CN100516855C - Method and device for investingating resistivity of powder metal - Google Patents
Method and device for investingating resistivity of powder metal Download PDFInfo
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- CN100516855C CN100516855C CNB2006100630694A CN200610063069A CN100516855C CN 100516855 C CN100516855 C CN 100516855C CN B2006100630694 A CNB2006100630694 A CN B2006100630694A CN 200610063069 A CN200610063069 A CN 200610063069A CN 100516855 C CN100516855 C CN 100516855C
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Abstract
The invention relates to new type powder metallic material resistivity testing method and device. It feature is that it measures the resistivity for the measured powder material with different density, calculates out the corresponding resistivity and conductivity to gain the curve described powder material electricity performance. The testing device is made up of pressure mechanism, micro displacement testing device, rigid bridge, and sample box. The pressure mechanism is used to change the powder material volume in the sample box. The micro displacement measuring device is used to record the change in real time. The rigid bridge is used to record corresponding powder resistance value. This measuring method and device can be used in nickel powder resistivity measuring, other metallic or non metallic powder material, nanometer material resistivity and conductivity measuring. Thus it will play an important role in materials, electronic technology etc.
Description
Technical field
The present invention relates to the measurement mechanism of a kind of powder metal material resistivity or conductivity.This device utilizes pressure to act on tested powder body material sample, not changing the density that changes powder body material under the tested powder body material microscopic appearance prerequisite, by measuring corresponding resistance and density, calculates resistivity and conductivity.
Background technology
Resistivity and conductivity are the important unit for electrical property parameters of electronic material.For common body material, the measurement of its resistivity is international and domestic codes and standards is arranged all, and the resistivity of many common used materials all enrolled relevant databook with conductivity can be for inquiring about.But for powder body material and nano-powder material, because the localization characteristic of electronics and the surface potential and the interfacial potential of powder make their resistivity different with the body material with conductivity.For example, the resistivity of the body material of nickel is 6.97 * 10 under 20 ℃ of normal pressures
-6Ω cm, and the resistivity of nickel powder is than at least four orders of magnitude that exceed of body material, and relevant with the production technology of nickel powder, store status, powder surface oxidation state etc.The porousness difference of commaterial, its resistivity are also different; The resistivity by the powder metal of the different size that becomes with a kind of element set that different manufacturers produce can't compare the quality of its electrical property.
The fast development that relates to the industry of powder metal material such as battery technology, low-cost electric thin technology has in recent years directly promoted the development of powder Metal Production technology, has driven the market demand of powder metal material.The manufacturing enterprise of material wishes to produce the material of different electrical properties to satisfy the application demand of expansion day by day; If can carry out scientific evaluation to the electrical property of material, just can go production technology according to material property, produce the powder metal material of different size.The user of material also wishes can be unit for electrical property parameters as one of basis of selecting material, thereby realizes scientific and reasonable materials used.Therefore relate to the production of material and the enterprise of application all wishes powder metal material electrical property is carried out the evaluation of science, the demand of the scientific evaluation method of powder metal material is seemed urgent day by day.
According to investigation, still domestic at present no matter in the world, all not to the codes and standards of metal powder material electric performance test.In conducting resinl and electrostatic screening industry, the powder metal material is mixed into to be used in the colloid, and the someone has studied electrical property measuring method in this case.But the producer of material and user more wish to understand the electrical property of metal material under the powder state.Golden south of the Five Ridges non-ferrous metal incorporated company has carried out joint study at the electric conductivity of fibrous nickel powder in Inst. of Optoelectronics, Shenzhen Univ. and the Shenzhen, summed up the method for testing of a cover powder metal, according to this method, make the powder metal material comprise that the evaluation of the electric conductivity of nano material becomes possibility, make powder body material electric conductivity foundation relatively arranged.The present invention produces on this basis.
Summary of the invention
The invention provides the method for testing of a kind of powder metallic resistance rate and conductivity, it can carry out scientific evaluation to the electric conductivity of powder metal material.The feature of this method is to exert pressure in the mode that increases progressively continuously to a certain amount of powder body material sample, the density of specimen material is changed, write down the resistance and the characteristic dimension of corresponding pressure, sample simultaneously, go out the resistivity and the conductivity of material again according to the various calculation of parameter of record.
We find in the research to fibrous nickel powder electric conductivity, and when increasing continuously pressure for the nickel powder of certain mass, the resistivity of nickel powder diminished rapidly before this, and promptly resistivity is very big with the rate of change of pressure; Afterwards, resistivity begins slowly to diminish; Along with the further increase of pressure, the variation of resistivity is more and more slower; After pressure was increased to a certain degree, resistivity was near the resistivity value (referring to Fig. 1) of body material.The effect of pressure is to change the volume of material sample, and under the constant situation of sample quality, the effect of pressure is exactly the density that changes powder sample.Therefore, resistivity has identical trend (referring to Fig. 2) with the variation of density with variation with pressure.Measure the resistivity under the different densities, just can contrast the electric conductivity of powder body material.This is basis of the present invention.
Based on said method, the invention provides a kind of measurement mechanism example.This measurement mechanism is made up of pressure apparatus, micro displacement testing device, precision type bridge, sample box etc.Wherein pressure apparatus offers sample continually varying pressure and can the pressure that be provided be measured accurately and show that it can be manual, also can be electronic, can also be to provide pressure by hydraulic pressure; Micro displacement testing device is used for writing down the displacement that the material of sample box produces along pressure direction under pressure; Precision type bridge is used for measuring samples resistance under pressure; Sample box provides a cylindrical or cuboid space to be used to adorn powder body material, and it is made up of two electrodes and insulating sleeve up and down, and electrode can be along the sleeve wall slip in sleeve, and the length of slip is by the micro displacement testing device record.
Based on above-mentioned measuring method and device, the invention provides a kind of easy Pressure generator.Its mechanism that produces pressure is mechanical spiral precession, and it not only can provide pressure, can also the pressure that provide be kept for a long time, to satisfy different testing requirements.
Based on above-mentioned measuring method and device, the invention provides a kind of easy micro-displacement measuring device, when an electrode of sample box fixedly the time, its displacement of producing under pressure of another electrode of measuring samples box accurately, thus determine specimen material volume change under pressure.
The present invention also provides a kind of structural design and making of powder body material sample box.The space that holds sample that it provides should have the geometric configuration of simple rule, can bear big pressure effect simultaneously.The electrode of sample box should have good electrical conductivity, and sleeve should have very high electrical insulating property.
Description of drawings
Accompanying drawing 1 resistivity is with the change curve of pressure.
Accompanying drawing 2 resistivity are with the change curve of density of material.
The stereoscan photograph of accompanying drawing 3 nickel powders under the state of nature of not passing through any ambient pressure effect.
Accompanying drawing 4 nickel powders are through the stereoscan photograph after 400 newton's pressure effects.
Accompanying drawing 5 powder metal material resistivity test device sketches.
Accompanying drawing 6 sample box structural representations.
Accompanying drawing 7 pressure apparatus structure diagrams.
In the accompanying drawing, 510 sample boxs, 520 pressure apparatus, 530 micro displacement testing device, 531 vertical rulers, 532 slide blocks, 533 rigidity straight-bars, 540 test electric bridges, 611 top electrodes, 612 insulating sleeves, 613 samples, 614 bottom electrodes, 721 rigidly fix piece, 722 supports, 723 screw rods, 724 slide blocks, 725 pressure gauges, 726 pressure transmit piece, 727 handle wheels, 728 bases.
Embodiment
Resistivity provided by the invention and conductivity measuring method are suitable for the electrical property evaluation of powder metal material.The powder metal material is meant the minimum unit of composition material here---to submillimeter scope, characteristic feature is of a size of several microns to the characteristic dimension of powder in nanometer.The shape of these micron particles, surface state and density of material etc. all directly affect the resistivity of powder body material.This just makes that the electrical property of powder metal material is measured and there is difficulty in evaluation, and the resistivity measurement method and the standard of conventional body material no longer are suitable for powder body material.The fast development of powder technology and nano material technology requires to be suitable for the electric performance test method of own characteristic.We propose to use resistivity-densimetric curve can not only objectively describe the electric conductivity of nickel powder, but also are convenient to comparison by to the research of nickel powder electric performance test.The present invention produces on this basis, and therefore, the measurement of resistivity-densimetric curve is a core of the present invention.
The powder metal generally is dispersed in them in colloid or other reagent or the material in use, and its granule-morphology should remain unchanged.Therefore the various external influences that when measuring its electric conductivity sample applied should guarantee that sample microscopic particles pattern is constant.This is a basic constraint of measuring method provided by the invention.Among the present invention, the change of sample rate relies on ambient pressure to realize, we find that in 400 newton, the variation of sample microscopic particles pattern is little to the sample applied pressure, has the phenomenon of conglomeration in the individual samples in to the research of nickel powder electric performance test.Fig. 3 is the stereoscan photograph of nickel powder in the state of nature of not passing through any ambient pressure effect, and Fig. 4 is the stereoscan photograph that the sample of same specification removes external force after through 400 newton's pressure effects again.By a large amount of contrasts and observation, we are defined as 400 newton with the upper pressure limit of using in the nickel powder resistivity measurement method.Fig. 1 is the resistivity-pressue-graph of nickel powder, and Fig. 2 is corresponding resistivity-densogram.As can be seen from the figure, very slow greater than the variation of resistivity after 200 newton when pressure, this is rational with regard to the pressure limit that we are described.
Fig. 5 is a measurement mechanism example provided by the invention, and it is made up of four parts such as sample box (510), pressure apparatus (520), micro displacement testing device (530) and test electric bridge (540).Sample box is the core component of this measurement mechanism, is used for placing tested powder metal sample, and Fig. 6 (A) is its structure diagram.It is made up of top electrode (611), bottom electrode (614), insulating sleeve (612) and sample (613).The structure and material of two electrodes is all identical, is processed into shape shown in Fig. 6 (B) with the copper rod that conducts electricity very well.The diameter of cylinder electrode is identical with the internal diameter of sleeve, and can be free to slide in sleeve.The disk of electrode is mainly used to bear and transmit pressure, and the size of its diameter does not have strict regulation, and generally with identical the getting final product of external diameter of sleeve, the thickness of disk can be taken as more than the 10mm.The difference of two electrodes only is the length of electrode column, and the electrode column length of following electrode (614) is short, and size can be taken as about 1/4th of length sleeve; The electrode column of top electrode (611) is longer, and its length is 0.8-1.2 times of length sleeve.In fact the value to the electrode column length of two electrodes does not all have strict regulation, but two electrode column length sums should be not less than length sleeve.The sleeve of sample box can be used the pottery or the plastic production of good insulation preformance, and its shape is shown in Fig. 6 (C).The size of external diameter can be selected according to the test needs in the sleeve, and internal diameter is elected 10mm as in this example, and external diameter is elected 30mm as.The length of sleeve also is according to the decision of test needs, elects 80mm in this example as.Sample (613) is put between the interior upper/lower electrode of sleeve.
Pressure apparatus among Fig. 5 (520) is used for providing pressure to sample, and its structural representation as shown in Figure 7.It transmits piece (726), handle wheel (727) and base (728) etc. and forms by rigidly fixing piece (721), support (722), screw rod (723), slide block (724), pressure gauge (725), pressure.Rigidly fix piece and support and rigidly fix together, screw axis is connected with slide block (724) spiral by rigidly fixing piece, and handle wheel and screw axis are rigidly connected.Pressure gauge and slide block are rigidly connected, and pressure transmits piece and the pressure gauge expansion link is rigidly connected.The turning handle wheel, screw axis and then rotates, and drives slide block and slides in two vertical rods of support.Pressure gauge and then moves up and down together, and pressure is delivered to pressure by manometric expansion link and transmits on the piece, remakes to be used for sample box.When the turning handle wheel reached required force value, this pressure can keep always.
Micro displacement testing device among Fig. 5 (530) is used for the displacement of measuring samples box top electrode.It is made up of two parts, promptly vertical ruler (531) and the slide block (532) that can on ruler, slide, and base (534) all is rigidly fixed on the same base plate with pressure apparatus and sample box.Displacement transducer, LCDs (LCD) and operation knob are housed in the slide block.Be rigidly connected by the expansion link of a rigidity straight-bar (533) the meter of the pressure side in slide block and the pressure apparatus.(precision can reach 1 micron to powder sample in the sample box any minute movement under pressure, precision is 10 microns in this example) all can pass on the manometric expansion link by the top electrode of sample box, the slide block (532) of rigidity drive gearshift moves again, thereby shows on LCD display.Micro displacement testing device also can be any electronic type or mechanical type displacement tester that satisfies above-mentioned requirements.
Resistance apparatus among Fig. 5 (540) is a precision type bridge.It is any single armed or the both arms direct current bridge that satisfies the measuring accuracy requirement.Electric bridge in this example is that precision is single both arms direct current bridge of 0.05.Two electrodes of sample box and the measurement binding post of electric bridge link to each other, and the resistance that wherein connects lead is as much as possible little.
The process of resistivity of measuring the powder metal material with Fig. 5 measurement mechanism provided by the invention is as follows:
1) clean sample box (comprising electrode, sleeve) with alcohol after, with two electric pole short circuits (in the sample box do not let alone what sample), connect line with electric bridge;
2) adjust pressure apparatus, the pressure of this moment is in the critical point of zero pressure; Adjust displacement tester, making its display position reading is zero;
3) continuously change pressure, write down corresponding resistance value and top electrode position coordinates;
4) relief pressure takes out sample box;
5) weigh up the quality of tested powder sample with precision balance, and sample is packed in the sample box, insert top electrode, be put on the pressure apparatus again;
6) repeating step 3);
7) data processing.
More than narration only is the exemplary implementation example of the present invention, need to prove that basic thought among the present invention and basic skills can have multiple variation, and each variation all can be implemented, and they should be limited by claims of the present invention.
Claims (1)
1. powder metallic resistance rate measurement mechanism, this measurement mechanism comprises: pressure apparatus, pressure gauge, test electric bridge and sample box are formed, be provided with upper and lower electrode in the sample box, top electrode transmits piece, manometric expansion link through pressure and is connected successively along axis with screw rod in the pressure apparatus, it is characterized in that:
A. set up the micro displacement testing device of forming by vertical ruler (531), slide block (532), rigidity straight-bar (533), base (534) (530) on the described measurement mechanism:
B. described slide block (532) is provided with displacement transducer, LCDs (LCD) and operation knob:
C. described base (534) is fixed on the base (728) of measurement mechanism, and slide block (532) is slidingly connected with vertical ruler (531), fixedlys connected with slide block (532) with manometric expansion link respectively in rigidity straight-bar (533) two ends.
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CNB2006100630694A CN100516855C (en) | 2006-10-13 | 2006-10-13 | Method and device for investingating resistivity of powder metal |
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CNB2006100630694A CN100516855C (en) | 2006-10-13 | 2006-10-13 | Method and device for investingating resistivity of powder metal |
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Families Citing this family (14)
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CN101685115B (en) * | 2008-09-28 | 2011-11-09 | 上海比亚迪有限公司 | Method for testing electrical conductivity of powdered material |
RU2467319C1 (en) * | 2011-06-23 | 2012-11-20 | Российская Федерация, от имени которой выступает Государственная корпорация по атомной энергии "Росатом" | Method to identify electrophysical parameter of powdered materials and device that implements it |
CN102565535A (en) * | 2012-03-07 | 2012-07-11 | 德州学院 | Experimental instrument for resistivity and dielectric constant of biological tissue |
CN102854385A (en) * | 2012-07-24 | 2013-01-02 | 烟台德邦科技有限公司 | Testing device and testing method for resistivity of metal powder |
CN103852642A (en) * | 2012-12-06 | 2014-06-11 | 天津工业大学 | Method for detecting electrical conductivity of small number of solids |
CN103149439B (en) * | 2013-02-22 | 2015-06-17 | 北京科技大学 | Device and method for testing electric conductivity of powder material and impedance of membrane electrode |
CN103728472A (en) * | 2013-10-10 | 2014-04-16 | 华南理工大学 | Fixture for measurement of electrical conductivity of proton exchange membrane |
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CN105823684B (en) * | 2015-12-09 | 2018-05-22 | 西安科技大学 | One kind is used to study conductive rubber mechanics and electrology characteristic device |
CN106324350A (en) * | 2016-08-31 | 2017-01-11 | 广东技术师范学院 | Device for measuring resistance of powder material |
CN106353372B (en) * | 2016-11-09 | 2018-11-13 | 北京工业大学 | It is a kind of to powder body material temperature, atmosphere and the regulatable resistivity measurement device of consistency |
CN107247184A (en) * | 2017-06-30 | 2017-10-13 | 深圳大学 | The test device and method of testing of a kind of electrical conductivity |
CN110411826B (en) * | 2019-07-03 | 2022-03-22 | 蜂巢能源科技有限公司 | Method for testing macroscopic strength of conductive material and application |
JP7411501B2 (en) * | 2020-05-13 | 2024-01-11 | 日東精工アナリテック株式会社 | Powder resistivity measuring device and resistivity measuring method |
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2006
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