CN101603956A - A kind of membrane-type gas enrichment device based on Kapton - Google Patents
A kind of membrane-type gas enrichment device based on Kapton Download PDFInfo
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- CN101603956A CN101603956A CNA2009100599854A CN200910059985A CN101603956A CN 101603956 A CN101603956 A CN 101603956A CN A2009100599854 A CNA2009100599854 A CN A2009100599854A CN 200910059985 A CN200910059985 A CN 200910059985A CN 101603956 A CN101603956 A CN 101603956A
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- thin film
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- kapton
- unsettled
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Abstract
The invention discloses a kind of membrane-type gas enrichment device based on Kapton, comprise a silicon substrate, a top cover and be arranged on silicon substrate and top cover between enrichment region, described enrichment region comprises unsettled diaphragm, thin film heater and adsorbent thin film, described unsettled diaphragm arrangement is on silicon substrate, described thin film heater and adsorbent thin film are arranged on the unsettled membrane surface, described top cover is provided with air intake opening and gas outlet, between unsettled diaphragm and top cover, form gas channel, it is characterized in that, described unsettled diaphragm adopts Kapton, and do not establish perforation, the air-flow in the gas channel is along its surface flow.Because Kapton has good toughness, so the size of polyimide diaphragm can be far longer than inorganic rigid material such as SiN, SiO
2Diaphragm and can not break, not only effectively increased the enrichment area, also taken into account air-flow simultaneously to contact, thereby improved accumulation rate with the effective of adsorbent thin film.
Description
Technical field
The present invention relates to the gas enricher technical field, be specifically related to a kind of membrane-type gas enrichment device based on Kapton.
Background technology
Detection to extremely low concentration atmosphere is the huge challenge that various analytical instrument face always, front end in gas chromatography (GC), mass spectrum (MS), ion mobility spectrometry (IMS), surface acoustic wave sensor (SAW), flame ion detector analytic systems such as (FID) is provided with 1-3 order of magnitude of detectivity lifting that enricher can make system, and enricher had become indispensable important composition parts of highly sensitive gas test system already.
Enricher mainly is made of sorbing material and well heater, and its principle of work is at first to make gas to be measured by sorbing material, and after enrichment a period of time, the heating sorbing material makes adsorbed gas desorption at short notice, thereby obtains high concentration gas.After the enrichment with enrichment before the ratio f of gas concentration be called accumulation rate, it is the most important index that characterizes enricher performance quality.The factor that influences accumulation rate mainly contains adsorption area, heating rate, gas flow, adsorption time etc.
Traditional enricher is a tubular structure, in fill sorbing material, twine heater strip outward or utilize stainless steel casing heating.This enricher thermal capacitance is big, the thermal efficiency is low, thereby it is slow to heat up, the spectrum peak width that gas desorption is attached, and accumulation ability is relatively poor.And adopt the novel enricher of micromachining technology (MEMS) preparation to compare with the tubular type enricher, because thermal capacitance is little, thermal efficiency height, the heating-up time can foreshorten to tens of milliseconds, therefore the transient state concentration that obtains is higher than traditional tubular type enricher far away, becomes the new research direction of enricher.Document Trends inAnalytical Chemistry, 2008,27 (4): 327-343 has carried out system summary to MEMS gas enricher present Research in recent years.
Document US P6171378; IEEE International Frequency Control Symposium, 1999,991-996; IEEE Sensor Journal, 2006,6 (3): 784-795 has reported the diaphragm type gas enricher of U.S. Sandia laboratory development, and its principal feature is to have adopted the SiN free standing structure film of low stress to do diaphragm, and diaphragm is provided with Pt thin film heater and chemisorbed film.Although this enricher has the fast advantage of the rate of heat addition, in order to guarantee the physical strength of SiN diaphragm, diaphragm small-sized only is 2.2 * 2.2mm
2, restricted the raising of accumulation rate.
Document Sensors ﹠amp; Actuators B, 2007,126:447-454 has reported the enricher of the CASPAR by name of US Naval Research Laboratory development, adopt Kapton (PI) to do diaphragm, and half area of PI film is a through hole, air-flow flows perpendicular to diaphragm, improves accumulation rate by improving gas flow (can reach 100L/min).But the CASPAR enricher is equivalent to a sieve, and air-flow flows through perpendicular to compass screen surface, has reduced with the effective of adsorbent thin film on the compass screen surface to contact, and is unfavorable for improving accumulation rate.And enricher is as the part of gas detector, and its gas flow must be subjected to the restriction of the suitable flow range of detector.For some detector, the advantage of the gas flow that CASPAR is big has no way of bringing into play.
Summary of the invention
Problem to be solved by this invention is: how a kind of membrane-type gas enrichment device is provided, this enricher can overcome more existing defectives in the prior art, not only keep the advantage that thermal capacitance is little, the rate of heat addition is fast, low in energy consumption, can also increase the adsorption area of enricher, increasing adsorbent thin film contacts with the effective of object gas, thereby improve total adsorbance of gas, obtain bigger bioaccumulation efficiency.
Technical matters proposed by the invention is to solve like this: a kind of membrane-type gas enrichment device based on Kapton is provided, comprise a silicon substrate, a top cover and be arranged on silicon substrate and top cover between enrichment region, described enrichment region comprises unsettled diaphragm, thin film heater and adsorbent thin film, described unsettled diaphragm arrangement is on silicon substrate, described thin film heater and adsorbent thin film are arranged on the unsettled membrane surface, described top cover is provided with air intake opening and gas outlet, between unsettled diaphragm and top cover, form gas channel, it is characterized in that, described unsettled diaphragm adopts Kapton, and do not establish perforation, the air-flow in the gas channel is along its surface flow.
According to the membrane-type gas enrichment device based on polyimide provided by the present invention, it is characterized in that unsettled diaphragm is of a size of 5 * 5mm
2～50 * 50mm
2
According to the membrane-type gas enrichment device based on Kapton provided by the present invention, it is characterized in that be provided with one deck heat conduction film between thin film heater and adsorbent thin film, material adopts silicon, aluminium nitride, silicon nitride or aluminium oxide.
According to the membrane-type gas enrichment device based on Kapton provided by the present invention, it is characterized in that described thin film heater is made of snakelike metallic film, material adopts a kind of in platinum, palladium, tungsten, molybdenum, tantalum and the alloy thereof.
Essence of the present invention is on the basis of U.S. Sandia enricher structure, replaces original SiN diaphragm with the polyimide diaphragm.Because polyimide is a kind of resistant to elevated temperatures polymeric material, and has flexibility, with inorganic diaphragm such as SiN, the SiO of rigidity
2Deng comparing, there is not the problem that causes rupture of diaphragm along with the increase of diaphragm size because of physical strength inadequately.Therefore, adopt polyimide to do diaphragm, the size of diaphragm can be done more, thereby improve accumulation rate.The CASPAR enricher of US Naval Research Laboratory has confirmed that polyimide does diaphragm and can realize bigger cavity structure (7.5 * 7.5mm
2), but the CASPAR enricher is equivalent to a sieve, and the polyimide diaphragm has the area of half to bore a hole, and air-flow flows through perpendicular to compass screen surface, has reduced with the effective of adsorbent thin film on the compass screen surface to contact, and is unfavorable for improving accumulation rate.The present invention combines the advantage of the above-mentioned two kinds of enrichers of the U.S., learn from other's strong points to offset one's weaknesses, utilize Kapton to make up plate enricher structure, when effectively increasing the enrichment area, also taken into account air-flow and contacted, thereby improved accumulation rate with the effective of adsorbent thin film.Enricher of the present invention has been simplified technological process, compares with U.S. Sandia enricher, does not need to adopt expensive chemical vapour deposition technique to prepare SiN or SiO
2Diaphragm; Compare with the CASPAR enricher, do not need to adopt the oxygen plasma etch technology on Kapton, to prepare perforation.
Description of drawings
Fig. 1 is the gas enricher structural representation based on the polyimide diaphragm of the present invention;
Fig. 2 is the gas enricher structural representation based on the polyimide diaphragm of band heat-conducting layer of the present invention.
Wherein, 1 is silicon base; 2 is unsettled diaphragm; 3 is thin film heater; 4 is adsorbent thin film; 5 is cavity; 6 is top cover; 7 is gas channel; 8 is air intake opening; 9 is the gas outlet; 10 are the heat conduction film.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further described:
Membrane-type gas enrichment device provided by the present invention, be to comprise a silicon substrate 1, a top cover 6 and be arranged on silicon substrate 1 and top cover 6 between enrichment region, enrichment region comprises unsettled diaphragm 2, thin film heater and adsorbent thin film, described unsettled diaphragm 2 is arranged on the silicon substrate, described thin film heater 3 and adsorbent thin film 4 are arranged on unsettled diaphragm 2 surfaces, described top cover is provided with air intake opening 8 and gas outlet 8, between unsettled diaphragm 2 and top cover 6, form gas channel 7, unsettled diaphragm 2 adopts Kapton, and do not establish perforation, air-flow in the gas channel 7 is along its surface flow, and wherein unsettled diaphragm is of a size of 5 * 5mm
2～50 * 50mm
2, between thin film heater 3 and adsorbent thin film 4, being provided with one deck heat conduction film 10, material adopts silicon, aluminium nitride, silicon nitride or aluminium oxide, and thin film heater 3 is made of snakelike metallic film, and material adopts a kind of in platinum, palladium, tungsten, molybdenum, tantalum and the alloy thereof.
Embodiment 1-polyimide diaphragm type gas enricher
Fig. 1 is the gas enricher structural representation based on the polyimide diaphragm, mainly comprises silicon base 1, unsettled diaphragm 2 (Kapton), thin film heater 3, adsorbent thin film 4, cavity 5, top cover 6 (glass roof), gas passage 7, air intake opening 8, gas outlet 9.The general thick silicon of about 500 μ m that adopts is as substrate.At first prepare Kapton at the silicon base 1 positive spin-coating method that adopts, 380 ℃ of curing under nitrogen atmosphere then, concrete technology is: the heating rate with 2 ℃/s is heated to 120 ℃, be incubated 15 minutes, be heated to 220 ℃ of insulations 30 minutes with same speed, be heated to 380 ℃ of insulations 1 hour at last.After the Kapton preparation is finished, deposit the thick metal platinum film of about 200nm thereon with magnetron sputtering method, and form snakelike thin film heater 3 through photoetching corrosion.Adopt reactive ion etching technology (DRIE) that the silicon base 1 of well heater below is eroded then, form the cavity 5 of the about 20mm * 20mm of area, dark 500 μ m, the polyimide of cavity top forms unsettled diaphragm 2.Adopt spraying process deposition one deck selective adsorption film 4 then on heating element 3, the thickness of film is several microns, and sorbing material decides according to the gas of want enrichment.At last in the front of diaphragm top cover 6 is set, main effect is the gas channel 7 that forms gas flow on adsorbent thin film, and the distance between top cover and the adsorbent thin film can guarantee that like this gas fully contacts with adsorbent thin film about 500 μ m.Glass roof is bigger slightly than the area of Kapton, adopts silicon glass bonding techniques closely to be connected with silicon base.Etch two pores respectively at the two ends of glass roof upside, as air intake opening 8 and gas outlet 9.
In this embodiment, adopt poly-methyl [3-(2-hydroxyl) phenyl] propyl-siloxane (PMPS) as the selective adsorption film, nerve gas simulant dimethyl methyl phosphonate (DMMP) is as test gas, and this enricher can be warmed up to 250 ℃ in the time of about 150ms, and accumulation rate can reach 280.
The polyimide diaphragm type gas enricher of embodiment 2-band heat-conducting layer
Fig. 2 is the polyimide diaphragm type gas enricher structural representation of band heat-conducting layer of the present invention.Its main implementation method is identical with example 1, and difference is after having prepared heating element 3, adopts radio frequency sputtering method to prepare one deck AlN film as heat conduction film 10 on heating element 3, the about 1 μ m of thickness, and then deposit adsorbent thin film 4 thereon.Because AlN has good heat conductivility, so the heating rate of this enricher is faster, can be warmed up to 250 ℃ in 70s, accumulation rate also increases, and is about 340.
Claims (4)
1, a kind of membrane-type gas enrichment device based on Kapton, comprise a silicon substrate, a top cover and be arranged on silicon substrate and top cover between enrichment region, described enrichment region comprises unsettled diaphragm, thin film heater and adsorbent thin film, described unsettled diaphragm arrangement is on silicon substrate, described thin film heater and adsorbent thin film are arranged on the unsettled membrane surface, described top cover is provided with air intake opening and gas outlet, between unsettled diaphragm and top cover, form gas channel, it is characterized in that, described unsettled diaphragm adopts Kapton, and do not establish perforation, the air-flow in the gas channel is along its surface flow.
2, the membrane-type gas enrichment device based on polyimide according to claim 1 is characterized in that, unsettled diaphragm is of a size of 5 * 5mm
2～50 * 50mm
2
3, the membrane-type gas enrichment device based on Kapton according to claim 1 is characterized in that, is provided with one deck heat conduction film between thin film heater and adsorbent thin film, and material adopts silicon, aluminium nitride, silicon nitride or aluminium oxide.
4, the membrane-type gas enrichment device based on Kapton according to claim 1 is characterized in that, described thin film heater is made of snakelike metallic film, and material adopts a kind of in platinum, palladium, tungsten, molybdenum, tantalum and the alloy thereof.
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| CNA2009100599854A CN101603956A (en) | 2009-07-14 | 2009-07-14 | A kind of membrane-type gas enrichment device based on Kapton |
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|---|---|---|---|
| CNA2009100599854A CN101603956A (en) | 2009-07-14 | 2009-07-14 | A kind of membrane-type gas enrichment device based on Kapton |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590398A (en) * | 2012-03-23 | 2012-07-18 | 电子科技大学 | Miniature gas enricher with membranes on double surfaces |
| CN106568640A (en) * | 2016-11-09 | 2017-04-19 | 西安交通大学 | Metal substrate-based micro-filling type enricher and preparation method thereof |
| CN107014666A (en) * | 2017-03-21 | 2017-08-04 | 西安交通大学 | A kind of micro gas enricher and preparation method thereof |
| WO2020162538A1 (en) * | 2019-02-08 | 2020-08-13 | 旭化成株式会社 | Sensor |
| JP2020128907A (en) * | 2019-02-08 | 2020-08-27 | 旭化成株式会社 | sensor |
| JP2021032844A (en) * | 2019-08-29 | 2021-03-01 | 旭化成株式会社 | sensor |
| JP2021092411A (en) * | 2019-12-09 | 2021-06-17 | 旭化成株式会社 | sensor |
-
2009
- 2009-07-14 CN CNA2009100599854A patent/CN101603956A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590398A (en) * | 2012-03-23 | 2012-07-18 | 电子科技大学 | Miniature gas enricher with membranes on double surfaces |
| CN106568640A (en) * | 2016-11-09 | 2017-04-19 | 西安交通大学 | Metal substrate-based micro-filling type enricher and preparation method thereof |
| CN106568640B (en) * | 2016-11-09 | 2019-03-01 | 西安交通大学 | A kind of miniature filled type enricher and preparation method based on metal substrate |
| CN107014666A (en) * | 2017-03-21 | 2017-08-04 | 西安交通大学 | A kind of micro gas enricher and preparation method thereof |
| CN107014666B (en) * | 2017-03-21 | 2019-06-11 | 西安交通大学 | A kind of micro gas enricher and preparation method thereof |
| WO2020162538A1 (en) * | 2019-02-08 | 2020-08-13 | 旭化成株式会社 | Sensor |
| JP2020128907A (en) * | 2019-02-08 | 2020-08-27 | 旭化成株式会社 | sensor |
| JP7145777B2 (en) | 2019-02-08 | 2022-10-03 | 旭化成株式会社 | sensor |
| JP2021032844A (en) * | 2019-08-29 | 2021-03-01 | 旭化成株式会社 | sensor |
| JP7269837B2 (en) | 2019-08-29 | 2023-05-09 | 旭化成株式会社 | sensor |
| JP2021092411A (en) * | 2019-12-09 | 2021-06-17 | 旭化成株式会社 | sensor |
| JP7273703B2 (en) | 2019-12-09 | 2023-05-15 | 旭化成株式会社 | sensor |
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