CN1228534A - Electrical measurement method for measuring conducting material structure - Google Patents
Electrical measurement method for measuring conducting material structure Download PDFInfo
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- CN1228534A CN1228534A CN 98126142 CN98126142A CN1228534A CN 1228534 A CN1228534 A CN 1228534A CN 98126142 CN98126142 CN 98126142 CN 98126142 A CN98126142 A CN 98126142A CN 1228534 A CN1228534 A CN 1228534A
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Abstract
The on-line in-situ and synchronous electric testing method for testing the structure and property of conductive material is characterized by that according to the structure of material sample, selecting proper method to make electrode on the sample, said electrode can be surface electrode, also can be end electrode, even can be two-side point electrode or non-symmetrical one-side surface electrode and another-side point electrode, and both electrodes are respectively equipped with a fine conductive wire whose exterior is covered with insulating layer, and said fine conductive wire is connected with resistance measuring instrument so as to make on-line in-situ and synchronous measurement of resistance of the material in the course of mechanical test and various analysis of the material, and can indirectly know the change of said material structure.
Description
The present invention relates to the electrical testing method of a kind of online, original position and synchronism detection conducting material structure and performance.It is applicable to the material system with certain conductive capability, as contains stupalith of the polymer matrix composites of carbon fiber, the macromolecular material that contains electroconductive stuffing and conduction etc.
At present, conductive material is being carried out the quasi-static test of mechanics (as tension test, compression test, bending test), the dynamic test of mechanics is (as torture test, impulse test), the envelope test of mechanics is (as creep test, stress relaxation test) and the thermometric analysis of material, in the time of thermogravimetic analysis (TGA) etc., can only provide the mechanical property and the thermal parameter of the material of measuring and monitoring the growth of standing timber, and can not synchronously obtain for the variation of the resistance value of the conductive capability of display material sensitively, because test can not be online, original position, synchronously carry out, both can not carry out under identical environment and load-up condition same sample, this has just caused test error to test.
The objective of the invention is, in the test of the mechanics of materials or thermal property, online, the original position and the resistance of testing conductive material are synchronously understood the variation of material structure indirectly.
Technical solution of the present invention is, according to the inner conductive structure of measured material, does electrode with electrically-conducting paint method or electrochemical plating or physics thin-layer method or Mechanical Method etc. on the sample of measured material, forms conductive channel between two electrodes; After electrode completes,, connect resistance test set, the resistance value of testing conductive material in the thermoanalytical process of MATERIALS ' DYNAMIC machinery with respectively connecting the thin wire silk of an outer insulating layer coating on two electrodes; Electrode can be that the face electrode also can be a termination electrode, even can to adopt two-sided point electrode or asymmetric one side be point electrode for face electrode another side; The method of doing electrode is, wherein the electrically-conducting paint method is in suitably degreasing or the slight polishing of the surface of need loading electrode, directly is coated with the silver slurry then, and on the surface of silver slurry coating, directly electrical lead in the soldering also can be stained with electrical lead with silver-colored the slurry again; The method of machinery loading electrode is copper mesh, particularly zinc-plated copper mesh hot pressing to be advanced to treat the superficial layer of loading electrode, electrical lead in copper mesh or the online soldering of tin-coated copper again; The method of bonding loading electrode is to treat the loading electrode surface earlier to carry out degreasing and grinding process, then metal film is stained with the cementing agent that contains silver powder, electrical lead in the soldering of metal film outside surface again, the cementing agent that contains silver powder must highly conduct electricity, and can be various suitable tackifier such as epoxy resin, polyurethane.
Advantage of the present invention is, in the measuring process of any one structure and performance, online, original position and the variation of synchronously measuring the resistance value of this material, thereby outside original test event, recognize the fresh information of the structure or the performance change of material extraly, the measurement of this structure or performance had both comprised the quasi-static test such as the tension test of mechanics, compression test, bending test etc., also comprise the dynamic test such as the torture test of mechanics, impulse test etc., the envelope test such as the creep test that also comprise mechanics, stress relaxation tests etc. the particularly important is, the present invention can also be used for the structure under the different temperatures and the analysis of performance, for example analyze in the process of (DMA) in MATERIALS ' DYNAMIC machinery heat, online, original position and the variation of synchronously measuring the material resistance value.By suitable demarcation, the present invention even be used in when material carried out thermometric analysis (DSC), thermogravimetic analysis (TGA) (TG) etc., online, original position and measuring resistance synchronously.The present invention has not only expanded quasistatic, the static state of material mechanical performance, the test specification of dynamic test, has also expanded the test function and the scope of commercial instrument such as dynamic mechanical analysis, thermometric analysis and thermogravimetic analysis (TGA).
Fig. 1 is online, original position, the synchro measure result of the E ＇-tan δ of conductive filler filled polyethylene face electrode of the present invention-R-T relation;
There is three-point bending load in Fig. 2 and is not having online, original position, synchro measure result and the comparison thereof of the R-T relation under the three-point bending loading condiction for conductive filler filled polyethylene face electrode of the present invention;
Online, the original position of E ＇-tan δ-R-T relation of high-performance thermosetting polymer matrix composites (end electrode) sample that Fig. 3 strengthens for unidirectional carbon fiber dimension, synchro measure result;
Online, the original position of E ＇-tan δ-R-T relation of high-performance thermosetting polymer matrix composites (face electrode) sample that Fig. 4 strengthens for unidirectional carbon fiber dimension, synchro measure result;
Fig. 5 is a resistance measurement synoptic diagram under the non axial pressure;
Fig. 6 is the relaxation curve of high density polyethylene/graphite (63.5/37.5) compound substance (face electrode) in different pressures lower volume resistivity.
The preparation of sample and test:
1. specimen preparation: according to the requirement of three-point bending loading mode in the dynamic mechanical analysis,
Sheet material is cut into dumbbell shaped, rectangle or foursquare sample, notice that the sample outward appearance is intact
Good, no significant defect.
2. electrode preparation (being example only) with electrically-conducting paint method and rectangular specimen: at rectangular specimen
Two surfaces (long * wide) or axial two end faces (high * wide) up and down, or horizontal
To two end faces (length * height) respectively plate one deck silver slurry or be coated with the last layer conductive gelatin,
After treating the coating complete stability, respectively connect carefully leading of an outer insulating layer coating with conductive liquid
Silk connects resistance test set, and having measured an initial resistivity value is normal condition.
3. resistance measurement: the requirement according to the dynamic mechanical analysis test will be connected to the examination of lead
Sample is put on the support of dynamic mechanical analysis instrument stove, and two leads are drawn, and connects
To a resistance test set, notice that total can not short circuit, also attention simultaneously
This sample and conductor mounting thereof do not influence the proper testing of DMA.
4. open the DMA instrument, record sample resistance under vibrational loading and programed temperature
The variation of value will record resistance change and be depicted as resistance value with temperature, time or its
The spectrogram that dependent variable changes.
The example of test findings:
The polythene material (face electrode) that example 1, conductive filler are filled: according to above experimental procedure, the spectrogram of the material resistance-temperature that obtains such as Fig. 1.Can find that between 40 ℃ to 130 ℃, resistance slightly descends, illustrate in temperature to reach under the volumetric expansion effect that causes thus, and under the three-point bending load at the same time, the conductive network of material internal trend is fine and close or perfect; In the time of＞130 ℃, fusion takes place in matrix material (tygon), causes paroxysmal big expansion and phase transformation, and at this moment, rapid increase also takes place resistance signal, produces the electric switch effect.The lax peak that this changes material corresponding increase suddenly and the die-offing of storage modulus after, when this material production electric switch effect was described, material itself had lost the support structure performance, will destroy under very little external force effect.The electric switch sex reversal speed that can find material from Fig. 2 is bigger, and the autohemagglutination of conducting particles motion aggravation in the material system is described under the perturbation action in this vibration field of force is used.
The high-performance thermosetting polymer matrix composites (end electrode) that example 2, unidirectional carbon fiber dimension strengthen: specimen preparation and method of testing are the same, the spectrogram of acquisition such as Fig. 3.Under the acting in conjunction of temperature and three-point bending load, material along fiber axis to resistance reduce earlier, may come from interfibrous contact point increases, explanation is when the material macro property is also very stable, oneself changes on the microstructure yardstick, and the mechanism that resistance subsequently increases is not quite clear, but its peak value exactly appears at before the relaxation, the great change of having predicted material property is about to take place, and this point has very important practical significance.
The high-performance thermosetting polymer matrix composites (face electrode) that example 3, unidirectional carbon fiber dimension strengthen: specimen preparation and method of testing are the same, the spectrogram of acquisition such as Fig. 4.The temperature variant mechanism of resistance that before 130 ℃, takes place and 2 similar, illustrate that the three-point bending pressurization causes interfibrous contact point to increase, its reason is that temperature and pressure makes resin deliquescing between fiber, easily deformable, the subtle change on this physical dimension is that all mechanical means are difficult to measure.Near the material matrix transition temperature time, interface resistance descends significantly, illustrates to contact between fiber at this moment to increase considerably.This signal also has a kind of advance notice character.
The quasistatic compression (face electrode) of example 4, dag filled polyethylene material:
(1), to get volume content be the tygon that 37.5% dag is filled, and is molded into any rectangle.Before mold pressing, on the power-on and power-off pole-face, place zinc-plated copper mesh simultaneously, and go into sample, 130 ± 5 ℃ of hot pressing conditions, 10 minutes with sample making course hot pressing;
(2), advance on the two sides copper mesh of specimen surface, copper conductor is drawn in each soldering in hot pressing
The utmost point;
(3), sample is loaded onto the material test specimen holder, carry out compression test by the mode of Fig. 5, simultaneously original position, online, synchronously measure the resistance variations of compression process;
(4), compression test can be carried out with reference to any standard;
(5), the result: stepped boosting as Fig. 6, find that the resistance of material changes thereupon, pressure is big more, resistivity is low more, demonstrates strict corresponding relationship between the variation of material compression deformation and resistivity of material.Secondly, pressurize on a certain pressure platform, the resistivity of finding material takes place over time, the non-constant of its pace of change, both resistivity reduced first quick and back slow, finally be tending towards an equilibrium value, be very similar to the mechanics creep process and the stress relaxation process of material, this method also demonstrates the quantitative sign ability to this time dependent process.
In like manner, to tension test and bending test, this method also has similar sign ability, and its data also have similar rule with compression test.
LogE ＇ is meant the logarithm value of the elastic energy that material stores among the figure in a deformation period; Tan δ is meant the ratio of loss modulus and storage modulus.
Claims (6)
1. the electrical testing method of a testing conductive material structure is characterized in that, utilizes electrically-conducting paint method or electrochemical plating or physics thin-layer method or mechanical loading electrode method to do electrode on sample, makes between two electrodes and forms conductive channel; With respectively connecting the thin seal wire of an outer insulating layer coating on two electrodes, connect resistance test set, in the thermoanalytical process of quasi-static or static mechanical test of MATERIALS ' DYNAMIC original position, synchronously, the resistance value of testing conductive material online.
2. the electrical testing method of testing conductive structure according to claim 1, it is characterized in that, the electrically-conducting paint method is in surperficial degreasing that needs the loading electrode sample or slight polishing, directly be coated with the silver slurry then, silver slurry coating surface directly tin plate electrical lead, also can be stained with electrical lead with silver-colored the slurry again.
3. the electrical testing method of testing conductive structure according to claim 1 is characterized in that, mechanical loading electrode method is that the superficial layer that sample material is treated loading electrode is advanced in the particularly zinc-plated copper mesh hot pressing of copper mesh, again electrical lead in copper mesh or the online soldering of tin-coated copper.
4. the electrical testing method of testing conductive structure according to claim 1, it is characterized in that bonding loading electrode method is to treat the loading electrode surface earlier to carry out degreasing and grinding process, then, metal film is stained with the cementing agent that contains silver powder, again electrical lead in the soldering of metal film outside surface.
5. the electrical testing method of testing conductive structure according to claim 4 is characterized in that, the cementing agent that contains silver powder is epoxy resin or polyurethane.
6. the electrical testing method of testing conductive structure according to claim 1 is characterized in that, electrode can be face electrode or termination electrode; Also can be that two-sided point electrode or asymmetric one side are that face electrode another side is the electrode form of point electrode.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 98126142 CN1100260C (en) | 1998-12-25 | 1998-12-25 | Electrical measurement method for measuring conducting material structure |
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| CN 98126142 CN1100260C (en) | 1998-12-25 | 1998-12-25 | Electrical measurement method for measuring conducting material structure |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100409003C (en) * | 2001-10-10 | 2008-08-06 | 株式会社日立制作所 | Resin thermal impedance testing method and tester using same |
| CN101846706A (en) * | 2010-05-18 | 2010-09-29 | 宁波大学 | Method for dynamically measuring high resistance of polymer sheets |
| CN101968511A (en) * | 2010-09-27 | 2011-02-09 | 成都理工大学 | Small electrode experiment device for measuring resistivity of mineral and solid insulating material |
| CN102759690A (en) * | 2012-06-25 | 2012-10-31 | 中国电力科学研究院 | Method for judging insulation aging degrees of alternating current (AC) cables |
| CN101750440B (en) * | 2008-12-11 | 2012-11-21 | 中国铝业股份有限公司 | Method for detecting assembly quality of cathode carbon block of electrolytic cell and test fixture |
| CN103048541A (en) * | 2012-12-27 | 2013-04-17 | 河北省电力公司电力科学研究院 | Testing method for conductivity change in service process of grounding material |
| CN103412007A (en) * | 2013-01-10 | 2013-11-27 | 哈尔滨飞机工业集团有限责任公司 | Method for monitoring fatigue crack |
| CN103529299A (en) * | 2013-09-30 | 2014-01-22 | 东北大学 | Four-line measuring method used for studying piezoresistive characteristics of conducting polymer composite materials |
| CN103869164A (en) * | 2012-12-14 | 2014-06-18 | 核工业西南物理研究院 | Insulation resistance test device of ceramic coating under high pressure state |
| CN105050318A (en) * | 2015-07-06 | 2015-11-11 | 南京本川电子有限公司 | PCB structure with embedded resistance testing zone and test method thereof |
| CN106706700A (en) * | 2016-11-11 | 2017-05-24 | 四川天策聚材科技有限公司 | Online monitoring system and method for phase change-resistance relation of conductive polymer composite material |
| CN109738331A (en) * | 2019-01-18 | 2019-05-10 | 中国航发北京航空材料研究院 | A method of detection honeycomb ceramics Density Distribution |
| CN111272830A (en) * | 2020-02-27 | 2020-06-12 | 成都飞机工业（集团）有限责任公司 | Method for detecting surface treatment quality of composite material |
| CN111505360A (en) * | 2020-05-21 | 2020-08-07 | 西部超导材料科技股份有限公司 | Sample preparation method for measuring resistance of non-tin-philic material by voltammetry |
| CN113406390A (en) * | 2021-05-19 | 2021-09-17 | 中航西安飞机工业集团股份有限公司 | Testing device and testing method for conductive colloid accumulated resistivity |
| CN117872026A (en) * | 2024-03-11 | 2024-04-12 | 深圳市聚芯源新材料技术有限公司 | Detection method and device for conductive adhesive material |
-
1998
- 1998-12-25 CN CN 98126142 patent/CN1100260C/en not_active Expired - Lifetime
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100409003C (en) * | 2001-10-10 | 2008-08-06 | 株式会社日立制作所 | Resin thermal impedance testing method and tester using same |
| CN101750440B (en) * | 2008-12-11 | 2012-11-21 | 中国铝业股份有限公司 | Method for detecting assembly quality of cathode carbon block of electrolytic cell and test fixture |
| CN101846706A (en) * | 2010-05-18 | 2010-09-29 | 宁波大学 | Method for dynamically measuring high resistance of polymer sheets |
| CN101846706B (en) * | 2010-05-18 | 2012-05-30 | 宁波大学 | Method for dynamically measuring high resistance of polymer sheets |
| CN101968511A (en) * | 2010-09-27 | 2011-02-09 | 成都理工大学 | Small electrode experiment device for measuring resistivity of mineral and solid insulating material |
| CN101968511B (en) * | 2010-09-27 | 2012-11-28 | 成都理工大学 | Small electrode experiment device for measuring resistivity of mineral and solid insulating material |
| CN102759690A (en) * | 2012-06-25 | 2012-10-31 | 中国电力科学研究院 | Method for judging insulation aging degrees of alternating current (AC) cables |
| CN103869164A (en) * | 2012-12-14 | 2014-06-18 | 核工业西南物理研究院 | Insulation resistance test device of ceramic coating under high pressure state |
| CN103048541A (en) * | 2012-12-27 | 2013-04-17 | 河北省电力公司电力科学研究院 | Testing method for conductivity change in service process of grounding material |
| CN103412007A (en) * | 2013-01-10 | 2013-11-27 | 哈尔滨飞机工业集团有限责任公司 | Method for monitoring fatigue crack |
| CN103529299B (en) * | 2013-09-30 | 2016-05-18 | 东北大学 | For studying the four lines measuring method of conductive polymer composite pressure drag characteristic |
| CN103529299A (en) * | 2013-09-30 | 2014-01-22 | 东北大学 | Four-line measuring method used for studying piezoresistive characteristics of conducting polymer composite materials |
| CN105050318B (en) * | 2015-07-06 | 2017-11-28 | 江苏本川智能电路科技股份有限公司 | With the pcb board structure and its method of testing for burying resistance test section |
| CN105050318A (en) * | 2015-07-06 | 2015-11-11 | 南京本川电子有限公司 | PCB structure with embedded resistance testing zone and test method thereof |
| CN106706700A (en) * | 2016-11-11 | 2017-05-24 | 四川天策聚材科技有限公司 | Online monitoring system and method for phase change-resistance relation of conductive polymer composite material |
| CN109738331A (en) * | 2019-01-18 | 2019-05-10 | 中国航发北京航空材料研究院 | A method of detection honeycomb ceramics Density Distribution |
| CN111272830A (en) * | 2020-02-27 | 2020-06-12 | 成都飞机工业（集团）有限责任公司 | Method for detecting surface treatment quality of composite material |
| CN111272830B (en) * | 2020-02-27 | 2021-06-08 | 成都飞机工业（集团）有限责任公司 | Method for detecting surface treatment quality of composite material |
| CN111505360A (en) * | 2020-05-21 | 2020-08-07 | 西部超导材料科技股份有限公司 | Sample preparation method for measuring resistance of non-tin-philic material by voltammetry |
| CN113406390A (en) * | 2021-05-19 | 2021-09-17 | 中航西安飞机工业集团股份有限公司 | Testing device and testing method for conductive colloid accumulated resistivity |
| CN117872026A (en) * | 2024-03-11 | 2024-04-12 | 深圳市聚芯源新材料技术有限公司 | Detection method and device for conductive adhesive material |
| CN117872026B (en) * | 2024-03-11 | 2024-05-14 | 深圳市聚芯源新材料技术有限公司 | Detection method and device for conductive adhesive material |
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Assignee: GUODIAN UNITED POWER TECHNOLOGY (CHIFENG) Co.,Ltd. Assignor: AVIC BEIJING INSTITUTE OF AERONAUTICAL MATERIALS Contract record no.: 2011990000127 Denomination of invention: Electrical measurement method for measuring conducting material structure Granted publication date: 20030129 License type: Exclusive License Open date: 19990915 Record date: 20110307 |
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