CN1737557A - The method of packaging electrochemical working electrode by nano material toughened epoxy resin - Google Patents
The method of packaging electrochemical working electrode by nano material toughened epoxy resin Download PDFInfo
- Publication number
- CN1737557A CN1737557A CN 200510016929 CN200510016929A CN1737557A CN 1737557 A CN1737557 A CN 1737557A CN 200510016929 CN200510016929 CN 200510016929 CN 200510016929 A CN200510016929 A CN 200510016929A CN 1737557 A CN1737557 A CN 1737557A
- Authority
- CN
- China
- Prior art keywords
- epoxy resin
- electrode
- working electrode
- mould
- nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the preparing technical field of electrochemical working electrode.Be specifically related to a kind of method of electrochemical working electrode of nano material toughened epoxy resin encapsulating material preparation, its step and condition are as follows; 1) electrode matrix material and the copper Metallic rod that embeds conduction are placed the mould of curing molding; 2) the nano material toughened epoxy resin encapsulating material of making is cast to 1) mould in; 3) after cooling, take out electrode, electrode cap is installed in polishing additional.The present invention has improved performances such as the toughness, pulling strengrth of the encapsulating material of electrochemical working electrode, therefore, the corrosion resistance that it has, available chloroazotic acid soaks, and do not deform, ftracture, and every function admirable; Solvent resistance is tested in organic solvent commonly used, all obtains good result; High temperature resistant, can be 150 ℃ of uses; Can encapsulate most of galvanochemistry working electrodes such as gold, platinum, vitreous carbon, graphite, but also the root a tree name need be made the working electrode of different color and lusters, different transparencies.
Description
Technical field
The invention belongs to the preparing technical field of electrochemical working 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.Mainly contain inorganic in the present employed electrode package material and organic material two big classes: 1. inorganic material is mainly used in the encapsulation of platinum electrode based on glass material.The existing solvent resistance of glass electrode is good, chemical inertness is high and the current potential of broad uses advantages such as zone, simultaneously its use limitation is arranged also, as is not suitable for high, the shortcoming such as cracked, temp. variation resistant ability easily of encapsulation, the encapsulation process power consumption of gold electrode; 2. employed organic material mainly contains following several in the electrochemical working electrode encapsulation: teflon (PTFE-F4), poly-trifluoro-ethylene (PCTFE-F3), epoxies plastic packaging material etc.1. teflon and poly-trifluoro-ethylene have good chemical stability, electrical insulating property and corrosion-resistant, solvent resistance, nearly all strong acid, highly basic, strong oxidizer and organic solvent are all inoperative to it, teflon can use under 250 ℃～260 ℃ high temperature for a long time, poly-trifluoro-ethylene has widely serviceability temperature-50～130 ℃, and the cohesiveness of metal is good, transparent.But these two kinds of materials all are difficult for melt fabrication, processing difficulties, the electrode that very easily causes encapsulating leaks, and causes electrode to be scrapped, the teflon encapsulating material of hydrophobic very easily has bubble attached on the electrode surface in determination of aqueous solution simultaneously, causes carrying out electrochemical measurement; Poly-trifluoro-ethylene organic solvent resistance is relatively poor, is not suitable for the electrochemical gaging of organic phase; 2. polyaryletherketone is the special engineering plastics of a series of excellent performances, have good rub resistance, fire-retardant, anti-hydrolysis and radiation resistance, good stability is easy to machine-shaping, and under conditions of work such as high temperature, high pressure and high humility, insulativity still can effectively keep; But this resinoid is as thermoplastics type's material, need higher temperature when carrying out melt-processed, and resin viscosity is bigger after the fusion, very easily bubble is wrapped near the electrode matrix, causes the electrode can't operate as normal, and starting material are comparatively expensive; 3. the epoxies plastic packaging material has the purity height, adhesion is good, cost is low, the worker saves advantages such as simple.But because of its curing material is crisp, resistance to cracking energy, shock resistance are lower, and poor heat resistance, make its application be subjected to certain restriction.
Summary of the invention
The method that the purpose of this invention is to provide a kind of packaging electrochemical working electrode by nano material toughened epoxy resin.Its step and condition are as follows;
1). the copper Metallic rod 10 of electrode matrix material 8 and embedding conduction is placed the mould of curing molding;
2). the nano material toughened epoxy resin encapsulating material of making is cast in the mould of step 1),, solidified 1-4 hour in 100-150 ℃ through vacuum defoamation 15-60 minute;
3). after cooling, take out electrode, electrode cap 11 is installed in polishing additional.
The said the 2nd) the nano material toughened epoxy resin preparation process and the condition of step usefulness are as follows:
With hardening agent 548 is measurement standard, takes by weighing material by following proportioning:
(1) hardening agent 548: epoxy resin DIS:, SiO
2Nano particle: the mass ratio of coupling agent TM-550 is 1: 1-3: 0.0025-0.015: 0.005-0.03; (2) take by weighing the coupling agent TM-550 of proportional quantity, it joined in the acetone soln of 50-100ml, after mixing, add while stirring proportional quantity in 90-100 ℃ of vacuum drying 20-25 hour SiO
2Nano particle, sonicated 15-25 minute then; (3) the epoxy resin DIS that gets proportional quantity contains SiO in 95-105 ℃ of heating 1-1.2 hour in above-mentioned 2
2The acetone soln of nano particle, coupling agent TM-550 is poured among the epoxy resin DIS, do not stop to stir, clarification back sonicated 15-25 minute, vacuum drying removes solvent, be warming up to 100-150 ℃ after, reacted 1-2 hour; (4) take by weighing the hardening agent 548 of proportional quantity, join while stirring in (3) and contain SiO
2Among the epoxy resin DIS that the acetone soln of nano particle, coupling agent TM-550 is handled well, make the nano material toughened epoxy resin encapsulating material;
The curing molding mould that the present invention is used is described below again: Fig. 1 is the structure and the assembling synoptic diagram of curing molding mould of the present invention; Among the figure: 1 die main body, 2 die main body electrode circular holes, 3 die main body set bolts, 4 mould underframe, positioning round orifice on 5 underframe, set bolt on 6 underframe, 7 underframe set bolts
Said step of placing electrode in the curing molding mould is as follows:
By shown in Figure 1, at first will be in electrode circular hole 2, the positioning round orifice 5 spraying release agent MR-1, the copper Metallic rod 10 and the electrode matrix material 8 of the conduction of intercalation electrode matrix material 8 placed the positioning round orifice 5 that has sprayed release agent MR-1 on the mould underframe; Mould underframe 4 is made its fluid-tight engagement by bolt 7, fix copper Metallic rod 10, die main body 1 is made its fluid-tight engagement by bolt 3, die main body 1 and underframe 4 are by bolt 6 fluid-tight engagement, so that Metallic rod 10 is concentric with electrode matrix material 8 outer rims all the time in the casting forming process, 1 centimetre on top distance electrode circular hole 2 tops of copper Metallic rod 10.
The electrochemical working electrode that the present invention is prepared except that having the advantage of conventional epoxy resin encapsulated electrode, adds the coupling agent TM-550 and the SiO of different proportion simultaneously
2Nano particle improves performances such as the toughness, pulling strengrth of encapsulating material, make it have advantages such as corrosion resistance, solvent resistance, high temperature resistant, good toughness and preparation equipment is simple, easy to operate: the corrosion resistance that it has, available chloroazotic acid soaks, do not deform, ftracture, and every function admirable; Solvent resistance is tested in organic solvent commonly used, all obtains good result; High temperature resistant, can be 150 ℃ of uses; Also but the root a tree name need be made the galvanochemistry working electrode of different color and lusters, different transparencies, can encapsulate most of galvanochemistry working electrodes such as gold, platinum, vitreous carbon, graphite.
Description of drawings
Fig. 1 is a curing molding mold structure synoptic diagram of the present invention.
Fig. 2 is the working electrode longitudinal profile structural map after the founding processing.
Embodiment
Embodiment 1:
1). the copper Metallic rod 10 of electrode matrix material 8 and the conduction that embeds is inserted mould: by shown in Figure 1, at first with electrode circular hole 2, spraying release agent MR-1 in the positioning round orifice 5, the material of electrode matrix 8 is a gold, 1 millimeter of workplace diameter, sprayed the positioning round orifice 5 of release agent MR-1 on placing the copper Metallic rod 10 of the conduction of intercalation electrode matrix 8 and electrode matrix 8 at the bottom of the mould, mould underframe 4 is made its fluid-tight engagement by bolt 7, fix copper Metallic rod 10, die main body 1 is made its fluid-tight engagement by bolt 3, spraying release agent MR-1 and underframe 4 are by bolt 6 fluid-tight engagement, so that Metallic rod 10 is concentric with electrode matrix material 8 outer rims all the time in the casting forming process, 1 centimetre on top distance electrode circular hole 2 tops of copper Metallic rod 10;
2). the nano material toughened epoxy resin encapsulating material of making is cast to 1) mould in step, the preparation of used nano material toughened epoxy resin: (1) presses hardening agent 548: epoxy resin DIS: SiO
2Nano particle: the mass ratio of coupling agent TM-500 is 1: 1: 0.015: 0.03, take by weighing epoxy resin DIS 20 grams, 548 hardening agent, 20 grams, SiO
2Nano particle 0.05 gram, coupling agent TM-5000.1 gram, SiO
2Nano particle is earlier 100 ℃ of vacuum drying 24 hours; (2) coupling agent TM-500 is joined in the acetone soln of 50ml, after mixing, add at 24 hours SiO of 100 ℃ of vacuum drying while stirring
2Nano particle, sonicated is 20 minutes then; (3) epoxy resin is in 100 ℃ of heating 1 hour, with the SiO that contains in above-mentioned (2)
2The acetone soln of nano particle, coupling agent TM-550 is poured in the epoxy resin, does not stop to stir, and clarification back sonicated is about 15 minutes, and vacuum drying removes solvent, is warming up to 100 ℃ of reactions and makes nano material toughened epoxy resin in 2 hours; (4) take by weighing the hardening agent 548 of proportional quantity, join while stirring in (3) and contain SiO
2Among the epoxy resin DIS that the acetone soln of nano particle, coupling agent TM-550 is handled well, make the nano material toughened epoxy resin encapsulating material and it is cast in the mould of step 1), through vacuum defoamation 15 minutes, solidified the encapsulating material main body 9 of formation electrode 4 hours in 100 ℃;
3). after cooling, the taking-up electrode, electrode cap 11 is installed in polishing additional.
The gold that is used to prepare, platinum, vitreous carbon, graphite electrochemistry working electrode are dark red, and be opaque.
Embodiment 2:
1). the step such as the embodiment 1 of the copper Metallic rod 10 of the conduction of mould and pack within it electrode matrix 8 and embedding, electrode matrix 8 is a vitreous carbon, 3 millimeters of workplace diameters;
2). press hardening agent 548: epoxy resin DIS: SiO
2Nano particle: the mass ratio of coupling agent TM-500 is 1: 2: 0.015: 0.03 takes by weighing material, takes by weighing epoxy resin DIS 20 grams, 548 hardening agent, 10 grams, SiO
2Nano particle 0.15 gram, coupling agent TM-5000.3 gram, acetone 80ml, initial disposal route is with embodiment 1, and vacuum drying removes solvent, is warming up to 120 ℃ of reactions 1.5 hours; Take by weighing the hardening agent 548 of proportional quantity, join the above-mentioned SiO that contains while stirring
2Among the epoxy resin DIS that the acetone soln of nano particle, coupling agent TM-550 is handled well, make the nano material toughened epoxy resin encapsulating material and it is cast in the mould of step 1), then, vacuum defoamation 30 minutes, 125 ℃ solidified 2 hours, formed the encapsulating material main body 9 of electrode;
3). after the cooling, take out electrode, electrode cap 11 is installed in polishing additional.Electrode is red, translucent.
Embodiment 3:
1). the copper Metallic rod 10 of mould and pack within it electrode matrix 8 and embedding conduction is as embodiment 1, and electrode matrix 8 is a platinum, 1 millimeter of workplace diameter;
2) press hardening agent 548: epoxy resin DIS: SiO
2Nano particle: the mass ratio of coupling agent TM-500 is 1: 3: 0.0025: 0.005 takes by weighing material, takes by weighing epoxy DIS 20 grams, 548 hardening agent, 6.7 grams, SiO
2Nano particle 0.25 gram, coupling agent TM-5000.5 gram, acetone 100ml, initial disposal route is with embodiment 1, and vacuum drying removes solvent, is warming up to 150 ℃ of reactions 1 hour; Take by weighing the hardening agent 548 of proportional quantity, join the above-mentioned SiO that contains while stirring
2Among the epoxy resin DIS that the acetone soln of nano particle, coupling agent TM-550 is handled well, make the nano material toughened epoxy resin encapsulating material and it is cast in the mould of step 1), then, take by weighing the hardening agent 548 of proportional quantity, join the above-mentioned SiO that contains while stirring
2Among the epoxy resin DIS that the acetone soln of nano particle, coupling agent TM-550 is handled well, make the nano material toughened epoxy resin encapsulating material and it is cast in the mould of step 1), then, vacuum defoamation 60 minutes, 150 ℃ solidified 1 hour, formed the encapsulating material main body 9 of electrode;
3). after the cooling, take out electrode, electrode cap 11 is installed in polishing additional.Electrode is red and transparent.
Claims (1)
1, a kind of method of packaging electrochemical working electrode by nano material toughened epoxy resin, it comprises:
1). the copper Metallic rod (10) of electrode matrix material (8) and embedding conduction is placed the mould of curing molding; It is characterized in that it also comprises:
2). the nano material toughened epoxy resin encapsulating material of making is cast to 1) mould in, through vacuum defoamation 15-60 minute, solidified 1-4 hour in 100-150 ℃;
3). after cooling, take out electrode, electrode cap (11) is installed in polishing additional;
The said the 2nd) the nano material toughened epoxy resin preparation process and the condition of step usefulness are as follows:
With hardening agent 548 is measurement standard, takes by weighing material by following proportioning:
1. hardening agent 548: epoxy resin DIS:, SiO
2Nano particle: the mass ratio of coupling agent TM-550 is 1: 1-3: 0.0025-0.015: 0.005-0.03;
2. take by weighing the coupling agent TM-550 of proportional quantity, it joined in the acetone soln of 50-100ml, after mixing, add while stirring proportional quantity in 90-100 ℃ of vacuum drying 20-25 hour SiO2 nano particle, sonicated 15-25 minute then;
3. the epoxy resin DIS that gets proportional quantity is in 95-105 ℃ of heating 1-1.2 hour, contains SiO with above-mentioned in 2.
2The acetone soln of nano particle, coupling agent TM-550 is poured among the epoxy resin DIS, do not stop to stir, clarification back sonicated 15-25 minute, vacuum drying removes solvent, be warming up to 100-150 ℃ after, reacted 1-2 hour;
4. take by weighing the hardening agent 548 of proportional quantity, contain SiO in joining 3. while stirring
2Among the epoxy resin DIS that the acetone soln of nano particle, coupling agent TM-550 is handled well, make the nano material toughened epoxy resin encapsulating material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100169294A CN100392386C (en) | 2005-07-01 | 2005-07-01 | Method for packaging electrochemical working electrode by nano material toughened epoxy resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100169294A CN100392386C (en) | 2005-07-01 | 2005-07-01 | Method for packaging electrochemical working electrode by nano material toughened epoxy resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1737557A true CN1737557A (en) | 2006-02-22 |
| CN100392386C CN100392386C (en) | 2008-06-04 |
Family
ID=36080426
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100169294A Expired - Fee Related CN100392386C (en) | 2005-07-01 | 2005-07-01 | Method for packaging electrochemical working electrode by nano material toughened epoxy resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100392386C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101894810A (en) * | 2009-05-21 | 2010-11-24 | 台湾积体电路制造股份有限公司 | Composite underfill, semiconductor package and its forming method |
| CN101434748B (en) * | 2008-12-04 | 2011-03-30 | 上海大学 | Preparation of nano zinc oxide modified organosilicon encapsulation adhesive |
| 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 |
| CN103558077A (en) * | 2013-11-06 | 2014-02-05 | 上海电机学院 | Packaging method for electrochemical testing sample |
| CN104103780A (en) * | 2013-04-15 | 2014-10-15 | 罗伯特·博世有限公司 | Battery cell with a cover consisting of at least two parts and a method of manufacturing same |
| CN111919156A (en) * | 2018-03-02 | 2020-11-10 | 古奇及豪斯格公共有限公司 | Mounting ring for maintaining alignment of optical devices |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050127329A1 (en) * | 2001-08-17 | 2005-06-16 | Chyi-Shan Wang | Method of forming nanocomposite materials |
| JP2004196977A (en) * | 2002-12-19 | 2004-07-15 | Kyoritsu Kagaku Sangyo Kk | Cation-curable silicone resin composition |
| CN1238459C (en) * | 2003-12-09 | 2006-01-25 | 清华大学 | High connecting intensity thermosetting conducting resin |
| 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 |
| CN100488758C (en) * | 2005-01-04 | 2009-05-20 | 武汉科技大学 | Nanometer carbon tube/epoxy resin composite material and its preparation method |
-
2005
- 2005-07-01 CN CNB2005100169294A patent/CN100392386C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101434748B (en) * | 2008-12-04 | 2011-03-30 | 上海大学 | Preparation of nano zinc oxide modified organosilicon encapsulation adhesive |
| CN101894810A (en) * | 2009-05-21 | 2010-11-24 | 台湾积体电路制造股份有限公司 | Composite underfill, semiconductor package and its forming method |
| CN104103780A (en) * | 2013-04-15 | 2014-10-15 | 罗伯特·博世有限公司 | Battery cell with a cover consisting of at least two parts and a method of manufacturing same |
| CN104103780B (en) * | 2013-04-15 | 2017-11-17 | 罗伯特·博世有限公司 | Battery battery core and its manufacture method with the cap being made up of at least two parts |
| CN103558077A (en) * | 2013-11-06 | 2014-02-05 | 上海电机学院 | Packaging method for electrochemical testing sample |
| CN103558077B (en) * | 2013-11-06 | 2016-03-02 | 上海电机学院 | The method for packing of electro-chemical test sample |
| CN111919156A (en) * | 2018-03-02 | 2020-11-10 | 古奇及豪斯格公共有限公司 | Mounting ring for maintaining alignment of optical devices |
| CN111919156B (en) * | 2018-03-02 | 2022-07-15 | 古奇及豪斯格公共有限公司 | Mounting ring for maintaining alignment of optical devices |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100392386C (en) | 2008-06-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100392386C (en) | Method for packaging electrochemical working electrode by nano material toughened epoxy resin | |
| CN106750899A (en) | A kind of basalt long fiber reinforced polypropylene compound material and application thereof | |
| CN105542227A (en) | Carbon fiber reinforcement and preparation method thereof | |
| CN109206849A (en) | A kind of high heat conductive insulating composition epoxy resin and preparation method | |
| CN102757712A (en) | Preparation method of high thermal conduction insulating varnish | |
| CN109205594A (en) | A kind of preparation method and applications of graphene conductive microballoon | |
| CN103694635A (en) | Room-temperature rapid self-repairing composite material based on microencapsulated epoxy resin and super-strong-acid curing agent | |
| CN103194166A (en) | Photo-thermal double-curing conductive adhesive and preparation method thereof | |
| CN108580796A (en) | A kind of casting inorganic binder and preparation method thereof | |
| CN103627107A (en) | Preparation method for polystyrene/silver/polypyrrole composite material | |
| CN102010566A (en) | Method for preparing epoxy moulding compound for packaging integrated circuit | |
| CN1601266A (en) | Method for fabricating electrochemical working-electrode | |
| CN101097208B (en) | Polymethyl methacryate and carbon nano-tube compound material electric pole and method for making same | |
| CN105255154A (en) | Method for preparing thermosetting-resin-based heat conduction composite | |
| CN101241098B (en) | Preparation method of double layer electrochemical working electrode with shielding outer layer | |
| CN1844269A (en) | Phase-transition energy-storage microcapsules and their preparing process | |
| Su et al. | Self-healing polymeric materials | |
| CN106608008B (en) | A kind of release agent and preparation method thereof and the application in epoxy resin encapsulated | |
| CN1554524A (en) | Method for preparing demolding agent for roducing epoxy glass fibre reinforced plastic composite material | |
| CN103657653B (en) | A kind of solid acid catalyst C/Fe3O4The method of MWCNTs and catalyzing cellulose hydrolysis thereof | |
| CN105885012A (en) | Method for preparing modified epoxy resin for LED (light emitting diode) packaging | |
| CN1238459C (en) | High connecting intensity thermosetting conducting resin | |
| CN101565535A (en) | Heat resistant epoxide resin and preparation method thereof | |
| CN101417946A (en) | Method for preparing pentachlorobenzoyl chloride | |
| CN111303498A (en) | Natural rubber and preparation process thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080604 Termination date: 20110701 |