CN105842289B - A kind of metal oxide gas sensing basis material and preparation method thereof - Google Patents
A kind of metal oxide gas sensing basis material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of metal oxide gas sensing basis materials and preparation method thereof.It is prepared from the following steps:First sulfuric acid and hydrogen peroxide are uniformly mixed, are cleaned by ultrasonic silicon wafer;By sodium hydroxide and deionized water mixed dissolution, it is cleaned by ultrasonic silicon wafer;Hydrofluoric acid and deionized water are mixed, it is cleaned by ultrasonic silicon wafer, silicon wafer is put into acetone and is cleaned by ultrasonic, it places into dehydrated alcohol and is cleaned by ultrasonic, then by hydrofluoric acid and N, dinethylformamide is uniformly mixed, it pours into etching tank, silicon wafer is inserted into etching tank and is corroded, finally iron powder, tellurium powder, nano silica, butylated hydroxy anisole and calcium oxide are mixed and are uniformly dispersed, is laid in crucible, it is inserted into two panels 2mm high potsherd, porous silicon chip is placed on it, and sealed crucible is put into Muffle furnace and calcines to obtain the final product.The sensitivity of metal oxide gas sensing basis material of the invention increases with the increase of gas concentration, and the stability of high sensitivity and recycling is good.
Description
Technical field
The present invention relates to Material Fields, and in particular to a kind of metal oxide gas sensing basis material and its preparation side
Method.
Background technique
With the rapid development of economy, people's lives level is also greatly improved, and at the same time, our life
Environment living is also by serious destruction, and especially our atmospheric environment, toxic and harmful gas are constantly discharged, nitrogen oxidation
Object is exactly wherein more serious one kind.It can cause the respiratory disease of the mankind, aggravate the state of an illness such as asthma and heart disease, very
To death can be caused.Therefore, in order to which the gaseous environment that we live is effectively detected, needing to research and develop one kind can have
Effect detects the gas sensor of nitrogen oxides in time.Gas sensor refers to can be by tested gas concentration and ingredient according to one
Set pattern rule is converted into the device or device of usable output signal.Wherein, nano-metal-oxide gas sensor is due to function
It consumes the advantages that low and performance is high and has obtained extensive concern, but there is also different disadvantages, such as poor selectivity, operating temperature
The disadvantages of higher, response regeneration rate is slowly and baseline electrical resistance is drifted about.Dimension constantly improves metal oxide air-sensitive material by studying
The performance of material has become the target studied jointly for numerous enterprises and researcher.
Summary of the invention
Technical problems to be solved:The object of the present invention is to provide a kind of metal oxide gas sensing basis material, holes
40% or so, sensitivity increases gap rate with the increase of gas concentration, and the stability of high sensitivity and recycling is good.
Technical solution:A kind of metal oxide gas sensing basis material is prepared by following component with parts by weight:Iron
5-10 parts of powder, 5-10 parts of tellurium powder, 1-2 parts of nano silica, 10-20 parts of silicon wafer, 20-30 parts of N,N-dimethylformamide, hydrogen
20-30 parts of fluoric acid, 0.1-0.3 parts of butylated hydroxy anisole, 1-2 parts of calcium oxide, 1-2 parts of sodium hydroxide, dehydrated alcohol 20-30
Part, 15-30 parts of sulfuric acid, 5-10 parts of hydrogen peroxide, 20-30 parts of acetone, 30-50 parts of deionized water.
It is further preferred that a kind of metal oxide gas sensing basis material, by following component with parts by weight
It is prepared:6-9 parts of iron powder, 6-9 parts of tellurium powder, 1.2-1.8 parts of nano silica, 12-18 parts of silicon wafer, N, N- dimethyl formyl
22-28 parts of amine, 22-28 parts of hydrofluoric acid, 0.15-0.25 parts of butylated hydroxy anisole, 1.3-1.7 parts of calcium oxide, sodium hydroxide
1.2-1.7 parts, 22-28 parts of dehydrated alcohol, 20-25 parts of sulfuric acid, 6-9 parts of hydrogen peroxide, 22-27 parts of acetone, deionized water 35-45
Part.
The preparation method of above-mentioned metal oxide gas sensing basis material includes the following steps:
Step 1:Sulfuric acid and hydrogen peroxide are uniformly mixed, silicon wafer is put into and is wherein cleaned by ultrasonic 30-40 minutes;
Step 2:By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon wafer is put into wherein 5-10 points of ultrasonic cleaning
Clock;
Step 3:10-20 parts of hydrofluoric acid and remaining deionized water are mixed, silicon wafer is put into wherein 30-40 points of ultrasonic cleaning
Clock;
Step 4:Silicon wafer is put into acetone and is cleaned by ultrasonic 5-10 minutes, places into and is cleaned by ultrasonic 5-10 points in dehydrated alcohol
Clock;
Step 5:Remaining hydrofluoric acid is uniformly mixed with n,N-Dimethylformamide, pours into etching tank, silicon wafer is inserted
Enter in etching tank and corroded, electric current 60-65mA, etching time is 5-10 minutes;
Step 6:Remaining ingredient is mixed and is uniformly dispersed, is laid in crucible, two panels 2mm high potsherd is inserted into, it will be porous
Silicon wafer is placed on it, sealed crucible, is put into Muffle furnace and calcines to obtain the final product, and calcination temperature is 380-420 DEG C, calcination time 2-3
Hour.
It is further preferred that scavenging period is 35 minutes in step 1.
It is further preferred that scavenging period is 6-9 minutes in step 2.
It is further preferred that scavenging period is 35 minutes in step 3.
It is further preferred that scavenging period is 6-9 minutes in acetone in step 4, scavenging period is 6-9 minutes in ethyl alcohol.
It is further preferred that electric current is 61-64mA in step 5, etching time is 6-9 minutes.
It is further preferred that calcination temperature is 390-410 DEG C in step 6, calcination time is 2.5 hours.
Beneficial effect:The porosity of metal oxide gas sensing basis material of the invention is 40% or so, sensitivity
Increase with the increase of gas concentration, works as NO2For gas concentration in 10ppm, sensitivity reaches as high as 3.23, repeats simultaneously
The stability utilized is fine.
Specific embodiment
Embodiment 1
A kind of metal oxide gas sensing basis material is prepared by following component with parts by weight:5 parts of iron powder, tellurium
5 parts of powder, 1 part of nano silica, 10 parts of silicon wafer, 20 parts of N,N-dimethylformamide, 20 parts of hydrofluoric acid, butylated hydroxy anisole
0.1 part, 1 part of calcium oxide, 1 part of sodium hydroxide, 20 parts of dehydrated alcohol, 15 parts of sulfuric acid, 5 parts of hydrogen peroxide, 20 parts of acetone, deionization
30 parts of water.
The preparation method of above-mentioned metal oxide gas sensing basis material is:First sulfuric acid and hydrogen peroxide are mixed equal
It is even, silicon wafer is put into and is wherein cleaned by ultrasonic 30 minutes;By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon wafer is put into it
Middle ultrasonic cleaning 5 minutes;10 parts of hydrofluoric acid and remaining deionized water are mixed, silicon wafer is put into and is wherein cleaned by ultrasonic 30 minutes,
Silicon wafer is put into acetone again and is cleaned by ultrasonic 5 minutes, places into dehydrated alcohol and is cleaned by ultrasonic 5 minutes, then by remaining hydrogen
Fluoric acid is uniformly mixed with n,N-Dimethylformamide, is poured into etching tank, and silicon wafer is inserted into etching tank and is corroded, electric current is
60mA, etching time are 5 minutes, finally mix remaining ingredient and are uniformly dispersed, be laid in crucible, are inserted into two panels 2mm Gao Tao
Tile, porous silicon chip is placed on it, sealed crucible are put into Muffle furnace and calcine to obtain the final product, and calcination temperature is 380 DEG C, when calcining
Between be 2 hours.
Embodiment 2
A kind of metal oxide gas sensing basis material is prepared by following component with parts by weight:6 parts of iron powder, tellurium
6 parts of powder, 1.2 parts of nano silica, 12 parts of silicon wafer, 22 parts of N,N-dimethylformamide, 22 parts of hydrofluoric acid, butylhydroxy fennel
0.15 part of ether, 1.3 parts of calcium oxide, 1.2 parts of sodium hydroxide, 22 parts of dehydrated alcohol, 20 parts of sulfuric acid, 6 parts of hydrogen peroxide, acetone 22
Part, 35 parts of deionized water.
The preparation method of above-mentioned metal oxide gas sensing basis material is:First sulfuric acid and hydrogen peroxide are mixed equal
It is even, silicon wafer is put into and is wherein cleaned by ultrasonic 35 minutes;By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon wafer is put into it
Middle ultrasonic cleaning 6 minutes;15 parts of hydrofluoric acid and remaining deionized water are mixed, silicon wafer is put into and is wherein cleaned by ultrasonic 35 minutes,
Silicon wafer is put into acetone again and is cleaned by ultrasonic 6 minutes, places into dehydrated alcohol and is cleaned by ultrasonic 6 minutes, then by remaining hydrogen
Fluoric acid is uniformly mixed with n,N-Dimethylformamide, is poured into etching tank, and silicon wafer is inserted into etching tank and is corroded, electric current is
61mA, etching time are 6 minutes, finally mix remaining ingredient and are uniformly dispersed, be laid in crucible, are inserted into two panels 2mm Gao Tao
Tile, porous silicon chip is placed on it, sealed crucible are put into Muffle furnace and calcine to obtain the final product, and calcination temperature is 390 DEG C, when calcining
Between be 2.5 hours.
Embodiment 3
A kind of metal oxide gas sensing basis material is prepared by following component with parts by weight:7.5 parts of iron powder,
7.5 parts of tellurium powder, 1.5 parts of nano silica, 15 parts of silicon wafer, 25 parts of N,N-dimethylformamide, 25 parts of hydrofluoric acid, butylhydroxy
0.2 part of anisole, 1.5 parts of calcium oxide, 1.5 parts of sodium hydroxide, 25 parts of dehydrated alcohol, 22 parts of sulfuric acid, 7.5 parts of hydrogen peroxide, third
25 parts of ketone, 40 parts of deionized water.
The preparation method of above-mentioned metal oxide gas sensing basis material is:First sulfuric acid and hydrogen peroxide are mixed equal
It is even, silicon wafer is put into and is wherein cleaned by ultrasonic 35 minutes;By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon wafer is put into it
Middle ultrasonic cleaning 7.5 minutes;15 parts of hydrofluoric acid and remaining deionized water are mixed, silicon wafer is put into and is wherein cleaned by ultrasonic 35 points
Clock, then silicon wafer is put into acetone and is cleaned by ultrasonic 7.5 minutes, it places into dehydrated alcohol and is cleaned by ultrasonic 7.5 minutes, then will remain
Remaining hydrofluoric acid is uniformly mixed with n,N-Dimethylformamide, is poured into etching tank, and silicon wafer is inserted into etching tank and is corroded,
Electric current is 63mA, and etching time is 7.5 minutes, finally mixes remaining ingredient and is uniformly dispersed, be laid in crucible, is inserted into two panels
2mm high potsherd, porous silicon chip is placed on it, sealed crucible are put into Muffle furnace and calcine to obtain the final product, and calcination temperature is 400 DEG C,
Calcination time is 2.5 hours.
Embodiment 4
A kind of metal oxide gas sensing basis material is prepared by following component with parts by weight:9 parts of iron powder, tellurium
9 parts of powder, 1.8 parts of nano silica, 18 parts of silicon wafer, 28 parts of N,N-dimethylformamide, 28 parts of hydrofluoric acid, butylhydroxy fennel
0.25 part of ether, 1.7 parts of calcium oxide, 1.7 parts of sodium hydroxide, 28 parts of dehydrated alcohol, 25 parts of sulfuric acid, 9 parts of hydrogen peroxide, acetone 27
Part, 45 parts of deionized water.
The preparation method of above-mentioned metal oxide gas sensing basis material is:First sulfuric acid and hydrogen peroxide are mixed equal
It is even, silicon wafer is put into and is wherein cleaned by ultrasonic 35 minutes;By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon wafer is put into it
Middle ultrasonic cleaning 9 minutes;15 parts of hydrofluoric acid and remaining deionized water are mixed, silicon wafer is put into and is wherein cleaned by ultrasonic 35 minutes,
Silicon wafer is put into acetone again and is cleaned by ultrasonic 9 minutes, places into dehydrated alcohol and is cleaned by ultrasonic 9 minutes, then by remaining hydrogen
Fluoric acid is uniformly mixed with n,N-Dimethylformamide, is poured into etching tank, and silicon wafer is inserted into etching tank and is corroded, electric current is
64mA, etching time are 9 minutes, finally mix remaining ingredient and are uniformly dispersed, be laid in crucible, are inserted into two panels 2mm Gao Tao
Tile, porous silicon chip is placed on it, sealed crucible are put into Muffle furnace and calcine to obtain the final product, and calcination temperature is 410 DEG C, when calcining
Between be 2.5 hours.
Embodiment 5
A kind of metal oxide gas sensing basis material is prepared by following component with parts by weight:10 parts of iron powder, tellurium
10 parts of powder, 2 parts of nano silica, 20 parts of silicon wafer, 30 parts of N,N-dimethylformamide, 30 parts of hydrofluoric acid, butylhydroxy fennel
0.3 part of ether, 2 parts of sodium hydroxide, 30 parts of dehydrated alcohol, 30 parts of sulfuric acid, 10 parts of hydrogen peroxide, 30 parts of acetone, is gone 2 parts of calcium oxide
50 parts of ionized water.
The preparation method of above-mentioned metal oxide gas sensing basis material is:First sulfuric acid and hydrogen peroxide are mixed equal
It is even, silicon wafer is put into and is wherein cleaned by ultrasonic 40 minutes;By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon wafer is put into it
Middle ultrasonic cleaning 10 minutes;20 parts of hydrofluoric acid and remaining deionized water are mixed, silicon wafer is put into and is wherein cleaned by ultrasonic 40 minutes,
Silicon wafer is put into acetone again and is cleaned by ultrasonic 10 minutes, places into dehydrated alcohol and is cleaned by ultrasonic 10 minutes, it then will be remaining
Hydrofluoric acid is uniformly mixed with n,N-Dimethylformamide, is poured into etching tank, and silicon wafer is inserted into etching tank and is corroded, electric current
For 65mA, etching time is 10 minutes, finally mixes remaining ingredient and is uniformly dispersed, be laid in crucible, is inserted into two panels 2mm high
Potsherd, porous silicon chip is placed on it, sealed crucible are put into Muffle furnace and calcine to obtain the final product, and calcination temperature is 420 DEG C, calcining
Time is 3 hours.
Comparative example 1
The difference of the present embodiment and embodiment 5 is without containing iron powder, with the replacement of tellurium powder.Specifically:
A kind of metal oxide gas sensing basis material is prepared by following component with parts by weight:20 parts of tellurium powder is received
Rice 2 parts of silica, 20 parts of silicon wafer, 30 parts of N,N-dimethylformamide, 30 parts of hydrofluoric acid, 0.3 part of butylated hydroxy anisole, oxygen
Change 2 parts of calcium, 2 parts of sodium hydroxide, 30 parts of dehydrated alcohol, 30 parts of sulfuric acid, 10 parts of hydrogen peroxide, 30 parts of acetone, 50 parts of deionized water.
The preparation method of above-mentioned metal oxide gas sensing basis material is:First sulfuric acid and hydrogen peroxide are mixed equal
It is even, silicon wafer is put into and is wherein cleaned by ultrasonic 40 minutes;By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon wafer is put into it
Middle ultrasonic cleaning 10 minutes;20 parts of hydrofluoric acid and remaining deionized water are mixed, silicon wafer is put into and is wherein cleaned by ultrasonic 40 minutes,
Silicon wafer is put into acetone again and is cleaned by ultrasonic 10 minutes, places into dehydrated alcohol and is cleaned by ultrasonic 10 minutes, it then will be remaining
Hydrofluoric acid is uniformly mixed with n,N-Dimethylformamide, is poured into etching tank, and silicon wafer is inserted into etching tank and is corroded, electric current
For 65mA, etching time is 10 minutes, finally mixes remaining ingredient and is uniformly dispersed, be laid in crucible, is inserted into two panels 2mm high
Potsherd, porous silicon chip is placed on it, sealed crucible are put into Muffle furnace and calcine to obtain the final product, and calcination temperature is 420 DEG C, calcining
Time is 3 hours.
Comparative example 2
The difference of the present embodiment and embodiment 5 is without containing sodium hydroxide.Specifically:
A kind of metal oxide gas sensing basis material is prepared by following component with parts by weight:10 parts of iron powder, tellurium
10 parts of powder, 2 parts of nano silica, 20 parts of silicon wafer, 30 parts of N,N-dimethylformamide, 30 parts of hydrofluoric acid, butylhydroxy fennel
0.3 part of ether, 2 parts of calcium oxide, 30 parts of dehydrated alcohol, 30 parts of sulfuric acid, 10 parts of hydrogen peroxide, 30 parts of acetone, 20 parts of deionized water.
The preparation method of above-mentioned metal oxide gas sensing basis material is:First sulfuric acid and hydrogen peroxide are mixed equal
It is even, silicon wafer is put into and is wherein cleaned by ultrasonic 40 minutes;20 parts of hydrofluoric acid and deionized water are mixed, silicon wafer are put into wherein ultrasonic
Cleaning 40 minutes, then silicon wafer is put into acetone and is cleaned by ultrasonic 10 minutes, is placed into and is cleaned by ultrasonic 10 minutes in dehydrated alcohol, so
Remaining hydrofluoric acid is uniformly mixed with n,N-Dimethylformamide afterwards, is poured into etching tank, by silicon wafer be inserted into etching tank in into
Row corrosion, electric current 65mA, etching time are 10 minutes, finally mix remaining ingredient and are uniformly dispersed, be laid in crucible, insert
Enter two panels 2mm high potsherd, porous silicon chip is placed on it, sealed crucible is put into Muffle furnace and calcines to obtain the final product, and calcination temperature is
420 DEG C, calcination time is 3 hours.
The following table 1 is the partial properties index situation of metal oxide gas sensing basis material, it will be seen that this hair
40% or so, sensitivity increases the porosity of bright material with the increase of gas concentration, works as NO2Gas concentration is in 10ppm
When, sensitivity reaches as high as 3.23, while the stability reused is fine.
The partial properties index of 1 metal oxide gas sensing basis material of table
Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example 1 | Comparative example 2 | |
Porosity(%) | 39.8 | 39.9 | 40.2 | 40.4 | 40.1 | 36.8 | 35.4 |
To NO2Sensitivity/10ppm | 3.16 | 3.18 | 3.19 | 3.23 | 3.21 | 3.03 | 3.11 |
Claims (3)
1. a kind of metal oxide gas sensing basis material, it is characterised in that:It is prepared by following component with parts by weight:Iron
5-10 parts of powder, 5-10 parts of tellurium powder, 1-2 parts of nano silica, 10-20 parts of silicon wafer, 20-30 parts of N,N-dimethylformamide, hydrogen
20-30 parts of fluoric acid, 0.1-0.3 parts of butylated hydroxy anisole, 1-2 parts of calcium oxide, 1-2 parts of sodium hydroxide, dehydrated alcohol 20-30
Part, 15-30 parts of sulfuric acid, 5-10 parts of hydrogen peroxide, 20-30 parts of acetone, 30-50 parts of deionized water, include the following steps:
Step 1:Sulfuric acid and hydrogen peroxide are uniformly mixed, silicon wafer is put into and is wherein cleaned by ultrasonic 30-40 minutes;
Step 2:By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon wafer is put into and is wherein cleaned by ultrasonic 5-10 minutes;
Step 3:10-20 parts of hydrofluoric acid and remaining deionized water are mixed, silicon wafer is put into and is wherein cleaned by ultrasonic 30-40 minutes;
Step 4:Silicon wafer is put into acetone and is cleaned by ultrasonic 5-10 minutes, places into dehydrated alcohol and is cleaned by ultrasonic 5-10 minutes;
Step 5:Remaining hydrofluoric acid is uniformly mixed with n,N-Dimethylformamide, is poured into etching tank, silicon wafer is inserted into rotten
Corroded in erosion slot, electric current 60-65mA, etching time is 5-10 minutes;
Step 6:Remaining ingredient is mixed and is uniformly dispersed, is laid in crucible, two panels 2mm high potsherd is inserted into, by porous silicon chip
Placed on it, sealed crucible is put into Muffle furnace and calcines to obtain the final product, and calcination temperature is 380-420 DEG C, and calcination time is 2-3 hours.
2. a kind of metal oxide gas sensing basis material according to claim 1, it is characterised in that:By following component
It is prepared with parts by weight:6-9 parts of iron powder, 6-9 parts of tellurium powder, 1.2-1.8 parts of nano silica, 12-18 parts of silicon wafer, N, N- bis-
22-28 parts of methylformamide, 22-28 parts of hydrofluoric acid, 0.15-0.25 parts of butylated hydroxy anisole, 1.3-1.7 parts of calcium oxide, hydrogen
1.2-1.7 parts of sodium oxide molybdena, 22-28 parts of dehydrated alcohol, 20-25 parts of sulfuric acid, 6-9 parts of hydrogen peroxide, 22-27 parts of acetone, deionization
35-45 parts of water.
3. a kind of metal oxide gas sensing basis material as described in claim 1, it is characterised in that:The silicon wafer is single
Face polishing, diameter 50mm, with a thickness of 300 μm.
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