CN102701264A - Combining method of Ag2S photoelectric detection material - Google Patents

Combining method of Ag2S photoelectric detection material Download PDF

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CN102701264A
CN102701264A CN2012101152233A CN201210115223A CN102701264A CN 102701264 A CN102701264 A CN 102701264A CN 2012101152233 A CN2012101152233 A CN 2012101152233A CN 201210115223 A CN201210115223 A CN 201210115223A CN 102701264 A CN102701264 A CN 102701264A
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photoelectric detection
detection material
silver nitrate
stablizer
precursor solution
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CN102701264B (en
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杨皖实
王德军
谢腾峰
蒋腾飞
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Jilin University
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Jilin University
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Abstract

The invention relates to a combining method of a Ag2S photoelectric detection material and belongs to the technical field of preparation of inorganic compound semiconductor materials. The method includes mixing sulfocompound and silver nitrate according to the molar ratio of 3-4:1, adding a stabilizer into the mixture, dissolving the mixture into water to prepare mixed solution, conducting reaction for 4-6 hours under the condition of 160-180 DEG C and conducting washing, centrifuging and drying to obtain Ag2S photoelectric detection material powder. The sulfocompound is thiocarbamide or sodium thiosulfate preferably, and the stabilizer is lauryl sodium sulfate or glutathione preferably. The combining method adopts a hydrothermal synthesis method, and is simple in whole operation process, good in repeatability and low in cost. Prepared Ag2S has good photoelectric response characteristics-wide band and high photoelectric response and can be applied to optical detectors.

Description

A kind of Ag 2The compound method of S Photoelectric Detection material
Technical field
The present invention relates to a kind of wide wavelength response range, high light electroresponse Ag 2The hydrothermal synthesis method of S Photoelectric Detection material belongs to the technical field of inorganic compound semiconductor material prepn.
Background technology
Along with the development of photoelectric detecting technology, utilize the semiconductor light electrical property to carry out the light detecter for semiconductor of response transmission, have efficiently, advantage is widely used accurately.Response interval division according to the photodetector incident light can be divided into UV-detector, visible light detector, infrared detector etc.Because Si excellent photoelectric performance between visible region, the visible light detector of present stage is still with the core component of Si material as device.And the related element of the core material that near infrared and infrared light detector used; Mostly be the LP element; There has been the common material that is used for infrared light detection of report that the sosoloid HgCdTe that is made up of HgTe and two kinds of materials of CdTe, InGaAs series material and Ge are arranged xSi 1-xDeng semiconductor material, and the wavelength region that can detect from 0.8 micron to more than 10 microns, but the present near infrared of reporting and the detectivity of infrared light detector below 800nm are still limited.Ultraviolet light detector utilizes semiconductor material for passing through atmospheric absorption, is in below the wavelength 300nm---and the photoelectric response of the UV-light of so-called " day blind area " is prepared from.Like SiC, GaN, AlGaN, ZnO etc. are the sophisticated semiconductor materials of development preparation.Synthetic convenient, with low cost also is one of UV-detector reason of becoming the swiftest and the most violent light detecter for semiconductor of present stage development.
But the photoelectric response interval of above-mentioned materials all is in the single wavelength interval, and its response light scope becomes and limits the bottleneck that these semiconductor materials are further used.Can the photoelectric response ability all be arranged for all wave band light of infrared-visible-ultraviolet if be used for the semiconductor material of photodetector, its using value and range of application all can increase greatly.Therefore, select response interval wide in range, response efficiency is high, the preparation method simple and safe semiconductor material become key problem.
Ag 2S is as a kind of narrow bandgap semiconductor material; Because of it has good chemicalstability and light amplitude limit under normal temperature condition; Just as a kind of special ionic conductor; Can ion and electronics conduct electricity jointly, have the potentiality of application at photoelectric field, be applied in photoelectric device and the solar cell.Lot of domestic and foreign study group is for Ag 2The also many unfolded based on this of the research of S.
For Ag 2The synthesis preparation method of S, sophisticated reaction mechanism are that react under the modification of stablizer in sulphur source and silver-colored source.Y.D.Ling, et.al. utilize stearylamine as stablizer, and the S powder is the sulphur source, utilize the high-temperature solvent by the use of thermal means to prepare Ag 2The S nano wire, prepared Ag 2The S nano wire has the air-sensitive response characteristic for oxygen.But be solid-state under the stearylamine normal temperature, and the effect of act as solvents in reaction process, so being under the high temperature, the entire reaction manipulation require carries out, and this is for preparation equipment, and operation and environment requirement are higher, and present stage, its device using value was not high.
L.H.Dong, et.al. mention and utilize thiocarbamide to be the sulphur source, and CTAB is tensio-active agent prepares the cubes pattern through hydro-thermal synthetic method Ag 2The S nanostructure.W.S.Chin, et.al. then utilize hexadecylamine (HDA) respectively, octylame (OA), and quadrol (EDA), Di-Octyl amine organism stablizers such as (DOA) prepares Ag 2The S nanocrystal.The two chooses selection with reaction conditions for Ag with stablizer 2The control of S nanocrystal pattern is explored, but above-mentioned document is in order to pursue Ag 2The pattern of S material does not propose the easy reaction conditions of realizing, on the optimization setting in experimental temperature and reaction times, still needs further improvement.
Summary of the invention
The technical problem that the present invention will solve is, is with comparatively easy preparation means, optimization experiment temperature and reaction times, prepares the Ag with the strong response of wide band 2S semiconductor crystal material can be widely used in the photodetector it.
A kind of wide wavelength response range is provided, high light electroresponse Ag 2The S material preparation method behind the solution uniform mixing with Silver Nitrate and sulfocompound (thiocarbamide or Sulfothiorine) and stablizer, reacts under the high-temperature and high-pressure conditions of hydro-thermal, final synthetic have wide band, the Ag of high light electroresponse 2The S material.
Technical scheme of the present invention is following:
A kind of Ag 2The compound method of S Photoelectric Detection material, step is following:
With mol ratio 3～4: 1 sulfocompound and Silver Nitrate are raw material, and raw material and stablizer are added in the entry, and ultrasonic or magnetic agitation mixes it, precursor solution; Wherein, the consumption of stablizer is 0～0.15 times of Silver Nitrate mole number, and the consumption of water is calculated as 0.03～0.04mol/L by the concentration of Silver Nitrate;
The precursor solution of gained is transferred in the stainless steel cauldron of inner liner polytetrafluoroethylene, under 160～180 ℃ of conditions, reacted 4～6 hours, naturally cool to room temperature; Products therefrom alternately washs 4～6 times with redistilled water and ethanol, and is dry again after the spinning, obtains Ag 2The powder of S Photoelectric Detection material.
Described sulfocompound is thiocarbamide or Sulfothiorine.
Described stablizer can be the stablizer that prior art is used, a kind of in preferably sodium dodecyl sulfate of the present invention, the gsh.
The technical scheme of further optimizing is:
With 1: 3 Silver Nitrate of mol ratio and Sulfothiorine is raw material; Sodium lauryl sulphate with 0～0.1 times of Silver Nitrate mole number is a stablizer; Raw material and stablizer are added in the entry; The consumption of water is counted 0.03～0.04mol/L by the consumption of Silver Nitrate, and ultrasonic agitation mixes it, gets precursor solution; Precursor solution is transferred in the stainless steel cauldron that liner is a tetrafluoroethylene,, naturally cools to room temperature 160 ℃～180 ℃ following isothermal reactions 4～6 hours; Spinning after products therefrom alternately washs 4 times with redistilled water and absolute ethyl alcohol through dry, obtains Ag again 2The powder of S Photoelectric Detection material.
The another kind of technical scheme of optimizing is:
With mol ratio 1: 3～4 Silver Nitrates and thiocarbamide is raw material; Gsh with 0.15 times of Silver Nitrate mole number is that stablizer adds raw material and stablizer in the entry; The consumption of water is counted 0.03～0.04mol/L by the consumption of Silver Nitrate, and ultrasonic agitation mixes it, gets precursor solution; Precursor solution is transferred in the stainless steel cauldron that liner is a tetrafluoroethylene,, naturally cools to room temperature 180 ℃ of following isothermal reactions 4 hours; Spinning after products therefrom alternately washs 4 times with redistilled water and absolute ethyl alcohol through dry, obtains Ag again 2The powder of S Photoelectric Detection material.
A kind of preparation Ag that the present invention proposes 2The Ag that the method for S is prepared 2S has good photoelectric response characteristic (wide band, high light electroresponse), and can be applied in the photodetector.Characteristics such as this method has easy and simple to handle, and synthesis condition is gentle, and speed of response is fast, and cost is low.And character stable homogeneous.
Description of drawings
Fig. 1 is a kind of wide wavelength response range of embodiment 1 preparation, high light electroresponse Ag 2The X ray diffracting spectrum of S Photoelectric Detection material powder;
Fig. 2 is a kind of wide wavelength response range of embodiment 1 preparation, high light electroresponse Ag 2The UV, visible light of S Photoelectric Detection material powder absorbs collection of illustrative plates;
Fig. 3 is a kind of wide wavelength response range of embodiment 1 preparation, high light electroresponse Ag 2The surface photovoltage spectrogram of S Photoelectric Detection material powder.
Fig. 4 is a kind of wide wavelength response range of embodiment 2 preparations, high light electroresponse Ag 2The X ray diffracting spectrum of S Photoelectric Detection material powder;
Fig. 5 is a kind of wide wavelength response range of embodiment 2 preparations, high light electroresponse Ag 2The UV, visible light of S Photoelectric Detection material powder absorbs collection of illustrative plates;
Fig. 6 is a kind of wide wavelength response range of embodiment 2 preparations, high light electroresponse Ag 2The surface photovoltage spectrogram of S Photoelectric Detection material powder.
Fig. 7 is a kind of wide wavelength response range of embodiment 3 preparations, high light electroresponse Ag 2The X ray diffracting spectrum of S Photoelectric Detection material powder;
Fig. 8 is a kind of wide wavelength response range of embodiment 3 preparations, high light electroresponse Ag 2The UV, visible light of S Photoelectric Detection material powder absorbs collection of illustrative plates;
Fig. 9 is a kind of wide wavelength response range of embodiment 3 preparations, high light electroresponse Ag 2The surface photovoltage spectrogram of S Photoelectric Detection material powder.
Figure 10 is for build surface photovoltage commercial measurement system architecture synoptic diagram certainly.
Embodiment
Below in conjunction with embodiment the present invention is further specified, but be not limited thereto.
The embodiment of the invention is raw materials used to be commercial analytical pure product, is not further purified before the use.
The wide wavelength response range of embodiment of the invention preparation, high light electroresponse Ag 2The thing of S Photoelectric Detection material powder is mutually through X-ray diffraction spectra (XRD) test (XRD, Rigaku Max-2550).
The wide wavelength response range of embodiment of the invention preparation, high light electroresponse Ag 2The ultraviolet-visible absorption spectroscopy of S Photoelectric Detection material powder through the uv-vis spectra scanner test (Shimadzu, UV-3600).
The wide wavelength response range of embodiment of the invention preparation, high light electroresponse Ag 2The surface photovoltage of S Photoelectric Detection material powder is measured through building surface photovoltage commercial measurement system certainly.Device is formed referring to Figure 10, and concrete: light source is a 500W xenon lamp (CHF-XQ500W Global xenon lamp power), and (Omni-5007, No.09010 Zolix) obtain monochromatic ray through grating monochromator.For lock phase photovoltaic technology, use Stanford chopper (Model SR540) modulated monochromatic light, modulating frequency is 20-70Hz, uses Stanford lock-in amplifier (Model SR830-DSP Lock-in Amplifier) to carry out the photovoltaic signal and amplifies.The sweep velocity of computer control monochromator, and use the lock-in amplifier image data.Spectral resolution is 1nm.
Measuring principle and method are: the monochromatic ray that light-source system provides is radiated at the material sample surface, and the light induced electron of generation separates under the effect of separation mechanism with the hole, forms photosignal, and signal is by the lock-in amplifier collection.Measured signal is a surface photovoltage intensity, and its intensity is relevant with the isolating quantity of photogenerated charge electron-hole pair.
Embodiment 1, a kind of wide wavelength response range, high light electroresponse Ag 2The hydrothermal synthesis method of S Photoelectric Detection material, step is following:
Take by weighing 1 mmole Silver Nitrate, 3 mmole Sulfothiorine, 0.1 mmole sodium lauryl sulphate, 30 ml waters respectively, ultrasonic agitation mixes it, gets precursor solution;
The precursor solution of step 1) gained is transferred in the stainless steel cauldron that liner is a tetrafluoroethylene; 180 ℃ of following isothermal reactions 4 hours; After finishing, reaction naturally cools to room temperature; Products therefrom is used spinning behind redistilled water and the absolute ethanol washing 4 times at ambient temperature, after the product drying after the separation, promptly obtains Ag 2The powder of S Photoelectric Detection material.
Present embodiment synthetic Ag 2The X ray diffracting spectrum of S Photoelectric Detection material powder is seen Fig. 1, synthetic Ag 2The UV, visible light of S Photoelectric Detection material powder absorbs collection of illustrative plates and sees Fig. 2, synthetic Ag 2The surface photovoltage spectrogram of S Photoelectric Detection material powder is seen Fig. 3.
Embodiment 2, a kind of wide wavelength response range, high light electroresponse Ag 2The hydrothermal synthesis method of S Photoelectric Detection material, step is following:
Take by weighing 1 mmole Silver Nitrate, 3 mmole thiocarbamides, 0.15 mmole gsh, 30 ml waters respectively, ultrasonic agitation mixes it, gets precursor solution;
The precursor solution of step 1) gained is transferred in the stainless steel cauldron that liner is a tetrafluoroethylene; 180 ℃ of following isothermal reactions 4 hours; After finishing, reaction naturally cools to room temperature; Spinning after products therefrom alternately washs 4 times with redistilled water and absolute ethyl alcohol at ambient temperature after the product drying after the separation, promptly obtains Ag 2The powder of S Photoelectric Detection material.
Present embodiment synthetic Ag 2The X ray diffracting spectrum of S Photoelectric Detection material powder is seen Fig. 4, synthetic Ag 2The UV, visible light of S Photoelectric Detection material powder absorbs collection of illustrative plates and sees Fig. 5, synthetic Ag 2The surface photovoltage spectrogram of S Photoelectric Detection material powder is seen Fig. 6.
Embodiment 3, a kind of wide wavelength response range, high light electroresponse Ag 2The hydrothermal synthesis method of S Photoelectric Detection material, step is following:
Take by weighing 1 mmole Silver Nitrate, 3 mmole Sulfothiorine, 30 ml waters respectively, ultrasonic agitation mixes it, gets precursor solution;
The precursor solution of step 1) gained is transferred in the stainless steel cauldron that liner is a tetrafluoroethylene; 180 ℃ of following isothermal reactions 4 hours; After finishing, reaction naturally cools to room temperature; Spinning after products therefrom alternately washs 4 times with redistilled water and absolute ethyl alcohol at ambient temperature after the product drying after the separation, promptly obtains Ag 2The powder of S Photoelectric Detection material.
Present embodiment synthetic Ag 2The X ray diffracting spectrum of S Photoelectric Detection material powder is seen Fig. 7, synthetic Ag 2The UV, visible light of S Photoelectric Detection material powder absorbs collection of illustrative plates and sees Fig. 8, synthetic Ag 2The surface photovoltage spectrogram of S Photoelectric Detection material powder is seen Fig. 9.
Embodiment 4, a kind of wide wavelength response range, high light electroresponse Ag 2The hydrothermal synthesis method of S Photoelectric Detection material, step is following:
Take by weighing 1 mmole Silver Nitrate, 4 mmole thiocarbamides, 0.15 mmole gsh, 30 ml waters respectively, ultrasonic agitation mixes it, gets precursor solution;
The precursor solution of step 1) gained is transferred in the stainless steel cauldron that liner is a tetrafluoroethylene; 180 ℃ of following isothermal reactions 4 hours; After finishing, reaction naturally cools to room temperature; Spinning after products therefrom alternately washs 4 times with redistilled water and absolute ethyl alcohol at ambient temperature after the product drying after the separation, promptly obtains Ag 2The powder of S Photoelectric Detection material.Products therefrom XRD, UV, visible light absorb and surface photovoltage characterizes with embodiment 2 basic identical.
Embodiment 5, a kind of wide wavelength response range, high light electroresponse Ag 2The hydrothermal synthesis method of S Photoelectric Detection material, step is following:
Take by weighing 1 mmole Silver Nitrate, 3 mmole Sulfothiorine, 0.1 mmole sodium lauryl sulphate, 30 ml waters respectively, ultrasonic agitation mixes it, gets precursor solution;
The precursor solution of step 1) gained is transferred in the stainless steel cauldron that liner is a tetrafluoroethylene; 160 ℃ of following isothermal reactions 6 hours; After finishing, reaction naturally cools to room temperature; Spinning after products therefrom alternately washs 4 times with redistilled water and absolute ethyl alcohol at ambient temperature after the product drying after the separation, promptly obtains Ag 2The powder of S Photoelectric Detection material.Products therefrom XRD, UV, visible light absorb and surface photovoltage characterizes with embodiment 1 basic identical.

Claims (5)

1. Ag 2The compound method of S Photoelectric Detection material, step is following:
With mol ratio 3～4: 1 sulfocompound and Silver Nitrate are raw material, and raw material and stablizer are added in the entry, and ultrasonic or magnetic agitation mixes it, precursor solution; Wherein, the consumption of stablizer is 0～0.15 times of Silver Nitrate mole number, and the consumption of water is calculated as 0.03～0.04mol/L by the concentration of Silver Nitrate;
The precursor solution of gained is transferred in the stainless steel cauldron of inner liner polytetrafluoroethylene, under 160～180 ℃ of conditions, reacted 4～6 hours, naturally cool to room temperature; Products therefrom alternately washs 4～6 times with redistilled water and ethanol, and is dry again after the spinning, obtains Ag 2The powder of S Photoelectric Detection material.
2. a kind of Ag according to claim 1 2The compound method of S Photoelectric Detection material is characterized in that, described sulfocompound is thiocarbamide or Sulfothiorine.
3. a kind of Ag according to claim 1 and 2 2The compound method of S Photoelectric Detection material is characterized in that, described stablizer is sodium lauryl sulphate or gsh.
4. a kind of Ag according to claim 1 2The compound method of S Photoelectric Detection material; It is characterized in that, be raw material with 1: 3 Silver Nitrate of mol ratio and Sulfothiorine, is stablizer with the sodium lauryl sulphate of 0～0.1 times of Silver Nitrate mole number; Raw material and stablizer are added in the entry; The consumption of water is counted 0.03～0.04mol/L by the consumption of Silver Nitrate, and ultrasonic agitation mixes it, gets precursor solution; Precursor solution is transferred in the stainless steel cauldron that liner is a tetrafluoroethylene,, naturally cools to room temperature 160 ℃～180 ℃ following isothermal reactions 4～6 hours; Spinning after products therefrom alternately washs 4 times with redistilled water and absolute ethyl alcohol through dry, obtains Ag again 2The powder of S Photoelectric Detection material.
5. a kind of Ag according to claim 1 2The compound method of S Photoelectric Detection material; It is characterized in that; With mol ratio 1: 3～4 Silver Nitrates and thiocarbamide is raw material, is that stablizer adds raw material and stablizer in the entry with the gsh of 0.15 times of Silver Nitrate mole number, and the consumption of water is counted 0.03～0.04mol/L by the consumption of Silver Nitrate; Ultrasonic agitation mixes it, gets precursor solution; Precursor solution is transferred in the stainless steel cauldron that liner is a tetrafluoroethylene,, naturally cools to room temperature 180 ℃ of following isothermal reactions 4 hours; Spinning after products therefrom alternately washs 4 times with redistilled water and absolute ethyl alcohol through dry, obtains Ag again 2The powder of S Photoelectric Detection material.
CN201210115223.3A 2012-04-19 2012-04-19 Combining method of Ag2S photoelectric detection material Expired - Fee Related CN102701264B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106995482A (en) * 2017-03-17 2017-08-01 安徽大学 A kind of preparation with hyperfluorescence material and its to Fe 3+Selective response
CN107746070A (en) * 2017-09-21 2018-03-02 东华大学 A kind of preparation method of oil-soluble vulcanization silver nano material
CN109054812A (en) * 2018-08-24 2018-12-21 南京邮电大学 A kind of method that water phase prepares two area's fluorescence silver sulfide quantum dot of near-infrared

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘皑若 等: "管状微纳米Ag2S晶体的水热法制备方法研究", 《化工时刊》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106995482A (en) * 2017-03-17 2017-08-01 安徽大学 A kind of preparation with hyperfluorescence material and its to Fe 3+Selective response
CN107746070A (en) * 2017-09-21 2018-03-02 东华大学 A kind of preparation method of oil-soluble vulcanization silver nano material
CN109054812A (en) * 2018-08-24 2018-12-21 南京邮电大学 A kind of method that water phase prepares two area's fluorescence silver sulfide quantum dot of near-infrared
CN109054812B (en) * 2018-08-24 2021-06-22 南京邮电大学 Method for preparing near-infrared two-region fluorescent silver sulfide quantum dots in water phase

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