CN104502428A - Miniature electrochemical sensor based on direct forming mesoporous carbon technology and manufacturing method - Google Patents
Miniature electrochemical sensor based on direct forming mesoporous carbon technology and manufacturing method Download PDFInfo
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- CN104502428A CN104502428A CN201510015290.1A CN201510015290A CN104502428A CN 104502428 A CN104502428 A CN 104502428A CN 201510015290 A CN201510015290 A CN 201510015290A CN 104502428 A CN104502428 A CN 104502428A
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Abstract
The invention belongs to the field of micro-sensors and micro-machining and particularly relates to a miniature electrochemical sensor based on a direct forming mesoporous carbon technology and a manufacturing method. The manufacturing method comprises the steps of using a silicon dioxide layer with 500 nm plasma enhanced chemical vapor deposition thickness as an insulation layer on a silicon wafer and obtaining a working electrode region through photo-etching and etching; obtaining graphs of a counter electrode and a reference electrode substrate region through photo-etching, evaporating 80 nm platinum and then stripping a photoresist; spin-coating an SU-8 photoresist and silicon oxide mixture on a silicon substrate template in the working electrode region, obtaining the working electrode region through photo-etching imaging and using hydrofluoric acid to remove template material silicon dioxide so as to obtain working electrode mesoporous carbon after 900 DEG C high-temperature carbonization; coating silver/silver chloride slurry on reference electrode substrate platinum to obtain solid silver/silver chloride reference electrode.
Description
Technical field
The invention belongs to microsensor and micromachined field, particularly relate to a kind of miniature electrochemical based on straight forming mesoporous carbon technology and method for making.
Background technology
Electrochemical sensor, as the one of sensor, characterizes the electrochemical properties of material by the change of measuring the electric signal such as current potential, electric current in electrochemical reaction.Electrochemical sensor is formed primarily of sensitive element and conversion element two parts, first electrochemical sensor is interacted by sensitive element and material to be measured, produce the change of chemical quantity, by conversion element, the change transitions of chemical quantity is become relevant electric signal again, finally by the correlation parameter process of these electric signal being drawn to test substance.The development trend of electrochemical sensor is integrated and microminiaturized, after electrochemical sensor microminiaturization, can be combined with micro-fluid chip and microfluid system, realize integrality and the diversity of its function.The reducing of electrochemical sensor volume has also widened its application in biosystem, the ecosystem further, more easily carries out implanted and distributed detection.Miniature electrochemical is by working electrode, form (three-electrode system) electrode and contrast electrode three part.After the micro fabrication microminiaturizations such as MEMS (Micro-Electro-Mechanical System), the smaller volume of working electrode, can carry out the design and production of batch; Can better suppress current noise, background interference simultaneously.Working electrode is the major interfaces that electrochemical sensor carries out detecting, also be the region that electrode function was uploaded, realized to sensitive material, the performance of working electrode will directly affect and determine the parameter index that the sensitivity, detectability etc. of sensor are important, and the selection therefore for working electrode base material seems very important.
2005, the people such as D.Lee found that the mesoporous carbon dusty material with nano aperture structure effectively also can significantly promote the process of living things catalysis by fixing biological molecules, and have prepared high performance glucose sensor with this material fixing glucose oxidase.2008, the performance of pasty electrode in electrochemical sensing and bio-sensing that the people such as L.Zhu compared for Graphene, prepared by carbon nano-tube, mesoporous carbon three kinds of materials, find that meso-porous carbon material can provide better electro transfer power, there is better electrochemical catalysis performance.2010, BJ Melde and BJ Johnson further illustrates the transfer that the oxygen-containing functional group on meso-porous carbon material surface and edge defect position can promote electronics, and can further by the finishing of meso-porous carbon material being promoted to the electric conductivity of material, specific surface area, absorption property and electron transfer rate.In most of the cases, present Powdered after meso-porous carbon material is shaping, need to use the cementing agents such as Nafion to make it shaping, this makes the application of meso-porous carbon material in miniature electrochemical working electrode material be restricted.Therefore, if the microminiaturization of meso-porous carbon material, graphical and straight forming can be realized, not only will contribute to the integrated of sensor, Batch Design and the production of miniature electrochemical can also be realized, advance the development based on meso-porous carbon material electrochemical sensor.
Summary of the invention
For the problems referred to above, the present invention's design achieves a kind of miniature electrochemical based on straight forming mesoporous carbon technology and method for making.
Based on a miniature electrochemical for straight forming mesoporous carbon technology, comprising: device substrate, insulation course, to electrode, contrast electrode, working electrode; Wherein, device substrate is rectangle, and its middle is covered with the working electrode of rectangle and certain electrical leads of extending from working electrode; In device substrate except working electrode and lead-in wire, all cover insulation course, and insulation course and keep gap between working electrode and contact conductor; On the insulating layer, centered by working electrode and contact conductor, be outwards covered with a little large U-shaped successively to electrode, wherein large U-shaped is covered with contrast electrode on electrode.
The described material to electrode is platinum.
The material of described contrast electrode is solid-state silver/silver chloride.
The material of described working electrode is mesoporous carbon.
Based on a method for making for the miniature electrochemical of straight forming mesoporous carbon technology, comprising:
Step 1, on silicon chip with plasma enhanced chemical vapor deposition silicon dioxide layer as insulation course, utilize etching to obtain working electrode area by photoetching;
Step 2, obtain the figure to electrode and contrast electrode substrate region by photoetching, evaporate certain thickness platinum, then stripping photoresist;
Step 3, in the silicon substrate template of working electrode area the potpourri of spin coating photoresist and nano silicon oxide, photolithography patterning obtains working electrode area, after high temperature cabonization, removes mould material silicon dioxide, obtain working electrode mesoporous carbon with hydrofluorite;
Step 4, on contrast electrode substrate platinum, apply silver/silver chloride slurry, obtain solid-state silver/silver chloride reference electrode.
In described step 1, the deposit thickness of silicon dioxide layer is 500nm.
The thickness of the platinum evaporated in described step 2 is 80nm.
In described step 3, photoresist adopts SU-8 photoresist.
In described step 3, high temperature cabonization temperature is 900 DEG C.
Beneficial effect of the present invention is: the working electrode of electrochemical sensor adopts the meso-porous carbon material with good electric chemical property, working electrode, to electrode and contrast electrode by micro-processing method straight forming on silicon chip, achieve a kind of miniature electrochemical of integrated form; Achieve the microminiaturization of working electrode meso-porous carbon material, graphical and straight forming, not only will contribute to the integrated of sensor, Batch Design and the production of miniature electrochemical can also be realized; Can different technological parameters be adopted according to different application demands to carry out the selection of thickness to working electrode meso-porous carbon material, realize the optimization of sensor performance; And different functionalized modifications can be carried out to working electrode meso-porous carbon material and realize its different application; Functional structure is complete, can directly apply in micro-fluid chip, microfluidic system and radio sensing network.
Accompanying drawing explanation
Fig. 1 a is the vertical view of miniature electrochemical, and Fig. 1 b is the cross sectional representation of device;
Fig. 2 a-Fig. 2 d is the manufacture craft of miniature electrochemical;
Wherein 1 is device substrate, and 2 is insulation course, 3 be platinum to electrode, 4 is the contrast electrode of solid-state silver/silver chloride, and 5 is the working electrode of mesoporous carbon.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment is elaborated.
Based on a miniature electrochemical for straight forming mesoporous carbon technology, as illustrated in figs. ia and ib, comprising: device substrate 1, insulation course 2, platinum to electrode 3, the contrast electrode 4 of solid-state silver/silver chloride, the working electrode 5 of mesoporous carbon; Wherein, device substrate 1 is rectangle, and its middle is covered with the working electrode 5 of the mesoporous carbon of rectangle and certain electrical leads of extending from the working electrode 5 of mesoporous carbon; In device substrate 1 except the working electrode 5 of mesoporous carbon and lead-in wire, all cover insulation course 2, and keep gap between the working electrode 5 of insulation course 2 and mesoporous carbon and contact conductor; On insulation course 2, be outwards covered with successively centered by the working electrode 5 of mesoporous carbon and contact conductor the platinum of a little large U-shaped to electrode 3, wherein large U-shaped platinum to the contrast electrode 4 electrode 3 being covered with solid-state silver/silver chloride.
Based on a method for making for the miniature electrochemical of straight forming mesoporous carbon technology, as shown in Fig. 2 a-Fig. 2 d, comprising:
Step 1, on silicon chip with plasma enhanced chemical vapor deposition thickness be the silicon dioxide layer of 500nm as insulation course, utilize etching to obtain working electrode area by photoetching;
Step 2, obtain the figure to electrode and contrast electrode substrate region by photoetching, evaporate 80nm platinum, then stripping photoresist;
Step 3, in the silicon substrate template of working electrode area the potpourri of spin coating SU-8 photoresist and nano silicon oxide, photolithography patterning obtains working electrode area, after 900 DEG C of high temperature cabonizations, remove mould material silicon dioxide with hydrofluorite, obtain working electrode mesoporous carbon;
Step 4, on contrast electrode substrate platinum, apply silver/silver chloride slurry, obtain solid-state silver/silver chloride reference electrode.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (9)
1. based on a miniature electrochemical for straight forming mesoporous carbon technology, it is characterized in that, comprising: device substrate, insulation course, to electrode, contrast electrode, working electrode; Wherein, device substrate is rectangle, and its middle is covered with the working electrode of rectangle and certain electrical leads of extending from working electrode; In device substrate except working electrode and lead-in wire, all cover insulation course, and insulation course and keep gap between working electrode and contact conductor; On the insulating layer, centered by working electrode and contact conductor, be outwards covered with a little large U-shaped successively to electrode, wherein large U-shaped is covered with contrast electrode on electrode.
2. sensor according to claim 1, it is characterized in that, the described material to electrode is platinum.
3. sensor according to claim 1, it is characterized in that, the material of described contrast electrode is solid-state silver/silver chloride.
4. sensor according to claim 1, it is characterized in that, the material of described working electrode is mesoporous carbon.
5., based on a method for making for the miniature electrochemical of straight forming mesoporous carbon technology, it is characterized in that, comprising:
Step 1, on silicon chip with plasma enhanced chemical vapor deposition silicon dioxide layer as insulation course, utilize etching to obtain working electrode area by photoetching;
Step 2, obtain the figure to electrode and contrast electrode substrate region by photoetching, evaporate certain thickness platinum, then stripping photoresist;
Step 3, in the silicon substrate template of working electrode area the potpourri of spin coating photoresist and nano silicon oxide, photolithography patterning obtains working electrode area, after high temperature cabonization, removes mould material silicon dioxide, obtain working electrode mesoporous carbon with hydrofluorite;
Step 4, on contrast electrode substrate platinum, apply silver/silver chloride slurry, obtain solid-state silver/silver chloride reference electrode.
6. method according to claim 5, it is characterized in that, in described step 1, the deposit thickness of silicon dioxide layer is 500nm.
7. method according to claim 5, it is characterized in that, the thickness of the platinum evaporated in described step 2 is 80nm.
8. method according to claim 5, is characterized in that, in described step 3, photoresist adopts SU-8 photoresist.
9. method according to claim 5, it is characterized in that, in described step 3, high temperature cabonization temperature is 900 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106887344A (en) * | 2017-02-06 | 2017-06-23 | 清华大学 | Electrode of super capacitor and preparation method thereof and ultracapacitor |
| CN107170794A (en) * | 2016-03-08 | 2017-09-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | The chip of electrochemical in-situ response measurement is carried out applied to TEM |
| CN107991227A (en) * | 2018-01-08 | 2018-05-04 | 东北大学 | A kind of embedded type sensor device suitable for the detection of corrosion-inhibiting coating electrochemistry noise |
| CN112666235A (en) * | 2021-01-19 | 2021-04-16 | 郑州轻工业大学 | PtNi bimetal-based two-electrode integrated enzyme-free glucose sensor and preparation method thereof |
-
2015
- 2015-01-12 CN CN201510015290.1A patent/CN104502428A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| CAIWEI SHEN 等: "Direct Prototyping of Patterned Nanoporous Carbon: A Route from Materials to On-chip Devices", 《SCIENTIFIC REPORTS》 * |
| FEI TENG 等: "A micro glucose sensor based on direct prototyping mesoporous carbon electrode", 《MICROSYST TECHNOL》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107170794A (en) * | 2016-03-08 | 2017-09-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | The chip of electrochemical in-situ response measurement is carried out applied to TEM |
| CN106887344A (en) * | 2017-02-06 | 2017-06-23 | 清华大学 | Electrode of super capacitor and preparation method thereof and ultracapacitor |
| CN107991227A (en) * | 2018-01-08 | 2018-05-04 | 东北大学 | A kind of embedded type sensor device suitable for the detection of corrosion-inhibiting coating electrochemistry noise |
| CN107991227B (en) * | 2018-01-08 | 2023-11-03 | 东北大学 | Implanted sensor device suitable for electrochemical noise detection of anti-corrosion coating |
| CN112666235A (en) * | 2021-01-19 | 2021-04-16 | 郑州轻工业大学 | PtNi bimetal-based two-electrode integrated enzyme-free glucose sensor and preparation method thereof |
| CN112666235B (en) * | 2021-01-19 | 2023-03-10 | 郑州轻工业大学 | PtNi bimetal-based two-electrode integrated enzyme-free glucose sensor and preparation method thereof |
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