CN108760836A - A kind of cold ethanol detection unit - Google Patents
A kind of cold ethanol detection unit Download PDFInfo
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- CN108760836A CN108760836A CN201811017472.2A CN201811017472A CN108760836A CN 108760836 A CN108760836 A CN 108760836A CN 201811017472 A CN201811017472 A CN 201811017472A CN 108760836 A CN108760836 A CN 108760836A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
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Abstract
The present invention relates to a kind of cold ethanol detection units, the detection unit is heater-type alcohol gas sensor, it includes ceramic tube substrate, it is equipped with a pair of of gold electrode on the both sides of ceramic tube substrate, gold electrode is connected with conducting wire, it is internally provided with heating element in ceramic tube substrate, sensitive material film is equipped in ceramic tube substrate surface;The sensitive material is metal composite oxide, specially ZnSnO3Nanosphere and SnO2The mixture of nano-particle.
Description
Technical field
The present invention relates to ethyl alcohol detection technique field more particularly to a kind of cold ethanol detection units.
Background technology
External information can be received and the device for being converted into available signal according to certain rule becomes sensor, gas sensor
It is a kind of physical device for gas sensitization.In people's daily life, the variation of atmosphere has significant effect the mankind,
For example, the leakage of imflammable gas can set off an explosion.Based on above-mentioned, gas sensor refers to that can be converted to tested gas concentration
The device or device exported at the electricity of certain relationship with it.
Specific to alcohol gas sensor, it can be common that the gas sensing based on metal oxide semiconductor sensitive material
Device, usually indirect heat resistance-type type.
However, in the prior art, the still unavoidable defect having in a certain respect of the ethanol sensor, such as operating temperature
It is higher, usually 200~400 DEG C etc..
Invention content
It is one of at least to solve the above problems, the present invention is intended to provide a kind of cold ethanol detection unit.
A kind of cold ethanol detection unit is provided in the embodiment of the present invention, the detection unit is heater-type ethanol gas
Body sensor comprising ceramic tube substrate is equipped with a pair of of gold electrode on the both sides of ceramic tube substrate, and gold electrode is connected with conducting wire,
It is internally provided with heating element in ceramic tube substrate, sensitive material film is equipped in ceramic tube substrate surface;The sensitive material
For metal composite oxide, specially ZnSnO3Nanosphere and SnO2The mixture of nano-particle.
Preferably, the ZnSnO3Nanosphere is core-shell nanospheres;Wherein, nuclear structure is Zn nano-particles, shell knot
Structure is ZnSnO3。
Preferably, nucleocapsid ZnSnO3In nanosphere, the Zn nano particle diameters are 500-1000nm, described
ZnSnO3Shell structure thickness is 100nm.
A kind of preparation method of cold ethanol detection unit is additionally provided in the embodiment of the present invention:
By Zn nano-particles in dilute hydrochloric acid and SnCl4Mixed solution in pre-process;
By zinc acetate, SnCl4·5H2O, pretreated Zn nano-particles and the mixing of NaOH aqueous solutions, it is anti-in polytetrafluoroethylene (PTFE)
Hydro-thermal reaction in kettle is answered to obtain nucleocapsid ZnSnO3Nanosphere;
By nucleocapsid ZnSnO3Nanosphere and SnO2Nano-particle is mixed to get sensitive material;
Pasty slurry is made in sensitive material dispersion in ethanol and is uniformly coated in ceramic substrate surface, after aging
Obtain the detection unit.
The technical solution that the embodiment of the present invention provides can include the following benefits:
Different from directly using ZnSnO3Nano material, after being prepared into above-mentioned nucleocapsid, internal nuclear structure tool
There is good thermal conductivity, the response of temperature can quickly be conducted to external shell structure, even if making external shell structure in low temperature
Under can also show sensitive reaction to alcohol gas, greatly reduce the operating temperature of sensitive material.On the other hand, should
SnO2Nano-particle and ZnSnO3Nanosphere mixes, it may have improves the effect of sensitive material sensitivity.
The additional aspect of the present invention and advantage will be set forth in part in the description, and will partly become from the following description
Obviously, or practice through the invention is recognized.It should be understood that above general description and following detailed description are only
It is exemplary and explanatory, the present invention can not be limited.
Description of the drawings
Using attached drawing, the invention will be further described, but the embodiment in attached drawing does not constitute any limit to the present invention
System, for those of ordinary skill in the art, without creative efforts, can also obtain according to the following drawings
Other attached drawings.
Fig. 1 is the structural schematic diagram of detection unit described in embodiment of the present invention.
Specific implementation mode
Example embodiments are described in detail here, and the example is illustrated in the accompanying drawings.Following description is related to
When attached drawing, unless otherwise indicated, the same numbers in different drawings indicate the same or similar elements.Following exemplary embodiment
Described in embodiment do not represent and the consistent all embodiments of the present invention.On the contrary, they be only with it is such as appended
The example of the consistent device and method of some aspects being described in detail in claims, of the invention.
Disclosed technique scheme relates in one aspect to a kind of cold ethanol detection unit, which is heater-type ethanol gas
Body sensor.
In conjunction with shown in Fig. 1, which is heater-type structure, including ceramic tube substrate 22, in ceramic tube substrate 22
Both sides are equipped with a pair of of gold electrode 21, and gold electrode is connected with conducting wire 25, heating element 24 is internally provided in ceramic tube substrate 22;?
22 surface of ceramic tube substrate is equipped with sensitive material film 23;
The thickness of the gold electrode 21 is 2mm, which is Pt heater strips;
Specifically, the sensitive material is metal composite oxide, specially ZnSnO3Nanosphere and SnO2Nano-particle
Mixture.
SnO2It is a kind of wide bandgap semiconductor metal oxide of rutile structure, energy gap is reachable at room temperature
3.65eV, due to typical n-type semiconductor property and resistivity and higher light transmittance, in gas sensor, solar energy
The fields such as battery, transparent electrode all have application prospect;In the prior art, due to SnO2Unique air-sensitive property, to a variety of
Gas has good gas sensing property and becomes the gas sensitive for most having application potential in numerous oxides.ZnSnO3It is a kind of typical case
Perovskite structure ternary metal oxide, in the prior art, it can be found that its for ethyl alcohol have good air-sensitive effect.
In the technical solution of the disclosure, which is based on above two semiconductor nano material, achieves expectation not
The sensitizing effect to ethyl alcohol arrived.
Specifically, above-mentioned ZnSnO3Nanosphere is core-shell nanospheres;
Wherein, nuclear structure is Zn nano-particles, shell structure ZnSnO3;
Different from directly using ZnSnO3Nano material, after being prepared into above-mentioned nucleocapsid, internal nuclear structure tool
There is good thermal conductivity, the response of temperature can quickly be conducted to external shell structure, even if making external shell structure in low temperature
Under can also show sensitive reaction to alcohol gas, greatly reduce the operating temperature of sensitive material.On the other hand, should
SnO2Nano-particle and ZnSnO3Nanosphere mixes, it may have improves the effect of sensitive material sensitivity.
Preferably, in above-mentioned sensitive material, ZnSnO3Nanosphere and SnO2The molar ratio of nano-particle is 1:4-7;
Preferably, nucleocapsid ZnSnO3In nanosphere, the Zn nano particle diameters are 500-1000nm, described
ZnSnO3Shell structure thickness is 100nm;
Preferably, the SnO2The grain size of nano-particle is 50nm.
On the other hand disclosed technique scheme is related to the preparation method of above-mentioned detection unit:
By Zn nano-particles in dilute hydrochloric acid and SnCl4Mixed solution in pre-process;
By zinc acetate, SnCl4·5H2O, pretreated Zn nano-particles and the mixing of NaOH aqueous solutions, it is anti-in polytetrafluoroethylene (PTFE)
Hydro-thermal reaction in kettle is answered to obtain nucleocapsid ZnSnO3Nanosphere;
By nucleocapsid ZnSnO3Nanosphere and SnO2Nano-particle is mixed to get sensitive material;
Pasty slurry is made in sensitive material dispersion in ethanol and is uniformly coated in ceramic substrate surface, after aging
Obtain the detection unit.
Wherein, it is described by Zn nano-particles in dilute hydrochloric acid and SnCl4Mixed solution in pretreatment be specially:
Zn nano-particles are cleaned by ultrasonic 20min first, Zn nano-particles are then placed in dilute hydrochloric acid and SnCl4Mixing
It in solution, stirs evenly, in 70 DEG C of isothermal holding 2h;
More specifically, a concentration of 0.4mol/L of HCl, SnCl in the mixed solution4A concentration of 0.2mol/L;
Wherein, described by zinc acetate, SnCl4·5H2O, pretreated Zn nano-particles and the mixing of NaOH aqueous solutions, poly-
Hydro-thermal reaction obtains nucleocapsid ZnSnO in tetrafluoroethene reaction kettle3Nanosphere is specially:
The NaOH aqueous solutions of 50ml are taken, the above-mentioned pretreated Zn nano-particles of 4.0mol are added, obtains solution A, stirs evenly,
Solution A is transferred in the reaction kettle with polytetrafluoroethyllining lining, 130 DEG C of reaction 1.5h is heated to, solution A is taken out after cooling;
Then zinc acetate and SnCl is added in solution A again4·5H2O obtains solution B, and solution B is transferred to polytetrafluoroethyl-ne
In the reaction kettle of alkene liner, 170 DEG C of reaction 3.5h are heated to, is taken out after cooling, precipitation is filtered, is cleaned up, are done at 60 DEG C
Dry 3h obtains nucleocapsid ZnSnO3Nanosphere;
More specifically, the NaOH concentration of aqueous solution is 0.2mol/L;
It is described that zinc acetate and SnCl are added in solution A4·5H2O is specially the zinc acetate that 2.0mol is added in solution A
With the SnCl of 6.0mol4·5H2O;
Wherein, the aging temperature is 300 DEG C;
Embodiment 1
The preparation process of above-mentioned detection unit is:
Step 1, pretreatment Zn nano-particles
Screen appropriate particle size Zn nano-particles, Zn nano-particles are cleaned by ultrasonic, wherein be cleaned by ultrasonic the time be
20min;
Then, Zn nano-particles are placed in dilute hydrochloric acid and SnCl4Mixed solution in, stir evenly, at 70 DEG C of heat preservations
Manage 2h, wherein HCl a concentration of 0.4mol/L, SnCl4A concentration of 0.2mol/L;
Zn nano-particles are filtered and are taken out, are cleaned up;
Step 2 prepares nucleocapsid ZnSnO3Nanosphere
The NaOH aqueous solutions of a concentration of 0.2mol/L of 50ml are taken, the above-mentioned pretreated Zn nano-particles of 4.0mol are added, obtain
Solution A stirs evenly, and solution A is transferred in the reaction kettle with polytetrafluoroethyllining lining, is heated to 130 DEG C and reacts 1.5h, cold
But solution A is taken out afterwards;
Then the SnCl of the zinc acetate and 6.0mol of 2.0mol is added in solution A again4·5H2O obtains solution B, by solution B
It is transferred in the reaction kettle with polytetrafluoroethyllining lining, is heated to 170 DEG C of reaction 3.5h, takes out, precipitation is filtered, clearly after cooling
Wash clean obtains nucleocapsid ZnSnO in 60 DEG C of dry 3h3Nanosphere;
Step 3 prepares sensitive material
By nucleocapsid ZnSnO obtained above3Nanosphere and SnO2Nano-particle is uniformly mixed, and is placed in ethanol solution,
Magnetic agitation is uniform, then filters, and sensitive material is obtained after dry;
Step 4 prepares detection unit
Pasty slurry is made in a certain amount of above-mentioned sensitive material dispersion in ethanol and it is uniformly coated in ceramics
Substrate surface should ensure that gold electrode is all covered in coating procedure, then a Pt heater strip is inserted into ceramics, 300 DEG C
After aging 2 days, heater-type gas sensor is made.
Wherein, in sensitive material, ZnSnO3Nanosphere and SnO2The molar ratio of nano-particle is 1:4.
Embodiment 2
The preparation process of above-mentioned detection unit is:
Step 1, pretreatment Zn nano-particles
Screen appropriate particle size Zn nano-particles, Zn nano-particles are cleaned by ultrasonic, wherein be cleaned by ultrasonic the time be
20min;
Then, Zn nano-particles are placed in dilute hydrochloric acid and SnCl4Mixed solution in, stir evenly, at 70 DEG C of heat preservations
Manage 2h, wherein HCl a concentration of 0.4mol/L, SnCl4A concentration of 0.2mol/L;
Zn nano-particles are filtered and are taken out, are cleaned up;
Step 2 prepares nucleocapsid ZnSnO3Nanosphere
The NaOH aqueous solutions of a concentration of 0.2mol/L of 50ml are taken, the above-mentioned pretreated Zn nano-particles of 4.0mol are added, obtain
Solution A stirs evenly, and solution A is transferred in the reaction kettle with polytetrafluoroethyllining lining, is heated to 130 DEG C and reacts 1.5h, cold
But it takes out afterwards;
Then the SnCl of the zinc acetate and 6.0mol of 2.0mol is added in solution A again4·5H2O obtains solution B, by solution B
It is transferred in the reaction kettle with polytetrafluoroethyllining lining, is heated to 170 DEG C of reaction 3.5h, takes out, precipitation is filtered, clearly after cooling
Wash clean obtains nucleocapsid ZnSnO in 60 DEG C of dry 3h3Nanosphere;
Step 3 prepares sensitive material
By nucleocapsid ZnSnO obtained above3Nanosphere and SnO2Nano-particle is uniformly mixed, and is placed in ethanol solution,
Magnetic agitation is uniform, then filters, and sensitive material is obtained after dry;
Step 4 prepares detection unit
Pasty slurry is made in a certain amount of above-mentioned sensitive material dispersion in ethanol and it is uniformly coated in ceramics
Substrate surface should ensure that gold electrode is all covered in coating procedure, then a Pt heater strip is inserted into ceramics, 300 DEG C
After aging 2 days, heater-type gas sensor is made.
Wherein, in sensitive material, ZnSnO3Nanosphere and SnO2The molar ratio of nano-particle is 1:5.
Embodiment 3
The preparation process of above-mentioned detection unit is:
Step 1, pretreatment Zn nano-particles
Screen appropriate particle size Zn nano-particles, Zn nano-particles are cleaned by ultrasonic, wherein be cleaned by ultrasonic the time be
20min;
Then, Zn nano-particles are placed in dilute hydrochloric acid and SnCl4Mixed solution in, stir evenly, at 70 DEG C of heat preservations
Manage 2h, wherein HCl a concentration of 0.4mol/L, SnCl4A concentration of 0.2mol/L;
Zn nano-particles are filtered and are taken out, are cleaned up;
Step 2 prepares nucleocapsid ZnSnO3Nanosphere
The NaOH aqueous solutions of a concentration of 0.2mol/L of 50ml are taken, the above-mentioned pretreated Zn nano-particles of 4.0mol are added, obtain
Solution A stirs evenly, and solution A is transferred in the reaction kettle with polytetrafluoroethyllining lining, is heated to 130 DEG C and reacts 1.5h, cold
But it takes out afterwards;
Then the SnCl of the zinc acetate and 6.0mol of 2.0mol is added in solution A again4·5H2O obtains solution B, by solution B
It is transferred in the reaction kettle with polytetrafluoroethyllining lining, is heated to 170 DEG C of reaction 3.5h, takes out, precipitation is filtered, clearly after cooling
Wash clean obtains nucleocapsid ZnSnO in 60 DEG C of dry 3h3Nanosphere;
Step 3 prepares sensitive material
By nucleocapsid ZnSnO obtained above3Nanosphere and SnO2Nano-particle is uniformly mixed, and is placed in ethanol solution,
Magnetic agitation is uniform, then filters, and sensitive material is obtained after dry;
Step 4 prepares detection unit
Pasty slurry is made in a certain amount of above-mentioned sensitive material dispersion in ethanol and it is uniformly coated in ceramics
Substrate surface should ensure that gold electrode is all covered in coating procedure, then a Pt heater strip is inserted into ceramics, 300 DEG C
After aging 2 days, heater-type gas sensor is made.
Wherein, in sensitive material, ZnSnO3Nanosphere and SnO2The molar ratio of nano-particle is 1:6.
Embodiment 4
The preparation process of above-mentioned detection unit is:
Step 1, pretreatment Zn nano-particles
Screen appropriate particle size Zn nano-particles, Zn nano-particles are cleaned by ultrasonic, wherein be cleaned by ultrasonic the time be
20min;
Then, Zn nano-particles are placed in dilute hydrochloric acid and SnCl4Mixed solution in, stir evenly, at 70 DEG C of heat preservations
Manage 2h, wherein HCl a concentration of 0.4mol/L, SnCl4A concentration of 0.2mol/L;
Zn nano-particles are filtered and are taken out, are cleaned up;
Step 2 prepares nucleocapsid ZnSnO3Nanosphere
The NaOH aqueous solutions of a concentration of 0.2mol/L of 50ml are taken, the above-mentioned pretreated Zn nano-particles of 4.0mol are added, obtain
Solution A stirs evenly, and solution A is transferred in the reaction kettle with polytetrafluoroethyllining lining, is heated to 130 DEG C and reacts 1.5h, cold
But it takes out afterwards;
Then the SnCl of the zinc acetate and 6.0mol of 2.0mol is added in solution A again4·5H2O obtains solution B, by solution B
It is transferred in the reaction kettle with polytetrafluoroethyllining lining, is heated to 170 DEG C of reaction 3.5h, takes out, precipitation is filtered, clearly after cooling
Wash clean obtains nucleocapsid ZnSnO in 60 DEG C of dry 3h3Nanosphere;
Step 3 prepares sensitive material
By nucleocapsid ZnSnO obtained above3Nanosphere and SnO2Nano-particle is uniformly mixed, and is placed in ethanol solution,
Magnetic agitation is uniform, then filters, and sensitive material is obtained after dry;
Step 4 prepares detection unit
Pasty slurry is made in a certain amount of above-mentioned sensitive material dispersion in ethanol and it is uniformly coated in ceramics
Substrate surface should ensure that gold electrode is all covered in coating procedure, then a Pt heater strip is inserted into ceramics, 300 DEG C
After aging 2 days, heater-type gas sensor is made.
Wherein, in sensitive material, ZnSnO3Nanosphere and SnO2The molar ratio of nano-particle is 1:7.
The sensitivity of detection unit, response recovery time etc. use this field usual definition in the present invention.Utilize air-sensitive spy
Property tester tests detection unit of the present invention:First certain density object gas is injected into sealing test chamber, is waited for
Object gas after mixing, then by detection unit is put into test chamber with the air in chamber.
First, the optimum working temperature of detection unit of the present invention is characterized, such as the following table 1 tests the inspection that embodiment 1-4 is obtained
Survey unit respectively under the alcohol gas of 100ppm concentration, operating temperature range be 50~250 DEG C when sensitivity, it is as follows:
Table 1:Sensitivity when operating temperature range is 50~250 DEG C in 100ppm concentration ethanol gases
50℃ | 90℃ | 130℃ | 170℃ | 210℃ | 250℃ | |
Embodiment 1 | 53 | 75 | 82 | 51 | 47 | 36 |
Embodiment 2 | 46 | 72 | 84 | 63 | 39 | 31 |
Embodiment 3 | 41 | 69 | 79 | 66 | 37 | 34 |
Embodiment 4 | 44 | 68 | 85 | 61 | 40 | 29 |
It can be seen that when operating temperature range is 50~250 DEG C, sensitivity is increased with the raising of temperature,
After more than optimum working temperature, temperature continues to increase, and sensitivity then declines.
In embodiment 1-4, when temperature reaches 130 DEG C, sensitivity is maximum;Show sensitive material to reducing work temperature
Degree plays good effect.
The foregoing is merely the preferred modes of the present invention, are not intended to limit the invention, all spirit and original in the present invention
Within then, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of cold ethanol detection unit, the detection unit is heater-type alcohol gas sensor, which is characterized in that it is wrapped
Ceramic tube substrate is included, is equipped with a pair of of gold electrode on the both sides of ceramic tube substrate, gold electrode is connected with conducting wire, in ceramic tube substrate
It is internally provided with heating element, sensitive material film is equipped in ceramic tube substrate surface;The sensitive material aoxidizes for composition metal
Object, specially ZnSnO3Nanosphere and SnO2The mixture of nano-particle.
2. a kind of low temperature detection unit according to claim 1, which is characterized in that the thickness of the gold electrode is 2mm, institute
It is Pt heater strips to state heating element.
3. a kind of low temperature detection unit according to claim 1, which is characterized in that the ZnSnO3Nanosphere is nucleocapsid knot
Structure nanosphere;Wherein, nuclear structure is Zn nano-particles, shell structure ZnSnO3。
4. a kind of low temperature detection unit according to claim 3, which is characterized in that nucleocapsid ZnSnO3In nanosphere, institute
It is 500-1000nm, the ZnSnO to state Zn nano particle diameters3Shell structure thickness is 100nm.
5. a kind of low temperature detection unit according to claim 1, which is characterized in that in sensitive material, the ZnSnO3Nanometer
Ball and SnO2The molar ratio of nano-particle is 1:4-7.
6. a kind of low temperature detection unit according to claim 1, which is characterized in that the SnO2The grain size of nano-particle is
50nm。
7. a kind of low temperature detection unit according to claim 1, which is characterized in that the preparation method of the detection unit
For:
By Zn nano-particles in dilute hydrochloric acid and SnCl4Mixed solution in pre-process;
By zinc acetate, SnCl4·5H2O, pretreated Zn nano-particles and the mixing of NaOH aqueous solutions, in ptfe autoclave
Middle hydro-thermal reaction obtains nucleocapsid ZnSnO3Nanosphere;
By nucleocapsid ZnSnO3Nanosphere and SnO2Nano-particle is mixed to get sensitive material;
Pasty slurry is made in sensitive material dispersion in ethanol and is uniformly coated in ceramic substrate surface, is obtained after aging
The detection unit.
8. a kind of low temperature detection unit according to claim 7, which is characterized in that it is described by Zn nano-particles in dilute hydrochloric acid
And SnCl4Mixed solution in pretreatment be specially:
Zn nano-particles are cleaned by ultrasonic 20min first, Zn nano-particles are then placed in dilute hydrochloric acid and SnCl4Mixed solution
In, it stirs evenly, in 70 DEG C of isothermal holding 2h.
9. a kind of low temperature detection unit according to claim 7, which is characterized in that described by zinc acetate, SnCl4·5H2O、
Pretreated Zn nano-particles and the mixing of NaOH aqueous solutions, hydro-thermal reaction obtains nucleocapsid in ptfe autoclave
ZnSnO3Nanosphere is specially:
The NaOH aqueous solutions of 50ml are taken, the above-mentioned pretreated Zn nano-particles of 4.0mol are added, obtains solution A, stirs evenly, it will be molten
Liquid A is transferred in the reaction kettle with polytetrafluoroethyllining lining, is heated to 130 DEG C of reaction 1.5h, solution A is taken out after cooling;
Then zinc acetate and SnCl is added in solution A again4·5H2O obtains solution B, and solution B is transferred to in polytetrafluoroethylene (PTFE)
In the reaction kettle of lining, be heated to 170 DEG C of reaction 3.5h, taken out after cooling, will precipitation filtering, clean up, in 60 DEG C of dry 3h,
Obtain nucleocapsid ZnSnO3Nanosphere.
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CN110044420A (en) * | 2019-05-08 | 2019-07-23 | 众诚恒祥(北京)科技有限公司 | A kind of greenhouse gas emissions detection device |
CN110044420B (en) * | 2019-05-08 | 2020-06-26 | 众诚恒祥(北京)科技有限公司 | Greenhouse gas emission detection device |
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