CN108531891A - A kind of method and application preparing gas filtration film using molecule and technique for atomic layer deposition - Google Patents
A kind of method and application preparing gas filtration film using molecule and technique for atomic layer deposition Download PDFInfo
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- CN108531891A CN108531891A CN201810482129.9A CN201810482129A CN108531891A CN 108531891 A CN108531891 A CN 108531891A CN 201810482129 A CN201810482129 A CN 201810482129A CN 108531891 A CN108531891 A CN 108531891A
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- gas filtration
- filtration film
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- layer deposition
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- 238000000231 atomic layer deposition Methods 0.000 title claims abstract description 38
- 238000001914 filtration Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000151 deposition Methods 0.000 claims abstract description 11
- 230000008021 deposition Effects 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000005516 engineering process Methods 0.000 claims abstract description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 4
- 230000004888 barrier function Effects 0.000 claims abstract description 3
- 239000002052 molecular layer Substances 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 238000010926 purge Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 abstract description 5
- 239000012528 membrane Substances 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/403—Oxides of aluminium, magnesium or beryllium
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a kind of method and applications preparing gas filtration film using molecule and technique for atomic layer deposition.This approach includes the following steps：Tin oxide sensing film surface is deposited by one layer of MLD film using molecular-layer deposition technology, then calcining removes organic moiety therein, forms Al2O3Microporous barrier；Above-mentioned material is placed in the reaction chamber of ALD reactors, ALD films is formed by deposition, circulation A LD as needed is to get gas filtration film.It can pass through Al when gas filtration film test gas of the present invention2O3Layer micropore and the variation for leading to sensor resistance is contacted with sensitive layer, by continuing to stack un-densified ALD films, so that un-densified ALD films are with certain thickness and with the aperture smaller relative to first part, the diffusion for stopping macromolecular gas by duct resistance and the aperture constantly reduced, efficiently solves SnO2Sensor H2The problem of poor selectivity.
Description
Technical field
The present invention relates to hydrogen detection technique fields, and in particular to a kind of to prepare gas using molecule and technique for atomic layer deposition
The method of body filter membrane and application.
Background technology
Hydrogen (H2) it is best one of clean energy resource carrier, it can be used for rocket and motor vehicle fuel, metal smelt, glass system
It makes, semiconductor machining, the industries such as oil exploitation and daily-use chemical industry.But due to H2Tasteless, colorless and odorless, the mankind can not detect
It arrives, and the ignition energy of hydrogen is low, combustible range is wide, inflammable and explosive.As a result, in H2Production, storage and use during, need
It fast and accurately to detect.Therefore, exploitation can quickly detect H2, response is high, and selectivity is good, and response restores fast H2Sensor gesture
It must go.In recent years, a large amount of research all concentrates on developing various H using various suitable materials2Gas sensor.Metal oxygen
Compound semiconductor especially stannic oxide (SnO2) due to its cost-effectiveness height, it is simple in structure, be easily integrated, stability is good, spirit
The features such as sensitivity is high, fast response time, it has also become hydrogen gas senses most common material.
However, SnO2For material due to its simple sensor mechanism, it can react right with the chemically adsorbing oxygen of material surface
After conductive variation occurs, make its lack selectivity, have general quick property.For example, SnO2Material is to ethyl alcohol (C2H6O), an oxidation
Carbon (CO) and methane (CH4) there is cross-sensitivity.In order to overcome SnO2The disadvantage of the intrinsic shortage selectivity of material, especially
To H2Selectivity, at present have several strategies, respectively be use different operating temperatures, using noble metal or catalyst and
Sensor surface uses filter membrane.However, first two also has some adverse effects, such as cause to sense since temperature is higher
Layer crystallite dimension or surface texture variation and can cause when precious metal adsorption is tested gas metal film cracking, blistering and
Layering causes the decrease of metal structure.The present invention is combined by atomic layer deposition (ALD) technology and prepares gas filtration film, effectively
Ground controls the diffusion of macromolecular diameter gas, such as ethyl alcohol, propane, methane.
Invention content
For current SnO2The deficiency of sensing material selectivity utilizing molecule and original the purpose of the present invention is to provide a kind of
Sublayer deposition technique prepares the method for gas filtration film and application, the gas filtration film effectively control macromolecular diameter gas
Diffusion, it is good to the selectivity of hydrogen, and preparation process is simple, it is easy to operate.
To solve prior art problem, the technical solution that the present invention takes is：
A method of gas filtration film being prepared using molecule and technique for atomic layer deposition, is included the following steps：
Step 1, tin oxide sensing film surface is deposited by one layer of MLD film using molecular-layer deposition technology, then calcining removes it
In organic moiety, formed Al2O3Microporous barrier；
Step 2, step 1 material is placed in the reaction chamber of ALD reactors, ALD films is formed by deposition, are recycled as needed
ALD is to get gas filtration film.
It is that one layer of MLD film of deposition described in step 1 refers to first pouring Al (CH as improved3)3Steam, then use
After 20sccm nitrogen purges 10 seconds, glycol steam is poured, finally 20sccm nitrogen is used to purge 10 seconds.
It is that it refers to first pouring Al (CH that deposition, which forms ALD films, in step 2 as improved3)3Steam, then with 20sccm nitrogen
After air-blowing sweeps 10 seconds, H is poured2O steam finally uses 20sccm nitrogen to purge 10 seconds.
Application of the gas filtration film of above-mentioned preparation on hydrogen detection field.
It is a concentration of 0-5000ppm of the hydrogen detection as improved.
Advantageous effect：
Compared with prior art, first part of the present invention as gas filtration layer, test gas can pass through Al2O3Layer it is micro-
Hole and the variation for leading to sensor resistance is contacted with sensitive layer, stack un-densified ALD films by continuing so that un-densified
ALD films pass through duct resistance and constantly diminution with certain thickness and with the aperture smaller relative to first part
Aperture stop the diffusion of macromolecular gas, the sensor is with good stability and gas-selectively.The present invention is effective
Ground solves SnO2Sensor H2The problem of poor selectivity.
Description of the drawings
Fig. 1 is the structure chart of gas filtration membrane structure prepared by the present invention, wherein 1. tin oxide sensing membranes, 2.MLD films
Layer, 3.ALD film layers.
Specific implementation mode
The present invention is further described in detail below by specific embodiment.
Embodiment 1
A method of gas filtration film being prepared using molecule and technique for atomic layer deposition, is included the following steps：
Step 1, tin oxide sensing membrane is placed in the reaction chamber of MLD reactors, and heats 10min at 100 DEG C, keep reaction
The vacuum pressure of intracavitary is less than 1Torr；Al (CH are alternately poured into the reaction chamber of MLD reactors3)3Steam and ethylene glycol steam
Vapour deposits 250 cycles；400 DEG C of calcining 2h.
Step 2, Al (CH are alternately poured into the reaction chamber of ALD reactors3)3Steam and H2O steam, until ALD replaces
Number is to 36 cycles to get gas filtration film.
Embodiment 2
A method of gas filtration film being prepared using molecule and technique for atomic layer deposition, is included the following steps：
Step 1, tin oxide sensing membrane is placed in the reaction chamber of MLD reactors, and heats 10min at 100 DEG C, keep reaction
The vacuum pressure of intracavitary is less than 1Torr；Al (CH are alternately poured into the reaction chamber of MLD reactors3)3Steam and ethylene glycol steam
Vapour deposits 250 cycles；400 DEG C of calcining 2h.
Step 2, Al (CH are alternately poured into the reaction chamber of ALD reactors3)3Steam and H2O steam, until ALD replaces
Number is to 96 cycles to get gas filtration film.
Embodiment 3
A method of gas filtration film being prepared using molecule and technique for atomic layer deposition, is included the following steps：
Step 1, tin oxide sensing membrane is placed in the reaction chamber of MLD reactors, and heats 10min at 100 DEG C, keep reaction
The vacuum pressure of intracavitary is less than 1Torr；Al (CH are alternately poured into the reaction chamber of MLD reactors3)3Steam and ethylene glycol steam
Vapour deposits 250 cycles；400 DEG C of calcining 2h.
Step 2, Al (CH are alternately poured into the reaction chamber of ALD reactors3)3Steam and H2O steam, until ALD replaces
Number is to 106 cycles to get gas filtration film.
Embodiment 4
A method of gas filtration film being prepared using molecule and technique for atomic layer deposition, is included the following steps：
Step 1, tin oxide sensing membrane is placed in the reaction chamber of MLD reactors, and heats 10min at 100 DEG C, keep reaction
The vacuum pressure of intracavitary is less than 1Torr；Al (CH are alternately poured into the reaction chamber of MLD reactors3)3Steam and ethylene glycol steam
Vapour deposits 250 cycles；400 DEG C of calcining 2h.
Step 2, Al (CH are alternately poured into the reaction chamber of ALD reactors3)3Steam and H2O steam, until ALD replaces
Number is to 116 cycles to get gas filtration film.
500ppm C are tested respectively to the embodiment 1-4 gas filtration films prepared2H6O、1000ppm C3H8、1000ppm
H2、1000ppm CH4, acquired results are as shown in table 1 below.
The performance table of the gas filtration film prepared under 1 different condition of table
In conclusion gas filtration film of the present invention can pass through Al in test gas2O3Layer micropore and contacted with sensitive layer
The variation for leading to sensor resistance stacks un-densified ALD films by continuing so that un-densified ALD films have certain thickness
The aperture smaller relative to first part is spent and had, macromolecular gas is stopped by duct resistance and the aperture constantly reduced
The diffusion of body, the gas filtration film is with good stability and gas-selectively.The present invention efficiently solves SnO2Sensor
To H2The problem of poor selectivity.
The foregoing is only a preferred embodiment of the present invention, protection scope of the present invention is without being limited thereto, it is any ripe
Those skilled in the art are known in the technical scope of present disclosure, the letter for the technical solution that can be become apparent to
Altered or equivalence replacement are each fallen in protection scope of the present invention.
Claims (5)
1. a kind of method preparing gas filtration film using molecule and technique for atomic layer deposition, which is characterized in that including following step
Suddenly：Step 1, tin oxide sensing film surface is deposited by one layer of MLD film using molecular-layer deposition technology, then calcining removes wherein
Organic moiety, formed Al2O3Microporous barrier；Step 2, step 1 material is placed in the reaction chamber of ALD reactors, by depositing shape
At ALD films, circulation A LD as needed is to get gas filtration film.
2. the method according to claim 1 for preparing gas filtration film using molecule and technique for atomic layer deposition, feature
It is, one layer of MLD film of deposition described in step 1 refers to first pouring Al (CH3)3Steam, then purged 10 seconds with 20sccm nitrogen
Afterwards, glycol steam is poured, finally 20sccm nitrogen is used to purge 10 seconds.
3. the method according to claim 1 for preparing gas filtration film using molecule and technique for atomic layer deposition, feature
It is, it refers to first pouring Al (CH that deposition, which forms ALD films, in step 23)3Steam, then with after 20sccm nitrogen purging 10 seconds, rush
Enter H2O steam finally uses 20sccm nitrogen to purge 10 seconds.
4. application of the gas filtration film based on claim 1 preparation on hydrogen detection field.
5. application according to claim 4, which is characterized in that a concentration of 0-5000 ppm of the hydrogen detection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810482129.9A CN108531891A (en) | 2018-05-18 | 2018-05-18 | A kind of method and application preparing gas filtration film using molecule and technique for atomic layer deposition |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810482129.9A CN108531891A (en) | 2018-05-18 | 2018-05-18 | A kind of method and application preparing gas filtration film using molecule and technique for atomic layer deposition |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110820123A (en) * | 2019-11-15 | 2020-02-21 | 大连理工大学 | Porous color carbon fiber material and preparation method thereof |
| CN114166902A (en) * | 2021-12-07 | 2022-03-11 | 上海大学 | Preparation method of limited-area hydrogen sensor |
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| CN110820123A (en) * | 2019-11-15 | 2020-02-21 | 大连理工大学 | Porous color carbon fiber material and preparation method thereof |
| CN110820123B (en) * | 2019-11-15 | 2021-06-01 | 大连理工大学 | Porous color carbon fiber material and preparation method thereof |
| CN114166902A (en) * | 2021-12-07 | 2022-03-11 | 上海大学 | Preparation method of limited-area hydrogen sensor |
| CN114166902B (en) * | 2021-12-07 | 2023-10-20 | 上海大学 | Preparation method of finite field type hydrogen sensor |
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Application publication date: 20180914 |