CN104406881B - A kind of piezoelectric sound wave biology sensor based on micro-nano structure - Google Patents
A kind of piezoelectric sound wave biology sensor based on micro-nano structure Download PDFInfo
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- CN104406881B CN104406881B CN201410660446.7A CN201410660446A CN104406881B CN 104406881 B CN104406881 B CN 104406881B CN 201410660446 A CN201410660446 A CN 201410660446A CN 104406881 B CN104406881 B CN 104406881B
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Abstract
The invention discloses a kind of piezoelectric sound wave biology sensor based on micro-nano structure, including quartz crystal and frequency meter, the bottom electrode that the quartz crystal includes quartz wafer, is arranged on the working electrode on quartz wafer top, is arranged on quartz wafer bottom, the frequency meter connection working electrode and bottom electrode, the quartz crystal surface sets micrometer structure or nanostructured.Compared with prior art, the present invention by micro-nano technology technique can accurately be made on quartz crystal surface different sizes, different-shape micron and nano, micron and nano can be adjusted according to different purposes, not only embody the application flexibility of the present invention, and a kind of new senser element is provided, enhance the application of this QCM biology sensors.
Description
Technical field
The present invention relates to a kind of piezoelectric sound wave biology sensor based on micro-nano structure.
Background technology
QCM (QCM) is that the piezo-electric effect based on quartz crystal is surveyed to the change of its electrode surface quality
The instrument of amount.Piezo-electric effect is to be found by Pierre Curie and Jacques Curie brothers in 1880, i.e., in quartz-crystal
Piece adds an electric field, and chip can produce mechanically deform.If on the contrary, applying mechanical pressure on chip, in the corresponding direction of chip
It is upper to produce certain electric field.Because it has the mass-basis response sensitivity of nanogram level so that QCM be widely used in industrial plated film,
Analytical chemistry, molecular biology, immunology, science of heredity, environmental science and some other be related to quality, density and viscosity etc. inspection
Survey field.The QCM instrument performances of the Q-Sense companies of Sweden maintain the leading position in the same industry, in biology field
In be mainly used in study bioactive molecule between interaction, such as protein adsorption dynamics adsorption kinetics, antigen/antibody phase interaction
With, in terms of DNA hybridization, aptamers-protein-interacting；In biomedical sector be used for study or detect antigen, antibody,
Haemocyte, pathogenic microorganism, nucleic acid and protein etc..
For a kind of highly sensitive biology sensor, an important parameter is exactly the sensitivity of its detection.It is right
In QCM, its mass sensitivity is relevant with its resonant frequency, and resonant frequency is higher, and its mass sensitivity is higher.Improve
The detection sensitivity of QCM instruments in itself, on the one hand can by using higher resonant frequency quartz crystal, in the market
The frequency of common quartz crystal is 5MHz.If using the quartz crystal of higher resonant frequency, although in theory can be with
Higher mass sensitivity is obtained, but the thickness of crystal-vibration-chip is inversely proportional with its resonant frequency, i.e., resonant frequency is higher, and it is brilliant
Shake piece thickness it is thinner.However, crystal-vibration-chip is by it when in use by way of " O " type rubber ring compresses sealing or bonding
Be fixed in liquid reactions flow cell, if some problems will be caused using relatively thin quartz crystal, be on the one hand sealing or
Extra mechanical stress will be produced for thin quartz crystal by pasting fixed mode, this by have a strong impact on QCM signal and
Its detection sensitivity；Still further aspect, thin quartz crystal is easier to damage in operation, and use cost is uprised.In this regard, business
The QCM of industry mainly takes two ways to improve detection sensitivity at present, such as Q-Sense companies use 5MHz crystal-vibration-chips
Higher order resonant frequencies (15MHz, 25MHz, 35MHz) mode, the QCM of German 3T companies then uses 10MHz quartz crystal.
Another method for improving the detection sensitivity of QCM instruments in itself is to be combined in increase unit area in quartz
The quantity of biomolecule in crystal-vibration-chip.However, commercialization QCM instruments are all adopted for the quartz crystal that biological species are detected at present
With the quartz crystal of polishing, smoothly, roughness is smaller, can regard the reaction of plane as on the quartz crystal surface of polishing
Surface；And unpolished quartz crystal surface roughness is larger, although the surface of crystal-vibration-chip can be improved to a certain extent
Product, but the pattern of its coarse structure and size are uncontrollable, this is determined by glossing, hardly results in high uniformity
Rough surface.
The content of the invention
The technical problem to be solved in the present invention is to increase the surface area of quartz wafer, is combined with this to increase in unit area
The quantity of biomolecule in quartz crystal, so as to improve the detection sensitivity of QCM biology sensors.
The present invention is to be achieved through the following technical solutions：
A kind of piezoelectric sound wave biology sensor based on micro-nano structure, including quartz crystal and frequency meter, the quartz
The bottom electrode that crystal-vibration-chip includes quartz wafer, is arranged on the working electrode on quartz wafer top, is arranged on quartz wafer bottom, institute
Frequency meter connection working electrode and bottom electrode are stated, the quartz crystal surface sets micrometer structure or nanostructured.
Further, one layer of photoresist of spin coating on quartz crystal, obtains micrometer structure or nano junction afterwards through exposure and development
Structure.
The preparation method of micrometer structure is：By quartz crystal successively with being dried up after acetone, each ultrasonic 10min of ethanol, use
Oxygen gas plasma handles 5min；One layer of HMDS is then spin coated onto, one layer of photoresist, photoresist thickness is then spin coated onto
Between 0.2~5 μm, 5~30min is dried at 90 DEG C, then, the quartz crystal for scribbling photoresist ultraviolet or deep ultraviolet is subjected to
Exposure, time for exposure 5s~3min, then, will after exposure quartz crystal immersion developer solution in, obtained after development positive photoresist or
Negtive photoresist micrometer structure.
The preparation method of micrometer structure or nanostructured is：Quartz crystal is used into acetone, each ultrasonic 10min of ethanol successively
After dry up, with oxygen gas plasma handle 5min；One layer of adhesive polyvinylpyrrolidone or trimethoxy silane are then spin coated onto,
Then each cleaning 10min in ethanol and deionized water is put it into, 5min is dried at 120 DEG C afterwards；It is then spin coated onto one layer of electronics
Beam photoresist, electron beam resist thickness dries 5~15min, then, will scribble electron beam light between 0.2~2 μm at 120 DEG C
The quartz crystal of photoresist carries out electron beam exposure, then, and the quartz crystal after exposure is immersed in developer solution, after development
To positive photoresist or negtive photoresist nanostructured or micrometer structure.
Compared with prior art, the present invention can accurately make difference by micro-nano technology technique on quartz crystal surface
The micron and nano of size, different-shape, can adjust micron and nano according to different purposes, not only embody this
The application flexibility of invention, and a kind of new senser element is provided, enhance the application model of this QCM biology sensors
Enclose.
Brief description of the drawings
Fig. 1 is structural representation of the invention.
Embodiment
The invention will be further described with reference to the accompanying drawings and examples：
As shown in figure 1, a kind of piezoelectric sound wave biology sensor based on micro-nano structure, including quartz crystal and frequency meter
1, the quartz crystal includes quartz wafer 2, is arranged on the working electrode 3 on the top of quartz wafer 2, is arranged on quartz wafer 2
The bottom electrode 4 of bottom, the connection working electrode 3 of frequency meter 1 and bottom electrode 4, the quartz crystal surface sets micron knot
Structure 5 or nanostructured 5.
In use, after quartz crystal cleaning, being chemically modified, being then immersed in 2.5% glutaraldehyde solution
Reaction 1 hour；Then the fixation of biomolecule recognition component 6 (biomolecule such as antibody, DNA, enzyme etc.) is can be carried out, afterwards
Carry out the detection of biomolecule to be measured.
Embodiment 1
By quartz crystal successively with being dried up after acetone, each ultrasonic 10min of ethanol, 5min is handled with oxygen gas plasma；
One layer of HMDS is then spin coated onto, one layer of photoresist is then spin coated onto, photoresist thickness is to dry 30min at 5 μm, 90 DEG C,
Then, the quartz crystal for scribbling photoresist is subjected to ultraviolet or deep UV lithography, time for exposure 5s, then, after exposure
In quartz crystal immersion developer solution, positive photoresist or negtive photoresist micrometer structure are obtained after development.
Embodiment 2
By quartz crystal successively with being dried up after acetone, each ultrasonic 10min of ethanol, 5min is handled with oxygen gas plasma；
One layer of HMDS is then spin coated onto, one layer of photoresist is then spin coated onto, photoresist thickness is to dry 5min at 0.5 μm, 90 DEG C,
Then, the quartz crystal for scribbling photoresist is subjected to ultraviolet or deep UV lithography, time for exposure 3min, then, after exposure
Quartz crystal immersion developer solution in, positive photoresist or negtive photoresist micrometer structure are obtained after development.
Embodiment 3
By quartz crystal successively with being dried up after acetone, each ultrasonic 10min of ethanol, 5min is handled with oxygen gas plasma；
One layer of adhesive polyvinylpyrrolidone or trimethoxy silane are then spin coated onto, is then put it into each in ethanol and deionized water
10min is cleaned, 5min is dried at 120 DEG C afterwards；One layer of electron beam resist is then spin coated onto, electron beam resist thickness is 2 μm,
15min is dried at 120 DEG C, then, the quartz crystal for scribbling electron beam resist electron beam exposure is subjected to.Then, it will expose
In quartz crystal immersion developer solution afterwards, positive photoresist or negtive photoresist nanoscale structures are obtained after development.
Embodiment 4
By quartz crystal successively with being dried up after acetone, each ultrasonic 10min of ethanol, 5min is handled with oxygen gas plasma；
One layer of adhesive polyvinylpyrrolidone or trimethoxy silane are then spin coated onto, is then put it into each in ethanol and deionized water
10min is cleaned, 5min is dried at 120 DEG C afterwards；One layer of electron beam resist is then spin coated onto, electron beam resist thickness is 0.2 μ
M, dries 5min at 120 DEG C, then, and the quartz crystal that will scribble electron beam resist carries out electron beam exposure.Then, it will expose
In quartz crystal immersion developer solution afterwards, positive photoresist or negtive photoresist nanoscale structures are obtained after development.
Embodiment 5
By quartz crystal successively with being dried up after acetone, each ultrasonic 10min of ethanol, 5min is handled with oxygen gas plasma；
One layer of adhesive polyvinylpyrrolidone or trimethoxy silane are then spin coated onto, is then put it into each in ethanol and deionized water
10min is cleaned, 5min is dried at 120 DEG C afterwards；One layer of electron beam resist is then spin coated onto, electron beam resist thickness is 1 μm,
10min is dried at 120 DEG C, then, the quartz crystal for scribbling electron beam resist electron beam exposure is subjected to.Then, it will expose
In quartz crystal immersion developer solution afterwards, positive photoresist or negtive photoresist micro/nano level structure are obtained after development.
Embodiment 6
Using SiO2The 10HMz quartz crystals of the photoresist of type, it is molten with 0.1%APTES toluene solution or ethanol
Liquid carries out amination modification, is then immersed in 2.5% glutaraldehyde water solution and reacts 1 hour；Then it can be carried out life
The fixation of the thing molecular recognition elements such as biomolecule such as antibody, DNA, enzyme, carries out the detection of biomolecule to be measured afterwards.
Claims (2)
1. a kind of piezoelectric sound wave biology sensor based on micro-nano structure, including quartz crystal and frequency meter, the quartz-crystal
The bottom electrode that the piece that shakes includes quartz wafer, is arranged on the working electrode on quartz wafer top, is arranged on quartz wafer bottom, it is described
Frequency meter connects working electrode and bottom electrode, it is characterised in that the quartz crystal surface sets micrometer structure, the micron
The preparation method of structure is：By quartz crystal successively with being dried up after acetone, each ultrasonic 10min of ethanol, oxygen gas plasma is used
Handle 5min；Be then spin coated onto one layer of HMDS, be then spin coated onto one layer of photoresist, photoresist thickness 0.2~5 μm it
Between, 5~30min is dried at 90 DEG C, then, the quartz crystal for scribbling photoresist ultraviolet or deep UV lithography is subjected to, during exposure
Between 5s~3min, then, by after exposure quartz crystal immerse developer solution in, obtained after development positive photoresist or negtive photoresist micron knot
Structure.
2. a kind of piezoelectric sound wave biology sensor based on micro-nano structure, including quartz crystal and frequency meter, the quartz-crystal
The bottom electrode that the piece that shakes includes quartz wafer, is arranged on the working electrode on quartz wafer top, is arranged on quartz wafer bottom, it is described
Frequency meter connects working electrode and bottom electrode, it is characterised in that the quartz crystal surface sets micrometer structure or nano junction
The preparation method of structure, the micrometer structure or nanostructured is：Quartz crystal is used into acetone, each ultrasonic 10min of ethanol successively
After dry up, with oxygen gas plasma handle 5min；One layer of adhesive polyvinylpyrrolidone or trimethoxy silane are then spin coated onto,
Then each cleaning 10min in ethanol and deionized water is put it into, 5min is dried at 120 DEG C afterwards；It is then spin coated onto one layer of electronics
Beam photoresist, electron beam resist thickness dries 5~15min, then, will scribble electron beam light between 0.2~2 μm at 120 DEG C
The quartz crystal of photoresist carries out electron beam exposure, then, and the quartz crystal after exposure is immersed in developer solution, after development
To positive photoresist or negtive photoresist nanostructured or micrometer structure.
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| CN101034077A (en) * | 2006-11-29 | 2007-09-12 | 电子科技大学 | Piezocrystal gas sensor and method for making same |
| CN201583522U (en) * | 2009-08-04 | 2010-09-15 | 香港城市大学 | Detecting device for piezoelectric ceramic oscillatory chip |
| CN101964307A (en) * | 2010-07-30 | 2011-02-02 | 上海宏力半导体制造有限公司 | Formation method for etching patterns |
| CN102967522A (en) * | 2012-11-15 | 2013-03-13 | 电子科技大学 | Quartz crystal microbalance (QCM) mass sensor |
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| JP5712129B2 (en) * | 2008-09-02 | 2015-05-07 | ザ ガバニング カウンシル オブ ザ ユニバーシティ オブ トロント | Nanostructured microelectrode and biosensing device incorporating the same |
| CN103991837B (en) * | 2014-03-07 | 2016-10-12 | 中山大学 | A kind of manufacture method of micro-nano ordered through hole array metal thin film sensor based on piezoelectric substrate thin slice |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101034077A (en) * | 2006-11-29 | 2007-09-12 | 电子科技大学 | Piezocrystal gas sensor and method for making same |
| CN201583522U (en) * | 2009-08-04 | 2010-09-15 | 香港城市大学 | Detecting device for piezoelectric ceramic oscillatory chip |
| CN101964307A (en) * | 2010-07-30 | 2011-02-02 | 上海宏力半导体制造有限公司 | Formation method for etching patterns |
| CN102967522A (en) * | 2012-11-15 | 2013-03-13 | 电子科技大学 | Quartz crystal microbalance (QCM) mass sensor |
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| A Dibutyl Phthalate Sensor Based on a Nanofiber Polyaniline Coated Quartz Crystal Monitor;You Wang, et al.;《Sensors》;20130318;第13卷;3765-3775 * |
| 从光固化聚硅氮烷到微/纳米图形结构;方庆玲;《中国博士学位论文全文数据库 信息科技Ⅰ辑》;20120715(第07期);第18页第1段至第19页第2段 * |
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