CN101967054B - Preparation method of In2O3/SnO2 gas sensitive material with porous structure - Google Patents
Preparation method of In2O3/SnO2 gas sensitive material with porous structure Download PDFInfo
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- CN101967054B CN101967054B CN2010102741838A CN201010274183A CN101967054B CN 101967054 B CN101967054 B CN 101967054B CN 2010102741838 A CN2010102741838 A CN 2010102741838A CN 201010274183 A CN201010274183 A CN 201010274183A CN 101967054 B CN101967054 B CN 101967054B
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- CN
- China
- Prior art keywords
- gas sensitive
- in2o3
- sno
- sintering
- porous structure
- Prior art date
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Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000000463 material Substances 0.000 title abstract description 7
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title abstract 12
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title abstract 6
- 239000007789 gas Substances 0.000 claims abstract description 44
- 238000005245 sintering Methods 0.000 claims abstract description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 21
- 235000015895 biscuits Nutrition 0.000 claims description 10
- 238000011065 in-situ storage Methods 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 8
- 238000004080 punching Methods 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 2
- 238000001778 solid-state sintering Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000007790 solid phase Substances 0.000 abstract 1
- 229910044991 metal oxide Inorganic materials 0.000 description 5
- 150000004706 metal oxides Chemical class 0.000 description 5
- 206010070834 Sensitisation Diseases 0.000 description 4
- 230000008313 sensitization Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000011540 sensing material Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention relates to a preparation method of an In2O3/SnO2 gas sensitive material with a porous structure. The method comprises the following steps: mixing commercial In2O3 powder and SnO2 powder in a weight ratio of 4:1 or 7:3 or 3:2 place and mixing, compressing into a green body, and then placing the green body in a sintering furnace with oxygen atmosphere and carrying out solid phase sintering to finally obtain the In2O3/SnO2 gas sensitive material with the porous structure. The method of the invention controls the sintering temperature to obtain the In2O3/SnO2 gas sensitive material with the micron or submicron grade porous structure with regular holes, thus the porous structure is adopted to increase the specific area so as to increase the gas sensitivity and the weight of In2O3/SnO2 is controlled to increase the selectivity to different gases. Therefore, the gas sensitive material with the porous structure which has high sensitivity and selectivity can be obtained. The method adopted by the invention has the advantages of easy preparation of raw material, low cost, clean production, is easy to control, and the like.
Description
Technical field
The present invention relates to the stupalith synthesis technical field, specifically a kind of In
2O
3/ SnO
2The preparation method of porous road structure gas sensitive.
Background technology
Along with science and technology development, to the detection of inflammable gas and poisonous gas, monitoring, warning require increasingly highly, this just has higher requirement to detecting the gas sensitive that relies on; Therefore, sensitivity, selectivity and the permanent stability of raising gas sensitive and reduction working temperature, shortening response recovery time etc. become the important directions of gas sensitive development.
The investigator generally believes that the method for improving the gas sensitive over-all properties mainly contains doped metal ion (comprising precious metal or REE) or MOX, increase gas sensitive specific surface area, strengthens the research of gas sensing mechanism etc. at present.
Structural metal, porous road oxide gas-sensing material utilizes the vesicular structure specific surface area big just; Mesoporous (several nanometers to tens nanometer) structure is strong to the adsorptivity of gas; Increased that this material microstructure characteristic of Activity of Chemical Reaction point proposes, the gas sensitization property of the MOX gas sensitive of this structure is much better than the common metal oxide composite.Though porous road microtexture has played vital role to improving gas sensitive gas sensitization property; But with a kind of MOX under specific temperature conditions not only to a kind of gas sensitization; Maybe be all responsive to several kinds of gases; Cause people to the difficulty that gaseous species detects, need the selectivity of gas sensitive further be improved, to realize prepared transmitter gas sensitization only in use being detected; The realization of this target only depends on very difficulty of a kind of metal oxide materials, and therefore, the gas sensitive research worker has proposed to adopt complex metal oxides to improve the selectivity of gas sensitive.Just be based on the susceptibility of cellular structure metals oxide compound to gas; And on complex metal oxides the basis that the selectivity and the susceptibility of gas is all increased; Exploitation pore passage structure composite metal oxide gas-sensing material, significant to the gas sensitive effect that improves the MOX gas sensitive.
Summary of the invention
The objective of the invention is development trend,, provide a kind of employing in-situ sintering growth method to synthesize In in conjunction with the susceptibility of porous road structure and complex phase MOX and characteristics optionally to gas sensitive
2O
3/ SnO
2The method of porous road structure gas sensitive.
The present invention adopts in-situ sintering to grow to prepare In
2O
3/ SnO
2Porous road structure gas sensitive.This method mainly is through to In
2O
3/ SnO
2The kinetics of complex phase MOX growth in situ is controlled in the regulation and control of gas sensitive sintering temperature and sintering atmosphere, thereby regulates and control the quantity of pore passage structure and coordination defective thereof, to obtain In
2O
3And SnO
2The porous road structure In that component proportions is different
2O
3/ SnO
2Gas sensitive.
The present invention realizes through following scheme:
At first with commercially available In
2O
3And SnO
2Powder is pressed into biscuit in the ratio of 4: 1 or 7: 3 or 3: 2 in punching block, biscuit is packed into carry out solid state sintering in the oxygen atmosphere sintering stove then, finally obtains porous road structure In
2O
3/ SnO
2Gas sensitive.
Raw material: commercially available In
2O
3And SnO
2Powder, powder size are between 50-500nm, and purity reaches 99.995%.
Punching block compacting: pressing pressure: 60-90Mpa; Dwell time: 2-5min.
In-situ sintering growth of oxygen atmosphere sintering condition:
1) oxygen that uses requires purity to be higher than 99.999%, and dew point is lower than-72 ℃;
2) sintering condition: temperature rise rate 50-500 ℃/h; Insulation is divided into two sections, and first section TR 600-700 ℃, second section TR 1250-1450 ℃; Soaking time 1-5 hour; Oxygen flow 3-8L/min.
The present invention obtains pass regular micron and submicron order pore passage structure In through the regulation and control to sintering temperature
2O
3/ SnO
2Gas sensitive increases specific surface area to improve gas sensing property, on the other hand through regulation and control/SnO through porous road structure on the one hand
2Amount improve selectivity to gas with various.The porous road structure gas sensitive that final acquisition is highly sensitive, selectivity is strong.The method that the present invention adopted has raw material and prepares simple, advantages such as cost is low, easy to control, production cleaning.
Embodiment
Embodiment 1:
With commercially available In
2O
3And SnO
2Powder (the In in the punching block that packs into
2O
3: SnO
2=4: 1), be 90MPa according to pressing pressure, the condition of pressurize 3min is pressed into biscuit; Then biscuit is put into sintering oven and carry out the in-situ sintering growth, sintering process is: be raised to 600 ℃ with 500 ℃/h temperature rise rate, behind the insulation 1h; Be warmed up to 1300 ℃ again, insulation 5h, last furnace cooling.Oxygen flow keeps 8L/min in temperature-rise period.
Embodiment 2:
With commercially available In
2O
3And SnO
2Powder (the In in the punching block that packs into
2O
3: SnO
2=7: 3), be 65MPa according to pressing pressure, the condition of pressurize 2min is pressed into biscuit; Then biscuit is put into sintering oven and carry out the in-situ sintering growth, sintering process is: be raised to 700 ℃ with 300 ℃/h temperature rise rate, behind the insulation 2h; Be warmed up to 1450 ℃ again, insulation 2h, preferably furnace cooling.Oxygen flow keeps 5L/min in temperature-rise period.
Embodiment 3:
With commercially available In
2O
3And SnO
2Powder (the In in the punching block that packs into
2O
3: SnO
2=3: 2), be 80MPa according to pressing pressure, the condition of pressurize 5min is pressed into biscuit; Then biscuit is put into sintering oven and carry out the in-situ sintering growth, sintering process is: be raised to 650 ℃ with 80 ℃/h temperature rise rate, behind the insulation 1h; Be warmed up to 1250 ℃ again, insulation 3h, preferably furnace cooling.Oxygen flow keeps 3L/min in temperature-rise period.
Claims (2)
1. In
2O
3/ SnO
2The preparation method of porous road structure gas sensitive is characterized in that: with commercially available In
2O
3And SnO
2Powder is pressed into biscuit in the ratio of 4: 1 or 7: 3 or 3: 2 in punching block, biscuit is packed into carry out solid state sintering in the oxygen atmosphere sintering stove then, obtains porous road structure In
2O
3/ SnO
2Gas sensitive; In-situ sintering growth of oxygen atmosphere sintering condition: temperature rise rate 50-500 ℃/h; Insulation is divided into two sections, and first section TR 600-700 ℃, second section TR 1250-1450 ℃; Soaking time 1-5 hour, oxygen flow 3-8L/min; Commercially available In
2O
3And SnO
2The powder size of powder is between 50-500nm, and purity reaches 99.995%; The pressing pressure of punching block compacting is: 60-90MPa, dwell time: 2-5min.
2. In according to claim 1
2O
3/ SnO
2The preparation method of porous road structure gas sensitive, the oxygen purity that uses when it is characterized in that sintering is higher than 99.999%, and dew point is lower than-72 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102741838A CN101967054B (en) | 2010-09-07 | 2010-09-07 | Preparation method of In2O3/SnO2 gas sensitive material with porous structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102741838A CN101967054B (en) | 2010-09-07 | 2010-09-07 | Preparation method of In2O3/SnO2 gas sensitive material with porous structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101967054A CN101967054A (en) | 2011-02-09 |
| CN101967054B true CN101967054B (en) | 2012-11-21 |
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|---|---|---|---|
| CN2010102741838A Expired - Fee Related CN101967054B (en) | 2010-09-07 | 2010-09-07 | Preparation method of In2O3/SnO2 gas sensitive material with porous structure |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103966697B (en) * | 2014-05-16 | 2016-04-27 | 北京化工大学 | A kind of p-n composite construction nano-metal-oxide and its preparation method and application |
| CN107352577B (en) * | 2017-06-28 | 2020-06-02 | 齐鲁工业大学 | Micro-nano net structure In2O3/SnO2Composite material and growing method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1990422A (en) * | 2005-12-26 | 2007-07-04 | 三井金属矿业株式会社 | Oxidate sintered body and method for making same, sputtering target and transparent conductive film |
| CN101201333A (en) * | 2006-04-21 | 2008-06-18 | 湖南大学 | Method for preparing ITO nanometer line and gas sensor thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6500225B2 (en) * | 1998-12-03 | 2002-12-31 | Sumitomo Chemical Company, Limited | Method for producing high density indium-tin-oxide sintered body |
-
2010
- 2010-09-07 CN CN2010102741838A patent/CN101967054B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1990422A (en) * | 2005-12-26 | 2007-07-04 | 三井金属矿业株式会社 | Oxidate sintered body and method for making same, sputtering target and transparent conductive film |
| CN101201333A (en) * | 2006-04-21 | 2008-06-18 | 湖南大学 | Method for preparing ITO nanometer line and gas sensor thereof |
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| Publication number | Publication date |
|---|---|
| CN101967054A (en) | 2011-02-09 |
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