CN108132237A - A kind of detection method containing sulfur photoelectric material of doping - Google Patents
A kind of detection method containing sulfur photoelectric material of doping Download PDFInfo
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- CN108132237A CN108132237A CN201810065429.7A CN201810065429A CN108132237A CN 108132237 A CN108132237 A CN 108132237A CN 201810065429 A CN201810065429 A CN 201810065429A CN 108132237 A CN108132237 A CN 108132237A
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- detection method
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- stearic acid
- containing sulfur
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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
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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Abstract
The invention belongs to optoelectronic materials technologies, and in particular to a kind of detection method containing sulfur photoelectric material of doping;Detection method includes pulverizing and sieving, be coated with sample preparation and spectral detection, and the raw material of the surface reinforcing agent includes stearic acid, supporting roller bush, reduced sugar, appropriate glycerine and appropriate amount of purified water;This method propose a kind of completely new detection method and surface reinforcing agents, stearic acid particles form metastable state liquid phase under the action of ultrasonic vibration in water, silver granuel can be formed when supporting roller bush is reacted with reduced sugar on stearic acid particles surface, simultaneously because it is added into metastable state liquid phase together with reduced sugar and glycerine, while silver granuel is formed, stearic acid particles also dissolve therewith, therefore the different silver granuel of many grain sizes can be formed in liquid phase, the roughness on sample table surface is increased, improves the effect of Raman surface enhancing detection.
Description
Technical field
The invention belongs to optoelectronic materials technologies, and in particular to a kind of detection method containing sulfur photoelectric material of doping.
Background technology
Organic micromolecular photoelectric material is a kind of organic material with photoelectric converting function, it is typically that there is big π to be total to
The organic molecule of yoke key, is widely used in OLED, OFET and OSC;It is with property is various, type is various, cost
It is cheap, be easily worked, be light-weight and the advantage that traditional inorganic material such as large area flexible device cannot compare can be fabricated to,
It is had been to be concerned by more and more people in terms of commercialization and industrialization;The organic photoelectrical material of wherein sulfur atom-containing is shown very
Good charge transport quality, is one of most worthy and the material of potential advantages, and to the organic photoelectrical material of sulfur atom-containing into
Its photoelectric properties can be further improved after row doping;Want to carry out photoelectric material deeper research just needs pair
There are one clearly recognize, such as organic material molecular structure and luminescent properties, carrier transport for the physical mechanism of organic interface
The relationship of characteristic;And molecular spectrum is the important means for studying molecular structure and molecular property, it, can with reference to density functional theory
Determine the important informations such as molecular geometry, vibration frequency, distribution of charges, energy level, macroscopic property;Therefore to organic molecule
The research of photoelectric material spectral quality is to study the basis of photoelectric properties;The spectral quality forefathers of such molecule seldom relate at present
And some only researchs are all only to have carried out measuring belonging to qualitatively experience, also there are larger differences, it is necessary to quantitative
Carry out in-depth study.
Raman spectrum is that a kind of molecular spectrum based on Raman scattering principle refers to trace identification method, when light and molecule phase interaction
With and when scattering, a few photons occur the Raman scattering in inelastic scattering and portion of energy are transferred to molecule, make scattering light
Frequency is subjected to displacement, and displacement carries molecular information;Due to molecular structure difference, then displacement is different, corresponding Raman collection of illustrative plates
Also it is different, the presence of chemical substance and relative amount in sample can be detected according to obtained Raman collection of illustrative plates.
But since Raman scattering effect is very weak, scattered light intensity is about the 10 of incident intensity-6~10-9, greatly
Limit the application and development of Raman spectrum.
Fleischmann et al. is adsorbed for the first time after 1974 are roughened smooth silver electrode surface
The Raman spectrum of the high quality of monolayer Pyridine Molecules in silver electrode surface;Subsequent Van Duyne and its partner pass through
The experiment of system and calculating find the Raman scattering signals of each Pyridine Molecules of the absorption on roughened silver surfaces in solution phase
The Raman scattering signal of pyridine compare, enhance about 6 orders of magnitude, it is indicated that this is a kind of with the relevant surface enhanced of rough surface
Effect is referred to as Surface enhanced Raman spectroscopy effect.
This method, which is laid particular emphasis on, is detected photoelectric material using Raman scattering effect, and proposes a kind of completely new detection
Method and surface reinforcing agent.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of detection method containing sulfur photoelectric material of doping, the party
Method can reach higher raman spectral signal intensity.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of doping containing sulfur photoelectric material, detection method includes the following steps:
A. it pulverizes and sieves:Detected materials are put into ball mill and carry out ball milling, and are mixed with KBr powder after ball milling
It is even;
B. it is coated with sample preparation:Surface reinforcing agent is coated on sample table surface, and the powder obtained by step a is applied to table
On the reinforcing agent of face, obtained component is denoted as sample to be tested b;
C. spectral detection:The sample to be tested b obtained through step b is put into Raman spectrum detector and is detected, treats window
After occurring the red curve of spectrum in mouthful, scanning result is preserved, detection terminates;
Preferably, the mesh number of ball milling is 300-1000 mesh in the step a.
Preferably, the raw material of surface reinforcing agent includes the raw material of following mass fraction in the step b:Stearic acid 10-15
Part, 10-30 parts of supporting roller bush, 10-30 parts of reduced sugar, appropriate glycerine and appropriate amount of purified water, the preparation packet of the surface reinforcing agent
Include following steps:
A. grinding is with liquid:Stearic acid is put into ball mill and carries out ball milling, then the stearic acid after ball milling is poured into pure water
In, obtained component is denoted as liquid a;
B. liquid stirring is mixed:Supporting roller bush is added in the liquid a obtained through step a, it is lasting to stir, and add ultrasound shake
It swings, obtained component is denoted as liquid b;
C. reaction concentration:The reduction that will be dissolved in glycerine after liquid b keeps metastable state under the action of ultrasonic vibration
Sugar is poured into liquid b, treats after reaction, mixed liquor to be put into baking oven and carries out concentration.
Preferably, the sample table in the step b can be put into baking oven after coating and toasted, oven temperature is set as
380-400℃。
Preferably, the mesh number in the step a after stearic acid ball milling is 50-300 mesh.
Preferably, the oven temperature in the step c is set as 90-120 DEG C.
Advantageous effect:
The present invention provides a kind of detection methods containing sulfur photoelectric material of doping, and this method propose a kind of completely new inspections
Survey method and surface reinforcing agent, stearic acid particles form metastable state liquid phase under the action of ultrasonic vibration in water, when support human relations examination
Agent can form silver granuel when being reacted with reduced sugar on stearic acid particles surface, simultaneously because reduced sugar is added together with glycerine
Enter in metastable state liquid phase, while silver granuel is formed, stearic acid particles also dissolve therewith, therefore many grain sizes can be formed in liquid phase
Different silver granuels increases the roughness on sample table surface, further improves the effect of Raman surface enhancing detection.
Specific embodiment
Purpose, technical scheme and advantage to make the embodiment of the present invention are clearer, below in conjunction with the embodiment of the present invention,
Technical solution in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
All other embodiments obtained under the premise of creative work, shall fall within the protection scope of the present invention.
Embodiment 1:
A kind of doping containing sulfur photoelectric material, detection method includes the following steps:
A. it pulverizes and sieves:Detected materials are put into ball mill and carry out ball milling, and are mixed with KBr powder after ball milling
It is even;
B. it is coated with sample preparation:Surface reinforcing agent is coated on sample table surface, and the powder obtained by step a is applied to table
On the reinforcing agent of face, obtained component is denoted as sample to be tested b;
C. spectral detection:The sample to be tested b obtained through step b is put into Raman spectrum detector and is detected, treats window
After occurring the red curve of spectrum in mouthful, scanning result is preserved, detection terminates;
Preferably, the mesh number of ball milling is 300 mesh in the step a.
Preferably, the raw material of surface reinforcing agent includes the raw material of following mass fraction in the step b:15 parts of stearic acid,
15 parts of supporting roller bush, 25 parts of reduced sugar, appropriate glycerine and appropriate amount of purified water, the preparation of the surface reinforcing agent include following step
Suddenly:
A. grinding is with liquid:Stearic acid is put into ball mill and carries out ball milling, then the stearic acid after ball milling is poured into pure water
In, obtained component is denoted as liquid a;
B. liquid stirring is mixed:Supporting roller bush is added in the liquid a obtained through step a, it is lasting to stir, and add ultrasound shake
It swings, obtained component is denoted as liquid b;
C. reaction concentration:The reduction that will be dissolved in glycerine after liquid b keeps metastable state under the action of ultrasonic vibration
Sugar is poured into liquid b, treats after reaction, mixed liquor to be put into baking oven and carries out concentration.
Preferably, the sample table in the step b can be put into baking oven after coating and toasted, oven temperature is set as
400℃。
Preferably, the mesh number in the step a after stearic acid ball milling is 50 mesh.
Preferably, the oven temperature in the step c is set as 110 DEG C.
Embodiment 2:
A kind of doping containing sulfur photoelectric material, detection method includes the following steps:
A. it pulverizes and sieves:Detected materials are put into ball mill and carry out ball milling, and are mixed with KBr powder after ball milling
It is even;
B. it is coated with sample preparation:Surface reinforcing agent is coated on sample table surface, and the powder obtained by step a is applied to table
On the reinforcing agent of face, obtained component is denoted as sample to be tested b;
C. spectral detection:The sample to be tested b obtained through step b is put into Raman spectrum detector and is detected, treats window
After occurring the red curve of spectrum in mouthful, scanning result is preserved, detection terminates;
Preferably, the mesh number of ball milling is 500 mesh in the step a.
Preferably, the raw material of surface reinforcing agent includes the raw material of following mass fraction in the step b:10 parts of stearic acid,
25 parts of supporting roller bush, 30 parts of reduced sugar, appropriate glycerine and appropriate amount of purified water, the preparation of the surface reinforcing agent include following step
Suddenly:
A. grinding is with liquid:Stearic acid is put into ball mill and carries out ball milling, then the stearic acid after ball milling is poured into pure water
In, obtained component is denoted as liquid a;
B. liquid stirring is mixed:Supporting roller bush is added in the liquid a obtained through step a, it is lasting to stir, and add ultrasound shake
It swings, obtained component is denoted as liquid b;
C. reaction concentration:The reduction that will be dissolved in glycerine after liquid b keeps metastable state under the action of ultrasonic vibration
Sugar is poured into liquid b, treats after reaction, mixed liquor to be put into baking oven and carries out concentration.
Preferably, the sample table in the step b can be put into baking oven after coating and toasted, oven temperature is set as
390℃。
Preferably, the mesh number in the step a after stearic acid ball milling is 150 mesh.
Preferably, the oven temperature in the step c is set as 100 DEG C.
Embodiment 3:
A kind of doping containing sulfur photoelectric material, detection method includes the following steps:
A. it pulverizes and sieves:Detected materials are put into ball mill and carry out ball milling, and are mixed with KBr powder after ball milling
It is even;
B. it is coated with sample preparation:Surface reinforcing agent is coated on sample table surface, and the powder obtained by step a is applied to table
On the reinforcing agent of face, obtained component is denoted as sample to be tested b;
C. spectral detection:The sample to be tested b obtained through step b is put into Raman spectrum detector and is detected, treats window
After occurring the red curve of spectrum in mouthful, scanning result is preserved, detection terminates;
Preferably, the mesh number of ball milling is 700 mesh in the step a.
Preferably, the raw material of surface reinforcing agent includes the raw material of following mass fraction in the step b:17 parts of stearic acid,
30 parts of supporting roller bush, 15 parts of reduced sugar, appropriate glycerine and appropriate amount of purified water, the preparation of the surface reinforcing agent include following step
Suddenly:
A. grinding is with liquid:Stearic acid is put into ball mill and carries out ball milling, then the stearic acid after ball milling is poured into pure water
In, obtained component is denoted as liquid a;
B. liquid stirring is mixed:Supporting roller bush is added in the liquid a obtained through step a, it is lasting to stir, and add ultrasound shake
It swings, obtained component is denoted as liquid b;
C. reaction concentration:The reduction that will be dissolved in glycerine after liquid b keeps metastable state under the action of ultrasonic vibration
Sugar is poured into liquid b, treats after reaction, mixed liquor to be put into baking oven and carries out concentration.
Preferably, the sample table in the step b can be put into baking oven after coating and toasted, oven temperature is set as
380℃。
Preferably, the mesh number in the step a after stearic acid ball milling is 250 mesh.
Preferably, the oven temperature in the step c is set as 90 DEG C.
Embodiment 4:
A kind of doping containing sulfur photoelectric material, detection method includes the following steps:
A. it pulverizes and sieves:Detected materials are put into ball mill and carry out ball milling, and are mixed with KBr powder after ball milling
It is even;
B. it is coated with sample preparation:Surface reinforcing agent is coated on sample table surface, and the powder obtained by step a is applied to table
On the reinforcing agent of face, obtained component is denoted as sample to be tested b;
C. spectral detection:The sample to be tested b obtained through step b is put into Raman spectrum detector and is detected, treats window
After occurring the red curve of spectrum in mouthful, scanning result is preserved, detection terminates;
Preferably, the mesh number of ball milling is 1000 mesh in the step a.
Preferably, the raw material of surface reinforcing agent includes the raw material of following mass fraction in the step b:13 parts of stearic acid,
10 parts of supporting roller bush, 10 parts of reduced sugar, appropriate glycerine and appropriate amount of purified water, the preparation of the surface reinforcing agent include following step
Suddenly:
A. grinding is with liquid:Stearic acid is put into ball mill and carries out ball milling, then the stearic acid after ball milling is poured into pure water
In, obtained component is denoted as liquid a;
B. liquid stirring is mixed:Supporting roller bush is added in the liquid a obtained through step a, it is lasting to stir, and add ultrasound shake
It swings, obtained component is denoted as liquid b;
C. reaction concentration:The reduction that will be dissolved in glycerine after liquid b keeps metastable state under the action of ultrasonic vibration
Sugar is poured into liquid b, treats after reaction, mixed liquor to be put into baking oven and carries out concentration.
Preferably, the sample table in the step b can be put into baking oven after coating and toasted, oven temperature is set as
380℃。
Preferably, the mesh number in the step a after stearic acid ball milling is 300 mesh.
Preferably, the oven temperature in the step c is set as 120 DEG C.
It should be noted that herein, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any this practical relationship or sequence.Moreover, term " comprising ", "comprising" or its any other variant are intended to
Non-exclusive inclusion, so that process, method, article or equipment including a series of elements not only will including those
Element, but also including other elements that are not explicitly listed or further include as this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
Also there are other identical elements in process, method, article or equipment including the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although with reference to the foregoing embodiments
The present invention is described in detail, it will be understood by those of ordinary skill in the art that:It still can be to aforementioned each implementation
Technical solution recorded in example modifies or carries out equivalent replacement to which part technical characteristic;And these modification or
It replaces, the spirit and scope for various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution.
Claims (7)
1. a kind of detection method containing sulfur photoelectric material of doping, it is characterised in that:Detection method includes the following steps for this:
A. it pulverizes and sieves:Detected materials are put into ball mill and carry out ball milling, and are uniformly mixed after ball milling with KBr powder;
B. it is coated with sample preparation:Surface reinforcing agent is coated on sample table surface, and will be applied to surface by the powder that step a is obtained
On reinforcing agent, obtained component is denoted as sample to be tested b;
C. spectral detection:The sample to be tested b obtained through step b is put into Raman spectrum detector and is detected, is treated in window
After there is the red curve of spectrum, scanning result is preserved, detection terminates.
2. a kind of detection method containing sulfur photoelectric material of doping according to claim 1, it is characterised in that:The step
The mesh number of ball milling is 300-1000 mesh in a.
3. a kind of detection method containing sulfur photoelectric material of doping according to claim 1, it is characterised in that:The step
The raw material of surface reinforcing agent includes the raw material of following mass fraction in b:10-15 parts of stearic acid, 10-30 parts of supporting roller bush, reduction
10-30 parts sugared, appropriate glycerine and appropriate amount of purified water, the preparation of the surface reinforcing agent include the following steps:
A. grinding is with liquid:Stearic acid is put into ball mill and carries out ball milling, then the stearic acid after ball milling is poured into pure water, institute
It obtains component and is denoted as liquid a;
B. liquid stirring is mixed:Supporting roller bush is added in the liquid a obtained through step a, it is lasting to stir, and add ultrasonic vibration, institute
It obtains component and is denoted as liquid b;
C. reaction concentration:The reduced sugar being dissolved in glycerine is fallen after liquid b keeps metastable state under the action of ultrasonic vibration
Enter in liquid b, treat that after reaction, it is thick liquid that mixed liquor is put into concentration in baking oven.
4. a kind of detection method containing sulfur photoelectric material of doping according to claim 1, it is characterised in that:It can be by described in
Sample table in step b is put into baking oven and toasts after coating, and oven temperature is set as 380-400 DEG C.
5. a kind of detection method containing sulfur photoelectric material of doping according to claim 3, it is characterised in that:The reduction
Sugar is one or more of glucose, fructose, galactolipin, lactose and maltose.
A kind of 6. detection method containing sulfur photoelectric material of doping according to claim 3, which is characterized in that the step
Mesh number in a after stearic acid ball milling is 50-300 mesh.
7. a kind of detection method containing sulfur photoelectric material of doping according to claim 3, it is characterised in that:The step
Oven temperature in c is set as 90-120 DEG C.
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Citations (2)
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CN101421050A (en) * | 2006-02-08 | 2009-04-29 | 艾克里麦德公司 | Methods and compositions for metal nanoparticle treated surfaces |
CN106525808A (en) * | 2016-09-21 | 2017-03-22 | 北京科技大学 | Method for preparing flexible surface-enhanced raman base with polymer substrate |
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2018
- 2018-01-23 CN CN201810065429.7A patent/CN108132237A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101421050A (en) * | 2006-02-08 | 2009-04-29 | 艾克里麦德公司 | Methods and compositions for metal nanoparticle treated surfaces |
CN106525808A (en) * | 2016-09-21 | 2017-03-22 | 北京科技大学 | Method for preparing flexible surface-enhanced raman base with polymer substrate |
Non-Patent Citations (2)
Title |
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Application publication date: 20180608 |