ELEC 2005

Crystal Growth

Summer term
Fundamentals of Semiconductor Technology
16 July 2012

A Presentation On
ELEC 2005
P. Bhattacharyya
2
Outline
Process flow chart
Silicon crystal growth from the melt
Silicon float zone process
Material Characterization
Crystal Characterization
16 July 2012
ELEC 2005 3
Process Flow Chart
16 July 2012 P. Bhattacharyya
Starting
material
Polycrystalline
Semiconductor
Single crystal
Water
Distillation
and
reduction
Crystal
growth
Grind, saw
polish
2
SiO
Si
Fig 1: process flow chart
ELEC 2005
P. Bhattacharyya
4
Outline
Process flow chart
Silicon crystal growth from the melt
Silicon float zone process
Material Characterization
Crystal Characterization
16 July 2012
ELEC 2005 5
Silicon Crystal Growth From The Melt
16 July 2012
P. Bhattacharyya
Step 1: Starting material
The starting material for silicon is pure form of sand (SiO
2
).
Various forms of silicon( coal, coke) placed in furnace for reaction.
SiC(solid)+SiO
2
(solid) Si(solid)+SiO(gas)+Co(gas)
The reaction produces 98% pure metallurgical grade silicon (MGS).
The above silicon is pulverized and treated with HCL at 300
0
C.
Si(solid)+3HCL(gas) SiHCL
3
(gas)+H
2
(gas)
To convert MGS to EGS, hydrogen reduction reaction is done with SiHCL
3.
SiHCL
3
(gas)+H
2
(gas) Si(solid)+3HCL(gas)
This EGS have impurity concentration parts per billion range.





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Silicon Crystal Growth From The Melt Conti..
16 July 2012
P. Bhattacharyya
Step 2: Czochralski Technique
The apparatus used for this technique is called
crystal puller.
The puller has three main components.
a. Furnace
includes fused silicon crucible, a graphite
susceptor, a rotation mechanism (CW),
a heating element and a power supply.
b. Crystal pulling mechanism
includes seed holder a rotation mechanism
(CCW).
c. An ambient control
includes gas source (argon), a flow control,
an exhaust system
Also puller has microprocessor based control
system to control process parameter such as
temperature, crystal diameter, pull rate and
rotation speeds



Fig 2: Czochralski crystal puller
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Silicon Crystal Growth From The Melt Conti..
16 July 2012
P. Bhattacharyya
Step 2: Czochralski Technique Conti
In last of starting material we get EGS.
Now EGS is placed in crucible and furnace is
heated above melting temperature of silicon.
A seed crystal is suspended over crucible in a
seed holder.
The seed is inserted into the melt.
Part of it melts, but the tip of the remaining seed
crystal still touches the liquid surface.
Then seed crystal is slowly withdrawn.
Progressive freezing at the solid liquid interface
yields a large single crystal.
Fig 3: Czochralski crystal puller
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Silicon Crystal Growth From The Melt Conti..
16 July 2012
P. Bhattacharyya
Distribution of Dopant
In crystal growth a known amount of dopant is added to get desired doping
concentration in grown crystal.
For silicon , boron (p type ) and phosphorous (n type) are the most used dopant .
Different doping concentration is used for crystal (solid) and melt (liquid) at the
interface.
The ratio of solid doping concentration to the liquid doping concentration is known
as equilibrium segregation coefficient, k
0 .


l
S
C
C
k =
0
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Silicon Crystal Growth From The Melt Conti..
16 July 2012
P. Bhattacharyya
Distribution of Dopant Conti.
Consider a crystal having initial weight M
0
and initial doping concentration c
0
in the
melt . After certain growth ,weight of crystal is M and dopant remaining in melt is S.

Let for an incremental amount of the crystal dM , the corresponding reduction of
the dopant(-dS) from the melt is
(1)
Remaining weight of the melt M
0
-M and doping concentration C
1

.(2)
Combining equitation 1 and 2 an substituting C
s
/C
1
=k
0


..(3)
dM
S
C
dM dS
S
C =
M M
S
C

=
0
1
|
|
.
|

\
|

=
M M
k
0
0
dM
S
dS
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Silicon Crystal Growth From The Melt Conti..
16 July 2012
P. Bhattacharyya
Distribution of Dopant Conti.
Given initial weight of the dopant C
0
M
0
. We can integrate equitation 3

..(4)

Solving equitation 4 and combining with equation 2 gives

(5)
As crystal growth progresses , the composition initially at k
0
C
0
will increase
continually for k
0
<1 and decrease continually for k
0
>1.


} }

=
M S
M C
M
k
0 0
0
M
dM
S
dS
0 0
1
0
0 0
0
M
1

|
|
.
|

\
|
=
k
S
M
C k C
ELEC 2005 11
Silicon Crystal Growth From The Melt Conti..
16 July 2012
P. Bhattacharyya
Effective Segregation Coefficient
Effective segregation coefficient is the ratio of doping concentration in solid(C
S
) to
the impurity concentration far away fro the interface.


For k
0
>1 dopants are constantly rejected into the melt during crystal growing.
Dopant can be transported away by diffusion or stirring.
If the rejection rate is higher than the rate at which the dopant can be transported
away , then concentration gradient will develop at the interface.




1
C
C
k
S
e
=
ELEC 2005
P. Bhattacharyya
12
Outline
Process flow chart
Silicon crystal growth from the melt
Silicon float zone process
Material Characterization
Crystal Characterization
16 July 2012
ELEC 2005 13
Silicon Float Zone Process
16 July 2012
P. Bhattacharyya
The process used to grow silicon that has lower
contamination.
A high purity polycrystalline rod with a seed crystal
at the bottom is held in vertical position and rotated.
The rod is enclose in a quartz envelop within which
an inert atmosphere (argon ) is maintained.
A RF heater is used to kept molten a small portion
of crystal.
The molten silicon retained by surface tension
between the melting and growing solid silicon faces.

Fig 4: Float zone process set up
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Silicon Float Zone Process Conti..
16 July 2012
P. Bhattacharyya
The floating zone moves upward, single crystal
silicon freezes at the zone retaining end.
The crystal grows as an extension of seed crystal.
Higher resistivity can be obtained from this process.
No crucible is used by this process.
This process used for high power and high voltage
devices.

Fig 5: Float zone process set up
ELEC 2005
P. Bhattacharyya
15
Outline
Process flow chart
Silicon crystal growth from the melt
Silicon float zone process
Material Characterization
Crystal Characterization
16 July 2012
ELEC 2005 16
Material Characterization
16 July 2012
P. Bhattacharyya
Wafer Shaping
The first shaping operation is to remove the seed and other end of ingot.
Then grind the surface of ingot so that diameter of the material is defined.
After that, one or more flat regions are ground along the length of the ingot.
The largest flat also called primary flat , used for device orientation.
The secondary flat regions are the specific orientation of the crystal and also used
to recognize the conductive type of the crystal .
The ingot is now ready for sliced by diamond saw into wafers.
Slicing determines four wafer parameter.
1. Surface orientation : (e.g., <111>or <100>)
2. Thickness: (e.g., 0.5-0.7mm)
3. Taper: Wafer thickness variation from one end to other end.
4. Bow: Surface curvature of the wafer from center of the wafer to the edge.


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Material Characterization
16 July 2012
P. Bhattacharyya
Wafer Shaping Conti..
After slicing, both sides of the wafer are lapped using mixture of Al
2
O
3



and

glycerin.
Due to lapped process the surface and edges of the wafer damages and
contaminated.
The chemical etching is done to remove the damages an contaminated.
The final step is polishing to provide a smooth and specular surface.
ELEC 2005
P. Bhattacharyya
18
Outline
Process flow chart
Silicon crystal growth from the melt
Silicon float zone process
Material Characterization
Crystal Characterization
16 July 2012
ELEC 2005 19
Crystal Characterization
16 July 2012
P. Bhattacharyya
Crystal Defects
Four type of crystal defects are a) point defects b) line defects c) area defects
d) volume defects

a) Point Defects
Any foreign atom incorporated into the lattice at either a substantial site or an
interstitial site is a point defect.


Substantial
impurity
Interstitial
impurity
Lattice
Vacancy
Frenkel type
defects
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Crystal Characterization Conti..
16 July 2012
P. Bhattacharyya
Crystal Defects Conti..
b) Line Defects :
Also called dislocation. Two types of line defects are edge defects and screw
defects. In case edge defects line of the dislocation would be perpendicular to
the plane of the edge. The screw line defects produced by cutting crystal
partway through and pushing upper part one spacing over.
c) Area Defects :
Twining boundaries: a change in the crystal orientation across a plane.
Grain boundary: no particular orientation relationship in the crystal.
Stacking fault: stacking sequence of an atomic layer is interrupted

d) Volume Defects :
These defect arise because of the inherent solubility of the impurity in the host
lattice. The volume mismatch between host lattice and participates results in
dislocation.
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Conclusion
16 July 2012
P. Bhattacharyya
So, throughout this presentation two crystal growth techniques , material
characterization and crystal defects are discussed.
For silicon single crystal sand (SiO
2
) is starting material, which is converted
to polycrystalline silicon to use as raw material for Czochralski techniques.
Float zone process offers lower contamination.
Float zone crystals are used for high power and high voltage devices where high
resistivity material are required .
After crystal grown , it goes for wafer shaping operation to give an end product of
highly polished wafer.
ELEC 2005
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