CN109270127A - A kind of planar semiconductor gas sensor chip and preparation method thereof - Google Patents
A kind of planar semiconductor gas sensor chip and preparation method thereof Download PDFInfo
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- CN109270127A CN109270127A CN201811132306.7A CN201811132306A CN109270127A CN 109270127 A CN109270127 A CN 109270127A CN 201811132306 A CN201811132306 A CN 201811132306A CN 109270127 A CN109270127 A CN 109270127A
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Abstract
The present invention relates to the preparation of gas sensor, a kind of planar semiconductor gas sensor chip and preparation method thereof is further related to.The method is by mesoporous Pd-SnO2Composite material suspension is added drop-wise in interdigital electrode, is calcined, then after cooling to obtain the final product.Semiconductor gas sensor resistance provided by the invention drops to 1M hereinafter, air-sensitive response rises to 90% or more；Gas sensor resistance is not much different under the same same calcination temperature of batch sample, meets the consistency of subsequent instrumentation gage requirement, saves time, cost etc.；The gas sensor chip is to H2There is preferable stability；The stability of chip surface material is enhanced, its gas sensitive in the assembling of subsequent instrumentation instrument, encapsulation process is made to be not easy to fall；Electrode passivation after the gas sensor chip vacuum anaerobic calcining, makes it not be affected by the external environment.
Description
Technical field
The present invention relates to the preparation of gas sensor, more particularly, to a kind of planar semiconductor gas sensor chip and
Preparation method.
Background technique
Hydrogen is a kind of common fuel gas, and compared to other fuel gas, hydrogen is with broader explosive range
(4-75%) and lower kindling energy (0.019mJ).Simultaneously as the molecular structure of hydrogen is small, and gas density is light, makes it
Leakage possibility in actual production and life is higher.It therefore, is the generation for preventing hydrogen gas leakage and explosion accident, for each
The real-time accurate detection of density of hydrogen and just especially important of alarming in class application environment.
In the field of gas sensing equipment, although domestic sensing terminal product occupies certain low-end market share,
In terms of high-end sensor element and detection device, still in backward status, and to be realized on transducer market and technology
Break developed country's monopolization it is necessary to start with from technology source.Existing gas detection terminal device, core are sensing element
Part, and the core of sensing element is sensing material, still, wherein most of new material has the following problems: (1) material
Expect that resistance itself is big, it is with high requirements and high cost to Au interdigital electrode；(2) response of material air-sensitive is low, and sensing capabilities are poor；(3) material
It is poor with element stability, make its gas sensitive in the assembling of subsequent instrumentation instrument, encapsulation process be easy to fall.And it is existing this
A series of problems makes the relevant technologies achievement stop at laboratory stage, and then it is caused to be difficult by scale of mass production and finally to answer
For launch products.
Therefore, combination technology research and development of the present invention and two key factors of actual production, are applied to pass to novel sensing material
Sensor chip is handled, it is made to be improved in terms of reducing component resistance, increasing response, enhancing stability.
Summary of the invention
The first object of the present invention is to provide a kind of preparation method of planar semiconductor gas sensor chip, including
Following steps:
By mesoporous Pd-SnO2Composite material suspension is added drop-wise in interdigital electrode, is calcined, then after cooling to obtain the final product.
Preferably, the calcination temperature of the calcining is 500-550 DEG C, calcination time 3-5h；It is further preferred that the calcining
Temperature is 500 DEG C.
The present invention creatively selects the spraying for carrying out sensitive layer to interdigital electrode with calcining manners, and further sends out
The better condition of effect and parameter are showed, under the conditions of above-mentioned parameter, gas sensor chip can effectively be prepared.
Preparation method of the present invention, it is preferable that inert gas is passed through when calcining, flow velocity is 60 ± 5sccm/s, and
It is calcined under vacuum low-pressure, condition is 3.8 ± 0.5 × 10-1Pa.Calcining helps to prevent two to a certain extent under vacuum low-pressure
Stannic oxide materials crystal phase changes.
Preparation method of the present invention, it is preferable that the mesoporous Pd-SnO is being added dropwise2When composite material suspension, control
System formed resulting film with a thickness of 5-11 μm；In above-mentioned thickness range, gas sensing performance is best.According to general scenario,
The mesoporous Pd-SnO2The dosage of composite material suspension is 0.05-0.08ml.
Preparation method of the present invention, it is preferable that the mesoporous Pd-SnO2In composite material, the molar ratio of Pd and Sn
For (0.03-0.05): 100；
It is highly preferred that the mesoporous Pd-SnO2Composite material suspension is Pd-SnO2Composite material is scattered in distilled water and obtains
It arrives, mass volume ratio is (0.5-1) mg/ (0.1-0.3) mL；
Preferably, the dispersion is ultrasonic disperse, and the condition of ultrasonic disperse is the frequency of 20KHz or so (20 ± 5KHz),
The cleaning temperature of aqueous cleaning is 40 ± 5 DEG C, ultrasonic time 1-3 (preferably 2) min.
As optimal technical scheme, the mesoporous Pd-SnO2Composite material suspension is prepared in the following manner:
The mesoporous Pd-SnO2The preparation of composite material suspension includes the following steps:
1) chlorine palladium acid solution and mesopore molecular sieve are sequentially added into the ethanol solution of stannous chloride, it is dry after mixing, it obtains
Pd-SnO2Composite material precursor；2) by the Pd-SnO2Composite material precursor calcines 4-6h at 500-550 DEG C, removes
The Pd-SnO is obtained after the mesopore molecular sieve2Nanocomposite；3) by mesoporous Pd-SnO2Ultrasound in distilled water is added in material
It makes it dissolve to obtain suspension；
Preferably, the mass ratio of the stannous chloride, chlorine palladium acid and mesopore molecular sieve is 317:(1.25-1.3): (180-
200)。
Preparation method of the present invention, the interdigital electrode are golden interdigital electrode；And/or the electricity of the interdigital electrode
Logarithm extremely pair is 6 pairs, interdigital width 0.120mm, it is adjacent it is interdigital between clearance distance be 0.100mm, the thickness of interdigital electrode
Spend 0.7mm.
Preparation method of the present invention, by mesoporous Pd-SnO2Composite material suspension is added drop-wise in interdigital electrode, is done
After dry, then calcined, cooled down；
The temperature of the drying is 60-80 DEG C, time 4-6h.It is dry at above-mentioned temperature, there is enhancing gas sensing
The advantages of energy.
Specifically, preparation method of the present invention includes the following steps:
1) the mesoporous Pd-SnO that will be prepared2Material is added ultrasound in distilled water and makes it dissolve；
2) suspension of dissolution is dripped in golden interdigital electrode, after dry, be placed in CVD furnace high-temperature, anaerobic, low pressure into
Row calcining.
3) it is naturally cooling to room temperature under anaerobic, low pressure and takes out Au interdigital electrode.
In a preferred embodiment of the invention, the mesoporous Pd-SnO2Material preparation method includes the following steps:
1) chlorine palladium acid solution and mesopore molecular sieve are sequentially added into the ethanol solution of stannous chloride, it is dry after mixing, obtain Pd-SnO2
Composite material precursor；2) by the Pd-SnO2Composite material precursor calcines 6h at 550 DEG C, removes the mesoporous molecular
The Pd-SnO is obtained after sieve2Nanocomposite.
The present invention provides above-mentioned any one technical solution preparation-obtained planar semiconductor gas sensor core together
Piece.
The high sensitivity of gas sensor chip provided by the present invention, stability is strong, fast response time, reproducible.
Further, the application that a kind of planar semiconductor gas sensor chip is used to detect hydrogen is provided.
Application of the present invention is preferably 140-160 DEG C (most preferably 150 DEG C) using temperature, humidity 10%-
The H in air is detected under conditions of 40%2。
Under the above conditions, testing result is more accurate.
Compared with prior art, the beneficial effects of the present invention are:
(1) semiconductor gas sensor processing technique provided by the invention and untreated gas sensor compare, untreated
Preceding mesoporous SnO2The resistance of-Pd sensor chip very about 450M or so, air-sensitive response are 50-60%, and by true
After sky, anaerobic, low pressure calcination processing, resistance drops to 1M hereinafter, air-sensitive response rises to 90% or more；
(2) semiconductor gas sensor processing technique provided by the invention and untreated gas sensor compare, untreated
Gas sensor same batch sample resistance difference it is larger, and after vacuum anaerobic calcination processing, same batch sample is same
Gas sensor resistance is not much different under one calcination temperature, meets the consistency of subsequent instrumentation gage requirement, can in high volume repeat to give birth to
It produces, saves time, cost etc.；
(3) gas sensor of semiconductor gas sensor processing technique preparation provided by the invention is 100ppm to concentration
H2There is preferable stability in 21 days, resistance is maintained at 1M hereinafter, air-sensitive response is stablized 90% or more；
(4) semiconductor gas sensor processing technique provided by the invention, the material on Au interdigital electrode surface vacuum without
Under oxygen high temperature, remaining a part of palladium dydroxide can dehydrogenation generation palladium oxide in material；
(5) gas sensor of semiconductor gas sensor processing technique preparation provided by the invention enhances chip surface
The stability of material makes its gas sensitive in the assembling of subsequent instrumentation instrument, encapsulation process be not easy to fall；
(6) after the gas sensor vacuum anaerobic calcining of semiconductor gas sensor processing technique preparation provided by the invention
Electrode passivation makes it not be affected by the external environment.
Detailed description of the invention
Fig. 1 is the sensitivity curve of treated the gas sensor detection 100ppm hydrogen of embodiment 1；
Fig. 2 is the sensitivity curve of treated the gas sensor detection 100ppm hydrogen of embodiment 2；
Fig. 3 is the sensitivity curve of treated the gas sensor detection 100ppm hydrogen of embodiment 3；
Fig. 4 is the sensitivity curve of treated the gas sensor detection 100ppm hydrogen of embodiment 4；
Fig. 5 is the sensitivity curve of treated the gas sensor detection 100ppm hydrogen of embodiment 5；
Fig. 6 is histogram shown in resistance-calcination time of treated the gas sensor detection 100ppm hydrogen of embodiment 6.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Such as not specified otherwise such as raw material involved in following embodiment, test example, reagent is both from commercially available.
Mesoporous Pd-SnO involved in following embodiment, test example2Material is prepared as follows:
1) chlorine palladium acid solution and mesopore molecular sieve are sequentially added into the ethanol solution of stannous chloride, it is dry after mixing, it obtains
Pd-SnO2Composite material precursor；Wherein the mass ratio of stannous chloride, chlorine palladium acid and mesopore molecular sieve is 317:(1.25-
1.3):(180-200)。
2) by the Pd-SnO2Composite material precursor calcines 6h at 550 DEG C, is then removed with sodium hydroxide solution
The mesopore molecular sieve, up to the mesoporous Pd-SnO after centrifugation, separation, drying2Material.
Embodiment 1
A kind of preparation method of planar semiconductor gas sensor chip is present embodiments provided, specifically according to the following steps
It carries out:
(1) by the mesoporous Pd-SnO of 0.5mg2Ultrasound in 0.1ml distilled water is added in material, and (ultrasound condition is 20KHz's or so
Frequency, the cleaning temperature of aqueous cleaning are 40 DEG C, ultrasonic time 2min) it makes it dissolve, obtain suspension；
(2) aaerosol solution that step (1) obtains is measured 0.05ml with liquid-transfering gun to drip in Au interdigital electrode, and 60
4h is dried at DEG C, and Gas Sensors of Electric Resistance Semiconductors is made；
(3) Gas Sensors of Electric Resistance Semiconductors that step (2) is prepared is placed in CVD furnace high-temperature, anaerobic, low
Pressure calcining, calcination temperature are 500 DEG C, calcination time 3h, are passed through inert gas argon gas, flow velocity 60sccm/s, vacuum low-pressure
It is 3.8 × 10-1Pa；
(4) Au interdigital electrode is taken out to be naturally cooling to room temperature under step (3) anaerobic, low pressure.
Embodiment 2
A kind of preparation method of planar semiconductor gas sensor chip is present embodiments provided, specifically according to the following steps
It carries out:
(1) by the mesoporous Pd-SnO of 0.5mg2Ultrasound in 0.1ml distilled water is added in material, and (ultrasound condition is 20KHz's or so
Frequency, the cleaning temperature of aqueous cleaning are 40 DEG C, ultrasonic time 2min) it makes it dissolve, obtain suspension；
(2) aaerosol solution that step (1) obtains is measured 0.05ml with liquid-transfering gun to drip in Au interdigital electrode, and 80
6h is dried at DEG C, and Gas Sensors of Electric Resistance Semiconductors is made；
(3) Gas Sensors of Electric Resistance Semiconductors that step (2) is prepared is placed in CVD furnace high-temperature, anaerobic, low
Pressure calcining, calcination temperature are 500 DEG C, calcination time 4h, are passed through inert gas argon gas, flow velocity 60sccm/s, vacuum low-pressure
It is 3.8 × 10-1Pa；
(4) Au interdigital electrode is taken out to be naturally cooling to room temperature under step (3) anaerobic, low pressure.
Embodiment 3
A kind of preparation method of planar semiconductor gas sensor chip is present embodiments provided, specifically according to the following steps
It carries out:
(1) by the mesoporous Pd-SnO of 0.5mg2Ultrasound in 0.1ml distilled water is added in material, and (ultrasound condition is 20KHz's or so
Frequency, the cleaning temperature of aqueous cleaning are 40 DEG C, ultrasonic time 2min) it makes it dissolve, obtain suspension；
(2) aaerosol solution that step (1) obtains is measured 0.05ml with liquid-transfering gun to drip in Au interdigital electrode, and 60
6h is dried at DEG C, and Gas Sensors of Electric Resistance Semiconductors is made；
(3) Gas Sensors of Electric Resistance Semiconductors that step (2) is prepared is placed in CVD furnace high-temperature, anaerobic, low
Pressure calcining, calcination temperature are 500 DEG C, calcination time 5h, are passed through inert gas argon gas, flow velocity 60sccm/s, vacuum low-pressure
It is 3.8 × 10-1Pa；
(4) Au interdigital electrode is taken out to be naturally cooling to room temperature under step (3) anaerobic, low pressure.
Embodiment 4
A kind of preparation method of planar semiconductor gas sensor chip is present embodiments provided, specifically according to the following steps
It carries out:
(1) by the mesoporous Pd-SnO of 0.8mg2Ultrasound in 0.2ml distilled water is added in material, and (ultrasound condition is 20KHz's or so
Frequency, the cleaning temperature of aqueous cleaning are 40 DEG C, ultrasonic time 2min) it makes it dissolve, obtain suspension；
(2) aaerosol solution that step (1) obtains is measured 0.08ml with liquid-transfering gun to drip in Au interdigital electrode, and 60
6h is dried at DEG C, and Gas Sensors of Electric Resistance Semiconductors is made；
(3) Gas Sensors of Electric Resistance Semiconductors that step (2) is prepared is placed in CVD furnace high-temperature, anaerobic, low
Pressure calcining, calcination temperature are 500 DEG C, calcination time 3h, are passed through inert gas argon gas, flow velocity 60sccm/s, vacuum low-pressure
It is 3.8 × 10-1Pa；
(4) Au interdigital electrode is taken out to be naturally cooling to room temperature under step (3) anaerobic, low pressure.
Embodiment 5
A kind of preparation method of planar semiconductor gas sensor chip is present embodiments provided, specifically according to the following steps
It carries out:
(1) by the mesoporous Pd-SnO of 1.0mg2Ultrasound in 0.3ml distilled water is added in material, and (ultrasound condition is 20KHz's or so
Frequency, the cleaning temperature of aqueous cleaning are 40 DEG C, ultrasonic time 2min) it makes it dissolve, obtain suspension；
(2) aaerosol solution that step (1) obtains is measured 0.08ml with liquid-transfering gun to drip in Au interdigital electrode, and 60
5h is dried at DEG C, and Gas Sensors of Electric Resistance Semiconductors is made；
(3) Gas Sensors of Electric Resistance Semiconductors that step (2) is prepared is placed in CVD furnace high-temperature, anaerobic, low
Pressure calcining, calcination temperature are 500 DEG C, calcination time 5h, are passed through inert gas argon gas, flow velocity 60sccm/s, vacuum low-pressure
It is 3.8 × 10-1Pa；
(4) Au interdigital electrode is taken out to be naturally cooling to room temperature under step (3) anaerobic, low pressure.
Embodiment 6
A kind of preparation method of planar semiconductor gas sensor chip is present embodiments provided, specifically according to the following steps
It carries out:
(1) by the mesoporous Pd-SnO of 1mg2Ultrasound in 0.2ml distilled water is added in sample, and (ultrasound condition is the frequency of 20KHz or so
Rate, the cleaning temperature of aqueous cleaning are 40 DEG C, ultrasonic time 2min) it makes it dissolve, obtain suspension；
(2) aaerosol solution that step (1) obtains is measured into 0.05ml with liquid-transfering gun respectively and drips to three Au interdigital electrodes
On, and dry 4h at 60 DEG C and Gas Sensors of Electric Resistance Semiconductors is made；
(3) three Gas Sensors of Electric Resistance Semiconductors of the same batch sample that step (2) is prepared are placed in CVD
Furnace high-temperature, anaerobic, low pressure calcining, calcination temperature are 500 DEG C, are passed through inert gas argon gas, flow velocity 60sccm/s, vacuum
Low pressure is 3.8 × 10-1Pa, calcination time are respectively 3h, 4h, 5h；
(4) Au interdigital electrode is taken out to be naturally cooling to room temperature under step (3) anaerobic, low pressure.
Test example 1
This test example provides the sensitivity verifying of planar semiconductor gas sensor chip provided by the above embodiment.
Test objective: the sensitivity of planar semiconductor gas sensor chip provided by verifying embodiment 1-6.
Test method:
It sequentially includes the following steps:
By gas sensor set temperature be 150 DEG C, under conditions of humidity is 20% to H2It is detected；
Having surveyed original untreated gas sensor resistance is 450M, and air-sensitive response is 64%；
The method for preparing original untreated gas sensor are as follows: by mesoporous Pd-SnO2Material is placed in mortar, is added suitable
Distilled water is measured, grinding obtains uniform suspension, then suspension is spin-coated in Au interdigital electrode, is placed in forced air drying
6h is dried in case at 80 DEG C to get original untreated gas sensor is arrived.
Test result:
Fig. 1 is the sensitivity curve of treated the gas sensor detection 100ppm hydrogen of embodiment 1, is passing through embodiment 1
Gas sensor resistance after processing is reduced to 600K hereinafter, after being passed through 3 circulation 100ppm hydrogen, and material air-sensitive responds
It improves to 92%, wherein sensitivity S=(Rg-Ra)/Ra × 100%.
Fig. 2 is the sensitivity curve of treated the gas sensor detection 100ppm hydrogen of embodiment 2, is passing through embodiment 2
Gas sensor resistance after processing is reduced to 800K or so, after being passed through 3 circulation 100ppm hydrogen, the response of material air-sensitive
It improves to 95%, wherein sensitivity S=(Rg-Ra)/Ra × 100%.
Fig. 3 is the sensitivity curve of treated the gas sensor detection 100ppm hydrogen of embodiment 3, is passing through embodiment 3
Gas sensor resistance after processing is reduced to 900K or so, after being passed through 3 circulation 100ppm hydrogen, the response of material air-sensitive
It improves to 97%, wherein sensitivity S=(Rg-Ra)/Ra × 100%.
Fig. 4 is the sensitivity curve of treated the gas sensor detection 100ppm hydrogen of embodiment 4, is passing through embodiment 4
Gas sensor resistance after processing is reduced to 120K hereinafter, after being passed through 3 circulation 100ppm hydrogen, and material air-sensitive responds
It improves to 90%, wherein sensitivity S=(Rg-Ra)/Ra × 100%.
Fig. 5 is the sensitivity curve of treated the gas sensor detection 100ppm hydrogen of embodiment 5, is passing through embodiment 5
Gas sensor resistance after processing is reduced to 60K hereinafter, after being passed through 3 circulation 100ppm hydrogen, and the response of material air-sensitive mentions
Up to 92%, wherein sensitivity S=(Rg-Ra)/Ra × 100%.
Test example 2
The planar semiconductor gas sensor chip that this test example verifies the offer of above-described embodiment 1 is being placed 21 days in
Air-sensitive stability.
Test objective: verifying embodiment 1 is being placed in 21 days to the air-sensitive response of 100ppm hydrogen and resistance.
Test method:
It is once tested within 7 days every to the planar semiconductor gas sensor chip of offer provided by embodiment 1, by
Will affect air-sensitive film in humidity, thus before each test to the planar semiconductor gas sensor chip at 60 DEG C
Lower drying 4h.
From, it can be found that the air-sensitive response measured in 21 days is not much different substantially, and resistance is also able to maintain in table 1
600K or so, this shows that the gas sensor after processing under the premise of keeping resistance and air-sensitive response is constant, still there is one
Preferable stability.
Table 1
| Electrode membrane material | Time | Resistance | Air-sensitive response |
| Mesoporous Pd-SnO2 | After 0 day | 600K | 93% |
| Mesoporous Pd-SnO2 | After 7 days | 586K | 91% |
| Mesoporous Pd-SnO2 | After 14 days | 596K | 90% |
| Mesoporous Pd-SnO2 | After 21 days | 623K | 92% |
Test example 3
This test example verifies the resistance homogeneity for the planar semiconductor gas sensor chip that embodiment 6 provides.
Test method:
The application of the processing technique of the planar semiconductor gas sensor chip provided in above-described embodiment 6 is by following step
It is rapid to carry out:
By gas sensor set temperature be 150 DEG C, under conditions of humidity is 20% to H2It is detected；
Having surveyed original untreated gas sensor resistance is 450M, and air-sensitive response is 64%；
The method for preparing original untreated gas sensor are as follows: by mesoporous Pd-SnO2Material is placed in mortar, is added suitable
Distilled water is measured, grinding obtains uniform suspension, then suspension is spin-coated in Au interdigital electrode, is placed in forced air drying
6h is dried in case at 80 DEG C to get original untreated gas sensor is arrived；
Test result:
Fig. 6 is histogram shown in resistance-calcination time of treated the gas sensor detection 100ppm hydrogen of embodiment 6,
When calcining 3h, resistance can be stablized in 800K or so gas sensor after handling by embodiment 6；When calcining 4h,
Resistance stabilization is in 550K or so；When calcining 5h, resistance stabilization is in 58K or so；This shows the gas sensitive element after this method processing
Part resistance has homogeneity, and extends with calcination time, and resistance is smaller；
Table 2 is treated the gas sensor of embodiment 6 detection 100ppm hydrogen resistance and air-sensitive response, with a batch of
Sample is tested three times respectively, and when calcining 3h, resistance can be stablized in 800K or so, and air-sensitive response is stablized 97%；?
When calcining 4h, resistance stabilization is stablized in 550K or so, air-sensitive response 95%；When calcining 5h, resistance stabilization in 58K or so,
Air-sensitive response is stablized 90%；This show this method processing after gas sensor resistance have homogeneity, and with
Calcination time extends, and resistance is smaller, and air-sensitive response slightly reduces, subsequent voluntarily to select according to demand.Wherein sensitivity S=
(Rg-Ra)/Ra × 100%.
Table 2
| 3h | 4h | 5h | |
| Resistance | 884K | 555K | 58K |
| Air-sensitive response | 97% | 95% | 90% |
| Resistance | 886K | 545K | 56K |
| Air-sensitive response | 97% | 94% | 92% |
| Resistance | 868K | 550K | 55K |
| Air-sensitive response | 98% | 94% | 89% |
Although above having used general explanation, specific embodiment and test, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is aobvious and easy to those skilled in the art
See.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to that the present invention claims guarantors
The range of shield.
Claims (10)
1. a kind of preparation method of gas sensor chip, which is characterized in that by mesoporous Pd-SnO2Composite material suspension is added dropwise
It onto interdigital electrode, is calcined, then after cooling to obtain the final product.
2. preparation method according to claim 1, which is characterized in that the calcination temperature of the calcining is 500-550 DEG C, is forged
The burning time is 3-5h；
Preferably, the calcination temperature is 500 DEG C.
3. preparation method according to claim 1 or 2, which is characterized in that need oxygen-free environment when calcining and in vacuum low-pressure
Lower calcining, condition are 3.8 ± 0.5 × 10-1Pa；
Preferably, it is passed through inert gas, flow velocity is 60 ± 5sccm/s.
4. preparation method according to claim 1-3, which is characterized in that the mesoporous Pd-SnO2Composite material
In, the molar ratio of Pd and Sn are (0.03-0.05): 100；
Preferably, the mesoporous Pd-SnO2It is (0.5-1) mg/ (0.1-0.3) that composite material suspension, which is according to mass volume ratio,
ML is by the mesoporous Pd-SnO2Composite material is scattered in what distilled water obtained；
It is further preferred that the frequency being separated into 20 ± 5KHz, cleaning temperature is 40 ± 5 DEG C, ultrasonic time 1-3min.
5. preparation method according to claim 1-4, which is characterized in that the mesoporous Pd-SnO2Composite material is outstanding
Turbid is prepared in the following manner:
1) chlorine palladium acid solution and mesopore molecular sieve are sequentially added into the ethanol solution of stannous chloride, it is dry after mixing, obtain Pd-
SnO2Composite material precursor；
2) by the Pd-SnO2Composite material precursor calcines 4-6h at 500-550 DEG C, obtains after removing the mesopore molecular sieve
The Pd-SnO2Nanocomposite；
3) by mesoporous Pd-SnO2Material is added dispersion in distilled water and makes it dissolve to obtain suspension；
Preferably, the mass ratio of the stannous chloride, chlorine palladium acid and mesopore molecular sieve is 317:(1.25-1.3): (180-200).
6. preparation method according to claim 1-5, which is characterized in that the interdigital electrode is the interdigital electricity of gold
Pole；
And/or
The electrode of the interdigital electrode is 6 pairs to logarithm, interdigital width 0.120mm, it is adjacent it is interdigital between clearance distance be
The thickness 0.7mm of 0.100mm, interdigital electrode.
7. preparation method according to claim 1-6, which is characterized in that by mesoporous Pd-SnO2Composite material is suspended
Drop is added in interdigital electrode, after dry, then calcined, is cooled down；
The temperature of the drying is 60-80 DEG C, time 4-6h.
8. a kind of gas sensor chip, which is characterized in that be prepared by the described in any item preparation methods of claim 1-7
It arrives.
9. described in gas sensor chip and/or claim 8 that preparation method of any of claims 1-7 obtains
Gas sensor chip be used to detect the application of hydrogen.
10. application according to claim 9, which is characterized in that temperature when detection is 140-160 DEG C, humidity 10%-
40%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811132306.7A CN109270127A (en) | 2018-09-27 | 2018-09-27 | A kind of planar semiconductor gas sensor chip and preparation method thereof |
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