CN114689614A - VOC gas sensor based on microwave resonator array - Google Patents

VOC gas sensor based on microwave resonator array Download PDF

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CN114689614A
CN114689614A CN202210311266.2A CN202210311266A CN114689614A CN 114689614 A CN114689614 A CN 114689614A CN 202210311266 A CN202210311266 A CN 202210311266A CN 114689614 A CN114689614 A CN 114689614A
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王昕�
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Wuxi Red Microelectronics Corp Co ltd
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Abstract

The invention discloses a VOC gas sensor based on a microwave resonator array, which comprises a sensing unit, a control unit and a control unit, wherein the sensing unit is used for detecting the VOC gas sensor; the sensing unit is divided into three layers, and the upper layer is a pattern of the sensing unit etched by copper; the middle layer is a Teflon substrate with the dielectric constant of 2.5, the loss tangent of 0.0065 and the thickness of 2.5 mm; the bottom layer is grounding metal copper; coating a sensitive material on a sensitive area of a sensing unit by using a glue transfer printing technology; according to the invention, through the modes of microwave multi-parameter, ultra-wideband, array design and the like, the sensitivity, resolution, selectivity and detection speed can be greatly improved, the VOC detection at room temperature can be realized, the preheating time is saved, the operation power consumption is greatly reduced, and the use safety factor is improved.

Description

VOC gas sensor based on microwave resonator array
Technical Field
The invention relates to the technical field of new crown detection, in particular to a VOC gas sensor based on a microwave resonator array.
Background
Volatile Organic Compounds (VOC) are common in industrial waste gas, automobile exhaust, decoration pollution and other scenes, are precondition for causing regional composite air pollution, seriously threaten the health of people, and restrict the national industrial modernization development. VOC emission sources are complex, various and wide in concentration range.
The conventional resistance and capacitance type gas-sensitive sensor has the defects that the detection parameters are single, fixed frequency detection can be implemented only under low frequency, and corresponding resistance and capacitance values can be read only, so that the heating temperature needs to be increased to improve the detection sensitivity and implement detection; the VOC has low proportion in the air and complex types, so that the problem of poor selectivity exists; the sensitivity shown by the sensitive material is not high.
Disclosure of Invention
The present invention is directed to solve the above problems of the background art, and provides a VOC gas sensor based on a microwave resonator array.
The purpose of the invention can be realized by the following technical scheme:
a VOC gas sensor based on a microwave resonator array comprises a sensing unit; the sensing unit is divided into three layers, and the upper layer is a pattern of the sensing unit etched by copper; the middle layer is a Teflon substrate with the dielectric constant of 2.5, the loss tangent of 0.0065 and the thickness of 2.5 mm; the bottom layer is grounding metal copper;
coating a sensitive material on a sensitive area of a sensing unit by using a glue transfer printing technology;
different sensing units are used for detecting the gas related to the new coronavirus, wherein the gas includes acetone, ethanol, methanol, formaldehyde, xylene and toluene.
As a further scheme of the invention: detecting acetone gas as one-dimensional nano material ZnO sensitive material and detecting ethanol gas as one-dimensional nano material SnO2Sensitive material for detecting methanol gas as one-dimensional nano material FeO3Sensitive material, one-dimensional nano material CoO for detecting formaldehyde gas3Sensitive material for detecting one-dimensional nano material MoO of dimethyl benzene gas4And the sensitive material is used for detecting toluene gas and is a one-dimensional nano NiO sensitive material.
As a further scheme of the invention: adjusting the distribution of the sensing units: the six different sensing units are arranged in an array mode, and a 2-by-3 mode is adopted.
As a further scheme of the invention: the mode of 2 x 3 is to be provided with 2 rows, three in each row, six in total.
As a further scheme of the invention: an electromagnetic shielding structure is designed among the microwave detection units, and the electromagnetic shielding material comprises one of a copper strip material, a copper wire material and a silver-plated copper wire material.
A detection system of a VOC gas sensor based on a microwave resonator array comprises an acquisition module, an analysis module and a data output module;
the frequency deviation values of corresponding acetone, ethanol, methanol, formaldehyde, xylene and toluene in the gas output by the acquisition module through the VOC gas sensor are a1, a2, a3, a4, a5 and a 6;
the analysis module compares the obtained frequency deviation values a1, a2, a3, a4, a5 and a6 with the standard frequency deviation values established in the earlier stage respectively, correspondingly outputs 0 or 1 signals, and adds and analyzes the six signal output values;
and the data output module compares the output total value obtained by the analysis module with a preset model to judge whether the gas environment is risk-free, medium risk or high risk.
As a further scheme of the invention: the model is that when the output total value is 0-2, the analysis of the gas containing the new coronavirus is no risk, when the output total value is 3-4, the analysis of the gas containing the new coronavirus is medium risk, and when the output total value is 5-6, the analysis of the gas containing the new coronavirus is high risk.
A preparation process of a sensitive material in a VOC gas sensor based on a microwave resonator array comprises the following steps:
step 1: preparing a precursor solution: dissolving PVP in deionized water, and stirring for 1h by using a magnetic stirrer until the PVP is completely dissolved; adding corresponding acetate into the solution, stirring for 1h to form a uniform mixture, standing for 1h to remove bubbles to form a spinning solution, and obtaining a precursor solution;
step 2: loading the precursor solution into an injector, and applying 12-20kV direct-current voltage between the metal nozzle and a collecting plate; when the spinning is finished after the machine works for 8 hours, collecting the nano fibers;
and step 3: drying the nano-fibers at room temperature for 1h, carefully taking out the nano-fibers from an aluminum foil, and putting the nano-fibers into a quartz boat; and (3) placing the quartz boat in a muffle furnace, raising the temperature to 400-600 ℃ within 2h, and keeping the temperature for 2h to prepare the sensitive material.
As a further scheme of the invention: the bolus injection speed is set to be 0.01mm/min, the translation speed is set to be 30mm/min, and the rotating speed of the collector is set to be 30-50 r/min; the temperature of the cavity is kept at 30-40 ℃, and the humidity is kept at 30-40% RH.
As a further scheme of the invention: the distance between the metal nozzle and the collecting plate is controlled to be 8-15 cm.
The invention has the beneficial effects that:
(1) microwave scattering parameter S based on microwave ultra-wideband frequency sweeping scheme11、S21By analyzing the changes of the resonance point and the transmission zero point under the change of the gas concentration, including parameters such as frequency shift, amplitude change and the like, and by using a microwave gas detection scheme, the detection of the room-temperature non-heating environment can be implemented. The principle is that different test object gases and different gas sensitive materials have unique sensitive frequency for the change of the dielectric property of the gas sensitive material, and the change of electrical parameters under the sensitive frequency can be captured through ultra-wideband frequency sweeping. In addition, the change of parameters such as frequency shift, amplitude, phase and the like of the resonance point corresponds to the change of dielectric constant and loss, and the concentration of the gas can be evaluated in multiple directions;
(2) the microwave array type design scheme is carried out, different gas-sensitive materials are deposited on different array units, and the respective frequency sweep test of the array units is realized by matching the radio frequency switch and the multiplexing module. In addition, the sensitivities of different gases are reflected in different frequency ranges, and the detection of the concentrations of different VOCs under the optimal frequency can be realized after the ultra-wideband frequency sweeping;
(3) the one-dimensional nano structure with uniform appearance and size can be efficiently prepared by a high-voltage electrostatic spinning method, and the controllability of the appearance of the material is strong; different arrangement modes of the nano fibers can cause certain influence on the performance of the nano fibers; the high-voltage electrostatic spinning technology can also obtain the sequence controllable nano-fiber by designing different receiving devices;
(4) in conclusion, the invention can greatly improve the sensitivity, the resolution, the selectivity and the detection speed by means of multi-parameter, ultra-wideband, array design and the like of microwave, can realize the detection of VOC at room temperature, avoids preheating time, greatly reduces the operation power consumption and improves the safety factor of use.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a bar graph of the present invention;
FIG. 2 is a simulation of a sensing unit of the present invention;
FIG. 3 is a system block diagram of the detection system of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The invention relates to a VOC gas sensor based on a microwave resonator array, which comprises a sensing unit, a control unit and a control unit, wherein the sensing unit comprises a sensing unit and a control unit; the sensing unit is divided into three layers, and the upper layer is etched with copper by a wet etching method to form a pattern of the sensing unit; a Teflon substrate with an interlayer dielectric constant of 2.5, a loss tangent of 0.0065 and a thickness of 2.5 mm; the bottom layer is grounding metal copper;
different sensitive materials are coated on different sensing units, the sensitive materials have different sensitivity degrees to different gases, and the accurate detection of the mixed VOC gas is realized according to the selectivity of different units;
coating a sensitive material on a sensitive area of a sensing unit by using a glue transfer printing technology, wherein the transfer printing technology is divided into direct transfer printing and indirect transfer printing, so that the sensitive material is firmly attached to the sensing unit, and the manufacturing of the VOC gas sensor is completed;
specifically, the different sensing units detect the gas related to the new coronavirus, wherein the gas includes acetone, ethanol, methanol, formaldehyde, xylene and toluene;
different gas related to new coronavirus corresponds to sensitive material of different material, and detection of acetone gas corresponds to one-dimensional nano material ZnO sensitive materialThe detected ethanol gas corresponds to one-dimensional nano material SnO2Sensitive material, which is one-dimensional nanometer material FeO corresponding to methanol gas detection3Sensitive material, which is one-dimensional nanometer material CoO corresponding to formaldehyde gas detection3Sensitive material, detecting dimethyl benzene gas corresponds to one-dimensional nano material MoO4The sensitive material is used for detecting toluene gas and corresponds to the one-dimensional nano material NiO sensitive material;
therefore, the different sensing units judge whether the respiratory gas of the user contains new coronavirus or not through the detection of the six gases and a system algorithm, and judge whether the surrounding environment contains the new coronavirus or not;
example 2
Adjusting the distribution of the sensing units: the six different sensing units are arranged in an array mode, 2-by-3 modes are adopted, namely 2 rows are arranged, and each row is provided with three sensing units, and the total number of the sensing units is six; therefore, the VOC gas sensor can detect a plurality of types at the same time;
when the six sensing units are arranged, mutual electromagnetic interference can occur, so that the final precision of the VOC gas sensor is influenced; therefore, an electromagnetic shielding structure is designed among the microwave detection units, high aspect ratio etching is carried out, and electromagnetic shielding materials are deposited, so that mutual interference of microwave resonance signals and external electromagnetic radiation interference are avoided, the spectral purity and the anti-electromagnetic interference capability of the sensor are improved, and the environmental adaptability of the sensor is improved;
specifically, an electromagnetic shielding structure is arranged at each sensing unit; the electromagnetic shielding structure is designed as follows: simulating the electromagnetic field distribution condition of the detection units by an electromagnetic simulation tool, and isolating mutual interference among the units and electromagnetic interference in an external environment by using a metal electromagnetic shielding material; selecting metal materials with different resistivity and magnetic permeability to form a multilayer shielding body according to different resonance frequencies of each resonance unit in the sensor array; the shielding effect of the electromagnetic shielding system can be expressed by shielding attenuation which represents the attenuation value of the interference field intensity through the shielding body; the shield can be attenuated by
Figure BDA0003568425340000061
Or
Figure BDA0003568425340000062
Obtaining the shielding attenuation value, wherein the larger the shielding attenuation value is, the better the shielding effect is;
the metal and other electromagnetic shielding materials comprise one of a copper belt material, a copper wire material and a silver-plated copper wire material;
example 3
Referring to fig. 1 to 3, 100 detection samples were taken, and the VOC gas sensor based on the microwave resonator array prepared in example 1 was used for detection, and the results of nucleic acid detection were also used for calibration, so that the frequency deviation values of acetone, ethanol, methanol, formaldehyde, xylene, and toluene were (2.3,2.5) MHz, 0.8, 1.0) MHz, 0.6,0.8, 0.7, 0.9) MHz, and 0.3,0.5) MHz, respectively, in the gas containing the new coronavirus;
according to the data, a detection system of the VOC gas sensor based on the microwave resonator array is established;
the detection system comprises an acquisition module, an analysis module and a data output module;
the frequency deviation values of corresponding acetone, ethanol, methanol, formaldehyde, xylene and toluene in the gas output by the acquisition module through the VOC gas sensor are a1, a2, a3, a4, a5 and a 6;
the analysis module compares the obtained frequency deviation values a1, a2, a3, a4, a5 and a6 with the standard frequency deviation values established in the earlier stage respectively, correspondingly outputs 0 or 1 signals, and adds and analyzes the six signal output values;
for example, when the value of a1 is in the range of (2.3,2.5) MHz, the value is recorded as 1, and conversely, when the value is out of the range, the value is recorded as 0; similarly, a2 compared to the frequency offset value of ethanol at (0.8, 1.0) MHz will also output either a1 or a 0;
therefore, the total output value of the six signals is (0,6), when the total output value is 0, the detected gas is not in the standard frequency deviation value, when the total output value is 6, the detected gas is in the standard frequency deviation value, and when the total output value is 1-5, the detected gas part is in the standard frequency deviation value;
the data output module compares the output total value obtained by the analysis module with a preset model to judge whether the gas environment is risk-free, medium risk or high risk;
by modeling the output total value, when the output total value is 0-2, the gas containing the new coronavirus is analyzed to be free of risk, when the output total value is 3-4, the gas containing the new coronavirus is analyzed to be medium risk, and when the output total value is 5-6, the gas containing the new coronavirus is analyzed to be high risk.
Example 4
The preparation process of the one-dimensional nano material ZnO sensitive material comprises the following steps:
step 1: preparing a precursor solution: dissolving PVP in deionized water, and stirring for 1h by using a magnetic stirrer until the PVP is completely dissolved; adding ZnAc into the solution, stirring for 1h to form a uniform mixture, standing for 1h to remove bubbles to form a spinning solution, and obtaining a precursor solution;
step 2: loading the precursor solution into an injector, and applying 12-20kV direct-current voltage between a metal nozzle and a collecting plate, wherein the injection speed is set to be 0.01mm/min, the translation speed is set to be 30mm/min, and the rotating speed of a collector is set to be 30-50 r/min; the temperature of the cavity is kept at 30-40 ℃, and the humidity is kept at 30-40% RH; when the spinning is finished after the machine works for 8 hours, collecting the nano fibers;
wherein the distance between the metal nozzle and the collecting plate is controlled to be 8-15 cm;
and 3, step 3: drying the nano-fibers at room temperature for 1h, carefully taking out the nano-fibers from an aluminum foil, and putting the nano-fibers into a quartz boat; placing the quartz boat in a muffle furnace, heating the quartz boat to 400-600 ℃ within 2h, and keeping the temperature for 2h to prepare a sensitive material;
wherein the temperature rise speed of the muffle furnace is set to be 1-3 ℃/min;
in the gel fiber prepared by the electrostatic spinning method, in the sintering process, the solvent is firstly volatilized rapidly along with the rise of the temperature, when the temperature continues to rise, the tackifier PVP starts to dehydrate and decompose, and carbon and hydrogen elements in the PVP are finally volatilized in a gaseous form to be separated from a fiber membrane, so that the diameter of the obtained nanofiber can be greatly reduced; meanwhile, during sintering, in order to avoid fiber fracture and influence on the performance of the fiber membrane, a lower heating rate is adopted as much as possible; therefore, the sensitive material prepared by the invention enhances the gas selectivity and improves the detection accuracy, thereby achieving the purpose of detecting the VOC (volatile organic compounds) in the exhaled gas of the Xinguan patient.
Example 5
The one-dimensional nano material SnO2And (3) a preparation process of the sensitive material, wherein ZnAc in the example 4 is replaced by tin acetate.
Example 6
The one-dimensional nano material FeO3The preparation process of the sensitive material is to replace ZnAc in the example 4 with iron acetate.
Example 7
The one-dimensional nano material CoO3The preparation process of the sensitive material is to replace ZnAc in the example 4 with cobalt acetate.
Example 8
The one-dimensional nano material MoO4The preparation process of the sensitive material is to replace ZnAc in the example 4 with molybdenum acetate.
Example 9
According to the preparation process of the one-dimensional nanomaterial NiO sensitive material, ZnAc in the embodiment 4 is replaced by nickel acetate.
While one embodiment of the present invention has been described in detail, the description is only a preferred embodiment of the present invention and should not be taken as limiting the scope of the invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.

Claims (10)

1. A VOC gas sensor based on a microwave resonator array is characterized by comprising a sensing unit; the sensing unit is divided into three layers, and the upper layer is a pattern of the sensing unit etched by copper; the middle layer is a Teflon substrate with the dielectric constant of 2.5, the loss tangent of 0.0065 and the thickness of 2.5 mm; the bottom layer is grounding metal copper;
coating a sensitive material on a sensitive area of a sensing unit by using a glue transfer printing technology;
different sensing units are used for detecting the gas related to the new coronavirus, wherein the gas includes acetone, ethanol, methanol, formaldehyde, xylene and toluene.
2. The microwave resonator array-based VOC gas sensor as claimed in claim 1, wherein the acetone gas is detected as a one-dimensional nanomaterial ZnO sensitive material, and the ethanol gas is detected as a one-dimensional nanomaterial SnO2Sensitive material for detecting methanol gas as one-dimensional nano material FeO3Sensitive material, one-dimensional nano material CoO for detecting formaldehyde gas3Sensitive material for detecting one-dimensional nano material MoO of dimethyl benzene gas4And the sensitive material is used for detecting toluene gas and is a one-dimensional nano NiO sensitive material.
3. A microwave resonator array-based VOC gas sensor according to claim 1, wherein the sensing cell distribution is adjusted by: the six different sensing units are arranged in an array mode, and a2 x 3 mode is adopted.
4. A microwave resonator array based VOC gas sensor according to claim 3, wherein 2 x 3 is such that there are 2 rows of three, six.
5. The microwave resonator array-based VOC gas sensor of claim 1, wherein an electromagnetic shielding structure is designed between the microwave detection units, and the electromagnetic shielding material comprises one of a copper strip material, a copper wire material and a silver-plated copper wire material.
6. The detection system of the VOC gas sensor based on the microwave resonator array is characterized by comprising an acquisition module, an analysis module and a data output module;
the frequency deviation values of corresponding acetone, ethanol, methanol, formaldehyde, xylene and toluene in the output gas of the VOC gas sensor are a1, a2, a3, a4, a5 and a6 by the acquisition module;
the analysis module compares the obtained frequency deviation values a1, a2, a3, a4, a5 and a6 with the standard frequency deviation values established in the earlier stage respectively, correspondingly outputs 0 or 1 signals, and adds and analyzes the six signal output values;
and the data output module compares the output total value obtained by the analysis module with a preset model to judge whether the gas environment is risk-free, medium risk or high risk.
7. The detection system of claim 6, wherein the model is that when the total output value is 0-2, the analysis of the gas containing new corona virus is risk-free, when the total output value is 3-4, the analysis of the gas containing new corona virus is intermediate risk, and when the total output value is 5-6, the analysis of the gas containing new corona virus is high risk.
8. A preparation process of a sensitive material in a VOC gas sensor based on a microwave resonator array is characterized by comprising the following steps:
step 1: preparing a precursor solution: dissolving PVP in deionized water, and stirring for 1h by using a magnetic stirrer until the PVP is completely dissolved; adding corresponding acetate into the solution, stirring for 1h to form a uniform mixture, standing for 1h to remove bubbles to form a spinning solution, and obtaining a precursor solution;
step 2: loading the precursor solution into an injector, and applying 12-20kV direct-current voltage between the metal nozzle and a collecting plate; when the spinning is finished after the machine works for 8 hours, collecting the nano fibers;
and 3, step 3: drying the nano-fibers at room temperature for 1h, carefully taking out the nano-fibers from an aluminum foil, and putting the nano-fibers into a quartz boat; and (3) placing the quartz boat in a muffle furnace, raising the temperature to 400-600 ℃ within 2h, and keeping the temperature for 2h to prepare the sensitive material.
9. The process for preparing the sensitive material in the VOC gas sensor based on the microwave resonator array as claimed in claim 8, wherein the injection speed is set to 0.01mm/min, the translation speed is set to 30mm/min, and the rotation speed of the collector is set to 30-50 r/min; the temperature of the cavity is kept at 30-40 ℃, and the humidity is kept at 30-40% RH.
10. The process of claim 8, wherein the distance between the metal nozzle and the collection plate is controlled to be 8-15 cm.
CN202210311266.2A 2022-03-28 2022-03-28 VOC gas sensor based on microwave resonator array Pending CN114689614A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117309906A (en) * 2023-09-27 2023-12-29 江南大学 VOCs sensor without sensitive material and VOCs detection method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117309906A (en) * 2023-09-27 2023-12-29 江南大学 VOCs sensor without sensitive material and VOCs detection method

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