Four Probe Method
(Measurement of Resistivity & Energy Band Gap of Germanium)
Solid States Lab
( MSc Physics Semester 1)
Submitted By -
1) Dhritiraj Das (Ramjas College)
DUIC - 24056031
2) Heena Panwar (Dept of Physics, University of Delhi)
DUIC - 24222072
3) Monika (Dept of Physics, University of Delhi)
DUIC - 24222193
4) Subhjeet Biswas (Dept of Physics, University of Delhi)
DUIC - 24222160
Electrical Conduction in Solids
The electrical properties of semiconductors involve the motion of charged particles
within them. Therefore, we must have an understanding of the forces which control
the motion of these particles. It is, of course, the physical structure of the solid
which exerts their control. This topic is very large, and hence only the high lights will
be covered. The reader is referred to many excellent sources which are listed at the
end, for more details on specific aspects.
Atoms, of which a solid is composed, consist of positively charged nuclei with
electron orbiting around them. The positive charge is compensated by negatively
charged electrons, so that a complete atom is electrically neutral. Electrons are
arranged in shells, and the closer they are to the nucleus the more strongly they are
bound. If we take the particular case of silicon, a well known semiconductor, we find
that it has 14 electrons which are accommodated in the shells as (1S)2, (2S)2,
(2P)6, (3S)2, (3P)2. Since the third shell is not even half filled, the 4 electrons are
available for chemical binding giving silicon a valency of four. (Germanium also has
a chemical valency of 4, but from the fourth shell). Fig. 1 shows an energy diagram
of an individual atom.
Let us now concentrate our attention on solids, if we bring many atoms close to one
another, interatomic forces become quite strong as electronic orbits begin to
overlap. The outer shell electrons play an important role, because their orbits are
the most disturbed. These electrons are no longer associated with a particular
atom, the outer shell electron may make an orbit around one atom and continue
about another. In this fashion, the outer shell or valency electrons are continually
traded among atoms and wander all over the solid. The continuous interchange of
valence electrons between atoms holds the solid together. This is the predominant
type of bonding in silicon and germanium, and is called the valence bonding.
In solids, atoms are usually arranged in a regular way to achieve a dense packing
and thereby form a crystal. The arrangement has very desirable characteristics, i.e.
the transport of holes and free electrons is very smooth in these structures. When
the arrangement is not crystalline complication arise. Here we will be concerned
only with the properties of perfect crystals. Silicon and germanium (and carbon)
crystallize with an identical crystal structure, the called diamond structure. Such a
structure is shown in fig. 2 The arrangement of atoms in the illustration form a Unit
Cell, and the crystal is made up of adjacent unit cells. Fig. 3 shows a potential
diagram of an array of atoms. An actual crystal is of course there dimensional. The
most important difference between the potential plot of an isolated atom and one
dimensional array is the splitting of energy levels. In fact, bringing N atoms together
we find 'N' times as many levels throughout the crystal. The spreading of energy
level depends on the degree of interaction, therefore, the inner orbits split into
levels combined in a narrow energy than the outer ones. As a result of the
interaction between the tremendous number of atoms in crystal (1022 per cm3), the
energy level found in isolated atoms will be split and form bands of allowed
energies which contain almost continuum of levels. Accordingly, electrons are
located in energy bands in crystalline solid. The band which contains the valence
electrons is called the valence band. The unoccupied energy levels also split up
and form another band called the conduction band. The interaction between the
unused shells is very large and they spread widely. Therefore, while there is a
bandgap, Eg (or forbidden region) between the valence and conduction bands,
splitting of higher orbit is so wide that they usually overlap. The bands below the
energy gap Eg are completely filled at absolute zero temperature and the
conduction band is empty. This is a very important point and has direct
consequences on the conduction properties, as we shall see soon. The
fundamental theory is that current conduction is not possible in empty and filled
bands. The reasons about the empty band is obvious since current is not possible
without carriers. The reason about the filled band is as follows : though the valence
electrons move about the crystal but they can not be accelerated because the
acceleration means gain of energy and there are no higher energy levels available
to which they could rise. We can now readily see that the crystal band structure
shown in Fig. 3 does not allow current conduction at T=0. If we increase the
temperature, however, thermal agitation increases and some valence electron will
gain energy greater than Eg and jump into the conduction band. The electron in the
conduction band is called a free electron, and its former place in the valence band
is called a hole. Electrons in conduction band can gain energy when a field is
applied, because there are many higher energy states available. The fact that
electrons left the valence band leaves some empty energy levels, this allows
conduction in the valence band as well. Electrons can now gain energy in the
valence band also, and we observe a motion of holes in the direction of the field.
Because of this we begin to speak of a hole as a current carrying particles.
According to the proceeding theory, an insulator must have a large bandgap, so
that at room temperature the conduction band is practically empty and the valence
band is practically filled and a semiconductors must have a narrower band gaps so
that appreciable number of carriers are present in the valence and conduction
bands at room temperature. In metals, however, the valence and conduction bands
overlap and application of an electric field can, therefore, accelerate a great sea of
electrons. The non-existence of a bandgap make conduction in metal almost
independent of temperature, as compared to semiconductors. Fig. 4 summarizes
the above points. The fact that electrons can be found in energy bands within a
crystal and other conclusions mentioned so far can be shown by quantum
mechanical calculations also which we shall not carry out here, but will use the
results for quantitative analysis.
Four Probe Method
Many conventional methods for measuring resistivity are unsatisfactory for
semiconductors because metal-semiconductor contacts are usually rectifying in
nature. Also there is generally minority carrier injection by one of the current
carrying contacts.
An excess concentration of minority carriers will affect the potential of other
contacts and modulate the resistance of the material. The method described here
overcomes the difficulties mentioned above and also offers several other
advantages. It permits measurements of resistivity in samples having a wide variety
of shapes, including the resistivity of small volumes within bigger pieces of
semiconductor. In this manner the resistivity of both sides of p-n junction can be
determined with good accuracy before the material is cut into bars for making
devices. This method of measurement is also applicable to silicon and other
semiconductor materials.
The basic model for all these measurements is indicated in Fig. 5. Four sharp
probes are placed on a flat surface of the material to be measured, current is
passed through the two outer electrodes, and the floating potential is measured
across the inner pair. If the flat surface on which the probes rest is adequately large
and the crystal is big the semiconductor may be considered to be a semi-infinite
volume. To prevent minority carrier injection and make good contacts, the surface
on which the probes rest, maybe mechanically lapped. The experimental circuit
used for measurement is illustrated schematically in Fig. 6. A nominal value of
probe spacing which has been found satisfactory is an equal distance of 2.0 mm
between adjacent probes. This permits measurement with reasonable current of n-
type or p-type semiconductor from 0.001 to 50 ohm. Cm.
In order to use this four probe method in semiconductor crystals or slides it is
necessary to assume that :
1. The resistivity of the material is uniform in the area of measurement.
2. If there is minority carrier injection into the semiconductor by the current -
carrying electrodes most of the carriers recombine near the electrodes so that their
effect on the conductivity is negligible. (This means that the measurements should
be made on surface which have a high recombination rate, such as mechanical
lapped surfaces).
3. The surface on which the probes rest is flat with no surface leakage.
4. The four probes used for resistivity measurements contact the surface at points
that lie in a straight line.
5. The diameter of the contact between the metallic probes and the semiconductor
should be small compared to the distance between probes.
6. The boundary between the current-carrying electrodes and the bulk material is
hemispherical and small in diameter.
7. The surfaces of the semiconductor crystal may be either conducting or
nonconducting.
(a) A conducting boundary is one on which a material of much lower resistivity than
semiconductor (such as copper) has been plated.
(b) A non-conducting boundary is produced when the surface of the crystal is in
contact with an insulator.
Formula Used :
Resistivity of a semiconductor is
𝜌 = 𝐴 exp*( 𝐸𝑔 /2𝑘𝐵𝑇 )
Where Eg is Band Gap in eV
kB is Boltzman constant =8.617*10-5 eVK-1 and
T is absolute Temperature.
Apparatus Required -
1. Probes Arrangement : It has four individually spring loaded probes, coated with
Zn at the tips. The probes are collinear and equally spaced. The Zn coating &
individual spring ensure good electrical contacts with the sample. The probes are
mounted in a teflon bush which ensures good electrical insulation between the
probes. A teflon spacer near the tips is also provided to keep the probes at equal
distance. The whole arrangement is mounted on a suitable stand and leads are
provided for current and voltage measurements.
2. Sample : Ge or Si crystal in the form of a chip/slice
3. Oven : It is a small oven for the variation of temperature of the crystal from room
temperature to about 200 °C.
4. Four Probes Set-up : (Measuring Unit) - It has three subunits all enclosed in
one cabinet. (i) Multirange Digital Voltmeter In this unit intersil 3½ digit single chip
A/D converter ICL 7107 has been used. It has high accuracy, auto zero to less than
10 µV, zero drift-less than 1 µV/°C, input bias current of 10 pA and roll over error of
less than one count. Since the use of internal reference causes the degradation in
performance due to internal heating, an external reference has been used.
SPECIFICATION Range : X 1 (0 - 200.0 mV) & X 10 (0 - 2.000 V) Resolution : 100
µV at X 1 range Accuracy : ± 0.1% of reading ± 1 digit Impedance : 10 M ohm
Display : 3½ digit, 7 segment, LED (12.5 mm height) with auto polarity and decimal
indication. Overload Indicator : Sign of 1 on the left and blanking of other digits.
(ii) Constant Current Generator - It is a IC regulated current generator to provide
a constant current to the outer probes irrespective of the changing resistance of the
sample due to change in temperatures. The basic scheme is to use the feedback
principle to limit the load current of the supply to preset maximum value. Variations
in the current are achieved by a potentiometer included for that purpose. The
supply is a highly regulated and practically ripple free d.c. source. The current is
measured by the digital panel meter.
SPECIFICATION Open circuit voltage : 18 V Current range : 0 - 20 mA Resolution :
10 µA Accuracy : ± 0.25% of the reading ±1 digit Load regulation : 0.03% for 0 to
full load Line regulation : 0.05% for 10% changes
(iii) Oven Power Supply - Suitable voltage for the oven is obtained through a
step down transformer with a provision for low and high rates of heating. A glowing
LED indicates when the oven power supply is 'ON'.
Experimental Procedure -
1. Put the sample on the base plate of the four probe arrangement. Unscrew the
pipe holding the four probes and let the four probes rest in the middle of the
sample. Apply a very gentle pressure on the probes and tighten the pipe in this
position. Check the continuity between the probes for proper electrical contacts.
CAUTION :
The Ge crystal is very brittle. Therefore, use only the minimum pressure required
for proper electrical contacts.
2. Connect the outer pair of probes (red/black) leads to the constant current power
supply and the inner pair (yellow/green leads) to the probe voltage terminals.
3. Place the four probe arrangement in the oven and fix the thermometer in the
oven through the hole provided.
4. Switch on the ac mains of Four Probe Set-up and put the digital panel meter in
the current measuring mode through the selector switch. In this position LED facing
mA would glow. Adjust the current to a desired value (Say 5 mA).
5. Now put the digital panel meter in voltage measuring mode. In this position LED
facing mV would glow and the meter would read the voltage between the probes.
6. Connect the oven power supply. Rate of heating may be selected with the help
of a switch - Low or High as desired. Switch on the power to the Oven. The glowing
LED indicates the power to the oven is 'ON'.
Case I: Resistivity Measurements on a Large Sample: We assume that the metal
tip is infinitesimal and samples are semi infinite in lateral dimensions. For bulk
samples where the sample thickness, W >> S , the probe spacing, we assume a
spherical protrusion of current emanating from the outer probe tips.
The resistivity is computed to be 𝜌𝑜 = ( 𝑉/ 𝐼 ) ∗ 2𝜋𝑠 where V = floating potential
difference between the inner probes, unit: volt 𝐼 =current through the outer pair of
probes, unit: ampere s = spacing between point probes, unit: meter ρ0 = resistivity,
unit: ohm meter
Case II: Resistivity Measurements on a Thin Slice-Nonconducting Bottom
Surface:
𝜌 = 𝜌0/ [𝐺7( 𝑤/𝑠)].
For the case of a nonconducting bottom on a slice the resistivity is computed from
Observations -
Graphs -
Result: 1.
1) The temperature dependence of the resistivity of semiconductor (germanium)
chip is as shown in the graph (2) . The resistivity decreases exponentially with the
increase in T. That is as at low temperatures resistivity is more and at high
temperatures the resistivity is less.
2. The energy band gap for the given semiconductor (germanium) is = ……eV.
Precautions:
1. The surface of the semiconductor should be flat.
2. All the four probes should be collinear.
3. The adjustment of 4-point probes should be done gently, as the semiconductor
chip is brittle.
4. The voltage should be measured using inner probes only using a high
impedance millivoltmeter.
5. Temperature of the oven should not exceed the limits set by the manufacturer of
the probes and chip.
