CN107328833A - The high temperature resistant wire beam electrode and preparation method characterized for combined material chip - Google Patents
The high temperature resistant wire beam electrode and preparation method characterized for combined material chip Download PDFInfo
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- CN107328833A CN107328833A CN201710560236.4A CN201710560236A CN107328833A CN 107328833 A CN107328833 A CN 107328833A CN 201710560236 A CN201710560236 A CN 201710560236A CN 107328833 A CN107328833 A CN 107328833A
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- stainless steel
- steel bar
- beam electrode
- wire
- combined material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
Abstract
The present invention provides a kind of high temperature resistant wire beam electrode characterized for combined material chip and preparation method, belongs to high-flux electric chemical characterization techniques field.The wire beam electrode include stainless steel bar, glass powder, wire and wire connector plug, by by stainless steel bar it is regularly arranged after with glass pouring sealing surely after connecting wire wire beam electrode is made.Combined material chip surface current Potential distribution is measured using wire beam electrode current level scanner.The wire beam electrode have the advantages that simple in construction, small volume, high temperature resistant, under vacuum conditions it is non-volatile, available for combined material chip high-flux electric chemical characterization under hot conditions, characterized for the chemical table of high-flux electric and provide a kind of measurement apparatus.
Description
Technical field
The present invention relates to high-flux electric chemical characterization techniques field, particularly relate to a kind of characterize for combined material chip
High temperature resistant wire beam electrode and preparation method.
Background technology
Combinatorial material chip approach is in nineteen ninety-five by Lawrence Berkeley laboratory Xiang Xiaodong et al.《Nature》
Put forward first, be primarily intended to the material sample by once testing simultaneously synthesizing up to 108 kinds, realize in high flux experiment
High flux prepare, this technology is studied and accelerated in multicomponent alloy phasor collection of illustrative plates by the fast developments of decades
The research and development of material and screening field achieve notable achievement.Although the high Throughput Preparation of material has reached its maturity,
Iron-enriched yeast under actual Service Environment but develop it is relatively slow, particularly electrochemical field lack always it is a kind of efficiently,
Quick characterization method.At present, the measurement of high-flux electric chemical field is main uses U.S. Princeton Applied
Research, AMETEK, the VersaSCAN microcell Electrochemical Scanning systems of Inc. exploitations, wherein the droplet experiment of scanning electrolyte
It is most with microcell electrochemical impedance experimental applications.Wire beam electrode as microcell electrochemistry important survey tool, with multiprobe
The characteristics of, larger potentiality are possessed in terms of high-flux electric chemical characterization.
At present, the wire beam electrode used is that the small probe of certain amount is evenly distributed, then uses epoxy resin encapsulation
Each probe can be used as the multiprobe electrode worked independently after solidification, independent patch.Wire beam electrode is mainly used in organic coating
Inhomogeneities evaluation and characterize metal local corrosion situation in terms of.But due to the epoxy resin fusing point for encapsulation compared with
It is low, in 200 DEG C of military services wire beam electrode only up to be caused not apply in high temperature environments.If it is intended to using wire beam electrode
, it is necessary to carry out surface coating to wire beam electrode under high vacuum environment when method evaluates the uniformity of film, but epoxy resin is super
High vacuum environment when sputtering it is readily volatilized go out organic substance, it is heavy on wire beam electrode that these organic substances can have a strong impact on film
Product quality, makes film-substrate cohesion drastically decline, the rupture or stripping for easily occurring film.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of high temperature resistant wire beam electrode characterized for combined material chip
And preparation method.
The wire beam electrode includes stainless steel bar, high melting point glass and wire, and stainless steel bar is regularly arranged in high melting point glass
In, stainless steel bar is connected with the wire outside high melting point glass.
Wherein, a diameter of 2mm of stainless steel bar, stainless steel bar quantity is no less than 4.
Spacing between stainless steel bar is 2-4mm.
High melting point glass is 900-1100 DEG C by fusing point, and softening temperature forms for 700-800 DEG C of glass powder firing.
Preparing this is used for the method for the high temperature resistant wire beam electrode that combined material chip is characterized, and comprises the following steps：
S1：Graphite jig is designed, the through hole no less than 4 fixed diameters, through hole rule are cut on flaky graphite surface
Arrangement, for fixing stainless steel bar；
S2：In the graphite through hole that stainless steel bar is inserted to well cutting in S1 respectively, glass dust is inserted in two panels graphitized mesophase
End, then will integrally be put into graphite sleeve, graphite sleeve inner surface covers last layer copper foil, is pressed into graphite flake tight with glass dust
Contiguity is touched；
S3：Graphite sleeve is put into water cooling hot pressing furnace and carries out pressure sintering, is forced into after glass softens and is incubated
60min, then cools to the furnace after room temperature and takes out；
S4：Two panels graphite is removed after taking out graphite sleeve, the high melting point glass after stainless steel bar and solidification, observation is left
Pattern ensures the open defect such as stainless steel and glass interface bubble-free crackle；
S5：Every stainless steel bar one end is connected into a wire, wire beam electrode is produced.It can be used for the plating of wire beam electrode surface
The high-flux electric chemical characterization of combined material chip under the uniformity and hot conditions of film measurement film.
The above-mentioned technical proposal of the present invention has the beneficial effect that：
1st, the present invention uses glass as encapsulating material has stability under ultrahigh vacuum, will not be waved in plated film
Hair influence forming thin film quality, can for evaluate film uniformity.
2nd, the present invention uses glass as encapsulating material, and glass has higher fusing point, can complete less than 600 DEG C of heat
Handling process, can be annealed or tempering process after surface coating.
3rd, the chemical property of combined material chip can be characterized in high temperature environments, realize high-flux electric chemistry under high temperature
Characterize.
Brief description of the drawings
Fig. 1 is used for the high temperature resistant wire beam electrode structural representation of combined material chip sign for the present invention's；
Fig. 2 is used for the high temperature resistant wire beam electrode pictorial diagram of combined material chip sign for the present invention's.
Wherein：1- stainless steel bars；2- high melting point glass；3- wires.
Embodiment
To make the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and tool
Body embodiment is described in detail.
The present invention provides a kind of high temperature resistant wire beam electrode characterized for combined material chip and preparation method.
As shown in figure 1, the wire beam electrode includes stainless steel bar 1, high melting point glass 2 and wire 3, the rule row of stainless steel bar 1
It is listed in high melting point glass 2, stainless steel bar 1 is connected with the wire 3 outside high melting point glass 2.
In a particular embodiment, wire beam electrode used is with 4 × 4 regularly arranged to be sealed in height by 16 stainless steel bars 1
Constituted in melting point glass 2, a diameter of 2mm of stainless steel bar 1, the spacing of stainless steel bar 1 is 2-4mm, and the quantity of wire beam electrode can
16-100 roots are made according to experiment demand.
Design graphite jig is used to fix stainless steel bar 1 first, is cut on flaky graphite surface 16 (4 × 4 arrangements)
Ф 2.1mm through hole.Then 16 stainless steel bars 1 are respectively penetrated in two panels graphite through hole, graphite flake is then put into stone
In black sleeve, glass dust (1000 DEG C or so of the fusing point, 750 DEG C of left sides of softening temperature of better heat stability are inserted in graphite sleeve
The right side, powder mesh number is 300 mesh), in order to discharge the air of inside, it is in close contact by mechanical compression to graphite flake and glass dust.
The graphite sleeve made is put into water cooling hot pressing furnace and carries out pressure sintering, is forced into after glass softens and is incubated necessarily
Time, subsequent furnace cooling, to room temperature after take out.Two panels graphite is removed after taking out graphite sleeve, the He of stainless steel bar 1 is only left
High melting point glass 2 after solidification, observation pattern ensures the open defect such as stainless steel bar 1 and glass interface bubble-free crackle, and
Ensure to keep insulation between each stainless steel bar 1 using universal meter measurement, specific pattern is as shown in Figure 2.Before use by every not
Become rusty a piece wire 3 of the one end of rod iron 1 connection, you can is used as wire beam electrode, can be used for the measurement of wire beam electrode surface coating thin
The high-flux electric chemical characterization of combined material chip under the uniformity and hot conditions of film.
Described above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, on the premise of principle of the present invention is not departed from, some improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of high temperature resistant wire beam electrode characterized for combined material chip, it is characterised in that：Including stainless steel bar (1), height
Melting point glass (2) and wire (3), stainless steel bar (1) are regularly arranged in high melting point glass (2), stainless steel bar (1) and high-melting-point
Outside wire (3) connection of glass (2).
2. the high temperature resistant wire beam electrode according to claim 1 characterized for combined material chip, it is characterised in that：It is described
Stainless steel bar (1) a diameter of 2mm, stainless steel bar (1) quantity is no less than 4.
3. the high temperature resistant wire beam electrode according to claim 1 characterized for combined material chip, it is characterised in that：It is described
Spacing between stainless steel bar (1) is 2-4mm.
4. the high temperature resistant wire beam electrode according to claim 1 characterized for combined material chip, it is characterised in that：It is described
High melting point glass (2) is 900-1100 DEG C by fusing point, and softening temperature forms for 700-800 DEG C of glass powder firing.
5. prepare is used for the method for the high temperature resistant wire beam electrode that combined material chip is characterized described in claim 1, its feature exists
In：Comprise the following steps：
S1：Graphite jig is designed, the through hole no less than 4 fixed diameters is cut on flaky graphite surface, through hole is regularly arranged,
For fixing stainless steel bar (1)；
S2：Stainless steel bar (1) is inserted respectively in S1 in the graphite through hole of well cutting, glass dust is inserted in two panels graphitized mesophase
End, then will integrally be put into graphite sleeve, graphite sleeve inner surface covers last layer copper foil, is pressed into graphite flake tight with glass dust
Contiguity is touched；
S3：Graphite sleeve is put into water cooling hot pressing furnace and carries out pressure sintering, is forced into after glass softens and is incubated
60min, then cools to the furnace after room temperature and takes out；
S4：Two panels graphite is removed after taking out graphite sleeve, the high melting point glass (2) after stainless steel bar (1) and solidification is left；
S5：Every stainless steel bar (1) one end is connected into a wire (3), wire produces tow electricity by connector plug connection
Pole.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710560236.4A CN107328833A (en) | 2017-07-11 | 2017-07-11 | The high temperature resistant wire beam electrode and preparation method characterized for combined material chip |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710560236.4A CN107328833A (en) | 2017-07-11 | 2017-07-11 | The high temperature resistant wire beam electrode and preparation method characterized for combined material chip |
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| CN107328833A true CN107328833A (en) | 2017-11-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710560236.4A Pending CN107328833A (en) | 2017-07-11 | 2017-07-11 | The high temperature resistant wire beam electrode and preparation method characterized for combined material chip |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107576696A (en) * | 2017-09-05 | 2018-01-12 | 北京科技大学 | The high temperature resistant wire beam electrode method of preparation and use characterized for combined material chip |
| CN107860707A (en) * | 2017-11-15 | 2018-03-30 | 上海大学 | The heteropical method of aluminum alloy surface microcell galvanic corrosion is characterized using wire beam electrode |
| CN108362748A (en) * | 2018-01-10 | 2018-08-03 | 北京科技大学 | A kind of preparation and application of heat-resisting wire beam electrode |
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| CN85102991A (en) * | 1985-04-01 | 1987-01-17 | 中国科学院新疆物理研究所 | high-temperature thermistor with high reproducibility |
| US6132593A (en) * | 1998-06-08 | 2000-10-17 | Tan; Yong-Jun | Method and apparatus for measuring localized corrosion and other heterogeneous electrochemical processes |
| CN104535253A (en) * | 2015-01-19 | 2015-04-22 | 北京大学 | High temperature pressure sensor and process method thereof |
| CN106769833A (en) * | 2017-01-03 | 2017-05-31 | 北京科技大学 | For the device and method of the high-flux electric chemical characterization of combined material chip |
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2017
- 2017-07-11 CN CN201710560236.4A patent/CN107328833A/en active Pending
Patent Citations (4)
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| CN85102991A (en) * | 1985-04-01 | 1987-01-17 | 中国科学院新疆物理研究所 | high-temperature thermistor with high reproducibility |
| US6132593A (en) * | 1998-06-08 | 2000-10-17 | Tan; Yong-Jun | Method and apparatus for measuring localized corrosion and other heterogeneous electrochemical processes |
| CN104535253A (en) * | 2015-01-19 | 2015-04-22 | 北京大学 | High temperature pressure sensor and process method thereof |
| CN106769833A (en) * | 2017-01-03 | 2017-05-31 | 北京科技大学 | For the device and method of the high-flux electric chemical characterization of combined material chip |
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| 刘圆圆: "液滴下金属表面电化学性质研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107576696A (en) * | 2017-09-05 | 2018-01-12 | 北京科技大学 | The high temperature resistant wire beam electrode method of preparation and use characterized for combined material chip |
| CN107860707A (en) * | 2017-11-15 | 2018-03-30 | 上海大学 | The heteropical method of aluminum alloy surface microcell galvanic corrosion is characterized using wire beam electrode |
| CN108362748A (en) * | 2018-01-10 | 2018-08-03 | 北京科技大学 | A kind of preparation and application of heat-resisting wire beam electrode |
| CN108362748B (en) * | 2018-01-10 | 2020-06-26 | 北京科技大学 | Preparation and application methods of heat-resistant tow electrode |
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