Czochralski Process

The Czochralski process is a method of crystal growth used to obtain single crystals of semiconductors (e.g), metals (e.g. palladium, platinum, silver, gold), salts and many oxide crystals ( LaAlO3, YAG, .and GGG etc ) The most important application may be the growth of large cylindrical ingots, or boules, of single crystal silicon. High-purity, semiconductor-grade silicon (only a few parts per million of impurities) is melted down in a crucible , which is usually made of Quartz. Dopant impurity atoms such as boron or phosphorus can be added to the molten intrinsic silicon in precise amounts in order to dope the silicon, thus changing it into n-type or p-type extrinsic silicon. This influences the electrical conductivity of the silicon. A seed crystal, mounted on a rod, is dipped into the molten silicon. The seed crystal's rod is pulled upwards and rotated at the same time. By precisely controlling the temperature gradients, rate of pulling and speed of rotation, it is possible to extract a large, single-crystal, cylindrical ingot from the melt. This process is normally performed in an inert atmosphere, such as argon, and in an inert chamber, such as quartz.

Crucibles used in Czochralski method

Crucible after being used

Silicon wafer with mirror finish (NASA) While the largest silicon ingots produced today are 400 mm in diameter and 1 to 2 metres in length, 200 mm and 300 mm diameter crystals are standard industrial processes. Thin silicon

wafers are cut from these ingots (typically about 0.75 mm thick) and polished to a very high flatness to be used for creating integrated circuits. Other semiconductors, such as gallium arsenide, can also be grown by this method, although lower defect densities in this case can be obtained using variants of the Bridgeman technique. When silicon is grown by the Czochralski method the melt is contained in a silica (quartz) crucible. During growth the walls of the crucible dissolve into the melt and Czochralski silicon therefore contains oxygen impurities with a typical concentration of 1018cm 3. Perhaps surprisingly, oxygen impurities can have beneficial effects. Carefully chosen annealing conditions can allow the formation of oxygen precipitates. These have the effect of trapping unwanted transition metal impurities in a process known as gettering. Additionally, oxygen impurities can improve the mechanical strength of silicon wafers by immobilising any dislocations which may be introduced during device processing. It has experimentally been proved in the 1990s that the high oxygen concentration is also beneficial for radiation hardness of silicon particle detectors used in harsh radiation environment ( eg. CERN's LHC/S-LHC projects) [1,2,3]. Therefore, radiation detectors made of Czochralski- and Magnetic Czochralski-silicon are considered to be promising candidates for many future high-energy physics experiments [5,6]. Occurrence of unwanted instabilities in the melt can be avoided by investigating and visualizing the temperature and velocity fields during the crystal growth process [4]. The process is named after Jan Czochralski, who discovered the method in 1916 while investigating the crystallization rates of metals. [edit]
References 1. 2. 3. 4. 5. 6. Z. Li et al., IEEE Trans Nucl. Sci. 39 (6) (1992) 1730. A. Ruzin et al., IEEE Trans Nucl. Sci. 46 (5) (1999) 1310. G. Lindstrm et al., Nucl. Instr. and Meth. A 466 (2001) 308 and cited literature therein. J. Aleksic et al., Ann. of NY Academy of Sci. 972 (2002) 158. CERN RD50 Status Report 2004, CERN-LHCC-2004-031 and LHCC-RD-005 and cited literature therein. J. Hrknen et al., Nucl. Instr. and Meth. A 541 (2005)202.

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Aside from the need to be single-crystalline in nature, silicon substrates must also have a high degree of chemical purity, a high degree of crystalline perfection, and high structure uniformity.

The acquisition of such high-grade starting silicon material involves two major steps: 1) refinement of raw material (such as quartzite, a type of sand) into electronic grade polycrystalline silicon (EGS) using a complex multi-stage process; and 2) growing of single-crystal silicon from this EGS either by Czochralski or Float Zone process. Czochralski Crystal Growth Czochralski (CZ) crystal growth, so named in honor of its inventor, involves the crystalline solidification of atoms from a liquid phase at an interface. The basic CZ crystal growing process is more or less still the same as what has been developed in the 1950's. CZ crystal growing consists of the following steps. 1) A fused silica crucible is loaded with a charge of undoped EGS together with a precise amount of diluted silicon alloy. 2) The gases inside the growth chamber are then evacuated. 3) The growth chamber is then back-filled with an inert gas to inhibit the entrance of atmospheric gases into the melt during crystal growing. 4) The silicon charge inside the chamber is then melted (Si melting point = 1421 deg C). 5) A slim seed of crystal silicon (5 mm dia. and 100-300 mm long) with preciseorientation tolerances is introduced into the molten silicon. 6) The seed crystal is then withdrawn at a very controlled rate. The seed crystal and the crucible are rotated in opposite directions while this withdrawal process occurs.

Fig. 1. Examples of Czochralski Pullers

Single Crystal Growing for Wafer Production (Page 2 of 2) <Back to Page 1>

Float Zone Crystal Growth The float zone (FZ) process is another method for growing single-crystal silicon. It involves the passing of a molten zonethrough a polysilicon rod that approximately has the same dimensions as the final ingot. The purity of an ingot produced by the FZ process is higher than that of an ingot produced by the CZ process. As such, devices that require ultrapure starting silicon substrates should use wafers produced using the FZ method. The FZ process consists of the following steps.

1. A polysilicon rod is mounted vertically inside a chamber, which may be under vacuum or filled with an inert gas. 2. A needle-eye coil that can run through the rod is activated to provide RF power to the rod, melting a 2-cm long zone in the rod. This molten zone can be maintained in stable liquid form by the coil. 3. The coil is then moved through the rod, and the molten zone moves along with it. 4. The movement of the molten zone through the entire length of the rod purifies the rod and forms the nearperfect single crystal. FZ growing equipment can also use a stationary coil, coupled with a mechanism that can move the silicon rod through it.

Fig. 2. Examples of Float Zone Crystal Growing Equipment After the single-crystal silicon ingot has been manufactured, it undergoes a routine evaluation of its resistivity, impurity content, crystal perfection, size and weight. It is thenground using diamond wheels to make it a perfect cylinder that has the right diameter. It then undergoes an etching process to remove the mechanical imperfections left by the grinding process.

Fig. 3. A Single-Crystal Silicon Rod The cylindrical ingot is then given one or more 'flats' by another round of grinding. The largest flat, called the primary flat, is used by automated wafer handling systems for alignment. Flats (primary and secondary) are also used to identify the crystallographicorientation and conductivity of the wafer.

The ingot is then sawn into thin wafer slices, each of which will be subjected to furtheretching and polishing until it is ready for use as substrates for VLSI fabrication. The above process of silicon growing, grinding, shaping, sawing, etching, and polishing to produce input wafers is known as wafering.

Fig. 4. An ingot slicer (left) and a wafer grinder/polisher (right)