CN102692437A - Gas sensitive material, carbon monoxide gas sensitive element adopting gas sensitive material and preparation method of carbon monoxide gas sensitive element - Google Patents
Gas sensitive material, carbon monoxide gas sensitive element adopting gas sensitive material and preparation method of carbon monoxide gas sensitive element Download PDFInfo
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Abstract
The invention belongs to the field of gas sensors and relates to a novel tin dioxide gas sensitive material, a gas sensitive element adopting the novel tin dioxide gas sensitive material and a preparation method of the gas sensitive element. The tin oxide gas sensitive material consists of the following substances in percentage by mass: 88 to 94 percent of tin dioxide, 1 to 5 percent of antimony trioxide, 0.5 to 5 percent of noble metal, 0.5 to 4 percent of metallic oxides and 0.5 to 4 percent of silicon dioxide. A carbon monoxide gas sensitive element adopting the tin dioxide gas sensitive material is structurally characterized in that a bottom layer is a heating body, a gas sensitive layer made of the tin dioxide gas sensitive material is covered on the heating body, the gas sensitive layer is connected with a lead wire, and a ceramic molecular sieve is covered on the gas sensitive layer. The carbon monoxide gas sensitive element adopting the tin dioxide gas sensitive material has the advantages that the sensitivity is high, the response is fast, the measuring range is wide, the size is small, the service life is long, and the cost is low.
Description
Technical field
The invention belongs to the gas sensor field; Relate to a kind of novel tin dioxide gas-sensitive material; Also relate to the resistance-type semiconductor gas sensor that is used for the test gas carbonomonoxide concentration of having used this novel tin dioxide gas-sensitive material, also relate to the preparation method of this gas sensor.
Background technology
(carbon monoxide is a kind of colourless, tasteless and non-irritating gas CO) to carbon monoxide, and carbon monoxide is bigger 250-300 times than the adhesion of oxygen and haemoglobin with the adhesion of haemoglobin, and carbon oxygen is blood red
The speed of dissociating of albumen again than oxyhemoglobin slowly many, the back carbon monoxide of therefore poisoning has lasting toxic action to human body, has hindered the function of carrying oxygen of haemoglobin, causes the body tissue anoxic downright bad, jeopardizes people's life.It is a kind of common poisonous substance that causes people's death by poisoning to be died.Therefore the indoor heating or use the gas heater improper ventilation and the anthracemia accident that takes place of lighting a fire in common winter in the life.On the one hand because people's awareness of safety strengthens, and environmentally safe property and the requirement of comfortable life property improve, because the CO gas alarm receives the promotion of government's security legislation, very fast to the research and the application development of CO gas sensor both at home and abroad on the other hand in recent years.
Reach the main electrochemical transducer[sensor of CO sensor of actual application level at present.Galvanochemistry CO sensor is owing to have unique advantages such as highly sensitive, favorable reproducibility, low in energy consumption, essential safety; But traditional carbon monoxide transducer is owing to contain flowing electrolyte solution; Like acid, alkali etc.; Thereby often having all disadvantages such as leakage, burn into dry up, serviceable life is short.In addition because of this sensor except that working electrode, auxiliary electrode, three electrodes of reference electrode are arranged, also need an electric liquid storeroom, so the cost of sensor is high, volume is big, is unfavorable for miniaturization.Because above drawback has numerous enterprises and researchist to develop the carbon monoxide transducer of the mobile electrolytic solution of all solid state nothing.For example, CN01252229.5 discloses a kind of solid polymer electrolyte carbon monoxide transducer and has had compact conformation, does not contain advantages such as the electrolytic solution that flows; But noble metals such as electrodes use platinum palladium, cost is high, and is merely serviceable life about 2 years.
Because tin dioxide nano material has good gas-sensitive property, so be widely used in the gas sensor manufacturing industry.For sensitivity and selectivity, response speed and the release time of improveing this type sensor; The research work that the researcher did in the industry at present mainly is the following aspects: (1) makes material granule thin as far as possible; Preferably process nano material, increase the unit specific surface area, improve sensitivity; (2) gas sensitive is processed film, so that the contact area of increase and gas improves sensitivity; (3) in the tin ash material of main part, mix precious metal element or REE, with the sensitivity and the selectivity of further raising material.For example, Chinese invention patent ZL200410052061.9 discloses a kind of novel stannic oxide based nanometer gas sensitive and preparation method.It is composed of the following components that this stannic oxide based nanometer gas sensitive is pressed net value mole (part) proportioning: stannous chloride (SnCl22H2O) 1; Neopelex (C18H29NaO3S) 1～2; Potassium borohydride (KBH4) 2; Antimony oxide (Sb2O3) 0.01～0.04; Ethyl orthosilicate C6H20O4Si) 0.02～0.05; CNT 0.1～0.4.
Summary of the invention
First technical matters to be solved by this invention provides a kind of novel tin dioxide gas-sensitive material, can significantly improve the sensitivity of carbon monoxide gas sensor.
Second technical matters to be solved by this invention provides a kind of semiconductor-type carbon monoxide gas sensor of having used this novel tin dioxide gas-sensitive material; That this gas sensor has is highly sensitive, the response fast, measurement range is wide, volume is little, the life-span is long, low cost and other advantages, has solved the carbon monoxide transducer cost height that exists in the prior art, sensitivity is poor, the life-span is low, bulky technical matters.
The 3rd technical matters to be solved by this invention provides the preparation method of above-mentioned carbon monoxide gas sensor.
The technical scheme that the present invention solves the problems of the technologies described above is following:
A kind of tin dioxide gas-sensitive material is made up of following material: tin ash (SnO by mass percentage
2) 88 ~ 94 %, antimony oxide (Sb
2O
3) 1 ~ 5 %, noble metal 0.5 ~ 5%, metal oxide 0.5 ~ 4 %, silicon dioxide (SiO
2) 0.5 ~ 4%.The effect of above-mentioned each component in whole material is following: because carbon monoxide is a kind of gas with reductibility, as it and semiconductor tin ash (SnO
2) when the surface contacted, platinum (Pt) or palladium (Pd) rose under the catalyst action and tin ash (SnO
2) oxygen of surface adsorption reacts, and makes tin ash (SnO
2) potential barrier of intercrystalline contact reduces, thereby the conductivity of element is increased, resistance reduces, and the size that then flows through the current value of this gas sensor through measurement is come the concentration height of carbon monoxide of reaction.Antimony oxide (the Sb that adds
2O
3) raising tin ash (SnO
2) to the performance of Carbon Monoxide Detection.Silicon dioxide (SiO
2) be a kind of sintering agent, can promote tin ash (SnO when making gas sensor
2) sintering.
Further, said noble metal is selected from least a in platinum, palladium, rhodium, iridium, the gold.
Further, said metal oxide is selected from least a in magnesium oxide, zinc paste, the titania.
Further, the particle diameter of the powder of said antimony oxide and tin ash all is lower than 200nm, and meso-position radius is less than 100nm.
A kind of carbon monoxide gas sensor of having used above-mentioned tin dioxide gas-sensitive material, its structure is: bottom is a calandria, is covered with the gas sensing layer that said tin dioxide gas-sensitive material makes on the calandria, gas sensing layer is connected with lead-in wire, is covered with ceramic molecular sieve on the gas sensing layer.
Further, said ceramic molecular sieve is the nano ceramics molecular sieve, and the aperture is less than 10nm.Its effect is other reducibility gas in the filtering gas, guarantees the accuracy of gas sensor test carbon monoxide, and the carbon monoxide of activation simultaneously makes the sensitivity of gas sensor test carbon monoxide higher.
Further, said calandria refers to heating electrode and is overlying on the last ceramic matrix and following ceramic matrix of heating electrode upper and lower that said heating electrode is connected with the heating electrode lead-in wire.
Further, the material of said heating electrode is any one of platinum, palladium, tungsten, molybdenum, chromic acid lanthanum, tantalum silicide, silicon molybdenum, platinum-rhodium alloy.
A kind of preparation method of above-mentioned carbon monoxide gas sensor, preparation process is:
(1) preparation gas sensing layer slurry and calandria;
(2) on calandria, be covered with the gas sensing layer slurry, form gas sensing layer (11) through serigraphy, spraying, sputtering technology;
(3) cover one deck pottery molecular sieve at the gas sensing layer upper surface, under 300 ~ 800 ℃ of conditions, carrying out sintering 2 ~ 8h then.
Further, the preparation method of said calandria is:
The green compact of ceramic matrix (21) and following ceramic matrix (23) on employing curtain coating, coating, the press forming prepared; On the green compact of last ceramic matrix (21), covering heating electrode (22) and heating electrode lead-in wire (24) then; Under 80 ~ 120 ℃ temperature and 10 ~ 20MPa pressure, carry out superimposed with the green compact of following ceramic matrix (23) again; Under 1300 ~ 1600 ℃ of conditions, carry out sintering, prepare calandria.
Further, the preparation method of said gas sensing layer slurry therewith is:
(1) takes by weighing the inorganic powder of gas sensing layer material in proportion, the electrodeless powder of 100 parts of quality is put into the ethanol solution of 250 parts of quality, stir 2 ~ 4h, obtain the emulsion that mixes with the speed of 200 ~ 300r/min;
(2) emulsion that mixes that obtains in the step (1) is carried out vacuum drying under 30 ℃ of conditions and remove absolute ethyl alcohol, make mixed-powder;
(3) take by weighing inorganic mixed-powder and the organic ink carrier that the gas sensing layer slurry is used in following ratio:
In mass; Get dry good mixed-powder 100 powder; Add 1.5 ~ 2.5 parts of triglycerides, 35 ~ 45 parts of terpinols, 5 ~ 8 parts of ethyl celluloses, 2 ~ 4 parts of polyvinyl butyrals, 1.5 ~ 3 parts of dibutyl phthalates grind with muller then and prepare the gas sensing layer slurry.
The present invention has following beneficial effect:
Tin dioxide gas-sensitive material of the present invention in the material that with the tin ash is main body, mix antimony oxide, calcium oxide, silicon dioxide and platinum, palladium noble metal make the carbon monoxide gas sensor of using this gas sensitive have higher sensitivity.
The carbon monoxide gas sensor that the present invention has used said tin dioxide gas-sensitive material has advantage highly sensitive, that response is fast, measurement range is wide, volume is little, the life-span is long; In addition; The present invention is owing to adopt solid semiconductor, and the volume with existing galvanochemistry carbon monoxide transducer reduces more than 50% relatively.
Description of drawings
Fig. 1 is the structural representation of carbon monoxide gas sensor of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is carried out detailed explanation, embodiment only is a preferred implementation of the present invention, is not limitation of the present invention.
Embodiment 1
The preparation method of present embodiment carbon monoxide gas sensor is following:
(1) preparation of calandria
The green compact of ceramic matrix (21) and following ceramic matrix (23) on employing curtain coating, coating, the press forming prepared; On the green compact of last ceramic matrix (21), adopt silk-screen printing technique to stamp heating electrode (3) and the heating electrode lead-in wire (24) that is the main body with the chromic acid lanthanum then; Under 90 ℃ temperature and 16MPa pressure, carry out superimposed with the green compact of following ceramic matrix (23) again; Sintering 2h under 1500 ℃ of conditions prepares calandria.
(2) preparation of gas sensing layer slurry therewith
1. the mass percent of according to the form below 1 takes by weighing the inorganic powder that gas sensing layer is used:
Table 1
| Inorganic component | SnO 2 | Sb 2O 3 | Pt | Pd | CaO | SiO 2 |
| Content (%) | 91 | 2.5 | 1 | 1.5 | 2 | 3 |
| Particle diameter (nm) | ≤150 | ≤150 | ? | ? | ? | ? |
| Meso-position radius (nm) | ≤70 | ≤70 | ? | ? | ? | ? |
To put into the ethanol solution of 250 parts of quality with the 100 parts of electrodeless powder of improving quality, and adopt the JJ-2 electric mixer to stir 3h, obtain the emulsion that mixes with the speed of 250r/min.
2. the 1. middle emulsion that mixes that obtains of step is put into the FZG of Nanjing Zhu Boai company series low-temperature vacuum drying case and under 30 ℃ of conditions, carry out vacuum drying removal absolute ethyl alcohol, make mixed-powder.
3. take by weighing inorganic mixed-powder and the organic ink carrier that the gas sensing layer slurry is used in following ratio:
With the good mixed-powder quality of drying is benchmark 100 powder; Add 2 parts of triglycerides, 40 parts of terpinols, 6 parts of ethyl celluloses, 2.5 parts of polyvinyl butyrals; 2 parts of dibutyl phthalates adopt ST-65 pottery three-roll grinder to grind then and prepare the gas sensing layer slurry.
(3) on calandria, be covered with the tin dioxide gas-sensitive material mixed-powder, form gas sensing layer (11) through serigraphy, spraying, sputtering technology;
(4) covering one deck pottery molecular sieve (13) at gas sensing layer (11) upper surface, under 600 ℃ of conditions, carrying out sintering 3h then, thereby make the carbon monoxide gas sensor of Fig. 1 structure.
Among the above-mentioned preparation method, it is conventionally known to one of skill in the art that casting technique prepares the superimposed and ceramic heating body co-firing technology that ceramic substrate, spraying, sputtering technology be covered with gas sensing layer and ceramic molecular sieve, lamination, does not give unnecessary details here.
The technical indicator of the carbon monoxide gas sensor that present embodiment makes is following:
| Project | Technical parameter |
| Sensing range ppm | 10-2500 |
| Working temperature ℃ | 150-200 |
| Sensitivity uA/ppm | 0.01±0.03uA/ppm |
| Gas sensor reflection time S | ＜20 |
| Device S release time | ＜50 |
| Zero point drift | ＜10ppm |
| Stability (/ year) | ＜5% |
Embodiment 2
The inorganic powder that the present embodiment gas sensing layer is used is as shown in table 2 by mass percentage:
Table 2
| Inorganic component | SnO 2 | Sb 2O 3 | Pt | Pd | CaO | SiO 2 |
| Content (%) | 88 | 5 | 2 | 3 | 1 | 1 |
| Particle diameter (nm) | ≤100 | ≤100 | ? | ? | ? | ? |
| Meso-position radius (nm) | ≤50 | ≤50 | ? | ? | ? | ? |
Other preparation process is identical with embodiment 1 with method, does not do being repeated in this description at this.
The technical indicator of the carbon monoxide gas sensor that present embodiment makes is following:
| Project | Technical parameter |
| Sensing range ppm | 10-3000 |
| Working temperature ℃ | 120-160 |
| Sensitivity uA/ppm | 0.01±0.03uA/ppm |
| Gas sensor reflection time S | ＜10 |
| Device S release time | ＜40 |
| Zero point drift | ＜10ppm |
| Stability (/ year) | ＜3% |
Embodiment 3
The inorganic powder that the present embodiment gas sensing layer is used is as shown in table 3 by mass percentage:
Table 3
| Inorganic component | SnO 2 | Sb 2O 3 | Pt | Pd | MgO | SiO 2 |
| Content (%) | 94 | 1 | 1 | / | 2 | 2 |
| Particle diameter (nm) | ≤200 | ≤100 | ? | ? | ? | ? |
| Meso-position radius (nm) | ≤100 | ≤50 | ? | ? | ? | ? |
Other preparation process is identical with embodiment 1 with method, does not do being repeated in this description at this.
The technical indicator of the carbon monoxide gas sensor that present embodiment makes is following:
| Project | Technical parameter |
| Sensing range ppm | 30-1000 |
| Working temperature ℃ | 180-250 |
| Sensitivity uA/ppm | 0.01±0.03uA/ppm |
| Gas sensor reflection time S | ＜30 |
| Device S release time | ＜60 |
| Zero point drift | ＜20ppm |
| Stability (/ year) | ＜5% |
Claims (9)
1. a tin dioxide gas-sensitive material is characterized in that, is made up of following material by mass percentage: tin ash 88 ~ 94 %, antimony oxide 1 ~ 5 %, noble metal 0.5 ~ 5%, metal oxide 0.5 ~ 4 %, silicon dioxide 0.5 ~ 4%.
2. tin dioxide gas-sensitive material according to claim 1 is characterized in that: the particle diameter of the powder of said antimony oxide and tin ash all is lower than 200nm, and meso-position radius is less than 100nm.
3. carbon monoxide gas sensor of having used 1 or 2 any said tin dioxide gas-sensitive materials; It is characterized in that: bottom is a calandria; Be covered with the gas sensing layer (11) that said tin dioxide gas-sensitive material makes on the calandria; Gas sensing layer (11) is connected with lead-in wire (12), is covered with ceramic molecular sieve (13) on the gas sensing layer (11).
4. carbon monoxide gas sensor according to claim 3 is characterized in that: said ceramic molecular sieve (13) is the nano ceramics molecular sieve, and the aperture is less than 10nm.
5. carbon monoxide gas sensor according to claim 3; It is characterized in that: said calandria refers to heating electrode (22) and is overlying on the last ceramic matrix (21) and the following ceramic matrix (23) of heating electrode (22) upper and lower that said heating electrode (22) is connected with heating electrode lead-in wire (24).
6. carbon monoxide gas sensor according to claim 5 is characterized in that: the material of said heating electrode (22) is any one of platinum, palladium, tungsten, molybdenum, chromic acid lanthanum, tantalum silicide, silicon molybdenum, platinum-rhodium alloy.
7. the preparation method of the said carbon monoxide gas sensor of claim 5 is characterized in that preparation process is:
(1) preparation gas sensing layer slurry and calandria;
(2) on calandria, be covered with the gas sensing layer slurry, form gas sensing layer (11) through serigraphy, spraying, sputtering technology;
(3) cover one deck pottery molecular sieve (13) at gas sensing layer (11) upper surface, under 300 ~ 800 ℃ of conditions, carrying out sintering 2 ~ 8h then.
8. the preparation method of carbon monoxide gas sensor according to claim 7 is characterized in that: the preparation method of said calandria is:
The green compact of ceramic matrix (21) and following ceramic matrix (23) on employing curtain coating, coating, the press forming prepared; On the green compact of last ceramic matrix (21), covering heating electrode (22) and heating electrode lead-in wire (24) then; Under 80 ~ 120 ℃ temperature and 10 ~ 20MPa pressure, carry out superimposed with the green compact of following ceramic matrix (23) again; Under 1300 ~ 1600 ℃ of conditions, carry out sintering, prepare calandria.
9. the preparation method of carbon monoxide gas sensor according to claim 7 is characterized in that: the preparation method of said gas sensing layer slurry therewith is:
(1) takes by weighing the inorganic powder of gas sensing layer material in proportion, the electrodeless powder of 100 parts of quality is put into the ethanol solution of 250 parts of quality, stir 2 ~ 4h, obtain the emulsion that mixes with the speed of 200 ~ 300r/min;
(2) emulsion that mixes that obtains in the step (1) is carried out vacuum drying under 30 ℃ of conditions and remove absolute ethyl alcohol, make mixed-powder;
(3) take by weighing inorganic mixed-powder and the organic ink carrier that the gas sensing layer slurry is used in following ratio:
In mass; Get dry good mixed-powder 100 powder; Add 1.5 ~ 2.5 parts of triglycerides, 35 ~ 45 parts of terpinols, 5 ~ 8 parts of ethyl celluloses, 2 ~ 4 parts of polyvinyl butyrals, 1.5 ~ 3 parts of dibutyl phthalates grind with muller then and prepare the gas sensing layer slurry.
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