Crystal Growth and Wafer Fabrication



Overview


After Mitsubishi, Dowa and ITTGasTek

The production of Gallium Arsenide (GaAs) semiconductors begins with crystal growth. There are many ways of growing GaAs single crystals, the most popular being the Liquid Encapsulated Czochralski (LEC) method. In the LEC method, there is a crucible loaded with gallium, arsenic and boric oxide. This crucible is placed in a pressure vessel. This vessel is evacuated, filled with argon and then pressurized. The temperature is raised within the vessel causing the gallium and arsenic elements to react and form gallium arsenide. As the temperature increases, the resulting gallium arsenide melts, as does the boric oxide. A seed is then dipped into the melt and slowly retracted creating a crystalline block that is often called an ingot or boule. After the ingot is completely retracted and cooled, individual wafers are sawed from the ingot. The wafers are then lapped, polished and ready for inspection. The completed wafers are inspected, packaged and finally shipped to a consumer. The consumer will put each wafer through various processes such as lithography, circuit design/mask creation, ion implantation and metallization in order to make the wafers into semiconductor devices. However, the process of creating a GaAs semiconductor can not occur without proper crystal growth and wafer fabrication, which begins with the Liquid Encapsulated Czochralski growth technique.

Crystal Growth


Source:Fullman Company

Crystal Pulling

The crystal growth begins after the melt temperature is stabilized. To initiate the single crystal growth, a seed made of GaAs with a (100) crystal orientation is lowered into the crucible. The pull shaft slowly lowers the seed into the crucible, through the boric oxide and into the melt. Throughout the process, the seed and crucible are rotated to reduce thermal gradients and to allow for more uniform ingot shapes [Williams]. As the seed makes contact to the melt and pulling begins, the neck of the crystal or ingot is formed by decreasing the ingot diameter below the diameter of the seed. The ingot diameter is then gradually increased to form the cone. The neck and cone play critical roles in reducing the dislocation density within the ingot. Finally, after the required diameter is achieved, the body of the ingot is grown maintaining the pulling rate.


Source:Fullman Company
Figure A

Source: Mitsubishi
Schematic of LEC Puller (Silicon)
Similar to GaAs LEC Puller

As one would predict, the ingot diameter increases as the pulling rate decreases and vice versa. Crystal pulling is not a trivial task; it is significantly affected by heat flux in the pressure vessel that can cause polycrystallinity. Other defects such as twins, dislocations and strains may occur as a result of thermal gradients or non-stoichiometric melts. However, these defects can be overcome. Once the ingot is grown to its desired length, it is annealed. Annealing is the process of heatingand slowly cooling in order to increase the strength and reduce the brittleness of the ingot. After annealing, the ingots are ready for grinding.


Courtesy of Semi
Movie shows LEC growth of Si ingot
Similar process for GaAs


Necking and Cone Angle

Necking is the process of reducing the seed diameter while pulling the seed from the melt. Dislocations are introduced to the crystal from the seed if the seed initially has dislocations. The dislocations can be transmitted from the seed to the crystal. This is the reason for necking the seed. When the seed is necked, the amount of dislocations that migrate to the crystal is reduced. Using a dislocation-free seed does not always prevent dislocations from forming in the crystal. However growing a cone after the neck reduces the amount of dislocations formed in the crystal. Figure A shows that etch pit density (EPD) decreases as cone angle increases, but only up to about 25 degrees. Beyond 25 degrees, the EPD stays approximately the same. As the cone is pulled from the melt, the dislocations start to increase, reach a maximum, and then decrease before reaching the maximum crystal diameter. With no cone, these dislocations would form in the body of the crystal and ruin the ingot. For cones with steep angles, the most dislocations occurr near the center of the cone. [Kirkpatrick]

Neck and Cone of the Ingot


Source:Fullman Company

Liquid Encapsulated Czochralski Growth

The wafers that ITT GaAsTek receives are semi-insulating gallium arsenide wafers. These wafers are cut from ingots of GaAs that are nearly intrinsic hence creating the semi-insulating quality of the wafers. These ingots, made by M/A-COM inc., are grown in a High Pressure Liquid Encapsulated Czochralski crystal puller (Figure A).


The process of growing ingots starts in a pyrolytic boron nitride crucible. The crucible is first loaded with exceedingly pure arsenic (As) and gallium (Ga) followed by a layer of boric oxide as seen in the picture below.

Source:Kirkpatrick

The crucible is then placed within a graphite heater in a stainless steel pressure vessel. The air in the vessel is then evacuated and back filled with argon Ar, an inert gas [M/A-COM Inc]. The gallium and arsenic compounding process begins by heating the crucible under an initial pressure of about 41 atmospheres. The Ga melts first and covers the As. As the temperature approaches 800 K the boric oxide melts and seals at the crucible wall, hence encapsulating the Ga and As charge. The compounding of Ga and As into GaAs (Galiquid +Assolid = GaAssolid) occurs rapidly while releasing heat at circa 1100 K under high argon pressures of about 70 atmospheres [Kirkpatrick]. The resulting GaAs melt is stoichiometric. The boric oxide and high vapor pressure defends against sublimation and evaporation of As. Without the high-pressure containment during compounding, control over the melt composition would be lost. The boric oxide also acts as a barrier to the melt, protecting it from contaminants in the crucible and the pressure vessel. After the melt temperature is stabilized, crystal growth begins.

Crystal Defects


Source:Park Scientific Instruments

Twins

There are some defects that occur when growing a crystal. The major defects are twins and dislocations. Twins can change the crystallographic orientation of the material as well as create large grain boundaries. Twinning can also lead polycrystallinity. Therefore, in order to achieve single-crystal wafers suitable for device fabrication, twinning must be eliminated. As it turns out, controlling the stoichiometry of the melt during the LEC growth can prevent twin formation in semi-insulating <100> GaAs crystals. Experiments show that using an undoped arsenic-rich melt, the probability of twinning decreased significantly thus allowing large diameter single crystals to be grown. Twinning is not correlated to other growth parameters [Kirkpatrick]. For gallium-rich melts, the probability for twinning increased significantly.


Dislocations and Etch Pit Density

Dislocations are defects in crystals that produce unsaturated bonds. Dislocations can cause all sorts of problems in wafer and device manufacturing. The main cause of dislocations is due to stress in the crystal caused by thermal gradients during crystal growth. Dislocation density can be quantified by counting etched pits created by etching wafer with potassium hydroxide. There is a direct relation between etch pit density (EPD) and dislocation density. These terms are used interchangeably [Williams]. There are many parameters that affect the amount of dislocations in the crystal including, cone angle and seed quality, boric oxide thickness, diameter control and melt stoichiometry. While pulling the seed, creating a neck and increasing the cone angle can reduce the amount of dislocations in the crystal.

Figure A


Source:Kirkpatrick


Experimental results also show that as the boric oxide layer is made thicker, the amount of dislocations decreases due to better heat flux and reduced thermal gradients. Diameter control also affects dislocation density. Good diameter control leads to lower dislocation densities. This result is much less pronounced than cone angle, seed quality and oxide thickness results. Melt stoichiometry also reduced the dislocation density when using an arsenic rich melt. Experimental results suggest using a As-rich melt composition of 0.505 to 0.535 for optimal reduction of dislocations. But like diameter control, the affects of melt stoichiometry on the dislocation density was less pronounced that of the others [Kirkpatrick].

Temperature Effects


After M/A-COM Inc.
Heat distribution during crystal growth


Heat Flux and Thermal Gradients

Heat flux plays a critical role during crystal growth. In order to grow a single crystal, the melt-solid interface must be maintained at a constant temperature of 1511 K, just below the melting point of GaAs. This allows for the melt to solidify onto the crystal. Since heat flux and isotherms are perpendicular to each other, analyzing the interface shape in figure A shows that significant heat flows from the crystal to the boric oxide layer. This can lead to polycrystallinity, hence reducing the heat flux into the boric oxide will produce a single crystal. Raising the boric oxide temperature close to the crystal temperature will reduce the heat flow rate from the crystal to the oxide layer. The resulting interface is seen in figure B, which will produce desirable long single crystals [Ware].

Figure A

Source:M/A-COM Inc.
Melt/crystal barrier leading to polycrystallinity
Figure B

Source:M/A-COM Inc.
Ideal melt/crystal barrier in producing single crystals


Steep temperature gradients are also established in GaAs crystals during LEC growth. Temperature gradients cause dislocation and can leave strains within the crystal. These strains can cause cracks in the crystal and render it useless. The strains are avoided by annealing the crystal before cutting, but dislocations are often still present. Dislocations decrease as the thermal gradients and heat flux decrease. Reducing thermal gradients is accomplished by heating the boric oxide layer (as explained above) or increasing the thickness of that layer. Figure C shows dislocation density (EPD) as a function of the boric oxide thickness.

Figure C

Source:Kirkpatrick

Dislocations at the front of the crystal drop significantly as the oxide layer thickness increases, but dislocations at the tail only drop slightly. However, as the boric oxide layer increases, the control over crystal diameter decreases [Kirkpatrick].

Grinding and Slicing


Source:Fullman Company

Grinding

Grinding is the process of rubbing two surfaces together to shape or sharpen an object with friction. In the case of a GaAs, there are two methods of grinding that take place. The first is known as surface grinding; the other is known as edge grinding.

Surface grinding is done to smooth the outer surface of the GaAs ingot. When the ingot comes out of the boule, the outside surface of the ingot is not uniform. Therefore, grinding is needed to shape the ingot as desired. In order to make the surface smooth the ingot is placed on a lathe and ground until its outer surface becomes smooth. Figure A shows the ingots after an ingot has been pulled out of the boule (left side) and after being smoothed on the lathe (right side).


Figure A

Source:DOWA



Texas Instruments
Grinding, Sawing and Polishing of Si ingot
Similar process for GaAs

Edge Grinding

Edge Grinding is the process in which " flats" are ground into the ingot. Flats are placed on the wafer to show the orientation of the crystal which helps to determine how the devices can be laid down on the wafer. In most situations, the flat on the wafer is in the <110> direction and the orientation of the crystal is in the <100> direction. Other things also depend on the orientation of the wafer, such as ion implantation and dry etching. That is why it is important to be consistent and precise when sawing and grinding the ingots. Most specification sheets that wafer manufacturers send out show that the wafers are oriented in the <100> direction but just off by a tenth of a degree. It turns out that this slight tilt allows for easier cutting of the wafer.

Sometimes two flats are ground on the ingot. Two flats make it even easier to determine the orientation of the crystal. The flat in the <110> direction is called the major flat. The minor flat is counter-clockwise from the major flat. This helps to determine the side with the best polish on it. The side with the best polish on it is known as the front side. The back side of a wafer has the minor flat clockwise from the major flat and is shown below in Figure B (Fullman).


Figure B

Source:Frieberger Compound Materials


Slicing

After the ingot’s outer surface has been smoothed out and taken off the lathe, the ingots need to be sliced into wafers. This is done by placing the ingot horizontally on a holder (Figure C) so that the holder can move the ingot up into the circular saw. This saw is commonly referred to as an "ID Saw" because its cutting edge of the blade is on the inside (Figure D). The "ID Saw" is notorious for producing a more precise cut as well as a wafer that is flatter (Fullman Company). The saws used to cut the ingot into wafers have a diamond blade or a blade made with a composite material that has diamonds in it (Williams). These saws cut wafers with a thickness of 625 micron. The wafers are thinned down later to approximately 100 micron. The wafers are sliced at 625 micron so that they aren’t as brittle as the 100 micron wafers when handling them (Figure E).

Figure C

Source:Mitsubishi
Figure D

Source:Fullman Company
Figure E

Source:ITT GaAsTek


Polishing and Inspection


Source:Fullman Company

Polishing

After the flats have been ground into the ingot and the wafers have been sliced, the wafers are lapped. Lapping is often done by applying a slurry of water and grit to the wafer. The grit is typically constructed of silicon carbide or alumina (Williams). This slurry helps to remove saw marks and to make the surfaces of the wafer more parallel. After lapping, the wafers are etched to remove surface damage done to the wafer by the previous process. Next, the wafers are polished. Polishing involves two or three steps of chemical processes. The wafers are also buffed with a slurry. Most (Fullman Company) companies use a polisher that polishes both sides of the wafers simultaneously. Figure F is a picture of a wafer polishing machine.

Figure F

Source:Speedfam


Inspection

When the wafers have been polished the next step is to inspect them for defects, such as particles and haze. Figure G (below) is an example of a machine that can perform the functions that are needed to inspect the wafers for such defects.

If the polished wafers pass inspection, they are packaged and sent off to the customers (like ITT GaAsTek). When the customer receives the shipment, the wafers are inspected to insure they meet each company's own standards. All companies check for defects, but also for brittleness. Since the wafers have to withstand the rest of the IC (Integrated Chip) manufacturing process, they must be strong. ITT GaAs Tek uses a test in which a machine places a Teflon ball on the wafer and presses down on the ball with the desired amount of weight. The Teflon ball keeps the wafer from being scratched. If the wafer handles the weight and does not crack, then it is passed on to the photolithography process. Most wafers that ITT GaAsTek obtains can handle up to 30 pounds of weight.

Figure G

Source:Tencor



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