Abstract:
Computer controlled quality control methods for manufacturing high purity polycrystalline granules are introduced. Polycrystalline silicon granules are sampled and converted into single crystal specimen in computer controlled system, eliminating the need of human operator in controlling the processing parameters. Single crystal silicon test samples, then characterized by FTIR and other standard analysis, are therefore more representative of the starting granular silicon.

Description:
CROSS-REFERENCE 
       [0001]    Priority is claimed from the U.S. provisional application No. 61/154,630, filed on Feb. 23, 2009 and the U.S. provisional Application No. 61/154,927, filed on Feb. 24, 2009, both which are hereby incorporated by reference in their entirety. 
     
    
     TECHNICAL FIELD 
       [0002]    This Application is directed, in general, to a process of silicon manufacturing and, more specifically, to a silicon micro-puller used for a conversion of polycrystalline silicon granules to monocrystaline silicon samples, as necessary for optical analysis. 
         [0003]    BACKGROUND 
         [0004]    Ultra-pure polysilicon is used in the semiconductor industry as the starting material for the growth of single crystals, from which then wafers are produced by grinding, slicing, lapping and polishing steps. Conductive polysilicon also finds applications as gate material for MOSFET and CMOS structures. 
         [0005]    Before the large scale growth of single crystal Silicon ingots, the concentration levels of contaminants and dopants (such as Carbon, Boron, Phosphorus, Arsenic) in the polycrystalline starting material has to be known. Then the controlled addition of dopants to the silicon melt can be achieved. 
         [0006]    Current standard practices for production control, quality assurance and material research is by Float-Zone Crystal Growth and Melter-Zoner Spectroscopies. See ASTM documents F 1708-96  “Standard Practice for Evaluation of Granular Polysilicon by Melter - Zoner Spectroscopies; ” F 1723-96  “Standard Practice for Evaluation of Polycrystalline Silicon Rods by Float - Zone Crystal Growth and Spectroscopy; ” F 1630-95  “Standard Test Method for Low Temperature FT - IR Analysis of Single Crystal Silicon for III - V impurities; ” F 1389-92  “Standard Test Methods for Photoluminescence Analysis of Single Crystal Silicon for III - V impurities; ” F 1391-93  “Standard Test Method for Substitutional Atomic Carbon Content of Silicon by Infrared Absorption. ” The cited documents are contained e.g. in the 1998 Annual Book of ASTM Standards, Volume 10.05 Electronics (II). These documents are hereby incorporated by reference in their entirety. 
         [0007]    The Document F 1723-96 “Standard Practice for Evaluation of Polycrystalline Silicon Rods by Float-Zone Crystal Growth and Spectroscopy,” applies to the treatment and test of polycrystalline silicon rods as produced by the Siemens Process. This process does not yield polycrystalline Si pebbles but large polycrystalline cylinders. Small diameter cylinders have to be cut and converted to single crystal by a process which is physically identical to the conversion of polysilicon pebbles. The applied test methods are then also identical. 
         [0008]    The current standard quality control for manufacturing granular polysilicon uses the Float-Zone Crystal Growth method which takes place in a vertical quartz tube under flowing high purity argon. The silicon is inductively heated to the melting point using a microwave generator and an rf coil surrounding the quartz tube. 
         [0009]    Briefly, samples of granular polysilicon pebbles are placed into the quartz tube of a Melter-Float Zone Apparatus in which the granular pebbles rest on a polytetrafluoroethylene (“PTFE”) plunger-diffuser. The tube is filled with polysilicon pebbles until the top of the pebble charge comes close to the lower part of the RF coil. A silicon pedestal is mounted on the upper chuck and centered within the quartz tube. The position of the whole carriage is manually adjusted so that the silicon pedestal extends into the rf coil. 
         [0010]    Argon gas is first blown at higher flow rate through the PTFE plunger-diffuser to replace the oxygen in the quartz tube. The flow rate is later adjusted to a value just sufficient enough that only the top layer of granules is fluidized. 
         [0011]    A hydrogen-air torch placed outside the quartz tube is ignited to heat the silicon pedestal to a temperature sufficiently high so that the electrical conductivity is raised until the silicon couples with the radio frequency (RF) field. An RF power coil is first turned to 80% of the operating power needed for melting silicon. Once the pedestal is observed to glow the torch is manually turned off and removed, and the RF power is manually increased until the bottom of the pedestal melts. 
         [0012]    The PTFE plunger is manually moved until the fluidized silicon pebbles at the top of the pebble column touch the liquid end of the pedestal and go into solution. As the Si granules melt into the pedestal and the melt volume increases, the operator starts moving the entire carriage upward. The upper boundary of the liquid Si moves out of the working zone of the RF coil. Silicon crystallizes and forms the consolidated polysilicon rod. 
         [0013]    The PTFE plunger-diffuser is then removed and a single crystal silicon seed (2.5×2.5×100 mm) (typically &lt;100&gt; oriented) is mounted in the lower chuck and the shaft is reinstalled. The lower shaft is manually moved upward until the seed crystal is about 5 mm below the tip of the consolidated polysilicon rod previously produced. The entire tube is purged with argon gas. 
         [0014]    The hydrogen torch is manually ignited while the RF power is set at 80% of the power needed to melt silicon. When the bottom of the consolidated polysilicon rod begins to glow indicating RF coupling, the torch is turned off and removed. The RF power is increased until the bottom of the consolidated rod is molten. The single crystal silicon seed is then manually raised to penetrate into the melt and is held in this position until thermal equilibrium is established between the tip of the seed, the melt, and the bottom of the consolidated polysilicon rod. 
         [0015]    Typically, an optimum RF power for the one-pass zone leveling process needs to be experimentally established. Next the motorized carriage movement is initiated. Moving the carriage downward, the liquid zone is moved upward and single crystal silicon growth is occurring. 
         [0016]    The appearance of four growth facet lines for the case of &lt;100&gt;-oriented seeds indicate single crystalline growth. 
         [0017]    When a sufficiently long Si single crystal has been grown, the lower chuck is manually moved downward to separate the grown single crystal from the melt. 
         [0018]    After a visual inspection of the harvested single crystal silicon one or several 2 to 4 mm thick slices are cut from specified locations and submitted to low temperature FTIR analysis and other standard analyses. 
         [0019]    Highest purity silicon has a background contamination level down to 1×10 12  per cubic centimeter, corresponding to an electrical conductivity of approximately 1 E4 ohm cm. In order to achieve full sensitivity of the available optical tests, such as low temperature FTIR, photoluminescence etc., required for these low concentration, the single crystal quality has to be as high as possible. 
         [0020]    The prior art manually-operated process often produces insufficient control of the growth environment and growth conditions (gas pressure, gas flow rate, temperature, growth rate i.e. movements of the seed crystal and the polycrystalline source material). Moreover, stresses and defects in the single crystal render the optical low temperature tests less sensitive. 
       SUMMARY 
       [0021]    In one preferred embodiment, small samples of polycrystalline semiconductor granules are taken from the production stream and are tested in a computer controlled quality control system wherein the granules are first consolidated into a polycrystalline rod. 
         [0022]    In another preferred embodiment, the consolidated polycrystalline semiconductor rod is further converted into a single crystal using a computer controlled micro-pulling machine. 
         [0023]    In another preferred embodiment, the computer controlled consolidation process and the computer controlled micro-pulling are performed in the same machine in situ. 
         [0024]    In another preferred embodiment the computer controlled consolidation process and the computer controlled micro-pulling process are performed in two separate machines in a coordinated fashion. The resulting single crystal samples are submitted to highly sensitive tests, e.g. FTIR, IR spectroscopy and others, for determination of contamination levels. 
         [0025]    In another preferred embodiment, previously used processing parameters are stored in the computer of the micro-pulling system for later use and analysis. A touch screen may be used to display the status of the process parameters. Parameters may be changed either by direct input commands to the touch screen or through other user interfaces, such as internet connection, at remote terminals. Remote terminals may also be used for process monitoring. 
     
    
     
       BRIEF DESCRIPTION 
         [0026]    Reference is now made to the following descriptions taken in conjunction with the accompanying drawings, in which: 
           [0027]      FIG. 1  presents a overview drawing of an example system in accordance with the present application. 
           [0028]      FIG. 2  shows a cross sectional drawing of the process quartz tube and attached components. The numbers refer to the List of Assigned Numbers which identifies these components by name. The insert  FIG. 2B  shows poly-silicon granules  257  supported by plunger  255 , within the argon gas purged quartz tube  213 . 
           [0029]      FIG. 3A  shows a cross sectional view of details of the components at the upper end of the quartz process tube: the base mount, the shaft guide in elevated position, and associated seals etc. as an example system in accordance with the present application. 
           [0030]      FIG. 3B  shows a cross sectional view of the upper components, adding the clamp  233  shown in the applied position which is used when the shaft guide and the base mount are to be pressed together in accordance with the present application. 
           [0031]      FIG. 4A and 4B  show cross-sectional side and top views of an example process tube, encircled by the rf-heating coil  211  and with the susceptor  271  in engaged and disengaged positions in accordance with the present application. 
           [0032]      FIG. 5  shows a schematic view of an example of the organization of the various components used for the Process Control of the whole System, organized in  6  drawers, and the CPU  515  and the automated rf matching network  215 , in accordance with the present application. 
           [0033]      FIG. 6  shows a schematic view of an example Ambient Control, to control gas pressure, gas flow, fluid flow, with components placed in identified drawers, in accordance with the present application. 
       
    
    
     DETAILED DESCRIPTION 
       [0034]    Generally, the present application discloses new approaches to the quality control process for manufacturing high purity polycrystalline semiconductor granules, such as by using computer control, for a consolidation process as well as a micro-pulling process. 
         [0035]    It is contemplated and intended that the system design applies to both single crystal growth from granular polysilicon pebbles and to single crystal growth from other polysilicon samples, for example, polysilicon samples cut from large polysilicon rods, for the process of quality control. 
         [0036]    The disclosed innovations, in various embodiments, provide one or more of at least the following advantages. However, not all of these advantages result from every one of the innovations disclosed.
       Improved precision of test results resulting in tighter process control   Higher reproducibility;   Faster turn around time.   Reduced learning curve for entry level operators.       
 
         [0041]    These factors can contribute to yield improvements for the process of mass production of granular silicon. 
         [0042]    Generally, when silicon is heated it reacts with water vapor or oxygen to form a surface layer of silicon dioxide. Pure silicon is a solid with the same crystalline structure as diamond. It has a melting point of 2570° F. (1410° C.). The high melting temperature provides a challenge for consolidating and converting polysilicon into single silicon crystal. The conversion process must be performed in an oxygen and water free environment and the temperature must be precisely controlled at all time. 
         [0043]    The presented automated process and system for converting polysilicon material into a single silicon crystal, performed at a temperature of around 1410° C. in pure argon gas, provides the controlled environment with the needed consistency and control. 
         [0044]    Turning to drawing  FIG. 1 , illustrated is a view of the micro-puller system in accordance with the present application. Generally, this micro-puller system is significantly smaller than prior art micro-pullers. Furthermore, most support components for the micro-puller system can be placed outside of a clean-room. Support has been assigned to two physical frames; one holding drawers containing power supplies, process control components, the RF generator  503 , and in some embodiments, containing everything other than the reaction tube  213 , such as a quartz tube, and any directly connected components, e.g. the base mounts  205  and  217  with shaft guides  203  and  219  etc. The inner frame can be rolled into the outer frame. The frames are connected together in a manner such that the weight is transferred to the outer frame near the floor, which leads to a low center of gravity for the outer frame with its attached process related hardware, thus offering maximum mechanical stability and resistance to vibrations. The outer frame also has provisions for mechanical anchoring to a solid floor. 
         [0045]      FIG. 2  presents a schematic drawing, a side view of the part of the system where the process takes place. 
         [0046]    The presented List Of Assigned Numerals defines names and functions of system and process components as used throughout the text. 
         [0000]    
       
         
               
             
               
               
               
             
           
               
                   
               
               
                 List of Assigned Numerals: 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                   
                 201  
                 Cooling water seal 
               
               
                   
                 203 
                 Upper shaft guide 
               
               
                   
                 205 
                 Upper base mount 
               
               
                   
                 207 
                 Upper chuck 
               
               
                   
                 209 
                 Si pedestal 
               
               
                   
                 211 
                 Rf coil 
               
               
                   
                 213 
                 Quartz tube 
               
               
                   
                 214 
                 Lower chuck 
               
               
                   
                 215 
                 Automated rf tuning network 
               
               
                   
                 217 
                 Lower base mount 
               
               
                   
                 219 
                 Lower shaft guide 
               
               
                   
                 221 
                 Lower gas port 
               
               
                   
                 223 
                 Carriage 
               
               
                   
                 227 
                 Rf-power connection 
               
               
                   
                 229 
                 Cooling gas port 
               
               
                   
                 231 
                 Upper gas port 
               
               
                   
                 233 
                 Base mount clamp 
               
               
                   
                 235 
                 Upper shaft 
               
               
                   
                 237 
                 Bayonette coupling 
               
               
                   
                 245 
                 Axis, shaft guide up/down 
               
               
                   
                 247 
                 Axis, carriage up/down 
               
               
                   
                 253 
                 Lower shaft 
               
               
                   
                 255 
                 Plunger 
               
               
                   
                 257 
                 Poly-Silicon granules 
               
               
                   
                 271 
                 Susceptor 
               
               
                   
                 501 
                 Rf power supply 
               
               
                   
                 503 
                 Rf generator 
               
               
                   
                 505 
                 System power supplies 
               
               
                   
                 507 
                 Fluid, vacuum, gas control unit 
               
               
                   
                 509 
                 Actuator drives, power supplies 
               
               
                   
                 511 
                 Controller, I/O boards 
               
               
                   
                 513 
                 Rf power cable 
               
               
                   
                 515 
                 CPU 
               
               
                   
                 603 
                 Flow control for cooling water 
               
               
                   
                 605 
                 Air supply to drawer #507 
               
               
                   
                 619, 621 
                 Shaft cooling water 
               
               
                   
                 615, 617  
                 Argon gas to quartz tube 
               
               
                   
                 607, 609 
                 Argon gas to drawer #507 
               
               
                   
                 611, 613 
                 Cooling air for base mount 
               
               
                   
                 623 
                 Vacuum to drawer #507 
               
               
                   
                   
               
               
                   
                 Also shown are lines for cooling water to drawers 501 and 503 
               
             
          
         
       
     
         [0047]    The power and control system is schematically shown in  FIG. 5 . Organized in  6  drawers, it includes an RF power supply  501 , an RF generator  503 , a system power supply  505 , a fluid vacuum and gas control unity  507 , actuator drivers with power supplies  509 , a controller and I/O cards  511 , a CPU  501 , a automated matching RF network  215 , which transmits rf power from the microwave power generator  503 , through cable  513  and the rf power connection  227  to the stationary rf coil  211 . 
         [0048]    The CPU  515  accepts programs and commands either remotely from a touch screen or a remote terminal. The remote terminal can operate the system in a similar manner as a local touch screen. The remote terminal can be employed via an Internet connection to the system, and can be operated by a remote operator. 
         [0049]    After instructions are received by the CPU  515 , they are converted into machine instructions. The machine instructions are communicated to the control unit  511  and to the RF power generator  503 , which in turn is powered by the RF power supply  501 . Inserted between the RF generator  503  and the RF coil  211  is the automated impedance matching network  215 . It measures the reflected and the forward microwave power and automatically adjusts tuning components to minimize the reflected rf power. 
         [0050]    Employment of the impedance matching network  215  leads improved rf-energy transfer, to better temperature stability and temperature control and thereby to improvements of the overall process control. 
         [0051]    The controller unit  511  sends signals to the ambient control unit  507 , which controls all gas/vacuum components (on/off valves, a mass flow controller etc.) and to the actuator unit  509 , which controls various motions, such as all motions of the upper shaft  235 , the lower shaft  253 , and the carriage  223 , all presented in  FIG. 2 , and to be discussed below. 
         [0052]    In the controller system, the CPU  515  receives data from a feedback unit or from a human operator. One critical parameter is the size of the liquid silicon melt. This feedback, originating either from a device or a human, enables the system to precisely follow a pre-programmed process sequence for the consolidation of polycrystalline silicon granules into a polysilicon rod and then for its conversion into a mono-crystalline test sample. 
         [0053]    Drawer  511  (controllers and I/O boards) also contains the rf power control unit, using connections to drawer  503  (rf generator) and to the Automated RF-Tuning Network  215 . Data from radiation sensors can flow to drawer  511  (controller &amp; I/O boards). Drives receive their commands from drawer  509  (actuator drives &amp; power supplies). 
         [0054]    The process takes place in a vertical quartz tube  213 , under flowing high purity argon. 
         [0055]    For processing polycrystalline Silicon granules, which have a typical, but not well defined, diameter of approx. 1 to 5 mm, the first step consists of a conversion into a polycrystalline silicon rod grown by this process onto a silicon pedestal  209 . 
         [0056]    For the consolidation of the silicon pebbles, a silicon rod, called pedestal  209 , is used as base. 
         [0057]    Extending from the upper shaft  235  the pedestal  209  is clamped into the chuck  207 . Both shafts  235  and  253  can be raised, lowered and rotated, thereby moving the silicon pedestal  209 , the plunger  255  or the mounted silicon seed. 
         [0058]    After installing the upper shaft  235  with the pedestal  209 , the upper shaft guide  203  and the shaft  235  are raised so that a path is cleared for loading Si pebbles through the upper port  231  into quartz tube  213 , while not breaking the seal between base mount  205  and shaft guide  203 . This design permits the loading of Si pebbles without removal of the upper shaft  235  from the system, while avoiding exposure of the Si pebbles to air. 
         [0059]    Using a feeding insert, poly-Si granules  257  can be loaded through feeding port  231 . The slopes of all tubes are selected so that the force of gravity is sufficient to let the Si pebbles slide/roll into tube  213 . 
         [0060]    The loaded Si pebbles rest on an inert plunger  255 , made of inert material like PTFE, which is clamped into the chuck  214 . 
         [0061]    The pebbles form a column in quartz tube  213 , e.g. 10 cm tall. High purity argon gas purges combined with vacuum cycles—controlled by Ambient Control Unit  507  connected to lower gas port  221 —are first used to form an oxygen-free environment. Then the argon gas flow, precisely controlled by control unit  507 , is adjusted so that the argon, after passing through a hole pattern in plunger  255 , causes the Si pebbles to become fluidized, meaning that the pebbles at the top portion of the column become suspended in the flowing argon gas stream. Pebbles at the top of the column carry less weight than those at the bottom and are the first to be lifted up by the gas stream. 
         [0062]    In one embodiment, purging efficiency can be enhanced by cycles of high and low pressure. “High pressure” can be generally defined as 2 atmospheres or higher, and “low pressure” can be generally defined as 1 milli-Torr and lower. 
         [0063]    Both shafts  235  and  253 , the tube  213 , and all support components are attached to carriage frame  223  which can also be raised or lowered. The heater i.e. the RF coil  211  with turns encircling the quartz tube  213  is stationary. Raising and lowering carriage  223  moves the heating zone, which is the area with high radio frequency fields, close to the RF coil  211 . 
         [0064]    The process steps performed by this equipment are executed by coordinated movements of the shafts and the carriage, and by control of the RF power and the argon flow. 
         [0065]    To render Si pedestal  209  sufficiently conductive for coupling into the RF field of the RF coil  211 , pedestal  209  is positioned adjacent to RF coil  211  such that the bottom section of pedestal  209  is heated the most. Pedestal  209  is pre-heated by radiation from the RF heated susceptor  271 . Once pedestal  209  is sufficiently hot and conductive and ready for further heating, susceptor  271  is moved sideways and out of the RF field, so that it does not interfere with subsequent process steps. 
         [0066]    In one embodiment of the process, high purity argon gas enters through a lower gas port  221  and exits through an upper gas port  231 . To prevent overheating of temperature sensitive parts, the base mount  205  has cooling ports  229  and internal cavities and passages for gas cooling of the base mount and of the end section of the quartz tube  213 . 
         [0067]    Both shafts  235  and  253  can be cooled by recirculating water and can rotate to equalize temperature non-uniformities, a common practice in the field of of crystal growth.  FIG. 2  identifies the cooling water seal  201  for the upper shaft  235 . Water cooling of the lower shaft  253  is presently considered not necessary for a process involving silicon. 
         [0068]    The shafts are connected to their motors with bayonet-type quick-disconnects, identified as  237  in  FIG. 2 . Shaft guides  203  and  219  provide sealing and mechanical guidance during rotational and vertical movements of the shafts. 
         [0069]    During removal of the shafts from the micro-puller for routine cleaning etc. shaft guide and shaft do not have to be taken apart. Handling of the shafts and the shaft guides as one unit, provides for easier and more precise assembly and disassembly. 
         [0070]    Base mounts, shafts and shaft guides are interchangeable and can be used in the upper or equally the lower location. 
         [0071]    In one embodiment, all metal surfaces that could come in contact with material in process are Teflon® coated, eliminating metal contamination. 
         [0072]    In one embodiment, the controller system uses an Opto-22® Control System. 
         [0073]      FIG. 3A and 3B  illustrate a cross-section of paths which extend capabilities of this described system over previous designs. In  FIG. 3A , the silicon pedestal  209  is clamped into the upper shaft  235 , which can rotate and perform vertical movements, while keeping the contents of the quartz tube  213  isolated from a contaminating outside environment. The shaft guides  203  and  219  can be raised sufficiently to provide a clear path for loading spherical silicon pebbles  257  into the quartz tube  213  without requiring removal of the shaft  235 . 
         [0074]      FIG. 3B  illustrates an upper clamp  233  which compresses the O-ring between the shaft guide  203  and the base mount  205 , securing a tight seal. 
         [0075]      FIGS. 4A and 4B  show detailed views of both engaged and disengaged positions of the metal susceptor  271 . In the engaged position the susceptor is heated by the rf-field, and then acts as radiative heat source for the silicon inside the quartz tube.  FIG. 4B  shows a top view with the susceptor  271  in the two positions. 
         [0076]    Once the susceptor has accomplished the pre-heating, as evidenced by a beginning glow of the silicon, the susceptor swings into the disengaged position ( FIG. 4A and 4B ), the RF power is raised until the bottom section of the pedestal  209  turns liquid. Next the lower shaft  253  is raised and the argon gas flow adjusted so that the fluidized part of the Si-pebble column is moved into the proximity of the liquid part of the pedestal and dancing hot Si pebbles come in contact with the melt and go into solution. An upward motion of carriage  223  is then initiated, causing the liquid zone to move downwards. Gradually, more Si pebbles go into solution while simultaneously the top section of the melt leaves the hot zone, solidifies, and thereby forms the consolidated poly silicon extension to the silicon pedestal  209 . Generally, employment of the susceptor  271  allows for an elimination of an open gas flame process, a significant safety improvement over prior art technology. 
         [0077]      FIG. 5  presents a schematic of the Power Distribution, the Environmental Control, and of the physical layout of the total system, arranged in drawers. Beginning with the bottom drawer, the rf-power supply  501  is followed by the rf-generator  503 , followed by System Power Supplies  505 , followed by Ambient Controls (gas, fluid, vacuum)  507 , followed by actuator drives and power supplies  509 , followed by controller I/O boards  511 , and the CPU  515 . Also shown is the automated rf-matching network  215 , and sections of the rf-power cable  513 , which connects the rf-generator  503  with the matching network  215 . The water cooled rf power connection  227  clamps directly into ports in the Tuning Network  215  and feeds rf energy to the water cooled rf coil  211 . 
         [0078]      FIG. 6  displays a preferred configuration for an ambient control system, which includes the Ambient Control unit  507 , which contains components to control the gas flow rate and pressure in the quartz tube  213 , plus the gas manifold (not illustrated) with on/off gas controls, which can include a gas pressure regulator and mass flow controller. The ambient control unit  507  also regulates cooling water flow and compressed air flow. 
         [0079]    Cooling water is re-circulated from a cooling water supply (not illustrated) through the rf power supply  501 , the rf generator  503 , the automated tuning rf network  215 , the rf coil, and the shafts  235  and  253 , if so desired. 
         [0080]    The control unit  507  receives argon through line  609  and emits argon to exhaust through line  607 . The quartz tube  213  is connected to drawer  507  via lines  615  and  617 . 
         [0081]    The following part of the disclosure will be generally related to process. 
         [0082]    Automated change between various positions of shaft guide  203  and  219  is achieved by a motor, such as a servo motor or a pneumatic motor. During the process, the shaft guide  203  is in the lowest position. All seals are in compressed state, ensuring a leak—and contamination—free environment. Pneumatic linear motors were selected for this function. 
         [0083]    The next process step is for the polycrystalline extension to the silicon pedestal  209  to become converted to single crystal silicon. 
         [0084]    The lower shaft  253  with shaft guide  219  and plunger  255  and the remaining, unconsumed, Si pebbles are taken out. Alternatively, the remaining, unconsolidated Si pebbles can also be removed through lower gas port  221 . Using an unloading insert in port  221 , the gravity driven round Si pebbles can be made to glide into a collection vessel. 
         [0085]    Next a monocrystalline Si seed crystal of proper orientation is mounted on the chuck  214 . The whole seed/chuck/shaft/shaft guide assembly is then re-installed into lower base mount  217 . 
         [0086]    The Si source material for the process of single silicon crystal conversion may also originate from silicon manufacturing processes that do not produce granules, but large bodies of polysilicon, such as the Siemens® process. For this machine the only requirement for a conversion from poly- to single crystal material is that the sample meets the geometrical specification. This can involve the use of maching tools. 
         [0087]    After argon purge cycles, the seed, mounted on chuck  215 , and the poly-silicon source mounted on chuck  207  is moved into position for preheating by the RF-heated susceptor  271 . After coupling of the poly-crystalline source material to the RF field is achieved, susceptor  271  is moved to the disengaged position and the RF power is raised to melt the bottom of the Si polysource material. 
         [0088]    The RF power, and the positions of both upper shaft  235  and lower shaft  253  with respect to the RF coil  211 , are then selected so that the melted tip of silicon poly-silicon source is in the center of the RF coil  211 , and is a few millimeters in length. When too thick, the melt will form a drop that causes damage when it disengages and falls down onto other components. 
         [0089]    To begin the single crystal growth process, the lower shaft  253  is raised until the tip of single seed touches the hanging melt of the polysilicon source. The growth rate and the geometry of a growing single crystal are controlled by movements of the carriage  223  and of the shafts  235 ,  253 . 
         [0090]    Following techniques common for single crystal growth, a slight melt back of the seed is performed, and, after the establishment of thermal equilibrium, a neck is grown, followed by letting the crystal grow to the desired diameter, before body growth is initiated. 
         [0091]    Precise control of all parameters i.e. the thermal environment and various movements, are critical for successful single crystal growth. Besides having tight control of the RF power generator  503  and automated matching network  215 , this described system features rotating shafts, thus improving the uniformity of the thermal environment and providing means to influence the convection pattern in the liquid silicon. 
         [0092]    After growing the desired crystal length, the growing crystal is separated from the melt, the system is cooled down. The crystal is harvested and several 2 to 4 mm thick slices are sawn off in specified locations for submission to precision tests, such as Fourier Transform Infra-Red (“FTIR.”) Misleading test results may be obtained when the test sample includes material from the Si pedestal or when too much seed material entered into the melt. 
         [0093]    In the present application, to maintain the relationship between the impurity concentration of the starting granular silicon and the final test sample, purification by the system and by the process is normally undesirable. However, independent control of shaft movements (vertical and rotational) gives the operator a capability to minimize deleterious contributions, such as the addition of Si-seed material to the material under test. 
         [0094]    Finally, a test sample is cut and prepared from the grown single crystal silicon, and submitted to tests, such as FTIR. 
         [0095]    In one embodiment, the process steps of consolidation and single-crystal growth, taking advantage of aspects of the system, can be summarized as a series of steps, as follows: 
       Consolidate Si Pebbles  
       [0000]    
       
           1 . Feed in Si pebbles. 
         2. Seal the system. 
         3. Argon purge the system with pressure/vacuum cycles. 
         4. Move shafts and carriage into position. 
         5. Position susceptor. 
         6. Do preheat. 
         7. Swing away susceptor. 
         8. Set Si-pedestal position and shaft movements. 
         9. Form liquid pedestal bottom (set RF-power). 
         10. Set argon flow to fluidize pebbles. 
         11. Run process using selected carriage and shaft movements. 
         12. Shut off process. 
         13. Remove bottom shaft assembly with plunger and remaining pebbles. 
       
     
         [0109]    The process using the system continues with the Single Crystal Growth phase.
   14. Mount shaft guide/shaft/seed assembly, and seal system.   15. Argon purge the system with pressure, which can include vacuum cycles;   16. Move shafts and carriage into position.   17. Select shaft movements.   18. Position susceptor.   19. Preheat bottom of poly-Si rod which was formed previously, using the RF-heated susceptor.   20. Swing away susceptor.   21. Melt bottom of poly-Si using the RF energy from the coil.   22. Do seed-dip by moving seed up.   23. Grow the single crystal making use of the adjustable parameters such as carriage movement, shaft movements, and temperature and gas controls.   24. Separate the single crystal from melt.   25. Unload the single crystal, prepare a test sample for e.g. Optical Tests.   
 
       Considerations of Cycle Time  
       [0122]    The steps requiring the longest period of time are the consolidation and single crystal growth because of the required achievement of thermal equilibrium and considerations of heat flow and heat of fusion. The time for the many short steps depend on the operator skill, and on the timely availability of prepared components. 
         [0123]    Some additional discussion of important construction and engineering details of the system. 
         [0124]    For use in a clean room environment, the system can be installed in such a manner, that only the parts directly associated with the quartz tube are on the clean side of a clean room wall. The areas of clean room wall penetrations are minimized. 
         [0125]    Microwave power is supplied by a water cooled coil which surrounds the quartz tube, driven by a nominally 10 kW, 3 MHz solid state power source through an water cooled automated matching network. Automatically minimizing the reflected microwave power compensates for impedance changes due to silicon conductivity and melt size changes, and to changes of the load location with regard to the stationary rf-coil. 
         [0126]    Safety improvements during the process of pre-heating of Silicon. 
         [0127]    To raise the Silicon conductivity enough to achieve coupling to the rf-field, a horseshoe shaped metallic structure, called susceptor  271 , is swung in, almost touching the quartz tube  213  and in very close proximity of the rf-coil  211 . Radiation from this glowing metal is absorbed by the Si and the Si temperature rises. Once rf-coupling sets in, a positive feedback cycle takes over: rising temperature causes increased conductivity with increased rf-absorption and so on. The temperature rises very fast. An automated mechanism then removes the susceptor  271 . Then the location of the Si is optimized for the next process step and the rf-power is adjusted to obtain the desired size of the molten silicon. The elimination of the use of an open flame for silicon pre-heating is considered to be a substantial safety improvement. 
         [0128]    The basic principles of the system employ modern drive and control components. All motions of the carriage and the 2 shafts (vertical and rotational) are achieved by stepping motors or servo motors. The shafts are designed for water cooling. The chassis design stresses mechanical stability, resistance to vibrations, ease of access, maintenance and transportation. The stack of heavy drawers with power sources and control components rests on its own inner frame. The inner frame is rolled into the outer frame and the frames connect at floor level, providing a low center of gravity. 
         [0129]    The outer frame, which holds all process related components, has provisions for bolting to the floor. 
         [0130]    In one embodiment, the micro-puller system is controlled from a touchscreen, which is linked to the process computer. Parameters like rf-power, gas flow rate, gas valve status, rotations and movements of the shafts, the movement of the carriage, are controlled, monitored and can be adjusted any time. The whole process profile, including the adjustments, is temporarily stored in the computer. It can be permanently saved under a different name, and it is then available for future use and study. Program modifications and process monitoring and control can also be made via Internet. 
         [0131]    The system offers water cooled shafts and shaft rotation. Shaft rotations provide for improved temperature uniformity and thereby better dimensional control of the growing crystal. The system offers the possibly to withdraw the shafts far enough out, without exposing the process volume to air, to present a clear path for pebble loading without removal of the upper shaft. 
       Operator Safety Considerations 
       [0132]    Generally, a quartz tube is the mechanically weak spot of the system. Micro cracks, possibly caused during the tube handling and installation, can cause failure under raised or lowered pressure. Operators need to be required to wear eye protection around the machine. Performance of pressure and leak rate tests should be considered after installation of a quartz tube. 
         [0133]    The disclosed system and methods can be applied to work with a variety of other materials which require high temperature processing and/or crystal formation. Besides silicon these materials may include Ge, Group III-V Semiconductors as well as some organic crystal materials. 
         [0134]    The system may be used for sample preparation from materials prepared by other techniques, such as crystal growth processes of Cz, LEC, and Bridgman, casting processes e.g. for ingots for solar cells, and for source material produced for thin film applications, such as vapor phase, liquid phase epitaxy, or evaporation, sputtering and plasma deposition, MBE and MOCVD processes, etc. 
         [0135]    Those skilled in the art to which this application relates will appreciate that other and further additions, deletions, substitutions and modifications may be made to the described embodiments.