WO1986006833A1 - Measuring hardness by contact resistance of indenter material - Google Patents

Measuring hardness by contact resistance of indenter material Download PDF

Info

Publication number
WO1986006833A1
WO1986006833A1 PCT/AU1986/000122 AU8600122W WO8606833A1 WO 1986006833 A1 WO1986006833 A1 WO 1986006833A1 AU 8600122 W AU8600122 W AU 8600122W WO 8606833 A1 WO8606833 A1 WO 8606833A1
Authority
WO
WIPO (PCT)
Prior art keywords
indenter
sample
electrical
resistance
hardness
Prior art date
Application number
PCT/AU1986/000122
Other languages
English (en)
French (fr)
Inventor
Hiroshi Julian Goldsmid
Victor Raymond Howes
Lech Wieczorek
Original Assignee
Unisearch Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Unisearch Limited filed Critical Unisearch Limited
Publication of WO1986006833A1 publication Critical patent/WO1986006833A1/en

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/40Investigating hardness or rebound hardness
    • G01N3/42Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/06Indicating or recording means; Sensing means
    • G01N2203/0617Electrical or magnetic indicating, recording or sensing means

Definitions

  • the present invention relates to a method for measuring the hardness of materials by measuring the electrical contact resistance between a conducting indenter and a metal object applicable to measuring the hardness of conducting materials such as metals and the hardness of non-conducting materials (such as ceramics and plastics) that have been coated with a thin metal layer.
  • a method for determining the hardness of certain materials from measurements of the thermal contact resistance has recently been described in H.J. Golds id and J.N. Johnston.J.Phys. E., Sci Instrum., 1 (1981) 1329, and H.J. Goldsmid and J.N. Johnston.J Materials Science, 1_7 (1982) 1012.
  • the method is really satisfactory only when the thermal conductivity of the material under test is very high.
  • the present invention thus consists in a method of determining the hardness of certain materials by the measurement of electrical resistance between a conducting indenter and an electrically conducting sample, wherein the indenter is made of a hard semi-conducting material, e.g. silicon carbide. It is preferred that the indenter be of a composition such that its electrical conductivity is almost independent of temperature. It is further preferred that the geometry of the indenter be the same as that of the Vickers pyramid diamond indenter to permit its use in conventional hardness test ng mac nes. T s g ves a major advantage of ready calibration against the Vickers hardness scale.
  • a pre-test operation consisting of passing an electrical discharge through the contact between the indenter and the material be carried out to improve the reproducibility of the contact resistance.
  • Fig. 1 shows electrical resistivity plotted against temperature for the silicon carbide material used in the indenter. Also shown is the data for two of the samples measured by Burgemeister et al as described in J. Appl. Phys. , _50. (1979) 5790.
  • Fig. 4 shows electrical resistance before and after condenser discharge plotted against reciprocal of the observed diagonal of the indentation for a typical steel sample.
  • Fig. 5 is a plot of electrical resistance against reciprocal of the diagonal for all the samples studied for loads between 0.2. and 10 kg.
  • Fig. 7 shows a variation of relative hardness (proportional to the square of the resistance) with time for indentations on metallised Perspex and CR-39.
  • Zwick hardness testing machine Type Z3.2A This machine is normally used for the performance of Vickers hardness tests, using loads of up to 10.kg.
  • leads were attached to the indenter and to the metallic test samples, the latter being electrically insulated from the rest of the machine.
  • the indenter In the Vickers test, the indenter consists of a diamond pyramid having an angle of 136 between opposite faces. In the present experiment, the diamond indenter was replaced by one of a number made from hot-pressed, high density silicon carbide, originally supplied by the American National Bureau of Standards in bar form. The indenters were either of the standard Vickers shape or were conical with a half-angle of 60°. The results were qualitatively similar for all the indenters but the data that are presented here refer specifically to one of the standard pyramidal shape, with well-polished faces, that was made from a particular bar of SiC. All of the measurements with the indenter were carried out at a temperature of 300°K.
  • the electrical resistance between the indenter and the metal sample was determined by observing the potential drop, using a multi-range digital voltmeter, for various values of the current. It was established that the only significant voltage occurred in the region of the contact between the two materials. Provision was later made for the discharge of a condenser through the contact, as will be described shortly.
  • Table 1 lists the samples that were studied together with their Vickers hardness numbers, as determined using a diamond indenter. The surfaces of the samples were polished, as is normal for hardness testing, and degreased, but no special cleaning procedure was necessary. As mentioned in the introduction, it is desirable that the electrical resistivity p of the indenter should be much greater than that of any of the metals that might be tested.
  • Figure 1 shows the observed values for p, over temperature range 300-450°K, obtained using a four-contact technique on a rectangular bar. The resistivity at 300°K is 0.37 ohm m, whereas metals and metallic alloys have resistivities in the range 10 -8 to
  • Fig. 1 also shows the variation of electrical resistivity with temperature for two of the crystalline samples that were studied by Burgeffle et al. referenced aboye. It is noted that whereas the negative temperature coefficient of the resistivity - (dp/dT)/p for the hot-pressed SiC is less than for the crystalline sample No. 4, it still has the relatively high value of 6.9 x 10 " K . However, the crystalline sample No. 1 has almost zero temperature coefficient and its electrical resistivity is still several orders of magnitude greater than that of a metal. Thus, an indenter made from material similar to Burgemeister's sample No. 1 would have the important additional advantage of virtual temperature independence.
  • the electrical resistivity of the semiconductor should not be too high or it is likely to encounter barrier problems such as those experienced in semiconductor rectifiers.
  • the resistivity of the semiconductor indenter is at least 100 times that of the electrically conducting sample but it is preferred that resistivity of the indenter be less than, say, 100 ohm metre.
  • the upper curves of Fig. 2 show typical behaviour of the electrical contact resistance, as measured over a wide range of applied voltage. The features that are apparent are: (i) a small difference in resistance according to whether the indenter is positive or negative with respect to the metal; (ii) an increase or decrease of resistance, according to the polarity, at low voltages; and ( ⁇ i) a substantial decrease at high voltages.
  • Fig. 2 applies specifically for a sample of steel, with a load of 0.2 kg applied to the indenter, but it was invariably found that the plateau region included measurements at an applied potential difference of lOmV, whatever the test metal or the load. For this reason, the observations were normally carried out with this value for the applied voltage.
  • the behaviour at very low voltages, including the effect of polarity, may be indicative of interfacial barrier effects, while the trend at high temperatures could be due to Joule heating.
  • Fig. 3 shows how the resistance of the contact fell, as the voltage on the 15 nF condenser was increased, for a variety of samples. There was little or no change for the gold sample Gl, but in all other cases there was a significant effect. It was apparent that little further reduction of resistance occurred after the condenser voltage reached 100 V. Thus, a discharge from the condenser at this voltage was adopted as a standard pre-test operation. There is, of course, no reason why the capacitance of 15 nF should be better than any other value, and further studies could be made on the optimisation of the discharge.
  • Fig. 5 shows R plotted against 1/d for all the samples listed in Table 1, at loads between 0.2. kg and 10 kg.
  • a single straight line of slope 0.083 ohm m satisfies all the data with a standard deviation of less than 10%. This slope is called the indenter constant C. It is concluded that the measured contact resistance can be employed to predict the length of the diagonal of the indentation for a given load and, thus, the hardness of the metal.
  • R Q is the resistance at zero time. It is seen that, whereas for gold the resistance is time-independent, it takes several minutes with CR-39 and Perspex before constant values are approached. Clearly, important information about the time-dependent mechanical properties of these materials is thus made available by a comparatively simple technique, much less time consuming than an equivalent optical microscope method.
  • the indenter constant In practice, we would expect the indenter constant to be somewhat greater than P /2, because a square of diagonal d occupies less area than a circle of diameter d and there is extra resistance associated with the part of the pyramid lying within the indentation.
  • the indenter constant would also be made larger by any imperfection in the contact between the surfaces. in fact, the observed value for the indenter constant is no more than 0.083 ohm m whereas p/2 is 0.185 ohm m.
  • the resistivity of the SiC near the tip of the indenter must be of lower resistivity than the value measured on the rectangular bar from which the indenter was cut.
  • the bar was found to be quite uniform on a microscopic scale but it is possible that it was microscopically inhomogeneous. There is some evidence for this, in that a different indenter constant was obtained when the SiC was reground and repolished. Be that as it may, the indenter constant is obviously of the same order as the predicted value which suggests that the surfaces must be in intimate electrical contact with one another, at least after the pre-test operation.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
PCT/AU1986/000122 1985-05-03 1986-05-02 Measuring hardness by contact resistance of indenter material WO1986006833A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AU41885 1985-05-03
AUPH0418 1985-05-03

Publications (1)

Publication Number Publication Date
WO1986006833A1 true WO1986006833A1 (en) 1986-11-20

Family

ID=3691185

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/AU1986/000122 WO1986006833A1 (en) 1985-05-03 1986-05-02 Measuring hardness by contact resistance of indenter material

Country Status (4)

Country Link
EP (1) EP0221165A1 (ja)
JP (1) JPS62503052A (ja)
DE (1) DE3690235T1 (ja)
WO (1) WO1986006833A1 (ja)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992008119A1 (en) * 1990-10-24 1992-05-14 Alfred Ernst Hardness tester and method for measuring the hardness of metallic materials
WO1995007454A1 (en) * 1993-09-10 1995-03-16 Alfred Ernst Electrical resistance hardness tester for metallic materials
DE10003836A1 (de) * 2000-01-28 2001-08-16 Fraunhofer Ges Forschung Indentor und Verfahren zu seiner Herstellung

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU232579A1 (ru) * Д. А. Саркис Индентор для автоматического измерения твердости токопроводящих материалов
US1781002A (en) * 1927-02-04 1930-11-11 Esnault-Pelterie Robert Method and apparatus for use in testing materials
DE841804C (de) * 1951-04-05 1952-06-19 Eberhard Dr-Ing Contius Unmittelbare Messung der Haertewerte bei Brinell- und Vickerspruefung
FR1060211A (fr) * 1952-07-08 1954-03-31 Renault Procédé de mesure de dureté de pièces métalliques
EP0052857A1 (en) * 1980-11-25 1982-06-02 Unisearch Limited Hardness tester

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU232579A1 (ru) * Д. А. Саркис Индентор для автоматического измерения твердости токопроводящих материалов
US1781002A (en) * 1927-02-04 1930-11-11 Esnault-Pelterie Robert Method and apparatus for use in testing materials
DE841804C (de) * 1951-04-05 1952-06-19 Eberhard Dr-Ing Contius Unmittelbare Messung der Haertewerte bei Brinell- und Vickerspruefung
FR1060211A (fr) * 1952-07-08 1954-03-31 Renault Procédé de mesure de dureté de pièces métalliques
EP0052857A1 (en) * 1980-11-25 1982-06-02 Unisearch Limited Hardness tester

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992008119A1 (en) * 1990-10-24 1992-05-14 Alfred Ernst Hardness tester and method for measuring the hardness of metallic materials
US5309754A (en) * 1990-10-24 1994-05-10 Alfred Ernst Hardness tester and method for measuring the hardness of metallic materials
WO1995007454A1 (en) * 1993-09-10 1995-03-16 Alfred Ernst Electrical resistance hardness tester for metallic materials
US5571954A (en) * 1993-09-10 1996-11-05 Ernst; Alfred Electrical resistance hardness tester for metallic materials
DE10003836A1 (de) * 2000-01-28 2001-08-16 Fraunhofer Ges Forschung Indentor und Verfahren zu seiner Herstellung
DE10003836C2 (de) * 2000-01-28 2002-04-25 Fraunhofer Ges Forschung Indentor und Verwendung desselben

Also Published As

Publication number Publication date
DE3690235T1 (ja) 1987-07-16
EP0221165A1 (en) 1987-05-13
JPS62503052A (ja) 1987-12-03

Similar Documents

Publication Publication Date Title
Imre et al. Electrochemical determination of the fractal dimension of fractured surfaces
Lim et al. Accurate determination of the mechanical properties of thin aluminum films deposited on sapphire flats using nanoindentations
Hainsworth et al. Analysis of nanoindentation load-displacement loading curves
Todoroki et al. Application of electric potential method to smart composite structures for detecting delamination
Jacobson et al. The use of fast heavy ions to improve thin film adhesion
Brainard et al. Adhesion and friction of PTFE in contact with metals as studied by Auger spectroscopy, field ion and scanning electron microscopy
Hauch et al. Energy balance in dynamic fracture, investigated by a potential drop technique
Pethica et al. Micromechanical investigations of amorphous hydrogenated carbon films on silicon
Jemaa Contacts conduction and switching in DC levels
WO1986006833A1 (en) Measuring hardness by contact resistance of indenter material
HONG et al. Thermally stimulated currents in sodium silicate glasses
Wieczorek et al. Electrical contact resistance and its relationship to hardness
Braunovic Effect of fretting on the contact resistance of copper, aluminum and nickel-coated aluminum wire connections
Delahaye et al. Electron glass effects in amorphous NbSi films
WO1988003644A1 (en) Hardness measuring with a diamond indenter having surface treatment or coating
Yamamoto et al. A study of the physical adhesive state between solids
EP0972182B1 (en) Electrostatic adhesion tester for thin film conductors
El-Kazzaz et al. The use of liquid metals for contact-charging experiments
US6002259A (en) Electrostatic adhesion tester for thin film conductors
CN112782211B (zh) 一种水相变的探测方法
Kim et al. Dynamic fracture test of metal thin films deposited on an insulating substrate by a high current pulse method
Putz The influence of high current densities on intact and cracked thin gold films on flexible polyimide substrate
Log et al. Technique for determining thermal shock resistance of carbon materials
SU1733960A1 (ru) Способ оценки контактных свойств материалов дл проводников
KR20060104119A (ko) 투명전도막의 접착력 시험방법

Legal Events

Date Code Title Description
AK Designated states

Kind code of ref document: A1

Designated state(s): AU DE GB JP US

AL Designated countries for regional patents

Kind code of ref document: A1

Designated state(s): FR

RET De translation (de og part 6b)

Ref document number: 3690235

Country of ref document: DE

Date of ref document: 19870716

WWE Wipo information: entry into national phase

Ref document number: 3690235

Country of ref document: DE