CN102074447A - Miniature ionizing gas analyzer, miniature gas ionizing device and manufacturing method thereof - Google Patents

Miniature ionizing gas analyzer, miniature gas ionizing device and manufacturing method thereof Download PDF

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Publication number
CN102074447A
CN102074447A CN 201010518022 CN201010518022A CN102074447A CN 102074447 A CN102074447 A CN 102074447A CN 201010518022 CN201010518022 CN 201010518022 CN 201010518022 A CN201010518022 A CN 201010518022A CN 102074447 A CN102074447 A CN 102074447A
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anode
gas
negative electrode
array
micro needlepoint
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董瑛
尤政
阮勇
赵嘉昊
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Tsinghua University
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Tsinghua University
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Abstract

The invention discloses a miniature ionizing gas analyzer, a miniature gas ionizing device and a manufacturing method thereof, which bring convenience to the field detection of a gas. The miniature gas ionizing device provided by the invention comprises a cathode, an anode, and a gas flowing-in/out channel formed between the cathode and the anode, wherein a micro-tip array is formed on or electrically connected to the anode. The miniature ionizing gas analyzer provided by the invention consists of the miniature gas ionizing device, a galvanometer and an adjustable DC voltage source, wherein the miniature gas ionizing device comprises the cathode, the anode, and the gas flowing-in/out channel formed between the cathode and the anode; the micro-tip array is also formed on or electrically connected to the anode; the anode and the cathode of the miniature gas ionizing device are connected with a positive electrode and a negative electrode of the adjustable DC voltage source; and the galvanometer is connected in series between the miniature gas ionizing device and the adjustable DC voltage source.

Description

Miniature ionization type gas analyzer, minitype gas ionization device and preparation method thereof
Technical field
The present invention relates to a kind of miniature ionization type gas analyzer, minitype gas ionization device and preparation method thereof.
Background technology
Gas detection technology has very important application at aspects such as industrial production, environmental protection, anti-terrorism safety.Gas detection technology can be divided into sensor technology and analytical instrumentation techniques two big classes.
Gas sensor is made up of chemical sensitive layer and physical sensors two parts, has advantages such as volume is little, power consumption is low, response speed is fast, can be used for on-the-spot gas detecting in real time.Owing to have certain selectivity, gas sensor can only detect a kind of or a class gas usually.Gas sensor is subjected to the influence of factors such as humidity, temperature and non-detected gas easily, so the lower problem of ubiquity precision.
Analytical instrument can provide certain physical energy, and for example light, heat, sound wave, electrostatic field etc., and certain spectrum signature by analytical gas molecule and energy interaction obtain the parameter about aerochemistry and physical property.Analytical instrument does not have selectivity, so the detection range broad.Gas detection technology antijamming capability based on Instrumental Analysis is stronger, has high-precision advantage than transducer.But problems such as that existing analytical instrument also exists usually is bulky, complicated operation, condition of work height are not suitable for gas on-site and detect.More than 500V, the existence of high voltage source makes the application of this gas analysis instrument be very restricted usually for for example existing ionization type gas analyzer, its operating voltage.
Summary of the invention
Main purpose of the present invention is to provide a kind of miniature ionization type gas analyzer, minitype gas ionization device and preparation method thereof, so that gas on-site detects.
Minitype gas ionization device provided by the invention comprises negative electrode and anode, is formed with the passage of gas turnover between above-mentioned negative electrode and the anode, wherein, forms or be electrically connected with the micro needlepoint array on the above-mentioned anode.
In a specific embodiment, be connected with the insulating spacer that two thickness equate between above-mentioned negative electrode and the anode, the thickness of above-mentioned insulating spacer is greater than the needle point height of above-mentioned micro needlepoint array, and above-mentioned micro needlepoint array places between two insulating spacers.
Preferable, the material of above-mentioned micro needlepoint array can be selected from conductor or semiconductor, and for example, its material can be selected from n type monocrystalline silicon.
Among the present invention, needle point is sharp more, thin more, close more good more.Preferable, the spacing of above-mentioned micro needlepoint array is less than 50 μ m, and tip diameter is less than 50nm.
Preferable, the thickness of above-mentioned two insulating spacers is 100~300 μ m.
Minitype gas ionization device provided by the present invention, anode adopts the micro needlepoint array structure, because can form strong inhomogeneous field near sharp-pointed needle point distributes, cause the corona discharge condition, even under the relatively low situation of voltage across poles, near the needle point local highfield also might surpass the field intensity of gas ionization, cause near the gas molecule ionization of needle point, and in gaps between electrodes, form avalanche effect, thereby the breakdown process of gas between intensifying ring makes self-maintained discharge to take place under relatively low voltage.Adopt the micro needlepoint array except reducing the ionization voltage, can also increase discharging current, this is because array structure has enlarged the surface area of anode, makes the ionization channels of gas molecule increase greatly, thereby can collect more electric charge, the sensitivity of current detecting is improved.
In the method for the above-mentioned minitype gas ionization device of making provided by the invention, the making of above-mentioned micro needlepoint array may further comprise the steps: silicon chip mixes and oxidation; Photoetching forms the array mask; Adopt the anisotropic wet corrosion to form the micro needlepoint array; Remove oxide layer.And also comprise: two insulating spacers are deployed in the both sides of micro needlepoint array, and are connected with anode and negative electrode respectively with the upper and lower surface of fluid sealant with two insulating spacers.
Miniature ionization type gas analyzer provided by the invention is made up of minitype gas ionization device, galvanometer and adjustable dc voltage source;
Above-mentioned minitype gas ionization device comprises negative electrode and anode, is formed with the passage of gas turnover between above-mentioned negative electrode and the anode, and also forms or be electrically connected with the micro needlepoint array on the anode;
The anode of wherein above-mentioned minitype gas ionization device links to each other with the positive and negative electrode in adjustable dc voltage source respectively with negative electrode, and above-mentioned galvanometer is connected between above-mentioned minitype gas ionization device and the adjustable dc voltage source.
Preferable, be connected with the insulating spacer that two thickness equate between above-mentioned negative electrode and the anode, the thickness of above-mentioned insulating spacer is greater than the needle point height of above-mentioned micro needlepoint array, and above-mentioned micro needlepoint array places between two insulating spacers.
Preferable, the material of above-mentioned micro needlepoint array can be selected from conductor or semiconductor, and for example, its material can be selected from n type monocrystalline silicon.
Preferable, the spacing of above-mentioned micro needlepoint array is less than 50 μ m, and tip diameter is less than 50nm.
Preferable, the thickness of above-mentioned two insulating spacers is 100~300 μ m.
Miniature ionization type gas analyzer provided by the present invention, owing to adopted the minitype gas ionization device, thereby make the volume of gas ionization device and operating voltage reduce greatly, making the ionization type gas analysis technology also can be used for gas on-site as transducer detects, kept simultaneously the high accuracy advantage of gas analysis instrument again, easy to carry and use.
Description of drawings
Fig. 1 is the structure chart of miniature ionization type gas analyzer provided by the invention;
Fig. 2 is the structure chart of minitype gas ionization device provided by the invention;
Fig. 3 is the making flow chart of micro needlepoint array provided by the invention.
Embodiment
Below in conjunction with Figure of description better embodiment of the present invention is done detailed description.
As shown in Figure 1, the disclosed a kind of miniature ionization type gas analyzer of preferred embodiment of the present invention is by a minitype gas ionization device, and an adjustable dc voltage source and a galvanometer are formed.Wherein the minitype gas ionization device is by a metallic cathode, and a micro needlepoint anode-array and two insulating spacers constitute.Anode links to each other with the positive and negative electrode in adjustable dc voltage source respectively with negative electrode, and galvanometer is connected in the circuit.
Fig. 2 is the structure chart of the minitype gas ionization device of present embodiment.As shown in Figure 2, this minitype gas ionization device comprises negative electrode 1, insulating spacer 2,3 and anode 4.In the present embodiment, negative electrode 1 adopts aluminum slice, and anode adopts n type monocrystalline silicon piece, the sheet glass that insulating spacer 2,3 adopts two thickness to equate.In the present embodiment, also be formed with micro needlepoint array 5 on the anode 4 between two insulating spacers 2,3.Wherein, present embodiment described " micro needlepoint array " is meant by miniature and (be meant that mainly tip diameter is nanoscale, and spacing is micron order; And among the present invention, needle point is sharp more, thin more, close more good more) similar in needle point and spacing conductor or the integrally-built general designation formed of semiconductor about equally.Optionally, the making of this micro needlepoint array can adopt wet corrosion technique to make, the process flow diagram of corrosion as shown in Figure 3:
(a) choose n type silicon chip as base material;
(b) oxidation is to form oxide layer on n type silicon chip;
(c) photoetching forms the quadrate array mask;
(d) adopt the anisotropic wet corrosion to form micro needlepoint array (corrosive liquid can adopt 40% KOH);
(e) remove oxide layer.
Treat that above-mentioned micro needlepoint matrix-like is formed in after the silicon chip, two sheet glass sheets are deployed in the both sides of micro needlepoint array, and be connected with aluminium flake and silicon chip respectively with the upper and lower surface of fluid sealant with two sheet glass sheets.So, the micro needlepoint array that then forms on the anode is sandwiched between two sheet glass, and the gap between two sheet glass is then as the passage of gas turnover.
Anode in little ionization device in the present embodiment adopts silica-based anisotropic wet etching process to make.Before carrying out wet etching, to mix to silicon chip earlier, so that substrate obtains good electrical conductivity.From reducing ionization voltage and improving the angle of current detecting sensitivity, wish that needle point is sharp-pointed more good more, array density is the bigger the better.Time and temperature, stirring condition and post-processing technologies such as employing oxidation or annealing by appropriate design etching mask, corrosive liquid concentration, corrosion can make needle point and array density reach requirement; In the present embodiment, preferable, the needle point tip diameter of micro needlepoint array between 10~50nm, needle tip spacing between 30~50 μ m, needle point height between 10~30 μ m; In an instantiation, can make a needle point height according to above-mentioned steps (a)~(e) and be about 20 μ m, spacing is about 40 μ m, and tip diameter is about the micro needlepoint array of 30nm.On the other hand, preferable, the distance between negative electrode and the anode should be controlled in 100~300 mu m ranges (for example: the thickness of choosing two insulating spacers is 200 μ m).
What deserves to be explained is: in other embodiments; also the micro needlepoint array that is made into by other material and technology directly can be fixed on the existing anode on the position between two insulating barriers; and electrically connect between micro needlepoint array after fixing and the anode; these variations are all the thinkable easily conversion of those skilled in the art, all belong to protection scope of the present invention.
Above-mentioned miniature ionization type gas analyzer when work, allows gas pass through between the electrode of minitype gas ionization device earlier, behind steady air current, open the adjustable dc voltage source, operating voltage from the low-key to the height, is measured corresponding discharging current with galvanometer simultaneously.When discharging current increased suddenly, the operating voltage of this moment was ionisation of gas voltage.Different gas has different ionization voltages, the size of discharging current relevant with the concentration of gas (hence one can see that: the output voltage range in adjustable dc voltage source has determined the detectable gas scope of miniature ionization type gas analyzer) during ionization.Therefore, the voltage during by detection ionization and the electric current of generation just can detect the type and the concentration of gas.
Among the present invention, the ionization type gas analyzer mainly comprises gas ionization device (corresponding above-mentioned minitype gas ionization device), voltage control part (corresponding above-mentioned adjustable dc voltage source) and current measurement part (corresponding above-mentioned galvanometer), major function is the electrostatic field that the field intensity continuous variable is provided by the voltage of regulating the electrode two ends, and measure discharging current under different operating voltage obtaining the ionisation of gas spectrum, thereby analyze the type and the concentration of gas.And miniature ionization type gas analyzer provided by the present invention, owing to adopted the minitype gas ionization device, thereby make the volume of gas ionization device and operating voltage reduce greatly, make the ionization type gas analysis technology also can as transducer, be easy to carry and can be used for gas on-site and detect, kept the high accuracy advantage of gas analysis instrument simultaneously again.
More than; only be preferred embodiment of the present invention, but protection scope of the present invention is not limited thereto, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection range that claim was defined.

Claims (9)

1. a minitype gas ionization device comprises negative electrode and anode, is formed with the passage of gas turnover between described negative electrode and the anode, it is characterized in that, forms or be electrically connected with the micro needlepoint array on the described anode.
2. minitype gas ionization device according to claim 1, it is characterized in that, be connected with the insulating spacer that two thickness equate between described negative electrode and the anode, the thickness of described insulating spacer is greater than the needle point height of described micro needlepoint array, and described micro needlepoint array places between two insulating spacers.
3. minitype gas ionization device according to claim 1 and 2 is characterized in that, the material of described micro needlepoint array is conductor or semiconductor.
4. minitype gas ionization device according to claim 3 is characterized in that, the needle tip spacing in the described micro needlepoint array is less than 50 μ m, and the needle point tip diameter is less than 50nm.
5. the method for making such as claim 1,2,3 or 4 described minitype gas ionization devices is characterized in that the making of described micro needlepoint array may further comprise the steps:
Silicon chip mixes and oxidation;
Photoetching forms the array mask;
Adopt the anisotropic wet corrosion to form the micro needlepoint array;
Remove oxide layer.
6. manufacture method according to claim 5 is characterized in that, also comprises:
The insulating spacer that two thickness are equal is deployed in the both sides of micro needlepoint array, and is connected with anode and negative electrode respectively with the upper and lower surface of fluid sealant with two insulating spacers.
7. a miniature ionization type gas analyzer is characterized in that, is made up of minitype gas ionization device, galvanometer and adjustable dc voltage source;
Described minitype gas ionization device comprises negative electrode and anode, is formed with the passage of gas turnover between described negative electrode and the anode, and also forms or be electrically connected with the micro needlepoint array on the anode;
The anode of wherein said minitype gas ionization device links to each other with the positive and negative electrode in adjustable dc voltage source respectively with negative electrode, and described galvanometer is connected between described minitype gas ionization device and the adjustable dc voltage source.
8. miniature ionization type gas analyzer according to claim 7, it is characterized in that, be connected with the insulating spacer that two thickness equate between described negative electrode and the anode, the thickness of described insulating spacer is greater than the needle point height of described micro needlepoint array, and described micro needlepoint array places between two insulating spacers.
9. according to claim 7 or 8 described miniature ionization type gas analyzers, it is characterized in that the material of described micro needlepoint array is conductor or semiconductor;
Needle tip spacing in the described micro needlepoint array is less than 50 μ m, and the needle point tip diameter is less than 50nm.
CN 201010518022 2010-06-30 2010-10-25 Miniature ionizing gas analyzer, miniature gas ionizing device and manufacturing method thereof Pending CN102074447A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103760221A (en) * 2014-02-14 2014-04-30 厦门大学 Needle tip discharge device for solid surface denudation
CN104062350A (en) * 2014-05-07 2014-09-24 西安交通大学 Multi-electrode microsensor for detecting copper metal vapor concentration
CN104792676A (en) * 2015-04-27 2015-07-22 无锡信大气象传感网科技有限公司 Method for measuring nanoparticle concentration of air with ionization method
CN106986302A (en) * 2017-02-24 2017-07-28 西安交通大学 A kind of micron order semiconductor transducer and preparation method thereof
CN108120904A (en) * 2016-11-30 2018-06-05 全球能源互联网研究院 A kind of SF6 gas sensors and preparation method thereof
CN114216808A (en) * 2021-11-18 2022-03-22 中国人民解放军军事科学院国防工程研究院工程防护研究所 Gas impurity detection device and detection method

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009066220A1 (en) * 2007-11-20 2009-05-28 Nxp B.V. Electrode for an ionization chamber and method producing the same

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Publication number Priority date Publication date Assignee Title
WO2009066220A1 (en) * 2007-11-20 2009-05-28 Nxp B.V. Electrode for an ionization chamber and method producing the same

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103760221A (en) * 2014-02-14 2014-04-30 厦门大学 Needle tip discharge device for solid surface denudation
CN103760221B (en) * 2014-02-14 2015-12-02 厦门大学 A kind of needle point electric discharge device degraded for solid surface
CN104062350A (en) * 2014-05-07 2014-09-24 西安交通大学 Multi-electrode microsensor for detecting copper metal vapor concentration
CN104062350B (en) * 2014-05-07 2017-04-19 西安交通大学 Multi-electrode microsensor for detecting copper metal vapor concentration
CN104792676A (en) * 2015-04-27 2015-07-22 无锡信大气象传感网科技有限公司 Method for measuring nanoparticle concentration of air with ionization method
CN108120904A (en) * 2016-11-30 2018-06-05 全球能源互联网研究院 A kind of SF6 gas sensors and preparation method thereof
CN106986302A (en) * 2017-02-24 2017-07-28 西安交通大学 A kind of micron order semiconductor transducer and preparation method thereof
CN114216808A (en) * 2021-11-18 2022-03-22 中国人民解放军军事科学院国防工程研究院工程防护研究所 Gas impurity detection device and detection method

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Application publication date: 20110525