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Techniques for Measuring the Electrical

Resistivity of Bulk Materials

Mary Anne Tupta


November 18, 2010

A GREATER MEASURE OF CONFIDENCE

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Resistivity Measurement Overview

• Definition of electrical resistivity of a material.

• Methods for making resistivity measurements of conductors,


insulators, and semiconductors.

• Key considerations for selecting equipment for measuring


resistivity.

• Sources of measurement errors and ways to optimize resistivity


measurements

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What is the Electrical Resistivity of a Material?

The electrical resistance of a material……


• is a basic material property
• defines how well the material will conduct an electric current
• is a common electrical measurement.

Ohm’s law relates the current (I) and the applied voltage (V) to the
material resistance (R) as follows:

V=IR
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What is the Electrical Resistivity of a Material?

Electrical Resistivity = longitudinal electrical resistance of a uniform


rod of unit length and unit cross-sectional area:

A
R
L
Current Source ρ = resistivity (Ω-cm)
R = resistance: V/I (Ω)
Voltmeter
V A = cross-sectional area of
L
sample (cm2)
L = distance between two
A
leads of voltmeter (cm)
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Typical Resistivity Values

The electrical resistivities of solid materials span over many magnitudes.

Three classifications of materials based on their resistivities:

Classification Type of Electrical Typical Resistivities


Conductor
Metals Good electrical 10-6 Ω-cm
conductors
Insulators Low electrical 109 to 1020 Ω-cm
conductivity
Semiconductors Intermediate levels of 10-3 to 107 Ω-cm
conductivity

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Comparison of Simplified Energy Bands

Conduction Band

Conduction Band Conduction Band

Energy
Energy Gap
Energy Gap

Valence Band
Valence Band
Valence Band

Metal Insulator Semiconductor

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Measuring the Resistivity of


Conductors:
Metals and Superconductors (very low resistance)

Graphene and other Nanomaterials


(low voltage and low power - use same techniques)

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Measuring the Resistivity of Conductors

Basic Test Procedure: Voltmeter

V
1. Source current (I) through the
L
sample using one pair of leads.
w

2. Measure the voltage drop (V) t Sample

across a second pair of leads a


known distance (L) apart.
Current Source
3. Calculate the resistivity (ρ) of
the sample using the cross-
V wt
sectional area (A=wt) and the    cm
distance between the voltmeter I L
leads.
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Sources of Error When Measuring Low Resistance

• Test Lead Resistance

• Thermoelectric Voltages

• Low Frequency Noise

• External Noise Sources

• Johnson Noise

• Voltmeter Not Sensitive Enough

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Eliminate Lead Resistance by Using the 4-Wire Method


2-Wire Method 4-Wire Method
I I

V V

RLead RLead
RLead RLead

RSample
RSample

Measured Resistance: Measured Resistance:


VM/I = RSample + 2RLead VM/I = RSample
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Thermoelectric Voltages
Voltmeter Voltmeter
Copper Test Leads
Copper Test Leads
Metal A V
Metal A V

Sample – Metal B Sample


T1 Metal B T2

Current Source Temperature Gradient

Thermoelectric voltages are generated when dissimilar metals (Metal A


and Metal B) in the circuit are at different temperatures (T1 and T2).

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Ways to Reduce Thermoelectric Voltages

• Construct test circuits using the same materials for interconnects.

• Minimize temperature gradients within the test circuit

• Allow the test equipment to warm up

• Use an offset compensation method

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Use the Current Reversal Method


to Eliminate Voltage Offsets (VEMF)
Measurement with Positive Polarity Measurement with Negative Polarity

VEMF VEMF

I+ VM+ I- VM-
R R

VM+ = VEMF + IR VM- = VEMF - IR


Voltage Measurement:

VM   VM  VEMF  IR  (VEMF  IR )
VM    IR
2 2
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Use the Delta Mode Method to Eliminate Voltage Offsets


and Noise

The Delta method consists of


alternating the current source
polarity and using a moving
average of voltage readings to
calculate the resistance.
Averaging reduces the noise
bandwidth and therefore the noise.

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External Noise Sources

• External Noise Sources = interferences created by motors, computer


screens, or other electrical equipment

• Control these External Noise Sources by:


– Shielding and filtering
– Remove or turn-off the noise source
– When using DC instruments, integrate each measurement for an integer number of
power line cycles. The line cycle noise will “average out” when the integration time
is equal to an integration number of power line cycles.

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Johnson Noise

• Johnson Noise – places a fundamental limit on resistance


measurements.

• In any resistance, thermal energy produces the motion of charged


particles. This charge movement results in Johnson noise.

• The formula for the voltage noise generated: V


rms  4kTRB
where k=Boltzmann’s constant, T= temp in K,
B=noise bandwidth in Hz, R=resistance of sample in ohms

• Reduce by:
1. reduce the measurement bandwidth –digital filtering (averaging
readings) or analog filtering
2. reduce temperature of the device
3. reduce the sample resistance (usually not practical)
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Use a Nanovoltmeter to Measure Voltage Drops


When measuring the resistances of conductors or other low power
materials, very small voltages are measured, typically in the microvolt and
nanovolt range.

To measure these very small voltage drops, use a sensitive voltmeter such
as a nanovoltmeter.
Verify the product specifications to
Model 2182A Nanovoltmeter make sure the measurement
resolution and accuracy will be
able to perform the sensitive
measurement of your application.

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Review of Measurement Considerations for Measuring


the Resistivity of Conductors Voltmeter

• Make a 4-wire measurement to eliminate the L

lead resistance from affecting the


measurement accuracy Sample

Current Source

• Use an offset compensation technique to


eliminate voltage offsets and reduce noise:
Current Reversal Method or Delta Method

• Eliminate external noise sources and use line


cycle integration.

Continued……

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Continued…..Review of Measurement Considerations

• Reduce Johnson noise by reducing the


measurement bandwidth, averaging Vrms  4kTRB
readings, and reducing the temperature
of the sample

Model 2182A
• Use a sensitive voltmeter, such as a Nanovoltmeter
nanovoltmeter, to measure the low
voltages

• Use a low noise, bipolar current source


that can perform current reversals Model 6221 AC Model 6220 DC
+ DC Current Current Source
Source
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Measuring the Resistivity of Insulators


(high resistance)

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Resistivity Measurements of Insulators

The resistance of an insulator


is measured by: Sample
I Resistance

1. Applying a voltage to the


sample for a specified R
time period Voltage
Source
V A Ammeter

2. Measuring the resulting


current

V
R
3. Calculating the resistivity
using Ohm’s Law and
geometrical considerations
I
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Volume Resistivity of Insulator

LO
Volume Resistivity is a measure of the leakage
current directly through a material. A

HI
Test Procedure for Volume Resistivity:
1. Please sample between 2 electrodes of area (A). Electrode t

Sample
2. Apply potential difference (V) between the 2
HI
electrodes.
Voltage
Source
3. Wait specified time (60 seconds) and measure LO
current (I) using sensitive ammeter.

V A

4. Calculate resistivity based on the area of the
electrodes and thickness of the sample (t). Units
are Ω-cm. I t
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Surface Resistivity of Insulator


I

Electrode
HI HI V w
 
L

Sample w A
LO
I L
LO

Surface Resistivity is defined as the electrical resistance of the surface of an


insulator.

Test Procedure for Surface Resistivity:


1. Place two electrodes a known distance (L) apart on sample.
2. Apply potential difference (V) between electrodes.
3. Wait specified time and measure current (I) with ammeter.
4. Calculate resistivity using width (w) of material and distance (L) between the
electrodes. The units are ohms or ohms per square.

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Sources of Error When Measuring High Resistance

• Improper Measurement Instrumentation

• Electrification Time

• Test Voltage

• Background Currents

• Electrodes and Geometrical Considerations

• Electrostatic Interference

• Humidity
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Use Sensitive Ammeter and Proper Cabling

Measuring the resistance of insulators usually involves measuring current in the


1E-9 and 1E-12 current range.

When measuring very small current, <100nA, it is important to use a sensitive


ammeter, such as an electrometer or picoammeter.

Electrometers and picoammeters have sub-picoamp (1E-12) sensitivity.

Model 6517B Electrometer/


Voltage Source:

The 6517B has 1E-15 A


Sensitivity!

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Time Dependency of High Resistance Measurement

•Apply 250V
•Wait 60s 250V Step Response of Antistatic Bag
•Measure Current
•Calculate Resistivity

At 5 s, current=
1.5x10-10

At 60 s, current=
2.5x10-12

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Test Voltage

• Resistivity measurements of insulators are dependent on the


applied voltage.

• In general, as the voltage increases


V
the resistivity decreases 
• Sometimes the voltage may be varied intentionally to determine
the voltage dependence of an insulator.

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Background Currents

When measuring very high resistances, background currents can cause


erroneous readings. Background may be due to:
•charge stored in the material
•static or triboelectric charge
•piezoelectric effects

Background currents can be equal or greater than the current stimulated by the
applied voltage.

If background current is same polarity as measured current, then resultant


current reading will be much higher than the true value.

If background current is the opposite polarity, these unwanted currents may


cause a reverse polarity current reading. This can cause the calculated
resistance to be negative!

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Alternating Polarity Method

Positive Voltage
Applied and
Exponential
Current Measured.

Negative Voltage
Applied and
Exponential
Current Measured.

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Electrodes

Electrodes for use on an insulating material:

• Has good contact to the material: paint on electrodes or use flat metal
plates with conductive rubber

• Should be much lower resistance than the sample and should not
contaminate the sample

• Enables easy calculation of resistivity from the geometrical


considerations
Where:
Aelectrode

ρ=Volume Resistivity
R A=area of electrode on sample
t t=thickness of sample
R=measured resistance V/I
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Volume Resistivity with the Model 8009 Resistivity Test


Fixtures
Electrodes
Top Electrode

Test
Sample
HI
HI Voltage
Ammeter A Source
LO
LO 0V Ring
Guard

Volume resistivity is a measure of the leakage Center Electrode


current through the material, between the top
electrode and center bottom electrode. The Model 8009
outside ring electrode is guard.
Resistivity Test Chamber
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Surface Resistivity with the Model 8009

The Surface Resistivity is


measured by placing two Electrodes
electrodes on the surface of the 0V Guard
test sample, applying a potential Test
difference between them, and Sample
measuring the resulting current. R
HI HI
Notice the surface resistivity (R) Ammeter A
is measured between the bottom
Center Electrode and the Ring LO LO
Electrode.

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Model 65 High Resistivity Measurement Package

8009
Resistivity
Test Fixture

6524
Software

6517B Electrometer/
Voltage Source

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Electrostatic Interference and Shielding

Shield

HI
HI
Ammeter Voltage
Sample Source
LO
LO

Connect Shield to LO terminal of Picoammeter or Electrometer

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Review of Measurement Considerations for Measuring


the Resistivity of Insulators

1. Use a picoammeter or electrometer for low current measurements

2. Use the same electrification time for each test to compare results

3. Use the same applied voltage for test comparisons Model 6517B

4. Use the Alternating Polarity Technique to reduce the effects of background


currents

5. Use proper electrodes and take geometrical considerations into account

6. Use electrostatic shielding to avoid errors due to electrostatic interference

7. Use an environmentally controlled room

Model 8009
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Measuring the Resistivity of


Semiconductors

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Measuring Resistivity of Semiconductors

The two most common methods for measuring the resistivity of


semiconductor materials are the

• Four-Point Collinear Probe Method

• van der Pauw Resistivity Method

Both of these methods use a 4-wire method to eliminate both the


lead resistance and the contact resistance from affecting
measurement accuracy.

Photo courtesy of Lucas Signatone

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4-Point Collinear Probe Method

Test Procedure:
HI LO
1. Place probes in center of wafer.
2. Source current from probes 1 to 4.
3. Measure voltage between probes 2 and 3.
4. Calculate resistivity: HI LO
V Measure

 V
Voltage
Source Current

Between 2
tk From 1 To 4 And 3
ln 2 I
4-Point
Where: Collinear
ρ= volume resistivity (ohm-cm) 1 2 3 4
Probe
V=voltage measured between 2 and 3
I=source current (A)
t = sample thickness (cm) Wafer
k=correction factor
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Sources of Measurement Error

1. Lead and contact resistance

2. Voltage offsets (use current reversal method to reduce)

3. Instrumentation

4. Issues with high resistance materials

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Test Set-Up Showing Circuit Resistances


Source Current
HI LO

RL=Lead Resistance
HI LO
V RC=Contact Resistance
RL1 RL2 RL3 RL4 RS=Semiconductor Resistance

1 2 3 4
RC1 RC2 RC3 RC4 Only the voltage drop due to RS2 is
V
measured by the voltmeter.
RS1 RS2 RS3
Measure Voltage
Between 2 And 3
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Instrumentation for Mid-Range Resistances


(100mohm to <1Mohm)

Use a standard DC current source (bipolar to perform current reversals) to


force the current and a DMM to measure the voltage drop.

OR

Use a SourceMeter which can source the current and measure the voltage
drop.

ALSO

Use a commercially available 4-point probe head.

Photo courtesy of Lucas Signatone


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Commercially Available Automatic Resistivity System

Photo courtesy of Lucas Signatone


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Issues for High Range Resistances (up to 1E12 ohms)

• Use a 4-point collinear probe that has excellent isolation between


the probes to avoid leakage current errors
• Use a current source with high output impedance (1E14) to avoid
loading errors
• Use a current source with a built-in guard to reduce the effects of
shunt capacitance
• Use voltmeters with high input impedance (1E14 ohms)
• Use shielding to avoid errors due to electrostatic interference
• Use differential electrometer method to avoid issues of common
mode current

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Common Mode Current Errors When Measuring High R


Current
Source
HI RC

AC

LO

Voltmeter Common
Mode
Current
V RV
i When the resistance of the
RIN
Contact AC sample, RS2, becomes on the
Resistance same order of magnitude as
HI LO
1 4
the isolation spec (input LO to
2 3
chassis) of the current source
RC1 RC2 RC3 RC4
and voltmeter, then common
RS1 RS2 RS3 mode current will flow
affecting the measurement
Sample Resistance accuracy.
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Making Differential Four-Point Probe Measurements


(For Very High Resistances >1Mohm)
HI LO

Voltmeter

V
HI LO

X1 X1
Buffer Buffer
HI LO HI LO

1 2 3 4
RC1 RC2 RC3 RC4

RS1 RS2 RS3

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van der Pauw Resistivity Method

van der Pauw resistivity is a 4-probe


Force
technique that involves applying a current Current
and measuring a voltage using four small
contacts on a circumference of a flat,
1
arbitrarily shaped sample.
4 2
Test Procedure:
•Force Current (I) on adjacent terminals Measure
3 Voltage

•Measure Voltage (V) on an opposite pair of V


adjacent terminals

•Repeat measurements around sample

•Calculate resistivity
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van der Pauw Resistivity Method

• vdp configuration is
useful for measuring
Force
very small samples Current

1
B
• Easy to measure Hall
voltage using an 4 2
electromagnet to apply Measure
3 Voltage
the B field
V

• Force I and Measure V Hall Configuration


on opposite terminals
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van der Pauw Resistivity


V5

1 2 1 2 1 2 1 2
V3 V7

4 3 4 3 4 3 4 3

V1

V6

1 2 1 2 1 2 1 2
V4 V8

4 3 4 3 4 3 4 3

V2

A series of 8 measurements are performed around the periphery of the sample


to compensate for offsets and are combined mathematically to compute the
resistivity.
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Switching to Perform vdp Measurements


1
Sample

Use a switch matrix to 4 2


automatically switch the current
3
source and voltmeter between all
four terminals of the sample.

1 2 3 4
Choose a switch system that will 1
not degrade the measurements. Current
Source

Use offset compensation 2

technique – current reversals – to


eliminate voltage offsets due to 3
the switch. V Voltmeter

Use same configuration to 4


Switch Matrix
measure the Hall voltage using
an electromagnet.
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High Resistance vdp Measurements

Model 7065 Hall Effect


Card Configuration

Matrix Card that switches


current source and
voltmeter to the 4 terminals
of the sample.

Has unity gain buffers on


the card to avoid problems
with isolation or needing to
use an electrometer to
measure the voltage drops

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Using Four SMUs to Measure High R Samples


Model 4200-SCS with 4 SMUs and 4 preamps
– Input impedance >1016 
– Accurate low current sourcing, pA SMU1 i SMU2
I Source
– No leakage errors due to V Measure
mechanical switches 1 2
– Includes software to automate V Difference
4 3
measurements and calculate
resistivity SMU4 SMU3
Common V Measure

Model 4200-SCS Semiconductor


Characterization System

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Making Good Measurements on High Resistance


Samples
• Use electrostatic shielding to minimize electrical interference
– Shield the DUT and all sensitive circuitry
– Use shielded cabling
– Connect the shield to the low terminal of the system

• Use guarding to reduce the effects of leakage current in system


– Guarded current source
– Guarded voltmeters
– Use triax cable instead of coax cable

• Allow sufficient settling time


– Source I and measure V as a function of time to determine appropriate
settling time
– A diamond sample can take several minutes for settling

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Settling Time of a 1012Ω Resistance Sample

Wait at least
20 seconds
for a settled
measurement

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Summary

Use an appropriate method for measuring the


resistivity. The method will depend on if the material is
a conductor, insulator, or semiconductor.

Choose the appropriate instrumentation.

Apply the proper measurement techniques to avoid


measurement errors.

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Reference Materials
www.keithley.com

Low Level Measurements Handbook, 6th


Edition

Application Notes: Hall effect, van der


Pauw method, four-point collinear probe
method, insulator resistivity, low voltage
measurements, low current
measurements, etc.

White Papers: Delta method, current


reversal techniques, etc.
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Contact Keithley for Further Information

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Outside the USA: +1-440-248-0400 Great Britain: (+44) 118 929 7500

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Additional offices: www.keithley.com Korea: (+82) 2-574-7778
Taiwan: (+886) 3-572-9077

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