CN108802116A - A kind of preparation method of acetone gas sensitive material - Google Patents
A kind of preparation method of acetone gas sensitive material Download PDFInfo
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- CN108802116A CN108802116A CN201810630550.XA CN201810630550A CN108802116A CN 108802116 A CN108802116 A CN 108802116A CN 201810630550 A CN201810630550 A CN 201810630550A CN 108802116 A CN108802116 A CN 108802116A
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The present invention relates to a kind of preparation methods of acetone gas sensitive material.It carries out as follows：By the ZnFe of hollow structure2O4Ag elements or Pt elements is added in nano material, and Ag activation hollow structures ZnFe is prepared2O4Nano material or Pt activation hollow structures ZnFe2O4Nano material.A kind of Ag/Pt activation hollow structures ZnFe provided by the invention2O4Semiconductor acetone gas sensing material is simple with suitable hollow structure, higher specific surface area, and preparation method, safe, and for raw material to obtain, practical level is high.When as gas sensitive, good air-sensitive performance is shown under 175 DEG C of operating temperature, excellent selectivity is demonstrated by acetone gas, and air-sensitive detection lower limit is 0.8 ppm, and good development prospect is shown in diabetes context of detection.
Description
Technical field
The present invention relates to technical field of inorganic nano-material preparation, design a kind of preparation side of acetone gas sensitive material
Method.
Background technology
In a large amount of industrial production activities, acetone is widely used in as a kind of important organic synthesis raw material
The production of organic glass, epoxy resin, medicine, pesticide, agrochemical.Further, since acetone is also a kind of good solvent,
Also there is a large amount of application in the industrial productions such as cordite, acetate fiber.However, it is contemplated that the chemical property that acetone is active,
Boiling point only has 56.53 DEG C, volatile, inflammable, it is toxic the features such as, in industrial production activities, when acetone vapor is mixed with air
Being easy to burn simultaneously causes to explode, and there is certain danger, when use to avoid open fire and high-heat environment as possible.
Acetone can generate centainly the health of human body with certain toxicity as a kind of volatile organic compounds
Harm.When the concentration of acetone in the gas that human body is breathed is more than 300 ppm, nose and eyes can be felt to stimulate, if concentration
When reaching 2000 ppm, acetone can generate anesthetic effect to the nerve center of human body, and it is bad existing dizziness, vomiting, nausea etc. occur
As.For a long time even death is can result in the excessively high environment of acetone concentration.
In addition, in medicine, acetone gas is also considered for the gas marker of diabetes.Diabetes are one kind by pancreas islet
Hypofunction or forfeiture and a kind of metabolic syndrome caused.Acetone is the special centre that body fat mass in human body acid decomposes in liver
Product.Under normal circumstances, micro acetone is only existed in human blood circulation, can largely be converted into C2, C3 compound,.But it is right
In diabetic, they have the case where can not efficiently using blood glucose and occur in vivo, and fat is largely decomposed for energizing, and is led
Content of acetone increase in blood in human body is caused, so that content of acetone rises in the gas of characteristics of contaminated respiratory droplets.Studies have shown that Healthy People
Exhaled gas in acetone concentration between 0.3-0.9 ppm, and in diabetic's exhaled gas acetone concentration be higher than 1.8
ppm。
In recent decades, metal oxide semiconductor is due to its outstanding physical and chemical properties, and relative to tradition
Gas detecting instrument, the gas-sensitive sensing element for preparing is small, price is low, the advantages such as simple in structure, easy of integration, in danger
Gas alarm and health detection field are largely paid close attention to.And it is had been achieved for largely by the research of certain time
Achievement, such as to ZnO, SnO2、WO3、α-Fe2O3、α-Ag2WO4、ZnFe2O4Deng research.But numerous studies show that binary is partly led
Body metal oxide（ZnO etc.）Gas sensor is poor to the selectivity of target detection gas.And relative to binary semiconductor gold
Belong to oxide, polynary metal oxide semiconductor（ZnFe2O4Deng）Relatively good selectivity then is shown to object gas.
ZnFe2O4As a kind of semiconductor material of composite metal oxide of spinel structure, mainly in catalysis material, biomedicine
It is widely studied and is applied in terms of material, magnetic memory materials.Due to narrow energy gap（1.9 ev）, in recent years, in gas
Quick sensory field is largely favored, especially its selectivity outstanding to object gas.
Currently, for ZnFe2O4Semiconductor acetone gas sensing material has been widely studied.Wherein study of the Song Dynasty will etc.（Patent
Numbers 201710699953.5）Metal-organic presoma is prepared using solvent-thermal method, passes through high-temperature calcination later and obtains ZnFe2O4
Nano material.Prepare ZnFe2O4The method green non-pollution of nano material, the nano material of acquisition is under 120 DEG C of operating temperature
9.7 are reached to the acetone gas response sensitivity of 20 ppm, the acetone gas response to 50 ppm is 20.5.To other gases
（Methanol, formaldehyde, ethyl alcohol and isopropanol）Also there is certain response, it is poor to the selectivity of object gas.And it is to acetone gas
Monitoring lower-cut be 5 ppm.Wang Gang etc.（The patent No. 201611237945.0）Propyl alcohol iron is prepared using hydro-thermal method and propanol zinc is received
The solid micron ball presoma of rice piece assembling, then use calcination method obtain zinc ferrite nanometer sheet assemble hollow micron ball as lithium from
Sub- cell negative electrode material.
Invention content
It is an object of the invention to overcome above-mentioned ZnFe2O4Nano material grinds the defect of the poor selectivity of acetone gas
Make a kind of Ag/Pt activation hollow structures ZnFe to acetone gas with excellent selectivity2O4Semiconductor acetone gas sensing material
Preparation method.
Another object of the present invention is to overcome above-mentioned ZnFe2O4Nano material is low to the Monitoring lower-cut of acetone gas to be lacked
It falls into, develops a kind of to low concentration（0.8 ppm）Acetone gas has the Ag/Pt activation hollow structures ZnFe of superior sensitivity2O4Half
The preparation method of conductor acetone gas sensing material.
Third object of the present invention is by Ag and Pt to hollow structure ZnFe2O4The activation of nano material improves
ZnFe2O4A kind of Ag/Pt activation to acetone gas with superior sensitivity is developed in sensitivity of the nano material to acetone gas
Hollow structure ZnFe2O4The preparation method of semiconductor acetone gas sensing material.
The purpose of the present invention can be achieved through the following technical solutions：This powder carries out as follows：
By the ZnFe of hollow structure2O4Ag elements or Pt elements is added in nano material, and Ag activation hollow structures are prepared
ZnFe2O4Nano material or Pt activation hollow structures ZnFe2O4Nano material.
The Ag activation hollow structures ZnFe2O4Preparation method of nano material is：
By AgNO3Powder mull after be dissolved in deionized water, AgNO is made after supersound process3Solution takes hollow structure
ZnFe2O4Nano material powder and uniform AgNO3Solution mixes, and is kept the temperature after supersound process, obtains Ag activation hollow structures ZnFe2O4
Nano material.
The Pt activation hollow structures ZnFe2O4Preparation method of nano material is：
Weigh the ZnFe of hollow structure2O4Nano material powder is placed in deionized water, is stirred continuously to uniform suspension, respectively
Lysine solution and platinum acid chloride solution is added, NaBH is added after supersound process4Solution is stirred to react, and by reaction product centrifugation, is washed
It after washing, is dried, obtains Pt activation hollow structures ZnFe2O4Nano material.
The ZnFe of the hollow structure2O4The preparation method of nano material is：
1）Under room temperature, by Zn (CH3COO)2·2H2O、Fe(NO3)3·9H2O, the mixed solution of glycerine and isopropanol, room
After being stirred evenly under temperature, it is transferred in reaction kettle and is reacted under the conditions of certain temperature；
2）Step 1）After middle reaction is cooled to room temperature, after reaction product centrifugation, washing, it is dried, calcines, obtain hollow
Structure ZnFe2O4Nano material.
The step（1）Middle Zn (CH3COO)2·2H2O and Fe (NO3)3·9H2The amount ratio of the substance of O is 1:2, glycerine
Volume ratio with isopropanol is 4:15, Zn (CH3COO)2·2H2The ratio of O and isopropanol is 1 mM:60 mL, reaction heating temperature
Degree is 180 DEG C, and reaction time 12h, the above ratio can zoom in or out in proportion.
The step（2）The middle reaction type of cooling is natural cooling, and reaction product drying temperature is 60-80 DEG C, and the time is
10-24h, reaction product calcination temperature are 400 DEG C, time 2h.
It is 25 DEG C that temperature is ultrasonically treated in preparation method, and isothermal holding temperature is 200 DEG C, time 2h.
A concentration of 0.01 M of lysine solution in preparation method, platinum acid chloride solution a concentration of 0.0026 M, NaBH4Solution
A concentration of 0.01 M, it is 2h to be stirred to react the time, and reaction product drying temperature is 60-90 DEG C, drying time 15-30h.
The present invention has following advantageous effects compared with prior art：
A kind of Ag/Pt activation hollow structures ZnFe provided by the invention2O4Semiconductor acetone gas sensing material has suitable
Hollow structure, higher specific surface area, and preparation method are simple, safe, and for raw material to obtain, practical level is high.As gas
When quick material, good air-sensitive performance is shown under 175 DEG C of operating temperature, and excellent selection is demonstrated by acetone gas
Property, and air-sensitive detection lower limit is 0.8 ppm, and good development prospect is shown in diabetes context of detection.
Description of the drawings
Fig. 1 is that Ag prepared by embodiment 1 and embodiment 2 activates hollow structure ZnFe2O4Semiconductor acetone gas sensing material
X-ray diffractogram.
Fig. 2 is that Pt prepared by embodiment 1 and embodiment 3 activates hollow structure ZnFe2O4Semiconductor acetone gas sensing material
X-ray diffractogram
Fig. 3 is that Ag prepared by embodiment 4 activates hollow structure ZnFe2O4Semiconductor acetone gas sensor moves acetone gas
State responds recovery curve.
Fig. 4 is that Pt prepared by embodiment 4 activates hollow structure ZnFe2O4Semiconductor acetone gas sensor is to acetone gas
Dynamic response recovery curve.
Fig. 5 is the Ag activation hollow structures ZnFe that Ag contents prepared by embodiment 4 are 0.25 wt%2O4Semiconductor acetone gas
Selectivity test of the body sensor to acetone gas.
Fig. 6 is the Pt activation hollow structures ZnFe that Pt contents prepared by embodiment 4 are 1.5 wt%2O4Semiconductor acetone gas
Selectivity test of the sensor to acetone gas.
Specific implementation mode
With reference to specific embodiment, the invention will be further described, it is clear that the content described in embodiment is only
A part of content of the present invention, rather than whole embodiments.
The required chemical raw material of the present invention can be bought from market.
Embodiment 1：
Prepare hollow structure ZnFe2O4Semiconductor acetone gas sensing material：
Under room temperature, by the Zn (CH of 0.5 mM3COO)2·2H2Fe (the NO of O and 1 mM3)3·9H2O be dissolved in 8mL glycerine and
In the mixed solution of 30mL isopropanols, magnetic agitation 30min makes solution be uniformly mixed, and is then transferred to reaction product
In 50mL reaction kettles, 12h is reacted at 180 DEG C.After reacting cooled to room temperature, by reaction product alternating deionized water
It washs and centrifuges with absolute ethyl alcohol, and 80 DEG C of dry 10h in drying box.Finally obtained powder is transferred in Muffle furnace, it is empty
The lower 400 DEG C of calcinings 2h in compression ring border, heating rate is 5 DEG C/min.Hollow structure ZnFe is obtained after above-mentioned steps2O4Semiconductor third
Ketone gas sensing material.
Embodiment 2：
Prepare Ag activation hollow structures ZnFe2O4Semiconductor acetone gas sensing material：
Under room temperature, by the Zn (CH of 1 mM3COO)2·2H2Fe (the NO of O and 2 mM3)3·9H2O is dissolved in 16 mL glycerine and 60
In the mixed solution of mL isopropanols, magnetic agitation 30min makes solution be uniformly mixed, and is then transferred to reaction product
In 100 mL reaction kettles, reacted at 180 DEG C after 12h after cooled to room temperature, by reaction product alternating deionized water with
Absolute ethyl alcohol centrifuges, and 60 DEG C of dryings are for 24 hours in drying box.Finally obtained powder is transferred in Muffle furnace, air environment
Lower 400 DEG C of calcinings 2h, heating rate is 5 DEG C/min, obtains hollow structure ZnFe2O4Nano material.Weigh 0.01663 g's
AgNO3It is dissolved in after powder mull in 5mL deionized waters, 30min is ultrasonically treated at 25 DEG C.Then weigh 0.5 respectively, 0.25,
The uniform AgNO of 0.125 and 0.05mL3Solution and a certain amount of deionized water be configured to 5 mL concentration be respectively 0.002,0.001,
The AgNO of 0.0005 and 0.0002 mol/L3Solution.The ZnFe for taking 0.1g to prepare2O4Solid powder is uniform with 4 groups of various concentrations
AgNO3Solution mixes, and after being ultrasonically treated 30min, is placed in drying box the isothermal holding 2h at 200 DEG C, you can obtains Ag contents
The Ag activation hollow structures ZnFe of respectively 1,0.5,0.25 and 0.1wt%2O4Semiconductor acetone air-sensitive material.
Embodiment 3：
Prepare Pt activation hollow structures ZnFe2O4Semiconductor acetone gas sensing material：
Under room temperature, by the Zn (CH of 1 mM3COO)2·2H2Fe (the NO of O and 2 mM3)3·9H2O is dissolved in 16 mL glycerine and 60
In the mixed solution of mL isopropanols, magnetic agitation 30min makes solution be uniformly mixed, and is then transferred to reaction product
In 100 mL reaction kettles, reacted at 180 DEG C after 12h after cooled to room temperature, by reaction product alternating deionized water with
Absolute ethyl alcohol centrifuges, and 60 DEG C of dryings are for 24 hours in drying box.Finally obtained powder is transferred in Muffle furnace, air environment
Lower 400 DEG C of calcinings 2h, heating rate is 5 DEG C/min, obtains hollow structure ZnFe2O4Nano material.Weighing 0.03042,
ZnFe prepared by 0.01014 and 0.006084 g2O4Solid powder is placed in 10mL deionized waters, is stirred continuously equal to suspension
It is even, it is then separately added into the platinum acid chloride solution of the lysine solution and a concentration of 0.0026M of 0.3 mL of a concentration of 0.01 M of 5 mL,
After being ultrasonically treated 30min, the NaBH of a concentration of 0.01 M of 5 mL is added4Solution is stirred to react 2h, and reaction product is alternately spent
After ionized water and absolute ethyl alcohol centrifugation, washing, be placed in drying box at 80 DEG C dry 15h, obtain Pt contents be respectively 0.5,
The Pt activation hollow structures ZnFe of 1.5 and 2.5wt%2O4Semiconductor nitrogen dioxide gas sensitive.
Embodiment 4：
Ag/Pt activates hollow structure ZnFe2O4Material air-sensitive performance is tested：
By the ZnFe of preparation2O4The ZnFe that solid powder, Ag are activated2O4The ZnFe of solid powder and Pt activation2O4Solid powder is ground
It is mixed to form uniform muddy mixture after mill with deionized water or alcohol respectively, is then coated to sensor gold electrode table
Face forms gas sensing layer.It is subsequently placed in drying box at 100 DEG C dry 10h, obtains acetone gas sensor.By the biography of preparation
Sensor is powered 12h under 300 mA electric currents, is then installed on air-sensitive test equipment, carries out acetone gas sensing testing.Pass through
The variation for calculating its resistance value under different atmosphere and different temperatures obtains its optimum working temperature and to the sensitive of acetone gas
Degree and selectivity.
Claims (8)
1. a kind of preparation method of acetone gas sensitive material, which is characterized in that carry out as follows：
By the ZnFe of hollow structure2O4Ag elements or Pt elements is added in nano material, and Ag activation hollow structures are prepared
ZnFe2O4Nano material or Pt activation hollow structures ZnFe2O4Nano material.
2. a kind of preparation method of acetone gas sensitive material according to claim 1, which is characterized in that the Ag activation
Hollow structure ZnFe2O4Preparation method of nano material is：
By AgNO3Powder mull after be dissolved in deionized water, AgNO is made after supersound process3Solution takes hollow structure
ZnFe2O4Nano material powder and uniform AgNO3Solution mixes, and is kept the temperature after supersound process, obtains Ag activation hollow structures ZnFe2O4
Nano material.
3. a kind of preparation method of acetone gas sensitive material according to claim 1, which is characterized in that the Pt activation
Hollow structure ZnFe2O4Preparation method of nano material is：
Weigh the ZnFe of hollow structure2O4Nano material powder is placed in deionized water, is stirred continuously to uniform suspension, respectively
Lysine solution and platinum acid chloride solution is added, NaBH is added after supersound process4Solution is stirred to react, and by reaction product centrifugation, is washed
It after washing, is dried, obtains Pt activation hollow structures ZnFe2O4Nano material.
4. a kind of preparation method of acetone gas sensitive material according to claim 1, which is characterized in that the hollow knot
The ZnFe of structure2O4The preparation method of nano material is：
1）Under room temperature, by Zn (CH3COO)2·2H2O、Fe(NO3)3·9H2O, the mixed solution of glycerine and isopropanol, room
After being stirred evenly under temperature, it is transferred in reaction kettle and is reacted under the conditions of certain temperature；
2）Step 1）After middle reaction is cooled to room temperature, after reaction product centrifugation, washing, it is dried, calcines, obtain hollow
Structure ZnFe2O4Nano material.
5. a kind of preparation method of acetone gas sensitive material according to claim 4, which is characterized in that the step
（1）Middle Zn (CH3COO)2·2H2O and Fe (NO3)3·9H2The amount ratio of the substance of O is 1:2, the volume ratio of glycerine and isopropanol
To be 4:15, Zn (CH3COO)2·2H2The ratio of O and isopropanol is 1 mM:60 mL, reaction heating temperature is 180 DEG C, when reaction
Between be 12h, the above ratio can zoom in or out in proportion.
6. a kind of preparation method of acetone gas sensitive material according to claim 4, which is characterized in that the step
（2）The middle reaction type of cooling is natural cooling, and reaction product drying temperature is 60-80 DEG C, and time 10-24h, reaction product is forged
It is 400 DEG C to burn temperature, time 2h.
7. a kind of preparation method of acetone gas sensitive material according to claim 2, which is characterized in that in preparation method
It is 25 DEG C to be ultrasonically treated temperature, and isothermal holding temperature is 200 DEG C, time 2h.
8. a kind of preparation method of acetone gas sensitive material according to claim 3, which is characterized in that in preparation method
A concentration of 0.01 M of lysine solution, platinum acid chloride solution a concentration of 0.0026 M, NaBH4Solution concentration is 0.01 M, stirring
Reaction time is 2h, and reaction product drying temperature is 60-90 DEG C, drying time 15-30h.
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Cited By (2)
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| CN111153438A (en) * | 2020-01-03 | 2020-05-15 | 济南大学 | ZnMn2O4 hollow rod and preparation method and application thereof |
| CN111484084A (en) * | 2020-04-02 | 2020-08-04 | 扬州大学 | Acetone gas-sensitive material and preparation method thereof |
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Application publication date: 20181113 |