CN104820006A - Preparation method and application of photoelectrochemical sensor for sensitively detecting Cd<2+> based on ZnO and CdS compound semiconductor material - Google Patents

Preparation method and application of photoelectrochemical sensor for sensitively detecting Cd<2+> based on ZnO and CdS compound semiconductor material Download PDF

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CN104820006A
CN104820006A CN201510245145.2A CN201510245145A CN104820006A CN 104820006 A CN104820006 A CN 104820006A CN 201510245145 A CN201510245145 A CN 201510245145A CN 104820006 A CN104820006 A CN 104820006A
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solution
electrode
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ito electrode
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CN104820006B (en
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王荣雨
于思琦
魏琴
马洪敏
王晓东
庞雪辉
杜斌
范大伟
李贺
吴丹
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University of Jinan
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Abstract

The invention belongs to the field of functional nano materials, sensing analysis and environment analysis, and provides a preparation method and application of a photoelectrochemical sensor for sensitively detecting Cd<2+> based on a ZnO and CdS compound semiconductor material. The preparation method comprises the steps of based on an ITO electrode as a substrate, inoculating ZnO seed crystal to the ITO electrode, and depositing CdS on the ITO electrode having crystallized ZnO through an electro-deposition method based on NaS2SO3 as a sulfur source, Cd<2+> in an environment sample as a cadmium source and EDTA as a stabilizing agent, so that the photoelectric signal is greatly enhanced, the detection range is 0.01-5.0mmol/L, and the detection limit is 5micromol/L.

Description

A kind of Sensitive Detection Cd based on ZnO and CdS composite semiconductor material 2+the preparation method of Optical Electro-Chemistry sensor and application
Technical field
The invention belongs to functionalized nano material, sensing assays and environmental analysis field, be specifically related to based on a kind of Sensitive Detection Cd 2+the preparations and applicatio of Optical Electro-Chemistry sensor.
Background technology
Cadmium is the heavy metal that toxicity is very strong, is the nonessential toxic element of human body, is called as " first of the five poisonous creatures: scorpion, viper, centipede, house lizard, toad ", is decided to be priority pollutant by the international labour hygiene heavy metal council.It is reported, can cause slow poisoning, make kidney hypofunction, osteoporosis at the cadmium ion by biologic chain enrichment in human body, the long-term caddy that sucks can cause lung inflammation, bronchitis even cancer, can also cause diabetes, the diseases such as hypertension.So a kind of method designing easy detection cadmium ion is very important.
Optical Electro-Chemistry refers to that molecule, ion or semiconductor material etc. make electronics be stimulated the charge transfer produced because of absorb photons, thus realizes the conversion process of luminous energy to electric energy.Charge separation or charge transfer process is there is in the material with Optical Electro-Chemistry activity by after optical excitation, thus coating-forming voltage or photocurrent.
ZnO is a kind of novel direct semiconductor material with wide forbidden band, energy gap under room temperature is 3.3 eV, exciton bind energy is approximately 60 eV, be expected to the multiple luminescent devices such as exploitation blue light, blue green light, ultraviolet light, be expected to become follow-on photoelectric device, be widely used in the fields such as photoelectric communication network, photoelectric display, photoelectricity storage, photoelectric conversion and photodetection, the dark extensive concern by people recently.
Cadmium sulfide is a kind of important semiconductor functional material, and high-purity cadmium sulfide has strong photoelectric effect to visible ray, can be used for photoelectric tube processed, solar cell.
The present invention uses NaS 2sO 3as sulphur source, the Cd in direct environment for use sample 2+as cadmium source, CdS is deposited to the surface of ZnO nanorod, form ZnO/CdS compound substance, make it have higher electricity conversion.Cd 2+concentration is different, and the amount depositing to the CdS on the surface of ZnO nanorod is different, and the photo-current intensity of Photoelectric Detection is just different, thus realizes Cd 2+quantitative detection.
Summary of the invention
Technical scheme of the present invention, comprises the following steps.
1. the Sensitive Detection Cd based on ZnO and CdS composite semiconductor material 2+the preparation method of Optical Electro-Chemistry sensor, comprise the following steps:
(1) pre-service of ITO electrode: ito glass is slit into 3 cm × 0.8 cm sizes, uses acetone, NaOH ethanolic solution, deionized water ultrasonic cleaning 15 min successively, dries up with nitrogen;
(2) take the NaOH of 0.02 ~ 0.03 g, the zinc acetate of 0.04 ~ 0.05 g is dissolved in 10 mL methyl alcohol respectively, obtains NaOH methanol solution and zinc acetate methanol solution; NaOH methanol solution is dropped in zinc acetate methanol solution, add hot reflux 2 ~ 3 h at 55 ~ 65 DEG C, be cooled to room temperature, obtain ZnO crystal seed;
(3) pretreated ITO electrode is vertically put into ZnO crystal seed, soak 1 ~ 5 min, take out, dry under infrared lamp, repeat 3 ~ 6 times, make ZnO crystal seed on ito glass surface seeding; Then at 300 ~ 400 DEG C of calcining 20 ~ 50 min, cooling, obtains the ITO electrode of ZnO crystallization;
(4) ITO electrode of ZnO crystallization is put into the reactor containing 5 mL zinc nitrate-hexamethylenetetramine mixed liquors, heat 5 ~ 7 h at 90 DEG C, cooling, with deionized water rinsing, natural drying, obtains white film, i.e. obtained a kind of detection Cd 2+optical Electro-Chemistry sensor;
Described zinc nitrate-hexamethylenetetramine mixed liquor mixes obtained by the hexamethylenetetramine aqueous solution of the zinc nitrate aqueous solution of 0.10 mol/L and 0.10 mol/L according to the ratio of 1 ~ 5:1.
2. Cd 2+detecting step as follows:
(1) Cd 2+the preparation of deposit solution: the Cd getting 0.01-5.0 mmol/L 2+standard solution, adds the sulphur source Na of 5-10 mmol/L 2s 2o 3with stabilizing agent EDTA, obtained Cd 2+deposit solution;
(2) adopt three electrodes, in three electrodes, saturated calomel electrode is contrast electrode, and platinum electrode is auxiliary electrode, and ITO electrode is working electrode, at the Cd that (1) obtains 2+in deposit solution, adopt i-t curve method to carry out electro-deposition, sedimentation potential is-1.06 V, and sedimentation time is 100 s;
(3) by post-depositional ITO electrode deionized water rinsing, and dry under infrared lamp;
(4) adopt i-t curve method to carry out Photoelectric Detection, bias voltage is set to 0 V; Every 10 s switch lamps, the changing value of electric current before and after record switch lamp, according to the Cd of variable concentrations 2+the different photocurrent values that deposit solution produces, drawing curve;
(5) Cd is replaced with testing sample 2+standard solution, carries out sample detection according to the method for step (1) ~ (4).
useful achievement of the present invention
(1) use ZnO array modified electrode for the preparation of Sensitive Detection Cd first 2+optical Electro-Chemistry sensor.
(2) the Optical Electro-Chemistry sensor of detection cadmium ion prepared of the present invention, can realize simple, quick and high-sensitivity detection, the range of linearity is 0.01 mmol/L ~ 5 mmol/L, detects and is limited to 5 μm of ol/L.
(3) sensor prepared by can realize for Cd in visible region 2+sensitive Detection, substantially increase the possibility of its practical application.
Specific embodiments
embodiment 1a kind of Sensitive Detection Cd based on ZnO and CdS composite semiconductor material 2+the preparation method of Optical Electro-Chemistry sensor
(1) ito glass is cut into 3 cm × 0.8 cm sizes, use acetone, NaOH ethanolic solution, deionized water ultrasonic cleaning 15 min according to this, dry up with nitrogen, obtain pretreated ITO electrode;
(2) take the NaOH of 0.02 g, the zinc acetate of 0.04 g is dissolved in 10 mL methyl alcohol respectively, obtain NaOH methanol solution and zinc acetate methanol solution; At 55 DEG C, dropped to by NaOH methanol solution in zinc acetate methanol solution, return stirring 2 h, transfers them in beaker, is cooled to room temperature, obtains the opalescent colloidal containing ZnO crystal seed;
(3) pretreated ITO electrode is vertically put into the opalescent colloidal containing ZnO crystal seed, soak 1 min, take out, dry under infrared lamp, repeat 4 times, make ZnO crystal seed on ito glass surface seeding; Put it into porcelain boat, be placed in muffle furnace, 300 DEG C of calcining 20 min, cooling, taking-up, obtain the ITO electrode of ZnO crystallization;
(4) ITO electrode of ZnO crystallization is put into the reactor containing 5 mL zinc nitrate-hexamethylenetetramine solution, 90 DEG C of heating 5 h, cooling, taking-up, with deionized water rinsing, natural drying, obtains on ITO electrode surface solidifying white film, obtained a kind of detection Cd 2+optical Electro-Chemistry sensor;
Described zinc nitrate-hexamethylenetetramine solution mixes obtained by the hexamethylenetetramine aqueous solution of the zinc nitrate aqueous solution of 0.10 mol/L and 0.10 mol/L according to the ratio of 1:1.
embodiment 2a kind of Sensitive Detection Cd based on ZnO and CdS composite semiconductor material 2+the preparation method of Optical Electro-Chemistry sensor
(1) ito glass is cut into 3 cm × 0.8 cm sizes, use acetone, NaOH ethanolic solution, deionized water ultrasonic cleaning 15 min according to this, dry up with nitrogen, obtain pretreated ITO electrode;
(2) take the NaOH of 0.03 g, the zinc acetate of 0.05 g is dissolved in 10 mL methyl alcohol respectively, obtain NaOH methanol solution and zinc acetate methanol solution; At 60 DEG C, dropped to by NaOH methanol solution in zinc acetate methanol solution, return stirring 2.5 h, transfers them in beaker, is cooled to room temperature, obtains the opalescent colloidal containing ZnO crystal seed;
(3) pretreated ITO electrode is vertically put into the opalescent colloidal containing ZnO crystal seed, soak 3 min, take out, dry under infrared lamp, repeat 5 times, make ZnO crystal seed on ito glass surface seeding; Put it into porcelain boat, be placed in muffle furnace, 350 DEG C of calcining 35 min, cooling, taking-up, obtain the ITO electrode of ZnO crystallization;
(4) ITO electrode of ZnO crystallization is put into the reactor containing 5 mL zinc nitrate-hexamethylenetetramine solution, 90 DEG C of heating 6 h, cooling, taking-up, with deionized water rinsing, natural drying, obtains on ITO electrode surface solidifying white film, obtained a kind of detection Cd 2+optical Electro-Chemistry sensor;
Described zinc nitrate-hexamethylenetetramine solution mixes obtained by the hexamethylenetetramine aqueous solution of the zinc nitrate aqueous solution of 0.10 mol/L and 0.10 mol/L according to the ratio of 3:1.
embodiment 3a kind of Sensitive Detection Cd based on ZnO and CdS composite semiconductor material 2+the preparation method of Optical Electro-Chemistry sensor
(1) ito glass is cut into 3 cm × 0.8 cm sizes, use acetone, NaOH ethanolic solution, deionized water ultrasonic cleaning 15 min according to this, dry up with nitrogen, obtain pretreated ITO electrode;
(2) take the NaOH of 0.030 g, the zinc acetate of 0.05 g is dissolved in 10 mL methyl alcohol respectively, obtain NaOH methanol solution and zinc acetate methanol solution; At 65 DEG C, dropped to by NaOH methanol solution in zinc acetate methanol solution, return stirring 3 h, transfers them in beaker, is cooled to room temperature, obtains the opalescent colloidal containing ZnO crystal seed;
(3) pretreated ITO electrode is vertically put into the opalescent colloidal containing ZnO crystal seed, soak 5 min, take out, dry under infrared lamp, repeat 6 times, make ZnO crystal seed on ito glass surface seeding; Put it into porcelain boat, be placed in muffle furnace, 400 DEG C of calcining 50 min, cooling, taking-up, obtain the ITO electrode of ZnO crystallization;
(4) ITO electrode of ZnO crystallization is put into the reactor containing 5 mL zinc nitrate-hexamethylenetetramine solution, 90 DEG C of heating 7 h, cooling, taking-up, with deionized water rinsing, natural drying, obtains on ITO electrode surface solidifying white film, obtained a kind of detection Cd 2+optical Electro-Chemistry sensor;
Described zinc nitrate-hexamethylenetetramine solution mixes obtained by the hexamethylenetetramine aqueous solution of the zinc nitrate aqueous solution of 0.10 mol/L and 0.10 mol/L according to the ratio of 5:1.
embodiment 4cd 2+the drafting of typical curve
(1) Cd 2+the preparation of deposit solution
Get the Cd of 0.01 ~ 5.0 mmol/L 2+standard solution, adds the sulphur source Na of 10 mmol/L 2s 2o 3with stabilizing agent EDTA, obtained Cd 2+deposit solution;
(2) adopt three electrodes, in three electrodes, saturated calomel electrode is contrast electrode, and platinum electrode is auxiliary electrode, and ITO electrode is working electrode, at the Cd that (1) obtains 2+in deposit solution, adopt i-t curve method to carry out electro-deposition, sedimentation potential is-1.06 V, and sedimentation time is 100 s;
(3) by post-depositional ITO electrode deionized water rinsing, and dry under infrared lamp;
(4) adopt i-t curve method to carry out Photoelectric Detection, bias voltage is set to 0 V; Every 10 s switch lamps, the changing value of electric current before and after record switch lamp, according to the Cd of variable concentrations 2+the different photocurrent values that deposit solution produces, drawing curve.
embodiment 5cd 2+the detecting step of content
Cd is replaced with testing sample 2+standard solution, other is identical with embodiment 4, and acquired results contrast working curve, calculates Cd in sample 2+content.

Claims (3)

1. the Sensitive Detection Cd based on ZnO and CdS composite semiconductor material 2+the preparation method of Optical Electro-Chemistry sensor and application
A kind of Sensitive Detection Cd based on ZnO and CdS composite semiconductor material 2+the preparation method of Optical Electro-Chemistry sensor, it is characterized in that, comprise the following steps:
(1) pre-service of ITO electrode: ito glass is slit into 3 cm × 0.8 cm sizes, uses acetone, NaOH ethanolic solution, deionized water ultrasonic cleaning 15 min successively, dries up with nitrogen;
(2) take the NaOH of 0.02 ~ 0.03 g, the zinc acetate of 0.04 ~ 0.05 g is dissolved in 10 mL methyl alcohol respectively, obtains NaOH methanol solution and zinc acetate methanol solution; NaOH methanol solution is dropped in zinc acetate methanol solution, add hot reflux 2 ~ 3 h at 55 ~ 65 DEG C, be cooled to room temperature, obtain ZnO crystal seed;
(3) pretreated ITO electrode is vertically put into ZnO crystal seed, soak 1 ~ 5 min, take out, dry under infrared lamp, repeat 3 ~ 6 times, make ZnO crystal seed on ito glass surface seeding; Then at 300 ~ 400 DEG C of calcining 20 ~ 50 min, cooling, obtains the ITO electrode of ZnO crystallization;
(4) ITO electrode of ZnO crystallization is put into the reactor containing 5 mL zinc nitrate-hexamethylenetetramine mixed liquors, heat 5 ~ 7 h at 90 DEG C, cooling, with deionized water rinsing, natural drying, obtains white film, i.e. obtained a kind of detection Cd 2+optical Electro-Chemistry sensor.
2. a kind of Sensitive Detection Cd based on ZnO and CdS composite semiconductor material as claimed in claim 1 2+the preparation method of Optical Electro-Chemistry sensor, described zinc nitrate-hexamethylenetetramine mixed liquor mixes obtained by the hexamethylenetetramine aqueous solution of the zinc nitrate aqueous solution of 0.10 mol/L and 0.10 mol/L according to the ratio of 1 ~ 5:1.
3. a kind of Sensitive Detection Cd based on ZnO and CdS composite semiconductor material as claimed in claim 1 2+the preparation method of Optical Electro-Chemistry sensor, it is characterized in that, for Cd 2+detection, step is as follows:
(1) Cd 2+the preparation of deposit solution: the Cd getting 0.01 ~ 5.0 mmol/L 2+standard solution, adds the sulphur source Na of 5 ~ 10 mmol/L 2s 2o 3with stabilizing agent EDTA, obtained Cd 2+deposit solution;
(2) adopt three electrodes, in three electrodes, saturated calomel electrode is contrast electrode, and platinum electrode is auxiliary electrode, and ITO electrode is working electrode, at the Cd that (1) obtains 2+in deposit solution, adopt i-t curve method to carry out electro-deposition, sedimentation potential is-1.06 V, and sedimentation time is 100 s;
(3) by post-depositional ITO electrode deionized water rinsing, and dry under infrared lamp;
(4) adopt i-t curve method to carry out Photoelectric Detection, bias voltage is set to 0 V; Every 10 s switch lamps, the changing value of electric current before and after record switch lamp, according to the Cd of variable concentrations 2+the different photocurrent values that deposit solution produces, drawing curve;
(5) Cd is replaced with testing sample 2+standard solution, carries out sample detection according to the method for (1) ~ (4).
CN201510245145.2A 2015-05-14 2015-05-14 A kind of preparation method and application of the Optical Electro-Chemistry sensor of Sensitive Detection Cd2+ based on ZnO and CdS composite semiconductor material Expired - Fee Related CN104820006B (en)

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CN114264706A (en) * 2021-10-13 2022-04-01 河海大学 P-benzoquinone detection and analysis method based on photocathode sensor

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN105651836A (en) * 2016-02-26 2016-06-08 浙江大学 Self-driven all-solid-state glucose biosensor and preparation method thereof
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CN105806911A (en) * 2016-05-09 2016-07-27 曲阜师范大学 ZnO-Au@CdS photoelectric composite material as well as preparation method and application thereof
CN105806911B (en) * 2016-05-09 2018-04-13 曲阜师范大学 A kind of ZnO Au@CdS photoelectricity composite materials and its preparation method and application
CN107988615A (en) * 2017-11-08 2018-05-04 常州大学 A kind of preparation and application of carbonitride modification ZnO/CdS light anode materials
CN114264706A (en) * 2021-10-13 2022-04-01 河海大学 P-benzoquinone detection and analysis method based on photocathode sensor
CN114264706B (en) * 2021-10-13 2022-10-21 河海大学 P-benzoquinone detection and analysis method based on photocathode sensor

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