CN110044969A - Load rodlike ZnO nano material of Au nanoparticle and preparation method thereof and its application in acetone gas sensor - Google Patents
Load rodlike ZnO nano material of Au nanoparticle and preparation method thereof and its application in acetone gas sensor Download PDFInfo
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Abstract
The present invention provides a kind of rodlike ZnO nano material for loading Au nanoparticle, its crystal is in rhabdolith, the average grain diameter of crystal particles is 50nm, Au nanoparticle uniform load provides the preparation method and its application in acetone gas sensor of the nano material in ZnO nanoparticle surface.The present invention, as sensitive material, not only applies its high specific surface area using the rodlike ZnO nano material of load Au nanoparticle, can also effectively utilize Au and improve air-sensitive response to the catalytic action on the surface ZnO and acetone gas；Furthermore acetone gas sensor of the invention is the improvement to existing structure, the rodlike ZnO nano material of above-mentioned load Au nanoparticle is coated on sensing element, it is simple with preparation method, it is low in cost, outstanding quick response recovery characteristics, the characteristics of can be mass-produced, have good detection performance to acetone gas.
Description
Technical field
The invention belongs to gas sensor technical fields, and in particular to a kind of rodlike ZnO nano of Au Nanoparticle Modified
Material is acetone gas sensor and its preparation side of gas sensitive material.
Background technique
Acetone is in the industrial production mainly as solvent for process hides, explosive, rubber, spray painting, plastics, grease, fiber etc.
In industry, synthesis iodoform, aceticanhydride, ketenes, polyisoprene rubber, chloroform, methyl methacrylate, asphalt mixtures modified by epoxy resin can also be used as
The important source material ingredient of the substances such as rouge.However acetone has biggish harm to human health, when being mainly shown as acute poisoning pair
There is nauseous, out of strength, dizzy, headache, emotional symptom in the anesthetic effect of central nervous system.Serious person then occur it is out of breath,
Vomiting, spasm, or even stupor.Gas is irritant to eye, nose, larynx.And the Chronic Effect of acetone has because Long Term Contact occurs
Calcination, spinning sensation, bronchitis, pharyngitis, emotional, out of strength etc..Long Term Contact skin can lead to dermatitis.Acetone itself has again
There is extremely inflammable, explosive characteristic.Quick, intelligent detection acetone gas sensor is thus developed as urgent demand.
In all kinds of gas sensors, MOS type gas sensor has highly sensitive, selection because of it
Property good, response restores fast, cost is relatively low and it is easy to carry the advantages that, become the gas sensor that is most widely used at present it
One.Metal-oxide semiconductor (MOS) gas sensor can use sensitive material and directly adsorb under test gas, so that the electricity of material
The features such as property change, and detect the dense of under test gas to the output signal variation of sensing element by detection peripheral circuit
Degree.There is also very big influences to air-sensitive performance for the different oxide semiconductor sensitive material of pattern, so can usually pass through
The sensitive material of different-shape is synthesized to improve the air-sensitive performance of material.In addition, air-sensitive performance of the catalysis material to sensitive material
Also there is very big influence.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of rodlike ZnO nano material for loading Au (gold) nanoparticle.
It is a further object of the present invention to provide the preparation methods of the rodlike ZnO nano material of load Au nanoparticle.
Another object of the present invention is to provide the rodlike ZnO nano material of load Au nanoparticle in acetone gas sensor
In application.
The rodlike ZnO nano material of the so-called load Au nanoparticle of the present invention, crystal are in rhabdolith, crystal particles
Average grain diameter be 50nm, Au nanoparticle uniform load is in ZnO nanoparticle surface.
The preparation method of the rodlike ZnO nano material of load Au nanoparticle of the invention, includes the following steps:
Step 1: preparing rodlike ZnO
Rodlike ZnO to prepare adoptable method more, such as hydro-thermal method, thermal evaporation zinc powder method, microwave heating method etc., this
Invention provides following preparation method:
1~4g NaOH is added in 30~45ml water by S11, is made it completely dissolved, and solution A is denoted as；
S12 is by 0.5~1.0g ZnSO4It is dissolved in 10~15ml water, makes it completely dissolved, be denoted as B solution；
S13A solution is placed under 55~70 DEG C of water-baths, and B solution is added dropwise in solution A, with stirring while dropwise addition；It
Afterwards with 40~60ml water dilute solution, then in 60~80 DEG C of dry 4~6 hours；Then it to mixed liquor centrifuge washing, will precipitate
Object is 12~24 hours dry at 60~80 DEG C, grinds after taking-up, obtains rodlike ZnO white powder.
Step 2: the preparation of the rodlike ZnO nano material of Au Nanoparticle Modified
S21 takes rodlike 0.02~0.1g of ZnO powder made from step 1 to be added in 25~50ml water, keeps it completely molten
Solution；
0.04~0.08ml, concentration are the HAuCl of 45~60mmol/L by S224Solution is added to solution made from S21
In, mix it uniformly；
S23 is by 1.0~3.0ml NH3·H2O is added in mixed solution made from S22, is reacted 1.5~3 hours；
S24 collects reaction product made from S23, is washed with deionized water and absolute alcohol, and at 55~70 DEG C dry 3~5
Hour, gained powder Muffle furnace is annealed 1~2 hour at 340~360 DEG C finally, is taken out powder mull 20~30 minutes
The rodlike ZnO nano material of Au Nanoparticle Modified is obtained afterwards.
Further, aqueous solvent used in step 1 and step 2 is deionized water or ultrapure water.
Further, the speed that B solution is added dropwise to solution A in above-mentioned steps S13 is 1 drop/sec, and control rate of addition makes sulphur
Sour zinc and sodium hydroxide fully reacting, and target can be made in the control of complex reaction object proportion and reaction temperature, drying parameter
Required rhabdolith ZnO.
The present invention loads application of the rodlike ZnO nano material of Au nanoparticle in acetone gas sensor, will load
The rodlike ZnO nano material of Au nanoparticle is coated on the sensing element of sensor.
Further, the sensitive layer of rodlike ZnO nano material formation of Au nanoparticle is loaded with a thickness of 20~40 μm.
Further, above-mentioned acetone gas sensor includes the rodlike ZnO nano of anti-explosion cover, coating load Au nanoparticle
The sensing element of material and six foot tube seats.
Further, above-mentioned acetone gas sensor, preparation method comprising steps of
(1) the rodlike ZnO nano material for loading Au nanoparticle is made after slurry and is coated uniformly on annular Au electricity
The Al of pole2O3Ceramic tube outer surface, forms the sensitive layer of 20~40 μ m-thicks, and annular Au electrode will be completely covered in sensitive layer；
(2) element that step (1) obtains is dried 1~3 hour at 60~80 DEG C；
(3) the Ni-Cr alloy heater strip that resistance value is 35~40 Ω is passed through into Al after2O3Ceramic tube is obtained as heater strip
Sensing element；
(4) above-mentioned sensing element is welded on six foot tube seats and be packaged.
Further, the production method of slurry is to load the rodlike of Au nanoparticle after drying in above-mentioned steps (1)
ZnO nano material is put into mortar, is ground 20~30 minutes；Then water is instilled into mortar be further continued for grinding 20~30 minutes,
Obtain the slurry of sticky shape.
Further, the rodlike ZnO nano material of load Au nanoparticle and the mass ratio of water are when above-mentioned slurry makes
5:1~3.
The advantages of the present invention: the rodlike ZnO nano material of load Au nanoparticle of the invention has height
Specific surface area, while the sensibility of acetone gas is improved by the modification ZnO of Au, therefore using load Au nanoparticle
Rodlike ZnO nano material not only applies its high specific surface area as sensitive material, can also effectively utilize Au to ZnO
The catalytic action of surface and acetone gas improves air-sensitive response；Furthermore acetone gas sensor of the invention is to existing structure
It improves, the rodlike ZnO nano material of above-mentioned load Au nanoparticle is coated on sensing element, there is preparation method letter
Single, low in cost, outstanding quick response recovery characteristics, the characteristics of can be mass-produced have good inspection to acetone gas
Survey performance.Generally the simple process that uses of the present invention, device volume obtained are small, are suitable for producing in enormous quantities, thus have weight
The application value wanted.
Detailed description of the invention
Fig. 1: SEM (a) and TEM (b) pattern of the rodlike ZnO nano material of Au Nanoparticle Modified of the present invention；
Fig. 2: the device architecture schematic diagram of acetone sensor prepared by the present invention；
Fig. 3: the XRD diagram of the rodlike ZnO nano material of Au Nanoparticle Modified prepared by the present invention；
Fig. 4: acetone sensor of the invention is in the case where operating temperature is 172 DEG C, sensitivity-concentration profiles of device；
Fig. 5: acetone sensor of the invention in the case where operating temperature is 172 DEG C, acetone gas concentration is 100ppm, device
Respond recovery curve；
Fig. 6: acetone sensor of the invention in the case where operating temperature is 172 DEG C, acetone gas concentration is 100ppm, device
Select characteristic.
Specific embodiment
The invention will be further described With reference to embodiment.
Embodiment 1
It is fabricated to heater-type acetone sensor as sensitive material using the rodlike ZnO nano material of Au Nanoparticle Modified,
As shown in Fig. 2, sensor is the sensing element of the rodlike ZnO nano material by explosive-proof protector cover 1, coating load Au nanoparticle
2 and six foot tube seat 3 form.
Specific production step is as follows:
(1) 2g NaOH is added in the deionized water of 37.5ml, makes it completely dissolved within magnetic agitation 5 minutes, is denoted as A
Solution；
(2) by 0.7189g ZnSO4·7H2O is dissolved in the deionized water of 12.5ml, makes within magnetic agitation 5 minutes it completely
Dissolution, is denoted as B solution；
(3) B solution is slowly dropped in the solution A for being placed in 60 DEG C of water-baths, magnetic agitation is to being added dropwise to complete, Zhi Houyong
50ml deionized water dilute solution is simultaneously transferred in baking oven in 60 DEG C of dry 6 hours；To mixed liquor deionized water by from
The heart is repeatedly washed, and sediment is 24 hours dry at 60 DEG C, is ground after taking-up, is obtained rodlike ZnO white powder；
(4) the rodlike ZnO powder of 0.05g is added in 40ml deionized water, is made it completely dissolved under magnetic agitation；
(5) HAuCl of 0.05076ml is taken4Solution (concentration 50mmol/L) is added in solution made from step (4), room
The lower magnetic agitation of temperature makes it completely dissolved；
(6) by 2.0ml NH3·H2O is added in solution made from step (5), after stirring 2 hours, is produced by being collected by centrifugation
Object is washed repeatedly with deionized water and absolute alcohol, and 4 hours dry in 60 DEG C of baking oven, finally by gained powder Muffle
Furnace is annealed 1 hour at 350 DEG C, is taken out after powder is ground 20~30 minutes in big mortar and is obtained the stick of Au Nanoparticle Modified
Shape ZnO nano material；
(7) powder of the rodlike ZnO nano material of the Au Nanoparticle Modified after drying is put into mortar, grinding 30
Minute；Then deionized water (mass ratio of nano material and water is 5:2) is instilled into mortar, is further continued for grinding 30 minutes, is obtained
To the slurry of sticky shape；Slurry is uniformly coated on the Al with annular Au electrode with writing brush type brush2O3Ceramic tube outer surface, shape
At the sensitive layer of 30 μ m-thicks, annular Au electrode will be completely covered in sensitive layer；
(8) Al of the rodlike ZnO nano material of Au Nanoparticle Modified will be coated2O3Ceramic tube is dried 1 hour at 70 DEG C；
Then the Ni-Cr alloy heater strip that resistance value is 38 Ω is passed through into Al2O3Ceramic tube is as heater strip, finally by above-mentioned sensitive member
Part is welded on six foot tube seats and is packaged, and finally obtains a kind of powder of the rodlike ZnO nano material of Au Nanoparticle Modified
Acetone gas sensor.
Embodiment 2
It is fabricated to heater-type acetone sensor as sensitive material using the rodlike ZnO nano material of Au Nanoparticle Modified,
As shown in Fig. 2, sensor is the sensing element of the rodlike ZnO nano material by explosive-proof protector cover 1, coating load Au nanoparticle
2 and six foot tube seat 3 form.
Specific production step is as follows:
(1) 1.5g NaOH is added in the deionized water of 33.0ml, makes it completely dissolved within magnetic agitation 5 minutes, is denoted as
Solution A；
(2) by 0.5113g ZnSO4·7H2O is dissolved in the deionized water of 10.5ml, makes within magnetic agitation 5 minutes it completely
Dissolution, is denoted as B solution；
(3) B solution is slowly dropped in the solution A for being placed in 60 DEG C of water-baths, magnetic agitation is to being added dropwise to complete, Zhi Houyong
50ml deionized water dilute solution is simultaneously transferred in baking oven in 80 DEG C of dry 4 hours；To mixed liquor deionized water by from
The heart is repeatedly washed, and sediment is 12 hours dry at 80 DEG C, is ground after taking-up, is obtained rodlike ZnO white powder；
(4) the rodlike ZnO powder of 0.02g is added in 25ml deionized water, is made it completely dissolved under magnetic agitation；
(5) HAuCl of 0.06123ml is taken4Solution (concentration 45mmol/L) is added in solution made from step (4), room
The lower magnetic agitation of temperature makes it completely dissolved；
(6) by 1.5ml NH3·H2O is added in solution made from step (5), after stirring 2 hours, is produced by being collected by centrifugation
Object is washed repeatedly with deionized water and absolute alcohol, and 4 hours dry in 60 DEG C of baking oven, finally by gained powder Muffle
Furnace is annealed 1 hour at 350 DEG C, is taken out after powder is ground 20~30 minutes in big mortar and is obtained the stick of Au Nanoparticle Modified
Shape ZnO nano material；
(7) powder of the rodlike ZnO nano material of the Au Nanoparticle Modified after drying is put into mortar, grinding 30
Minute；Then deionized water (mass ratio of nano material and water is 5:1) is instilled into mortar, is further continued for grinding 30 minutes, is obtained
To the slurry of sticky shape；Slurry is uniformly coated on the Al with annular Au electrode with writing brush type brush2O3Ceramic tube outer surface, shape
At the sensitive layer of 40 μ m-thicks, annular Au electrode will be completely covered in sensitive layer；
(8) Al of the rodlike ZnO nano material of Au Nanoparticle Modified will be coated2O3Ceramic tube is dried 1 hour at 70 DEG C；
Then the Ni-Cr alloy heater strip that resistance value is 38 Ω is passed through into Al2O3Ceramic tube is as heater strip, finally by above-mentioned sensitive member
Part is welded on six foot tube seats and is packaged, and finally obtains a kind of powder of the rodlike ZnO nano material of Au Nanoparticle Modified
Acetone gas sensor.
Embodiment 3
It is fabricated to heater-type acetone sensor as sensitive material using the rodlike ZnO nano material of Au Nanoparticle Modified,
As shown in Fig. 2, sensor is the sensing element of the rodlike ZnO nano material by explosive-proof protector cover 1, coating load Au nanoparticle
2 and six foot tube seat 3 form.
Specific production step is as follows:
(1) 3g NaOH is added in the deionized water of 42.0ml, makes it completely dissolved within magnetic agitation 5 minutes, is denoted as A
Solution；
(2) by 0.9357g ZnSO4·7H2O is dissolved in the deionized water of 14.0ml, makes within magnetic agitation 5 minutes it completely
Dissolution, is denoted as B solution；
(3) B solution is slowly dropped in the solution A for being placed in 60 DEG C of water-baths, magnetic agitation is to being added dropwise to complete, Zhi Houyong
50ml deionized water dilute solution is simultaneously transferred in baking oven in 80 DEG C of dry 4 hours；To mixed liquor deionized water by from
The heart is repeatedly washed, and sediment is 12 hours dry at 80 DEG C, is ground after taking-up, is obtained rodlike ZnO white powder；
(4) the rodlike ZnO powder of 0.1g is added in 50ml deionized water, is made it completely dissolved under magnetic agitation；
(5) HAuCl of 0.07800ml is taken4Solution (concentration 55mmol/L) is added in solution made from step (4), room
The lower magnetic agitation of temperature makes it completely dissolved；
(6) by 3.0ml NH3·H2O is added in solution made from step (5), after stirring 2 hours, is produced by being collected by centrifugation
Object is washed repeatedly with deionized water and absolute alcohol, and 4 hours dry in 60 DEG C of baking oven, finally by gained powder Muffle
Furnace is annealed 1 hour at 350 DEG C, is taken out after powder is ground 20~30 minutes in big mortar and is obtained the stick of Au Nanoparticle Modified
Shape ZnO nano material；
(7) powder of the rodlike ZnO nano material of the Au Nanoparticle Modified after drying is put into mortar, grinding 30
Minute；Then deionized water (mass ratio of nano material and water is 5:3) is instilled into mortar, is further continued for grinding 30 minutes, is obtained
To the slurry of sticky shape；Slurry is uniformly coated on the Al with annular Au electrode with writing brush type brush2O3Ceramic tube outer surface, shape
At the sensitive layer of 40 μ m-thicks, annular Au electrode will be completely covered in sensitive layer；
(8) Al of the rodlike ZnO nano material of Au Nanoparticle Modified will be coated2O3Ceramic tube is dried 1 hour at 70 DEG C；
Then the Ni-Cr alloy heater strip that resistance value is 38 Ω is passed through into Al2O3Ceramic tube is as heater strip, finally by above-mentioned sensitive member
Part is welded on six foot tube seats and is packaged, and finally obtains a kind of powder of the rodlike ZnO nano material of Au Nanoparticle Modified
Acetone gas sensor.
ZnO nano crystal made from the various embodiments described above is observed, each embodiment result is similar, therefore only enumerates reality
Example 1 is applied to be illustrated.As shown in Figure 1, finding out that the ZnO nano crystal of Au Nanoparticle Modified is rhabdolith in (a) figure, (b)
Figure finds out that the particle size of the rodlike ZnO nano material of Au Nanoparticle Modified is 50nm；As shown in figure 3, sample XRD spectra goes out
Existing ZnO characteristic peak illustrates that sample includes ZnO crystal.
Acetone sensor performance made from the various embodiments described above is detected, each embodiment result is similar, therefore only arranges
It is illustrated for embodiment 1.As shown in figure 4, the sensitivity of device is with acetone concentration when device is in the case where operating temperature is 172 DEG C
Increase and increase, curve is that good linear relationship is presented in 10-200ppm in acetone concentration range.As shown in figure 5, when device exists
Operating temperature is 172 DEG C, acetone concentration is under 100ppm, and the response time of device is 1 second, and the recovery time of device is 24 seconds.
Excellent response recovery characteristics are shown, have good detection to acetone gas.As shown in fig. 6, when device is in operating temperature
It is under 100ppm for 172 DEG C, gas concentration, device is all larger than other detection gas to the sensitivity of acetone, and device shows good
Good selectivity.
The present embodiments relate to the material arrived, reagent and experimental facilities, are coincidence senser material unless otherwise instructed
The commercial product in material field.
The above is merely a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise of not departing from core of the invention technology, improvements and modifications can also be made, these improvements and modifications are also answered
Belong to scope of patent protection of the invention.With any change in the comparable meaning and scope of claims of the present invention, all
It is considered as being included within the scope of the claims.
Claims (11)
1. loading the rodlike ZnO nano material of Au nanoparticle, which is characterized in that its crystal is in rhabdolith, crystal particles
Average grain diameter is 50nm, and Au nanoparticle uniform load is in ZnO nanoparticle surface.
2. the method for the rodlike ZnO nano material of preparation load Au nanoparticle, which comprises the steps of:
Step 1: preparing rodlike ZnO using hydro-thermal method, thermal evaporation zinc powder method or microwave heating method, the ZnO of rhabdolith is obtained
White powder；
Step 2: the preparation of the rodlike ZnO nano material of Au Nanoparticle Modified, as follows:
S21 takes rodlike 0.02~0.1g of ZnO powder made from step 1 to be added in 25~50ml water, makes it completely dissolved；
0.04~0.08ml, concentration are the HAuCl of 45~60mmol/L by S224Solution is added in solution made from S21, makes it
Uniformly mixing；
S23 is by 1.0~3.0ml NH3·H2O is added in mixed solution made from S22, is reacted 1.5~3 hours；
S24 collects reaction product made from S23, is washed with deionized water and absolute alcohol, and 3~5 hours dry at 55~70 DEG C,
Gained powder Muffle furnace is annealed 1~2 hour at 340~360 DEG C finally, is obtained after taking out powder mull 20~30 minutes
The rodlike ZnO nano material of Au Nanoparticle Modified.
3. the method for the rodlike ZnO nano material of preparation load Au nanoparticle as claimed in claim 2, which is characterized in that institute
State the method that step 1 prepares rodlike ZnO are as follows:
1~4g NaOH is added in 30~45ml water by S11, is made it completely dissolved, and solution A is denoted as；
S12 is by 0.5~1.0g ZnSO4It is dissolved in 10~15ml water, makes it completely dissolved, be denoted as B solution；
S13A solution is placed under 55~70 DEG C of water-baths, and B solution is added dropwise in solution A, with stirring while dropwise addition；It uses later
40~60ml water dilute solution, then in 60~80 DEG C of dry 4~6 hours；Then to mixed liquor centrifuge washing, sediment is existed
It is 12~24 hours dry at 60~80 DEG C, it is ground after taking-up, obtains rodlike ZnO white powder.
4. the method for the rodlike ZnO nano material of preparation load Au nanoparticle as claimed in claim 2, which is characterized in that institute
Stating aqueous solvent used in rapid one and step 2 is deionized water or ultrapure water.
5. the method for the rodlike ZnO nano material of preparation load Au nanoparticle as claimed in claim 3, which is characterized in that institute
Stating B solution in step S13 and being added dropwise to the speed of solution A is 1 drop/sec.
6. loading application of the rodlike ZnO nano material of Au nanoparticle in acetone gas sensor, which is characterized in that will bear
The rodlike ZnO nano material for carrying Au nanoparticle is coated on the sensing element of sensor.
7. rodlike ZnO nano material the answering in acetone gas sensor of load Au nanoparticle as claimed in claim 6
With, which is characterized in that the sensitive layer thickness that the rodlike ZnO nano material of the load Au nanoparticle is formed on sensing element
It is 20~40 μm.
8. rodlike ZnO nano material the answering in acetone gas sensor of load Au nanoparticle as claimed in claim 6
With, which is characterized in that the acetone gas sensor includes the rodlike ZnO nano material of anti-explosion cover, coating load Au nanoparticle
The sensing element of material and six foot tube seats.
9. rodlike ZnO nano material the answering in acetone gas sensor of load Au nanoparticle as claimed in claim 6
With, which is characterized in that the acetone gas sensor preparation method comprising steps of
(1) the rodlike ZnO nano material for loading Au nanoparticle is made and is coated uniformly on after slurry with annular Au electrode
Al2O3Ceramic tube outer surface, forms the sensitive layer of 20~40 μ m-thicks, and annular Au electrode will be completely covered in sensitive layer；
(2) element that step (1) obtains is dried 1~3 hour at 60~80 DEG C；
(3) the Ni-Cr alloy heater strip that resistance value is 35~40 Ω is passed through into Al after2O3Ceramic tube obtains sensitivity as heater strip
Element；
(4) sensing element is welded on six foot tube seats and be packaged.
10. rodlike ZnO nano material the answering in acetone gas sensor of load Au nanoparticle as claimed in claim 9
With, which is characterized in that the production method of slurry is the rodlike ZnO of the load Au nanoparticle after drying in the step (1)
Nano material is put into mortar, is ground 20~30 minutes；Then water is instilled into mortar and be further continued for grinding 20~30 minutes, obtain
The slurry of sticky shape.
11. the rodlike ZnO nano material of load Au nanoparticle is in acetone gas sensor as claimed in claim 10
Using, which is characterized in that the flower-shaped ZnO nano material of load Au nanoparticle and the mass ratio of water are 5 when the slurry makes:
1~3.
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| CN110711863A (en) * | 2019-11-06 | 2020-01-21 | 郑州大学 | AuPd alloy nanoparticle loaded 3DOM WO3Preparation method of (1) |
| CN112326741A (en) * | 2020-09-17 | 2021-02-05 | 上海大学 | MEMS (micro-electromechanical system) diabetes exhaled breath detection sensor and preparation method and application thereof |
| CN112710704A (en) * | 2020-12-04 | 2021-04-27 | 安徽大学 | Au nanoparticle loaded porous ZnO nanobelt and preparation method and application thereof |
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