CN105842289A - Metal oxide gas-sensitive sensing substrate material and preparation method thereof - Google Patents
Metal oxide gas-sensitive sensing substrate material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a metal oxide gas-sensitive sensing substrate material and a preparation method thereof. The metal oxide gas-sensitive sensing substrate material is prepared by the following steps: firstly, mixing sulfuric acid and hydrogen peroxide evenly, and carrying out ultrasonic cleaning of a silicon slice; mixing sodium hydroxide and deionized water and dissolving, and carrying out ultrasonic cleaning of the silicon slice; mixing hydrofluoric acid and deionized water evenly, and carrying out ultrasonic cleaning of the silicon slice; putting the silicon slice into acetone, and carrying out ultrasonic cleaning; then putting the silicon slice into absolute ethyl alcohol, and carrying out ultrasonic cleaning; next mixing hydrofluoric acid and N,N-dimethylformamide evenly, pouring the mixture into a corrosion tank, inserting the silicon slice into the corrosion tank, and corroding; and finally mixing and dispersing an iron powder, a tellurium powder, nano silica, butylated hydroxyanisole and calcium oxide evenly, flatly laying the mixture in a crucible, inserting two ceramic slices with the height of 2 mm, placing the porous silicon slice on the ceramic slices, sealing the crucible, putting the crucible into a muffle furnace, and calcining. The sensitivity of the metal oxide gas-sensitive sensing substrate material is increased along with increase of the gas concentration; and the sensitivity is high, and the reutilization stability is good.
Description
Technical field
The present invention relates to Material Field, be specifically related to a kind of metal-oxide gas sensing matrix material and preparation method thereof.
Background technology
Along with economic fast development, the living standard of people have also been obtained the biggest raising, meanwhile, serious destruction has also been suffered in our living environment, especially our atmospheric environment, toxic and harmful is constantly discharged, and nitrogen oxides is exactly the most serious one.It can cause the respiratory system disease of the mankind, increases the weight of the state of an illness such as asthma and heart disease, even can cause death.Therefore, in order to effectively detect the gaseous environment of our life, need to research and develop a kind of gas sensor that can detect nitrogen oxides the most in time.Gas sensor refers to according to certain rule, tested gas concentration and composition are converted into device or the device of usable output signal.Wherein, nano-metal-oxide gas sensor has obtained paying close attention to widely owing to having low in energy consumption and performance advantages of higher, but there is also different shortcomings, and such as poor selectivity, operating temperature is higher, response regeneration rate is slow and the shortcoming such as baseline electrical resistance drift.Dimension, the performance constantly being improved metal-oxide gas sensitive by research has become numerous enterprises and the target of researcher joint research.
Summary of the invention
Solve the technical problem that:It is an object of the invention to provide a kind of metal-oxide gas sensing matrix material, porosity is about 40%, and its sensitivity increases along with the increase of gas concentration, the highly sensitive and good stability of recycling.
Technical scheme:A kind of metal-oxide gas sensing matrix material, it is prepared from weight portion by following component: iron powder 5-10 part, tellurium powder 5-10 part, nano silicon 1-2 part, silicon chip 10-20 part, DMF 20-30 part, Fluohydric acid. 20-30 part, Butylated hydroxyanisole 0.1-0.3 part, calcium oxide 1-2 part, sodium hydroxide 1-2 part, dehydrated alcohol 20-30 part, sulphuric acid 15-30 part, hydrogen peroxide 5-10 part, acetone 20-30 part, deionized water 30-50 part.
Further preferred, described a kind of metal-oxide gas sensing matrix material, it is prepared from weight portion by following component: iron powder 6-9 part, tellurium powder 6-9 part, nano silicon 1.2-1.8 part, silicon chip 12-18 part, DMF 22-28 part, Fluohydric acid. 22-28 part, Butylated hydroxyanisole 0.15-0.25 part, calcium oxide 1.3-1.7 part, sodium hydroxide 1.2-1.7 part, dehydrated alcohol 22-28 part, sulphuric acid 20-25 part, hydrogen peroxide 6-9 part, acetone 22-27 part, deionized water 35-45 part.
The preparation method of above-mentioned metal-oxide gas sensing matrix material comprises the following steps:
Step 1: by sulphuric acid and hydrogen peroxide mix homogeneously, silicon chip is put into wherein ultrasonic cleaning 30-40 minute；
Step 2: by sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon chip is put into wherein ultrasonic cleaning 5-10 minute；
Step 3: by 10-20 part Fluohydric acid. and residue deionized water mixing, silicon chip is put into wherein ultrasonic cleaning 30-40 minute；
Step 4: silicon chip is put into ultrasonic cleaning 5-10 minute in acetone, places into ultrasonic cleaning 5-10 minute in dehydrated alcohol；
Step 5: mixed homogeneously with DMF by remaining Fluohydric acid., pours in etching tank, is inserted in etching tank by silicon chip and corrodes, and electric current is 60-65mA, and etching time is 5-10 minute；
Step 6: remaining ingredient mixing be uniformly dispersed, be laid in crucible, inserts two panels 2mm height potsherd, and porous silicon chip is placed on it, and sealed crucible is put into and calcined in Muffle furnace and get final product, and calcining heat is 380-420 DEG C, and calcination time is 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 minute in step 2.
It is further preferred that scavenging period is 35 minutes in step 3.
It is further preferred that in acetone, scavenging period is 6-9 minute in step 4, in ethanol, scavenging period is 6-9 minute.
It is further preferred that electric current is 61-64mA in step 5, etching time is 6-9 minute.
It is further preferred that calcining heat is 390-410 DEG C in step 6, calcination time is 2.5 hours.
Beneficial effect:The porosity of the metal-oxide gas sensing matrix material of the present invention is about 40%, and its sensitivity increases along with the increase of gas concentration, works as NO2Gas concentration is when 10ppm, and its sensitivity reaches as high as 3.23, and the stability simultaneously reused is fine.
Detailed description of the invention
Embodiment 1
A kind of metal-oxide gas sensing matrix material, it is prepared from weight portion by following component: iron powder 5 parts, 5 parts of tellurium powder, nano silicon 1 part, silicon chip 10 parts, DMF 20 parts, Fluohydric acid. 20 parts, Butylated hydroxyanisole 0.1 part, calcium oxide 1 part, sodium hydroxide 1 part, dehydrated alcohol 20 parts, 15 parts of sulphuric acid, hydrogen peroxide 5 parts, 20 parts of acetone, deionized water 30 parts.
The preparation method of above-mentioned metal-oxide gas sensing matrix material is: first by sulphuric acid and hydrogen peroxide mix homogeneously, silicon chip is put into wherein ultrasonic cleaning 30 minutes；By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon chip is put into wherein ultrasonic cleaning 5 minutes；By 10 parts of Fluohydric acid .s and residue deionized water mixing, silicon chip is put into wherein ultrasonic cleaning 30 minutes, silicon chip is put into ultrasonic cleaning 5 minutes in acetone again, place into ultrasonic cleaning 5 minutes in dehydrated alcohol, then by remaining Fluohydric acid. and N, dinethylformamide mix homogeneously, pour in etching tank, silicon chip is inserted in etching tank and corrodes, electric current is 60mA, etching time is 5 minutes, finally remaining ingredient mixing is uniformly dispersed, it is laid in crucible, insert two panels 2mm height potsherd, porous silicon chip is placed on it, sealed crucible, put into and Muffle furnace is calcined and get final product, calcining heat is 380 DEG C, calcination time is 2 hours.
Embodiment 2
A kind of metal-oxide gas sensing matrix material, it is prepared from weight portion by following component: iron powder 6 parts, 6 parts of tellurium powder, nano silicon 1.2 parts, silicon chip 12 parts, DMF 22 parts, Fluohydric acid. 22 parts, Butylated hydroxyanisole 0.15 part, calcium oxide 1.3 parts, sodium hydroxide 1.2 parts, dehydrated alcohol 22 parts, 20 parts of sulphuric acid, hydrogen peroxide 6 parts, 22 parts of acetone, deionized water 35 parts.
The preparation method of above-mentioned metal-oxide gas sensing matrix material is: first by sulphuric acid and hydrogen peroxide mix homogeneously, silicon chip is put into wherein ultrasonic cleaning 35 minutes；By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon chip is put into wherein ultrasonic cleaning 6 minutes；By 15 parts of Fluohydric acid .s and residue deionized water mixing, silicon chip is put into wherein ultrasonic cleaning 35 minutes, silicon chip is put into ultrasonic cleaning 6 minutes in acetone again, place into ultrasonic cleaning 6 minutes in dehydrated alcohol, then by remaining Fluohydric acid. and N, dinethylformamide mix homogeneously, pour in etching tank, silicon chip is inserted in etching tank and corrodes, electric current is 61mA, etching time is 6 minutes, finally remaining ingredient mixing is uniformly dispersed, it is laid in crucible, insert two panels 2mm height potsherd, porous silicon chip is placed on it, sealed crucible, put into and Muffle furnace is calcined and get final product, calcining heat is 390 DEG C, calcination time is 2.5 hours.
Embodiment 3
A kind of metal-oxide gas sensing matrix material, it is prepared from weight portion by following component: iron powder 7.5 parts, 7.5 parts of tellurium powder, nano silicon 1.5 parts, silicon chip 15 parts, DMF 25 parts, Fluohydric acid. 25 parts, Butylated hydroxyanisole 0.2 part, calcium oxide 1.5 parts, sodium hydroxide 1.5 parts, dehydrated alcohol 25 parts, 22 parts of sulphuric acid, hydrogen peroxide 7.5 parts, 25 parts of acetone, deionized water 40 parts.
The preparation method of above-mentioned metal-oxide gas sensing matrix material is: first by sulphuric acid and hydrogen peroxide mix homogeneously, silicon chip is put into wherein ultrasonic cleaning 35 minutes；By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon chip is put into wherein ultrasonic cleaning 7.5 minutes；By 15 parts of Fluohydric acid .s and residue deionized water mixing, silicon chip is put into wherein ultrasonic cleaning 35 minutes, silicon chip is put into ultrasonic cleaning 7.5 minutes in acetone again, place into ultrasonic cleaning 7.5 minutes in dehydrated alcohol, then by remaining Fluohydric acid. and N, dinethylformamide mix homogeneously, pour in etching tank, silicon chip is inserted in etching tank and corrodes, electric current is 63mA, etching time is 7.5 minutes, finally remaining ingredient mixing is uniformly dispersed, it is laid in crucible, insert two panels 2mm height potsherd, porous silicon chip is placed on it, sealed crucible, put into and Muffle furnace is calcined and get final product, calcining heat is 400 DEG C, calcination time is 2.5 hours.
Embodiment 4
A kind of metal-oxide gas sensing matrix material, it is prepared from weight portion by following component: iron powder 9 parts, 9 parts of tellurium powder, nano silicon 1.8 parts, silicon chip 18 parts, DMF 28 parts, Fluohydric acid. 28 parts, Butylated hydroxyanisole 0.25 part, calcium oxide 1.7 parts, sodium hydroxide 1.7 parts, dehydrated alcohol 28 parts, 25 parts of sulphuric acid, hydrogen peroxide 9 parts, 27 parts of acetone, deionized water 45 parts.
The preparation method of above-mentioned metal-oxide gas sensing matrix material is: first by sulphuric acid and hydrogen peroxide mix homogeneously, silicon chip is put into wherein ultrasonic cleaning 35 minutes；By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon chip is put into wherein ultrasonic cleaning 9 minutes；By 15 parts of Fluohydric acid .s and residue deionized water mixing, silicon chip is put into wherein ultrasonic cleaning 35 minutes, silicon chip is put into ultrasonic cleaning 9 minutes in acetone again, place into ultrasonic cleaning 9 minutes in dehydrated alcohol, then by remaining Fluohydric acid. and N, dinethylformamide mix homogeneously, pour in etching tank, silicon chip is inserted in etching tank and corrodes, electric current is 64mA, etching time is 9 minutes, finally remaining ingredient mixing is uniformly dispersed, it is laid in crucible, insert two panels 2mm height potsherd, porous silicon chip is placed on it, sealed crucible, put into and Muffle furnace is calcined and get final product, calcining heat is 410 DEG C, calcination time is 2.5 hours.
Embodiment 5
A kind of metal-oxide gas sensing matrix material, it is prepared from weight portion by following component: iron powder 10 parts, 10 parts of tellurium powder, nano silicon 2 parts, silicon chip 20 parts, DMF 30 parts, Fluohydric acid. 30 parts, Butylated hydroxyanisole 0.3 part, calcium oxide 2 parts, sodium hydroxide 2 parts, dehydrated alcohol 30 parts, 30 parts of sulphuric acid, hydrogen peroxide 10 parts, 30 parts of acetone, deionized water 50 parts.
The preparation method of above-mentioned metal-oxide gas sensing matrix material is: first by sulphuric acid and hydrogen peroxide mix homogeneously, silicon chip is put into wherein ultrasonic cleaning 40 minutes；By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon chip is put into wherein ultrasonic cleaning 10 minutes；By 20 parts of Fluohydric acid .s and residue deionized water mixing, silicon chip is put into wherein ultrasonic cleaning 40 minutes, silicon chip is put into ultrasonic cleaning 10 minutes in acetone again, place into ultrasonic cleaning 10 minutes in dehydrated alcohol, then by remaining Fluohydric acid. and N, dinethylformamide mix homogeneously, pour in etching tank, silicon chip is inserted in etching tank and corrodes, electric current is 65mA, etching time is 10 minutes, finally remaining ingredient mixing is uniformly dispersed, it is laid in crucible, insert two panels 2mm height potsherd, porous silicon chip is placed on it, sealed crucible, put into and Muffle furnace is calcined and get final product, calcining heat is 420 DEG C, calcination time is 3 hours.
Comparative example 1
The present embodiment is not contain iron powder with the difference of embodiment 5, replaces with tellurium powder.Specifically:
A kind of metal-oxide gas sensing matrix material, it is prepared from weight portion by following component: 20 parts of tellurium powder, nano silicon 2 parts, silicon chip 20 parts, DMF 30 parts, Fluohydric acid. 30 parts, Butylated hydroxyanisole 0.3 part, calcium oxide 2 parts, sodium hydroxide 2 parts, dehydrated alcohol 30 parts, 30 parts of sulphuric acid, hydrogen peroxide 10 parts, 30 parts of acetone, deionized water 50 parts.
The preparation method of above-mentioned metal-oxide gas sensing matrix material is: first by sulphuric acid and hydrogen peroxide mix homogeneously, silicon chip is put into wherein ultrasonic cleaning 40 minutes；By sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon chip is put into wherein ultrasonic cleaning 10 minutes；By 20 parts of Fluohydric acid .s and residue deionized water mixing, silicon chip is put into wherein ultrasonic cleaning 40 minutes, silicon chip is put into ultrasonic cleaning 10 minutes in acetone again, place into ultrasonic cleaning 10 minutes in dehydrated alcohol, then by remaining Fluohydric acid. and N, dinethylformamide mix homogeneously, pour in etching tank, silicon chip is inserted in etching tank and corrodes, electric current is 65mA, etching time is 10 minutes, finally remaining ingredient mixing is uniformly dispersed, it is laid in crucible, insert two panels 2mm height potsherd, porous silicon chip is placed on it, sealed crucible, put into and Muffle furnace is calcined and get final product, calcining heat is 420 DEG C, calcination time is 3 hours.
Comparative example 2
The present embodiment is not contain sodium hydroxide with the difference of embodiment 5.Specifically:
A kind of metal-oxide gas sensing matrix material, it is prepared from weight portion by following component: iron powder 10 parts, 10 parts of tellurium powder, nano silicon 2 parts, silicon chip 20 parts, DMF 30 parts, Fluohydric acid. 30 parts, Butylated hydroxyanisole 0.3 part, calcium oxide 2 parts, dehydrated alcohol 30 parts, 30 parts of sulphuric acid, hydrogen peroxide 10 parts, 30 parts of acetone, deionized water 20 parts.
The preparation method of above-mentioned metal-oxide gas sensing matrix material is: first by sulphuric acid and hydrogen peroxide mix homogeneously, silicon chip is put into wherein ultrasonic cleaning 40 minutes；20 parts of Fluohydric acid .s and deionized water are mixed, silicon chip is put into wherein ultrasonic cleaning 40 minutes, silicon chip is put into ultrasonic cleaning 10 minutes in acetone again, place into ultrasonic cleaning 10 minutes in dehydrated alcohol, then by remaining Fluohydric acid. and N, dinethylformamide mix homogeneously, pour in etching tank, silicon chip is inserted in etching tank and corrodes, electric current is 65mA, etching time is 10 minutes, finally remaining ingredient mixing is uniformly dispersed, it is laid in crucible, insert two panels 2mm height potsherd, porous silicon chip is placed on it, sealed crucible, put into and Muffle furnace is calcined and get final product, calcining heat is 420 DEG C, calcination time is 3 hours.
Table 1 below is the partial properties index situation of metal-oxide gas sensing matrix material, it will be seen that the porosity of material of the present invention is about 40%, its sensitivity increases along with the increase of gas concentration, works as NO2Gas concentration is when 10ppm, and its sensitivity reaches as high as 3.23, and the stability simultaneously reused is fine.
The partial properties index of table 1 metal-oxide gas sensing matrix material
| 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 (10)
1. a metal-oxide gas sensing matrix material, it is characterized in that: be prepared from weight portion by following component: iron powder 5-10 part, tellurium powder 5-10 part, nano silicon 1-2 part, silicon chip 10-20 part, DMF 20-30 part, Fluohydric acid. 20-30 part, Butylated hydroxyanisole 0.1-0.3 part, calcium oxide 1-2 part, sodium hydroxide 1-2 part, dehydrated alcohol 20-30 part, sulphuric acid 15-30 part, hydrogen peroxide 5-10 part, acetone 20-30 part, deionized water 30-50 part.
A kind of metal-oxide gas sensing matrix material the most according to claim 1, it is characterized in that: be prepared from weight portion by following component: iron powder 6-9 part, tellurium powder 6-9 part, nano silicon 1.2-1.8 part, silicon chip 12-18 part, DMF 22-28 part, Fluohydric acid. 22-28 part, Butylated hydroxyanisole 0.15-0.25 part, calcium oxide 1.3-1.7 part, sodium hydroxide 1.2-1.7 part, dehydrated alcohol 22-28 part, sulphuric acid 20-25 part, hydrogen peroxide 6-9 part, acetone 22-27 part, deionized water 35-45 part.
3. a kind of metal-oxide gas sensing matrix material as claimed in claim 1, it is characterised in that: described silicon chip is single-sided polishing, a diameter of 50mm, and thickness is 300 μm.
4. the preparation method of a kind of metal-oxide gas sensing matrix material described in any one of claim 1 to 2, it is characterised in that: comprise the following steps:
Step 1: by sulphuric acid and hydrogen peroxide mix homogeneously, silicon chip is put into wherein ultrasonic cleaning 30-40 minute；
Step 2: by sodium hydroxide and 20 parts of deionized water mixed dissolutions, silicon chip is put into wherein ultrasonic cleaning 5-10 minute；
Step 3: by 10-20 part Fluohydric acid. and residue deionized water mixing, silicon chip is put into wherein ultrasonic cleaning 30-40 minute；
Step 4: silicon chip is put into ultrasonic cleaning 5-10 minute in acetone, places into ultrasonic cleaning 5-10 minute in dehydrated alcohol；
Step 5: mixed homogeneously with DMF by remaining Fluohydric acid., pours in etching tank, is inserted in etching tank by silicon chip and corrodes, and electric current is 60-65mA, and etching time is 5-10 minute；
Step 6: remaining ingredient mixing be uniformly dispersed, be laid in crucible, inserts two panels 2mm height potsherd, and porous silicon chip is placed on it, and sealed crucible is put into and calcined in Muffle furnace and get final product, and calcining heat is 380-420 DEG C, and calcination time is 2-3 hour.
The preparation method of a kind of metal-oxide gas sensing matrix material the most according to claim 4, it is characterised in that: in described step 1, scavenging period is 35 minutes.
The preparation method of a kind of metal-oxide gas sensing matrix material the most according to claim 4, it is characterised in that: in described step 2, scavenging period is 6-9 minute.
The preparation method of a kind of metal-oxide gas sensing matrix material the most according to claim 4, it is characterised in that: in described step 3, scavenging period is 35 minutes.
The preparation method of a kind of metal-oxide gas sensing matrix material the most according to claim 4, it is characterised in that: in described step 4, in acetone, scavenging period is 6-9 minute, and in ethanol, scavenging period is 6-9 minute.
The preparation method of a kind of metal-oxide gas sensing matrix material the most according to claim 4, it is characterised in that: in described step 5, electric current is 61-64mA, and etching time is 6-9 minute.
The preparation method of a kind of metal-oxide gas sensing matrix material the most according to claim 4, it is characterised in that: in described step 6, calcining heat is 390-410 DEG C, and calcination time is 2.5 hours.
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Cited By (1)
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| CN110993739A (en) * | 2019-12-13 | 2020-04-10 | 陕西易莱德新材料科技有限公司 | Production method of membrane electrode for solar cell |
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| CN102574111A (en) * | 2009-10-09 | 2012-07-11 | 大野绿水株式会社 | Process for production of composite oxide catalyst |
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