CN1334461A - Process for preparing air/fuel ratio thick-film sensor with wide temp range and narrow resistance band - Google Patents
Process for preparing air/fuel ratio thick-film sensor with wide temp range and narrow resistance band Download PDFInfo
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- CN1334461A CN1334461A CN 01128775 CN01128775A CN1334461A CN 1334461 A CN1334461 A CN 1334461A CN 01128775 CN01128775 CN 01128775 CN 01128775 A CN01128775 A CN 01128775A CN 1334461 A CN1334461 A CN 1334461A
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Abstract
An air/fuel ratio sensor with wide temp range and narrow resistance band and its preparing process are disclosed. The rutile-type TiO2 structure is used for internal N-type doping and the P-type complex diffusion is performed to crystal interface. As a result, the electric conductivity of specimen is sharply lowered in oxidizing atmosphere, or sharply raised in reducing atmosphere. The thick film technology is used to make the specimen have 1-3 orders of magnitude of resistance difference in 250-800 deg.C. Its advantages are greatly improved performance and low cost.
Description
One, technical field
The present invention relates to a kind of air/fuel than the control sensor, the air/fuel that further relates to all kinds of engines, combustion apparatus, utensil is than the preparation method of control with sensor.
Two, background technology
Air-fuel ratio control has appeared at the ZrO that has on the market with sensor
2Concentration cell type, TiO
2And the resistor-type of the single-phase mixing of other oxide.ZrO
2The concentration cell type exists saturnism, structural phase transition and price problem of higher in ℃ scope of room temperature～800, in use have the higher shortcoming of initial failure and cost.For this reason, people are to TiO
2And the single-phase hybrid resistor type of other oxide sensor carried out a large amount of research, owing to exist in the wide temperature range of room temperature～800 ℃: (1) wide stopband, go back under the ortho states and present high-impedance state; (2) life-span is shorter; (3) shortcoming such as signal circuit complexity.So do not come into operation in a large number yet so far.Recently carried out the research of IBMD method again, but because preparation cost is higher, performance is difficult to problems such as assurance, heating-up temperature height, also fails to popularize.But along with the rising of automobile quantity, the air pollution in city is mainly derived from emission of automobile wastes, and all kinds of combustion apparatus, utensil and motor car engine than not at that time, can be discharged a large amount of harmful gases, contaminated environment at air/fuel on the one hand; The energy can not be fully used, cause waste.
Three, summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, the preparation method of a kind of long-life, low price, high performance wide temp range and narrow resistance band air/fuel ratio thick-film sensor is provided.The technical solution used in the present invention is: according to the raising of N type transition metal oxide semiconductor crystal boundary barrier height under oxidizing atmosphere, rutile TiO is adopted in the reduction of crystal boundary barrier height under the reducing atmosphere
2Structure is mixed to carrying out the N type in the body, and crystal boundary carries out the compound diffusion of P type.Make sample under oxidizing atmosphere, electricity is led rapid reduction, under the reducing atmosphere, sharply increases.Adopt thick-film technique to make sample in 250 ℃～800 ℃ scopes, make the also difference of ortho states 1～3 order of magnitude of high value appearance down of minimum resistance and low-temperature end under the temperature end oxidation state.
Preparation technology of the present invention is:
1) can synthesize (TiSnNb) O
2Behind the semiconductor porcelain powder reagent porphyrize base of the rutile structure of base, place 1000 ℃～1350 ℃ to drink burning 30 minutes～4 hours;
2) warm glass dust mixes after the fine-powdered and among (0～20) %wt, makes printing with responsive powder slurry;
3) after serigraphy becomes interdigital electrode on the alumina substrate, place 800 ℃～1000 ℃ to drink burning 20 minutes～1 hour;
4) use the responsive powder slurry of serigraphy again after, place 1000 ℃～1350 ℃ to drink and burnt 1～2 hour, cooling velocity is controlled at 120 ℃～180 ℃ of per minutes, make the sample cooling, make sensitive element;
5) weld with the interdigital electrode exit of platinum slurry again, place 800 ℃～1000 ℃ to drink burning 10～20 minutes, make the sample natural cooling platinum filament and sensitive element;
6) at sensitive element back side serigraphy well heater slurry and place 650 ℃～850 ℃ drink to burn 10～45 minutes;
7) flood or apply 10%～50% catalyzer salt solusion after, place 700 ℃～1000 ℃ to drink and burnt 30 minutes～2 hours.
Adopt preparation method of the present invention, improved the air/fuel ratio sensor performance, reduced manufacturing cost, the control effect of air-fuel ratio sensor is further improved.
Four, the specific embodiment
Embodiment 1: be 0.63TiO to component2＋0.2SnO
2＋0.05Nb
2O
5＋0.12Bi2O
3Porcelain powder sample Behind the reagent porphyrize base, drank burning 30 minutes at 1000 ℃, make and print with responsive powder slurry; In oxidation After serigraphy becomes interdigital electrode on the aluminium substrate, place 800 ℃ to drink burning 20 minutes; Use again serigraphy quick Behind the sense powder slurry, place 1000 ℃ to drink burning 1 hour, cooling velocity is controlled at 120 ℃ of per minutes, make Sensing element is made in the sample cooling; Use again the platinum slurry with the interdigital electrode exit of platinum filament and sensing element Weld, place 800 ℃ to drink burning 10 minutes, sample is cooled off naturally; In the serigraphy of the sensing element back side The heater slurry, and place 650 ℃ of meals with wine to burn half an hour; Impregnated in 10% catalyst P dCl2Behind the solution, Place 700 ℃ to drink burning 30 minutes.
Made sample is under oxidizing atmosphere: in 250 ℃～800 ℃, resistance is 50k Ω～1000k Ω.
Under reducing atmosphere: in 250 ℃～800 ℃, resistance is 95 Ω～50 Ω.
Embodiment 2: be 0.63TiO to component2＋0.2SnO
2＋0.05Nb
2O
5＋0.12Bi
2O
3Porcelain powder sample Behind the reagent porphyrize base, drink to burn 4 hours at 1350 ℃, warm glass dust is mixed after the fine-powdered and among the 20%wt Close, make and print with responsive powder slurry; After serigraphy becomes interdigital electrode on the alumina substrate, place Drink for 1000 ℃ and burnt 1 hour; After using again the responsive powder slurry of serigraphy, place 1350 ℃ to drink burning 2 hours, Cooling velocity is controlled at 180 ℃ of per minutes, makes the sample cooling, make sensing element; Use again the platinum slurry The interdigital electrode exit of platinum filament and sensing element is welded, place 1000 ℃ to drink burning 20 minutes, make sample Product cool off naturally; At sensing element back side serigraphy heater slurry, and place 850 ℃ to drink burning 10 minutes Clock; The catalyst H of coating 30%4PtCl
2Behind the solution, place 1000 ℃ to drink burning 2 hours.
Made sample is under oxidizing atmosphere: in 250 ℃～800 ℃, resistance is 50k Ω～1000k Ω.
Under reducing atmosphere: in 250 ℃～800 ℃, resistance is 95 Ω～250 Ω.
Embodiment 3: be 0.63TiO to component2＋0.2SnO
2＋0.05 Nb
2O
5＋0.12Bi
2O
3Porcelain powder sample After reagent porphyrize system is bad, place 1150 ℃ to drink and burnt 2 hours, warm glass dust after the fine-powdered and among the 10%wt Mix, make and print with responsive powder slurry; After serigraphy becomes interdigital electrode on the alumina substrate, put Drank burning 40 minutes in 900 ℃; After using again the responsive powder slurry of serigraphy, place 1150 ℃ of meal with wine burnings 1.5 little The time, cooling velocity is controlled at 150 ℃ of per minutes, make the sample cooling, make sensing element; Use again platinum Slurry welds the interdigital electrode exit of platinum filament and sensing element, places 900 ℃ to drink burning 15 minutes, makes Sample cools off naturally; At sensing element back side serigraphy heater slurry, and place 700 ℃ to drink burning 45 Minute; Behind the catalyst salt PdCl2 solution of coating 50%, place 900 ℃ to drink burning 1 hour.
Made sample is under oxidizing atmosphere: in 250 ℃～800 ℃, resistance is 50k Ω～1000k Ω.
Under reducing atmosphere: in 250 ℃～800 ℃, resistance is 95 Ω～250 Ω.
Embodiment 4: to component 0.64TiO2＋0.3SnO
2＋0.06Nb
2O
5Porcelain powder sample reagent porphyrize system Behind the base, drank burning 30 minutes at 1000 ℃, make and print with responsive powder slurry; Silk on alumina substrate After reticulated printing becomes interdigital electrode, place 800 ℃ to drink burning 20 minutes; After using again the responsive powder slurry of serigraphy, Place 1000 ℃ to drink burning 1 hour, cooling velocity is controlled at 120 ℃ of per minutes, make the sample cooling, system Become sensing element; Weld with the interdigital electrode exit of platinum slurry with platinum filament and sensing element again, place 800 ℃ drink to burn 10 minutes, sample is cooled off naturally; At sensing element back side serigraphy heater slurry, and Place 650 ℃ to drink burning 10 minutes; Impregnated in 10% catalyst H4PtCl
2Behind the solution, at 700 ℃ of meals with wine Burnt 30 minutes.
Made sample is under oxidizing atmosphere: in 250 ℃～800 ℃, resistance is 50k Ω～1000k Ω.
Made sample is under reducing atmosphere: in 250 ℃～800 ℃, resistance is 85 Ω～150 Ω.
Embodiment 5: to component 0.64TiO2＋0.3SnO
2＋0.06Nb
2O
5Porcelain powder sample reagent porphyrize system Behind the base, place 1200 ℃ drink to burn 2 hours, warm glass dust mixes after the fine-powdered and among the 8%wt, makes seal Brush with responsive powder slurry; After serigraphy becomes interdigital electrode on the alumina substrate, place 900 ℃ to drink burning 40 Minute; After using again the responsive powder slurry of serigraphy, place 1100 ℃ to drink burning 1.5 hours, with cooling velocity Be controlled at 150 ℃ of per minutes, make the sample cooling, make sensing element; Use again the platinum slurry with platinum filament and quick The interdigital electrode exit of sensing unit welds, and places 900 ℃ to drink burning 16 minutes, and sample is cooled off naturally; At sensing element back side serigraphy heater slurry, and place 700 ℃ to drink burning 25 minutes; Impregnated in 25% Catalyst P dCl2Behind the solution, drank burning 1 hour at 900 ℃.
Made sample is under oxidizing atmosphere: in 250 ℃～800 ℃, resistance is 50k Ω～1000k Ω.
Made sample is under reducing atmosphere: in 250 ℃～800 ℃, resistance is 85 Ω～150 Ω.
Embodiment 6: to component 0.64TiO2＋0.3SnO
2＋0.06Nb
2O
5Porcelain powder sample reagent porphyrize system Behind the base, place 1350 ℃ drink to burn 4 hours, warm glass dust mixes after the fine-powdered and among the 20%wt, makes Print with responsive powder slurry; After serigraphy becomes interdigital electrode on the alumina substrate, place 1000 ℃ of meals with wine Burnt 1 hour; After using again the responsive powder slurry of serigraphy, place 1350 ℃ to drink burning 2 hours, will cool off speed Degree is controlled at 180 ℃ of per minutes, makes the sample cooling, makes sensing element; Use again the platinum slurry with platinum filament and The interdigital electrode exit of sensing element welds, and places 1000 ℃ to drink burning 20 minutes, makes sample naturally cold But; At sensing element back side serigraphy heater slurry, and place 850 ℃ to drink burning 45 minutes; Coating 50% catalyst H4PtCl
2Behind the solution, drank burning 2 hours at 1000 ℃.
Made sample is under oxidizing atmosphere: in 250 ℃～800 ℃, resistance is 50k Ω～1000k Ω.
Made sample is under reducing atmosphere: in 250 ℃～800 ℃, resistance is 85 Ω～150 Ω.
Embodiment 7: to component 0.63TiO2＋0.30SnO
2＋0.07Nb
2O
5Porcelain powder sample reagent porphyrize system Behind the base, place 1000 ℃ drink to burn 4 hours, warm glass dust mixes after the fine-powdered and among the 20%wt, makes Print with responsive powder slurry; After serigraphy becomes interdigital electrode on the alumina substrate, drink burning 1 at 800 ℃ Hour; After using again the responsive powder slurry of serigraphy, place 1000 ℃ to drink burning 2 hours, with the cooling velocity control Built in 120 ℃ of per minutes, make the sample cooling, make sensing element; Use again the platinum slurry with platinum filament and sensitivity The interdigital electrode exit of element welds, and places 1000 ℃ to drink burning 10 minutes, and sample is cooled off naturally; At sensing element back side serigraphy heater slurry, and place 850 ℃ to drink burning 10 minutes; Coating 50% Catalyst P dCl2Behind the solution, drank burning 2 hours at 700 ℃.
Made sample is under oxidizing atmosphere: in 250 ℃～800 ℃, resistance is 200k Ω～5 * 106Ω。
Made sample is under reducing atmosphere: in 250 ℃～8000 ℃, resistance is 150 Ω～220 Ω.
Embodiment 8: to component 0.63TiO2＋0.30SnO
2＋0.07Nb
2O
5Porcelain powder sample reagent porphyrize system Behind the base, place 1350 ℃ to drink burning 30 minutes, make and print with responsive powder slurry; On alumina substrate After serigraphy becomes interdigital electrode, drank burning 20 minutes at 1000 ℃; Use again the responsive powder slurry of serigraphy After, place 1350 ℃ to drink burning 1 hour, cooling velocity is controlled at 180 ℃ of per minutes, make the sample cooling, Make sensing element; Weld with the interdigital electrode exit of platinum slurry with platinum filament and sensing element again, place Drink for 800 ℃ and burnt 20 minutes, sample is cooled off naturally; At sensing element back side serigraphy heater slurry, And place 650 ℃ to drink burning 45 minutes; Impregnated in 10% catalyst H4PtCl
2In the solution, at 1000 ℃ Drink and burnt 30 minutes.
Made sample is under oxidizing atmosphere: in 250 ℃～800 ℃, resistance is 200k Ω～5 * 106Ω。
Made sample is under reducing atmosphere: in 250 ℃～800 ℃, resistance is 150 Ω～220 Ω.
Embodiment 9: to component 0.63TiO2＋0.30SnO
2＋0.07Nb
2O
5Porcelain powder sample reagent porphyrize system Behind the base, place 1200 ℃ drink to burn 3 hours, warm glass dust mixes after the fine-powdered and among the 15%wt, makes Print with responsive powder slurry; After serigraphy becomes interdigital electrode on the alumina substrate, drink burning 45 at 920 ℃ Minute; After using again the responsive powder slurry of serigraphy, place 1280 ℃ to drink burning 1.5 hours, with cooling velocity Be controlled at 140 ℃ of per minutes, make the sample cooling, make sensing element; Use again the platinum slurry with platinum filament and quick The interdigital electrode exit of sensing unit welds, and places 900 ℃ to drink burning 18 minutes, and sample is cooled off naturally; At sensing element back side serigraphy heater slurry, and place 750 ℃ of meals with wine to burn half an hour, impregnated in 28% Catalyst P dCl2Behind the solution, drank burning 1 hour at 950 ℃.
Made sample is under oxidizing atmosphere: in 250 ℃～800 ℃, resistance is 200k Ω～5 * 106Ω。
Made sample is under reducing atmosphere: in 250 ℃～800 ℃, resistance is 150 Ω～220 Ω.
Claims (8)
1, the preparation method of wide temp range and narrow resistance band air/fuel ratio thick-film sensor is characterized in that:
1) can synthesize (TiSnNb) O
2Behind the semiconductor porcelain powder reagent porphyrize base of the rutile structure of base, place 1000 ℃～1350 ℃ to drink burning 30 minutes～4 hours;
2) warm glass dust mixes after the fine-powdered and among 0～20%wt, makes printing with responsive powder slurry;
3) after serigraphy becomes interdigital electrode on the alumina substrate, drank burning 20 minutes～1 hour at 800 ℃～1000 ℃;
4) be placed on 1000 ℃～1350 ℃ with the responsive powder slurry of serigraphy again and drank burning 1～2 hour, cooling velocity is controlled at 120 ℃～180 ℃ of per minutes, make the sample cooling, make sensitive element;
5) weld with the interdigital electrode exit of platinum slurry again, place 800 ℃～1000 ℃ to drink burning 10～20 minutes, make the sample natural cooling platinum filament and sensitive element;
6), and place 650 ℃～850 ℃ to drink burning 15～45 minutes at sensitive element back side serigraphy well heater slurry;
7) flood or apply 10%～50% catalyzer salt solusion, drink at 700 ℃～1000 ℃ and burnt 30 minutes～2 hours.
2, the preparation method of wide temp range and narrow resistance band air/fuel ratio thick-film sensor according to claim 1 is characterized in that:
1) can synthesize (TiSnNb) O
2Behind the semiconductor porcelain powder reagent porphyrize base of the rutile structure of base, place 1000 ℃ to drink burning 30 minutes;
2) make printing after the fine-powdered with responsive powder slurry;
3) after serigraphy becomes interdigital electrode on the alumina substrate, drank burning 20 minutes at 800 ℃;
4) use the responsive powder slurry of serigraphy again after, place 1000 ℃ to drink and burnt 1 hour, the cooling velocity of sample is controlled at 120 ℃ of per minutes makes it cooling, make sensitive element;
5) weld with the interdigital electrode exit of platinum slurry again, place 800 ℃ to drink burning 10 minutes, make the sample natural cooling platinum filament and sensitive element;
6), and place 650 ℃ to drink burning 10 minutes at sensitive element back side serigraphy well heater slurry;
7) impregnated in 10% catalyzer salt solusion, drink at 700 ℃ and burnt 30 minutes.
3, the preparation method of wide temp range and narrow resistance band air/fuel ratio thick-film sensor according to claim 1 is characterized in that:
1) can synthesize (TiSnNb) O
2Behind the semiconductor porcelain powder reagent porphyrize base of the rutile structure of base, place 1100 ℃ to drink burning 2 hours;
2) warm glass dust mixing among the 10%wt after the fine-powdered is made and is printed with responsive powder slurry;
3) after serigraphy becomes interdigital electrode on the alumina substrate, drank burning 40 minutes down at 900 ℃;
4) use the responsive powder slurry of serigraphy again after, place 1100 ℃ to drink and burnt 1.5 hours, cooling velocity is controlled at 150 ℃ of per minutes, make the sample cooling, make sensitive element;
5) weld with the interdigital electrode exit of platinum slurry again, place 900 ℃ to drink burning 15 minutes, make the sample natural cooling platinum filament and sensitive element;
6), and place 750 ℃ of meals with wine to burn half an hour at sensitive element back side serigraphy well heater slurry;
7) coating 30% catalyzer salt solusion was drunk burning 1 hour at 850 ℃.
4, the preparation method of wide temp range and narrow resistance band air/fuel ratio thick-film sensor according to claim 1 is characterized in that:
1) can synthesize (TiSnNb) O
2Behind the semiconductor porcelain powder reagent porphyrize base of the rutile structure of base, drank burning 4 hours at 1350 ℃;
2) warm glass dust mixes after the fine-powdered and among the 20%wt, makes printing with responsive powder slurry;
3) after serigraphy becomes interdigital electrode on the alumina substrate, drank burning 1 hour down at 1000 ℃;
4) use the responsive powder slurry of serigraphy again after, place 1350 ℃ to drink and burnt 2 hours, cooling velocity is controlled at 180 ℃ of per minutes, make the sample cooling, make sensitive element;
5) weld with the interdigital electrode exit of platinum slurry again, place 1000 ℃ to drink burning 20 minutes, make the sample natural cooling platinum filament and sensitive element;
6), and place 850 ℃ to drink burning 45 minutes at sensitive element back side serigraphy well heater slurry;
7) impregnated in 50% catalyzer salt solusion, drink down at 1000 ℃ and burnt 2 hours.
5, the preparation method of wide temp range and narrow resistance band base air/fuel ratio thick-film sensor according to claim 1 is characterized in that: said (TiSnNb) O
2TiO in the base
2Content be 0.63mol～0.64mol.
6, the preparation method of wide temp range and narrow resistance band air/fuel ratio thick-film sensor according to claim 1 is characterized in that: said (TiSnNb) O
2SnO in the base
2Content be 0.2mol～0.3mol.
7, the preparation method of wide temp range and narrow resistance band air/fuel ratio thick-film sensor according to claim 1 is characterized in that: said (TiSnNb) O
2Nb in the base
2O
5Content be 0.05mol～0.07mol.
8, the preparation method of wide temp range and narrow resistance band air/fuel ratio thick-film sensor according to claim 1 is characterized in that: said salt solusion is PdCl
2Or H
4PtCl
2Solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011287756A CN1160565C (en) | 2001-09-03 | 2001-09-03 | Process for preparing air/fuel ratio thick-film sensor with wide temp range and narrow resistance band |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011287756A CN1160565C (en) | 2001-09-03 | 2001-09-03 | Process for preparing air/fuel ratio thick-film sensor with wide temp range and narrow resistance band |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1334461A true CN1334461A (en) | 2002-02-06 |
| CN1160565C CN1160565C (en) | 2004-08-04 |
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ID=4668604
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011287756A Expired - Fee Related CN1160565C (en) | 2001-09-03 | 2001-09-03 | Process for preparing air/fuel ratio thick-film sensor with wide temp range and narrow resistance band |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1160565C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106053550A (en) * | 2016-06-06 | 2016-10-26 | 怀远县金浩电子科技有限公司 | Preparation method of gas-sensitive semiconductor device |
| CN109716120A (en) * | 2016-07-07 | 2019-05-03 | 俄罗斯联邦诺萨顿国家原子能公司 | For determining the device of the parameter of a formula superconductor |
-
2001
- 2001-09-03 CN CNB011287756A patent/CN1160565C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106053550A (en) * | 2016-06-06 | 2016-10-26 | 怀远县金浩电子科技有限公司 | Preparation method of gas-sensitive semiconductor device |
| CN109716120A (en) * | 2016-07-07 | 2019-05-03 | 俄罗斯联邦诺萨顿国家原子能公司 | For determining the device of the parameter of a formula superconductor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1160565C (en) | 2004-08-04 |
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