VLSI Technology (Crystal Growth)

Czochralski Method of Crystal Growth Apparatus:

The apparatus used for CZ method of crystal growth is called puller having weight of 17,600 kg and is 6.5 m tall. The puller can hold a melt charge of 60 kg of Silicon, which can be transformed into a crystal of 100 mm diameter and 3.0 m length. The puller has 4 subsystems which are as follows: 1. Furnace: crucible, susceptor, rotation mechanism, heating element, power supply and chamber. 2. Crystal-pulling mechanism: seed shaft or chain, rotation mechanism and seed chuck. 3. Ambient control: gas source, flow control, purge tube and exhaust or vacuum system. 4. Control system: microprocessor, sensors and outputs. Furnace: It consist of crucible which contains the molten silicon, hence crucible material should be unreactive with molten silicon. This is a major consideration, because the electrical properties of silicon are sensitive to even ppb levels of impurities. Other characteristics of crucible material are a high melting point, thermal stability and hardness. The materials used
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VLSI Technology (Crystal Growth)

for crucible are Silicon Nitride (Si3N4) and fused Silica (SiO2), the latter of which is in exclusive use today. Fused Silica, however, reacts with the molten Silicon, releasing Silicon and Oxygen into the melt. Most of the Oxygen in the melt escapes by the formation of gaseous Silicon monoxide. The SiO condenses on the inside of the chamber, creating a cleanliness problem in the puller. The purity of Silica itself also affects the Silicon purity because the Silica can contain sufficient acceptor impurities to limit the upper values of the resistivity of the Silicon that is being grown. The susceptor is used to support the crucible. It also provides for better thermal conditions. Graphite is used because of its high temperature properties for susceptor. A high-purity, nuclear grade graphite is usually specified. This high purity is required to prevent the contamination in the crystal grown from impurities volatilized from the graphite. The susceptor rests on a pedestal whose shaft is connected to a motor that provides rotation. The whole assembly can usually be raised and lowered to keep the melt level equidistant from a fixed reference point, which is needed for automatic diameter control. The furnace structure must be airtight to prevent contamination from the atmosphere, and have a specific design that does not allow any part of the chamber to become so hot that its vapor pressure would be a factor in contaminating the crystal. To melt the charge, radio frequency or resistance heating is have been used. Induction heating is useful for small melt sizes, but resistance heating is used exclusively in large pullers. Crystal-pulling mechanism: The pull rate and crystal rotation are two parameters control through this process, so it must be with minimal vibration and great precision. Seed crystals are prepared to precise orientation tolerances and the seed holder and puling mechanism must maintain this precise orientation perpendicular to the melt surface. The crystal leaves the furnace through purge tube where ambient gas is directed along the surface of the crystal to cool it. From the purge tube crystal enters an upper chamber, which is usually separated from the surface by an isolation valve. Ambient control: CZ growth of Silicon must be conducted in an inert gas or vacuum because (i) (ii) The hot graphite must be protected from Oxygen to prevent erosion The gas around the process should not react with the molten Silicon.

Growth in a vacuum meets these requirements; it also has the advantage of removing SiO from the system thus preventing its buildup inside furnace chamber. Growth in gaseous atmosphere generally used for large growers, must use an inert gas such as He or Argon.

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VLSI Technology (Crystal Growth)

Control system: The control system provides control of process parameters such as temperature, crystal diameter, pull rate and rotation speeds. The sensor output is linked to the pulling mechanism and controls the diameter by varying pull rate. The trend in control system is to use digital, microprocessor based systems. Operation: The growth of a CZ crystal involves the solidification of atoms from a liquid phase at an interface. The speed of growth is determined by the number of sites the face of the crystal and specifics of heat transfer at the interface. The below figure shows the transport process and temperature gradient involved.

Fig: Temperature gradient, solidification and transport process in CZ method The heat transfer conditions about the interface can be modeled by the following equation:

-----------(1) Where L = latent heat of fusion; dm/dt = mass solidification rate; T= temperature; kl and ks are thermal conductivities of liquid and solid; dT/dx1 and dT/dx2 are thermal gradients at point 1 and 2; A1 and A2 are the area of isotherms at position 1 & 2. From equation 1 maximum pull rate of a crystal under condition of zero thermal gradient in the melt (i.e. dT/dx1=0 ) can be deduced. Converting the mass solidification rate to growth rate using density and area yields

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VLSI Technology (Crystal Growth)

Where Vmax = maximum pull rate and d is the density of solid Si. The below figure shows the experimentally determined temperature gradient in Si crystal

The pull rate influence the incorporation of impurities into the crystal and is a factor in defect generation. Generally, when the temperature gradient in the melt is small, the heat transferred to the crystal is the latent heat of fusion. As a result, the pull rate varies inversely with diameter. The pull rate obtained in practice is 30% to 50% slower than the maximum values suggested by theoretical consideration. Growth rate or growth velocity of the crystal is actually distinct from the pull rate. Pull rate is the macroscopic indication of the net solidification rate, whereas growth rate is the instantaneous solidification rate. The two are differ because of temperature fluctuations at interface. The growth rate can exceed pull rate or even be negative at a given time. When it is negative remelting is said to be occur. The growth rate influences the defect structure and dopant distribution in the crystal on a microscopic scale. Pull rate affects the defects properties in the following way: the condensation of the thermal point defects into small dislocation loops occurs as the crystal cools from the solidification temperature. This process occurs above 9500C. The number of defects depends upon cooling rate, which is function of pull rate and diameter at 9500C. A pull rate of 2 mm/min eliminates defect formation from quenching the point defects. A related phenomenon remelting can also be suppressed by attaining a pull rate of 2.7 mm/min which is half of Vmax.

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VLSI Technology (Crystal Growth)

Crystals in which remelt has not been suppressed exhibit impurity striation and defect swirls. As we know that every impurity has a solid solubility in Silicon. The impurity has different equilibrium solubility in the melt. For dilute solutions commonly encountered in Si growth, an equilibrium segregation coefficient k0 may be defined as k0= Cs/Cl where Cs and Cl are the equilibrium concentration of impurity in the solid and liquid near the interface respectively. The distribution of impurity in the growth crystal can be described mathematically by

Where X is fraction of melt solidified, C0 is initial concentration, Cs is solid concentration. The below figure illustrates the segregation behavior of several segregation coefficients. It is found experimentally that segregation coefficients differ from equilibrium values and it is necessary to define effective segregation coefficient constant ke

Where V is pull rate, D is diffusion coefficient of dopant in the melt, B is stagnant layer thickness.

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