CN107064099A - A kind of method for measuring micro substance - Google Patents
A kind of method for measuring micro substance Download PDFInfo
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- CN107064099A CN107064099A CN201610988240.6A CN201610988240A CN107064099A CN 107064099 A CN107064099 A CN 107064099A CN 201610988240 A CN201610988240 A CN 201610988240A CN 107064099 A CN107064099 A CN 107064099A
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- thin layer
- mos
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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
Abstract
The invention discloses a kind of method for measuring micro substance, belong to nano semiconductor material field.Its technological process is：ZnO nano-rod array sample is prepared first with hydro-thermal method, then using chemical vapour deposition technique in ZnO nanorod superficial growth thin layer MoS2Material, ultimately forms the thin layer MoS of ZnO nanorod support2Material, utilizes thin layer MoS2Two Raman vibration peak E1 2gAnd A1gSpacing δ as detecting parameter, by micro substance to be measured absorption in thin layer MoS2On material, δ is detected using Raman spectrum, the content of test substance can just be detected according to δ change.The present invention has preparation technology simple, and reaction condition is gentle, the advantages of cost of raw material and equipment is relatively low, accuracy of detection is high.
Description
Technical field
The invention belongs to nano semiconductor material field, and in particular to a kind of method of measurement micro substance.
Background technology
Minimal feeding technology is particularly significant to engineer equipment, Environmental security, counterterrorist activity and scientific research etc..Example
Such as, in high power solid-state laser device, micro organic pollution just can have a strong impact on optical element performance, or even trigger light
Learn the damage from laser of element, it is therefore desirable to monitor the pollutant of nanogram magnitude on-line；Environmental security and counterterrorist activity are generally required
Scene, the micro substance in real time, rapidly detecting the danger such as poisonous, inflammable, explosive, to carry out the Accurate Analysis, pre- of data
First take preventive measures, prevent trouble before it happens.With the progress of detection technique and equipment, the accuracy and sensitivity of detection obtains very big
Lifting, for example, using high resolution transmission electron microscopy, the material of atom size can be detected.However, these installation costs
With extremely expensive, structure is extremely complex, and operating environment requirements are harsh, need technical professional to operate and analyze again,
Therefore it is limited to a certain extent to use.Research and develop the minimal feeding that a kind of price is relatively cheap, structure is relatively simple
Technology, is the target seek assiduously for a long time.
Thin layer molybdenum disulfide MoS2Material is a kind of new functional material, with layer structure, individual layer MoS2The thickness of molecule
Degree is only 0.7nm or so, and it is combined by weaker Van der Waals force between layers.Research discovery, thin layer MoS2The layer of material
It is several that its Raman spectrum is had a significant effect, for example, individual layer MoS2The E of Raman spectrum1 2gAnd A1gDifference on the frequency (δ) between peak is
18cm-1, and double-deck reach 21cm-1More than, the change of only one molecular layers thick will produce 3cm-1Difference.
At present, a variety of methods prepare thin layer MoS2Material, such as mechanical stripping, liquid phase stripping, chemical vapor deposition,
Plasma is thinned, thermal evaporation is thinned etc., and wherein chemical vapour deposition technique is most advantageous, can prepare large-area high-quality
Thin layer MoS2Material, the existing thin layer MoS of in the market2Merchandise sales.Raman spectrum detection technique has developed highly developed,
There is portable high performance Raman spectroscopy instrument selling.
The content of the invention
A kind of simple, the method that micro substance can be detected the purpose of the present invention is to propose to equipment requirement.The technology of the present invention
Scheme is in thin layer MoS2One layer of micro substance to be detected of upper absorption, this layer material is not needed and MoS2Atom formation ion
The strong effect such as key, covalent bond, itself and thin layer MoS2Van der Waals interaction between material atom is just enough to make MoS2Difference on the frequency
The change of observable, δ variable quantity and the thickness of sorbing material, sorbing material and thin layer MoS occur for δ2The intermolecular forces of material
The factor such as size, property it is closely related.By detecting MoS2The E of Raman spectrum1 2gAnd A1gDifference on the frequency δ between peak, as long as handle
δ and absorption micro substance concentration or the parameter such as thickness are calibrated, just can be by the content of δ measure of the change micro substance.
A kind of method for measuring micro substance of the present invention, comprises the following steps：
1. clean substrate
Substrate is cleaned, the pollution such as dust, greasy dirt of substrate surface is removed.
2. grow ZnO Seed Layers
Configuration concentration is 5-25mmol/L zinc acetate ethanol solution, and solution is added drop-wise on substrate, and covering substrate is just
Face, after waiting 10-30 minutes, dries substrate；After repetition said process 5-15 times, substrate is heat-treated, obtained with ZnO
The substrate of Seed Layer.
3. growing ZnO nanorod arrays
Zinc solution and alkaline solution are pressed into Zn+：HO-Mol ratio=1:0.8~1.5 ratio mixing, and stir；
Then the substrate face down with ZnO Seed Layers is placed in mixed solution；Constant temperature places 5- in 70-90 DEG C of drying box
After 12 hours, substrate and clean substrate surfaces are taken out, obtain growing the substrate for having ZnO nanorod.
4. grow MoS2Auxiliary layer
Substrate immersion concentration with ZnO nanorod is auxiliary for 10-20mg/L 3,4,9,10- tetracarboxylic anhydrides (PTCDA)
Help in layer solution 5-15 minutes, take out substrate and dry, obtain the ZnO with 3,4,9,10- tetracarboxylic anhydride (PTCDA) auxiliary layers and receive
Rice rod substrate.
5. thin layer MoS is grown on ZnO nanorod2
It is 1 to weigh mass ratio:4~6 molybdenum trioxide powder (MoO3) and sulphur powder (S), it is contained in respectively in two containers；Will be long
The ZnO nanorod substrate face down for having 3,4,9,10- tetracarboxylic anhydrides (PTCDA), which is positioned over, is loaded with MoO3The top of container and not
With MoO3Contact；MoO will be loaded with3It is placed in the container of S powder in quartz tube furnace, is loaded with MoO3Container be located at quartz tube furnace
Heating zone center, the container for being loaded with S powder is located at heating area edge, at room temperature, to quartz tube furnace with 20-100SCCM's
Flow is passed through the air in inert gas, drain；Keep under aeration condition, S powder is in the upper direction of air-flow, MoO3It is in
Wind underside is to quartz tube furnace was rapidly heated to 500-800 DEG C in 10-20 minutes, naturally cold after being incubated 5-30 minutes
But to room temperature, sample is taken out, the thin layer MoS of ZnO nanorod support is obtained2Sample.
6. measure ZnO nanorod support thin layer MoS2The Raman spectrum of sample；
The Raman spectrum of sample is measured using Raman spectrometer, MoS is obtained2E1 2gWith A1gThe position of vibration mode and its
Between frequency-splitting, with δ1Represent.
7. measurement standard curve
According to test substance species, the substance solution of configuration various concentrations (σ)；The thin layer that ZnO nanorod is supported
MoS2Sample is immersed in the solution of various concentrations, the thin layer MoS for making test substance absorption be supported in ZnO nanorod2On sample.
The thin layer MoS that ZnO nanorod is supported after measuring the solution processing through various concentrations using Raman spectrometer2The Raman light of sample
Spectrum, obtains MoS2E1 2gWith A1gThe position of vibration mode and its between frequency-splitting, with δ2Represent, by φ=δ2-δ1Obtain
The change of frequency-splitting, makes σ and φ standard curve before and after absorption test substance.According to specific test request, setting is linear
The correlation coefficient threshold R of fitting0And relative error Δ0, wherein R0≤ 1, choose and meet the one of test request on the standard curve
Section curve, does linear fit, its linearly dependent coefficient R to this section of curve1Not less than R0, relative error Δ1Δ should be not more than0；It is right
This section of selected curve carries out the linear functional relation that linear fit obtains σ and φ：
σ=k φ
Wherein k is the proportionality coefficient relevant with test substance.
8. measure test substance.
Test substance is dissolved into solution, the thin layer MoS that ZnO nanorod is supported2Sample is immersed in the solution, makes to treat
Survey the thin layer MoS that material absorption is supported in ZnO nanorod2On sample, then MoS is measured using Raman spectrometer2E1 2gWith A1g
The position of vibration mode and its between frequency-splitting δ2, by φ=δ2-δ1The change of frequency-splitting before and after acquisition absorption test substance
Change, test substance concentration is obtained according to σ=k φ.
The essence of the present invention is to adsorb test substance in thin layer MoS2On, utilize thin layer MoS before and after absorption2Raman spectrum
Change detect test substance.
The minimal feeding method that the present invention is provided, ZnO nanorod, thin layer MoS needed for it2The preparation technology of material
Simply, reaction condition is gentle, and the cost of raw material and equipment is relatively low；Used Raman spectroscopy instrument popularization is high, Er Qieyi
There is portable product.Therefore, this method has huge application value.
Brief description of the drawings
Fig. 1 is present invention process schematic flow sheet；
Fig. 2 is the thin layer MoS that ZnO nanorod is supported2Scanning electron microscope diagram；
Fig. 3 is the thin layer MoS that ZnO nanorod is supported2Adsorb the Raman spectrum before and after RDX；
Fig. 4 is RDX solution concentrations σ and φ standard curve.
Embodiment
Step one, it is cleaned by ultrasonic silicon chip more than 15 minutes, Ran Houyong in acetone, ethanol, deionized water solution successively
Air blow drying substrate.
Step 2, configures the ethanol solution (15mmol/l) of zinc acetate, and it is some to draw the solution, is added drop-wise to silicon chip front
On (burnishing surface), solution is covered whole substrate surface, solution is dried up with air after waiting 10 minutes；Again on substrate
Zinc acetate solution is added dropwise, waits and being dried up after 10 minutes clocks, repeat the process 10 times；Then, it is substrate is small in 300 DEG C of heat treatments 1
When, obtain the substrate with ZnO Seed Layers.
Step 3, is all 50mmol/L zinc nitrate aqueous solution and the hexamethylenetetramine aqueous solution with 1 by concentration:1 ratio
Mixing, magnetic agitation more than 20 minutes is well mixed solution.Substrate with Seed Layer is placed in mixed solution, substrate
Face down, swims in mixed solution surface.Finally, after constant temperature grows 6 hours in 80 DEG C of drying box, take out substrate and spend
Ionized water cleans surface, with air blow drying, obtains the substrate with ZnO nanorod.
Step 4,3,4,9, the 10- tetracarboxylic anhydrides for being 10mg/L by the substrate immersion concentration with ZnO nanorod
(PTCDA) 5 minutes in solution, make PTCDA absorption on ZnO nanorod surface, take out substrate and dry, obtain with auxiliary layer
ZnO nanorod sample.
Step 5, weighs 0.4g molybdenum trioxides (MoO3) and 1.6g sulphur powders (S), it is contained in respectively in two ceramic boats；It will inhale
Attached PTCDA ZnO nanorod substrate face down, which is supported on, is loaded with MoO3On the edge of ceramic boat, substrate is located at MoO3Powder
Surface and not with MoO3Powder is contacted；MoO will be loaded with3It is placed in the ceramic boat of S powder in quartz tube furnace, is loaded with MoO3Ceramics
Boat is located at quartz tube furnace heating zone center, and the ceramic boat for being loaded with S powder is located at heating area edge, and above air-flow
To the spacing of two ceramic boats is 9cm；At room temperature, argon gas is passed through with 50SCCM flow to quartz tube furnace, ventilated 10 minutes
More than, the air in drain；Keep under aeration condition, quartz tube furnace was rapidly heated in 15 minutes to 650 DEG C, and was kept
10 minutes；Room temperature is naturally cooled to afterwards, obtains the thin layer MoS of ZnO nanorod support2Sample.
Step 6, the thin layer MoS of ZnO nanorod support is measured using Raman spectrometer2The Raman spectrum of sample, is obtained
E1 2gWith A1gThe position of vibration mode and its between frequency-splitting δ1。
Step 7, by taking hexogen RDX as an example, the RDX acetone solns of configuration various concentrations (σ) support ZnO nanorod
Thin layer MoS2Sample is immersed in the solution of various concentrations 1 minute, the thin layer MoS for making RDX absorption be supported in ZnO nanorod2Sample
On.The thin layer MoS that ZnO nanorod is supported after measuring the solution processing through various concentrations using Raman spectrometer2The Raman of sample
Spectrum, obtains MoS2E1 2gWith A1gThe position of vibration mode and its between frequency-splitting δ2, by φ=δ2-δ1Absorption is obtained to treat
The change of frequency-splitting, obtains σ and φ standard curve before and after survey material.Set correlation coefficient threshold R0=0.9, relative error
Δ0=15%, choose one section of curve that test request is met on the standard curve：Linear fit is made to this section of curve, its line
Property coefficient R1Not less than R0, relative error Δ1Δ should be not more than0；σ scopes are 0-0.8 μm of ol/L in the present embodiment, to institute
This section of curve progress linear fit chosen obtains φ and σ functional relation is：
The φ of σ=0.1007
Coefficient R1=0.97, relative error Δ1=12%.
Step 8, solution is dissolved into by RDX to be measured, the thin layer MoS that ZnO nanorod is supported2Sample is immersed in the solution
In, the thin layer MoS for making test substance absorption be supported in ZnO nanorod2On sample, then MoS is measured using Raman spectrometer2's
E1 2gWith A1gThe position of vibration mode and its between frequency-splitting δ2, by φ=δ2-δ1Obtain frequency before and after absorption test substance
The change of difference, test substance concentration is obtained according to the φ of σ=0.1007.If for example, measuring φ=0.4cm-1, then can obtain
The concentration of detected materials is about 0.04 μm of ol/L.
The present invention prepares ZnO nano-rod array sample first with hydro-thermal method, then using chemical vapour deposition technique in ZnO
Nanorod surfaces growth thin layer MoS2Material, ultimately forms the thin layer MoS of ZnO nanorod support2Material, utilizes thin layer MoS2's
Two Raman vibration peak E1 2gAnd A1gSpacing δ as detecting parameter, by micro substance to be measured absorption in thin layer MoS2On material,
δ is detected using Raman spectrum, the content of test substance can just be detected according to δ change.Fig. 2 is ZnO- thin layers MoS2Scanning
Electron microscope picture.Fig. 3 is ZnO- thin layers MoS2The Raman spectrum before and after hexogen (RDX) is adsorbed, Raman spectrum is sent out after absorption
Obvious change has been given birth to, has illustrated effectiveness of the invention.Fig. 4 is RDX solution concentrations σ and φ standard curve, it can be seen from Fig. 4 that
In the case of low concentration, σ and φ is substantially met in the case of proportional relationship, high concentration, and φ is no longer changed significantly.
Claims (5)
1. a kind of method for measuring micro substance, comprises the following steps：
Step 1. cleans substrate；
Step 2. grows ZnO Seed Layers；
Step 3. growing ZnO nanorod arrays；
Step 4. grows MoS2Auxiliary layer；
Step 5. grows thin layer MoS on ZnO nanorod2；
Step 6. measurement ZnO nanorod support thin layer MoS2The Raman spectrum of sample；
The Raman spectrum of sample is measured using Raman spectrometer, MoS is obtained2E1 2gWith A1gThe position of vibration mode and its between
Frequency-splitting, with δ1Represent；
Step 7. measurement standard curve；
According to test substance species, the substance solution of configuration various concentrations (σ)；The thin layer MoS that ZnO nanorod is supported2Sample
It is immersed in the solution of various concentrations, the thin layer MoS for making test substance absorption be supported in ZnO nanorod2On；Utilize Raman spectrum
The thin layer MoS that ZnO nanorod is supported after solution processing of the instrument measurement through various concentrations2The Raman spectrum of sample, obtains MoS2's
E1 2gWith A1gThe position of vibration mode and its between frequency-splitting, with δ2Represent, by φ=δ2-δ1Obtain before absorption test substance
The change of frequency-splitting afterwards, makes σ and φ standard curve；According to specific test request, the coefficient correlation of linear fit is set
Threshold value R0And relative error Δ0, wherein R0≤ 1, one section of curve that test request is met on the standard curve is chosen, to the section
Curve does linear fit, its linearly dependent coefficient R1Not less than R0, relative error Δ1Δ should be not more than0；To the selected section
Curve carries out the linear functional relation that linear fit obtains σ and φ：
σ=k φ
Wherein k is the proportionality coefficient relevant with test substance；
Step 8. measures test substance；
Test substance is dissolved into solution, the thin layer MoS that ZnO nanorod is supported2Sample is immersed in the solution, makes determinand
The thin layer MoS that matter absorption is supported in ZnO nanorod2On sample, then MoS is measured using Raman spectrometer2E1 2gWith A1gVibration
The position of pattern and its between frequency-splitting δ2, by φ=δ2-δ1The change of frequency-splitting before and after acquisition absorption test substance,
Test substance concentration is obtained according to σ=k φ.
2. a kind of method for measuring micro substance as claimed in claim 1, it is characterised in that：The step 2 grows ZnO seeds
Layer is specifically included：Configuration concentration is 5-25mmol/L zinc acetate ethanol solution, and solution is added drop-wise on substrate, and covering substrate
Front, after waiting 10-30 minutes, dries substrate；Repeat after above-mentioned dropwise addition solution and drying process 5-15 time, substrate is carried out hot
Processing, obtains the substrate with ZnO Seed Layers.
3. a kind of method for measuring micro substance as claimed in claim 2, it is characterised in that：The step 3 grows ZnO nano
Rod array is specifically included：Zinc solution and alkaline solution are pressed into Zn+：HO-Mol ratio=1:0.8~1.5 ratio mixing, and stir
Mix uniform；Then the substrate face down with ZnO Seed Layers is placed in mixed solution；It is permanent in 70-90 DEG C of drying box
After temperature is placed 5-12 hours, substrate and clean substrate surfaces are taken out, obtain growing the substrate for having ZnO nanorod.
4. a kind of method for measuring micro substance as claimed in claim 3, it is characterised in that：The step 4 grows MoS2Auxiliary
Layer is specifically included：Substrate immersion concentration with ZnO nanorod is auxiliary for 10-20mg/L 3,4,9,10- tetracarboxylic anhydrides PTCDA
Help in layer solution 5-15 minutes, take out substrate and dry, obtain the ZnO nanorod base with 3,4,9,10- tetracarboxylic anhydride auxiliary layers
Piece.
5. a kind of method for measuring micro substance as claimed in claim 4, it is characterised in that：The step 5 is in ZnO nanorod
Upper growth thin layer MoS2Specifically include：It is 1 to weigh mass ratio:4~6 molybdenum trioxide powder MoO3With sulphur powder S, two are contained in respectively
In container；ZnO nanorod substrate face down with 3,4,9,10- tetracarboxylic anhydrides PTCDA is positioned over and is loaded with MoO3Container
Top and not with MoO3Contact；MoO will be loaded with3It is placed in the container of S powder in quartz tube furnace, is loaded with MoO3Container be located at
Quartz tube furnace heating zone center, the container for being loaded with S powder is located at heating area edge；At room temperature, to quartz tube furnace with 20-
100SCCM flow is passed through the air in inert gas, drain；Keep under aeration condition, S powder is in the top of air-flow
To MoO3In wind underside to quartz tube furnace was warming up to 500-800 DEG C in 10-20 minutes, insulation 5-30 minutes
Afterwards, room temperature is naturally cooled to, sample is taken out, the thin layer MoS of ZnO nanorod support is obtained2Sample.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110108697A (en) * | 2019-06-25 | 2019-08-09 | 北威(重庆)科技股份有限公司 | Surface enhanced Raman scattering micro-nano chip and preparation method thereof, application and Raman spectrum test macro |
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