CN111398364A - High-selectivity array MOS sensor and preparation method thereof - Google Patents
High-selectivity array MOS sensor and preparation method thereof Download PDFInfo
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- CN111398364A CN111398364A CN202010359782.3A CN202010359782A CN111398364A CN 111398364 A CN111398364 A CN 111398364A CN 202010359782 A CN202010359782 A CN 202010359782A CN 111398364 A CN111398364 A CN 111398364A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/128—Microapparatus
Abstract
A high-selectivity array MOS sensor and a preparation method thereof are provided, the high-selectivity array MOS sensor comprises: a substrate; the plurality of sensitive units are formed on the substrate and form an array structure; the heater is formed on the substrate and is arranged at the periphery of the sensitive unit; the electrode layer is formed on the substrate and is electrically connected with the sensitive unit and the heater; the electrode layer comprises a plurality of leading-out terminals for monitoring the terminal potential of different sensitive unit combinations. According to the invention, the connection circuit of different sensitive unit combinations is formed by adopting a plurality of sensitive units with array structures and a plurality of leading-out ends of the electrode layer, so that high-sensitivity response of different gases can be realized.
Description
Technical Field
The invention relates to the technical field of semiconductor sensors, in particular to a high-selectivity array MOS sensor and a preparation method thereof.
Background
With the development of industrial and urban traffic, a great amount of toxic and harmful gases released from industrial parks, industrial boilers, automobile exhaust, furniture and building materials cause the living environment to be full of a great amount of toxic and harmful gases (mainly CO and CO)2、SO2、NO2、H2S, formaldehyde and the like), how to realize effective treatment, and the key problem is to solve the high-precision, high-sensitivity and quick detection of the pollution source. Therefore, there is a great need for a large number of high-sensitivity and high-precision sensors to perform on-site analysis or on-line monitoringAnd (6) measuring.
The metal oxide detector is an important and widely-used detector, and the detector is very widely used due to low price and very wide gas detection range (a corresponding sensitive film can be selected according to gas components to realize detection of various gases).
However, the existing Metal Oxide Semiconductor (MOS) has poor specificity due to design concept and limitation of sensitive materials, and can respond to some other gas components in addition to high sensitivity to a designed gas, which is very easy to cause detection errors and even errors, thereby failing to effectively reflect the real condition of the gas in the environment.
Disclosure of Invention
In view of the above, the present invention provides a high selectivity array MOS sensor and a method for manufacturing the same, which is intended to at least partially solve at least one of the above-mentioned technical problems.
In order to achieve the purpose, the technical scheme of the invention is as follows:
as an aspect of the present invention, there is provided a high selectivity array MOS sensor, including:
a substrate;
the plurality of sensitive units are formed on the substrate and form an array structure;
the heater is formed on the substrate and is arranged at the periphery of the sensitive unit;
the electrode layer is formed on the substrate and is electrically connected with the sensitive unit and the heater;
the electrode layer comprises a plurality of leading-out terminals for monitoring the terminal potential of different sensitive unit combinations.
As another aspect of the present invention, there is also provided a method for preparing the high selectivity array MOS sensor as described above, including the following steps:
forming a heater on a substrate;
forming an electrode layer on a substrate;
coating photoresist on a substrate to obtain a photoresist mask of an exposed sensitive area; wherein the sensitive region comprises a partial electrode layer region and a substrate region;
spraying a sensitive material on a sensitive area;
removing the photoresist mask by adopting a reactive ion etching technology;
and aging in a nitrogen flow environment to obtain the high-selectivity array MOS sensor.
Based on the technical scheme, compared with the prior art, the invention has at least one or one part of the following beneficial effects:
(1) the sensing unit adopts a unique array structure design, the structure is provided with a plurality of sensing units, the electrode layer comprises a plurality of leading-out ends, and the high-precision detection of various gases can be realized through the connection mode of different combinations of the plurality of leading-out ends leading out the sensing units;
(2) at the bottom of the sensitive area, a silicon substrate is hollowed to leave a base of only 5-10 microns as a supporting beam, and the structure can reduce the heat loss of the base;
(3) the double-heater structural design is adopted, the structure enables the heat distribution of the sensitive area to be more balanced, and the high-selectivity array MOS sensor can be ensured to work at an ideal working temperature;
(4) the high-selectivity array MOS sensor is externally connected with an adjustable T4The power module at the end of the fourth leading-out terminal can intelligently select a corresponding sensitive unit from the multiple sensitive units to be in an ideal working state according to different components to be detected, so that high-sensitivity response to different gases is realized;
(5) each sensitive unit is modified with a high-specificity sensitive material, graphene quantum dots are used as a basic material, transition metals such as Co, Mn, Cu, Au and Ag are selectively doped, the pore concentration of the graphene quantum dots is improved, charge electron transfer is promoted, and then the graphene quantum dots and SnO are reacted2、ZnO、In2O3、TiO2、WO3The high selectivity of the gas components is realized by utilizing molecular imprinting or template molecular technology;
(6) on the modification and fixation of the nano sensitive material, a precise mask and large-area spraying method is adopted to realize the high-precision uniform coating of the sensitive material, the uniformity of the sensitive unit prepared by the technology is good, the thickness of the sensitive unit can be precisely controlled, and the spot coating technology cannot realize the purpose.
Drawings
FIG. 1 is a schematic diagram of a high selectivity array MOS sensor according to an embodiment of the invention;
FIG. 2 is a bridge circuit diagram of a high selectivity array MOS sensor according to an embodiment of the invention;
FIG. 3 is a schematic cross-sectional view A-A of FIG. 1;
FIG. 4 is a schematic diagram of a high selectivity array MOS sensor spray operation according to an embodiment of the present invention;
FIG. 5 is a schematic diagram of a parallel plate electrode structure of a motor layer according to an embodiment of the present invention;
FIG. 6 is a schematic diagram of an interdigital electrode structure of an electrode layer in accordance with an embodiment of the present invention.
In the above figures, the reference numerals have the following meanings:
1-an electrode layer; 2-a heater; 3-a sensitive unit; 4-a substrate; 41-a silicon substrate; a 42-silicon nitride layer; 5-photoresist mask; t is1-a first lead-out; t is2-a second lead-out; t is3-a third lead-out; t is4-a fourth terminal.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
As one aspect of the present invention, as shown in fig. 1, there is provided a high selectivity array MOS sensor, including: a substrate 4, a plurality of sensing units 3, a heater 2 and an electrode layer 1; wherein a plurality of sensitive units 3 are formed on a substrate 4, and the plurality of sensitive units 3 form an array structure; the heater 2 is formed on the substrate 4, and the heater 2 is positioned at the periphery of the sensitive unit 3; and the electrode layer 1 is formed on the substrate 4, the electrode layer 1 is electrically connected with the sensitive units 3 and the heater 2, and the electrode layer 1 comprises a plurality of leading-out terminals for monitoring the terminal potential of different combinations of the sensitive units 3.
The working principle of the high-selectivity array MOS sensor is that gas is introduced and adsorbed on the sensitive unit 3, so that the resistance value of the resistor of the sensitive unit 3 is changed, and the voltage value at two ends of the electric connection is correspondingly changed, thereby changing the potential of the output end of the electrode layer 1.
In the embodiment of the invention, one of the terminals is used for grounding, the other terminal is used for connecting the adjustable potential, and the rest terminals are potential detection terminals. The leading-out end of the high-selectivity array MOS sensor, which is connected with the high potential, is externally connected with a power module with adjustable voltage, and a corresponding sensitive unit 3 in the plurality of sensitive units 3 can be intelligently selected to be in an ideal working state according to different components to be detected.
In a preferred embodiment of the invention, three rectangular sensitive cells 3 (S)1、S2、S3) Forming a rectangular array structure, as shown in fig. 1 and 2, the electrode layer 1 includes four terminals, which are respectively defined as first terminals T1A second lead-out terminal T2And a third terminal T3And a fourth terminal T4(ii) a First leading-out terminal T1And a fourth terminal T4Arranged diagonally and having a second lead-out terminal T2And a third terminal T3Arranged diagonally; wherein, the first leading-out terminal T1The grounding device is used for grounding; fourth terminal T4For connecting an adjustable potential; second terminal T2And a third terminal T3Respectively, a potential detecting end. In addition, the heater 2 comprises two heaters which are respectively and symmetrically formed at the periphery of the three sensitive units 3.
For example, as shown in FIG. 2, when U is monitoredTIT3、UT1T2、UT2T4The variation of each voltage value comprising a variation of the potential of at least one sensitive unit 3, e.g. UT1T2Is RS1And RS2Sum of potential changes of UT2T4Is Rs3And measuring the potential changes of the end points, and obtaining the concentration of each component in the mixed gas through a neural network algorithm.
Here, the different terminal potentials include the resistance changes caused by different sensitive materials, and thus each terminal potential includes at least one gas-generated response. The invention combines the voltages of the test ends and obtains the accurate concentration of each gas component to be tested through a neural network algorithm.
The neural network algorithm is a mature algorithm, the principle of the algorithm is equivalent to the simultaneous connection of several equations containing unknowns, and the quantity of each unknowns is obtained by solving. The function of finding the concentration of the measured gas component by using the neural network algorithm can be realized based on conventional hardware such as a single chip microcomputer and the like and conventional software programming, so the invention does not relate to improvement on the program and the algorithm.
The number of the sensing units 3 and the number of the leading-out terminals are not limited to the preferred embodiment, i.e. three sensing units 3 and four leading-out terminals, and the corresponding number and the corresponding circuit connection mode can be designed according to the actual requirements of the high-selectivity array MOS sensor, so as to meet the actual monitoring requirements for the measured gas components.
On one hand, the invention improves the selectivity and the sensitivity of gas detection by the array structure design of the sensitive units and the detection of different end potentials formed by a plurality of leading-out ends; on the other hand, the invention also improves the selectivity of detection through the selection of the sensitive material of the sensitive unit 3.
In an embodiment of the present invention, the sensing unit 3 includes a sensing material in which graphene quantum dots, transition metals, and metal oxides are compounded.
Each sensing unit 3 of the invention is modified with a sensing material with high specificity, and high-precision detection of one or more gas components can be realized according to different choices of the sensing material of each sensing unit 3, such as the sensing materials are the same, all the sensing materials are different, or parts of the sensing materials are the same (such as two sensing materials). For example, the plurality of sensitive units 3 comprise a sensitive material, response H, which is specifically responsive to formaldehyde2S sensitive material and response NH3One or more of the sensitive materials of (a).
In an embodiment of the invention, the sensitive material is a nano-sized particle; transition metals including Co, Mn, Cu, Au, AgOne or more of (a); the metal oxide comprises SnO2、ZnO、In2O3、TiO2、WO3One or more of (a).
More specifically, the sensitive material of the embodiment of the invention takes Graphene Quantum Dots (GQDs) as a basic material, and improves the hole concentration of the graphene quantum dots and promotes charge electron transfer aiming at doping transition metals Co, Mn, Cu, Au, Ag and the like with different gas selectivity; reselected SnO2、ZnO、In2O3、TiO2、WO3The metal oxide materials are compounded with the nano-sensitive material to form the nano-sensitive material.
In embodiments of the present invention, the sensitive material may be, but is not limited to, Au-graphene quantum dots/In2O3And Co-graphene quantum dots/SnO2And the like.
In the embodiment of the invention, as shown in fig. 1, the heater adopts a double-heater structure design and is symmetrically formed on the periphery of the sensitive unit 3; the structure ensures that the heat distribution of the sensitive region is more balanced, the sensitive unit 3 is heated uniformly, and the high-selectivity array MOS sensor can work at an ideal working temperature.
In the embodiment of the present invention, the electrode layer 1 is a parallel plate electrode structure as shown in fig. 5, but is not limited thereto, and the electrode layer 1 may also be an interdigitated electrode structure as shown in fig. 6.
In the embodiment of the present invention, as shown in fig. 3 and 4, the base 4 includes, from bottom to top, a silicon substrate 41 and a silicon nitride layer 42;
the back of the silicon substrate 41 forms a back cavity, the back cavity corresponds to the sensitive area position of the sensitive unit 3, the base of the back cavity corresponding to the position forms a support beam,
as shown in FIG. 3, the thickness H of the support beam is 5-10 μm;
according to the high-selectivity array MOS sensor, the silicon substrate 41 is adopted to empty the base 4 with only 5-10 microns left as a supporting beam at the bottom of the sensitive area, and the structure can reduce the heat loss of the base 4.
The thickness of the silicon nitride layer 42 is 0.2-1 micron, and the silicon nitride layer 42 is designed to ensure that the support beam has a certain strength and is not easily affected by air flow.
As a preferred embodiment, the silicon nitride layer 42 is 1 micron thick.
As another aspect of the present invention, there is also provided a method for preparing the high selectivity array MOS sensor as described above, including the following steps:
photoetching the surface of the silicon nitride layer 42 to obtain a structural diagram of the heater 2, sputtering a layer of Pt/Cr with the thickness of 100-300 nm, preferably 120nm, and then stripping to obtain the heater 2.
Photoetching the surface of the silicon nitride layer 42 to obtain a structure diagram of the electrode layer 1, sputtering a layer of Au/Cr with the thickness of 100-300 nm, preferably 200nm, and then stripping to obtain the electrode layer 1.
It should be noted that the sequence of the steps of forming the heater 2 and the electrode layer 1 on the substrate 4 is not limited as long as the heater 2 and the electrode layer 1 are electrically connected.
As shown in fig. 4, a photoresist with a thickness of 2-3 μm is coated on the silicon nitride layer 42 to obtain a photoresist mask 5 exposing the sensitive region; wherein the sensitive area comprises a partial electrode layer area and a substrate area;
more specifically, the sensitive region is exposed, the photoresist in the non-sensitive region is retained, and a protective mask for the non-sensitive region is formed when the sensitive material is sprayed.
In the embodiment of the invention, the sensitive material is sprayed on the sensitive area; as shown in fig. 4, the prepared sensitive material is uniformly sprayed on a predetermined sensitive area by using a spraying technique, and the thickness is determined according to the characteristics of the sensitive material.
Before spraying, the sensitive material forms a selective recognition structure for the gas to be detected by utilizing a molecular imprinting technology or a template molecular technology, so that an adsorption and analysis structure containing a characteristic shape of a certain gas is obtained, and high selectivity is realized.
In the embodiment of the present invention, a spot coating technique may be selected for modifying the sensitive material, but in the preferred embodiment of the present invention, as shown in fig. 4, by using a photoresist mask 5 and combining a large-area spraying technique, an effect of good consistency of the sensitive unit 3 may be achieved, and the thickness of the sensitive unit 3 may be accurately controlled according to the spraying rate and time.
And removing the photoresist mask 5 by adopting a reactive ion etching technology to expose the leading-out end of the electrode layer 1.
And aging in a nitrogen flow environment, namely aging the thermistor at high temperature to obtain the high-selectivity array MOS sensor.
In an embodiment of the present invention, the specific conditions of aging include: the temperature is 400-600 ℃, and the time is 4-8 hours.
As a preferred embodiment, the aging temperature may be selected to be 350 ℃.
In the embodiment of the present invention, before the step of obtaining the photoresist mask 5 of the exposed sensitive region, the preparation method further includes the following steps: and removing part of the substrate 4 corresponding to the sensitive area by adopting an etching technology to form a back cavity.
In an embodiment of the present invention, before the step of forming the electrode layer 1 on the substrate 4, the preparation method further includes: the silicon substrate 41 is cleaned, and then a silicon nitride layer 42 is grown on the surface of the silicon substrate 41.
In conclusion, the high-precision uniform coating of the sensitive material is realized by adopting a precise mask and a large-area spraying method on the modification and fixation of the nano sensitive material, and the sensitive unit 3 prepared by the technology has good uniformity and the thickness of the sensitive unit 3 can be precisely controlled, which cannot be realized by the spot coating technology.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An arrayed MOS sensor, comprising:
a substrate;
the plurality of sensitive units are formed on the substrate and form an array structure;
the heater is formed on the substrate and is arranged at the periphery of the sensitive unit;
the electrode layer is formed on the substrate and is electrically connected with the sensitive unit and the heater;
the electrode layer comprises a plurality of leading-out terminals for monitoring the terminal potential of different sensitive unit combinations.
2. The arrayed MOS sensor of claim 1, wherein one of the plurality of terminals is for ground, another terminal is for connection to an adjustable potential, and the remaining other terminals are potential sensing terminals.
3. The arrayed MOS sensor of claim 1 or 2, wherein the highly selective arrayed MOS sensor comprises:
the three rectangular sensitive units form a rectangular array structure;
the four leading-out ends are respectively positioned at the four end parts of the rectangular array structure and are respectively defined as a first leading-out end, a second leading-out end, a third leading-out end and a fourth leading-out end; the first leading-out end is used for grounding; the fourth leading-out terminal is used for connecting an adjustable potential; the second leading-out end and the third leading-out end are potential detection ends respectively;
and the two heaters are respectively and symmetrically formed at the periphery of the sensitive unit.
4. The arrayed MOS sensor of claim 1, wherein the electrode layer comprises a parallel plate electrode structure or an interdigitated electrode structure;
the electrode layer is made of Au/Cr, and the thickness of the electrode layer is 100-300 nm;
preferably, the thickness of the electrode layer is 200 nm.
5. The arrayed MOS sensor of claim 1,
the sensitive materials of the plurality of sensitive units are the same, different or partially the same;
the sensitive unit comprises a sensitive material compounded by graphene quantum dots, transition metals and metal oxides;
the sensitive material is nano-sized particles;
the transition metal comprises one or more of Co, Mn, Cu, Au and Ag;
the metal oxide comprises SnO2、ZnO、In2O3、TiO2、WO3One or more of (a).
6. The arrayed MOS sensor of claim 1,
the heater is made of Pt/Cr, and the thickness of the heater ranges from 100 nm to 300 nm;
preferably, the thickness of the heater is 120 nm.
7. The arrayed MOS sensor of claim 1,
the substrate comprises a silicon substrate and a silicon nitride layer from bottom to top;
a back cavity is formed on the back of the silicon substrate, the back cavity corresponds to the position of a sensitive area of the sensitive unit, and a support beam is formed on the base of the back cavity corresponding to the position;
the thickness of the support beam is 5-10 microns;
the thickness of the silicon nitride layer comprises 0.2-1 micron.
8. A method of manufacturing a MOS sensor array as claimed in any of the claims 1 to 7, comprising the steps of:
forming a heater on a substrate;
forming an electrode layer on a substrate;
coating photoresist on a substrate to obtain a photoresist mask of an exposed sensitive area; wherein the sensitive region comprises a partial electrode layer region and a substrate region;
spraying a sensitive material on a sensitive area;
removing the photoresist mask by adopting a reactive ion etching technology;
and aging in a nitrogen flow environment to obtain the high-selectivity array MOS sensor.
9. The method of claim 8, wherein prior to the step of spraying the sensitive material on the sensitive area, the method further comprises the steps of: and forming the sensitive material into a selective recognition structure for the gas to be detected by adopting a molecular imprinting technology or a template molecular technology.
10. The method of claim 8, wherein prior to the step of masking the photoresist to expose sensitive areas, the method further comprises the steps of: removing part of the silicon substrate corresponding to the sensitive area by adopting an etching technology to form a back cavity;
the specific conditions for aging include: the temperature is 400-600 ℃, and the time is 4-8 hours.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112014439A (en) * | 2020-08-31 | 2020-12-01 | 南京信息工程大学 | Graphene quantum dot functionalization-based composite nano film material and gas-sensitive sensing element |
| CN112439658A (en) * | 2020-11-04 | 2021-03-05 | 中国科学院空天信息创新研究院 | Spraying method for wafer-level sensitive material and semiconductor sensor |
| CN113740382A (en) * | 2021-09-06 | 2021-12-03 | 奥维尔斯智能科技(苏州)有限公司 | Manufacturing process of miniature gas sensor and sensor thereof |
| CN113830753A (en) * | 2021-08-27 | 2021-12-24 | 中国科学院空天信息创新研究院 | Pd-doped rGO/ZnO-SnO2Heterojunction quaternary composite material, preparation method and application thereof |
| CN113970577A (en) * | 2021-09-09 | 2022-01-25 | 中国科学院空天信息创新研究院 | Co, N-GQDs-COOH/SnO2Nano composite material, preparation method and application thereof |
| EP4016065A1 (en) * | 2020-12-21 | 2022-06-22 | Infineon Technologies AG | Method for manufacturing an electronic component |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112014439A (en) * | 2020-08-31 | 2020-12-01 | 南京信息工程大学 | Graphene quantum dot functionalization-based composite nano film material and gas-sensitive sensing element |
| CN112439658A (en) * | 2020-11-04 | 2021-03-05 | 中国科学院空天信息创新研究院 | Spraying method for wafer-level sensitive material and semiconductor sensor |
| EP4016065A1 (en) * | 2020-12-21 | 2022-06-22 | Infineon Technologies AG | Method for manufacturing an electronic component |
| US11728073B2 (en) | 2020-12-21 | 2023-08-15 | Infineon Technologies Ag | Method for manufacturing an electronic component |
| CN113830753A (en) * | 2021-08-27 | 2021-12-24 | 中国科学院空天信息创新研究院 | Pd-doped rGO/ZnO-SnO2Heterojunction quaternary composite material, preparation method and application thereof |
| CN113740382A (en) * | 2021-09-06 | 2021-12-03 | 奥维尔斯智能科技(苏州)有限公司 | Manufacturing process of miniature gas sensor and sensor thereof |
| CN113970577A (en) * | 2021-09-09 | 2022-01-25 | 中国科学院空天信息创新研究院 | Co, N-GQDs-COOH/SnO2Nano composite material, preparation method and application thereof |
| CN113970577B (en) * | 2021-09-09 | 2023-06-13 | 中国科学院空天信息创新研究院 | Co, N-GQDs-COOH/SnO 2 Nanocomposite, preparation method and application thereof |
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