CN107576696A - The high temperature resistant wire beam electrode method of preparation and use characterized for combined material chip - Google Patents
The high temperature resistant wire beam electrode method of preparation and use characterized for combined material chip Download PDFInfo
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- CN107576696A CN107576696A CN201710792651.2A CN201710792651A CN107576696A CN 107576696 A CN107576696 A CN 107576696A CN 201710792651 A CN201710792651 A CN 201710792651A CN 107576696 A CN107576696 A CN 107576696A
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- stainless steel
- high temperature
- temperature resistant
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Abstract
The present invention relates to electrode technology, there is provided a kind of high temperature resistant wire beam electrode characterized for combined material chip, including more stainless steel bars, some wires and wire connector plug；The more stainless steel bars are arranged in parallel, and the more stainless steel bars turn to one by high-melting-point high thermal stability glass pouring sealing；The a diameter of 2mm of stainless steel bar, the spacing between stainless steel bar is 2 4mm；High-melting-point high thermal stability glass melting point is 1000 DEG C or so, 750 DEG C or so of softening temperature.Present invention also offers the method for preparation and use of above-mentioned high temperature resistant wire beam electrode.The present invention uses glass as encapsulating material has stability under ultrahigh vacuum, and volatilization will not occur in plated film influences forming thin film quality, can be used for evaluating the uniformity of film；The chemical property of combined material chip can be characterized in high temperature environments, realize high-flux electric chemical characterization under high temperature.
Description
Technical field
The present invention relates to electrode technology, more particularly to a kind of high temperature resistant wire beam electrode characterized for combined material chip,
Method of preparation and use.
Background technology
Combinatorial material chip approach is in nineteen ninety-five by Lawrence Berkeley laboratory Xiang Xiaodong et al.《Science》
Put forward first, be primarily intended to by once testing simultaneously synthesizing up to 108The material sample of kind, 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 develops relatively slowly, particularly electrochemical field lack always it is a kind of efficiently,
Quick characterization method.At present, high-flux electric chemical field measurement mainly 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.Important survey tool of the wire beam electrode as microcell electrochemistry, has 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 with epoxy resin encapsulation
Solidify, each probe can be as the multiprobe electrode to work independently after independent patch.Wire beam electrode is mainly used in organic coating
Inhomogeneities evaluation and characterize local corrosion situation etc. of metal.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, these organic substances can have a strong impact on that film is heavy on wire beam electrode
Product quality, makes film-substrate cohesion drastically decline, and the rupture or stripping of film easily occurs.
The content of the invention
The purpose of the present invention is exactly overcome the deficiencies in the prior art, there is provided a kind of for the resistance to of combined material chip sign
High temperature wire beam electrode, method of preparation and use, the subsequent heat treatment of film can be realized under high temperature and ultra-high vacuum environment
Technique and the wire beam electrode that combined material chip characterizes is completed, and realize using the electrode high flux of combined material chip
Electrochemical Detection.
A kind of high temperature resistant wire beam electrode characterized for combined material chip of the present invention, including it is more stainless steel bars, some
Root wire and wire connector plug；The more stainless steel bars are arranged in parallel, and the more stainless steel bars pass through Gao Rong
Point high thermal stability glass pouring envelope is fixed as one；The exposed one end of every stainless steel bar is respectively connected with the wire.
Further, a diameter of 2mm of the stainless steel bar, the spacing between the stainless steel bar is 2-4mm.
Further, the high-melting-point high thermal stability glass melting point is 1000 ± 100 DEG C, softening temperature 750 ± 100
℃。
Further, the quantity of the stainless steel bar is 16~100.
Further, described encapsulation is fixed makes stainless steel bar and glass using water cooling hot pressing furnace progress high-temperature pressurizing sintering
Between combine closely, occur without open defect.
A kind of preparation method of the high temperature resistant wire beam electrode characterized for combined material chip of the present invention, including following step
Suddenly：
Step 1：Graphite jig is designed, multiple Ф 2.1mm through hole is cut on flaky graphite surface, for fixing stainless steel
Rod；
Step 2：Stainless steel bar is inserted respectively in two panels graphite through hole, the good glass of heat endurance is inserted in two panels graphitized mesophase
It powder, then will be put into all in graphite sleeve, and be pressed into graphite flake and be in close contact with glass dust；The glass dust fusing point 1000
± 100 DEG C, 750 ± 100 DEG C of softening temperature；
Step 3：Graphite sleeve is put into water cooling hot pressing furnace and carries out pressure sintering, is forced into after glass softens and is incubated one
Fix time, subsequent furnace cooling, to room temperature after take out；
Step 4：Two panels graphite is removed after taking out graphite sleeve, leaves the glass after stainless steel and solidification, observation pattern ensures
The open defect such as stainless steel and glass interface bubble-free crackle；
Step 5, the exposed one end of every stainless steel bar are all connected with a wire, produce the high temperature resistant wire beam electrode.
Further, number of openings described in step 1 is 16, by 4 × 4 arrangements.
A kind of application method of the above-mentioned high temperature resistant wire beam electrode characterized for combined material chip of the present invention, including it is as follows
Step：
Step 1: the high temperature resistant wire beam electrode is put into magnetic control sputtering device, using the method for two target co-sputterings described resistance to
Every stainless steel bar surface of high temperature wire beam electrode deposits the different thin-film material of a composition of layer, and adds mask and cause table
Film is separated from each other everywhere in face, ensures electric insulation；
It is Step 2: sweet as auxiliary electrode, saturation as working electrode, Pt pieces using the high temperature resistant wire beam electrode for being coated with film
Mercury（SCE）As reference electrode, the electricity of glucose current equation scanner each stainless steel bar surface film of quick point-to-point measurement is used
Chemical information, the Electrochemistry Information include current potential and electric current；
Step 3: the current level for the every stainless steel bar that the high temperature resistant wire beam electrode measurement is obtained is distributed and every stainless
The thin film composition of rod iron mutually compares, it is possible to disposably obtains the electrochemistry of the high temperature resistant wire beam electrode surface Multiple components
Information, so as to realize the high-flux electric chemical characterization of combined material chip.
Further, current level scanner described in step 2 is CST520 wire beam electrode glucose current equation scanners.
Beneficial effects of the present invention are：
1st, the present invention uses glass as encapsulating material has stability under ultrahigh vacuum, and the shadow that volatilizees will not occur in plated film
Forming thin film quality is rung, can be used for evaluating the uniformity of film；
2nd, the present invention uses glass as encapsulating material, and glass has higher fusing point, can complete less than 600 DEG C of heat treatment
Technique, 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 inspection under high temperature
Survey；
4th, stainless steel bar（Probe）Number can change according to requirement of experiment, disclosure satisfy that the high flux detection of experimental data, greatly
Width reduces experimental period and experimental cost.
Brief description of the drawings
Fig. 1 show a kind of high temperature resistant wire beam electrode structural representation characterized for combined material chip of the embodiment of the present invention
Figure.
Wherein：1- stainless steel bars, 2- high-melting-point high thermal stability glass；3- wires.
Embodiment
The specific embodiment of the invention is described in detail below in conjunction with specific accompanying drawing.It should be noted that in following embodiments
The combination of the technical characteristic or technical characteristic of description is not construed as isolated, and they can be mutually combined so as to reach
To superior technique effect.In the accompanying drawing of following embodiments, identical label that each accompanying drawing occurs represent identical feature or
Person's part, it can be applied in different embodiments.
As shown in figure 1, a kind of high temperature resistant wire beam electrode characterized for combined material chip of the present invention, including more stainless
Rod iron 1, some wires 3 and wire connector plug；The quantity of stainless steel bar 1 is 16-100 roots, the more stainless steels
Rod 1 is arranged in parallel, the more stainless steel bars 1 by the encapsulation of high-melting-point high thermal stability glass 2 solidification is integrated, it is described not
Become rusty 1 a diameter of 2mm of rod iron or so, and the spacing between the stainless steel bar 1 is 2-4mm, the high-melting-point high thermal stability glass 3
Fusing point is 1000 ± 100 DEG C, 750 ± 100 DEG C of softening temperature.
High temperature resistant wire beam electrode of the present invention can be made by following steps：
Step 1：Graphite jig is designed first, is cut on flaky graphite surface multiple（Such as 16,4 × 4 arrangements）Ф
2.1mm through hole, for fixing stainless steel bar（Probe）；
Step 2：By stainless steel bar（Probe）Respectively insert two panels graphite through hole in, two panels graphitized mesophase insert heat endurance compared with
Good glass dust（1000 DEG C or so of fusing point, 750 DEG C or so of softening temperature）, then will be put into graphite sleeve, press all over
It is in close contact to graphite flake and glass dust；
Step 3：Graphite sleeve is put into water cooling hot pressing furnace and carries out pressure sintering, is forced into after glass softens and is incubated one
Fix time, subsequent furnace cooling, to room temperature after take out；
Step 4：Two panels graphite is removed after taking out graphite sleeve, leaves the glass after stainless steel and solidification, observation pattern ensures
The open defect such as stainless steel and glass interface bubble-free crackle.
Every probe one end is connected into a wire during use, you can used as wire beam electrode, can be used for tow electricity
The high-flux electric chemical characterization of combined material chip under the uniformity and hot conditions of pole surface coating measurement film.
The application method of high temperature resistant wire beam electrode of the present invention is as follows：
Step 1: the high temperature resistant wire beam electrode is put into magnetic control sputtering device, using the method for two target co-sputterings described resistance to
Every stainless steel bar surface of high temperature wire beam electrode deposits the different thin-film material of a composition of layer, and adds mask and cause table
Film is separated from each other everywhere in face, ensures electric insulation；
It is Step 2: sweet as auxiliary electrode, saturation as working electrode, Pt pieces using the high temperature resistant wire beam electrode for being coated with film
Mercury（SCE）As reference electrode, CST520 wire beam electrode glucose current equation scanners each stainless steel of quick point-to-point measurement is used
The Electrochemistry Information of rod surface film, the Electrochemistry Information include current potential and electric current；
Step 3: the current level for the every stainless steel bar that the high temperature resistant wire beam electrode measurement is obtained is distributed and every stainless
The thin film composition of rod iron mutually compares, it is possible to disposably obtains the electrochemistry of the high temperature resistant wire beam electrode surface Multiple components
Information, so as to realize the high-flux electric chemical characterization of combined material chip.
Although having been presented for several embodiments of the present invention herein, it will be appreciated by those of skill in the art that
Without departing from the spirit of the invention, the embodiments herein can be changed.Above-described embodiment be it is exemplary, no
Restriction that should be using the embodiments herein as interest field of the present invention.
Claims (9)
1. it is a kind of for combined material chip characterize high temperature resistant wire beam electrode, it is characterised in that if including more stainless steel bars,
Dry root wire and wire connector plug；The more stainless steel bars are arranged in parallel, and the more stainless steel bars pass through height
Fusing point high thermal stability glass pouring envelope is fixed as one；The exposed one end of every stainless steel bar is respectively connected with the wire.
2. as claimed in claim 1 for combined material chip characterize high temperature resistant wire beam electrode, it is characterised in that it is described not
Become rusty a diameter of 2mm of rod iron, and the spacing between the stainless steel bar is 2-4mm.
3. the high temperature resistant wire beam electrode characterized as claimed in claim 1 for combined material chip, it is characterised in that the height
Fusing point high thermal stability glass melting point is 1000 ± 100 DEG C, 750 ± 100 DEG C of softening temperature.
4. the high temperature resistant wire beam electrode for being used for combined material chip and characterizing as described in claim any one of 1-3, its feature exist
In the quantity of the stainless steel bar is 16~100.
5. the high temperature resistant wire beam electrode for being used for combined material chip and characterizing as described in claim any one of 1-3, its feature exist
In, described encapsulation is fixed to be made to combine closely between stainless steel bar and glass using water cooling hot pressing furnace progress high-temperature pressurizing sintering,
Occur without open defect.
6. a kind of preparation method of the high temperature resistant wire beam electrode characterized for combined material chip, it is characterised in that including as follows
Step：
Step 1：Graphite jig is designed, multiple Ф 2.1mm through hole is cut on flaky graphite surface, for fixing stainless steel
Rod；
Step 2：Stainless steel bar is inserted respectively in two panels graphite through hole, the good glass of heat endurance is inserted in two panels graphitized mesophase
It powder, then will be put into all in graphite sleeve, and be pressed into graphite flake and be in close contact with glass dust；The glass dust fusing point 1000
± 100 DEG C, 750 ± 100 DEG C of softening temperature；
Step 3：Graphite sleeve is put into water cooling hot pressing furnace and carries out pressure sintering, is forced into after glass softens and is incubated one
Fix time, subsequent furnace cooling, to room temperature after take out；
Step 4：Two panels graphite is removed after taking out graphite sleeve, leaves the glass after stainless steel and solidification, observation pattern ensures
Stainless steel and glass interface bubble-free crackle open defect；
Step 5, the exposed one end of every stainless steel bar are all connected with a wire, produce the high temperature resistant wire beam electrode.
7. the preparation method of the high temperature resistant wire beam electrode characterized as claimed in claim 6 for combined material chip, its feature
It is, number of openings described in step 1 is 16, by 4 × 4 arrangements.
A kind of 8. user for being used for the high temperature resistant wire beam electrode that combined material chip characterizes as described in claim any one of 1-4
Method, it is characterised in that comprise the following steps：
Step 1: the high temperature resistant wire beam electrode is put into magnetic control sputtering device, using the method for two target co-sputterings described resistance to
Every stainless steel bar surface of high temperature wire beam electrode deposits the different thin-film material of a composition of layer, and adds mask and cause table
Film is separated from each other everywhere in face, ensures electric insulation；
It is Step 2: sweet as auxiliary electrode, saturation as working electrode, Pt pieces using the high temperature resistant wire beam electrode for being coated with film
Mercury（SCE）As reference electrode, the electricity of glucose current equation scanner each stainless steel bar surface film of quick point-to-point measurement is used
Chemical information, the Electrochemistry Information include current potential and electric current；
Step 3: the current level for the every stainless steel bar that the high temperature resistant wire beam electrode measurement is obtained is distributed and every stainless
The thin film composition of rod iron mutually compares, it is possible to disposably obtains the electrochemistry of the high temperature resistant wire beam electrode surface Multiple components
Information, so as to realize the high-flux electric chemical characterization of combined material chip.
9. the application method of the high temperature resistant wire beam electrode characterized as claimed in claim 8 for combined material chip, its feature exist
In current level scanner described in step 2 is CST520 wire beam electrode glucose current equation scanners.
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| CN201710792651.2A CN107576696B (en) | 2017-09-05 | 2017-09-05 | Preparation and use methods of high-temperature-resistant tow electrode for combined material chip characterization |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109632623A (en) * | 2018-12-14 | 2019-04-16 | 青岛理工大学 | CNT component film is modified steel wire array electrode, preparation method and applications |
| CN113916769A (en) * | 2021-10-26 | 2022-01-11 | 西南石油大学 | High-temperature and high-pressure resistant tow electrode and preparation method thereof |
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| 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 |
| CN107328833A (en) * | 2017-07-11 | 2017-11-07 | 北京科技大学 | The high temperature resistant wire beam electrode and preparation method characterized for combined material chip |
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| 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109632623A (en) * | 2018-12-14 | 2019-04-16 | 青岛理工大学 | CNT component film is modified steel wire array electrode, preparation method and applications |
| CN109632623B (en) * | 2018-12-14 | 2021-05-11 | 青岛理工大学 | CNT (carbon nanotube) assembled film modified steel wire array electrode as well as preparation method and application thereof |
| CN113916769A (en) * | 2021-10-26 | 2022-01-11 | 西南石油大学 | High-temperature and high-pressure resistant tow electrode and preparation method thereof |
| 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 |
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