CN100392388C - Preparation method of electrochemical combined electrode - Google Patents
Preparation method of electrochemical combined electrode Download PDFInfo
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- CN100392388C CN100392388C CNB2005100171608A CN200510017160A CN100392388C CN 100392388 C CN100392388 C CN 100392388C CN B2005100171608 A CNB2005100171608 A CN B2005100171608A CN 200510017160 A CN200510017160 A CN 200510017160A CN 100392388 C CN100392388 C CN 100392388C
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Abstract
The present invention relates to a preparation method of a nanometer material toughening epoxy resin seal electrochemical combined electrode, which comprises three steps: (1) working electrode base materials 10 are embedded in a conductive supporting copper rod 11, the outer surfaces of the copper rods are wrapped with insulation heat contracting pipes, a hole-shaped silver reference electrode 8 is welded with a supporting copper rod 12 wrapped with the insulation heat contracting pipe, the lower end of a hole-shaped platinum counter electrode 7 is welded with a supporting copper rod 9 wrapped with the insulation heat contracting pipe, the working electrode base materials 10 are arranged in the middle, the hole-shaped silver reference electrode 8 and the hole-shaped platinum counter electrode 7 are successively arranged from the inner direction to the outer direction, the top ends of the hole-shaped silver reference electrode 8, the working electrode base materials 10 and the hole-shaped platinum counter electrode 7 are in the same plane, the supporting copper rods of the hole-shaped silver reference electrode 8, the working electrode base materials 10 and the hole-shaped platinum counter electrode 7 are fixed by the insulation heat contracting pipes, and the hole-shaped silver reference electrode 8, the working electrode base materials 10 and the hole-shaped platinum counter electrode 7 are put in molds and are fixed; (2) prepared nanometer material toughening epoxy resin seal materials are cast in the molds of the fixed electrodes, and the process of vacuum degassing and solidification is carried out; (3) after the molds are cooled, the electrodes are taken out and are polished. The preparation method of a nanometer material toughening epoxy resin seal electrochemical combined electrode can prepare combined electrodes which are used for organic phase and are combined by working electrodes, counter electrodes, and reference electrodes, such as a carbon electrode.
Description
Technical field
The invention belongs to a kind of preparation method of electrochemical combined electrode.
Background technology
In electrochemical research was measured, main research was the aspects such as course of reaction that taken place on electrode surface, so electrode and preparation method thereof has irreplaceable status in electrochemical field.Electrochemistry experiment is generally three-electrode system, independent separately to electrode, working electrode, contrast electrode, the position is unfixing, each interelectrode distance is bigger to the measurement result influence, and influence the reappearance of electrode measurement, the electrochemical cell volume is less simultaneously, has only several milliliters usually, each exposed electrode easily contacts and is short-circuited in the measurement, electrochemical workstation is caused badly damaged.The combination electrode of reporting is arranged, (China Patent No.: 03137469.7) but its suitable water use, integrated level is low; Owing to adopt glass-encapsulated, limited by encapsulating material, its have the encapsulation, the encapsulation process power consumption that are not suitable for gold electrode high, easily cracked, temp. variation resistant ability, clean shortcomings such as difficulty, cost of manufacture height.
Summary of the invention
The method that the purpose of this invention is to provide a kind of nano material toughened epoxy resin packaging electrochemical compound electrode is characterized in working electrode, electrode, contrast electrode is integrated into a compound electrode, contrast electrode and be that bilateral is poroid to electrode.The step and the condition of the inventive method are as follows;
1) working electrode that φ 1-3mm working electrode matrix material 10 is embedded conduction is supported copper bar 11, and working electrode supports copper bar 11 outsides to be surrounded by isolating shrinkable tube; The thick 0.1mm-0.5mm of poroid silver-colored contrast electrode 8 hole walls, interior diameter 0.2-0.9cm, long 0.5-1cm, the lower end be surrounded by the isolating shrinkable tube contrast electrode and support 12 welding of copper bar; Poroid platinum is to electrode 7 thick 0.1mm-0.5mm, interior diameter 0.3-1.0cm, during actual fabrication its inner diameter size greater than poroid silver-colored contrast electrode 8, long 0.5-1cm, the lower end be surrounded by isolating shrinkable tube electrode supported 9 welding of copper bar; Working electrode matrix material 10 is in the centre during assembling, by interior poroid silver-colored contrast electrode 8, the poroid platinum of being followed successively by outward to electrode 7, the three top at grade, three's support copper bar is fixed together with isolating shrinkable tube, it is fixing to put into mould then;
2). the nano material toughened epoxy resin encapsulating material of making is cast in the curing molding mould that fixes electrode, and through vacuum defoamation 30 minutes, in cold curing 24 hours, 100 ℃ solidified 1 hour; After cooling, take out electrode, polishing;
Said step of placing compound electrode in the curing molding mould is as follows; By shown in Figure 1, at first with electrode circular hole 2, spraying release agent MR-1 in the positioning round orifice 5, support copper bar 11 with electrochemical combined electrode to be packaged, one end of the electrodeless matrix material of copper bar 12 and copper bar 9 places positioning round orifice 5 on the mould underframe, fix with AB glue then, guarantee that it is vertical with mould underframe 4, make its two parts in conjunction with tight by bolt hole 3 usefulness bolts die main body 1, by bolt hole 6 usefulness bolts its two parts are combined closely on die main body 1 and mould underframe 4, working electrode matrix material 10 in the casting forming process all the time in the center of die main body electrode circular hole 2, main body electrode circular hole 2 keeps concentric with positioning round orifice 5, and working electrode matrix material 10 exceeds 1 centimetre on electrode circular hole 2 tops.
Nano material toughened epoxy resin preparation process of the present invention and condition are as follows:
Material therefor: DIS epoxy resin, hardening agent are LB-308, and silane coupling agent TM-550 is r-aminopropyl triethoxysilane (hereinafter to be referred as coupling agent TM-550), SiO
2Nano particle, mean grain size 20nm, release agent MR-1; ,
With nano particle SiO
2Be measurement standard, take by weighing material by following proportioning:
(1) hardening agent LB-308: DIS epoxy resin: nano particle: the mass ratio of coupling agent TM-550 is 20: 50: 0.5: 1; (2) take by weighing the coupling agent TM-550 of proportional quantity, join in the acetone soln of 50-100ml, after mixing, add while stirring proportional quantity in 24 hours nanometer SiO of 100 ℃ of vacuum drying
2Particle, sonicated is about 20 minutes then; (3) the DIS epoxy resin of getting proportional quantity will contain nanometer SiO in above-mentioned (2) in 100 ℃ of heating 1 hour
2The acetone soln of particle, coupling agent TM-550 is poured in the epoxy resin, do not stop to stir, clarification back sonicated 20 minutes, vacuum drying removes solvent, be warming up to 100 ℃ after, reacted 1 hour; (4) take by weighing the hardening agent LB-308 of proportional quantity, join while stirring and contain nanometer SiO in (3)
2In the epoxy resin of particle, coupling agent TM-55O, make the nano material toughened epoxy resin encapsulating material.
The electrochemical working electrode that this method is prepared, one of its characteristics be working electrode, contrast electrode to combination of electrodes together, the position relative fixed is measured accurately, favorable reproducibility, and be difficult for being short-circuited, easily polish and clean; Two of its characteristics are to adopt self-control nano-particle toughening epoxy resin as encapsulating material, remove and have the advantage of conventional epoxy resin encapsulated electrode, simultaneously, make it have corrosion resistance, solvent resistance, high temperature resistant, good toughness owing to add the performances such as toughness, pulling strengrth that coupling agent TM-550 and nano silicon improve encapsulating material; Three of its characteristics are to adopt from molding jig, and equipment is simple, easy to operate, cost of manufacture is low, can prepare carbon electrode, noble metal electrode, microelectrode, little biobelt and the tiny array electrode etc. that use in organic phase.
Description of drawings
Fig. 1 is the structure and the assembling synoptic diagram of solidified forming mould of the present invention.Among the figure, the 1st, die main body part, the 2nd, die main body electrode circular hole, the 3rd, die main body fixed bolt hole, 4 mould underframe, positioning round orifice on 5 underframe, fixed bolt hole on 6 underframe.
Fig. 2 is the cross-sectional view of the compound electrode for preparing of the present invention.Among the figure, the 7th, platinum is to electrode, and the 8th, silver-colored contrast electrode, the 9th, electrode is supported the copper bar, the 10th, the working electrode matrix material, the 11st, the working electrode matrix material is supported the copper bar, the 12nd, contrast electrode is supported the copper bar.
Embodiment
The technical solution adopted in the present invention further describes as follows in conjunction with the accompanying drawings and embodiments:
Embodiment 1:
By shown in Figure 1, at first with electrode circular hole 2, spraying release agent MR-1 in the positioning round orifice 5, with diameter is 0.3cm, the electrode matrix material 10 that long 1cm glass carbon is working electrode embeds the working electrode matrix material of conduction and supports copper bar 11, poroid silver-colored contrast electrode 8 thick 0.5mm, interior diameter 0.9cm, long 1cm, lower end and contrast electrode are supported 12 welding of copper bar, poroid platinum is to electrode 7 thick 0.1mm, interior diameter 1.0cm, long 1cm, weld with electrode being supported copper bar 9 lower end, working electrode matrix material 10 is in the centre, by the interior ring-type contrast electrode silver strip 8 that is followed successively by outward, ring-type is to electrode platinized platinum 7, the three top at grade, each electrode supports the copper bar to have isolating shrinkable tube to separate, three support the copper bar reusable heat draw to be fixed together then, the support copper bar of electrode to be packaged is not had matrix material one end place the positioning round orifice 5 that has polished on the mould underframe, fix with AB glue, guarantee that it is vertical with mould underframe 4, make its two parts in conjunction with tight by bolt hole 3 usefulness bolts die main body 1,1 combines closely by bolt hole 6 usefulness bolts with underframe 4, so that working electrode matrix material 10 in the casting forming process all the time at die main body electrode circular hole 2 centers, working electrode matrix material 10 exceeds 1 centimetre on electrode circular hole 2 tops, puts 80 ℃ of preheatings of baking oven after fixing.By hardening agent LB-308: epoxy resin DIS: nano particle: the mass ratio of coupling agent TM-550 is 20: 50: 0.5: 1 takes by weighing material: the coupling agent TM-550 that takes by weighing 0.4g, join in the acetone soln of 50ml, after mixing, add while stirring 0.2g in 24 hours nanometer SiO of 100 ℃ of vacuum drying
2Particle, sonicated is about 20 minutes then; The DIS epoxy resin of getting 20g will contain nanometer SiO in 100 ℃ of heating 1 hour
2The acetone soln of particle, coupling agent TM-550 is poured in the epoxy resin, do not stop to stir, clarification back sonicated 20 minutes, vacuum drying removes solvent, be warming up to 100 ℃ after, reacted 1 hour; Take by weighing 8g hardening agent LB-308, join while stirring and contain nanometer SiO
2In the epoxy resin of particle, coupling agent TM-550, mix and pour mould fast into, vacuum defoamation 30 minutes, cold curing 24 hours, 100 ℃ solidified 1 hour.After cooling, take out electrode, polishing.
Embodiment 2:
Working electrode matrix material 10 is a platinum filament, 1 millimeter of workplace diameter, and long 0.8cm, poroid silver-colored contrast electrode 8 thick 0.3mm, interior diameter 0.6cm, long 0.8cm, poroid platinum is to electrode 7 thick 0.3mm, interior diameter 0.8cm, long 0.8cm, operating process such as embodiment 1.
Embodiment 3:
Working electrode matrix material 10 is a spun gold, 1 millimeter of workplace diameter, and long 0.5cm, poroid silver-colored contrast electrode 8 thick 0.1mm, interior diameter 0.2cm, long 0.5cm, poroid platinum is to electrode 7 thick 0.1mm interior diameter 0.3cm, long 0.5cm, specific operation process such as embodiment 1.
Claims (2)
1. the preparation method of an electrochemical combined electrode is characterized in that, it comprises three steps: 1). working electrode matrix material (10) is embedded the support copper bar (11) that conducts electricity, and copper bar outside is surrounded by isolating shrinkable tube; The thick 0.1mm-0.3mm of poroid silver-colored contrast electrode (8), interior diameter 0.2-0.6cm, long 0.5-1cm and is surrounded by isolating shrinkable tube and supports copper bar (12) welding; Poroid platinum is to the thick 0.1mm-0.5mm of electrode (7), interior diameter 0.3-1cm, during actual fabrication its inner diameter size greater than poroid silver-colored contrast electrode (8), long 0.5-1cm,, lower end and support copper bar (9) welding that is surrounded by isolating shrinkable tube; Working electrode matrix material (10) is in the centre, by interior poroid silver-colored contrast electrode (8), the poroid platinum of being followed successively by outward to electrode (7), the three top at grade, three's support copper bar is fixed together with heat-shrink tube, puts into mould then and fixes; 2). the nano material toughened epoxy resin encapsulating material of making is cast in the mould that fixes electrode, through vacuum defoamation 30 minutes, cold curing 24 hours, 100 ℃ solidified 1 hour; 3). after cooling, take out electrode, polishing.
2. the preparation method of a kind of electrochemical combined electrode as claimed in claim 1, it is characterized in that: the preparation method of used nano material toughened epoxy resin is as follows 2):
1. hardening agent LB-308: DIS epoxy resin: nano particle: the mass ratio of coupling agent TM-550 is 20: 50: 0.5: 1; 2. take by weighing coupling agent TM-550 by proportional quantity, join in the acetone soln of 50-100ml, after mixing, add while stirring proportional quantity in 24 hours nanometer SiO of 100 ℃ of vacuum drying
2Particle, sonicated is about 20 minutes then; 3. the DIS epoxy resin of getting proportional quantity is in 100 ℃ of heating 1 hour, will be above-mentioned 2. in acetone soln pour in the epoxy resin, stirred after the clarification sonicated 20 minutes, vacuum is in the dry solvent that removes, be warming up to 100 ℃ after, reacted 1 hour; 4. take by weighing the hardening agent LB-308 of proportional quantity, in the epoxy resin in joining 3. while stirring, make the nano material toughened epoxy resin encapsulating material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100171608A CN100392388C (en) | 2005-09-23 | 2005-09-23 | Preparation method of electrochemical combined electrode |
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| CNB2005100171608A CN100392388C (en) | 2005-09-23 | 2005-09-23 | Preparation method of electrochemical combined electrode |
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| CN1758056A CN1758056A (en) | 2006-04-12 |
| CN100392388C true CN100392388C (en) | 2008-06-04 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102890108A (en) * | 2012-10-11 | 2013-01-23 | 中国科学院长春应用化学研究所 | Method for manufacturing ultra-micro array electrode |
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| CN101241098B (en) * | 2008-03-14 | 2011-08-10 | 中国科学院长春应用化学研究所 | Preparation method of double layer electrochemical working electrode with shielding outer layer |
| CN102359985B (en) * | 2011-08-01 | 2013-11-13 | 南京大学 | Coaxial microelectrode for microfluidic chip and preparation method thereof |
| CN107144613B (en) * | 2017-05-09 | 2019-01-18 | 中国石油大学(华东) | Three electrod-array Local electrochemical information test macros and test method |
| CN110146561A (en) * | 2019-05-16 | 2019-08-20 | 大连诚泽检测有限公司 | A kind of 15 microlitres of negotiable electrolytic cells |
| CN110884014A (en) * | 2019-11-28 | 2020-03-17 | 哈尔滨理工大学 | Polypropylene-based needle plate electrode sample preparation mold and preparation method |
| CN111207981B (en) * | 2020-03-01 | 2022-09-02 | 东北石油大学 | Method for manufacturing three-layer heterogeneous flat plate electrode core |
| WO2022082824A1 (en) * | 2020-10-21 | 2022-04-28 | 浙江久立特材科技股份有限公司 | Sealing structure and sealing method for electrochemical sample used in high-temperature high-pressure aqueous solution environment |
| CN113916769B (en) * | 2021-10-26 | 2023-10-20 | 西南石油大学 | High-temperature-resistant high-pressure-resistant tow electrode and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2182446A (en) * | 1985-11-08 | 1987-05-13 | Bert Settler | Antimony electrode assembly |
| JP2000055866A (en) * | 1998-08-07 | 2000-02-25 | Apurikusu:Kk | COMBINED ELECTRODE FOR pH MEASUREMENT AND FOR OXIDATION-REDUCTION POTENTIAL MEASUREMENT |
| CN2593190Y (en) * | 2003-01-14 | 2003-12-17 | 河北科技大学 | Ternary composite electrode |
| CN1462882A (en) * | 2003-06-25 | 2003-12-24 | 袁倬斌 | Method for producing complex type microelectrode |
| CN1601266A (en) * | 2004-10-08 | 2005-03-30 | 中国科学院长春应用化学研究所 | Method for fabricating electrochemical working-electrode |
| CN1601267A (en) * | 2004-10-15 | 2005-03-30 | 中国科学院长春应用化学研究院 | Micro array and prepn, method of micro double-band electrodes |
-
2005
- 2005-09-23 CN CNB2005100171608A patent/CN100392388C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2182446A (en) * | 1985-11-08 | 1987-05-13 | Bert Settler | Antimony electrode assembly |
| JP2000055866A (en) * | 1998-08-07 | 2000-02-25 | Apurikusu:Kk | COMBINED ELECTRODE FOR pH MEASUREMENT AND FOR OXIDATION-REDUCTION POTENTIAL MEASUREMENT |
| CN2593190Y (en) * | 2003-01-14 | 2003-12-17 | 河北科技大学 | Ternary composite electrode |
| CN1462882A (en) * | 2003-06-25 | 2003-12-24 | 袁倬斌 | Method for producing complex type microelectrode |
| CN1601266A (en) * | 2004-10-08 | 2005-03-30 | 中国科学院长春应用化学研究所 | Method for fabricating electrochemical working-electrode |
| CN1601267A (en) * | 2004-10-15 | 2005-03-30 | 中国科学院长春应用化学研究院 | Micro array and prepn, method of micro double-band electrodes |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102890108A (en) * | 2012-10-11 | 2013-01-23 | 中国科学院长春应用化学研究所 | Method for manufacturing ultra-micro array electrode |
| CN102890108B (en) * | 2012-10-11 | 2014-08-27 | 中国科学院长春应用化学研究所 | Method for manufacturing ultra-micro array electrode |
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| CN1758056A (en) | 2006-04-12 |
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