Abstract:
A vacuum recycling apparatus for refining solar grade polysilicon is provided which contains a vacuum degassing (VD) device and a vacuum recycling (RH) device. By storing liquid silicon in a bucket in the VD device, controlling the pressure inside the VD and RH devices, and introducing inert gas into the apparatus, the liquid silicon is stirred for the removal of impurities. With the present invention, solar grade polysilicon can be directly produced with a specified purity, significantly reducing the production time and cost.

Description:
(a) TECHNICAL FIELD OF THE INVENTION 
       [0001]    The present invention generally relates to solar cells, and especially relates to a USB female connector immune from the crosstalk problem resulted from high-frequency signal. 
       (b) DESCRIPTION OF THE PRIOR ART 
       [0002]    There are two major applications to polysilicon material. One application is for the production of solar cells. The other application is for integrated circuits. The two applications have different requirements to polysilicon material. The electronic grade polysilicon is required to have its purity between 9N and 11N whereas the solar grade polysilicon is required to have a less purity between 5N and 7N for achieving sufficient photoelectric conversion efficiency and life span. 
         [0003]    The electronic grade polysilicon is usually produced by a high-cost chemical method which is improved from the original Siemens method. The solar grade polysilicon on the other hand can be produced by a certain physical method for reduced cost. In addition to the improved Siemens methods, there are metallurgical method, dilution method, and fluidized bed method, etc. 
         [0004]    As the solar grade polysilicon is not required to have high purity, highly pure polysilicon has to be appropriately doped by boron and phosphorus to reduce its purity for photovoltaic purpose. This not only is ironic but also causes a high cost. 
         [0005]    RH vacuum process, or vacuum recycling process, is taught jointly by two German companies: Ruhrstahl and Heraeus. The process submerges two pipes of a vacuum chamber into molten steel, and vacuums the chamber to raise the molten steel to a specific level. Then, by driving inert gas into an input pipe to force molten steel into the vacuum chamber for vacuum processing, the molten steel then flow back into the container through an output pipe. This process is conventionally applied in a steel factory for vacuuming processing molten steel. The present inventor has taught a metallurgical method for refining polysilicon in a Taiwan patent application numbered 099136030 and filed on Oct. 22, 2010. The teaching uses a RH device to remove boron and phosphorous. However, some residual of molten steel is accumulated at corners of the input and output pipes, leading to inferior circulation of the molten steel and the product&#39;s purity. 
       SUMMARY OF THE INVENTION 
       [0006]    In order to overcome the above problems of the prior arts, the present invention provides a vacuum recycling apparatus and a method for refining solar grade polysilicon. The present invention is able to directly produce solar grade polysilicon with a specified purity. For example, the produced polysilicon would have solar grade purity between 5N and 7N. The present invention does not produce polysilicon of a greater-than-7N purity and requires the addition of impurities such as boron and phosphorous so as to lower its purity. The present invention therefore can greatly reduce production time and cost. In addition, the present invention does not rely on input and output pipes and as such obviates the problem of residual solution. 
         [0007]    To achieve the above objectives, is provided which contains a vacuum degassing (VD) device and a vacuum recycling (RH) device. The VD device contains a vacuum chamber, a silicon-stored bucket, and an inert gas introduction device. The vacuum chamber contains a first degassing outlet and a joining opening. The silicon-stored bucket is positioned in the vacuum chamber and beneath the joining opening for storing liquid silicon solution or for storing solid silicon. The inert gas introduction device is configured in the silicon-stored bucket. The RH device contains a second degassing outlet and a connection pipe. The connection pipe is plugged into the silicon-stored bucket through the joining opening. The joining opening is then tightly sealed so that introduced inert gas by the inert gas introduction device moves towards the connection pipe. By vacuuming the VD device and the RH device through the first and second degassing outlets, respectively, and by adjusting the degrees of vacuum of the VD device and the RH device, the height of the liquid silicon solution in the RH device is controlled. 
         [0008]    The vacuum recycling apparatus is able to directly produce polysilicon of a specified purity, significantly saving production time and cost. 
         [0009]    Preferably, the VD device is integrated with a furnace into a single device so as to reduce thermal loss and to enhance heating efficiency. 
         [0010]    Preferably, the silicon-stored bucket is integrated into the VD device as an integral chamber so as to reduce the dimension of the VD device. 
         [0011]    Preferably, the silicon-stored bucket is integrated into the VD device as an integral chamber; and the VD device is further integrated with a furnace into a single device. 
         [0012]    Preferably, the degrees of the vacuum of the vacuum chamber of the VD device and the RH device are between 0.1 to 0.9 atm, and between 0.001 to 1,000 Pa, respectively. 
         [0013]    Preferably, the RH device further contains a real-time measuring device so as to measure and monitor the amount of impurities in the silicon solution in the silicon-stored bucket; and the VD device further contains at least a plasma gun so as to remove the impurities of the silicon solution in the silicon-stored bucket. 
         [0014]    The present invention further provides a method of applying the vacuum recycling apparatus to refine solar grade polysilicon. The method contains (a) a liquefaction step; (b) a vacuuming step; (c) a stir step; (d) an impurity removal step; (e) a confirmation step; and (f) a formation step. The method can directly produce solar grade polysilicon of a specified purity with reduced production time and cost compared to the prior arts. 
         [0015]    Preferably, the confirmation step disrupts the supply of the inert gas when the amount of phosphorous in the silicon solution is less than 0.8 ppm and the amount of boron in the silicon solution is less than 0.4 ppm, so as to precisely control the amount of impurities. 
         [0016]    Preferably, the formation step crushes the solidified silicon solution into 50 to 150 meshes for better acid-cleaning. 
         [0017]    The foregoing objectives and summary provide only a brief introduction to the present invention. To fully appreciate these and other objects of the present invention as well as the invention itself, all of which will become apparent to those skilled in the art, the following detailed description of the invention and the claims should be read in conjunction with the accompanying drawings. Throughout the specification and drawings identical reference numerals refer to identical or similar parts. 
         [0018]    Many other advantages and features of the present invention will become manifest to those versed in the art upon making reference to the detailed description and the accompanying sheets of drawings in which a preferred structural embodiment incorporating the principles of the present invention is shown by way of illustrative example. 
     
    
     
       BRIEF DESCRIPTION OF THE DRAWINGS 
         [0019]      FIG. 1  is a sectional diagram showing a vacuum recycling apparatus for refining solar grade polysilicon according an embodiment of the present invention. 
           [0020]      FIG. 2  is a sectional diagram showing the vacuum recycling apparatus of  FIG. 1  joined to a silicon-stored steel bucket. 
           [0021]      FIG. 3  is a flow diagram showing the steps of refining solar grade polysilicon using the vacuum recycling apparatus of  FIG. 1 . 
       
    
    
     DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS 
       [0022]    The following descriptions are exemplary embodiments only, and are not intended to limit the scope, applicability or configuration of the invention in any way. Rather, the following description provides a convenient illustration for implementing exemplary embodiments of the invention. Various changes to the described embodiments may be made in the function and arrangement of the elements described without departing from the scope of the invention as set forth in the appended claims. 
         [0023]      FIG. 1  is a sectional diagram showing a vacuum recycling apparatus for refining solar grade polysilicon according an embodiment of the present invention.  FIG. 2  is a sectional diagram showing the vacuum recycling apparatus joined to a silicon-stored steel bucket.  FIG. 3  is a flow diagram showing the steps of refining solar grade polysilicon using the vacuum recycling apparatus of  FIG. 1 . As shown in  FIG. 1 , the vacuum recycling apparatus contains a vacuum degassing (VD) device  1  and a vacuum recycling device  2  (i.e., a RH device). 
         [0024]    The VD device  1  contains a vacuum chamber  11 , a silicon-stored bucket  12 , and an inert gas introduction device  13 . The vacuum chamber  11  contains a first degassing outlet  111  and a joining opening  112 . The silicon-stored bucket  12  is positioned in the vacuum chamber  11  and beneath the joining opening  112  for storing liquid silicon solution L or for storing solid silicon. The inert gas introduction device  13  is configured in the silicon-stored bucket  12  so that inert gas can be introduced into the silicon-stored bucket  12 . 
         [0025]    The RH device  2  contains a second degassing outlet  21  and a connection pipe  22 . The connection pipe  22  is plugged into the silicon-stored bucket  12  through the joining opening  112 . The joining opening  112  is then tightly sealed so that the introduced inert gas by the inert gas introduction device  13  moves towards the connection pipe  22 . By vacuuming the VD device  1  and the RH device  2  through the first and second degassing outlets  111  and  21 , respectively, as indicated by the arrows in the drawings, and by adjusting the degrees of vacuum of the VD device  1  and the RH device  2 , the height of the liquid silicon solution L in the RH device  2  can be controlled. 
         [0026]    Through the vacuum recycling apparatus described above, the process of refining polysilicon requires a less amount of time, thereby leading to a reduced cost. More details will be given later. 
         [0027]    Furthermore, the VD device  1  can be further integrated with a furnace into a single device to facilitate heating and to prevent thermal loss, so as to achieve superior heating efficiency. As the integration of the VD device  1  and the furnace should be straightforward to those of related arts, and the integration result is close to what is shown in  FIG. 1 , the details are omitted here. 
         [0028]    In addition, the RH device  2  is configured with a real-time measuring device  23  so as to measure and monitor the amount of impurities in the silicon solution L in the silicon-stored bucket  12 . Plasma guns  14  are configured in the VD device  1  so as to remove the impurities of the silicon solution L in the silicon-stored bucket  12 . 
         [0029]    As shown in  FIG. 2 , the silicon-stored bucket  12  can be integrated into the VD device  1  as an integral chamber  12 ′ so as to improve efficiency and to reduce the dimension of the VD device  1 . 
         [0030]    The above-mentioned furnace can be a medium frequency furnace. 
         [0031]    More specifically, to refine solar grade polysilicon, the degrees of the vacuum of the vacuum chamber  11  of the VD device  1  and the RH device are between 0.1 to 0.9 atm, and between 0.001 to 1,000 Pa, respectively. 
         [0032]    A method of applying the vacuum recycling apparatus to refine solar grade polysilicon contains (a) a liquefaction step S 1 , (b) a vacuuming step S 2 , (c) a stir step S 3 , (d) an impurity removal step S 4 , (e) a confirmation step S 5 , and (f) a formation step S 6 . The details of these steps are as follows. 
         [0033]    The liquefaction step S 1  liquefies and pours silicon raw material into the silicon-stored bucket  12  until the silicon solution L has a level higher than the aperture of the connection pipe  22 . 
         [0034]    The vacuuming step S 2  degasses the VD device  1  and the RH device  2  until their degrees of the vacuum are between 0.1 to 0.9 atm, and between 0.001 to 1,000 Pa, respectively. 
         [0035]    The stir step S 3  agitates the silicon solution L by introducing inert gas through the inert gas introduction device  13  and, as the inert gas moves towards the connection pipe  22 , achieves diffusing and degassing effects. 
         [0036]    The impurity removal step S 4  uses the plasma guns  14  to remove impurities. 
         [0037]    The confirmation step S 5  disrupts the supply of the inert gas when the amount of boron in the silicon solution L is less than 0.4 ppm, and the amount of phosphorous is less than 0.8 ppm. The degree of vacuum in the RH device  2  is also reduced so that the silicon solution L flows back into the silicon-stored bucket  12 . 
         [0038]    The formation step S 6  pours the silicon solution L processed by the above steps into a slow-condensing container. After cooling, the less pure offcuts are removed and the solidified silicon is crushed, acid-cleaned for removing impurities, and then casted into directional ingot. Solar grade polysilicon is as such produced. 
         [0039]    Unlike the prior arts where impurities are first removed and then added so as to achieve solar grade polysilicon, the present invention is able to achieve a shorter process time and a lower production cost. 
         [0040]    In the formation step S 6 , the solidified silicon solution is crushed into 50 to 150 meshes so as to facilitate the subsequent acid-cleaning. 
         [0041]    To facilitate the understanding of the present method, together with  FIG. 1 , an embodiment of the above steps is described as follows, 
         [0042]    Firstly, solid 2N to 4N metallic silicon raw material is heated into liquid metallic silicon solution L and then poured into the silicon-stored bucket  12 . 
         [0043]    Secondly, the silicon-stored bucket  12  is positioned in the vacuum chamber  11  and heated (about 1,000 to 1,800° C.) so as to maintain the high-temperature, liquid metallic silicon solution state. 
         [0044]    Thirdly, the connection pipe  22  of the RH device  2  is plugged into the silicon-stored bucket  12  in the vacuum chamber  11  of the VD device  1  and submerged into the liquid silicon solution L. 
         [0045]    Fourthly, the VD device  1  and the RH device  2  are sealed tightly and vacuumed so that their degrees of vacuum are between 0.1 to 0.9 atm, and between 0.001 to 1,000 Pa, respectively. Inert gas such as Ar, He, or N 2 , is introduced into the connection pipe  22 . 
         [0046]    Fifthly, the inert gas produces bubbles in the silicon solution L as shown in the drawings. Then, through the control of degree of vacuum and therefore the level of the liquid silicon solution L and the stir of the liquid silicon solution L by the bubbles, the impurities such as Fe, Al, Ca, C, O, P, B, etc., can be effectively removed and highly pure polysilicon can be obtained. 
         [0047]    Sixthly, the silicon solution L is heated (or kept at a temperature) by configuring electronic beam or plasma guns on the VD device. Then, boron (B) is removed and Ar, H 2 O vapor, H 2  are added. 
         [0048]    Seventhly, after the recycling, diffusion, and degassing for a period of time (about 10 minutes to 10 hours), the provision of the inert gas is disrupted when the real-time measuring device  23  detects that the amount of boron is less than 0.4 ppm and phosphorous is less than 0.8 ppm. Then, the degree of vacuum in the RH device  2  is reduced and the liquid silicon solution L flows back into the silicon-stored bucket  12  in the VD device  1 . 
         [0049]    Eighthly, the highly pure (4N to 6N), degassed, de-boron, and de-phosphorus polysilicon solution L in the silicon-stored bucket  12  is poured into the slow-condensing container. After cooling for a long period of time (4 to 72 hours), the less pure offcuts are removed and the solidified silicon is crushed into 50 to 150 meshes, acid-cleaned for removing impurities such as Fe, Al, and Ca, etc., and then casted into directional ingot. Highly pure (6N to 7N) solar grade polysilicon (UMG-Si) is as such produced, and can be directly cut for the production of solar cells. 
         [0050]    In alternative embodiments, the VF device  1  can be integrated with a medium frequency furnace into a single device. As such, solid silicon can be directly heated (1,000 to 1,800° C.) through the medium frequency furnace in the VD device  1  into high-temperature liquid silicon solution L. Alternatively, as shown in  FIG. 2 , the silicon-stored bucket  12  can be integrated into the VD device  1  as an integral chamber  12 ′. Furthermore, the VD device  1 , the medium frequency furnace, and the silicon-stored bucket  12  can be integrated together so as to reduce the time and effort to transfer material between these devise. 
         [0051]    While certain novel features of this invention have been shown and described and are pointed out in the annexed claim, it is not intended to be limited to the details above, since it will be understood that various omissions, modifications, substitutions and changes in the forms and details of the device illustrated and in its operation can be made by those skilled in the art without departing in any way from the spirit of the present invention.