CN108760629A - A kind of preparation method and applications of multi-metal oxygen cluster functionalization cadmium sulfide nano wires sensor array - Google Patents
A kind of preparation method and applications of multi-metal oxygen cluster functionalization cadmium sulfide nano wires sensor array Download PDFInfo
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- CN108760629A CN108760629A CN201810496318.1A CN201810496318A CN108760629A CN 108760629 A CN108760629 A CN 108760629A CN 201810496318 A CN201810496318 A CN 201810496318A CN 108760629 A CN108760629 A CN 108760629A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
Abstract
The invention discloses a kind of preparation method and applications of multi-metal oxygen cluster functionalization cadmium sulfide nano wires sensor array, cross multi-metal oxygen cluster modification, specific recognition accumulation ability of the material to drugs is improved, the detection sensitivity of single photoelectric sensor is improved and shortens the response time；It is constructed by sensor array, increases cross-sensitivity of the sensor array to variety classes drugs.By this project implementation, it is expected that structure is based on a kind of nano photoelectric gas sensor array, enhancing sensing primitive is to structure similar to the response discrimination of drugs, it realizes and the contactless identification of common drugs opium, heroin, methamphetamine, ketamine, ***e is detected, sensitive material basis is established for portable drugs survey meter.It can be applied to accurate, non-contact detection towards hiding trace drugs.
Description
Technical field
The invention belongs to technical field of chemistry, are related to one kind and can be used for contactless drugs atmosphere detection sensor array preparation
Method and its application.
Background technology
Mainly have about the detection technique of drugs both at home and abroad：1) electrochemical assay：Such as 2012, Aso Navaee1 were sharp
Morphine, coscopin, heroin are detected simultaneously with graphene nanometer sheet modified glassy carbon electrode, this method is reported for the first time based on him
Electrochemical oxidation characteristic simultaneously measure three kinds of drugs；2013, Zhengzhou University Baoxian Ye etc. manufactured a kind of new
Morphine electrochemical sensor based on composite graphite alkene and perfluorinated sulfonic acid membrane modifying glass-carbon electrode, hence it is evident that improve its sensibility；
Toshiyasu etc. is realized using chiral capillary electrophoretic techniques/bis- mass-spectrometric techniques of chemical modification to amphetamine substance
Detection.2) chromatography：Such as The 2nd Army Medical College Feng Lu are by thin-layer chromatography (TLC) and surface enhanced Raman technique
(SERS) it combines, realizes the Site Detection for adding illegal drug in food；In addition, chromatography (GC-MS), height is used in conjunction using makings
The qualitative and quantitative analysis to most drugs can be achieved in the technologies such as effect liquid phase chromatogram (HPLC).3) spectroscopic methodology：Such as the Chinese Academy of Sciences
Hefei Yang Liangbao researcher seminar of intelligent machine research institute is with NaYF4:Yb,Er@SiO2@Ag are SERS active-substrate, close red
Under outer light excitation, the highly sensitive detection of p-Methylamphetamine (methamphetamine) is realized；Shohre etc. loads a kind of thiophene derivant
To SiO2Nanometer ball surface, the detection to crystal methamphetamine in solution is realized using fluorescence spectroscopy technique.Raman spectroscopy
To common drugs such as amphetamine sulfate, meth hydrochloride, morphine hydrochloride, Heroinhydrochlorides.Pass through analysis ratio
Compared with Raman line, it is possibility to have effect distinguishes drug species, can complete the important chemical raw material Chinese ephedra of synthesis " methamphetamine " at the scene
The Raman non-destructive testing analysis of element and the levamisol for pretending to be ephedrine synthesis " methamphetamine ", can also realize whether take illicit drug
The quick detection of object and drugs.4) immunoassay：1979, Baumgartner etc. was successfully detected with radioimmunoassays for the first time
Heroin and its metabolite in drug addict's hair, and thus carried out the deduction of medication period to drug addict.Thereafter, enzyme
Connection is immune, colloidal gold method is widely applied in drugs identification field.5) Ion mobility spectrometry (IMS)：IMS not only can be with
It realizes the detection to drugs trace particle, the synthetic drug in human hair can also be detected.
Although the above method can realize qualitative analysis to drugs such as opium, heroin, methamphetamine, ketamines, however, these
Method also has shortcoming, and such as the X-ray detection of technology maturation, instrument is heavy, expensive, and there are radiation risks.Chromatography
Analysis method is generally only applicable to lab samples detection, cannot meet the purpose of field quick detection.Immunoassay rule is more
For the detection of drugs in urine, saliva, blood, hair, it is intended to whether judging that related personnel takes drugs.In addition, the above method is equal
For contact measurement, and it is most need to complete in laboratory, have portable, contactless trace drugs steam detection method fresh
It has been reported that.And peddle with criminal of drugs transport's crime be China's Drug-related crimes principal mode, and Stealth Modus is strange changeable, therefore,
In transit and the contactless quick detection identification of malicious live drug hidden is made and trafficed for drugs, is one and has much challenge
Project.And the solution of the problem will confirm that drugs, evidence obtaining provides facility in time for prohibition of drug department scene.Currently, Shaanxi is pedagogical big
It learns professor Fang Yu and develops a kind of self assembly fluorescence membrane PDC, realize p-Methylamphetamine analogies (N- methyl -2- benzene second
Amine) detection, detection limit be about 5.5ppb.Shanghai micro-system institute of Chinese Academy of Sciences Cheng Jiangong researcher has synthesized two kinds of fluorescent moleculars
FBT and PFT utilizes " Fluorescence Increasing (turn-on) " principle to be realized respectively to 1.9ppm and 6.4ppm crystal methamphetamine atmosphere
Selective enumeration method.Angelika etc. then realizes the inspection to amphetamine class drugs atmosphere using surface ionization detection technique
It surveys.Bouchikhi etc. has constructed a kind of hand-hold electric nasus of low cost using metal oxide, realizes and contains poisonous substance to five kinds
The detection and classification of matter (hemp bud, cannabis plants, Cannador, snuff and Tobacco Leaf).Andreas etc. also devises one
Kind is based on metal oxide (SnO2) gas sensor electronic nose, can pass through human skin detect hemp metabolism product.
However still lack for the selective enumeration method means of variety classes drugs atmosphere.
Currently, the gas sensor based on nano material have it is small, low energy consumption, high sensitivity, response it is fast, non-contact
The advantages that, the deficiency of traditional sensing techniques is compensated for, there is important application value in trace illicit drugs inspection.Wherein, it partly leads
Body nano wire by its big specific surface area and with the comparable breadth wise dimension of Debye length, simple and large batch of production work
Many advantages outstanding such as skill, the higher stability of nano crystal, lower operating temperature, which become, prepares high performance air-sensitive biography
The ideal material of sensor.Relative to traditional thin film materials, semiconductor nanowires gas sensor has the advantages that following：(i)
The dimension of micro-nano size is conducive to reduce sensor bulk, improves integrated level, reduces power consumption and cost；(ii) big table volume ratio
Be conducive to the Rapid Accumulation of charge with high surface-active, improve response speed and sensitivity；High quality of materials can be minimum
Lattice scattering and the capture of defect trap for changing carrier, are conducive to the minor change for detecting crystal face gas absorption, improve detection spirit
Sensitivity.These advantages solve stability present in conventional semiconductors gas sensor, reproducibility and work in a way
Make the problems such as temperature is high；(iii) since it has high crystalline quality, crystal boundary is there's almost no, therefore, can be efficiently reduced
Unstability caused by jump between lattice.
Cadmium sulfide nano wires (CdS NWs) are a kind of good semi-conducting materials, due to its unique physics and chemically
Matter has made solar cell, photonic crystal, photocatalysis, gas sensor, the fields such as electrochromism and self-cleaning material
One of material studied extensively.However, the separative efficiency of its photo-generated carrier it is relatively low be hinder one of the Materials it is important
Factor.In addition, simple nano material easily assembles and (influences gas absorption and diffusion).Passing through principal component analysis, sensitive material
There are problems that response signal overlapping to the response signal otherness very little of drugs, or even part.Easily by ring in practical application
Border influences, and be easy to cause sensor and reports by mistake, reason is that the nano material of surface exposure is difficult to meet qualitative recognition not
With the current demand of drugs.It is reported that in US airports, sensor rate of false alarm reduces 90%, will save 2.5 hundred million dollars of expenditures.
Therefore, by the nano-sensor of surface modification, the purpose of enrichment (or isolation) certain components is on the one hand can reach, on the other hand
The signal difference that different component in mixing drugs can then be amplified has sensor practical application to reduce sensor rate of false alarm
It is significant.
Oxometallate (Polyoxometalate, POM), also known as metal-oxygen cluster compound, be one kind by molybdenum, tungsten etc. before
Transition metal connects the inorganic metal oxygen cluster to be formed by oxygen bridge.Their necessary architectural characteristics are that there are the dual ends of metal-oxygen
Key in polyanionic surface, thus inhibits further bonding so as to cause with weakly alkaline atomic oxygen distribution.POM is one
The good electron acceptor of kind, when receiving a large amount of electronics, its structure can keep being basically unchanged.In addition, POM has redox
The adjustable denaturation of active and higher thermal stability and structure.With the change that heteropoly compound forms, redox electricity
Gesture changes correspondingly so that electrocatalysis characteristic is controllable.Typical polyacid is mostly nano-grade size, and particle is uniform, and grain size is not present
Distribution.POM types are various, and structure is changeable, are the compounds of a kind of substantial amounts.From the point of view of geometry angle, polyacid molecule is logical
It is often to be combined with each other as basic construction unit by the polyhedron of some rules or half rule.It is basic just because of these
The planform of construction unit is various, combination is changeable, just give chemists design synthesize when flexible and changeable choosing
Select, can obtain with previous completely different molecular structure, also so that polyacid Inorganic synthese field have without and human relations
The advantage of ratio.Meanwhile the application study of polyacid compound almost relates to all fields, such as catalysis, light, sulfate ferroelectric functional material with
And pharmaceutical chemistry.
POM can effectively capture light induced electron, inhibit answering for electrons and holes as a kind of good electronics capturing agent
It closes, improves photocatalysis and the photoelectric properties of CdS nanostructures.In addition, a large amount of hapto in the surfaces POM (coordination site) can be into one
Step improves the adsorption site of nanosensor primitive, alternative enrichment complex component drug numerator, and passes through electric charge transfer, surface
The mechanism such as light-catalyzed reaction distinguish the signal of different drug numerators, reach selective enumeration method drugs, especially multicomponent drugs point
The purpose of son.Effective synthetic method is researched and developed, by polyacid and semi-conducting material by forming the shapes such as covalent bond or coordinate bond
What formula was more stablized be combined with each other, and so that electrons and holes is efficiently generated and is shifted between acceptor and donor, to carry
The transfer efficiency of high semi-conducting material has important theory significance；Polyacid modifying semiconductor is detected for drugs steam, will be opened up
Open up application range of the polyacid as photoelectric functional material
POM with different energy levels and property is modified by Coordination interaction to CdS nanostructured surfaces (CdS@
POMs), one group of sensor array can be constructed.It is different that sensor array can utilize each sensor to respond complicated ingredient gas
The characteristics of and principal component analysis, qualitative recognition different atmosphere may be implemented.However, response difference of the material to different atmosphere itself
Size is still the basic guarantee of later stage principle component analysis data point discreteness quality.Therefore, a series of surface modifications are constructed
Nano material, give full play to surface modification and Photoelectric Detection cooperates with advantage, the surface modification method that will be detected for photoelectricity atmosphere
Developing brings new intension.
Invention content
It is an object of the invention to overcome defect existing in the prior art, atmosphere drugs photoelectric sensing material is further increased
The sensitivity of material is realized and is amplified to common drugs signal difference, provides a kind of multi-metal oxygen cluster functionalization cadmium sulfide nano wires
The preparation method and applications of sensor array.Using photoelectric sensing detection method, mating surface modification technique, sensor array structure
It builds and principal component analysis technology, preparing and build can the common drugs photosensor arrays of qualitative recognition.POM introducings CdS is received
Rice body structure surface, 1) intensity that electron-hole detaches, improves photoelectric current can be effectively facilitated, it is rung to improve sensitivity and shorten
Between seasonable；2) specific recognition accumulation ability of the material to drugs can be improved, improve the detection sensitivity of single photoelectric sensor；
3) cross-sensitivity of sensor array can be increased, realize that especially multicomponent mixing drugs atmosphere is qualitative to common drugs
Identification.This research by for trace atmosphere drugs in real time, the research of qualitative detection technology new thinking is provided.
Its specific technical solution is：
A kind of preparation method of multi-metal oxygen cluster functionalization cadmium sulfide nano wires sensor array, includes the following steps：
A) synthesis of multi-metal oxygen cluster
B) preparation of CdS nanostructures
Cadmium nitrate and thiocarbamide are added in ethylenediamine, and CdS nano wires are obtained by hydrothermal method, and pattern is characterized by SEM,
Its crystal form of XRD characterization；
C) the multi-metal oxygen cluster functionalization of CdS nanostructures
Using the strong coordination ability of multi-metal oxygen cluster end oxygen, by different quality ratio (1:1-1:20) multi-metal oxygen cluster with
CdS nanostructures ultrasound 30min in aqueous solution, obtains the CdS nanostructures of multi-metal oxygen cluster in-situ modification, multi-metal oxygen cluster
The CdS nanostructures of functionalization are handled in 120 DEG C of oven dryings, and fourier infrared converts absorption spectrum, ultra-violet absorption spectrum table
Levy the surface modification situation of CdS nanostructures；
D) appropriate CdSNWs@POMs and water are mixed, is ground into uniform paste in the agate mortar.It is stained with small writing brush
Suitable pasty mass is taken, is uniformly applied on electrode slice, film is formed.Film thickness is determined by the number smeared.Later will
The substrate for being coated with material places natural drying in air one day to get the photoelectric sensing built to CdS/ZnO core-shell nano lines
Device and gas sensor, electrode slice are inserted Ag-Pd electrodes by aluminium oxide ceramics substrate and finger and are constituted, and several electrode slice parallel connections, which are constituted, to be passed
Sensor array.
Further, the mass ratio of CdSNWs@POMs water mixing is 4：1.
Further, the size of foundation base of aluminium oxide ceramics substrate is 13.4mm × 7mm × 0.6mm, refers to slotting width and spacing
It is 20 μm.
Multi-metal oxygen cluster functionalization cadmium sulfide nano wires sensor array prepared by the present invention is during illicit drugs inspection
Using.
Compared with prior art, beneficial effects of the present invention：
The present invention selects CdS nano wires as Photo-electric gas-sensitivity sensing material, for the type of different drugs, in sensing material
Different types of multi-metal oxygen cluster is modified on surface respectively.Sensor array is built on this basis, during principal component analysis
Increase different drugs signal differences and reduces signal discrete degree.Multi-metal oxygen cluster functionalization cadmium sulfide prepared by the present invention is received
Rice noodles sensor array has the characteristics that signaling zone indexing is big, rate of false alarm is low, can realize to opium, heroin, methamphetamine, ketamine,
The qualitative recognition of the common drugs atmosphere such as ***e, head-shaking pill, hemp.
Description of the drawings
Fig. 1 is that sensor array constructs (left side) and sensing primitive (right side) schematic diagram；
Fig. 2 is drugs photoelectric detection system schematic diagram, wherein 1 is ceramic bases, and 2 be comb electrode, and 3 be multi-metal oxygen
The CdS nanostructures of cluster functionalization sense primitive, and 4 be power supply, and 5 be ammeter, and 6 be light source.
Specific implementation mode
Technical scheme of the present invention is described in more detail with specific embodiment below in conjunction with the accompanying drawings.
1) the CdS nanostructures sensing primitive of multi-metal oxygen cluster functionalization is constructed
A) synthesis of multi-metal oxygen cluster
Multi-metal oxygen cluster of the reference literature synthesis with different catalytic performances and different energy levels, including：H3PW12O40
(PW12),H4SiW12O40(SiW12),H4GeW12O40(GeW12),K6CoW12O40(CoW12),H3PMo12O40(PMo12),
H3SiMo12O40(SiMo12),H3GeMo12O40(GeMo12),H6P2Mo18O62(P2Mo18),K6P2W18O62(P2W18),K8SiW11O39
(SiW11),K10P2W17O61·20H2O(P2W17),H9P2W15V3(P2W15V3),SiW9Co3。
By taking PW12 is synthesized as an example, principle is：
12Na2WO4·2H2O+H3PO4+24HCl→H3PW12O40+24NaCl+36H2O
Specifically, by 100g Na2WO4·2H2O is dissolved in 100ml water, and being heated to boiling makes its hydrolysis, and 10ml 85% is added
H3PO4.Then the dense HCl of 80ml are added, it is cooling.Crystal precipitation to be had is filtered under diminished pressure to as dry as possible, ether, dense HCl extractions
It takes repeatedly, bottom etherate is transferred to another beaker, and 10ml water is added, and heating water bath obtains white to there is crystal precipitation
H3PW12O40, i.e. PW12。
The synthetic method of other multi-metal oxygen clusters is roughly the same, specific synthetic method can refer to document (J.Biol.Chem.,
1920,43,189-220)。
B) preparation of CdS nanostructures
Cadmium nitrate and thiocarbamide are added in ethylenediamine, obtain CdS nano wires by hydrothermal method, specific preparation method can join
According to document (ACS applied materials&interfaces, 2011,3,2253-2258).Pattern, XRD are characterized by SEM
Characterize its crystal form.
C) the multi-metal oxygen cluster functionalization of CdS nanostructures
Using the strong coordination ability of multi-metal oxygen cluster end oxygen, the multi-metal oxygen cluster of different proportion and CdS nanostructures are existed
Ultrasound 30min in aqueous solution, obtains the CdS nanostructures of multi-metal oxygen cluster (passing through Coordination interaction) in-situ modification.It is extra
Multi-metal oxygen cluster through washing process.The CdS nanostructures of multi-metal oxygen cluster functionalization are handled in 120 DEG C of oven dryings.Fourier
The surface modification situation of the infrared transformation absorption spectrum of leaf, ultra-violet absorption spectrum characterization CdS nanostructures.
2) drugs photoelectric sensing array is constructed and Performance Evaluation
A) construction method of senser element
Appropriate CdSNWs@POMs and water are mixed, the mass ratio of the two is 4：1.It is ground into the agate mortar uniform
Paste.Suitable pasty mass is picked with small writing brush, is uniformly applied on electrode slice, film is formed.Film thickness is by smearing
Number determine.The substrate for being coated with material is placed later and spontaneously dries one day in air to get to CdS/ZnO core-shell nanos
The photoelectric sensor and gas sensor of line structure.Electrode slice inserts Ag-Pd electrodes by aluminium oxide ceramics substrate and finger and constitutes (substrate
Size is 13.4mm × 7mm × 0.6mm, and it is 20 μm to refer to slotting width and spacing).Several electrode slice parallel connections constitute sensor array
Row.As shown in Figure 1.
B) photoelectric properties are tested
Sensor is built by primitive of the multi-metal oxygen cluster functionalization CdS nanostructures of above-mentioned preparation, to CdS nanostructures
(including I-V characteristic, the I-t under different radiation wavelengths are special with the photoelectric properties of the CdS nanostructures of multi-metal oxygen cluster functionalization
Property, response time, recovery time etc.) it is tested.Investigate the front and back photoelectric properties variation of multi-metal oxygen cluster modification.
C) air-sensitive performance is tested
Light source is selected, tests photoelectric respone of the sensor under different drugs steams and different drugs vapor concentrations respectively
Curve, and calculate response magnitude.Different sensing primitives is investigated under the conditions of dark condition and light to common drugs in above-mentioned 12
The response characteristic of saturated vapour pressure at room temperature.Test device is as shown in Figure 2.
3) data analysis and processing
Sensor is passed through into principal component analysis to a series of response datas of different drug numerators saturated vapor at room temperature
Method is converted to principal component analysis figure, obtains different drugs corresponding region different in principal component analysis figure, investigates multi-metal oxygen
The variation of the front and back Cluster zone (signal) of cluster modification.According to area distribution, sensor array is advanced optimized.Sensor array passes through
Repeatedly optimization obtains one group of sensor array combination that response signal difference is big, dispersion degree is small.Pass through transducing signal again group
It closes, establishes different drugs response databases.
The foregoing is only a preferred embodiment of the present invention, protection scope of the present invention is without being limited thereto, it is any ripe
Those skilled in the art are known in the technical scope of present disclosure, the letter for the technical solution that can be become apparent to
Altered or equivalence replacement are each fallen in protection scope of the present invention.
Claims (4)
1. a kind of preparation method of multi-metal oxygen cluster functionalization cadmium sulfide nano wires sensor array, which is characterized in that including following
Step：
A) synthesis of multi-metal oxygen cluster
B) preparation of CdS nanostructures
Cadmium nitrate and thiocarbamide are added in ethylenediamine, and CdS nano wires are obtained by hydrothermal method, and pattern, XRD are characterized by SEM
Characterize its crystal form；
C) the multi-metal oxygen cluster functionalization of CdS nanostructures
Using the strong coordination ability of multi-metal oxygen cluster end oxygen, by different quality than 1:1-1:20 multi-metal oxygen cluster with CdS nanometers
Structure ultrasound 30min in aqueous solution, obtains the CdS nanostructures of multi-metal oxygen cluster in-situ modification, extra multi-metal oxygen cluster
Through washing process, the CdS nanostructures of multi-metal oxygen cluster functionalization are handled in 120 DEG C of oven dryings, and fourier infrared transformation is inhaled
Receive spectrum, ultra-violet absorption spectrum characterizes the surface modification situation of CdS nanostructures；
D) appropriate CdSNWs@POMs and water are mixed, is ground into uniform paste in the agate mortar；It is picked with small writing brush suitable
The pasty mass of amount, is uniformly applied on electrode slice, forms film；Film thickness is determined by the number smeared；It will be coated with later
The substrate of material place spontaneously dry in air one day to get photoelectric sensor build to CdS/ZnO core-shell nano lines with
Gas sensor, electrode slice are inserted Ag-Pd electrodes by aluminium oxide ceramics substrate and finger and are constituted, and several electrode slice parallel connections constitute sensors
Array.
2. the preparation method of multi-metal oxygen cluster functionalization cadmium sulfide nano wires sensor array according to claim 1, special
Sign is that the mass ratio of CdSNWs@POMs water mixing is 4：1.
3. the preparation method of multi-metal oxygen cluster functionalization cadmium sulfide nano wires sensor array according to claim 1, special
Sign is that the size of foundation base of aluminium oxide ceramics substrate is 13.4mm × 7mm × 0.6mm, and it is 20 μm to refer to slotting width and spacing.
4. the multi-metal oxygen cluster functionalization cadmium sulfide nano wires sensor array prepared by claim any one of 1-3 is in illicit drugs inspection
Application in the process.
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| CN113406155A (en) * | 2021-06-23 | 2021-09-17 | 长春理工大学 | Tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material and preparation method thereof |
| CN115032335A (en) * | 2022-05-17 | 2022-09-09 | 广州铂鑫科技有限公司 | Fixed drug-arresting detector |
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| CN113406155A (en) * | 2021-06-23 | 2021-09-17 | 长春理工大学 | Tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material and preparation method thereof |
| CN113406155B (en) * | 2021-06-23 | 2022-08-05 | 长春理工大学 | Tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material and preparation method thereof |
| CN115032335A (en) * | 2022-05-17 | 2022-09-09 | 广州铂鑫科技有限公司 | Fixed drug-arresting detector |
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