CN105445353B - A kind of electrochemistry material chip - Google Patents

A kind of electrochemistry material chip Download PDF

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Publication number
CN105445353B
CN105445353B CN201410816018.9A CN201410816018A CN105445353B CN 105445353 B CN105445353 B CN 105445353B CN 201410816018 A CN201410816018 A CN 201410816018A CN 105445353 B CN105445353 B CN 105445353B
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sample
substrate
current collector
electrochemistry
material chip
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CN105445353A (en
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张晓琨
张海涛
向勇
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Ningbo Xinghe Material Technology Co., Ltd.
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INFINITE MATERIALS TECHNOLOGY Co Ltd
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Abstract

The present invention relates to Experiment of Material Science technical fields, more particularly to a kind of electrochemistry material chip, by integrating sample area array in a substrate, and current collector and sample to be tested are provided in the region, and being electrically connected for current collector and golden finger is realized by a contact conductor, and then realize each sample independently pass through current collector, contact conductor, golden finger interface and an outside electrochemical test form current path, and carry out subsequent chemical property analysis, and the efficiency of electrochemical property test can be greatly improved and fully meet the requirement of high-throughput electrochemical property test.

Description

A kind of electrochemistry material chip
Technical field
The present invention relates to Experiment of Material Science technical field more particularly to a kind of electrochemistry material chips.
Background technology
Combinatorial material chip approach [" A Combinatorial since last century, the mid-90 was by invention Approach to Materials Discovery " X.-D.Xiang, Xiaodong Sun, Gabriel Briceno, Yulin Lou, Kai-An Wang, Hauyee Chang, William Gregory Wallace-Freedman, Sung-Wei Chen, Peter G.Schultz, Science268,1738 (1995)], material science research field obtain it is extensive and huge at Work(.Researchers develop numerous high-throughput experimental study tools for various functions material, structural material [Combinatorial Approaches as Effective Tools in the Study of Phase Diagrams And Composition-structure-property Relationships, Ji-Cheng Zhao, Prog.Mater.Sci.51,557 (2006)].However, being directed to the high-throughput experimental technique of functional material chemical property at present Development more lag.For the high pass quantity research of a certain military service performance of material, it is often based on through high-throughput combined material The combined material chip sample expansion that preparation means obtain, therefore, it is intended to develop the high pass for functional material chemical property Experimental technique is measured, the combined material chip for Electrochemical Properties should be developed first.Existing combinatorial material chip approach, It is such as directed to the combined material chip of fluorescent material, dielectric material, structural material, only need to realize a large amount of samples in smaller area It is integrated, then visited by external probe, such as microcell Fluorescence spectrum probe, near-field microwave scanning probe microscopy, nano impress microcell Needle etc., you can complete the high-throughput experimental study for its a certain feature.However, the most of feelings of the electrochemical property test of material Structure electrochemical device or half device of electrochemistry are needed under condition, by collecting, understanding at the current collector contacted with material sample Signal can be realized.The combinatorial material chip approach of early stage is not related to including the device or half device configuration of electrode structure substantially, Therefore high-throughput Electrochemical Properties be cannot achieve.Some of recent new development are directed to the group of semi-conducting material high flux screening Condensation material chip technology [" High Throughput Combinatorial Screening of Semiconductor Materials " Samuel S.Mao, Appl.Phys.A105,283 (2011)], although introducing device or half device architecture, But due to lacking the targeted design for electrochemical property test, it is also difficult to fully meet high-throughput electrochemical property test It is required that.
Invention content
In view of the above problems, the present invention provides a kind of electrochemistry material chip, to solve high-throughput material electrochemical Characteristic test is lack of pertinence the defect of design.
Technical solution is used by the present invention solves above-mentioned technical problem:
A kind of electrochemistry material chip, including:
Substrate;
Several sample areas are integrated in the upper surface of substrate and are in array distribution, are provided in each sample area Current collector, and cover the sample of the current collector upper surface;
Interface is located at the side of the substrate;
Non-touching several contact conductors, the contact conductor are set to the upper surface of the substrate and interface, realize Each current collector is electrically connected with the interface;
Wherein, at least with the different sample of two kinds of material compositions or structure in the substrate.
Preferably, above-mentioned electrochemistry material chip, wherein be additionally provided between the current collector and the sample One barrier layer.
Preferably, above-mentioned electrochemistry material chip, wherein the material on barrier layer is one kind in Ti-N, Ti, Ta Or multiple combinations.
Preferably, above-mentioned electrochemistry material chip, wherein the interface is golden finger interface.
Preferably, above-mentioned electrochemistry material chip, wherein the thickness of the substrate is less than 5mm, the adjacent sample Spacing between product is more than 1mm.
Preferably, above-mentioned electrochemistry material chip, wherein the material of the substrate is low thermal conductivity solid material Material.
Preferably, above-mentioned electrochemistry material chip, wherein the array of the sample area is m rows × n row,
M and n is positive integer.
Preferably, above-mentioned electrochemistry material chip, wherein the material of the current collector and the contact conductor For metal.
Preferably, above-mentioned electrochemistry material chip, wherein further include a thermocouple;The thermocouple is set to institute Lower surface or the sample upper surface for stating substrate, to monitor the temperature of the sample.
Preferably, above-mentioned electrochemistry material chip, wherein the thermocouple is set to the substrate, sample or collection Galvanic electricity extremely in, to monitor the temperature of the sample.
Above-mentioned technical proposal has the following advantages that or advantageous effect:
1, can be that the research of high-throughput material electrochemical performance carries the invention discloses a kind of electrochemistry material chip For sample basis, in the integrated preparation and Electrochemical Properties of realizing a large amount of samples in the substrate compared with small area, and according to grinding Study carefully demand, in combined material chip the density of sample preparation can flexibility adjustment, Efficiency can be improved to several orders of magnitude.
2, the invention discloses a kind of electrochemistry material chip, wherein each sample passing through independently collects galvanic electricity Pole, contact conductor, golden finger interface and an outside electrochemical test form current path, can pass through an electric signal scanning side Formula realizes high-throughput electrochemical property test, and compared with common probe scanning mode, which mechanism is simple, and testing efficiency is more It is high.
3, for having the test of the high pass quantity research of discrete thermodynamic condition requirement, electrochemistry material disclosed by the invention Chip is by selecting base material appropriate and underlying structure, cooperation microcell heating tool that sample room thermal insulation substantially may be implemented State.
Specific description of the drawings
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, the present invention and its feature, outer Shape and advantage will become more apparent.Identical label indicates identical part in whole attached drawings, while can also not press Attached drawing is drawn according to ratio, focuses on the purport for showing the present invention.
Fig. 1 is the vertical view of electrochemistry material chip in the present invention;
Fig. 2 is the partial side view of electrochemistry material chip in the present invention.
Specific implementation mode
Core of the invention thought is:Sample area array is integrated in a substrate, and is provided with afflux in the region Electrode and sample to be tested, and being electrically connected for current collector and golden finger is realized by a contact conductor, and then realize various kinds Product independently to form electric current by current collector, contact conductor, golden finger interface and an outside electro-chemical test instrument logical Road, and carry out subsequent test technology.
The present invention is further illustrated with specific embodiment below in conjunction with the accompanying drawings, but not as the limit of the present invention It is fixed.
To solve the defect that high-throughput material electrochemical characteristic test is lack of pertinence design, the invention discloses a kind of electricity Chemical combination material chip, as depicted in figs. 1 and 2.
Fig. 1 is the vertical view of electrochemistry material chip, and wherein the electrochemistry material chip includes for a group The substrate 1 of condensation material chip, the substrate 1 provide space and the mechanical support of preparation for sample;It is integrated in the upper surface of the substrate It is in m rows × n array column distributions to have several uniform sample areas 2, several sample areas 2, and wherein m, n is positive integer.
In an embodiment of the present invention, as shown in Fig. 2, the electrochemistry material chip further includes having several current collectors 22, each current collector 22 is set in above-mentioned each sample region 2, and is located at 1 upper surface of substrate;Each current collector 22 is upper simultaneously Surface is also covered with a sample 21, which is electrically connected with current collector 22, it is preferred that 21 size of each sample be 0.5cm × 0.5cm, and the spacing between the neighboring samples 21 of arbitrary a line and/or any one row is more than 1mm, preferably 0.5cm.
In an embodiment of the present invention, the substrate 1 be the size of a rectangle structure and the substrate 1 be 22.5cm × 7.5cm and the thickness of substrate 1 are less than 5mm, as a preferred embodiment, the size of the substrate 1 be 22.5cm × 7.5cm × 500um.1 surface of substrate is further prepared with the rectangular-shaped sample array that 6 rows × 20 arrange (partial array is only shown in figure), amounts to The size of the sample 21 of 120 kinds of material compositions or structure, the current collector 22 is preferably identical as the size of sample 21.
Positioned at the one side of the substrate 1 it is also integrated with golden finger interface 3, is connect with outside electro-chemical test instrument with realizing Mouth interconnection, several non-touching contact conductors 4 are additionally provided in the upper surface of the golden finger interface 3 and substrate 1, each to realize Current collector 22 is electrically connected with golden finger interface 3, because the presence of current collector 22 and contact conductor 4 makes in electro-chemical test The test signal that sample 21 generates is transmitted to the external electro-chemical test instrument being connect with golden finger interface 3 and carries out chemical property Analysis can flexibly select parallel signal acquisition pattern or channel according to the actual conditions of external electro-chemical test instrument certainly Scan pattern, such as:When the sample number matches on external electro-chemical test instrument channel and electrochemistry material chip Parallel signal acquisition pattern can be used, or scan channel pattern can be used based on single pass electro-chemical test instrument.
In addition, due on combined material chip 21 density of sample it is higher, the line width and wiring pattern of contact conductor 4 need root Be designed according to specific experiment demand, it is preferred that the line width of each contact conductor 4 be 0.3mm, and between adjacent electrode lead 4 between Away from for 0.5mm.And in the research of actual combined material, the preparation of each sample 21 may need different thermodynamic conditions, Thermodynamic condition variable is main research object in some cases.Therefore, ideally various kinds on combined material chip It should thermal insulation between product 21.Existing scientific and technological level, it is difficult to realize thermal insulation in combined material chip as described in the present invention. Therefore, when needing the thermodynamic condition of each sample preparation in stringent differentiation electrochemistry material chip, following 3 can be passed through Approach approaches thermal insulation state as far as possible:1) thermal output area and the area matched heat source of sample 21 are used so that heating mesh Other samples outside standard specimen product can only obtain heat by the heat transfer in chip plane;2) base of electrochemistry material chip Bottom 1 selects the alap material of thermal coefficient to make;3) due in combined material sample preparation, providing sample 21 chemical anti- Answer, mass transfer diffusion or crystallization needed for energy effective heat transfer process be mostly along perpendicular to the direction of combined material chip plane into Row, therefore in the preparation of electrochemistry material chip, 21 thickness of substrate 1 and sample is thinned as far as possible so that heat is in group The path length for being transferred to another sample in condensation material chip plane by a sample is much larger than chip thickness, reduces electrochemistry group Condensation material chip thickness also further increases the thermal resistance in chip plane, is conducive to material sample and obtains institute within a short period of time Calorific requirement, i.e. cut-off heat source, heat not yet propagate at other samples at this time.But as a preferred embodiment, this hair For the CMS (Ca of Choice of substrate materials low thermal conductivity in bright0.5Mg0.25Sr0.25Zr4(PO4)6) ceramics be used as main material, It can select other low thermal conductivity solid materials such as ceramic material, fibrous material, plastic material and inorganic non-metallic material Deng.
In an embodiment of the present invention, the material of current collector 22 and contact conductor 4 is metal, preferably metal molybdenum, To ensure the stability of electrode material during the heat treatment of sample 21, characterization test and Reusability.Certainly other meet electricity Metal (such as aluminium, copper or gold), the alloy of the requirement of chemical characteristic research can also be used for afflux in electrochemistry material chip The material of electrode 22.
As shown in Figure 2 is the partial side view of electrochemistry material chip in the present invention, wherein each sample 21 is logical Current collector 22, contact conductor 4 and golden finger interface 3 are crossed, separately forming circuit with external electro-chemical test instrument connects It is logical, it can be achieved that non-interfering electric signal sweep test, while to prevent pollution of the current collector 22 to sample 21, in sample and Also there is the barrier layer (not shown) of a suitable thickness, which is chosen as in Ti-N, Ti, Ta between current collector One or more combinations and the lower material of other diffusion coefficients, and according to the demand of actual experiment, in combined material chip Substrate or sample upper surface arrange thermocouple (not shown) to monitor the temperature of sample, can also be prepared in chip Thermocouple is embedded in substrate 1, sample 21, current collector 22 or above-mentioned barrier layer in journey.
For above-mentioned sample 21, high Throughput Preparation appropriate can be used and be deposited in sample area 2, be preferably based on The physical vapour deposition (PVD) of discrete template can targetedly develop the better high pass of using effect according to the different characteristics of material certainly Measure technology of preparing, while electrochemistry material chip of the present invention, size, the shape of the sample area of array distribution And arrangement mode (such as annular array and other array ways), area, thickness, shape and the material therefor of substrate 1, sample 21 area, thickness, shape and density, area, thickness, shape, density and the material therefor of current collector, contact conductor 4 The concrete form of line width and wiring pattern, golden finger interface 3 should all be according to the feature of specific high-flux electric chemical research activity Targetedly adjusted design is carried out, and to the present invention without materially affect, it is same in practical applications to adapt to.
In conclusion a kind of electrochemistry material chip disclosed by the invention, by integrating sample area in a substrate Domain array, and current collector and sample to be tested are set in the region, and current collector and gold are realized by a contact conductor The electrical connection of finger, so realize each sample independently by current collector, contact conductor, golden finger interface and one outside Electrochemical test forms current path, and carries out subsequent test technology, has the advantages that simultaneously:
1, sample basis can be provided for the research of high-throughput material electrochemical performance, it is big in being realized in the substrate compared with small area Integrated preparation and the Electrochemical Properties of sample are measured, and according to Research Requirements, the density of sample preparation in combined material chip Can flexibility adjustment, Efficiency can be improved to several orders of magnitude.
2, each sample independently pass through current collector, contact conductor, golden finger interface and an outside electro-chemical test Instrument forms current path, high-throughput electrochemical property test can be realized by an electric signal scan mode, with common probe Scan mode is compared, and which mechanism is simple, testing efficiency higher.
3, for having the test of the high pass quantity research of discrete thermodynamic condition requirement, electrochemistry material disclosed by the invention Chip is by selecting base material appropriate and underlying structure, cooperation microcell heating tool that sample room thermal insulation substantially may be implemented State.
It should be appreciated by those skilled in the art that those skilled in the art are combining the prior art and above-described embodiment can be with Realize the change case, this will not be repeated here.Such change case does not affect the essence of the present invention, not superfluous herein It states.
Presently preferred embodiments of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned Particular implementation, wherein the equipment and structure be not described in detail to the greatest extent are construed as giving reality with the common mode in this field It applies;Any technical person familiar with the field, without departing from the scope of the technical proposal of the invention, all using the disclosure above Methods and technical content many possible changes and modifications are made to technical solution of the present invention, or be revised as equivalent variations etc. Embodiment is imitated, this is not affected the essence of the present invention.Therefore, every content without departing from technical solution of the present invention, foundation The technical spirit any simple modifications, equivalents, and modifications made to the above embodiment of the present invention, still fall within the present invention In the range of technical solution protection.

Claims (8)

1. a kind of electrochemistry material chip, which is characterized in that including:
The material of substrate, the substrate is low thermal conductivity solid material;
Several sample areas are integrated in the upper surface of substrate and are in array distribution, afflux is provided in each sample area Electrode, and cover the sample of the current collector upper surface;
Interface is located at the side of the substrate;
Non-touching several contact conductors, the contact conductor are set to the upper surface of the substrate and interface, realize each institute State being electrically connected for current collector and the interface;
Wherein, at least with the different sample of two kinds of material compositions or structure in the substrate;
Wherein, the thickness of the substrate is less than 5mm, and the spacing of the adjacent sample room is 0.5cm;
Wherein, it is to be heated with the matched microcell heating tool of sample area using output area to the mode of heating of sample;
The sample being formed by the current collector, contact conductor, interface and an outside electrochemical test independently Current path.
2. electrochemistry material chip as described in claim 1, which is characterized in that the current collector and the sample it Between be additionally provided with a barrier layer.
3. electrochemistry material chip as claimed in claim 2, which is characterized in that the material on the barrier layer be Ti-N, One or more combinations in Ti, Ta.
4. electrochemistry material chip as described in claim 1, which is characterized in that the interface is golden finger interface.
5. electrochemistry material chip as described in claim 1, which is characterized in that the array of the sample area is m rows × n is arranged,
M and n is positive integer.
6. electrochemistry material chip as described in claim 1, which is characterized in that the current collector and the electrode draw The material of line is metal.
7. electrochemistry material chip as described in claim 1, which is characterized in that further include a thermocouple;
The thermocouple is set to lower surface or the sample upper surface of the substrate, to monitor the temperature of the sample.
8. electrochemistry material chip as described in claim 1, which is characterized in that further include a thermocouple;
The thermocouple is set in the substrate, sample or current collector, to monitor the temperature of the sample.
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CN106483469B (en) * 2016-09-30 2020-09-01 成都亦道科技合伙企业(有限合伙) Device for improving battery test flux
CN107478694B (en) * 2017-07-24 2023-05-30 南昌大学 High-flux testing platform for lithium battery material
CN110161401A (en) * 2019-06-05 2019-08-23 中国科学院理化技术研究所 A kind of superconduction chip low temperature test device
CN110335982B (en) * 2019-07-28 2021-04-27 电子科技大学 Micro-nano integrated solid film lithium battery and preparation method thereof
CN110646468B (en) * 2019-09-29 2022-02-11 天津职业技术师范大学(中国职业培训指导教师进修中心) Method for characterizing high-throughput materials

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Address before: 315000 No. 1299 Juxian Road, Ningbo High-tech Zone, Zhejiang Province

Patentee before: INFINITE MATERIALS TECHNOLOGY CO., LTD.