CN112051307B - Multi-sensor array based on quartz crystal microbalance and preparation method thereof - Google Patents
Multi-sensor array based on quartz crystal microbalance and preparation method thereof Download PDFInfo
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- 238000003380 quartz crystal microbalance Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 33
- 239000013078 crystal Substances 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000001259 photo etching Methods 0.000 claims abstract description 19
- 238000000151 deposition Methods 0.000 claims abstract description 10
- 239000007772 electrode material Substances 0.000 claims abstract description 6
- 239000010453 quartz Substances 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- 238000004528 spin coating Methods 0.000 claims description 9
- 238000005566 electron beam evaporation Methods 0.000 claims description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 3
- 238000000206 photolithography Methods 0.000 claims 2
- 238000001514 detection method Methods 0.000 abstract description 15
- 239000007789 gas Substances 0.000 description 9
- 238000003491 array Methods 0.000 description 7
- 238000011161 development Methods 0.000 description 5
- 230000010355 oscillation Effects 0.000 description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 244000052616 bacterial pathogen Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
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- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a quartz crystal microbalance-based multi-sensor array and a preparation method thereof. The preparation method mainly comprises the following steps: photoetching an electrode pattern on the surface of the crystal oscillator wafer; stripping the photoresist outside the electrode pattern and the electrode material on the surface of the photoresist; photoetching a sensitive layer pattern on the surface of the electrode; depositing a sensitive layer material on the surface of the sensitive layer pattern; stripping the photoresist outside the sensitive layer pattern and the sensitive material on the surface of the photoresist; and repeating the operation, and carrying out alignment on the surface of the electrode with the pattern of the sensitive layer until the sensitive array is prepared. The quartz crystal microbalance-based multi-sensor array and the preparation method thereof can simultaneously detect multiple target sensing objects, improve the detection range, improve the detection efficiency and obtain more accurate test results.
Description
Technical Field
The invention belongs to the field of micro-nano sensing, and particularly relates to a quartz crystal microbalance-based multi-sensor array and a preparation method thereof.
Background
With the development of times economy and the improvement of the health and medical level, the quality requirements of people on the health condition and the environment are gradually improved. The traditional approach to a disease and a gas sensor is becoming less and less satisfactory. For example, most of the current detection of a certain environmental gas depends on a specific gas detection device, if a plurality of gases need to be detected, a plurality of corresponding sensors need to be matched, and the data are processed separately. Thereby greatly increasing sensor volume, cost, and subsequent data-information transfer pressure. The detection aiming at human diseases or germs at present depends on a single channel to realize single detection, and for the detection of various germs, more blood needs to be collected, and various detection devices are adopted to carry out the detection, so that the problems of high cost, low detection efficiency and the like are caused.
Therefore, the exploration and development of the sensor can simultaneously detect a plurality of sensing objects, effectively distinguish and identify the sensing objects, greatly reduce the size of the sensor and greatly reduce the sensing and detection cost.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a quartz crystal microbalance-based multi-sensor array and a preparation method thereof, and aims to solve the problem that the existing single sensor is single in detection.
In order to achieve the above object, according to an aspect of the present invention, there is provided a quartz crystal microbalance-based multi-sensor array, which is characterized by comprising a quartz crystal oscillator plate, upper and lower electrodes coated on the surface of the quartz crystal oscillator plate, and a sensitive layer array formed at a fixed point on the surface of the upper electrode on the surface of the quartz crystal oscillator plate.
Further, the lower electrode of the multi-sensor array comprises positive and negative electrode contact points.
Further, the thickness of the electrode is 100nm to 1000 nm.
Further, the material of the electrode is metal Au.
Furthermore, the natural frequency of the quartz crystal oscillation plate is 3 MHz-100 MHz.
Further, the kinds of the sensitive materials are at least 2.
According to another aspect of the invention, there is provided a method for preparing a multi-sensor array based on a quartz crystal microbalance,
(1) preparing an electrode pattern on the surface of a quartz crystal vibrating piece by using a photoetching technology, wherein the electrode pattern comprises spin-coating photoresist, prebaking, placing an electrode pattern mask, exposing, developing, cleaning and hardening;
(2) preparing an electrode by adopting magnetron sputtering or electron beam evaporation;
(3) stripping the photoresist outside the electrode pattern and the electrode material on the surface of the photoresist to obtain an electrode on the crystal oscillator wafer;
(4) photoetching a sensitive layer pattern on the surface of the electrode, wherein the sensitive layer pattern comprises spin-coating photoresist, prebaking, placing a mask, exposing, developing, cleaning and hardening;
(5) depositing a sensitive layer material on the surface of the sensitive layer pattern, and preparing the sensitive layer by adopting magnetron sputtering or electron beam evaporation;
(6) stripping the photoresist outside the sensitive layer pattern and the sensitive material on the surface of the photoresist by adopting acetone or a degumming solution to obtain a sensitive layer pattern;
(7) and (4) repeating the steps (4) to (6), and carrying out alignment on the electrode surface with the pattern of the sensitive layer until the sensitive array is prepared.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts the multi-sensor sensitive array, can simultaneously detect various target objects, improves the detection efficiency, greatly reduces the energy consumption of the sensor, reduces the preparation cost and prolongs the service life;
(2) the device has simple structural design and is easy to process the array sensor. The sensor sensitive array adopts mature processes such as photoetching, deposition, stripping and the like, does not need complex processing conditions and can be produced and prepared in large scale;
(3) the contact sites of the electrodes of the device are positioned on the same side, so that the device is beneficial to easily processing the side electrode surface, providing more placing spaces for the sensor array, protecting the electrodes, isolating the electrodes from contact solution or gas and being easy to use for a long time;
(4) the sensing array can be set according to requirements, can realize sensing detection in a complex environment, and improves the detection precision by utilizing multi-sensor data fusion.
Drawings
FIG. 1 is a schematic diagram of the construction of a quartz crystal microbalance of the present invention; wherein 1 is quartz, 2-1 is an upper electrode, and 2-2 is a lower electrode;
FIG. 2 is a flow chart of a lithographic sensitive layer provided in embodiment 1 of the present invention; wherein, 3-1 is a photoetching development area, and 3-2 is a photoetching reserved area;
FIG. 3 is a flow chart of depositing a sensitive layer provided in example 1 of the present invention; wherein 4-1 is a sensitive layer I;
FIG. 4 is a flow chart of the stripping sensitive layer provided in example 1 of the present invention; wherein 4-2 is a sensitive layer I array;
FIG. 5 is a flow chart of a lithographic sensor layer provided in embodiment 1 of the present invention; wherein, 3-3 is a photoetching development area, and 3-4 is a photoetching reserved area;
FIG. 6 is a flow chart of depositing a sensitive layer provided in example 1 of the present invention; wherein 5-1 is a sensitive layer II;
FIG. 7 is a flow chart of the stripping of a sensitive layer provided in example 1 of the present invention; wherein 5-2 is a sensitive layer I array;
FIG. 8 is a flow chart of a lithographic sensor layer provided in embodiment 1 of the present invention; wherein, 3-5 is a photoetching development area, and 3-6 is a photoetching reserved area;
FIG. 9 is a flow chart of depositing a sensitive layer provided in example 1 of the present invention; wherein 6-1 is a sensitive layer III;
FIG. 10 is a flow chart of the stripping of a sensitive layer provided in example 1 of the present invention; wherein 6-2 is a sensitive layer I array;
FIG. 11 is a top view of a type I device provided in embodiment 1 of the present invention;
FIG. 12 is a top view of a type II device provided in embodiment 2 of the present invention;
fig. 13 is a top view of a type III device provided in embodiment 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
When the device is placed in a complex environment, including a solution environment or a gas environment, the sensor array adsorbs target gas in the environment, the higher the concentration is, the more the adsorption is, the more the frequency change of the quartz crystal oscillator is obvious, and the position of the different sensor arrays and the quantity of the sensing target gas are related to the frequency change. Therefore, the types and concentrations of the plurality of gases can be determined by detecting the frequency change.
The invention provides a quartz crystal microbalance-based multi-sensor array based on the working principle, which comprises a quartz crystal vibrating piece, an upper electrode and a lower electrode which are coated on the surface of the quartz crystal vibrating piece, and a sensitive layer array formed on the surface of the upper electrode on the surface of the quartz crystal vibrating piece at fixed points.
Specifically, the lower electrode of the multi-sensor array comprises positive and negative electrode contact points.
Specifically, the thickness of the electrode is 100nm to 1000 nm.
Specifically, the material of the electrode is metallic Au.
Specifically, the natural frequency of the quartz crystal oscillation plate is 3 MHz-100 MHz.
Specifically, the kinds of the sensitive materials are at least 2.
Example 1
As shown in fig. 1, a quartz crystal microbalance-based multi-sensor array includes the following parts, 1) electrodes (upper electrode 2-1, lower electrode 2-2); 2) a crystal oscillation plate 1; 3) the sensitive layer arrays 4-2, 5-2 and 6-2. The preparation method is shown in fig. 2 to fig. 10, and mainly comprises the following steps:
(1) photoetching an electrode pattern on the surface of a crystal oscillator wafer, including spin-coating photoresist, prebaking, placing an electrode pattern mask, exposing, developing, cleaning and hardening;
(2) preparing a device electrode by adopting magnetron sputtering, wherein the material is Au, and the thickness is 100 nm;
(3) stripping the photoresist outside the electrode pattern and the electrode material on the surface of the photoresist to obtain an electrode on a crystal oscillator plate, wherein the crystal oscillator plate is subjected to AT cutting, and the natural frequency is 3 MHz;
(4) photoetching a sensitive layer pattern on the surface of the electrode, wherein the sensitive layer pattern comprises spin-coating photoresist AZ5214, prebaking, placing a mask of the sensitive layer 4, exposing, developing, cleaning and hardening;
(5) depositing a sensitive layer material on the surface of the sensitive layer pattern, and preparing the sensitive layer by adopting magnetron sputtering, wherein the sensitive material is molybdenum and has the thickness of 50 nm;
(6) stripping the photoresist outside the sensitive layer pattern and the sensitive material on the surface of the photoresist by using acetone to obtain a sensitive layer 4-2 pattern;
(7) and (5) repeating the steps (4) to (6), and carrying out alignment on the electrode surface with the pattern of the sensitive layer until the sensitive arrays 5-2 and 6-2 are prepared.
By adopting the preparation method, 3 sensitive layers can be prepared on the surface of the same quartz crystal microbalance device, and as shown in fig. 11, the device can simultaneously detect 3 target sensing objects.
Example 2
A quartz crystal microbalance-based multi-sensor array comprises the following parts, 1) electrodes (upper electrode 2-1, lower electrode 2-2); 2) a crystal oscillation plate 1; 3) the sensitive layer arrays 4-2, 5-2, 6-2, 7-2, 8-2 and 9-2. The preparation method mainly comprises the following steps:
(1) photoetching electrode patterns 2-1 and 2-2 on the surface of a crystal oscillator wafer 1, including spin-coating photoresist, prebaking, placing an electrode pattern mask, exposing, developing, cleaning and hardening;
(2) preparing a device electrode by adopting electron beam evaporation, wherein the material is Au, and the thickness is 500 nm;
(3) stripping the photoresist outside the electrode pattern and the electrode material on the surface of the photoresist to obtain an electrode on a crystal oscillator plate, wherein the crystal oscillator plate is subjected to AT cutting, and the natural frequency is 50 MHz;
(4) photoetching a sensitive layer pattern on the surface of the electrode, wherein the sensitive layer pattern comprises spin-coating photoresist NR7-1500PY, prebaking, placing a mask of the sensitive layer 4, exposing, postbaking, developing, cleaning and hardening;
(5) depositing a sensitive layer material on the surface of the sensitive layer pattern, and preparing the sensitive layer by adopting electron beam evaporation, wherein the sensitive layer material is molybdenum and has the thickness of 50 nm;
(6) stripping the photoresist outside the sensitive layer pattern and the sensitive material on the surface of the photoresist by using acetone to obtain a sensitive layer 4-2 pattern;
(7) and (4) repeating the steps (4) to (6), and carrying out alignment on the electrode surface with the existing sensitive layer pattern until the sensitive arrays 5-2, 6-2, 7-2, 8-2 and 9-2 are prepared.
By adopting the preparation method, 6 sensitive layers can be prepared on the surface of the same quartz crystal microbalance device, and as shown in figure 12, the device can simultaneously detect 6 target sensing objects.
Example 3
A quartz crystal microbalance-based multi-sensor array comprises the following parts, 1) electrodes (upper electrode 2-1, lower electrode 2-2); 2) a crystal oscillation plate 1; 3) the sensitive layer arrays 4-2, 5-2, 6-2, 7-2, 8-2, 9-2, 10-2, 11-2, 12-2, 13-2, 14-2 and 15-2. The preparation method mainly comprises the following steps:
(1) photoetching electrode patterns 2-1 and 2-2 on the surface of a crystal oscillator wafer 1, including spin-coating photoresist, prebaking, placing an electrode pattern mask, exposing, developing, cleaning and hardening;
(2) preparing a device electrode by adopting electron beam evaporation, wherein the material is Au, and the thickness is 1000 nm;
(3) stripping the photoresist outside the electrode pattern and the electrode material on the surface of the photoresist to obtain an electrode on a crystal oscillator plate, wherein the crystal oscillator plate is subjected to AT cutting, and the natural frequency is 100 MHz;
(4) photoetching a sensitive layer pattern on the surface of the electrode, wherein the sensitive layer pattern comprises spin-coating photoresist PR-12000, pre-baking, placing a mask plate of a sensitive layer 4, exposing, post-baking, developing, cleaning and hardening;
(5) depositing a sensitive layer material on the surface of the sensitive layer pattern, and preparing the sensitive layer by adopting electron beam evaporation, wherein the sensitive layer material is molybdenum and has the thickness of 50 nm;
(6) stripping the photoresist outside the sensitive layer pattern and the sensitive material on the surface of the photoresist by using acetone to obtain a sensitive layer 4-2 pattern;
(7) and (4) repeating the steps (4) to (6), and carrying out alignment on the electrode surface with the existing sensitive layer pattern until the sensitive arrays 5-2, 6-2, 7-2, 8-2, 9-2, 10-2, 11-2, 12-2, 13-2, 14-2 and 15-2 are prepared.
By adopting the preparation method, 12 sensitive layers can be prepared on the surface of the same quartz crystal microbalance device, and as shown in figure 13, the device can simultaneously detect 12 target sensing objects.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A multi-sensor array based on a quartz crystal microbalance is characterized by comprising a quartz crystal oscillator piece, an upper electrode, a lower electrode and a sensitive layer array, wherein the upper electrode and the lower electrode are coated on the surface of the quartz crystal oscillator piece; the types of the sensitive materials are at least 2.
2. The multi-sensor array of claim 1, wherein the lower electrode of the multi-sensor array comprises positive and negative electrode contacts.
3. The multi-sensor array of claim 2, wherein the upper or lower electrode has a thickness of 100nm to 1000 nm.
4. The multi-sensor array of claim 2, wherein the material of the upper or lower electrodes is metallic Au.
5. The multi-sensor array according to claim 1, wherein the natural frequency of the quartz crystal plate is 3MHz to 100 MHz.
6. A method for preparing a multi-sensor array based on a quartz crystal microbalance as claimed in any one of claims 1 to 5, comprising the steps of:
(1) preparing an electrode pattern on the surface of the quartz crystal vibrating piece by using a photoetching technology;
(2) preparing an electrode by adopting magnetron sputtering or electron beam evaporation;
(3) stripping the photoresist outside the electrode pattern and the electrode material on the surface of the photoresist;
(4) preparing a sensitive layer pattern on the surface of the electrode by using a photoetching technology;
(5) depositing a sensitive layer material on the surface of the sensitive layer pattern, and preparing the sensitive layer by adopting magnetron sputtering or electron beam evaporation;
(6) stripping the photoresist outside the sensitive layer pattern and the sensitive material on the surface of the photoresist by adopting acetone or a degumming solution;
(7) and (4) repeating the steps (4) to (6), and carrying out alignment on the electrode surface with the pattern of the sensitive layer until the sensitive array is prepared.
7. The method according to claim 6, wherein the photolithography in step (1) comprises spin-coating a photoresist, pre-baking, placing an electrode pattern mask, exposing, developing, cleaning, and hardening.
8. The method according to claim 6, wherein the photolithography in step (4) comprises spin-on resist, pre-baking, mask-placing, exposing, developing, cleaning, and hardening.
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