CN109946133A - A kind of metal-ceramic air-sensitive coating and preparation method thereof with schottky junction - Google Patents
A kind of metal-ceramic air-sensitive coating and preparation method thereof with schottky junction Download PDFInfo
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- CN109946133A CN109946133A CN201910215261.8A CN201910215261A CN109946133A CN 109946133 A CN109946133 A CN 109946133A CN 201910215261 A CN201910215261 A CN 201910215261A CN 109946133 A CN109946133 A CN 109946133A
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Abstract
The invention discloses a kind of metal-ceramic air-sensitive coating and preparation method thereof with schottky junction, the coating layer thickness is 5~20 μm, the grain size of ceramic phase is about 50~200nm in coating, the metal phase grain size of doping is about 10-50nm, doping is mutually uniformly distributed in entire coating, and it is in contact with ceramics closely, it is sent among particular heat source by the ceramics or its precursor pulp that will adulterate a small amount of metal nanoparticle, air-sensitive coating is prepared using liquid material plasma spray technology, metal and ceramics are in interface formation schottky junction in resulting composite air-sensitive coating, due to the difference of two kinds of material fermi energy levels, electronic barrier layer is formed when reaching equilibrium state, increase the initial resistance of composite coating, to make composite coating that there is extremely excellent air-sensitive performance, simple process, it is easily-controllable, cost compared with It is low, it is suitable for industrialization promotion.
Description
Technical field
The present invention relates to gas sensor technical field more particularly to a kind of metal-ceramic air-sensitives with schottky junction
Coating and preparation method thereof.
Background technique
The fields such as industry, environment and medical treatment are required to pernicious gas (NO, NO in air2、CO、SO2、H2S etc.) concentration progress
Real-time detection needs to develop high performance gas sensor.Semiconductor gas sensor is due to the simple, service life with structure
Long, compact and need not maintenance the advantages that, be the more successful seed type of commercial applications in sensor.Semi-conductor gas
The core of sensor is air-sensitive coating, and the material for being traditionally used for preparation sensor coatings is mainly zinc oxide (ZnO), tin oxide
(SnO2) and iron oxide (Fe2O3), but there is selectivity and stability is poor, power consumption is high, is influenced etc. to limit to by ambient temperature and humidity
Property.Relative to traditional material, WO3To NO2It is that one kind can be used for gas sensor coating with high sensitivity and resolution ratio
Ideal material.
The common production technology of Commercial semiconductors sensor air-sensitive coating is silk-screen printing and magnetron sputtering at present.But
Silk-screen printing coating structure is less reproducible, it is necessary to (organic in coating in order to remove using time-consuming high-temperature post-treatment technique
Binder and raising anchoring strength of coating).Sputtering equipment needs that vacuum working environment, sputter rate are slow, forming cost is high, film
Porosity poor controllability, so efficient, the inexpensive preparation air-sensitive coating technology for developing a kind of substitution above method is always
The target of industry.Liquid phase plasma spraying is a kind of emerging technology for preparing micro-structure controllable coatings, due to directly using metal
For salt as presoma, the crystal grain of prepared coating and the smaller of defect and controllable, specific surface area is bigger, is particularly suited for
Sensor air-sensitive coating.Meanwhile there is higher bond strength using the air-sensitive coating of liquid phase plasma spraying technology preparation,
And this method be not necessarily to after be heat-treated and vacuum equipment, with the incomparable advantage of conventional method on production cost and efficiency.
Result of study shows that metal (Ag, Pt and Au etc.) doping can be obviously improved the sensitivity of gas sensor, Chen etc.
It is prepared for the WO of Ag doping3Sensor, Ag doping can be WO3The test temperature of based sensor drops to 200 DEG C or less.
Senguttuvan T.D. etc. is the study found that adulterate WO by the Pt of calcining preparation3To NH3Response and selectivity be higher than it is commercially available
Pure WO3, and it is unrelated with calcination temperature.Shim etc. is prepared for Au and is doping to dome-type nanometer WO3, with pure WO3Compare, it is right
NO2, CH3COCH3, C2H5OH, NH3, CO, H2And C6H6The response of equal gases at least improves 5 times.Hoel etc. is prepared for Pd doping
WO3Film finds that the sensor mixed with Pd can reduce recovery time, increase to low concentration H2The response of S is shown extremely strong
Room temperature sensibility (sensitivity about 5000), can also detect the CHOH of low concentration.As it can be seen that utilizing metal-doped improvement coating
Air-sensitive performance has become current research hotspot, but the influence of the type of doping metals and ratio to coating air-sensitive performance is advised
The gas sensing mechanism of composite coating need to be furtherd investigate after rule and doping.Meanwhile doping metals in existing air-sensitive coating
Method is extremely complex, is unfavorable for large-scale industrial production.
Summary of the invention
In view of the above shortcomings of the prior art, the purpose of the present invention is to provide a kind of metal-pottery with schottky junction
Porcelain air-sensitive coating and preparation method thereof, this method is easy to operate, process flow is few, at low cost, and coating air-sensitive performance is good, is suitble to
Industrialized production effectively solves the problems, such as easy ablation and difficulty of transportation in nano-powder thermal spray process using liquid feeding, comprehensive
Alloy belongs to and the ceramic difference in terms of electric conductivity, forms schottky junction, solves the problems, such as that traditional air-sensitive coating sensibility is lower.
The present invention realizes technical solution used by foregoing invention purpose are as follows:
In a first aspect, the preparation method of the metal-ceramic air-sensitive coating with schottky junction, specifically, including following step
It is rapid:
(1) it prepares thermal spraying slurry: deionized water, dehydrated alcohol and surfactant being mixed according to a certain percentage
It is even, and nano ceramics or ceramic forerunner powder and nano-metal particle is added carries out magnetic agitation and be uniformly mixed, obtain thermal jet
Apply slurry；Wherein: in the slurry, the mass percentage of the nano ceramics or ceramic forerunner powder be 3wt%~
20wt%, the mass percentage of the nano-metal particle are 1wt%~5wt%, the quality percentage of the surfactant
Content is 0.03wt%~0.25wt%, and the volume ratio of the deionized water and dehydrated alcohol is 1:1~4；
(2) substrate pretreated: including being cleaned to matrix, the processing of degreasing and rust removal and roughing in surface；
(3) matrix surface thermal spray metal-ceramics air-sensitive coating: using hot-spraying technique, the heat that will be prepared in step (1)
Spraying slurry with the flow velocity of 10~50mL/min by diameter be 0.05~0.2mm nozzle, vertically into spraying heat source root,
Solvent evaporation occurs under Source, ceramic particle forming core, crystallizes and grows up, obtains solid particle；The solid particle warp
Fusing or semi-molten, and accelerating impact forms the metal-ceramic air-sensitive coating with a thickness of 5~30 μm to matrix surface.
Further, in step (1), the surfactant includes ammonium polyacrylate, ammonium polymethacrylate and poly- second
The combination of one or more of glycol.
Further, in step (1), the nano-metal particle includes one of Au, Ag, Pt, Cu, Fe, Zn and Al
Or any two or more mixture, average grain diameter are 10~50nm.
Further, in step (1), the ceramics include WO3、ZnO、TiO2、SnO2And Fe2O3One of or it is two kinds any
The nanometer powder mixed above or its precursor powder, average grain diameter are 50~200nm.
Further, in step (2), the method for described matrix roughing in surface includes in sandblasting, cutting thread, annular knurl and electric plucking
One kind.
Further, in step (3), the hot-spraying technique includes plasma spraying, flame-spraying, electric arc spraying and Supersonic
One kind of fast flame-spraying.
Further, in step (3), the hot-spraying technique uses plasma spraying, and its spray parameters are as follows: electric current is
450~750A, voltage be 50~75V, spray coating liquor stream amount be 10~50mL/min, spray distance be 130~200mm, wait from
Sub- spray gun movement speed is 300~500mm/s, and coating spraying pass is 15~40 times.
Second aspect, the metal-ceramic air-sensitive coating with schottky junction are obtained by above-mentioned preparation method, with a thickness of
5~30 μm, there is porous nanostructure and schottky junction.
Further, the grain size of ceramic phase is 50~200nm in coating, the metal phase grain size of doping is 10~
50nm, and doping is mutually uniformly distributed in coating, is in contact closely with the ceramics.
Compared with prior art, the beneficial effects of the present invention are:
(1) ceramic slurry of precious metal doping is sent directly into thermal spraying heat source in the present invention, the metal of doping is uniform
It is distributed in entire coating, and realizes and be in close contact with ceramics, overcome the shortcomings that nano-powder cannot spray, coating is still kept
Nanostructure, and coated porous has biggish specific surface area, high sensitivity.
(2) metal-doped in the present invention to enter nano ceramics phase, Schottky is formed in the interface of metal and ceramic crystalline grain
Knot, due to the difference of two kinds of material fermi energy levels, forms electronic barrier layer when reaching equilibrium state, makes the initial electricity of composite coating
Resistance increases, and further promotes the air-sensitive performance of coating.
(3) metal-ceramic air-sensitive coating being prepared using hot-spraying technique, simple process, thickness is controllable, and deposition efficiency is high,
Production cost is low, can large area preparation, be suitable for industrialization metaplasia produce, environmental protection, electronics industry especially gas sensor field
With good application value and market prospects.
Detailed description of the invention
Fig. 1 is Au-WO obtained in the embodiment of the present invention 13The XRD spectrum of air-sensitive coating；There was only WO in coating3With Au's
Characteristic peak does not occur the two reaction and generates other interphases, illustrates that combination reaction does not occur for two-phase in the composite coating of preparation.
Fig. 2 is Au-WO obtained in the embodiment of the present invention 13The EDS of coating is analyzed；In the microcell of observed composite coating
In, there is the characteristic peak of apparent element W, O and Au, illustrates that this three kinds of elements are distributed in microcell.From element ratio
From the point of view of example, the atomic ratio (22.21:74.53) of W and O illustrate to form WO in coating close to 1:33Phase illustrates to utilize this hair
Bright liquid phase plasma spraying method successfully prepares the WO of Au doping3Base composite coating.
Fig. 3 is Au-WO in the embodiment of the present invention 13The schematic diagram of composite coating formation schottky junction: (a) pure WO3Coating；
(b)Au-WO3Coating.Figure (b) shows due to the conductor that Au is function admirable, WO3Work function for the semiconductor of N-shaped, and Au is wanted
Greater than WO3.As Au and WO3After close contact, WO3Electronics in conduction band will be flowed to Au, in semiconductor WO when stablizing3Surface
Electronic barrier layer is formed, WO in composite coating is caused3Energy band be bent upwards, constitute schottky junction.
Specific embodiment
Present invention is further described in detail for embodiment with reference to the accompanying drawing, it should be pointed out that implementation as described below
Example is intended to convenient for the understanding of the present invention, and does not play any restriction effect to it.
In following instance, to characterize the metal-ceramic air-sensitive coating performance with schottky junction being prepared, X is utilized
X ray diffractometer x (XRD) and field emission scanning electron microscope (FESEM) and its subsidiary energy disperse spectroscopy (EDS) are to prepared painting
Layer sample is characterized, while measuring coating sample to 100ppmNO2The response resistance signal of gas.
Embodiment 1
Select the Al of basis material thickness about 2mm2O3Potsherd, nanometer Au adulterates WO on the matrix3Coating with a thickness of 5 μ
M, coating WO3Porous structure made of nanocrystal stacking, it is specific the preparation method is as follows:
1, by deionized water and the dehydrated alcohol wiring solution-forming of 1:1 mixing by volume, the surface-active of 0.08wt% is added
Agent polyethylene glycol PEG20000, by commercially available WO3Presoma (WCl6) and Au nanometer powder (partial size be 5~15nm) be added to
It states in the solution prepared, WCl is uniformly made by magnetic agitation6Solid content is 10wt%, and Au doping is the spray coating liquor of 6wt%
Material.
2, matrix is cleaned, carries out surface sand-blasting pretreatment using 60 mesh corundum sands, its roughness is made to reach spray
It applies and requires, improve the bond strength of coating and matrix.
3, using feeding style outside plasma spray gun, liquid material is at the uniform velocity by outlet diameter under wriggling pumping actionNozzle be vertically sent into flame root, and be voluntarily atomized pyrolysis with flame, form the painting with a thickness of 5 μm on matrix
Layer.Wherein, Plasma Spray Parameters are as follows: electric current 600A, voltage 50V, liquid material flow 25ml/min, spray distance 180mm, wait from
Sub- spray gun movement speed 600mm/s is sprayed number 20 times.
Utilize X-ray diffractometer (XRD) and field emission scanning electron microscope (FESEM) and its subsidiary energy disperse spectroscopy
(EDS) prepared coating sample is characterized, as a result as depicted in figs. 1 and 2, while measures coating sample to 100ppm
NO2The response resistance signal of gas, when temperature is 100 DEG C, the response resistance maximum value of coating sample reaches 4.8 × 107Ohm, table
Bright coating has preferable air-sensitive performance.
Embodiment 2
In the present embodiment, the doping of nanometer Au is changed into 9wt%, other preparation conditions and spray parameters and embodiment
It is identical in 1.Coating sample is measured to 100ppm NO2The response resistance signal of gas, when temperature is 100 DEG C, coating sample
The response resistance maximum value of product reaches 5.7 × 107Ohm shows that coating has preferable air-sensitive performance.
Embodiment 3
In the present embodiment, the doping of nanometer Au is changed into 3wt%, other preparation conditions and spray parameters and embodiment
It is identical in 1.Coating sample is measured to 100ppm NO2The response resistance signal of gas, when temperature is 100 DEG C, coating sample
The response resistance maximum value of product reaches 3.5 × 107Ohm shows that coating has preferable air-sensitive performance.
Embodiment 4
In the present embodiment, doping phase nanometer Au is changed to Pt nano particle, in other preparation conditions and spray parameters and embodiment 1
It is identical.Coating sample is measured to 100ppm NO2The response resistance signal of gas, when temperature is 100 DEG C, coating sample
Response resistance maximum value reach 3.5 × 107Ohm shows that coating has preferable air-sensitive performance.
Embodiment 5
In the present embodiment, by ceramic phase nanometer WO3It is changed to nano-ZnO, other preparation conditions and spray parameters and embodiment 1
In it is identical.Coating sample is measured to 100ppm NO2The response resistance signal of gas, when temperature is 100 DEG C, coating sample
The response resistance maximum value of product reaches 5.2 × 107Ohm shows that coating has preferable air-sensitive performance.
Embodiment 6
In the present embodiment, by basis material Al2O3Potsherd is changed to stainless steel substrates, other preparation conditions and spray parameters with
It is identical in embodiment 1.Coating sample is measured to 100ppm NO2The response resistance signal of gas, when temperature is 100 DEG C,
The response resistance maximum value of coating sample reaches 4.7 × 107Ohm shows that coating has preferable air-sensitive performance.
Embodiment 7
In the present embodiment, heat spraying method is changed to flame-spraying, ingredient, ratio and the preparation method of spraying slurry with
It is identical in embodiment 1.Composite coating it is specific the preparation method is as follows:
Matrix is cleaned, surface sand-blasting pretreatment is carried out using 60 mesh corundum sands, its roughness is made to reach spraying
It is required that improving the bond strength of coating and matrix；
Using feeding style outside flame spraying gun, liquid material is at the uniform velocity by outlet diameter under wriggling pumping action
Nozzle be vertically sent into flame root, and be voluntarily atomized pyrolysis with flame, form the coating with a thickness of 5 μm on matrix.Wherein,
Flame-spraying parameter are as follows: respectively in 12bar and 4bar, flow is respectively 8L/min and 15L/min for combustion-supporting gas and flammable atmospheric pressure,
The flow of liquid material is 10mL/min, and the distance of spraying is 150mm, and flame gun movement speed is 300mm/s, sprays number 30
Time.
Coating sample is measured to 100ppm NO2The response resistance signal of gas, when temperature is 100 DEG C, the sound of coating sample
Resistance maximum value is answered to reach 3.9 × 107Ohm shows that coating has preferable air-sensitive performance.
In conclusion metal-ceramic air-sensitive coating prepared by the present invention, has porous nanostructure, is able to satisfy air-sensitive
To the requirement of coating high-specific surface area in sensor field.In addition, be doped with a certain amount of metal, in metal and ceramic crystalline grain
Interface forms schottky junction, increases the initial resistance of composite coating, further improves the air-sensitive performance of coating.And it prepares
Simple process, thickness is controllable, and deposition efficiency is high, and production cost is low, can large area preparation, be suitable for industrialization metaplasia and produce, environmental protection,
Electronics industry especially gas sensor field has good application value and market prospects.
Claims (9)
1. a kind of preparation method of the metal-ceramic air-sensitive coating with schottky junction, which comprises the following steps:
(1) it prepares thermal spraying slurry: deionized water, dehydrated alcohol and surfactant is uniformly mixed according to a certain percentage, and
Nano ceramics or ceramic forerunner powder is added and nano-metal particle carries out magnetic agitation and is uniformly mixed, obtains thermal jet pasting
Material；Wherein: in the slurry, the mass percentage of the nano ceramics or ceramic forerunner powder is 3wt%~20wt%,
The mass percentage of the nano-metal particle is 1wt%~5wt%, and the mass percentage of the surfactant is
The volume ratio of 0.03wt%~0.25wt%, the deionized water and dehydrated alcohol is 1:1~4；
(2) substrate pretreated: including being cleaned to matrix, the processing of degreasing and rust removal and roughing in surface；
(3) matrix surface thermal spray metal-ceramics air-sensitive coating: using hot-spraying technique, the thermal spraying that will be prepared in step (1)
The nozzle that slurry is 0.05~0.2mm by diameter with the flow velocity of 10~50mL/min, vertically into spraying heat source root, in heat
Source effect is lower to be occurred solvent evaporation, ceramic particle forming core, crystallizes and grow up, and solid particle is obtained；The solid particle is through melting
Or semi-molten, and accelerating impact forms the metal-ceramic air-sensitive coating with a thickness of 5~30 μm to matrix surface.
2. the preparation method of metal-ceramic air-sensitive coating according to claim 1, which is characterized in that described in step (1)
Surfactant include one or more of ammonium polyacrylate, ammonium polymethacrylate and polyethylene glycol combination.
3. the preparation method of metal-ceramic air-sensitive coating according to claim 1, which is characterized in that described in step (1)
Nano-metal particle include the two or more mixture of one of Au, Ag, Pt, Cu, Fe, Zn and Al or any, be averaged
Partial size is 10~50nm.
4. the preparation method of metal-ceramic air-sensitive coating according to claim 1, which is characterized in that described in step (1)
Ceramics include WO3、ZnO、TiO2、SnO2And Fe2O3One of or any two or more mixed nanometer powders or its presoma
Powder, average grain diameter are 50~200nm.
5. the preparation method of metal-ceramic air-sensitive coating according to claim 1, which is characterized in that described in step (2)
The method of matrix surface roughening includes one of sandblasting, cutting thread, annular knurl and electric plucking.
6. the preparation method of metal-ceramic air-sensitive coating according to claim 1, which is characterized in that described in step (3)
Hot-spraying technique includes one kind of plasma spraying, flame-spraying, electric arc spraying and supersonic flame spraying.
7. the preparation method of metal-ceramic air-sensitive coating according to claim 1 or 6, which is characterized in that in step (3), institute
It states hot-spraying technique and uses plasma spraying, and its spray parameters are as follows: electric current is 450~750A, and voltage is 50~75V, spraying
Liquid material flow is 10~50mL/min, and spray distance is 130~200mm, and plasma gun movement speed is 300~500mm/s,
Coating spraying pass is 15~40 times.
8. the metal-ceramic air-sensitive coating with schottky junction, which is characterized in that it passes through described in any one of claim 1-7
The preparation method of metal-ceramic air-sensitive coating is made, and coating layer thickness is 5~30 μm, has porous nanostructure and Schottky
Knot.
9. metal-ceramic air-sensitive coating according to claim 8, which is characterized in that the grain size of ceramic phase in coating
For 50~200nm, the metal phase grain size of doping is 10~50nm, and doping is mutually uniformly distributed in coating, with the pottery
Porcelain is in contact closely.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103741089A (en) * | 2013-12-30 | 2014-04-23 | 中国科学院宁波材料技术与工程研究所 | Method and product for preparing ultra-thin porous WO3 gas-sensitive coating by using thermal spraying technology |
| CN103924184A (en) * | 2014-04-30 | 2014-07-16 | 绍兴斯普瑞微纳科技有限公司 | WO3 gas sensitive coating in porous micro-nano structure and preparation method thereof |
| CN104278228A (en) * | 2013-07-08 | 2015-01-14 | 中国科学院宁波材料技术与工程研究所 | Precious metal-doped WO3 gas-sensitive coating and preparation method thereof |
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2019
- 2019-03-21 CN CN201910215261.8A patent/CN109946133A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104278228A (en) * | 2013-07-08 | 2015-01-14 | 中国科学院宁波材料技术与工程研究所 | Precious metal-doped WO3 gas-sensitive coating and preparation method thereof |
| CN103741089A (en) * | 2013-12-30 | 2014-04-23 | 中国科学院宁波材料技术与工程研究所 | Method and product for preparing ultra-thin porous WO3 gas-sensitive coating by using thermal spraying technology |
| CN103924184A (en) * | 2014-04-30 | 2014-07-16 | 绍兴斯普瑞微纳科技有限公司 | WO3 gas sensitive coating in porous micro-nano structure and preparation method thereof |
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Application publication date: 20190628 |