CN109884122A - Organic gas detection chip based on sulfuration rhenium nano-device - Google Patents
Organic gas detection chip based on sulfuration rhenium nano-device Download PDFInfo
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Abstract
The invention discloses a kind of organic gas detection chips based on sulfuration rhenium nano-device, utilize sulfuration rhenium (ReS2) nano material electrical properties anisotropic properties and organic gas adsorb caused by electrical anisotropy property dimension of the variation as gas detection, realize the qualitative and quantitative analysis of organic gas.The present invention is based on the structure of the organic gas detection chip of sulfuration rhenium nano-device and preparation method are simple, detection sensitivity is high, can be realized qualitative, the quantitative judge of organic gas；The organic gas detection chip is having a size of micron order, super low-power consumption, its preparation process is integrated circuit (IC) manufacturing process of standard, it is compatible with system on chip (SOC) integrated technique, device can be easily embedded in various mobile terminals, convenient for the real-time monitoring of organic gas.
Description
Technical field
The invention belongs to detection method fields, detect more particularly to a kind of organic gas based on sulfuration rhenium nano-device
Chip.
Background technique
Organic gas is the main of Chemical Manufacture byproduct, indoor air chemical pollution and characteristics of contaminated respiratory droplets gas disease detection and prevention
Marker, realizes the qualitative recognition of organic gas and quantitative detection has very important significance and practical value.
At present on the market there are two types of organic gas detecting instruments: one is the detectors for using gas chromatography；Second
It is the portable organic gas detector based on photoelectricity ion detection.Gas chromatography (GC): point for first separating and detecting afterwards is used
Analysis method has many advantages, such as that high sensitivity, selectivity is good, high-effect, qualitative and quantitative accuracy is high, but the detection method price
Expensive, detection method complexity, detecting instrument volume are big, greatly limit its application prospect.As an improvement, occurring based on photoelectricity
Ion (PID) detection portable organic gas detector: its have the characteristics that it is portable, highly sensitive, it can be difficult to realize pair
The qualitative recognition of organic gas detects, i.e., only in the case where known gas type, can obtain its gas concentration value, it is difficult to
The identity detection for realizing gas, limits its practical value.
A large amount of research is done to the qualitative, quantitative identification of organic gas at present, main approaches are using biography
The method for feeling array is responded by cross sensitivity of the array sensing unit to organic gas, and the sensing for establishing organic gas is rung
Database is answered, realizes qualitative, the quantitative judge of organic gas by algorithm for pattern recognition, it is this method high sensitivity, qualitative and fixed
Accuracy of measurement is high, but the manufacture of multiple sensing units and integrated, increases its and prepares difficulty；In addition, this method is related at big data
Reason and arithmetic programming, software view require height, limit its practical application significantly.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of organic gas inspection based on sulfuration rhenium nano-device
Chip is surveyed, sulfuration rhenium (ReS is utilized2) nano material electrical properties anisotropic properties and organic gas adsorb caused by electricity
Dimension of the variation of anisotropic properties as gas detection, realizes the qualitative and quantitative analysis of organic gas.
The present invention is achieved by the following technical solutions:
A kind of organic gas detection chip based on sulfuration rhenium nano-device, including sulfuration rhenium nano flake, first electrode,
Second electrode and silica substrate；The sulfuration rhenium nano flake is bonded with silica upper surface of substrate, and described
One electrode, second electrode are grown along the anisotropy axis of sulfuration rhenium.
In the above-mentioned technical solutions, the sulfuration rhenium nano flake is obtained using mechanical stripping or dry method transfer method,
Length and width are micron order, with a thickness of nanoscale.
In the above-mentioned technical solutions, the first electrode and second electrode are gold electrode, steam golden legal system using electron beam
, the angle between first electrode and second electrode is 60 ° or 120 °.
On the other hand, a kind of preparation method of the organic gas detection chip based on sulfuration rhenium nano-device:
Step 1: silicon wafer being put into the mixed liquor of 30wt.% hydrogen peroxide and the 98wt.% concentrated sulfuric acid and impregnate 29-31min,
The hard particles of silicon chip surface are removed, the volume ratio of 30wt.% hydrogen peroxide and the 98wt.% concentrated sulfuric acid is 1:3 in above-mentioned mixed liquor；
It is rinsed well with deionized water in the mixed liquor for being placed on 40wt.% hydrofluoric acid and deionized water and impregnates 19-
21min removes the SiO on surface2Layer, the volume ratio of 40wt.% hydrofluoric acid and deionized water is 1:1 in above-mentioned mixed liquor；
Silicon wafer is sequentially placed into deionized water, acetone solvent and dehydrated alcohol and is cleaned by ultrasonic 9-11min respectively, removes table
It is put into after the organic impurities of face in dehydrated alcohol as silica substrate；
Step 2: using mechanical stripping method or dry method transfer method, and it is micron order, with a thickness of nanoscale sulphur that length and width, which are made,
Change rhenium nano flake and be transferred into silica substrate, is bonded it with silica upper surface of substrate；
Step 3: golden method (e-beam evaporation) is steamed using electron beam, is grown along two anisotropy axis of sulfuration rhenium
First electrode and second electrode.
In the above-mentioned technical solutions, described is gold electrode, angle between first electrode and second electrode be 60 ° or
120°。
In the above-mentioned technical solutions, the first electrode in the step 3 and second electrode are respectively set to be parallel to each other
Two, the conducting channel formed between the electrode that every two is parallel to each other is as independent sensitive zones.
On the other hand, application of the sulfuration rhenium nano material (device) in organic gas detection.
On the other hand, a kind of detection method of the organic gas detection chip based on sulfuration rhenium nano-device:
Apply identical voltage to first electrode and second electrode, forms base current I1And I2, when same gas absorption, two
A independent sensitive zones generate different curent changes | Δ I1| and | Δ I2|, and pass through current sample port 1 and end
Mouth 2 is transferred to display terminal, draws Δ I1/I1-ΔI2/I2Curve, calculated curve slope, compares with database data
Afterwards, the type of qualitative discrimination organic gas, the sound then changed on sulfuration rhenium anisotropy axis with concentration according to organic gas
Should figure quantitatively determine the concentration of organic gas, realize qualitative, the quantitative measurment of organic gas；
The anisotropy axis of sulfuration rhenium is sulphur-rhenium chain rivet and rhenium chain rivet, defines anisotropy axis sulphur-rhenium chain rivet of sulfuration rhenium
For a axis, rhenium chain rivet is b axis；Define sensitivity:That is a axis sensitivity isB axis
Sensitivity is
Each organic gas is different with the matched curve track of b axle response about a axle response, is realized using this feature
The identification of organic gas measures organic gas acetone, ethyl alcohol, methanol, the linear pass of isopropanol a axle response and b axle response respectively
System, linear equation are as follows:
Acetone: y=0.3+1.025x, degree of fitting R2It is 0.984；
Ethyl alcohol: y=0.68+0.5x, degree of fitting R2It is 0.988；
Methanol: y=1.766+2.8x, degree of fitting R2It is 0.991；
Isopropanol: y=2.1+1.810x, degree of fitting R2It is 0.951；
Wherein x is the corresponding a axis sensitivity response value of each organic gas, and y is the corresponding b axis of each organic gas
Sensitivity response value；
Measurement organic gas acetone respectively, ethyl alcohol, methanol, sensitivity response value of the isopropanol within the scope of 0-500ppm
Linear relationship, linear equation are as follows:
Acetone b axis: y=0.14+0.0126x, degree of fitting R2It is 0.991, minimum detectability 13ppm；
Acetone a axis: y=0.4095+0.013x, degree of fitting R2It is 0.995, minimum detectability 24ppm；
Ethyl alcohol b axis: y=-0.03945+0.04964x, degree of fitting R2It is 0.999, minimum detectability 2ppm；
Ethyl alcohol a axis: y=0.65122+0.02492x, degree of fitting R2It is 0.99, minimum detectability 12ppm；
Methanol b axis: y=0.81671+0.01256x, degree of fitting R2It is 0.997, minimum detectability 14ppm；
Methanol a axis: y=4.04744+0.03526x, degree of fitting R2It is 0.991, minimum detectability 5ppm；
Isopropanol b axis: y=-1.20708+0.01697x, degree of fitting R2It is 0.972, minimum detectability 21ppm；
Isopropanol a axis: y=-0.35137+0.03163x, degree of fitting R2It is 0.996, minimum detectability 3ppm；
Wherein x is the corresponding concentration of each organic gas, and y is the corresponding sensitivity response value of each organic gas.
Sulfuration rhenium intra-face anisotropy axis is respectively rhenium chain rivet and rhenium-sulphur chain rivet, and rhenium chain rivet electron mobility is rhenium-sulphur chain
3-4 times of axis.Suction type of the organic gas on two anisotropy axis of sulfuration rhenium is different, and caused electric charge transfer quantity is not
Together, it can simultaneously, it is independent from identical gas absorption obtain two dimensions electrical signal | Δ I1| and | Δ I2|, it builds
The vertical Δ I changed with concentration1/I1-ΔI2/I2Geometric locus, wherein I1And I2The respectively base current of anisotropy axis.Due to every
A kind of suction type of organic gas on sulfuration rhenium anisotropy axis is different, and electric charge transfer quantity is different, i.e., each is organic
Gas can all form oneself unique Δ I1/I1-ΔI2/I2Curve, to realize qualitative, the quantitative judge of organic gas.
The invention has the advantages and beneficial effects that:
The present invention is based on the structure of the organic gas detection chip of sulfuration rhenium nano-device and preparation method are simple, detection spirit
Sensitivity is high, can be realized qualitative, the quantitative judge of organic gas；The organic gas detection chip is having a size of micron order, ultralow function
Consumption, preparation process is integrated circuit (IC) manufacturing process of standard, compatible with system on chip (SOC) integrated technique, can be incited somebody to action
Device is easily embedded in various mobile terminals, convenient for the real-time monitoring of organic gas.
Detailed description of the invention
Fig. 1 is the structural diagram of the present invention；
Fig. 2 is acetone of the present invention, and ethyl alcohol, methanol, isopropanol gas is on sulfuration rhenium anisotropy axis with concentration variation
Response diagram；
Fig. 3 is acetone of the present invention, ethyl alcohol, methanol, the Δ I of isopropanol gas1/I1-ΔI2/I2Curve graph
Wherein: 1, silica substrate；2, sulfuration rhenium nano flake；3, first electrode；4, second electrode.
Specific embodiment
Present invention is further described in detail with specific embodiment with reference to the accompanying drawing.Under it should be understood that
State embodiment be it is illustrative, be not restrictive, cannot be limited the scope of protection of the present invention with following embodiments.Silicon wafer is adopted
The 4 inches of single-sided polishing p-type silicon chips of Prime grade provided with Suzhou Jing Xi Electronic Science and Technology Co., Ltd., crystal orientation are<100>, resistance
Rate is 9-10 Ω cm, with a thickness of 500 μm.
Referring to a kind of Fig. 1 to tool of the organic gas detection chip based on sulfuration rhenium nano-device of the present invention shown in Fig. 3
Body embodiment, it can be seen that the present invention includes sulfuration rhenium nano flake 2, first electrode 3, second electrode 4 and silica substrate
1；The sulfuration rhenium nano flake 2 is obtained using mechanical stripping, and length and width are micron order, with a thickness of nanoscale, with silica
The fitting of 1 upper surface of substrate, sulfuration rhenium intra-face anisotropy axis is respectively rhenium chain rivet and rhenium-sulphur chain rivet, rhenium chain rivet electron mobility
It is 3-4 times of rhenium-sulphur chain rivet；The first electrode 3, second electrode 4 are gold electrode, steam golden method using electron beam and are made, by
In the anisotropy of sulfuration rhenium, the anisotropy axis of the sulfuration rhenium of removing: rhenium chain rivet and rhenium-sulphur axis, are in 60 ° or hexagonal angle,
Angle between first electrode 3 and second electrode 4 is 60 °, and grows along the anisotropy axis of sulfuration rhenium.
The preparation of the above-mentioned organic gas detection chip based on sulfuration rhenium nano-device is completed according to the following steps:
Step 1: silicon wafer is put into the mixed liquor of 30wt.% hydrogen peroxide and the 98wt.% concentrated sulfuric acid and impregnates 30min, removed
The hard particles of silicon chip surface, the volume ratio of 30wt.% hydrogen peroxide and the 98wt.% concentrated sulfuric acid is 1:3 in above-mentioned mixed liquor；
It is rinsed well with deionized water in the mixed liquor for being placed on 40wt.% hydrofluoric acid and deionized water and impregnates 20min, gone
Except the SiO on surface2Layer, the volume ratio of 40wt.% hydrofluoric acid and deionized water is 1:1 in above-mentioned mixed liquor；
Silicon wafer is sequentially placed into deionized water, acetone solvent and dehydrated alcohol and is cleaned by ultrasonic 10min respectively, removes surface
It is put into after organic impurities in dehydrated alcohol as silica substrate 1；
Step 2: use mechanical stripping method be made length and width for micron order, with a thickness of nanoscale sulfuration rhenium nano flake 2 simultaneously
It is transferred into silica substrate 1, is bonded it with 1 upper surface of silica substrate；
Step 3: steaming golden method using electron beam, grows first electrode 3 and second along two anisotropy axis of sulfuration rhenium
Electrode 4, the angle between first electrode 3 and second electrode 4 are 60 °, and first electrode 3 and second electrode 4 are respectively set to mutually
Parallel two, the conducting channel formed between the electrode that every two is parallel to each other is as independent sensitive zones.
The detection method of the above-mentioned organic gas detection chip based on sulfuration rhenium nano-device:
Apply identical voltage to first electrode 3 and second electrode 4, forms base current I1And I2, when same gas absorption,
Two independent sensitive zones generate different curent changes | Δ I1| and | Δ I2|, and pass through 1 He of current sample port
Port 2 is transferred to display terminal, draws Δ I1/I1-ΔI2/I2Curve, calculated curve slope, compares with database data
Afterwards, the type of qualitative discrimination organic gas, the sound then changed on sulfuration rhenium anisotropy axis with concentration according to organic gas
Should figure quantitatively determine the concentration of organic gas, realize qualitative, the quantitative measurment of organic gas, details are as follows:
The anisotropy axis of sulfuration rhenium is sulphur-rhenium chain rivet and rhenium chain rivet, defines anisotropy axis sulphur-rhenium chain rivet of sulfuration rhenium
For a axis, rhenium chain rivet is b axis；Define sensitivity:That is a axis sensitivity isB axis
Sensitivity is
Select organic gas acetone, ethyl alcohol, methanol and isopropanol for detection gas sample, each organic gas is about a
Axle response is different with the matched curve track of b axle response, and the identification of organic gas is realized using this feature, is measured respectively organic
Gas acetone, ethyl alcohol, methanol, the linear relationship of isopropanol a axle response and b axle response, linear equation are as follows:
Acetone: y=0.3+1.025x, degree of fitting R2It is 0.984, wherein x is the corresponding a axis sensitivity response value of acetone, y
For the corresponding b axis sensitivity response value of acetone；
Ethyl alcohol: y=0.68+0.5x, degree of fitting R2It is 0.988, wherein x is the corresponding a axis sensitivity response value of ethyl alcohol, y
For the corresponding b axis sensitivity response value of ethyl alcohol；
Methanol: y=1.766+2.8x, degree of fitting R2It is 0.991, wherein x is the corresponding a axis sensitivity response value of methanol, y
For the corresponding b axis sensitivity response value of methanol；
Isopropanol: y=2.1+1.810x, degree of fitting R2It is 0.951, wherein x is the corresponding a axis sensitivity response of isopropanol
Value, y are the corresponding b axis sensitivity response value of isopropanol；
Then organic gas acetone, ethyl alcohol, methanol, sensitivity response of the isopropanol within the scope of 0-500ppm are measured respectively
The linear relationship of value, linear equation are as follows:
Acetone b axis: y=0.14+0.0126x, degree of fitting R2It is 0.991, minimum detectability 13ppm；
Acetone a axis: y=0.4095+0.013x, degree of fitting R2It is 0.995, minimum detectability 24ppm；
Ethyl alcohol b axis: y=-0.03945+0.04964x, degree of fitting R2It is 0.999, minimum detectability 2ppm；
Ethyl alcohol a axis: y=0.65122+0.02492x, degree of fitting R2It is 0.99, minimum detectability 12ppm；
Methanol b axis: y=0.81671+0.01256x, degree of fitting R2It is 0.997, minimum detectability 14ppm；
Methanol a axis: y=4.04744+0.03526x, degree of fitting R2It is 0.991, minimum detectability 5ppm；
Isopropanol b axis: y=-1.20708+0.01697x, degree of fitting R2It is 0.972, minimum detectability 21ppm；
Isopropanol a axis: y=-0.35137+0.03163x, degree of fitting R2It is 0.996, minimum detectability 3ppm；
Wherein x is the corresponding concentration of each organic gas, and y is the corresponding sensitivity response value of each organic gas.
Sulfuration rhenium intra-face anisotropy axis is respectively rhenium chain rivet and rhenium-sulphur chain rivet, and rhenium chain rivet electron mobility is rhenium-sulphur chain
3-4 times of axis.Suction type of the organic gas on two anisotropy axis of sulfuration rhenium is different, and caused electric charge transfer quantity is not
Together, it can simultaneously, it is independent from identical gas absorption obtain two dimensions electrical signal | Δ I1| and | Δ I2|, it builds
The vertical Δ I changed with concentration1/I1-ΔI2/I2Geometric locus, wherein I1And I2The respectively base current of anisotropy axis.Due to every
A kind of suction type of organic gas on sulfuration rhenium anisotropy axis is different, and electric charge transfer quantity is different, i.e., each is organic
Gas can all form oneself unique Δ I1/I1-ΔI2/I2Curve, to realize qualitative, the quantitative judge of organic gas.
In conclusion the present invention is based on the structure of the organic gas detection chip of sulfuration rhenium nano-device and preparation method letters
Single, detection sensitivity is high, can be realized qualitative, the quantitative judge of organic gas；The organic gas detection chip is having a size of micron
Grade, super low-power consumption, preparation process is integrated circuit (IC) manufacturing process of standard, simultaneous with system on chip (SOC) integrated technique
Hold, device can be easily embedded in various mobile terminals, convenient for the real-time monitoring of organic gas.
The organic gas inspection based on sulfuration rhenium nano-device can be achieved according to the adjustment that summary of the invention carries out technological parameter
The preparation of chip is surveyed, and shows the performance almost the same with above-described embodiment.Illustrative description has been done to the present invention above,
It should be noted that in the case where not departing from core of the invention, any simple deformation, modification or other this field skills
Art personnel can not spend the equivalent replacement of creative work to each fall within protection scope of the present invention.
Claims (10)
1. a kind of organic gas detection chip based on sulfuration rhenium nano-device, it is characterised in that: including sulfuration rhenium nano flake,
First electrode, second electrode and silica substrate；The sulfuration rhenium nano flake is bonded with silica upper surface of substrate,
The first electrode, second electrode are grown along the anisotropy axis of sulfuration rhenium.
2. the organic gas detection chip according to claim 1 based on sulfuration rhenium nano-device, it is characterised in that: described
Sulfuration rhenium nano flake obtained using mechanical stripping or dry method transfer method, length and width are micron order, with a thickness of nanoscale.
3. the organic gas detection chip according to claim 1 based on sulfuration rhenium nano-device, it is characterised in that: described
First electrode and second electrode be gold electrode, golden method is steamed using electron beam and is made, the angle between first electrode and second electrode
Degree is 60 ° or 120 °.
4. the preparation method of the organic gas detection chip based on sulfuration rhenium nano-device as described in claim 1, feature
It is:
Step 1: silicon wafer is put into the mixed liquor of 30wt.% hydrogen peroxide and the 98wt.% concentrated sulfuric acid and impregnates 29-31min, removed
The hard particles of silicon chip surface, the volume ratio of 30wt.% hydrogen peroxide and the 98wt.% concentrated sulfuric acid is 1:3 in above-mentioned mixed liquor；
It is rinsed well with deionized water in the mixed liquor for being placed on 40wt.% hydrofluoric acid and deionized water and impregnates 19-21min, gone
Except the SiO on surface2Layer, the volume ratio of 40wt.% hydrofluoric acid and deionized water is 1:1 in above-mentioned mixed liquor；
Silicon wafer is sequentially placed into deionized water, acetone solvent and dehydrated alcohol and is cleaned by ultrasonic 9-11min respectively, removal surface has
It is put into after machine object impurity in dehydrated alcohol as silica substrate；
Step 2: using mechanical stripping method or dry method transfer method, and it is micron order, with a thickness of nanoscale sulfuration rhenium that length and width, which are made,
Nano flake is simultaneously transferred into silica substrate, is bonded it with silica upper surface of substrate；
Step 3: steaming golden method using electron beam, grows first electrode and second electrode along two anisotropy axis of sulfuration rhenium.
5. the preparation method of the organic gas detection chip according to claim 4 based on sulfuration rhenium nano-device, special
Sign is: described is gold electrode, and the angle between first electrode and second electrode is 60 ° or 120 °.
6. the preparation method of the organic gas detection chip according to claim 4 based on sulfuration rhenium nano-device, special
Sign is: first electrode and second electrode in the step 3 are respectively set to be parallel to each other two, and every two is mutually flat
The conducting channel formed between capable electrode is as independent sensitive zones.
7. application of the sulfuration rhenium nano material in organic gas detection.
8. the detection method of the organic gas detection chip based on sulfuration rhenium nano-device as described in claim 1, feature
It is:
Apply identical voltage to first electrode and second electrode, forms base current I1And I2, when same gas absorption, two solely
Vertical sensitive zones generate different curent changes | Δ I1| and | Δ I2|, and pass through current sample port 1 and port 2,
It is transferred to display terminal, draws Δ I1/I1-ΔI2/I2Curve, calculated curve slope are fixed after comparing with database data
Property differentiate organic gas type, then according to organic gas on sulfuration rhenium anisotropy axis with concentration variation response diagram come
The concentration for quantitatively determining organic gas realizes qualitative, the quantitative measurment of organic gas.
9. the detection method of the organic gas detection chip according to claim 8 based on sulfuration rhenium nano-device, special
Sign is:
Each organic gas is different with the matched curve track of b axle response about a axle response, is realized using this feature organic
The identification of gas measures organic gas acetone, ethyl alcohol, methanol, the linear relationship of isopropanol a axle response and b axle response, line respectively
Property equation is as follows:
Acetone: y=0.3+1.025x, degree of fitting R2It is 0.984；
Ethyl alcohol: y=0.68+0.5x, degree of fitting R2It is 0.988；
Methanol: y=1.766+2.8x, degree of fitting R2It is 0.991；
Isopropanol: y=2.1+1.810x, degree of fitting R2It is 0.951；
Wherein x is the corresponding a axis sensitivity response value of each organic gas, and y is that the corresponding b axis of each organic gas is sensitive
Spend response.
10. the detection method of the organic gas detection chip according to claim 8 based on sulfuration rhenium nano-device, special
Sign is:
Respectively measure organic gas acetone, ethyl alcohol, methanol, sensitivity response value of the isopropanol within the scope of 0-500ppm it is linear
Relationship, linear equation are as follows:
Acetone b axis: y=0.14+0.0126x, degree of fitting R2It is 0.991, minimum detectability 13ppm；
Acetone a axis: y=0.4095+0.013x, degree of fitting R2It is 0.995, minimum detectability 24ppm；
Ethyl alcohol b axis: y=-0.03945+0.04964x, degree of fitting R2It is 0.999, minimum detectability 2ppm；
Ethyl alcohol a axis: y=0.65122+0.02492x, degree of fitting R2It is 0.99, minimum detectability 12ppm；
Methanol b axis: y=0.81671+0.01256x, degree of fitting R2It is 0.997, minimum detectability 14ppm；
Methanol a axis: y=4.04744+0.03526x, degree of fitting R2It is 0.991, minimum detectability 5ppm；
Isopropanol b axis: y=-1.20708+0.01697x, degree of fitting R2It is 0.972, minimum detectability 21ppm；
Isopropanol a axis: y=-0.35137+0.03163x, degree of fitting R2It is 0.996, minimum detectability 3ppm；
Wherein x is the corresponding concentration of each organic gas, and y is the corresponding sensitivity response value of each organic gas.
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| WO2022112079A1 (en) * | 2020-11-27 | 2022-06-02 | IFP Energies Nouvelles | Method for the selective hydrogenation of a gasoline in the presence of a catalyst on a mesoporous-macroporous substrate |
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