CN100362342C - A kind of preparation method of carbon fiber ultramicro disk electrode - Google Patents
A kind of preparation method of carbon fiber ultramicro disk electrode Download PDFInfo
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- CN100362342C CN100362342C CNB2005100198314A CN200510019831A CN100362342C CN 100362342 C CN100362342 C CN 100362342C CN B2005100198314 A CNB2005100198314 A CN B2005100198314A CN 200510019831 A CN200510019831 A CN 200510019831A CN 100362342 C CN100362342 C CN 100362342C
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Abstract
本发明涉及碳纤维超微盘电极的制备方法，包括以下步骤：将穿有碳纤维的玻璃管的一端加热直至其熔融闭合并使碳纤维前端固定在玻璃管中；通过玻璃管的另一端对玻璃管抽真空；在保持抽真空条件下，对有碳纤维的玻璃管部位加热熔融，使碳纤维熔封在玻璃管中；将锡粉或焊锡丝从玻璃管的开口端装入，加热玻璃管至金属锡熔化，使其落入玻璃管底部与碳纤维形成良好接触；在金属锡固化前插入电子导线，形成电联接；对封有碳纤维的一段进行打磨，即得到碳纤维超微盘电极。本发明操作简单，成本低廉，制备的碳纤维微盘电极具有密封严实、电子电阻小、电化学性能优良、盘电极表面易更新，抗震动能力强等优点。
The invention relates to a preparation method of a carbon fiber ultramicrodisk electrode, comprising the following steps: heating one end of a glass tube pierced with carbon fiber until it melts and closes and fixing the front end of the carbon fiber in the glass tube; pumping the glass tube through the other end of the glass tube Vacuum; under the condition of maintaining vacuum, heat and melt the glass tube with carbon fiber, so that the carbon fiber is sealed in the glass tube; put tin powder or solder wire into the open end of the glass tube, heat the glass tube until the metal tin melts , so that it falls into the bottom of the glass tube to form a good contact with the carbon fiber; insert the electronic wire before the metal tin solidifies to form an electrical connection; polish a section sealed with the carbon fiber to obtain a carbon fiber ultra-microdisk electrode. The invention has simple operation and low cost, and the prepared carbon fiber micro-disk electrode has the advantages of tight sealing, small electronic resistance, excellent electrochemical performance, easy renewal of the surface of the disc electrode, strong anti-vibration ability and the like.
Description
Technical field
The present invention relates to a kind of preparation method of carbon fiber ultramicro disc electrode.
Background technology
Carbon fiber electrode is used widely in Electroanalytical Chemistry and life science because of the advantage of himself.The carbon fiber electrode of traditional preparation process often adopts epoxy sealing, the leakage of the easy initial ring epoxy resins of electrode of this method preparation, thus can pollute electrochemical system, and cause the sensitivity of electrode and the signal to noise ratio (S/N ratio) of detection signal to reduce; In addition, the electrode of epoxy sealing can not be worked in organic electrolyte and hot environment.The carbon fiber electrode of glass head seal can effectively address the above problem.Generally there are two kinds of methods can realize the glass head seal of carbon fiber electrode: first method (Huang, Wei-Hua; Pang, Dai-Wen; Tong, Hua; Wang, Zong-Li; Cheng, Jie-Ke.Analytical Chemistry (2001), 73 (5), 1048-1052.) be that carbon fiber is placed in the kapillary of drawing-down, with kapillary quick sealing by fusing on flame, can prepare carbon fiber post electrode then, this electrode can be used for monitoring in real time single celled dispose procedure, but because electrode true shape and effective surface area be difficult to determine, so quantitative test has difficulties; This electrode is difficult to prepare microdisk electrode because front end is too thin in addition.Another kind method (Zhang, Xueji; Zhang, Wuming; Zhou, Xingyao; Ogorevc, Bozidar.AnalyticalChemistry (1996), 68 (19), it is heat-sealable 3338-3343.) to be that the kapillary that will carbon fiber be housed adds with resistance wire in vacuum tank, and an end of carbon fiber is connected with electronic wire with Ag powder epoxy resin; External commercial carbon fiber electrode all adopts this method preparation at present, the carbon fiber microdisk electrode of this method preparation has advantages such as sealing effectiveness is better, the surface is renewable, yet, because apparatus expensive, complicated operation, cause the electrode cost of manufacture high (commercial diameter be several microns carbon fiber microdisk electrode price about 1000RMB/root), in addition, the electrode of this method preparation in use, the phenomenon that carbon fiber and electronic wire loose contact or disconnecting are touched can appear, in a single day this phenomenon occurs, and just can't remedy.
Summary of the invention
The objective of the invention is: the preparation method that carbon fiber ultramicro disc electrode a kind of simple to operate, with low cost is provided.This method can overcome the drawback of epoxide-resin glue envelope carbon fiber electrode, can solve the contact problems of carbon fiber and electronic wire in the heat-sealable technology of traditional glass again.
As follows for realizing preparation technology's method that the object of the invention takes: a kind of preparation method of carbon fiber ultramicro disc electrode may further comprise the steps: (1) will be installed with diameter is that the end heating of glass tube of the following carbon fiber of 10 μ m is closed and the carbon fiber front end is fixed in the glass tube until its fusion; (2) other end by glass tube vacuumizes glass tube, and inner air tube is extracted out; (3) vacuumize under the condition in maintenance, to the glass tube position heating and melting of carbon fiber is arranged, the glass tube of fusion is subjected to the effect of external pressure and forms closely knit combining with the interior carbon fiber surface of pipe, and carbon fiber is sealed in the glass tube; (4) solder powder or solder stick are packed into from the openend of glass tube, the heating glass pipe makes it fall into the glass tube bottom and forms good the contact with carbon fiber to melts soldering tin; (5) insert electronic wire before scolding tin solidifies, formation electrically connects; (6) there is the end face of an end of carbon fiber to polish to envelope, promptly obtains carbon fiber ultramicro disc electrode.
The present invention can be when step (2) vacuumize, to the glass tube heating, make residual air expanded by heating in the pipe and are taken away.
The present invention also can use the openend of fluid sealant sealed glass tube in step (6) afterwards, with the contact resistance increase that prevents to be caused by airborne dioxygen oxidation because of tin.
The length of above-mentioned carbon fiber sealing by fusing in glass tube is 1 ± 0.5cm.
Described electronic wire is copper wire or filamentary silver.
The present invention is simple to operate, with low cost, the preparation the carbon fiber microdisk electrode have the sealing tight, between carbon fiber post surface and seal glass, do not have bubble, electronics resistance is little, chemical property is good, the surperficial easy renewal of disc electrode, the strong advantages such as (during strenuous vibration, carbon fiber still can keep good the contact with electronic wire) of anti-vibration ability; Behind electrode front end sharpening, also can be made into the probe electrode of scan-type electrochemical microscope method (SECM), be used for the microcell electrochemical activity of quantitative detecting analysis inorganic material and biosome.In addition, the carbon fiber microdisk electrode of this method preparation is in long-term use, if the loose contact of carbon fiber and electronic wire, available little fiery heating electrode stalk makes scolding tin fusion again, can improve contact.
Description of drawings:
Fig. 1 is the structural representation of carbon fiber ultramicro disc electrode of the present invention.
Fig. 2 is that the optics at electrode sealing by fusing place amplifies 200 times photo (not polishing, clip alveolate the last period).
Fig. 3 amplifies 200 times photo for the optics at the carbon fiber electrode sealing by fusing place of direct flame sealing by fusing (not vacuumizing).
Fig. 4 amplifies 5000 times stereoscan photograph for the carbon fiber ultramicro disc electrode end face of the present invention's preparation.
Fig. 5 amplifies 5000 times stereoscan photograph for the carbon fiber ultramicro disc electrode end face of direct flame sealing by fusing (not vacuumizing).
Fig. 6 is the cyclic voltammetry curve of carbon fiber ultramicro disc electrode in the potassium ferricyanide solution of 20mM.
Embodiment:
Referring to Fig. 1, carbon fiber (d≤10 μ m) was used acetone, absolute ethyl alcohol, ultrapure water ultrasonic cleaning 3～5 minutes successively, use a large amount of ultrapure water drip washing after the taking-up again; It is standby then the carbon fiber of cleaning to be placed in the vacuum drying chamber 50 degrees centigrade of dryings 10 hours.With the diameter that cleaned is that carbon fiber 1 that 7 μ m are about 2cm inserts internal diameter and is about in the glass tube 4 of cleaning that 2mm is about 6cm, and a section an of end 8 about 0.5mm of carbon fiber 1 is exposed to outside the glass tube 4; Closed and the carbon fiber front end is fixed in the glass tube 4 to end 7 heating of glass tube 4 that carbon fiber 1 is arranged until its fusion.The other end 6 of glass tube 4 (being openend) is linked to each other with vacuum pump by plastic tube, vacuumized 20 minutes; Then when keeping vacuumizing,, make the interior residual air expanded by heating of pipe and taken away by vacuum pump glass tube 4 fast moving heating (residual gas is heated and not fusion of glass can guarantee like this to manage in) 3 minutes back and forth on spirit lamp flame; Then with alcohol blast burner or gaslight flame with the carbon fiber 1 sealing by fusing 1cm in the glass tube 4; After sealing by fusing finishes, plastic tube is pulled away from the glass tube openend; The solder stick 2 that is 0.5mm to diameter inserts from glass tube openend 6, and heating glass pipe 4 on spirit lamp makes solder stick 2 fusings, and falls into the glass tube bottom with carbon fiber 1 complete embedding; Before scolding tin 2 solidifies, a copper wire 3 (or filamentary silver) that is about 10cm is inserted in the scolding tin 2 of molten state; After scolding tin 2 solidifies, coat epoxy resin 5 sealings at glass tube openend 6.Behind the epoxy resin cure, the end face of polishing electrode can obtain carbon fiber ultramicro disc electrode.The electrode structure synoptic diagram as shown in Figure 1.Fig. 2 has provided this electrode side optics and has amplified 200 times photo; Fig. 3 amplifies 200 times photo for the carbon fiber electrode side optics of direct flame sealing by fusing (not vacuumizing); Comparison diagram 2 Fig. 3, combine between the carbon fiber ultramicro disc electrode carbon fiber of this method preparation and glass as can be known tight, do not have bubble, surface advantages such as renewal of can polishing; And it is a lot of not vacuumize between the electrode carbon fiber of direct flame sealing by fusing and glass bubble, uncomfortable cooperation microdisk electrode.Fig. 4 electrode end surface polishing back for this reason amplifies 5000 times electromicroscopic photograph, Fig. 5 amplifies 5000 times electromicroscopic photograph for the carbon fiber electrode end face polishing back of direct flame sealing by fusing (not vacuumizing), comparison diagram 4 Fig. 5, the carbon fiber electrode sealing effectiveness that further specifies direct flame sealing by fusing (not vacuumizing) is poor, and the carbon fiber electrically of this method preparation has the characteristic of good seal.Fig. 6 cyclic voltammetry curve of carbon fiber electrode in the potassium ferricyanide solution of 20mM for this reason (sweeps speed and is 10mV s
-1), this figure has illustrated that the carbon fiber ultramicro disc electrode of this method preparation has good electrochemical properties.
Claims (5)
1. the preparation method of a carbon fiber ultramicro disc electrode is characterized in that may further comprise the steps: (1) will be installed with diameter is that the end heating of glass tube of the following carbon fiber of 10 μ m is closed and the carbon fiber front end is fixed in the glass tube until its fusion; (2) other end by glass tube vacuumizes glass tube, and inner air tube is extracted out; (3) vacuumize under the condition in maintenance, to the glass tube position heating and melting of carbon fiber is arranged, the glass tube of fusion is subjected to the effect of external pressure and forms closely knit combining with the interior carbon fiber surface of pipe, and carbon fiber is sealed in the glass tube; (4) solder powder or solder stick are packed into from the openend of glass tube, the heating glass pipe makes it fall into the glass tube bottom and forms good the contact with carbon fiber to melts soldering tin; (5) insert electronic wire before scolding tin solidifies, formation electrically connects; (6) there is the end face of an end of carbon fiber to polish to envelope, promptly obtains carbon fiber ultramicro disc electrode.
2. preparation method according to claim 1 is characterized in that: when step (2) vacuumizes, to glass tube heating, make residual air expanded by heating in the pipe and taken away.
3. preparation method according to claim 1 and 2 is characterized in that: in step (6) afterwards, and with the openend of fluid sealant sealed glass tube.
4. preparation method according to claim 1 and 2 is characterized in that: the length of carbon fiber sealing by fusing in glass tube is 1 ± 0.5cm.
5. preparation method according to claim 1 and 2 is characterized in that: described electronic wire is copper wire or filamentary silver.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100198314A CN100362342C (en) | 2005-11-18 | 2005-11-18 | A kind of preparation method of carbon fiber ultramicro disk electrode |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100198314A CN100362342C (en) | 2005-11-18 | 2005-11-18 | A kind of preparation method of carbon fiber ultramicro disk electrode |
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| CN1776415A CN1776415A (en) | 2006-05-24 |
| CN100362342C true CN100362342C (en) | 2008-01-16 |
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| CNB2005100198314A Expired - Fee Related CN100362342C (en) | 2005-11-18 | 2005-11-18 | A kind of preparation method of carbon fiber ultramicro disk electrode |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100533135C (en) * | 2006-12-29 | 2009-08-26 | 中国科学院长春应用化学研究所 | rotating point-disk electrode |
| CN100545648C (en) * | 2007-05-15 | 2009-09-30 | 中国科学院长春应用化学研究所 | A kind of preparation method of microdisk electrode or microdisk array electrode |
| CN102436997B (en) * | 2011-12-02 | 2014-01-22 | 哈尔滨工业大学 | Preparation method of carbon fiber cathode emitting large area uniform electron beams |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5254235A (en) * | 1992-02-26 | 1993-10-19 | The Yellow Springs Instrument Company | Microelectrode arrays |
| CN1110786A (en) * | 1994-04-29 | 1995-10-25 | 武汉大学 | Ultramicro nm electrode and ultramicro sensor |
| JP2001021580A (en) * | 1999-06-22 | 2001-01-26 | Ind Technol Res Inst | Method of manufacturing probe device |
| CN1282870A (en) * | 1999-07-30 | 2001-02-07 | 武汉大学 | Process for preparing low-noise non-class carbon fibre electrode |
| CN1544928A (en) * | 2003-11-17 | 2004-11-10 | 中国科学院长春应用化学研究所 | Preparing method of micro disk array electrode |
-
2005
- 2005-11-18 CN CNB2005100198314A patent/CN100362342C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5254235A (en) * | 1992-02-26 | 1993-10-19 | The Yellow Springs Instrument Company | Microelectrode arrays |
| CN1110786A (en) * | 1994-04-29 | 1995-10-25 | 武汉大学 | Ultramicro nm electrode and ultramicro sensor |
| JP2001021580A (en) * | 1999-06-22 | 2001-01-26 | Ind Technol Res Inst | Method of manufacturing probe device |
| CN1282870A (en) * | 1999-07-30 | 2001-02-07 | 武汉大学 | Process for preparing low-noise non-class carbon fibre electrode |
| CN1544928A (en) * | 2003-11-17 | 2004-11-10 | 中国科学院长春应用化学研究所 | Preparing method of micro disk array electrode |
Non-Patent Citations (4)
| Title |
|---|
| Fabrication of carbon microelectrodes with an effective radiusof 1 nm. Shengli Chen etc.Electrochemistry Communications,Vol.4 . 2002 * |
| Fabrication, Characterization, and Potential Application ofCarbon Fiber Cone Nanometer-SizeElectrodes. Xueji Zhang etc.Anal. Chem.,Vol.68 No.19. 1996 * |
| 再生碳纤维电极的新方法. 张丽瑶等.分析科学学报，第18卷第6期. 2002 * |
| 碳纤维组合超微圆盘电极的伏安特性与理论验证. 赵凯元等.分析化学研究报告，第31卷第2期. 2003 * |
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