专利摘要:
The laboratory reactor is used for the deposition of polysilicon from a process gas on a thin rod (62) of silicon, which bridges two electrodes (34) within a hood (20), which are inserted into a bottom plate (18). It is provided that the inner wall (80) of the hood (20) and the inwardly facing bottom surface (44) of the bottom plate (18) are coated with silver and that also the thin rod (62) receiving the head (56) of the two electrodes ( 34) is silvered.
公开号:AT13092U1
申请号:TGM101/2012U
申请日:2012-03-19
公开日:2013-06-15
发明作者:
申请人:Silcontec Gmbh;
IPC主号:
专利说明:

Austrian Patent Office AT13 092 U1 2013-06-15
description
LABORATORY REACTOR
The invention relates to a laboratory reactor for the deposition of polysilicon from a process gas on a thin rod made of silicon, which bridges two electrodes within a hood, which are inserted into a bottom plate.
For the recovery of silicon silicon atoms are deposited by the Siemens process at very high temperatures from a process gas, which are deposited on a support. This process is carried out in large reactors under exclusion of air, whereby considerable purity requirements must be observed.
The invention has for its object to provide a laboratory reactor available that allows quality analysis and quality assurance during the process, so that impurities in the deposition of silicon can be determined early online to be able to intervene in the production process.
To solve this problem, the laboratory reactor formed according to the invention, which is characterized in that the inner wall of the hood and the inwardly facing bottom surface of the bottom plate are coated with silver and that also the thin rod receiving head of the two electrodes is silvered ,
The inventively provided silver coating has the double advantage that on the one hand the purity is guaranteed in the laboratory reactor and that on the other hand, a homogeneous temperature field can be realized with high temperatures, the energy consumption is significantly reduced.
In a further development of the invention, the two electrodes have a water-cooled cavity, to which each electrode consists of a connected to a voltage source, electrically conductive tube in which a coaxial cooling water pipe is used. Both the electrically conductive tube of the electrode and the cooling water pipe can according to a further feature of the invention consist of copper or a copper alloy.
The water-cooled electrodes of the laboratory reactor according to the invention and their silvered head have the advantage of stabilizing a constant, relatively low temperature at the junctions of the electrodes on the silicon thin rod.
In a further aspect of the projecting beyond the bottom plate in the hood head of each electrode is formed as a cone on which a conical graphite head is fitted form-fitting, which has a blind bore for receiving the lower end of the respective thin rod. It is advantageous if the blind bore is flared outward, whereby a frictional fixation of the thin rod is ensured.
According to a further feature of the invention, the hood is placed over a bell made of quartz glass, which allows a view of the thin rod during the process and is absolutely pure.
In the space provided for a nitrogen filling annulus between the hood and bell can be arranged according to a further feature of the invention, an electric preheating, for example, a preheat.
Further features and advantages of the invention will become apparent from the claims and from the following description of an embodiment which is illustrated in the drawing. 1 shows the view of an opened cabinet with a laboratory reactor housed therein in accordance with the invention, FIG. 2 shows a schematic sectional view of the laboratory reactor according to the invention and FIG. 1/7 Austrian Patent Office AT 13 092 U1 2013-06-15 Figure 3 on an enlarged scale one of the two electrodes.
Figure 1 shows the view of a housing 10 in the form of a cabinet, which has a cabinet 12 in its upper part, in which a laboratory reactor 14 is housed according to the invention. The cabinet 12 has two hinged doors 16 which can be swiveled through at least 90 ° so that the interior of the cabinet 12 is easily and unhindered accessible.
As the sectional view of Figure 2 shows, the laboratory reactor 14 has a bottom plate 18, on which a non-illustrated compression fittings a hood 20 is attached. This includes a smaller, also dome-shaped bell 22, which consists of quartz glass.
The double-walled outer cover 20 made of stainless steel has a water-cooled cavity between the two walls 24. For further cooling of the laboratory reactor 14 and the existing stainless steel bottom plate 18 is hollow and provided on one side with a cooling water connection 26.
On one side, the hood 20 has a coupling element 28 to which a lifting device, not shown, can act to transport and lift the entire laboratory reactor 14.
On the coupling element 28 opposite side of the hood 20, a sight glass 30 is provided, through which the interior of the laboratory reactor 14 can be viewed.
In the central region of the bottom plate 18, two vertical receiving holes 32 are provided, in each of which an electrode 34 shown in more detail in Figure 3 is inserted from above. The electrode 34 consists of an electrically conductive cylindrical tube 36 made of copper or a copper alloy. The tube 36 is insulated from the bottom plate 18 by a bush 38 of electrically non-conductive material and sealed by an O-ring 40. The bush 38 is supported via a flange 42 on the bottom surface 44 of the bottom plate 18. For axial attachment of the tube 36 to the bottom plate 18 is a ring nut 46th
In the axial cavity 48 of the tube 36, a cooling water pipe 50 is inserted, which may also consist of copper or a copper alloy. The cooling water pipe 50 has at its lower end an inlet opening 52 for the cooling water, which enters the cavity 48 at the upper, open end of the cooling water pipe 50 and leaves it at the lower end via a drain connection 54.
As Figure 3 further shows, the head 56 of the electrode 34 is formed as a cone on which a conical graphite head 58 is fitted form-fitting manner. The graphite head 58 has a conically outwardly widened blind bore 60, which serves to receive the lower end of a thin rod (slimrod) 62 made of silicon indicated in FIG. As further indicated in Figure 2, the two upper ends of the thin rods 62 are connected by a horizontal, a bridge 64 forming silicon thin rod.
From Figure 2 also shows that in the annular space 66 between the bell 22 and the hood 20, an inlet valve 68 leads, so that the annular space 66 can be filled with nitrogen. On the opposite side, an outlet valve 70 is provided for the nitrogen.
In the center of the bottom plate 18 is a closable feed opening 72 for the entry of a process gas into the interior 74 of the bell 22nd
In the annular space 66 between the hood 20 and the bell 22, a preheating 76, for example, a preheating arranged, which can be connected via two electrodes 78 to a voltage source.
According to the invention, it is finally provided that the inner wall 80 of the outer hood 20 and the bottom surface 44 of the bottom plate 18 are coated with silver. In addition, the head 56 of the electrode 34 is also coated with silver, this silver coating occupying the entire surface of the head 56 up to the O-ring 40 shown in FIG. 3 ,
For the operation of the laboratory reactor 14, the two thin rods 62 are first inserted with the thin-rod bridge 64 made of silicon in the blind holes 60 of the two electrodes 34, whereupon the inner bell 22 and the outer hood 20 are mounted on the bottom plate 18. Following this, it must be ensured that the entire interior is free of oxygen. For this purpose, a nitrogen purge is performed, both via the feed opening 72 for the process gas and via the leading into the annulus 66 inlet valve 68th
At the beginning of the following process, the two electrodes 34 are connected to a voltage source, which is regulated to 400 volts, so that the silicon rods 62, 64 are glowing and reach a temperature of about 1000 ° C. At this temperature, the process gas is introduced via the supply port 72, which consists of TCS (trichlorosilane) and hydrogen. At the high process temperature mentioned, the TCS gas splits into HCl as well as hydrogen and silane. The silicon contained in silane settles on the thin rods 62, 64 and grows to these to the desired strength. Since the described deposition proceeds relatively quickly within a few hours, a test result is available after a short time, with which the purity of the entire process can be checked much faster than in a large reactor.
After the end of the process, a system purge with nitrogen is carried out again.
The site of the laboratory reactor 14 receiving, self-contained cabinet 12 is independent of explosion protection, since the cabinet 12 has a not further shown supply and exhaust air system. 3.7
权利要求:
Claims (13)
[1]
Austrian Patent Office AT 13 092 U1 2013-06-15 Claims 1. A laboratory reactor for depositing polysilicon from a process gas on a thin rod (62) made of silicon, which bridges two electrodes (34) within a hood (20), which are embedded in a bottom plate ( 18) are used, characterized in that the inner wall (80) of the hood (20) and the inwardly facing bottom surface (44) of the bottom plate (18) are coated with silver and that also the thin rod (62) receiving the head (56 ) of the two electrodes (34) is silvered.
[2]
2. Laboratory reactor according to claim 1, characterized in that the two electrodes (34) have a water-cooled cavity (48).
[3]
3. Laboratory reactor according to claim 2, characterized in that each electrode (34) consists of a connected to a voltage source, electrically conductive tube (36) in which a coaxial cooling water pipe (50) is inserted.
[4]
4. Laboratory reactor according to claim 3, characterized in that both the electrically conductive tube (36) of the electrode (34) and the cooling water pipe (50) consists of copper or a copper alloy.
[5]
5. Laboratory reactor according to one of the preceding claims, characterized in that on the bottom plate (18) in the hood (20) projecting head (56) of each electrode (34) is formed as a cone on which a conical graphite head (58) form fit is attached, which has a blind bore (60) for receiving the lower end of the respective thin rod (62).
[6]
6. Laboratory reactor according to claim 5, characterized in that the blind bore (60) is flared outwardly.
[7]
7. Laboratory reactor according to one of the preceding claims, characterized in that through the bottom plate (18) a closable feed opening (72) for the process gas in the interior (74) of the hood (20) leads.
[8]
8. Laboratory reactor according to one of the preceding claims, characterized in that the hood (20) and the bottom plate (18) consist of stainless steel.
[9]
9. Laboratory reactor according to claim 8, characterized in that both the hood (20) and the bottom plate (18) have water-cooled cavities.
[10]
10. Laboratory reactor according to one of the preceding claims, characterized in that the hood (20) is slipped over a bell (22) made of quartz glass, in whose interior (74) the feed opening (72) opens for the process gas.
[11]
11. Laboratory reactor according to claim 10, characterized in that in the annular space (66) between the hood (20) and bell (22), an electric preheating element (76) is arranged.
[12]
12. Laboratory reactor according to claim 11, characterized in that the annular space (66) is filled with nitrogen.
[13]
13. Laboratory reactor according to one of the preceding claims, characterized in that it is housed in a cabinet (12), the interior of which is accessible via two hinged doors (16) which can be pivoted by at least 90 ° each. 3 sheets of drawings 4/7
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法律状态:
2014-06-15| MA04| Withdrawal (renunciation)|Effective date: 20140206 |
优先权:
申请号 | 申请日 | 专利标题
DE201220100839|DE202012100839U1|2012-03-08|2012-03-08|laboratory reactor|
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