CN104897735A - Double layer structural photocatalytic formaldehyde sensor and preparation method thereof - Google Patents
Double layer structural photocatalytic formaldehyde sensor and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a double layer structural photocatalytic formaldehyde sensor and a preparation method thereof. The formaldehyde sensor includes a light source, an electrode, a formaldehyde sensitive material layer and a formaldehyde adsorption material layer, the electrode is covered with the formaldehyde sensitive material layer, the formaldehyde sensitive material layer is covered with the formaldehyde adsorption material layer. Preferably, the formaldehyde sensitive material layer is cadmium doped zinc oxide nanoparticles, and the formaldehyde adsorption material layer is porous silica nanoparticles. The light source is an ultraviolet light source, and irradiates to a double layer structure area. During detecting of formaldehyde pollutants in air, the formaldehyde adsorption material can increase concentration of the formaldehyde on the surface of the formaldehyde sensitive material layer so as to increase the sensor sensitivity, and the low concentration formaldehyde sensitivity can be improved. The double layer structural photocatalytic formaldehyde sensor greatly improves the low concentration formaldehyde sensitivity of the cadmium doped zinc oxide formaldehyde sensor, the progress in the practical application of the sensor can be and promoted, the double layer structural photocatalytic formaldehyde sensor has a good application prospect.
Description
Technical field
The invention belongs to formaldehyde gas monitoring, formaldehyde sensor technical field, be specifically related to a kind of double-deck photocatalysis formula formaldehyde sensor and preparation method thereof.
Background technology
The formaldehyde gas that Long Term Contact exceedes safe concentration restriction is very harmful to health, and this may cause the burning sensation of eyes and throat, and expiratory dyspnea even can cause fatal disease, such as rhinocarcinoma, myelomatosis etc.At present still very serious at Chinese formaldehyde pollution, nearly 70% newly-decorated house is all subject to the puzzlement of formaldehyde pollution, is exactly therefore formaldehyde at the most worrying indoor polluted gas of China.
For air quality product, the technology of sensor is very important, if this is because the true effect of consumer's uncertain air quality product, so they will throw doubt upon to Related product.If current business-like sensor main is based on electrochemical type sensor, this kind of sensor becomes very expensive owing to using platinum electrode, and the degree of accuracy of this kind of sensor, stability and selectivity are all not fully up to expectations in addition.
Compare with electrochemical sensor, the advantage that semiconductor transducer has it special, comprise that cost is low, the life-span is long, and there is huge room for promotion.Current commercial sensor all needs to work more than 200 DEG C, and organic contaminant nearly all in this temperature can react and detect, so the non-constant of the selectivity of this kind of sensor.In order to improve the selectivity to gas, part researcher has also made the photocatalytic semiconductor formaldehyde sensor of room temperature operation, but the Monitoring lower-cut (being greater than 1ppm) of these sensors is still very high for application.That table 1 lists some existing sensing materials and its Problems existing.
The existing sensing material of table 1.
Patented claim CN2007153341 (formaldehyde air sensing material and formaldehyde air sensing equipment preparation method) relates to formaldehyde gas sensing material and preparation method thereof, also comprises the method for making of formaldehyde gas sensor part.This sensing material is by SnO
2-TiO
2bielement nano powder constituent, the mol ratio of Ti/Sn is 0.2-0.5, and mix the cadmium of 2%-5%, by material and absolute ethyl alcohol and polyglycol co-ground to pasty state, then it is coated onto on electrode tube uniformly, by electrode tube 400 DEG C annealing 2-4 hour after by welding, aging, sealing can obtain formaldehyde gas sensor.This sensor operations temperature is low, PARA FORMALDEHYDE PRILLS(91,95) highly sensitive and have very strong antijamming capability for the indoor polluted gas such as benzene,toluene,xylene, ammonia, and has very short response time and the feature of turnaround time.This sensor is mainly used in the formaldehyde gas that detecting chamber interior decoration produces.But the working temperature of this sensor is 260-300 DEG C, and indoor organic pollutant nearly all at such a temperature can be oxidized at surface of sensing materials, so the selectivity of material is not fully up to expectations, particularly can not well distinguish ethanol and formaldehyde.In addition the detection limit of this technology is 20ppm, and this exceeds two orders of magnitude than safe concentration (0.06ppm).
Patented claim CN201410461045.9 (a kind of photocatalysis formaldehyde sensing material and synthetic method and formaldehyde sensor) thereof relates to a kind of photocatalysis formaldehyde sensing material and synthetic method thereof and formaldehyde sensor.This photocatalysis formaldehyde sensing material is primarily of Zinc oxide nanoparticle and cadmium adjuvant composition.Synthesize in the process of this material, first pre-synthesis Zinc oxide nanoparticle is dispersed in cadmium salt soln, the solvent evaporated while of stirring also, form slurry by grinding and be dispersed in specific solvent after the sediment high-temperature calcination obtained, finally slurry to be coated with on the electrode being printed on specific pattern thus to obtain formaldehyde sensor.This solution provides the photocatalysis formaldehyde sensing material of a kind of low cost, high sensitivity, high selectivity, by optimizing the incorporation of cadmium in zinc paste, greatly reducing cost, improve selectivity, and significantly improving detection limit.But, although the Monitoring lower-cut of formaldehyde has been dropped to 0.5ppm by this technology, still exceed nearly order of magnitude than safe concentration (0.06ppm), be unsuitable for practical application in living environment.
Summary of the invention
The present invention is directed to the problems referred to above, provide one to have double-deck photocatalysis formula formaldehyde sensor and preparation method thereof, the sensitivity of formaldehyde sensor can be improved.
The technical solution used in the present invention is as follows:
A kind of double-deck photocatalysis formula formaldehyde sensor, it is characterized in that, comprise light source, electrode, formaldehyde sensitive material and methyl aldehyde adsorption material layer, described formaldehyde sensitive material covers on the electrodes, and described methyl aldehyde adsorption material layer covers on described formaldehyde sensitive material.
Further, be advisable can irradiate described formaldehyde sensitive material in the position of described light source.Such as light source is arranged on methyl aldehyde adsorption material layer side, methyl aldehyde adsorption material layer has light transmission, and the light that light source sends arrives formaldehyde sensitive material by methyl aldehyde adsorption material layer.Or light source is arranged on formaldehyde sensitive material side, formaldehyde sensitive material described in direct irradiation.Now for avoiding electrode part to be lived by light trap, can adopt can through the transparency electrode of ultraviolet light.
Further, described formaldehyde sensitive material is cadmium (Cd) doped zinc oxide nano particle, and described methyl aldehyde adsorption material layer is porous oxidation nano silicon particles.
Further, the thickness of described formaldehyde sensitive material is 5 microns ~ 100 microns, and the thickness of described methyl aldehyde adsorption material layer is 1 micron ~ 50 microns.
Further, described light source is ultraviolet source, the ultraviolet lamp tube of such as 365nm wavelength or the ultraviolet light-emitting diode of 385nm wavelength; Described electrode is interdigital electrode, array electrode or band electrode.
Prepare a method for above-mentioned double-deck photocatalysis formula formaldehyde sensor, its step comprises:
1) cadmium doped zinc oxide nano particle is synthesized: be immersed in cadmium salt soln by previously prepared good Zinc oxide nanoparticle, then heating up makes solvent volatilize, and heating makes sample drying, calcines subsequently to sample, after calcining, sample ground to form fine powder and form slurry with ethanol dispersion;
2) synthesizing porous monox nanometer particle: water, ethanol, CATC (hexadecyltrimethylammonium chloride), DEA (diethanolamine) mixing are also heated in a water bath, then the mode that TEOS (ethyl orthosilicate) is stirred by dropping limit, limit is joined in potpourri, after continuing to stir certain hour, product is distributed in ethanol and forms sol dispersion;
3) by step 1) the cadmium doping zinc-oxide slurry prepared is coated on electrode, and oven dry makes solvent volatilize, then by step 2) sol dispersion of porous silica prepared is coated on cadmium doping zinc-oxide layer, and oven dry makes solvent volatilize, then increase light source and make formaldehyde sensor.When detecting formaldehyde, with ultraviolet source irradiation double-decker region, the resistance variations of sensor under ultraviolet source irradiation may be used for the concentration calculating formaldehyde.
Further, step 1) Zinc oxide nanoparticle is immersed in after in cadmium salt soln, being warming up to 70 ~ 90 DEG C makes solvent volatilize, and to heat at such a temperature 10 ~ 14 hours and 110 ~ 130 DEG C of heating make sample drying in 1 ~ 3 hour, subsequently sample is calcined 400 ~ 500 DEG C (being preferably 450 DEG C).
Further, step 2) after described mixing, heat 20 ~ 40 minutes in 50 ~ 70 DEG C of water-baths; Ethyl orthosilicate is joined after in potpourri and continue stirring 1 ~ 3 hour.
The present invention, by easy method, significantly improves the sensitivity of cadmium doping zinc-oxide formaldehyde sensor for low concentration formaldehyde, has promoted the practical progress of this sensor, had a good application prospect.
Accompanying drawing explanation
Fig. 1 is formaldehyde sensor structural representation of the present invention.
Fig. 2 is the present invention's preferred sensor double-decker partial schematic diagram.
Fig. 3 is double-decker sensor production step schematic diagram.
Fig. 4 is the Static Adsorptive capacity figure of porous oxidation nano silicon particles (sample size 5mg, test container 1L).。
Fig. 5 is the comparison diagram for formaldehyde sensitivity after coating porous oxidation nano silicon particles, ZIF-8 and active carbon adsorption material layer.
Fig. 6 is cadmium doping zinc-oxide sensor and the formaldehyde sensitivity curve comparison diagram adding porous silica coating sensor.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, and below by specific embodiments and the drawings, the present invention will be further described.
Due to the indoor decoration pollution problem that China is serious, be badly in need of the formaldehyde sensor product of a kind of low cost, high selectivity.The invention provides one and there is double-deck photocatalysis formula formaldehyde sensor.As shown in Figure 1, this sensor comprises the material coating structure of light source, electrode and bilayer.The formaldehyde sensitive material that this double-decker comprises one deck photocatalysis principle directly overlays on electrode, and a methyl aldehyde adsorption material layer covers on formaldehyde sensitive material.Light source is ultraviolet source, irradiates to this double-decker region.When detecting the formaldehyde pollutants in air, this methyl aldehyde adsorption material layer can increase the concentration of formaldehyde on formaldehyde sensitive material surface, thus realizes the effect increasing sensor sensitivity, namely can improve the sensitivity for low concentration formaldehyde.
As shown in Figure 2, in this sensor, formaldehyde sensitive material preferably adopts cadmium (Cd) the doped zinc oxide nano particle of PARA FORMALDEHYDE PRILLS(91,95) sensitivity, and methyl aldehyde adsorption material layer preferably adopts porous oxidation nano silicon particles, and electrode can adopt interdigital electrode etc.This methyl aldehyde adsorption material layer has following characteristics: 1. have adsorptive power for formaldehyde; 2. have light transmission (can pass through ultraviolet light), the light that light source can be made to send arrives sensitive material by sorbing material; 3. electric property, photoelectric properties etc. are comprised for the characteristic of semiconductor of sensitive material not have a negative impact.The present invention tests multiple sorbing material formaldehyde to adsorptive power, comprising: porous silica, activated charcoal, carbon black, ZIF-8 etc.Wherein only have porous oxidation nano silicon particles to have the effect in front for the formaldehyde examination of sensor, namely its reason is that porous oxidation nano silicon particles has These characteristics.It should be noted that, light source also can be arranged on formaldehyde sensitive material side by the present invention, with formaldehyde sensitive material described in direct irradiation.Now for avoiding electrode part to be lived by light trap, can adopt can through the transparency electrode of ultraviolet light.
Double-decker sensor production step of the present invention as shown in Figure 3, illustrates preparation process below by embodiment.
Embodiment 1:
Step one: the synthesis of Zinc oxide nanoparticle
By 10.77g ZnSO
47H
2o (375mmol) is dissolved in 25mL deionized water.Dropwise is joined 50mL100g/L (1.36mmol/L) NH
4hCO
3in solution, under 40 DEG C of water-baths, stir 1h.Remove supernatant, each with the washing precipitation of 15mL deionized water, wash three times altogether, then will be deposited in 80 DEG C of dry 12h, at 120 DEG C of dry 2h.After having dried, sample is put into muffle furnace 500 DEG C calcining 2h.
Step 2: the interpolation of cadmium element
Take the previously prepared Zinc oxide nanoparticle of 0.4g and be dispersed in (3CdSO in 60mL cadmium salt soln
48H
2o0.019g), solution stirs and solvent evaporated at 80 DEG C, then will be deposited in 80 DEG C of dry 12h, at 120 DEG C of dry 2h.Calcine at being deposited in 450 DEG C after this.
Step 3: the synthesis of porous oxidation nano silicon particles
CATC (hexadecyltrimethylammonium chloride) solution of 6.4mL water, 0.9g ethanol, 1.04g25% percentage by weight, mixed being incorporated in 60 DEG C of water-baths of 0.02gDEA (diethanolamine) are heated 30 minutes.Then the mode that 0.73mLTEOS (ethyl orthosilicate) is stirred by dropping limit, limit is joined in potpourri, then continue stirring 2 hours.
Step 4: sensitive material applies
Solid product step 2 obtained is dispersed in absolute ethyl alcohol after being ground to micro mist and makes slurry, is then coated with on electrode by prepared slurry, is dried up (1min) by ethanol with hair dryer.
Step 5: sorbing material layer applies
Sol dispersion is made in product ethanol dispersion step 3 obtained, and be then coated with by obtained dispersion liquid on sensitive material that step 4 obtains, electricity consumption dries up to form double-decker.
Step 6: formaldehyde examination
Ultraviolet source produces photocatalytic effect for sensitive material, for the detection of formaldehyde.The ultraviolet lamp tube of 365nm wavelength or the ultraviolet light-emitting diode of 385nm wavelength can be used as ultraviolet source.When ultraviolet source is opened, due to the photic conductance effect of zinc oxide material, the resistance of sensor starts to reduce.After certain hour (normally 5 minutes), resistance value reaches stable.Time in clean air, this resistance value is set to R
0.When in the air that sensor is transferred to containing formaldehyde from clean air, the resistance value of sensor there will be reduction.After the regular hour (normally 3 minutes), resistance value reaches stable, and is set to R
s.According to predetermined relation, the concentration of formaldehyde can by R
s/ R
0calculate.After detection completes, because photocatalysis effect has dismantling-cleaning effect for the formaldehyde that sensor material adsorbs, the resistance value of this sensor can automatically return to R
0.
The Static Adsorptive capacity curve of porous oxidation nano silicon particles as shown in Figure 4,5mg porous silica nanoparticle sample in 1L container for formaldehyde be adsorbed on about 200s time reach balance.
After mixing cadmium Zinc oxide nanoparticle surperficial coating respectively porous oxidation nano silicon particles, ZIF-8 and active carbon adsorption material layer for the contrast of formaldehyde sensitivity as shown in Figure 5.Can see, mix cadmium Zinc oxide nanoparticle compared to what do not increase sorbing material coating, the sample of coating porous oxidation nano silicon particles brings up to 45% for the sensitivity of 3ppm formaldehyde from 30%.And the sample of ZIF-8 and activated charcoal coating all makes the sensitivity of sensor significantly reduce.This is because although ZIF-8 and activated charcoal have adsorptive power for formaldehyde, the two can hinder ultraviolet lighting to be mapped to sensitive material, and has negative effect for the photoelectric properties of zinc paste itself.
Fig. 6 is cadmium doping zinc-oxide sensor and the formaldehyde sensitivity curve comparison diagram adding porous silica coating sensor, and its horizontal ordinate is concentration of formaldehyde, and ordinate is that sensor is in the ratio R containing the resistance in formaldehyde air and the resistance in clean air
s/ R
0.R
s/ R
0numerical value less, illustrate that the sensitivity for formaldehyde is higher.Can finding out, under same concentration of formaldehyde, adding the transducer sensitivity of porous oxidation silicon coating apparently higher than not having cated cadmium doping zinc-oxide sensor.
Embodiment 2:
In embodiment 1, the method for step 2 can replace with following scheme:
Step 2: the interpolation of cadmium element
Take the previously prepared Zinc oxide nanoparticle of 0.4g and be dispersed in (3CdSO in 60mL cadmium salt soln
48H
2o0.019g), solution stirs and solvent evaporated at 70 DEG C, then will be deposited in 70 DEG C of dry 10h, at 110 DEG C of dry 1h.Calcine at being deposited in 400 DEG C after this.
Embodiment 3:
In embodiment 1, the method for step 2 can replace with following scheme:
Step 2: the interpolation of cadmium element
Take the previously prepared Zinc oxide nanoparticle of 0.4g and be dispersed in (3CdSO in 60mL cadmium salt soln
48H
2o0.019g), solution stirs and solvent evaporated at 90 DEG C, then will be deposited in 90 DEG C of dry 14h, at 130 DEG C of dry 3h.Calcine at being deposited in 500 DEG C after this.
Embodiment 4:
In embodiment 1, the method for step 3 can replace with following scheme:
Step 3: the synthesis of porous oxidation nano silicon particles
CATC (hexadecyltrimethylammonium chloride) solution of 6.4mL water, 0.9g ethanol, 1.04g25% percentage by weight, mixed being incorporated in 50 DEG C of water-baths of 0.02gDEA (diethanolamine) are heated 20 minutes.Then the mode that 0.73mLTEOS (ethyl orthosilicate) is stirred by dropping limit, limit is joined in potpourri, then continue stirring 1 hour.
Embodiment 5:
In embodiment 1, the method for step 3 can replace with following scheme:
Step 3: the synthesis of porous oxidation nano silicon particles
CATC (hexadecyltrimethylammonium chloride) solution of 6.4mL water, 0.9g ethanol, 1.04g25% percentage by weight, mixed being incorporated in 70 DEG C of water-baths of 0.02gDEA (diethanolamine) are heated 40 minutes.Then the mode that 0.73mLTEOS (ethyl orthosilicate) is stirred by dropping limit, limit is joined in potpourri, then continue stirring 3 hours.
Above embodiment is only in order to illustrate technical scheme of the present invention but not to be limited; those of ordinary skill in the art can modify to technical scheme of the present invention or equivalent replacement; and not departing from the spirit and scope of the present invention, protection scope of the present invention should be as the criterion with described in claims.
Claims (10)
1. a double-deck photocatalysis formula formaldehyde sensor, it is characterized in that, comprise light source, electrode, formaldehyde sensitive material and methyl aldehyde adsorption material layer, described formaldehyde sensitive material covers on the electrodes, and described methyl aldehyde adsorption material layer covers on described formaldehyde sensitive material.
2. double-deck photocatalysis formula formaldehyde sensor as claimed in claim 1, it is characterized in that: described light source is arranged on described methyl aldehyde adsorption material layer side, described methyl aldehyde adsorption material layer has light transmission, and the light that described light source sends arrives described formaldehyde sensitive material by described methyl aldehyde adsorption material layer.
3. double-deck photocatalysis formula formaldehyde sensor as claimed in claim 1, is characterized in that: described light source is arranged on described formaldehyde sensitive material side, formaldehyde sensitive material described in direct irradiation.
4. double-deck photocatalysis formula formaldehyde sensor as claimed any one in claims 1 to 3, is characterized in that: described formaldehyde sensitive material is cadmium doped zinc oxide nano particle, and described methyl aldehyde adsorption material layer is porous oxidation nano silicon particles.
5. double-deck photocatalysis formula formaldehyde sensor as claimed in claim 4, it is characterized in that: the thickness of described formaldehyde sensitive material is 5 ~ 100 microns, the thickness of described methyl aldehyde adsorption material layer is 1 ~ 50 micron.
6. double-deck photocatalysis formula formaldehyde sensor as claimed in claim 1, it is characterized in that: described light source is ultraviolet source, described electrode is interdigital electrode, array electrode or band electrode.
7. double-deck photocatalysis formula formaldehyde sensor as claimed in claim 6, is characterized in that: described ultraviolet source is the ultraviolet lamp tube of 365nm wavelength or the ultraviolet light-emitting diode of 385nm wavelength.
8. prepare a method for double-deck photocatalysis formula formaldehyde sensor, its step comprises:
1) be immersed in cadmium salt soln by previously prepared good Zinc oxide nanoparticle, then heating up makes solvent volatilize, and heating makes sample drying, calcines subsequently to sample, after calcining, sample is ground to form fine powder and forms slurry with ethanol dispersion;
2) water, ethanol, hexadecyltrimethylammonium chloride, diethanolamine mixing are also heated in a water bath, then the mode that ethyl orthosilicate is stirred by dropping limit, limit is joined in potpourri, after continuing to stir certain hour, product is distributed in ethanol and forms sol dispersion;
3) by step 1) the cadmium doping zinc-oxide slurry prepared is coated on electrode, and oven dry makes solvent volatilize, then by step 2) sol dispersion of porous silica prepared is coated on cadmium doping zinc-oxide, and oven dry makes solvent volatilize, then increase light source and make formaldehyde sensor.
9. method as claimed in claim 8, it is characterized in that: step 1) Zinc oxide nanoparticle is immersed in after in cadmium salt soln, being warming up to 70 ~ 90 DEG C makes solvent volatilize, and heat 10 ~ 14 hours at such a temperature, then within 1 ~ 3 hour, make sample drying 110 ~ 130 DEG C of heating, subsequently sample is calcined at 400 ~ 500 DEG C.
10. method as claimed in claim 8, is characterized in that: step 2) after described mixing, heat 20 ~ 40 minutes in 50 ~ 70 DEG C of water-baths; Ethyl orthosilicate is joined after in potpourri and continue stirring 1 ~ 3 hour.
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| CN201510208449.1A CN104897735B (en) | 2015-04-28 | 2015-04-28 | A kind of photocatalysis formula formaldehyde sensor of double-decker and preparation method thereof |
| JP2016059182A JP6239668B2 (en) | 2015-04-28 | 2016-03-23 | Double-layer photocatalytic formaldehyde sensor and manufacturing method thereof |
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|---|---|---|---|
| CN201510208449.1A CN104897735B (en) | 2015-04-28 | 2015-04-28 | A kind of photocatalysis formula formaldehyde sensor of double-decker and preparation method thereof |
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| CN104897735B CN104897735B (en) | 2017-12-19 |
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| CN112034016A (en) * | 2019-12-20 | 2020-12-04 | 湘潭大学 | Holmium ferrite formaldehyde gas sensor in red light auxiliary mode and preparation method thereof |
| CN112179956A (en) * | 2020-09-29 | 2021-01-05 | 西安交通大学 | Preparation method of MEMS formaldehyde sensor based on aluminum-doped zinc oxide porous nano film |
| CN112179956B (en) * | 2020-09-29 | 2021-11-19 | 西安交通大学 | Preparation method of MEMS formaldehyde sensor based on aluminum-doped zinc oxide porous nano film |
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| CN117571794A (en) * | 2024-01-15 | 2024-02-20 | 电子科技大学中山学院 | Laser enhancement type zinc oxide formaldehyde detection device |
| CN117571794B (en) * | 2024-01-15 | 2024-03-19 | 电子科技大学中山学院 | Laser enhancement type zinc oxide formaldehyde detection device |
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| JP2016212087A (en) | 2016-12-15 |
| JP6239668B2 (en) | 2017-11-29 |
| CN104897735B (en) | 2017-12-19 |
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