CN1749745A - Electric heating double parameter detecting chip and preparation method thereof - Google Patents
Electric heating double parameter detecting chip and preparation method thereof Download PDFInfo
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- CN1749745A CN1749745A CNA2004100746757A CN200410074675A CN1749745A CN 1749745 A CN1749745 A CN 1749745A CN A2004100746757 A CNA2004100746757 A CN A2004100746757A CN 200410074675 A CN200410074675 A CN 200410074675A CN 1749745 A CN1749745 A CN 1749745A
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Abstract
Electric heating double parameter detecting chip of the present invention and preparation method thereof belongs to field of sensing technologies, the particularly detection of certain chemical substance in air, water and the biosome.This chip comprises substrate, support diaphragm, measure temperature sensor that thermal parameter changes, measure potential electrode that electrical quantity changes and with the measured object effect after certain sensitive membrane reversible or irreversible physicochemical change can take place; Its chip substrate is a shaped as frame, there is a through hole in the centre, its upper surface affixed one supports diaphragm, support the diaphragm upper surface central part, be positioned at the center of through hole, be connected with a sensitive membrane, supporting between diaphragm upper surface and the sensitive membrane lower surface, at least one pair of potential electrode and at least one temperature sensor are arranged.The present invention detects two parameters of electric heating simultaneously, has improved detection accuracy; Because of adopting the micro-electronic mechanical system technique preparation, detection system cost, volume and power consumption have been reduced; And making the thermal capacity of diaphragm very little, the measuring accuracy of thermal parameter improves greatly.
Description
Technical field
The invention belongs to field of sensing technologies, particularly relate to the detection of certain chemical substance in air, water and the biosome, as the residues of banned pesticides in the toxin in airborne flammable explosive gas, toxic gas, chemical and biological weapons, explosive and the water, pollutant and the food, veterinary drug and adjuvant etc.
Background technology
Progress and development of science and technology along with society, the requirement of environmentally safe property of people and life comfortableness is more and more higher, safety to air, water source and food is more and more paid attention to, and these all relate to the detection to some chemical substance in air, water and the biosome.Present detection means mainly is a chemical analysis method, needs the sampling back to carry out in specialized laboratory, and analysis time is long, and the cost height is very inconvenient.Some chemical substances also can be utilized strip/reagent to carry out the scene and detect, but this method reliability is poor, and need the professional to operate.At present, but the detecting instrument of some works on the spot is arranged also, but exist the cost height, problem such as volume is big, power consumption is high and detection accuracy is low.
In recent years, some high molecule sensitivity materials are widely used in the detection of residues of banned pesticides, veterinary drug in toxin, pollutant and the food in flammable explosive gas, toxic gas and the water.Mainly can be divided into following several according to detecting the sensor of principle based on macromolecular material: 1, impedance based sensor, detect measured object according to macromolecular material electric capacity or changes in resistance.2, semiconductor type sensor detects measured object according to the variation of its semiconductor parameter (as diode characteristic) behind the macromolecular material contact measured object.3, mode of resonance sensor causes the device resonance frequency to change owing to quality or elastic modulus behind the macromolecular material absorption measured matter change, and detects measured object by the change of measuring resonance frequency.4, electrochemical sensor, the specific function relation detection measured object according to electrode potential or electric current and measured object concentration can be divided into potentiometer type, galvanometer formula etc.5, calorimetric type sensor, cardinal principle are to measure the temperature variation that causes in physics between measured object and the macromolecular material or the chemical process.6, optical fiber sensor, its principle are based on the variation of the propagation of sensitive thin film glazing, absorption or emission characteristics, and finally export an optical signalling.Possible structure comprises: optronics type, core type, incrusting type, interferometer and other Fibre Optical Sensor.
Since can with the multiple material that has of certain high molecule sensitivity material generation physics or chemical reaction, so, make that owing to selectivity is not high overall performance can not be satisfactory though these sensor sensitivity based on the high molecule sensitivity material are very high.
Summary of the invention
The objective of the invention is to propose a kind of electric heating double parameter detecting chip based on microelectromechanical systems (MEMS) technology, by measuring the variation of sensitive material electrical quantity and thermal parameter simultaneously, improved selectivity, and then improved the reliability that detects measured object.
A further object of the present invention provides a kind of preparation method, makes electric heating double parameter detecting chip of the present invention can adopt this method to realize preparation low-costly and in high volume.
For achieving the above object, technical scheme of the present invention is as follows:
A kind of electric heating double parameter detecting chip, based on microelectromechanical systems (MEMS) technology, comprise substrate, passive support diaphragm, measure temperature sensor that thermal parameter changes, measure potential electrode that electrical quantity changes and with the measured object effect after certain sensitive membrane reversible or irreversible physicochemical change can take place; It is characterized in that: chip substrate is a shaped as frame, there is a through hole in the centre, its upper surface affixed one supports diaphragm, support the diaphragm upper surface central part, be positioned at the center of through hole, be connected with a sensitive membrane, between the upper surface and sensitive membrane lower surface that support diaphragm, at least one pair of potential electrode and at least one temperature sensor arranged.
Described electric heating double parameter detecting chip, it also comprises at least one heating electrode that is used for the control chip working temperature, between the upper surface and sensitive membrane lower surface that support diaphragm; Heating electrode is made by metallic film or by polysilicon.
Described electric heating double parameter detecting chip, it also comprises one deck dielectric film at least, is supporting between diaphragm and the sensitive membrane, described at least one pair of potential electrode is fixed in the upper surface or the lower surface of dielectric film; At least one temperature sensor is fixed in the lower surface or the upper surface of dielectric film; At least one heating electrode is fixed in the lower surface or the upper surface of dielectric film.
Described electric heating double parameter detecting chip, its described potential electrode is one or more pairs of interdigital electrodes, is made by platinum/tantalum films material.
Described electric heating double parameter detecting chip, its described support diaphragm is complete diaphragm or the outstanding film that supported by beam; The material that supports diaphragm and dielectric film is a kind of in silicon, monox, silicon nitride, metal, metal oxide, pottery, the glass, or the composite membrane formed of above-mentioned various material.
Described electric heating double parameter detecting chip, its described temperature sensor is metallic film thermal resistance or polysilicon thermal resistance; Or thermocouple or the thermal reactor formed by metal, silicon or metallic compound; Or by other temperature sensor of microelectronic technique preparation.
Described electric heating double parameter detecting chip, its described sensitive membrane is made of at least a certain component reversible or irreversible physicochemical change that can take place under the measured object effect, and its area is less than substrate through vias area suitable for reading.
Described electric heating double parameter detecting chip, its described sensitive membrane, it is metal-oxide film, organic polymer thin film, a kind of in the biological membrane preferably is embedded with the organic membrane of metal oxide nanoparticles, metal oxide nano-wire, metal nanoparticle, metal nanometer line, carbon black nano particle, carbon nano-tube or enzyme.
Described electric heating double parameter detecting chip, the electric heating parameter signal of its chip output is a differential signal.
Described electric heating double parameter detecting chip, its described chip is silicon materials, can form array chip.
A kind of preparation method of electric heating double parameter detecting chip as claimed in claim 1 adopts microelectromechanical systems (MEMS) technology to make, and comprising:
1, preparing substrate: the twin polishing silicon chip in 100 crystal orientation;
2, preparation support membrane:, adopt O in furnace temperature 1150
2/ H
2O/O
2The monox of thermal oxide 300nm under the alternating oxidation condition, the low stress nitride silicon of low-pressure chemical vapor deposition (LPCVD) 200nm;
3, preparation temperature sensor: the photoetching platinum resistance, peel off the preparation platinum resistance, as temperature sensor;
4, the potential electrode of electrical quantity is measured in preparation: the photoetching interdigital electrode, and sputter platinum/tantalum (Pt/Ta) 200nm peels off the preparation interdigital electrode, as the potential electrode of measuring electrical quantity;
5, form diaphragm structure: the photoetching back surface corrosion window, with sulfur hexafluoride (SF
6) reactive ion etching (RIE) silicon nitride film, with buffered hydrofluoric acid solution (BHF) corrosion oxidation silicon, use potassium hydroxide (KOH) solution anisotropic etch silicon to form diaphragm structure then;
6, preparation sensitive membrane: be dissolved in organic polymer in the solvent and mix an amount of charcoal nano particle, adopt the way of biological point sample that it is deposited on the chip;
7, sliver, encapsulation.
The preparation method of described electric heating double parameter detecting chip, the low-pressure chemical vapor deposition of its (2) step, condition is a furnace temperature 850, the source is silane SiH
4, ammonia NH
3And nitrogen N
2
The preparation method of described electric heating double parameter detecting chip, its (3), the order of (4) step can exchange or merge into a step process; Wherein photoetching is positive photoresist, and film thickness is between 1 micron to 5 microns.
The preparation method of described electric heating double parameter detecting chip, the photoetching back surface corrosion window of its (5) step is a positive photoresist, film thickness is between 2 microns to 5 microns.
The preparation method of described electric heating double parameter detecting chip, its (6), the order of (7) step can exchange.
The preparation method of described electric heating double parameter detecting chip, its processing technology are body silicon processing technique or Surface-micromachining process or body silicon processing technique and the combining of Surface-micromachining process.
Advantage of the present invention and good effect:
The present invention can detect two parameters of electric heating simultaneously, has improved detection accuracy greatly; The present invention adopts the preparation of microelectromechanical systems (MEMS) technology, has reduced cost, volume and the power consumption of detection system; What is more important, the present invention adopts the preparation of microelectromechanical systems (MEMS) technology to make that the thermal capacity of diaphragm is very little, and the measuring accuracy of thermal parameter improves greatly.
Description of drawings
Fig. 1 is the structural representation of electric heating double parameter detecting chip of the present invention;
Fig. 2 is several different structure synoptic diagram of electric heating double parameter detecting chip of the present invention; Wherein:
(a) structure shown in is complete support diaphragm 2; (b) be depicted as the support diaphragm 2 that hangs membrane structure; (c) structure shown in is complete support diaphragm 2; (d) be depicted as the support diaphragm 2 that hangs membrane structure;
Fig. 3 is preparation technology's schematic flow sheet of electric heating double parameter detecting chip.
Specific implementation
As shown in Figure 1, be the structural representation of electric heating double parameter detecting chip of the present invention.1 is substrate among the figure, and 2 for supporting diaphragm, and 3 for being used for the electrode of electric parameter measurement, and 4 for being used for the temperature sensor of thermal parameter measurement, and 5 is sensitive membrane.Substrate 1 is a shaped as frame, and material is a silicon chip, and there is a through hole 6 in the centre.The upper surface of substrate 1 affixed one supports diaphragm 2, supporting diaphragm 2 is the composite membranes that constitute with monox and silicon nitride, its upper surface central part, be positioned at the center of through hole 6, be connected with a sensitive membrane 5, its area is less than through hole 6 area suitable for reading, and sensitive membrane 5 is the organic polymer thin films that are embedded with the charcoal nano particle.Between the upper surface and sensitive membrane 5 lower surfaces that support diaphragm 2, the temperature sensor 4 that platinum/tantalum (Pt/Ta) interdigital electrode 3 is arranged and prepare with film platinum resistor.Interdigital electrode 3 is as the electrode of measuring electrical quantity, and temperature sensor 4 is used for measuring thermal parameter, and platinum resistance also is the well heater of control chip working temperature simultaneously.
As shown in Figure 2, several different structure synoptic diagram for electric heating double parameter detecting chip of the present invention, wherein structure shown in (a) is complete support diaphragm 2, and the electrode 3, the temperature sensor 4 (and heating electrode) that are used for electric parameter measurement are in the same one deck that supports diaphragm 2; (b) be depicted as the support diaphragm 2 that hangs membrane structure, the electrode 3, the temperature sensor 4 (and heating electrode) that are used for electric parameter measurement are in the same one deck that supports diaphragm 2; (c) structure shown in is complete support diaphragm 2, is used for the electrode 3 of electric parameter measurement, the different layers that temperature sensor 4 (and heating electrode) is in diaphragm, is isolated by dielectric film 7 each other; (d) be depicted as the support diaphragm 2 that hangs membrane structure, be used for the electrode 3 of electric parameter measurement, the different layers that temperature sensor 4 (and heating electrode) is in diaphragm, isolate by dielectric film 7 each other.Dielectric film 7 and support diaphragm 2 all are the composite membranes that constitutes with monox and silicon nitride.
The material that supports diaphragm 2 and dielectric film 7 is a kind of in silicon, monox, silicon nitride, metal, metal oxide, pottery, the glass, or the composite membrane formed of above-mentioned various material.
Temperature sensor 4 (and heating electrode) is metallic film thermal resistance or polysilicon thermal resistance; Or thermocouple or the thermal reactor formed by metal, silicon or metallic compound; Or by other temperature sensor of microelectronic technique preparation.
Electric heating double parameter detecting chip of the present invention, the electric heating parameter signal of output is a differential signal, can form array chip.
As shown in Figure 3, preparation technology's schematic flow sheet for electric heating double parameter detecting chip, wherein (1) is preparing substrate, (2) be the preparation support membrane, (3) be preparation temperature sensor and the potential electrode of measuring electrical quantity, (4) for forming diaphragm structure, (5) are the preparation sensitive membrane, and (6) are sliver, encapsulation.
Be the representative technological process of preparation electric heating double parameter detecting chip below:
1) preparing substrate: 300 micron thickness, the twin polishing silicon chip in 100 crystal orientation.
2) preparation support membrane: (furnace temperature 1150 adopts O to the monox of thermal oxide 300nm
2/ H
2O/O
2Alternating oxidation), (furnace temperature 850, source are silane SiH to the low stress nitride silicon of low-pressure chemical vapor deposition (LPCVD) 200nm
4, ammonia NH
3And nitrogen N
2).
3) preparation platinum resistance and interdigital electrode: photoetching platinum resistance and interdigital electrode (positive photoresist, film thickness is between 1 micron to 5 microns, representative value is 2 microns), sputter platinum/tantalum (Pt/Ta) (200nm) is peeled off preparation platinum resistance and interdigital electrode respectively as temperature sensor and measure the potential electrode of electrical quantity.
4) form diaphragm structure: photoetching back surface corrosion window (positive photoresist, film thickness are between 2 microns to 5 microns, and representative value is 4 microns), with sulfur hexafluoride (SF
6) reactive ion etching (RIE) silicon nitride film, with buffered hydrofluoric acid solution (BHF) corrosion oxidation silicon, use potassium hydroxide (KOH) solution anisotropic etch silicon to form diaphragm structure then.
5) preparation sensitive membrane: be dissolved in organic polymer in the solvent and mix an amount of carbon nano-particle, adopt the way of biological point sample that it is deposited on the chip.
6) sliver, encapsulation.
Claims (16)
1, a kind of electric heating double parameter detecting chip, based on microelectromechanical systems (MEMS) technology, comprise substrate, passive support diaphragm, measure temperature sensor that thermal parameter changes, measure potential electrode that electrical quantity changes and with the measured object effect after certain sensitive membrane reversible or irreversible physicochemical change can take place; It is characterized in that: chip substrate is a shaped as frame, there is a through hole in the centre, its upper surface affixed one supports diaphragm, support the diaphragm upper surface central part, be positioned at the center of through hole, be connected with a sensitive membrane, between the upper surface and sensitive membrane lower surface that support diaphragm, at least one pair of potential electrode and at least one temperature sensor arranged.
2, electric heating double parameter detecting chip as claimed in claim 1 is characterized in that: also comprise at least one heating electrode that is used for the control chip working temperature, between the upper surface and sensitive membrane lower surface that support diaphragm; Heating electrode is made by metallic film or by polysilicon.
3, electric heating double parameter detecting chip as claimed in claim 1 is characterized in that: also comprise one deck dielectric film at least, supporting between diaphragm and the sensitive membrane that described at least one pair of potential electrode is fixed in the upper surface or the lower surface of dielectric film; At least one temperature sensor is fixed in the lower surface or the upper surface of dielectric film; At least one heating electrode is fixed in the lower surface or the upper surface of dielectric film.
4, as claim 1 or 3 described electric heating double parameter detecting chips, it is characterized in that: described potential electrode is one or more pairs of interdigital electrodes, is made by platinum/tantalum films material.
5, as claim 1 or 3 described electric heating double parameter detecting chips, it is characterized in that: described support diaphragm is complete diaphragm or the outstanding film that supported by beam; The material that supports diaphragm and dielectric film is a kind of in silicon, monox, silicon nitride, metal, metal oxide, pottery, the glass, or the composite membrane formed of above-mentioned various material.
6, electric heating double parameter detecting chip as claimed in claim 1 is characterized in that: described temperature sensor is metallic film thermal resistance or polysilicon thermal resistance; Or thermocouple or the thermal reactor formed by metal, silicon or metallic compound; Or by other temperature sensor of microelectronic technique preparation.
7, electric heating double parameter detecting chip as claimed in claim 1, it is characterized in that: described sensitive membrane, be made of at least a certain component reversible or irreversible physicochemical change that can take place under the measured object effect, its area is less than substrate through vias area suitable for reading.
8, as claim 1 or 7 described electric heating double parameter detecting chips, it is characterized in that: described sensitive membrane, it is metal-oxide film, organic polymer thin film, a kind of in the biological membrane preferably is embedded with the organic membrane of metal oxide nanoparticles, metal oxide nano-wire, metal nanoparticle, metal nanometer line, carbon black nano particle, carbon nano-tube or enzyme.
9, electric heating double parameter detecting chip as claimed in claim 1 is characterized in that: the electric heating parameter signal of chip output is a differential signal.
10, electric heating double parameter detecting chip as claimed in claim 1 is characterized in that: described chip is silicon materials, can form array chip.
11, a kind of preparation method of electric heating double parameter detecting chip as claimed in claim 1 adopts microelectromechanical systems (MEMS) technology to make; It is characterized in that, comprising:
(1) preparing substrate: the twin polishing silicon chip in 100 crystal orientation;
(2) preparation support membrane:, adopt O in furnace temperature 1150
2/ H
2O/O
2The monox of thermal oxide 300nm under the alternating oxidation condition, the low stress nitride silicon of low-pressure chemical vapor deposition (LPCVD) 200nm;
(3) preparation temperature sensor: the photoetching platinum resistance, peel off the preparation platinum resistance, as temperature sensor;
(4) potential electrode of electrical quantity is measured in preparation: the photoetching interdigital electrode, and sputter platinum/tantalum (Pt/Ta) 200nm peels off the preparation interdigital electrode, as the potential electrode of measuring electrical quantity;
(5) form diaphragm structure: the photoetching back surface corrosion window, with sulfur hexafluoride (SF
6) reactive ion etching (RIE) silicon nitride film, with buffered hydrofluoric acid solution (BHF) corrosion oxidation silicon, use potassium hydroxide (KOH) solution anisotropic etch silicon to form diaphragm structure then;
(6) preparation sensitive membrane: be dissolved in organic polymer in the solvent and mix an amount of carbon nano-particle, adopt the way of biological point sample that it is deposited on the chip;
(7) sliver, encapsulation.
12, the preparation method of electric heating double parameter detecting chip as claimed in claim 11 is characterized in that: the low-pressure chemical vapor deposition of (2) step, condition are furnace temperature 850, and the source is silane SiH
4, ammonia NH
3And nitrogen N
2
13, the preparation method of electric heating double parameter detecting chip as claimed in claim 11 is characterized in that: (3), the order of (4) step can exchange or merge into a step process; Wherein photoetching is positive photoresist, and film thickness is between 1 micron to 5 microns.
14, the preparation method of electric heating double parameter detecting chip as claimed in claim 11 is characterized in that: the photoetching back surface corrosion window of (5) step is a positive photoresist, and film thickness is between 2 microns to 5 microns.
15, the preparation method of electric heating double parameter detecting chip as claimed in claim 11 is characterized in that: (6), the order of (7) step can exchange.
16, the preparation method of electric heating double parameter detecting chip as claimed in claim 11 is characterized in that: processing technology is body silicon processing technique or Surface-micromachining process or body silicon processing technique and the combining of Surface-micromachining process.
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| CN101089908B (en) * | 2006-06-13 | 2010-05-26 | 富士施乐株式会社 | Sensor |
| CN101738417B (en) * | 2009-12-08 | 2012-09-05 | 清华大学 | Chip for detecting biochemical substances based on cold field electrons, and detection method |
| CN103274349A (en) * | 2013-04-26 | 2013-09-04 | 北京大学 | Thermal stress insulating MEMS micro heater interconnected substrate and method for manufacturing thermal stress insulating MEMS micro heater interconnected substrate |
| CN103718031A (en) * | 2011-06-08 | 2014-04-09 | 阿尔法莫斯公司 | Chemoresistor type gas sensor having a multi-storey architecture. |
| CN104950015A (en) * | 2015-06-15 | 2015-09-30 | 苏州慧闻纳米科技有限公司 | Preparation method of multi-channel array gas sensor |
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| CN101089908B (en) * | 2006-06-13 | 2010-05-26 | 富士施乐株式会社 | Sensor |
| CN101738417B (en) * | 2009-12-08 | 2012-09-05 | 清华大学 | Chip for detecting biochemical substances based on cold field electrons, and detection method |
| CN103718031A (en) * | 2011-06-08 | 2014-04-09 | 阿尔法莫斯公司 | Chemoresistor type gas sensor having a multi-storey architecture. |
| CN103718031B (en) * | 2011-06-08 | 2016-03-30 | 阿尔法莫斯公司 | There is the change sensitive resistor type gas sensor of multiple-unit layer structure |
| CN103274349A (en) * | 2013-04-26 | 2013-09-04 | 北京大学 | Thermal stress insulating MEMS micro heater interconnected substrate and method for manufacturing thermal stress insulating MEMS micro heater interconnected substrate |
| CN104950015A (en) * | 2015-06-15 | 2015-09-30 | 苏州慧闻纳米科技有限公司 | Preparation method of multi-channel array gas sensor |
| CN104950015B (en) * | 2015-06-15 | 2020-03-27 | 江苏智闻智能传感科技有限公司 | Preparation method of multi-channel array gas sensor |
| CN106198602A (en) * | 2016-07-01 | 2016-12-07 | 电子科技大学 | A kind of measurement device for thin-film material thermophysical property |
| CN106959169A (en) * | 2017-04-18 | 2017-07-18 | 上海交通大学 | A kind of Multifunction sensor chip and preparation method thereof |
| CN106959169B (en) * | 2017-04-18 | 2019-05-17 | 上海交通大学 | A kind of novel and multifunctional sensor chip and preparation method thereof |
| CN107643228A (en) * | 2017-08-31 | 2018-01-30 | 中国船舶重工集团公司第七〇九研究所 | Measure chip of mercury vapour and preparation method thereof, sensor and its application method |
| CN108548844A (en) * | 2018-05-11 | 2018-09-18 | 东南大学 | The hot physical property sensor and measurement method of annulus heating excitation central point thermometric |
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| CN100410657C (en) | 2008-08-13 |
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