CN109850934A - A kind of preparation method of metal oxide suspension and the method for forming high-specific surface area air-sensitive coating is sprayed under liquid material flame - Google Patents
A kind of preparation method of metal oxide suspension and the method for forming high-specific surface area air-sensitive coating is sprayed under liquid material flame Download PDFInfo
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Abstract
Spray the invention discloses a kind of preparation method that can be applied to a kind of industrial metal oxide suspension and under liquid material flame the method for forming high-specific surface area air-sensitive coating.The present invention using the synthesis of compound soft template method there is the hollow ball thicker than conventional hollow ball wall thickness (to improve the structural strength of hollow ball, its intrinsic pattern can be saved after colliding with matrix) metal oxide suspension, then using the suspension as liquid material, air-sensitive coating is prepared using flame flow velocity degree and the relatively mild liquid material presoma flame spray technique of temperature (Liquid Precursor Flame Spray-LPFS).The air-sensitive coating with hollow ball pattern being prepared generates high sensitivity, faster response/recovery time and good long-time stability to specific gas under conditions of low temperature even room temperature.
Description
Technical field
The invention discloses a kind of preparation method that can be applied to a kind of industrial metal oxide suspension and
The method for forming high-specific surface area air-sensitive coating is sprayed under liquid material flame, belongs to engineering and material science and technology field.
Background technique
A large amount of nitrogen dioxide (NO of industry and vehicular emission2) it is the major reason for causing various diseases.It is common at present
Gas analyzer it is expensive, structure is complicated, maintenance cost is high.Metal-oxide semiconductor (MOS) gas sensor is relative to gas
Analyzer has many advantages, such as small in size, non-maintaining, at low cost, is suitable for distributed large area and layouts online monitoring.
Manufacturing metal oxide semiconductor gas sensing layer includes two exemplary steps: being had firstly, being synthesized by chemical synthesis
There are the sensing material of specific modality, such as hydro-thermal method, solvent-thermal method, sol-gel method and compound soft template method；Then, pass through
Synthetic material is transferred on sensor by ad hoc approach, such as manual coating process, spray coating method, magnetron sputtering method and chemical vapor deposition
Deng.Hydro-thermal method and solvent-thermal method are most widely used two kinds of chemical synthesis in current research, but synthesis cycle is long and closes
At its industrialized application of amount lower limit, and synthesis material cannot be carried out according to designed pattern, and compound soft template method
Raw material can not only be mass produced, and can be synthesized according to designed pattern.Relative to magnetron sputtering and chemical gas
Xiang Fa, spray coating method is at low cost and can generate more Shi zhimings in the coating, and Shi zhiming is the weight that carrier generates
One of reason is wanted, it plays key effect to the raising of sensor air-sensitive performance.Meanwhile it is most common relative to laboratory research
Manual coating process, spray coating method production efficiency is higher, is suitble to industrialized production, and the air-sensitive coating prepared is more uniform, performance is more
It is good.Hollow structure material has high specific surface area, is conducive to the absorption and reaction of object gas；Surface porosity, can
To accelerate the diffusion of object gas on the surface of the material；Relatively thin shell structurre is not susceptible to assemble, and is conducive to improve sensor
Stability.Above-mentioned advantage makes hollow metal oxide semiconductor have the speciality as excellent sensitive material, is suitable as room
Warm gas sensitive.However, hollow structure material is difficult to completely preserve under the spraying flame stream of high temperature and high speed, therefore studies and close
The technology of suitable extensive deposition hollow ball pattern air-sensitive coating is current research hotspot.
CN104569080A discloses the preparation side of the acetone sensor based on hollow flower ball-shaped zinc ferrite nano material
Hollow flower-shaped zinc ferrite nanometer powder is prepared by hydrothermal synthesis method, by powder coating to Al in method2O3After insulator surface
Calcining forms gas sensing layer.The sensor is heated by Ni-Cr coil, Al2O3The annular electrode of surface of insulating layer is passed for exporting
Feel signal, the gas sensing layer with hollow flower ball-shaped has response well to the acetone of low concentration.
CN103924184A discloses a kind of porous micro-nano structure WO3Air-sensitive coating and preparation method thereof, using liquid phase heat
Spraying process, by liquid material conveying device by nanometer WO3Liquid material is sent into thermal spraying flame, WO obtained3Coating is obtained with conventional method
Obtain WO3Coating is compared, and has higher specific surface area, is conducive to play WO3The gas-sensitive property of coating.In addition, preparation WO3It applies
The equipment of layer and simple process, easily-controllable, it is low in cost, it is convenient for industrialized production.
CN104195499A discloses a kind of method that plasma spraying with liquid feedstock prepares micro-nano compound structure coating, the powder
Solid powder is dissolved in solvent and is sprayed, effective solution fine powder mobility it is bad and caused by powder feeding it is difficult, simultaneously
Solvent evaporates in plasma flame flow can absorb partial heat, reduce the growth temperature of powder, therefore the coating prepared can solve
Certainly thermal barrier coating, air-sensitive coating, present in wear-resisting and lubricant coating because crystal grain, which is grown up, causes coating performance to decline the problem of.
Summary of the invention
The problem of being difficult to the intact preservation in the spraying flame stream of high temperature and high speed the invention solves hollow structure material proposes
A kind of simplicity, low cost and the method that can be applied to large-scale industrial production that can prepare hollow pattern air-sensitive coating.
Thus the technical solution adopted by the present invention is that: a kind of metal oxide suspension, in metal oxidation suspension
Solid particle be hollow micron ball, the hollow micron bulb diameter be 1.2-1.4 μm.
Further, the hollow micron ball by metal oxide nanoparticles in soft template ordering growth and constitute
Spherical shell structure micron ball, the metal oxide nanoparticles diameter are 10-20 nm.
Further, the hollow ball metal oxide suspension is prepared using compound soft template method.
A method of it sprays to form air-sensitive coating using the metal oxide suspension, using liquid material flame-spraying side
The metal oxide suspension is sprayed to substrate and forms air-sensitive painting by method using oxygen-acetylene combustion flame as heat source
Layer.
Further, it follows the steps below: by peristaltic pump by metal oxide suspension, passing through axial feeding side
Formula is sent to flame flame flow center；In spraying process, the movement speed of spray gun is 150-250 mm/s, is sprayed 40-60 times, spray
It applies apart from substrate between 180-280 mm, by adjusting O2And the flow of acetylene controls flame stream mode, spraying obtains gas
Quick coating.
Further, metal oxide suspension flow is 25-40 mL/min, and acetylene flow is 0.07 MPa, O2Flow
In 0.4 MPa, 1 MPa of compressed air pressure.
Further, before being sprayed to the substrate, first substrate is preheated, preheating temperature 400-500
℃。
The invention firstly uses improved compound soft template method synthesis to have the hollow ball thicker than conventional hollow ball wall thickness
(improving the structural strength of hollow ball, its intrinsic pattern can be saved after colliding with matrix) metal oxide suspension, then
Using the suspension as liquid material, using flame flow velocity degree and the relatively mild liquid material presoma flame spray technique (Liquid of temperature
Precursor Flame Spray-LPFS) preparation air-sensitive coating.
The air-sensitive coating with hollow ball pattern being prepared, to specific gas under conditions of low temperature even room temperature
Generate high sensitivity, faster response/recovery time and good long-time stability.
Compared with prior art, the invention has the following advantages:
First, the present invention proposes compound soft template method-liquid material presoma flame-spraying (Composite Soft Template-
Liquid Precursor Flame Spray, CST-LPFS) technology, prepare the metal oxide air-sensitive with hollow ball pattern
Coating.Specifically, being exactly to prepare the hollow ball forerunner thicker than conventional hollow ball wall thickness using improved compound soft template method
Body fluid material is that raw material is sprayed, and realizes that coating preparation and powder preparation are combined into one, improves work efficiency.CST-LPFS liquid
Granule-morphology in material has formed, in flame-spraying, due to oxy-acetylene flame stream temperature relative to plasma temperature substantially
Decline, it is easier to realize that particle surface layer is melted, core keeps original state.Traditional plasma spraying with liquid feedstock cannot achieve coating morphology
Effective Regulation, can only prepare the coating of nano particle pattern, thus air-sensitive performance is poor and needs work at relatively high temperatures
Make.CST-LPFS coating can overcome the shortcomings that traditional plasma spraying with liquid feedstock, and the nano-structured coating with hollow pattern has
There are biggish specific surface area, more Shi zhiming, therefore can even obtain at room temperature excellent gas sensing property in lower temperature
Energy.
Second, hollow micro-nano structure air-sensitive coating is prepared using this quick, simple method of liquid material flame-spraying.
The parameter in ingredient and spraying process by changing CST-LPFS liquid material obtains the optimized parameter of prepares coating, is had
The room temperature NO of good air-sensitive performance2Gas sensor.Most importantly the preparation method of the gas sensing layer is at low cost, and flame-spraying is set
It is standby simple, plasma arc light is not generated, and noise is small, can be applied to large-scale industrial production.
Third, compared to patent CN104569080A by the way that by the powder coating of hydrothermal synthesis to sensor surface, this is specially
The liquid material flame spraying process that benefit uses, shaping speed is fast, and method is easy, and production efficiency is higher, is saving the same of microscopic appearance
When can also bring more Shi zhimings into, therefore the hollow micro-nano structure gas sensing layer being prepared may be implemented quickly at room temperature
Response.Compared to the air-sensitive coating that patent CN103924184A uses hot spray process preparation, the method that this patent provides can be prepared
Air-sensitive coating with special hollow pattern is realized at room temperature to the quick response of specific gas.Compared to
CN104195499A is using the micro-nano compound structure coating of the chemical deposition preparation of plasma spraying with liquid feedstock technology preparation, this is specially
The spray parameters that benefit provides more optimize specifically, and flame stream temperature is lower, it is easy to accomplish part is melted, adjustable flame properties
(oxidizing flame-neutral flame-reducing flame), the air-sensitive painting layer-selective synthesized is higher, and preparation cost is lower, therefore is more suitable for reality
Using and large-scale production.
Detailed description of the invention
Fig. 1: the preparation facilities schematic diagram of hollow micro-nano structure gas sensing layer.
1. preheating table in figure, 2. sensor bases, 3. gas sensing layers, 4. melt granules, 5. flame flame streams, 6. axial nozzles,
7. flame gun, 8. 6 shaft mechanical arms, 9. peristaltic pumps, 10.CST-LPFS liquid material.
Fig. 2: the hollow structure In in example 12O3The XRD diagram of air-sensitive coating.
Fig. 3: the hollow structure In of example 12O3Air-sensitive coating surface SEM figure.
Fig. 4: the hollow In in example 12O3Particle TEM figure.
Specific embodiment
The invention will be further described combined with specific embodiments below, it is clear that described embodiment is the present invention one
Section Example, rather than whole embodiments.Based on the embodiment of the present invention, those skilled in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Chemical raw material required for the present invention is commercially available.
The matrix that the present invention uses can be bought for pure zirconia aluminium flake from market.
Embodiment 1:
1. using aluminium oxide as insulating body, alumina wafer is sequentially placed in deionized water and ethyl alcohol, and auxiliary with
Ultrasound is cleaned 10 minutes, is dried for standby.Using the method for vacuum coating, using metal mask pattern, one layer of chromium is first prepared, is used
Bond strength is improved, then in front one layer of gold of vapor deposition of alumina wafer, obtains interdigitated electrodes.In alumina wafer
Reverse side first prepares one layer of chromium using the method for vacuum coating, to improve bond strength, then steams in the front of alumina wafer
One layer of platinum is plated, interdigital heating electrode, i.e. sensor base 2 are obtained.
2. under 60 DEG C of magnetic agitations, weighs DL- aspartic acid and be dissolved in deionized water and stir 10min, PEG- is added
4000 solution continue to stir 30min.In (NO is then added3)3Solution and urea stir at 102 DEG C, continue after solution is muddy
Stirring, prevents solution evaporation during reaction with atmospheric pressure reflux method.It is cooling heavy to above-mentioned suspension in order to increase the wall thickness of hollow ball
Behind shallow lake, supernatant liquor (template) is sucked out, isometric deionized water, In (NO is added3)3After solution and urea, continuation is being heated
Growth, obtains the thicker CST-LPFS liquid material to be sprayed of ball wall.
3., will under the action of peristaltic pump 9 using the preparation facilities of hollow micro-nano structure gas sensor shown in FIG. 1
CST-LPFS liquid material 10 passes through the center that axial nozzle 6 is injected into flame stream 5 with the flow velocity of 25 mL/min.In spraying process, spraying
Distance: 180 mm adjust oxygen flow, obtain reducing flame, spray gun reciprocal time: 40 times, spraying obtains the gas with a thickness of 12 μm
Quick coating 3.Before spraying, 500 DEG C of preheatings are carried out to aluminum oxide substrate.
4. the hollow micro-nano structure air-sensitive coating being prepared is passed through X-ray diffraction XRD, scanning electron microscope sem and transmission
Electronic Speculum tem analysis, the results showed that coating is cubic phase In2O3, and coating shows hollow spheres structure, sees Fig. 2,3,4.It is made
The hollow spheres In obtained2O3Sensor, under conditions of test condition is 50 DEG C, to NO2Gas shows the gas of n-type semiconductor
Quick characteristic is passed through 1 ppm NO2When gas, sensitivity 43.2.
Embodiment 2:
The present embodiment difference from example 1 is that: in step 3 select liquid material flow velocity be 40mL/min, spraying advance
400 DEG C of row preheatings, adjustment oxygen flow obtain neutral flame and are prepared in the case that spray distance is 250 mm with a thickness of 22
μm hollow micro-nano structure In2O3Coating.When test condition is 25 DEG C, NO of the coating to 10 ppm2Sensitivity is 32.5.
Embodiment 3:
The present embodiment difference from example 1 is that: that be added in step 2 is 100 mL, 0.3 mol/L Zn (NO3)3
Solution.The liquid material flow selected in step 3 is 40mL/min, and 500 DEG C of preheatings are carried out before spraying, and adjustment oxygen flow obtains oxygen
Change flame and the hollow micro-nano structure ZnO coating with a thickness of 25 μm is prepared in the case that spray distance is 250 mm.It is testing
When condition is room temperature, NO of the coating to 10 ppm2Sensitivity is 26.8.
Embodiment 4:
The present embodiment difference from example 1 is that: that be added in step 2 is 120 mL, 0.2 mol/L SnO2·
2H2O solution.The liquid material flow selected in step 3 is 40mL/min, and 450 DEG C of preheatings are carried out before spraying, and adjustment oxygen flow obtains
The hollow micro-nano structure SnO with a thickness of 35 μm is prepared in the case that spray distance is 200mm to neutral flame stream2Coating.
When test condition is 75 DEG C, NO of the coating to 10 ppm2Sensitivity is 22.7.
Embodiment 5:
The present embodiment difference from example 1 is that: that be added in step 2 is 80 mL, 0.2 mol/LFe (NO3)3It is molten
Liquid.450 DEG C of preheatings are carried out in step 3 before spraying, adjustment oxygen flow obtains reducing flame stream, and spray distance is 280 mm's
In the case of, the hollow micro-nano structure Fe with a thickness of 15 μm is prepared2O3Coating.When test condition is 50 DEG C, coating is to 10
The NO of ppm2Sensitivity is 32.5.
Claims (9)
1. a kind of metal oxide suspension, which is characterized in that the solid particle in the metal oxidation suspension is hollow micro-
Rice ball, the hollow micron bulb diameter are 1.2-1.4 μm.
2. a kind of metal oxide suspension according to claim 1, which is characterized in that the hollow micron ball is by metal
Oxide nano particles ordering growth and the spherical shell structure micron ball that constitutes, metal oxide nanoparticles in soft template
Diameter is 10-20 nm.
3. a kind of preparation method of metal oxide suspension, which is characterized in that prepared using compound soft template method described hollow
Ball metal oxide suspension.
4. a kind of preparation method of metal oxide suspension according to claim 3, which is characterized in that at 55-65 DEG C
It under magnetic agitation, weighs DL- aspartic acid and is dissolved in deionized water and stir 6-15min, PEG-4000 solution is added and continues to stir
25-40min；
In (NO is then added3)3Solution and urea stir at 100-110 DEG C, continue to stir after solution is muddy, during reaction
Solution evaporation is prevented with atmospheric pressure reflux method；
In order to increase the wall thickness of hollow ball, after the cooling precipitating of above-mentioned suspension, supernatant liquor (template) is sucked out, the bodies such as addition
Long-pending deionized water, In (NO3)3After solution and urea, continue to obtain the thicker CST- to be sprayed of ball wall in heat growth
LPFS liquid material.
5. a kind of spray the method to form air-sensitive coating, feature using metal oxide suspension described in the claim 1
It is, the metal oxide is suspended using oxygen-acetylene combustion flame as heat source using liquid material flame spraying method
Liquid sprays to substrate and forms air-sensitive coating.
6. according to claim 5 spray the method to form air-sensitive coating, spy using the metal oxide suspension
Sign is, follows the steps below: by peristaltic pump by metal oxide suspension, being sent to fire by axial feeding style
Flame flame flow center；In spraying process, the movement speed of spray gun is 150-250 mm/s, is sprayed 40-60 times, spray distance substrate
Between 180-280 mm, by adjusting O2And the flow of acetylene controls flame stream mode, spraying obtains air-sensitive coating.
7. according to claim 5 spray the method to form air-sensitive coating, spy using the metal oxide suspension
Sign is that metal oxide suspension flow is 25-40 mL/min, and acetylene flow is 0.05-0.1 MPa, O2Flow is in 0.2-
0.7 MPa, compressed air pressure 0.8-1.5 MPa.
8. according to claim 5 spray the method to form air-sensitive coating, spy using the metal oxide suspension
Sign is, before spraying to the substrate, first preheats to substrate, and preheating temperature is 400-500 DEG C.
9. according to claim 5 spray the method to form air-sensitive coating, spy using the metal oxide suspension
Sign is that the preparation process of the substrate is as follows: using aluminium oxide as insulating body, alumina wafer being sequentially placed in going
In ionized water and ethyl alcohol, and assist being dried for standby after cleaning with ultrasound；
Using the method for vacuum coating, using metal mask pattern, first prepares one layer of chromium and then exist for improving bond strength
Front one layer of gold of vapor deposition of alumina wafer, obtains interdigitated electrodes；
In the reverse side of alumina wafer, using the method for vacuum coating, first prepares one layer of chromium and then existed with improving bond strength
Front one layer of platinum of vapor deposition of alumina wafer, obtains interdigital heating electrode.
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| CN112194187A (en) * | 2020-09-25 | 2021-01-08 | 南京理工大学 | Method for synthesizing zinc ferrite spherical nano material by premixed flame |
| CN112209423A (en) * | 2020-09-25 | 2021-01-12 | 南京理工大学 | Method for synthesizing ultrathin hollow sphere micron zinc aluminate by flame synthesis method in one step |
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| CN112209423B (en) * | 2020-09-25 | 2022-03-18 | 南京理工大学 | Method for synthesizing ultrathin hollow sphere micron zinc aluminate by flame synthesis method in one step |
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Application publication date: 20190607 |