prussian blue no enzymuria acid sensor, except the Prussia in Prussian blue carbon slurry
Blue mass fraction is except 5%, remaining structure is identical without enzymuria acid sensor as in embodiment 1.
In the present embodiment, based on the preparation method of Prussian blue no enzymuria acid sensor, successively the following steps are included:
1) pet substrate is placed in pure water and is cleaned by ultrasonic 15min, be put into baking oven 90 DEG C, 30min drying.
2) with chlorination silver paste in substrate surface printed circuit cable layer and to electrode, 120 DEG C, 15min baking are put into baking oven
It is dry;Conductor layer includes electrode terminal, two recognition terminals, the first conducting wire and the second conducting wire.
3) prussian blue powder, which is added in carbon slurry, is mixed, prepares Prussian blue carbon slurry, general Shandong in Prussian blue carbon slurry
The mass fraction of scholar's indigo plant is 5%;The method for mixing Prussian blue and carbon slurry is Prussia's blue powder to be added in carbon slurry, stirred with machinery
It mixes machine and stirs 200 turns, 10min then is stirred by ultrasonic with ultrasonic oscillation instrument.
4) it prints Prussian blue carbon on substrate to starch to form Prussian blue carbon slurry coating, Prussian blue carbon slurry coating is as work
Make electrode;And conducting wire and recognition terminal in printing covering conductor layer are starched with Prussian blue carbon.
5) 100 DEG C, 8min drying are put into baking oven.
6) it in organic solvent by epoxy resin dissolution, is printed on electrode layer with the organic solvent dissolved with epoxy resin absolutely
Edge layer, is put into baking oven 90 DEG C, 15min drying, and insulating layer has the notch intersected with to electrode and working electrode.
7) notch is made on double-sided adhesive, on the insulating layer by sticking double faced adhesive tape, sticking double faced adhesive tape in insulating layer, it is two-sided
Glue notch is overlapped with insulating layer notch, double-sided adhesive with a thickness of 0.2mm.
8) hydrophilic membrane is covered on double-sided adhesive.
Embodiment 4
The present embodiment it is identical without enzymuria acid sensor as embodiment 2 based on Prussian blue no enzymuria acid sensor.
Preparation method of the present embodiment based on Prussian blue no enzymuria acid sensor is different from embodiment 2, difference
It is for the step 4) in embodiment 2 to be substituted for: Prussian blue carbon is added dropwise on substrate and starches to form Prussian blue carbon slurry coating, it is general
Shandong scholar's indigo plant carbon starches coating as working electrode;And the conducting wire in Prussian blue carbon slurry covering conductor layer and recognition terminal is added dropwise.This
Remaining step of preparation method without enzymuria acid sensor in embodiment is identical as the step in embodiment 2.
Embodiment 5
The present embodiment based on Prussian blue no enzymuria acid sensor, except working electrode includes carbon slurry coating, carbon pulp layer
On have except Prussian blue carbon slurry coating, remaining structure is identical without enzymuria acid sensor as in embodiment 2.
Preparation method based on Prussian blue no enzymuria acid sensor in the present embodiment, successively the following steps are included:
1) pet substrate is placed in pure water and is cleaned by ultrasonic 15min, be put into baking oven 90 DEG C, 30min drying.
2) with chlorination silver paste in substrate surface printed circuit cable layer and to electrode, 120 DEG C, 15min baking are put into baking oven
It is dry;Conductor layer includes electrode terminal, two recognition terminals, the first conducting wire and the second conducting wire.
3) carbon is printed on substrate to starch to form carbon slurry coating, drying.
4) prussian blue powder, which is added in carbon slurry, is mixed, prepares Prussian blue carbon slurry, general Shandong in Prussian blue carbon slurry
The mass fraction of scholar's indigo plant is 3.5%;The method for mixing Prussian blue and carbon slurry is Prussia's blue powder to be added in carbon slurry, with machinery
Blender stirs 300 turns, and 30min then is stirred by ultrasonic with ultrasonic oscillation instrument.
5) Prussian blue carbon is printed on carbon slurry coating to starch to form Prussian blue carbon slurry coating;And it is starched and is printed with Prussian blue carbon
Conducting wire and recognition terminal in brush covering conductor layer.
6) it dries, drying temperature is 80 DEG C~100 DEG C, and drying time is 8~15min.
7) it in organic solvent by epoxy resin dissolution, is printed on electrode layer with the organic solvent dissolved with epoxy resin absolutely
Edge layer is put into baking oven 90 DEG C, 15min drying, organic solvent is made to volatilize, and insulating layer has to intersect with to electrode and working electrode
Notch.
8) notch is made on double-sided adhesive, on the insulating layer by sticking double faced adhesive tape, sticking double faced adhesive tape in insulating layer, it is two-sided
Glue notch is overlapped with insulating layer notch, double-sided adhesive with a thickness of 0.15mm.
9) hydrophilic membrane is covered on double-sided adhesive.
Embodiment 6
The present embodiment it is identical without enzymuria acid sensor as embodiment 5 based on Prussian blue no enzymuria acid sensor.
Preparation method of the present embodiment based on Prussian blue no enzymuria acid sensor is different from embodiment 5.Difference
It is, the preparation method based on Prussian blue no enzymuria acid sensor in the present embodiment replaces the step 5) in embodiment 5
It changes into: Prussian blue carbon being added dropwise on carbon slurry coating and starches to form Prussian blue carbon slurry coating;And it is covered with Prussian blue carbon slurry is added dropwise
Conducting wire and recognition terminal in lid conductor layer.Preparation method based on Prussian blue no enzymuria acid sensor in the present embodiment
Remaining step is identical as the step in embodiment 5.
Comparative example 1
Prepared in the present embodiment based on Prussian blue no enzymuria acid sensor, except the Prussia in Prussian blue carbon slurry
Blue mass fraction is except 0.2%, remaining structure can be identical without enzymuria acid sensor as in embodiment 1.
In the present embodiment, based on the preparation method of Prussian blue no enzymuria acid sensor, successively the following steps are included:
1) pet substrate is placed in pure water and is cleaned by ultrasonic 15min, be put into baking oven 90 DEG C, 30min drying.
2) with chlorination silver paste in substrate surface printed circuit cable layer and to electrode, 120 DEG C, 15min baking are put into baking oven
It is dry;Conductor layer includes electrode terminal, two recognition terminals, leads for connection electrode terminal and working electrode or to the first of electrode
Line and the second conducting wire for connecting two recognition terminals.
3) prussian blue powder, which is added in carbon slurry, is mixed, prepares Prussian blue carbon slurry, general Shandong in Prussian blue carbon slurry
The mass fraction of scholar's indigo plant is 0.2%;The method for mixing Prussian blue and carbon slurry is Prussia's blue powder to be added in carbon slurry, with machinery
Blender stirs 300 turns, and 30min then is stirred by ultrasonic with ultrasonic oscillation instrument.
4) with Prussian blue carbon starch printing work electrode, and with Prussian blue carbon slurry printing covering conductor layer in conducting wire with
Recognition terminal is put into baking oven 90 DEG C, 10min drying.
5) it in organic solvent by epoxy resin dissolution, is printed on electrode layer with the organic solvent dissolved with epoxy resin absolutely
Edge layer, be put into baking oven 90 DEG C, 15min drying, so that organic solvent is sufficiently volatilized, insulating layer have with to electrode and working electrode
The notch of intersection.
6) notch is made on double-sided adhesive, on the insulating layer by sticking double faced adhesive tape, sticking double faced adhesive tape in insulating layer, it is two-sided
Glue notch is overlapped with insulating layer notch, double-sided adhesive with a thickness of 0.15mm.
7) hydrophilic membrane is covered on double-sided adhesive.
Comparative example 2
Prepared in the present embodiment based on Prussian blue no enzymuria acid sensor, except the Prussia in Prussian blue carbon slurry
Blue mass fraction is except 6%, remaining structure can be identical without enzymuria acid sensor as in embodiment 1.
In the present embodiment, based on the preparation method of Prussian blue no enzymuria acid sensor, successively the following steps are included:
1) pet substrate is placed in pure water and is cleaned by ultrasonic 15min, be put into baking oven 90 DEG C, 30min drying.
2) with chlorination silver paste in substrate surface printed circuit cable layer and to electrode, 120 DEG C, 15min baking are put into baking oven
It is dry;Conductor layer includes electrode terminal, two recognition terminals, leads for connection electrode terminal and working electrode or to the first of electrode
Line and the second conducting wire for connecting two recognition terminals.
3) prussian blue powder, which is added in carbon slurry, is mixed, prepares Prussian blue carbon slurry, general Shandong in Prussian blue carbon slurry
The mass fraction of scholar's indigo plant is 6%;The method for mixing Prussian blue and carbon slurry is Prussia's blue powder to be added in carbon slurry, stirred with machinery
It mixes machine and stirs 300 turns, 30min then is stirred by ultrasonic with ultrasonic oscillation instrument.
4) with Prussian blue carbon starch printing work electrode, and with Prussian blue carbon slurry printing covering conductor layer in conducting wire with
Recognition terminal is put into baking oven 90 DEG C, 10min drying.
5) it in organic solvent by epoxy resin dissolution, is printed on electrode layer with the organic solvent dissolved with epoxy resin absolutely
Edge layer, be put into baking oven 90 DEG C, 15min drying, so that organic solvent is sufficiently volatilized, insulating layer have with to electrode and working electrode
The notch of intersection.
6) notch is made on double-sided adhesive, on the insulating layer by sticking double faced adhesive tape, sticking double faced adhesive tape in insulating layer, it is two-sided
Glue notch is overlapped with insulating layer notch, double-sided adhesive with a thickness of 0.15mm.
7) hydrophilic membrane is covered on double-sided adhesive.
Examples 1 to 6, the comparison of the testing result of comparative example 1~2
At room temperature, it is had studied in embodiment 2 using cyclic voltammetry (CV) and is in concentration without enzymuria acid sensor
Electrochemical behavior in the uric acid solution of 0mmol/L, 0.4mmol/L, 1mmol/L and 2mmol/L.Fig. 5 is embodiment 2 without enzyme
Cyclic voltammogram of the uric acid sensor in various concentration uric acid solution.It it can be seen that, is 0.4~0.5V in voltage from Fig. 5
Between occur an oxidation peak;And with the increase of uric acid concentration, the oxidation peak of uric acid also gradually increases between 0.4~0.5V
Add.At room temperature, the uric acid solution time electricity that different, concentration range is 0~2mmol/L to a variety of concentration under 0.45V voltage
Stream method is tested, and time current curve shown in fig. 6 is obtained.Detection time is chosen from the time current curve of Fig. 6 is
Multiple test points of 5s, multiple test points are marked in uric acid concentration-current graph of Fig. 7, and are carried out to multiple test points linear
Fitting obtains uric acid concentration-electric current fitting a straight line that detection time is 5s.With same method obtain embodiment 2 without enzymuria
Acid sensor when detecting between for uric acid concentration-electric current fitting a straight line under 10s and 15s, as shown in Figure 7.It is also shown in Fig. 7 each
The corresponding linear equation of fitting a straight line.Calculate related coefficient square (R2).In the present invention, related coefficient square refers to electric current
Variation total sum of squares in, the shared ratio of the variation of the quadratic sum as caused by uric acid concentration.The size table of related coefficient square
Bright electric current level of intimate relevant to uric acid concentration.Work as R2When closer 1, indicate that linear fit is more accurate, uric acid sensor
Detection accuracy is higher;On the contrary, R2When closer 0, indicate that linear fit is more inaccurate, the detection accuracy of uric acid sensor is got over
It is low.
It is detected in embodiment 1, embodiment 3~6, comparative example 1 and comparative example 2 with method similarly to Example 2 without enzymuria
Acid sensor concentration range be 0~2mmol/L, multiple and different concentration uric acid solution in electrochemical behavior.That is,
Cyclic voltammogram of the measurement without enzymuria acid sensor in various concentration uric acid solution first, passes through Prussia in cyclic voltammogram
The oxidation peak of indigo plant oxidation uric acid finds response voltage range, a voltage is then chosen within the scope of response voltage, in the voltage
The lower time current curve detected under different uric acid concentrations;It is respectively 5s, 10s that detection time is chosen from time current curve
It is marked in uric acid concentration-current graph with multiple test points of 15s, and dense to the uric acid that detection time is 5s, 10s and 15s respectively
Degree-current detecting point carries out linear fit, obtains uric acid concentration-electric current Linear Fit Chart.Fig. 3, Fig. 6, Fig. 8, Figure 10, Figure 12,
Figure 14, Figure 16 and Figure 18 be respectively in Examples 1 to 6, comparative example 1 and comparative example 2 without enzymuria acid sensor in concentration range
For 0~2mmol/L, a variety of various concentrations uric acid solution in carry out detecting resulting when m- current curve.Fig. 4, Fig. 9, figure
11, Figure 13, Figure 15, Figure 17 and Figure 19 are respectively and pass in embodiment 1, embodiment 3~6, comparative example 1 and comparative example 2 without enzymuria acid
Uric acid concentration-electric current Linear Fit Chart of sensor.Comparison diagram 4, Fig. 7, Fig. 9, Figure 11, Figure 13, Figure 15, Figure 17 and Figure 19 can be with
Find out, when mass fraction Prussian blue in Prussian blue carbon slurry is 0.5% or more, have between multiple test points preferable
Linear relationship;When Prussian blue mass fraction is lower than 0.5%, sensor detection signal is weak, the line between multiple test points
Sexual intercourse is poor.Table 1 list Examples 1 to 6 and comparative example 1~2 without enzymuria acid sensor when detecting between for 10s when it is related
Coefficient square R2.As can be seen from Table 1, when mass fraction Prussian blue in Prussian blue carbon slurry is 0.5% or more, sensing
Device related coefficient square is greater than 0.98, illustrates that sensor detection results are accurate;When Prussian blue mass fraction is lower than 0.5%
When, related coefficient square is up to 0.931, illustrates that sensor detection results are more inaccurate.
Related coefficient square without enzymuria acid sensor in 1 Examples 1 to 6 of table and comparative example 1~2
Repeated detection is carried out with uric acid solution of no enzymuria acid sensor to same concentration, obtains multiple current values, is calculated
The relative standard deviation (RSD) of multiple current values.RSD is the standard deviation and calculated result arithmetic mean of instantaneous value of electric current in the present invention
Ratio.The RSD of electric current is smaller, the consistency of sensor detection is better, shows that the stability of sensor is good.Table 2 is embodiment 1
~6 and comparative example 1~2 in the surveyed electric current without enzymuria acid sensor relative standard deviation (RSD).As can be seen from Table 2, when
When Prussian blue mass fraction is 5% or less in Prussian blue carbon slurry, RSD is smaller, sensor stability is good;When Prussian blue
Mass fraction be higher than 5% when, RSD is larger, sensor stability is poor.
Relative standard deviation (RSD) in 2 Examples 1 to 6 of table and comparative example 1~2 without the surveyed electric current of enzymuria acid sensor
Table 3 is the detection time without enzymuria acid sensor in Examples 1 to 6 and comparative example 1~2.It can from table 3
It arrives, with the increase of Prussian blue concentration, detection time shortens.When Prussian blue mass fraction is 0.5%~5%, detection
Time is 20~25s.When Prussian blue concentration is lower than 0.5%, detection speed is slower.
Detection time without enzymuria acid sensor in 3 Examples 1 to 6 of table and comparative example 1~2
According to Fig. 3~19, table 1~3 experimental result it is found that when Prussian blue mass fraction be 0.5%~5% when,
The present invention is based on Prussian blue no enzymuria acid sensors to have stronger sensor detection signal, accuracy in detection height, performance
Stablize and detection speed is fast.
Content described in this specification embodiment is only enumerating to the way of realization of inventive concept, protection of the invention
Range should not be construed as being limited to the specific forms stated in the embodiments, and protection scope of the present invention is also and in art technology
Personnel conceive according to the present invention it is conceivable that equivalent technologies mean.
Claims (6)
1. it is a kind of based on Prussian blue no enzymuria acid sensor, including the substrate, conductor layer and electrode layer successively to splice, electrode
Layer includes to electrode and working electrode, it is characterised in that: working electrode is the Prussian blue carbon slurry coating on substrate, Prussian blue
Carbon slurry is mixed by prussian blue powder and carbon slurry.
2. as described in claim 1 based on Prussian blue no enzymuria acid sensor, it is characterised in that: to electrode and work electricity
It is great to have respective electrode terminal, the first conducting wire is passed through to electrode and working electrode respectively and is connect with respective electrode terminal, electricity
Extreme son and the first conducting wire are respectively positioned on conductor layer, and the first conducting wire includes argentine chloride coating and the Pu Lu that is covered on argentine chloride coating
Scholar's indigo plant carbon starches coating.
3. as claimed in claim 2 based on Prussian blue no enzymuria acid sensor, it is characterised in that: conductor layer includes two
Recognition terminal and the second conducting wire for connecting two recognition terminals, recognition terminal and the second conducting wire include argentine chloride coating and
The Prussian blue carbon slurry coating being covered on argentine chloride coating.
4. as claimed in claim 3 based on Prussian blue no enzymuria acid sensor, it is characterised in that: this is sensed without enzymuria acid
Device further includes the insulating layer successively to splice, layers of two-sided and hydrophilic membrane, and insulating layer splices on electrode layer, insulating layer and double
Face glue-line is all provided with jagged, and notch intersects with to electrode and working electrode, substrate, insulating layer notch, layers of two-sided notch and parent
Water film is collectively formed for sample to be tested to be drained to working electrode and to the siphon passage of electrode.
5. as claimed in claim 4 based on Prussian blue no enzymuria acid sensor, it is characterised in that: hydrophilic membrane has saturating
Stomata, air hole are provided at the through-hole on hydrophilic membrane, air hole and siphon passage and connect close to one end of substrate center.
6. the preparation method as claimed in claim 5 based on Prussian blue no enzymuria acid sensor, it is characterised in that: general
Scholar's indigo plant carbon slurry in Shandong is Prussia's blue powder to be added in carbon slurry, stir 200 ~ 500 turns with machine mixer, then uses ultrasonic oscillation
The slurry that 10 ~ 60 min are formed is stirred by ultrasonic in instrument.
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