CN108828039A - A kind of double modifying foam nickel electrodes and preparation method thereof and electrochemistry formaldehyde sensor using the electrode - Google Patents
A kind of double modifying foam nickel electrodes and preparation method thereof and electrochemistry formaldehyde sensor using the electrode Download PDFInfo
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- CN108828039A CN108828039A CN201810936473.0A CN201810936473A CN108828039A CN 108828039 A CN108828039 A CN 108828039A CN 201810936473 A CN201810936473 A CN 201810936473A CN 108828039 A CN108828039 A CN 108828039A
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- G—PHYSICS
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- 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
Abstract
A kind of double modifying foam nickel electrodes and preparation method thereof and electrochemistry formaldehyde sensor mould group using the electrode.The foam nickel electrode is the foam nickel electrode of surface modification porous gold and transition metal phosphide, after the method for modifying of porous gold is first deposited Au tin alloy, then removes the tin in alloy, transition metal phosphide modification is to use hydro-thermal method.Formaldehyde is detected using double modifying foam nickel electrodes as formaldehyde electrochemical sensor, there is higher sensitivity stability and accuracy, can be improved the precision of formaldehyde examination.
Description
Technical field
The present invention relates to a kind of foam nickel electrode, more particularly, to a kind of double modifying foam nickel electrodes and preparation method thereof and
Using the electrochemistry formaldehyde sensor mould group of the electrode, belong to technical field of electrochemical detection.
Background technique
Air quality problems after interior decoration have caused the extensive concern of people, and wherein formaldehyde in air content is evaluation
Whether new finishing environment is suitable for the important indicator for using or living.The mainstream solution of formaldehyde sensor is to use at present
Infrared sensor and gas sensor, wherein small to interfere the advantages of infrared sensor, accuracy is high, and disadvantage is that sensor is attached
Equipment is many and diverse, cannot achieve miniaturization, portability；Gas sensor is the main direction of development of current formaldehyde sensor, but gas
The principle of dependent sensor is to change the electrical properties of air-sensitive film after adsorbing by air-sensitive film and formaldehyde, is rung to obtain signal
Answer, limitation of the air-sensitive film due to adsorption capacity and desorbing gas are difficult, can not larger concentration range and in the long period it is accurate
Detect the concentration of formaldehyde.
Gas eletrochemistry detection is a kind of detection technique of new development in recent years, can be accurately using electrochemical sensor
The number for the amount that formaldehyde reacts in decomposable process detected, thus in precise measurement space formaldehyde variation.At present much just
The formula formaldehyde monitor of taking also starts using electrochemical detection method, and wherein electrochemistry formaldehyde sensor is its most important member
Device has the good characteristics such as low-power consumption, high sensitivity, the linearity be good.But current existing electrochemical sensor is by external wet
The factors such as degree, interfering substance influence to will lead to that testing result is unstable, the bad disadvantage of repeatability, cause in different times or not
Result fluctuation with environment measurement is larger, and stability is to be improved.
The present invention is based on principle of electrochemical reaction to detect concentration of formaldehyde, can make high, stability height small in size, repeatable
Electrochemistry formaldehyde sensor.
Summary of the invention
The object of the present invention is to provide a kind of double modifying foam nickel electrodes and preparation method thereof and using nickel foam electricity
The formaldehyde electrochemical sensor of pole preparation.
An object of the present invention is to provide a kind of double modifying foam nickel electrodes, specifically repairs on foam nickel electrode surface
Adorn the microneedle electrodes of porous gold and transition metal phosphide.
Further, the transition metal phosphide is at least one of cobalt, copper or phosphide of nickel.
Further, the transition metal phosphide is phosphatization cobalt (Co2P)。
The second object of the present invention is to provide a kind of preparation method of double modifying foam nickel electrodes, including steps are as follows：
1) foam nickel electrode is surface-treated, obtains surface-treated foam nickel electrode；
2) in the porous gold of foam nickel electrode surface modification：After first deposited Au tin alloy, then with chemical corrosion method or electrification
Learn the tin in etch removal alloy；
3) in the foam nickel electrode surface modification transition metal phosphide for having modified porous gold：The foam of porous gold will be modified
Nickel electrode immerse water heating kettle in, in water heating kettle equipped with transition metal salt, oleic acid amine and triphenylphosphine mixed liquor, under vacuum into
Foam nickel electrode is placed in electric dry oven after hydro-thermal reaction and roasts by row hydro-thermal reaction, it is cooling after pure water clean, be drying to obtain modification
The double modifying foam nickel electrodes of porous gold and transition metal phosphide.
Further, the step 1) specifically includes：Surface treatment is oil removal treatment；Preferably, the oil removal treatment
It is organic solvent cleaning or ultrasonic cleaning.
Further, gold-tin alloy solution composition used in electrochemical deposition is sulfurous acid gold, methyl in the step 2)
Sulfonic acid tin, citric acid, potassium pyrophosphate and potassium sulfate；
It is preferred that the group of the gold-tin alloy solution becomes：10~50g/L of sulfurous acid gold, 10~50g/L of tin methane sulfonate,
40~90g/L of citric acid, 50~90g/L of potassium pyrophosphate, 10~30g/L of potassium sulfate；
The group of preferred gold-tin alloy solution becomes：20~40g/L of sulfurous acid gold, 20~40g/L of tin methane sulfonate, lemon
50~80g/L of lemon acid, 60~80g/L of potassium pyrophosphate, 15~25g/L of potassium sulfate.
Further, electrochemical deposition temperature is 40~60 DEG C in the step 2), and current density is 0.2~0.8A/
dm2, the time is 15~40min；
It is furthermore preferred that the electrodeposition temperature is 45~55 DEG C, current density is 0.3~0.7A/dm2, the time 20
~30min；
Further, chemical corrosion method is used when preferably removing tin, it is specific to be corroded using the lye of concentration 2-20M.
Further, in the step 3), preferably transition metal salt is cobalt nitrate, cobalt acetate or citric acid cobalt；It is preferred that vinegar
Sour cobalt；
Further, in the mixed liquor acetic acid cobalt concentration be 0.5mM~12.0mM, oleic acid amine concentration be 0.5mM~
25.0mM, triphenylphosphine concentration are 1.0mM~15.0mM；
Preferred acetic acid cobalt concentration is 0.8mM~10.0mM, and oleic acid amine concentration is 1.0mM~20.0mM, and triphenylphosphine is dense
Degree is 1.5mM~12.0mM；
The hydrothermal temperature is 300~360 DEG C, and the reaction time is 10~20min；
The preferred hydrothermal temperature is 320 DEG C, reaction time 15min.
The third object of the present invention is to provide a kind of formaldehyde electrochemical sensor, comprising substrate, including the conduction of positive and negative anodes
Layer and conversion zone, sensor anode and negative conductive layer surface are respectively provided with conversion zone, and the conversion zone is using prepared by the present invention double
Modifying foam nickel electrode.
Further, the formaldehyde electrochemical sensor base material be aluminium oxide, aluminium nitride, epoxy resin, PMMA,
Any one of PET, PC, PS and its polymer；
The conductive layer is the metal layer that one of Ag, Au, Cu, Pd, Pt are formed or in which the conjunction that at least two form
Layer gold；
It is preferred that the electrochemical sensor configures AD conversion module, output digit signals；
More preferably the AD conversion module outlet line is serial bus or I2C bus.
The beneficial effects of the invention are as follows：
(1) quick, accurate, low-power consumption the detection of formaldehyde sensor electrode PARA FORMALDEHYDE PRILLS(91,95), inspection are realized using electrochemical principle
It is more stable compared to traditional detection to survey effect, repeatability is higher.
(2) increased by the active surface area in the porous gold of foam nickel electrode surface modification contacting, it, increase sensing
The load of active material can be significantly increased by porous gold modification, improve the sensitivity of electrochemical sensing for the sensitivity of device.
(3) porous fitting has higher stability, is easy to load various sensitive active materials on the surface thereof, can adapt to
Various different detection environment.
(4) there is I2C bus or serial bus, realize digital signal output, can support I2C or serial digital with other
The mould group of signal is adapted to.
Detailed description of the invention
Fig. 1 is load C o on porous gold (NPG)/Ni foam2The schematic diagram of the electrochemistry formaldehyde sensor preparation process of P；
Fig. 2 (a1)-(a3) be method of the invention on foam nickel electrode after electro-deposition gold-tin alloy in 0.5A/dm2, 45
Gold-tin alloy/Ni foam electrode scanning electron microscope (SEM) photograph at DEG C；
Fig. 3 (b1)-(b3) is porous gold modifying foam nickel electrode made from method of the invention in 0.5A/dm2, at 45 DEG C
The scanning electron microscope (SEM) photograph of NPG/Ni foam electrode；
Fig. 4 is double modifying foam nickel electrode (Co that embodiment 1 is prepared2P@NPG/Ni foam electrode) scanning electricity
Mirror figure；
Fig. 5 is double modifying foam nickel electrode (Co that embodiment 2 is prepared2P@NPG/Ni foam electrode) scanning electricity
Mirror figure；
Fig. 6 is double modifying foam nickel electrode (Co that embodiment 3 is prepared2P@NPG/Ni foam electrode) scanning electricity
Mirror figure.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1,
Foam nickel electrode is surface-treated：Ultrasonic cleaning oil removing is carried out to electrode, is cleaned later with deionized water
Completely.
To electrode modification nano-porous gold and phosphatization cobalt (Co2P)：Contain the substrate of Ni foam as work using circuit surface
Electrode, platinized platinum are to electrode, and gold-tin alloy solution is electroplate liquid, and 45 DEG C of constant temperature, the group of gold-tin alloy solution becomes：Sulfurous acid gold
20g/L, tin methane sulfonate 30g/L, citric acid 40g/L, potassium pyrophosphate 55g/L, potassium sulfate 20g/L, in 0.5A/dm2Electric current is close
Spend lower electro-deposition 20min.It after plating, is cleaned with deionized water, is then dried in air, then electrode in etching liquor
30min is impregnated in middle immersion, taking-up in deionized water, and 60 DEG C of heating, dryings obtain porous gold and repair in natural air drying or baking oven
Adorn electrode.
Then exposed porous gold is immersed in water heating kettle, in kettle be equipped with 0.8mM cobalt acetate, 1.0mM oleic acid amine and
1.5mM triphenylphosphine.Then water heating kettle is vacuumized in the electric dry oven for be placed in 350 DEG C and heats 15min.Room temperature is naturally cooled to,
Electrode is completely placed on to 60 DEG C of heating, drying 1h in baking oven with pure water rinsing.
Attached drawing 1 is double modification microneedle electrodes that the phosphatization cobalt that embodiment 1 is prepared is carried on alloy microneedle electrodes
Pattern control experiment electron microscope.
Embodiment 2,
Foam nickel electrode is surface-treated：Washes of absolute alcohol oil removing is carried out to electrode, it is clear with deionized water later
Wash clean.
To electrode modification nano-porous gold and phosphatization cobalt：It is cleaned up to after electrode oil removing with deionized water.With circuit table
The substrate that Ni foam is contained in face is working electrode, and platinized platinum is to electrode, and gold-tin alloy solution is electroplate liquid, 60 DEG C of constant temperature, golden tin
The group of alloy solution becomes：Sulfurous acid gold 10g/L, tin methane sulfonate 20g/L, citric acid 50g/L, potassium pyrophosphate 50g/L, sulfuric acid
Potassium 15g/L, in 0.8A/dm2Electro-deposition 20min under current density.It after plating, is cleaned with deionized water, is then done in air
It is dry, electrode is impregnated in etching liquor then, takes out and impregnates 30min in deionized water, in natural air drying or baking oven
60 DEG C of heating, dryings obtain porous golden modified electrode.
Then exposed porous gold is immersed in water heating kettle, in kettle be equipped with 0.8mM cobalt nitrate, 1.0mM oleic acid amine and
1.5mM triphenylphosphine.Then water heating kettle is vacuumized in the electric dry oven for be placed in 340 DEG C and heats 10min.Room temperature is naturally cooled to,
Electrode is completely placed on to 60 DEG C of heating, drying 1h in baking oven with pure water rinsing.
Attached drawing 2 is double modification microneedle electrodes that the phosphatization cobalt that embodiment 2 is prepared is carried on alloy microneedle electrodes
Pattern control experiment electron microscope.
Embodiment 3,
Foam nickel electrode is surface-treated：Ultrasonic cleaning oil removing is carried out to electrode, is cleaned later with deionized water
Completely.
To electrode modification nano-porous gold and phosphatization cobalt：It is cleaned up to after electrode oil removing with deionized water.With circuit table
The substrate that Ni foam is contained in face is working electrode, and platinized platinum is to electrode, and gold-tin alloy solution is electroplate liquid, 50 DEG C of constant temperature, golden tin
The group of alloy solution becomes：Sulfurous acid gold 40g/L, tin methane sulfonate 40g/L, citric acid 70g/L, potassium pyrophosphate 70g/L, sulfuric acid
Potassium 30g/L, in 0.9A/dm2Electro-deposition 15min under current density.It after plating, is cleaned with deionized water, is then done in air
It is dry, electrode is impregnated in etching liquor then and is taken out, impregnates 30min in deionized water, in natural air drying or baking oven
60 DEG C of heating, dryings obtain porous golden modified electrode.
Then exposed porous gold is immersed in water heating kettle, in kettle be equipped with 10.0mM cobalt nitrate, 20.0mM oleic acid amine and
12.0mM triphenylphosphine.Then water heating kettle is vacuumized in the electric dry oven for be placed in 320 DEG C and heats 20min.Room temperature is naturally cooled to,
Electrode is completely placed on to 60 DEG C of heating, drying 1h in baking oven with pure water rinsing.
Application examples,
According to double modifying foam nickel electrodes prepared by the preparation method of embodiment 1, substrate uses alumina substrate, to implement
For double modifying foam nickel electrodes of example 1-3 as conversion zone, conductive layer is Ag and Pd alloy-layer；Electrochemical sensor configures AD conversion
Module, outlet line are I2C bus output digit signals.By above three formaldehyde examination sensor and Britain Dart company, with
And the electric chemical formula formaldehyde gas sensor of domestic cubic photoelectricity repeats detection 5 times in the space of 1mg/L concentration, calculates each time
The Mean Deviation value of value and average value, the average deviation of embodiment 1-3 is 0.01ppm, 0.02ppm, 0.01ppm, Britain Dart
The average deviation of company and cubic photoelectricity is 0.03ppm and 0.05ppm respectively.
It can be seen that double modifying foam nickel electrodes that the present invention is prepared are used for formaldehyde electrochemical sensor with higher
Stability and sensitivity, and repeated testing result is also very outstanding, all better than formaldehyde electrochemical sensor both domestic and external.
The above, the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although referring to before
Stating embodiment, invention is explained in detail, those skilled in the art should understand that：It still can be to preceding
Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features；And these
It modifies or replaces, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of double modifying foam nickel electrodes, it is characterised in that：Porous gold and transition metal are modified on foam nickel electrode surface
The microneedle electrodes of phosphide.
2. double modifying foam nickel electrodes according to claim 1, it is characterised in that：The transition metal phosphide is
At least one of manganese, cobalt, copper, ruthenium, iridium, phosphide of rhodium.
3. double modifying foam nickel electrodes according to claim 1, it is characterised in that：The transition metal phosphide is phosphorus
Change cobalt.
4. the preparation method of double modifying foam nickel electrodes according to claim 1 to 3, it is characterised in that including
Steps are as follows：
1) foam nickel electrode is surface-treated, obtains surface-treated foam nickel electrode；
2) in the porous gold of foam nickel electrode surface modification：After first deposited Au tin alloy, then it is rotten with chemical corrosion method or electrochemistry
Erosion method removes the tin in alloy；
3) in the foam nickel electrode surface modification transition metal phosphide for having modified porous gold：The nickel foam electricity of porous gold will be modified
Pole immerse water heating kettle in, in water heating kettle equipped with transition metal salt, oleic acid amine and triphenylphosphine mixed liquor, under vacuum conditions into
Foam nickel electrode is placed in electric dry oven after hydro-thermal reaction and roasts by row hydro-thermal reaction, it is cooling after pure water clean, be drying to obtain modification
The double modifying foam nickel electrodes of porous gold and transition metal phosphide.
5. a kind of preparation method as claimed in claim 4, it is characterised in that step 1) specifically includes：Surface treatment is at oil removing
Reason；Preferably, the oil removal treatment is organic solvent cleaning or ultrasonic cleaning.
6. the preparation method according to claim 4, it is characterised in that gold-tin alloy used in electrochemical deposition in step 2)
Solution composition is sulfurous acid gold, tin methane sulfonate, citric acid, potassium pyrophosphate and potassium sulfate；
It is preferred that the group of the gold-tin alloy solution becomes：10~50g/L of sulfurous acid gold, 10~50g/L of tin methane sulfonate, lemon
40~90g/L of acid, 50~90g/L of potassium pyrophosphate, 10~30g/L of potassium sulfate；
The group of preferred gold-tin alloy solution becomes：20~40g/L of sulfurous acid gold, 20~40g/L of tin methane sulfonate, citric acid
50~80g/L, 60~80g/L of potassium pyrophosphate, 15~25g/L of potassium sulfate.
7. the preparation method according to claim 4, it is characterised in that electrochemical deposition temperature is 40~60 DEG C in step 2),
Current density is 0.2~0.8A/dm2, the time is 15~40min；
It is furthermore preferred that the electrodeposition temperature is 45~55 DEG C, current density is 0.3~0.7A/dm2, the time be 20~
30min；
Chemical corrosion method is used when it is preferred that removing tin, it is specific to be corroded using the lye of concentration 2-20M.
8. the preparation method according to claim 4, it is characterised in that in step 3), preferably transition metal salt be cobalt nitrate,
Cobalt acetate or citric acid cobalt；
Transition metal salinity is 0.5mM~12.0mM in mixed liquor, and oleic acid amine concentration is 0.5mM~25.0mM, triphenylphosphine
Concentration is 1.0mM~15.0mM；
Preferred acetic acid cobalt concentration is 0.8mM~10.0mM, and oleic acid amine concentration is 1.0mM~20.0mM, and triphenylphosphine concentration is
1.5mM~12.0mM；
The hydrothermal temperature is 300~360 DEG C, and the reaction time is 10~20min；
The preferred hydrothermal temperature is 340 DEG C, reaction time 15min.
9. a kind of formaldehyde electrochemical sensor, comprising substrate, the conductive layer including positive and negative anodes and conversion zone, sensor anode and
Negative conductive layer surface is respectively provided with conversion zone, it is characterised in that conversion zone uses according to claim 1 to 3
Double modifying foam nickel electrodes or the double modifying foam nickel electrodes prepared according to claim 4-9 any one method.
10. formaldehyde electrochemical sensor according to claim 9, it is characterised in that：
Formaldehyde electrochemical sensor base material is aluminium oxide, aluminium nitride, epoxy resin, PMMA, PET, PC, PS and its polymer
Any one of；
The conductive layer is the metal layer that one of Ag, Au, Cu, Pd, Pt are formed or in which the alloy-layer that at least two form；
It is preferred that the electrochemical sensor configures AD conversion module, output digit signals；
More preferably the AD conversion module outlet line is serial bus or I2C bus.
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| CN109916977A (en) * | 2019-03-04 | 2019-06-21 | 广州钰芯传感科技有限公司 | A kind of preparation method and applications of the porous gold electrode of VOC detection supported cobaltosic oxide |
| CN110044980A (en) * | 2019-04-30 | 2019-07-23 | 西南大学 | Application of the pyrophosphoric acid cobalt nano material in building nitric oxide electrochemical sensor |
| CN110243894A (en) * | 2019-06-27 | 2019-09-17 | 惠州市钰芯电子材料有限公司 | Platinum/nano-porous gold tin/carbon fiber paper combination electrode preparation method that is a kind of while detecting ascorbic acid, dopamine, uric acid |
| CN110261454A (en) * | 2019-05-28 | 2019-09-20 | 广州钰芯传感科技有限公司 | A kind of nano-porous gold of urine detection dopamine is without enzyme sensing electrode and the preparation method and application thereof |
| CN110320255A (en) * | 2019-06-27 | 2019-10-11 | 广州钰芯传感科技有限公司 | A kind of nano-porous gold/carbon fiber paper multiple sensing electrodes preparation method and application can be used for detecting uric acid and dopamine simultaneously |
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| CN112946035A (en) * | 2021-01-29 | 2021-06-11 | 华中科技大学 | Long-acting reference electrode for monitoring corrosion of steel bar and preparation method thereof |
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| CN110261454A (en) * | 2019-05-28 | 2019-09-20 | 广州钰芯传感科技有限公司 | A kind of nano-porous gold of urine detection dopamine is without enzyme sensing electrode and the preparation method and application thereof |
| CN110243894A (en) * | 2019-06-27 | 2019-09-17 | 惠州市钰芯电子材料有限公司 | Platinum/nano-porous gold tin/carbon fiber paper combination electrode preparation method that is a kind of while detecting ascorbic acid, dopamine, uric acid |
| CN110320255A (en) * | 2019-06-27 | 2019-10-11 | 广州钰芯传感科技有限公司 | A kind of nano-porous gold/carbon fiber paper multiple sensing electrodes preparation method and application can be used for detecting uric acid and dopamine simultaneously |
| CN111957327A (en) * | 2020-07-29 | 2020-11-20 | 国网浙江省电力有限公司电力科学研究院 | Cobalt phosphide nanowire array material and application thereof |
| CN112946035A (en) * | 2021-01-29 | 2021-06-11 | 华中科技大学 | Long-acting reference electrode for monitoring corrosion of steel bar and preparation method thereof |
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