CN115159528A - Graphite assembly for polycrystalline silicon reduction furnace and using method thereof - Google Patents
Graphite assembly for polycrystalline silicon reduction furnace and using method thereof Download PDFInfo
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- CN115159528A CN115159528A CN202210820176.6A CN202210820176A CN115159528A CN 115159528 A CN115159528 A CN 115159528A CN 202210820176 A CN202210820176 A CN 202210820176A CN 115159528 A CN115159528 A CN 115159528A
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- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
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Abstract
The invention provides a graphite component for a polysilicon reduction furnace, which comprises: the middle part of the clamping body is provided with a through silicon core mounting hole for fixing the silicon core; one side end face of the graphite base is connected with the electrode, and the other side end face of the graphite base is connected with the clamping body and is abutted against one side end part of the silicon core; the middle part of the fastener is provided with a fixing hole, the lower end of the fixing hole is sleeved on the graphite base, and the middle part of the fixing hole is abutted against the side face of the clamping body so as to fix the clamping body on the graphite base. The graphite assembly for the polycrystalline silicon reduction furnace can effectively prevent the graphite assembly from being embedded into the silicon rod by coating, and meanwhile, when the silicon rod is separated from the graphite assembly, the section is mainly formed at the integral upper plane of the graphite assembly, so that the separation of a graphite accessory and the silicon rod can be thoroughly realized, and the difficulty of rejecting carbon head materials is reduced, thereby being beneficial to quality control and improving the quality control level of polycrystalline silicon.
Description
Technical Field
The invention relates to the technical field of graphite assembly structures, in particular to a graphite assembly for a polycrystalline silicon reduction furnace and a using method of the graphite assembly for the polycrystalline silicon reduction furnace.
Background
The polysilicon is a main raw material for producing semiconductors and solar photovoltaic products, and the main methods for producing the polysilicon at present comprise an improved Siemens method, a silane method, a fluidized bed method and the like, wherein the improved Siemens method and the silane method both need to deposit carriers in the reduction process, and silicon cores which comprise square silicon cores, round silicon cores and the like are widely used at present.
When the improved Siemens method is adopted and the polycrystalline silicon is prepared by chemical vapor deposition, the graphite component plays a role in conducting electricity and clamping a silicon core. According to the method, high-purity trichlorosilane and hydrogen are used as raw materials, silicon is continuously deposited on an initial silicon core through a chemical vapor deposition reaction at the high temperature of about 1050 ℃, and finally the silicon grows to form a polycrystalline silicon rod. The reaction temperature in the process is maintained by heating of the silicon core or the silicon rod through current, the silicon core in the reduction furnace is in an inverted U shape, and the bottom of the silicon core is connected with the metal electrode through a graphite assembly. The graphite has the characteristics of high temperature resistance, stable property, high conductivity and the like, so the graphite is an ideal conductive medium for connecting the metal electrode and the silicon core.
However, since the lower portion of the silicon rod is connected to a graphite assembly during the reaction, in which a graphite clamp portion for holding a silicon core is gradually embedded inside the silicon rod as the polycrystalline silicon rod grows, the polycrystalline silicon material, i.e., the carbon head material, is produced.
The quality of the carbon head material is judged to be low, and the price is low. Usually, the partial material needs to be removed from the whole silicon rod, the removal length is 80-100 mm, the removal process is difficult, a large amount of manpower is consumed, and cost reduction and efficiency improvement of polycrystalline silicon are not facilitated. On the other hand, because the graphite clamping flaps are embedded deeply, graphite residues are difficult to find during selection, product quality control is not facilitated, and quality accidents are easy to cause.
Disclosure of Invention
In view of the above problems, it is an object of the present invention to provide a graphite assembly for a polycrystalline silicon reduction furnace and a method of using the same to solve the above problems.
According to an aspect of the present invention, there is provided a graphite assembly for a polycrystalline silicon reduction furnace, including:
the middle part of the clamping body is provided with a silicon core mounting hole which penetrates through the clamping body and is used for fixing the silicon core;
the end face of one side of the graphite base is connected with the electrode, and the end face of the other side of the graphite base is connected with the clamping body and is abutted against the end part of one side of the silicon core;
the middle part of the fastener is provided with a fixing hole, the lower end of the fixing hole is sleeved on the graphite base, and the middle part of the fixing hole is abutted against the side face of the clamping body so as to fix the clamping body on the graphite base.
In addition, it is preferable that a side surface of the clamping body and a middle portion of the fixing hole have an inclined contact surface.
In addition, the preferable structure is that the clamping body comprises at least two petal bodies, and a contraction joint is arranged between the adjacent petal bodies; wherein, the first and the second end of the pipe are connected with each other,
when the fixing hole is tightly abutted to the side face of the clamping body, the contraction joint is gradually reduced, and meanwhile, the size of the silicon core mounting hole is reduced.
Preferably, a top portion of the holding member on a side away from the graphite base is a flat surface or a tapered surface.
In addition, it is preferable that the clamping body includes at least two clamping members.
In addition, the preferable structure is that the silicon core mounting hole is a square hole, a round hole or a taper hole.
In addition, the preferable structure is that one end of the graphite base is provided with an installation groove in which the electrode can be embedded.
In addition, the graphite base is preferably formed in a cylindrical shape, and the outer periphery thereof is screwed to the lower end of the fixing hole.
According to another aspect of the present invention, there is provided a method of using a graphite assembly for a polycrystalline silicon reduction furnace, the method being performed using the graphite assembly for a polycrystalline silicon reduction furnace, the method including:
fixing an electrode in an electrode hole of a chassis of a reduction furnace, and sleeving a graphite base on the electrode;
the clamping body is arranged on the graphite base, the fastening piece is sleeved on the clamping body and connected to the graphite base, meanwhile, the silicon core is inserted into the silicon core mounting hole to be abutted against the graphite base, and the fastening piece is screwed, so that the clamping body is fixedly arranged on the surface of the graphite base.
In addition, a preferable embodiment further includes: and after the silicon core grows, separating the silicon rod with the grown silicon core from the fastener.
According to the above description and practice, the graphite assembly for polysilicon reduction furnace and the use method thereof have at least the following advantages:
firstly, among the graphite subassembly, the cramping body of fixed silicon core is the formula structure that sinks, and the later stage will not be by the cladding embedding silicon rod inside, simultaneously, when silicon rod and graphite subassembly separate, will mainly form the section in the last plane department of fastener, can thoroughly realize the separation of graphite subassembly and silicon rod, reduce the degree of difficulty of rejecting the carbon head material simultaneously.
Secondly, the graphite component can realize effective separation of graphite and the silicon rod, thereby being beneficial to quality control and improving the quality control level of polycrystalline silicon.
Thirdly, the weight ratio of the carbon head material can be reduced by more than 50 percent, and the proportion of finished polysilicon is increased, which is beneficial to improving the economic benefit.
To the accomplishment of the foregoing and related ends, one or more aspects of the invention comprise the features hereinafter fully described and particularly pointed out in the claims. The following description and the annexed drawings set forth in detail certain illustrative aspects of the invention. These aspects are indicative, however, of but a few of the various ways in which the principles of the invention may be employed. Further, the present invention is intended to include all such aspects and their equivalents.
Drawings
Other objects and results of the present invention will become more apparent and more readily appreciated as the same becomes better understood by reference to the following description and appended claims, taken in conjunction with the accompanying drawings. In the drawings:
FIG. 1 illustrates an axial cross-sectional structure of a graphite assembly for a polycrystalline silicon reduction furnace according to an embodiment of the present invention;
FIG. 2 illustrates a nose down measurement of a clamp body according to an embodiment of the invention;
fig. 3 shows a flow chart of a method for using the graphite assembly for the polycrystalline silicon reduction furnace according to the present invention.
Description of the reference numerals:
1. a silicon core; 2. a fastener; 3. a clamping body; 4. a graphite susceptor; 5. mounting grooves; 6. silicon core mounting holes.
The same reference numbers in all figures indicate similar or corresponding features or functions.
Detailed Description
In the following description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of one or more embodiments. It may be evident, however, that such embodiment(s) may be practiced without these specific details.
Specific embodiments of the graphite assembly for a polycrystalline silicon reduction furnace according to the present invention will be described in detail with reference to the accompanying drawings.
FIG. 1 illustrates an axial cross-sectional structure of a graphite assembly for a polycrystalline silicon reduction furnace according to an embodiment of the present invention; fig. 2 shows a dive axis measurement of a gripping body according to an embodiment of the present invention.
As shown in fig. 1 and 2, the graphite assembly for a polycrystalline silicon reduction furnace of the present invention includes a fastening member 2, a clamping body 3, and a graphite susceptor 4.
Wherein, the middle part of the clamping body 3 is provided with a silicon core mounting hole 6 which penetrates through and is used for fixing the silicon core 1. One side end face of the graphite base 4 is connected with an electrode, the other side end face of the graphite base 4 is connected with the clamping body 3 and is abutted with one side end part of the silicon core 1, and the graphite base 4 is used as a conductive medium to electrically communicate the electrode and the silicon core 1. The middle part of fastener 2 is provided with the fixed orifices, and the lower pot head of fixed orifices is established on graphite pedestal 4, and the middle part butt of fixed orifices is at the side of supporting body 3 to fix supporting body 3 on graphite pedestal 4.
When the electrode is used, the graphite base 4 is sleeved on the electrode, so that good contact between the electrode and the electrode is ensured, and a basic guarantee is provided for a subsequent chemical vapor deposition reaction. Then, the holding body 3 is abutted against the graphite base 4, the fastening member 2 is sleeved on the holding body 3 and connected to the graphite base 4, and meanwhile, the silicon core 1 is inserted into the silicon core mounting hole 6 and abutted against the graphite base 4, so that smooth proceeding of the reaction is ensured. And finally, the clamping body 3 is clamped and fixed through the fastener 2, so that the silicon core 1 is prevented from entering the graphite component 4 in the growth process, and the assembly of the graphite component for the polycrystalline silicon reduction furnace is completed. Then alright carry out the preparation of polycrystalline silicon, because the holding body 3 of fixed silicon core is the formula structure that sinks, consequently inside its later stage can not be embedded into the silicon rod by the cladding, simultaneously, when the silicon rod separates with the graphite subassembly, will mainly form the section in the last plane department of fastener 2, can thoroughly realize the separation of graphite subassembly and silicon rod, reduce the degree of difficulty of rejecting the carbon head material simultaneously.
Specifically, the graphite base 4 is connected to the holder 3. In practical use, one side end face of the graphite base 4 can be a plane or a mounting groove capable of embedding the clamping body 3 is arranged in the plane, in detail, when one side end face of the graphite base 4 far away from the electrode is a plane, the clamping body 3 may be dislocated in the fastening process, so that the fastening piece 2 is not convenient to screw, but the separation after the growth of the silicon core 1 is completed is more convenient; when the mounting groove of the clamping body 3 is embedded in the plane of one side of the graphite base 4, the position of the clamping body 3 is fixed, displacement is not easy to generate, and the fastening piece 2 is convenient to screw.
Specifically, the side surface of the clamping body 3 and the middle part of the fixing hole have inclined contact surfaces, and the clamping body 3 is tightly abutted on the graphite base 4 through the fixing hole, so that the clamping body 3 is fixed. The shape of the clamping body 3 can be a truncated cone shape with an inclined plane or an inverted T-shaped structure or other shapes. When the clamping body 3 is in a round table shape, the inner wall of the fixing hole is an inclined surface which is abutted with the inclined surface; when the shape of the clamping body 3 is an inverted T-shaped structure, the inner wall of the fixing hole is a right-angle structure matched with the inverted T-shaped structure, so that the clamping body 3 is stably fixed by the fastening piece 2, and meanwhile, the silicon core 1 can be ensured to be stably connected in the growth process by the tight connection, the deposition of silicon cannot enter the inside of the graphite assembly, and the follow-up separation of the silicon rod and the graphite assembly which are completed in growth is facilitated.
Specifically, the clamping body 3 comprises at least two petal bodies, and a contraction joint is arranged between the adjacent petal bodies; when the fixing hole is tightly abutted to the side face of the clamping body 3, the contraction joint gradually becomes small, the size of the silicon core mounting hole 6 becomes small, the silicon core mounting hole 6 gradually clamps the silicon core 1 through the connection process of the fixing hole, and meanwhile, the clamping body 3 sinks on the graphite base 4 to complete the connection and fixation of the graphite component for the polycrystalline silicon reduction furnace. Certainly, when the clamping body 3 is an inverted T-shaped structure, the fixing hole is a right-angle structure matched with the fixing hole, the silicon core mounting hole 6 is a hole position matched with the size of the silicon core 1, shrinkage is not needed, the silicon core 1 can be fixed, the clamping body 3 is directly abutted against the graphite base 4, and the clamping body 3 can be fixed by directly connecting the clamping body with the silicon core 1 in place through the fastening piece 2. The holder 3 may have other shapes, and when the shape of the holder 3 is changed, the shape of the fixing hole that is in close contact with the holder 3 is also changed.
Meanwhile, when the clamping body 3 is a conical or multi-petal combined clamping body, and the fastening piece 2 is gradually fixed on the graphite base, the silicon core mounting holes 6 in the clamping body 3 can be synchronously tightened, so that the limitation and fixation of the silicon core 1 arranged in the clamping body 3 are realized.
More specifically, when the position where the fixing hole is connected to the clamping body 3 is an inclined plane, the upper portion of the fixing hole may be a cylindrical hole or an inverted conical hole. As can be seen from fig. 1, in this embodiment, the upper portion of the fixing hole is a cylindrical hole, which can observe the clamping state of the silicon core 1 in the silicon core mounting hole 6, and determine whether the placing position of the clamping body 3 is accurate, so that the polysilicon can be more effectively reduced from being embedded into the fastener 2 during the preparation process, and the silicon rod and the fastener 2 can be separated from each other. When the upper portion of fixed orifices is the back taper hole, fastener 2 is more stable, inseparable to the fixed of clamping body 3, increases the area of contact of polycrystalline silicon embedding graphite subassembly, simultaneously, increases the stability in silicon rod production stage. The two structures have respective advantages and disadvantages, and can be selectively used according to actual production conditions.
More specifically, the top of the clamping body 3 on the side far away from the graphite base 4 is a plane or a conical surface. As can be seen from fig. 1, in this embodiment, the top of the clamping body 3 is a plane, and in an ideal state, the top has a certain taper, so that the silicon core 1 in the middle of the top can be more stably fixed, but in the preparation process, when a current flows through the top, the light spot on the conical surface is easily generated, i.e., the temperature is too high, and the silicon core 1 is melted, so that the silicon core 1 is damaged. Therefore, in the present embodiment, the top of the clamping body 3 is a plane to avoid the above problems.
Specifically, in this embodiment, the number of the petal bodies is four, and a contraction joint is formed between the adjacent petal bodies, so that the silicon core 1 can be conveniently clamped subsequently under the action of the fastener 2. In the fastening process of the fastener 2, the petal bodies exert pressure on the silicon core 1 in different directions, so that the stress of the silicon core 1 is uniform, and the use effect is improved.
More specifically, the material of the clamping body 3 is graphite, so that the silicon core 1 has good conductivity, and the silicon core 1 is tightly surrounded by the graphite base 4 and the clamping body 3, so that the stable growth of the silicon core 1 is ensured.
More specifically, the silicon core mounting hole 6 is a square hole, a circular hole, or a tapered hole. The specific setting shape is determined according to the shape of the silicon core 1 to be fixed, so that the silicon core 1 is ensured to be firmly clamped and is abutted against the graphite base 4 without displacement.
Specifically, the one end of graphite susceptor 4 is equipped with the mounting groove 5 that can inlay and establish the electrode, and the electrode inlays and establishes in mounting groove 5, and graphite susceptor 4 is cylindrical, and its periphery threaded connection is at the lower extreme of fixed orifices, and further, can also connect through modes such as buckle between graphite susceptor 4 and fastener 2, adjusts according to the actual conditions at scene. In the embodiment of the invention, the graphite pedestal 4 is used as a conductive medium between the electrode and the silicon core 1 and provides a fixed groove for the electrode. When the electrode is used, the electrode is arranged in the electrode hole of the chassis of the reduction furnace, and then the graphite base 4 is sleeved on the electrode, so that the electrode is firmly contacted with the graphite base 4, and the conductive effect is ensured.
Fig. 3 shows a flow chart of a method for using the graphite assembly for the polycrystalline silicon reduction furnace according to the present invention.
As shown in fig. 3, another aspect of the present invention provides a method for using a graphite assembly for a polycrystalline silicon reduction furnace, which is performed using the graphite assembly for a polycrystalline silicon reduction furnace, the method including:
s1, fixing an electrode in an electrode hole of a chassis of a reduction furnace, and sleeving a graphite base 4 on the electrode;
through the steps, the graphite base 4 is ensured to be in good contact with the electrode, and basic guarantee is provided for the subsequent chemical vapor deposition reaction.
S2, the clamping body 3 is arranged on the graphite base 4, the fastening piece 2 is sleeved on the clamping body 3 and connected onto the graphite base 4, meanwhile, the silicon core 1 is inserted into the silicon core mounting hole 6 and abutted against the graphite base 4, and the fastening piece 2 is screwed, so that the clamping body 3 is fixedly arranged on the surface of the graphite base 4.
The silicon core 1 is abutted against the surface of the graphite base 4, and meanwhile, the silicon core mounting hole 6 in the middle of the clamping body 3 is tightened through the fastener 2, so that the silicon core 1 is fixed.
Specifically, the method further comprises the following steps: after the silicon core 1 is grown, the silicon rod grown by the silicon core 1 is separated from the fastener 2. The problem that the graphite component is gradually coated and embedded into the silicon rod along with the growth of the polycrystalline silicon rod is avoided, and the working efficiency and the production quality can be effectively improved.
In order to better explain the graphite component for the polycrystalline silicon reduction furnace and the using method thereof, the invention provides a more specific embodiment.
In the graphite component for the polycrystalline silicon reduction furnace in the embodiment of the invention, the fastening piece 2 is a cylindrical structural piece which is hollow and has a certain wedge angle, and one side end part of the interior of the fastening piece is provided with an internal thread. The clamping body 3 is a truncated cone-shaped split structural member, and a square silicon core mounting hole 6 is formed in the middle of the clamping body 3. The graphite base 4 is a cylindrical concave structural member, and an outer ring thereof is provided with an external thread.
During specific use, install the electrode in the electrode hole on reduction furnace chassis, cup joint graphite base 4 again on fixed electrode, then, place cramping body 3 on graphite base 4, then, detain fastener 2 from the top down on cramping body 3, through screw thread threaded connection on graphite base 4, this moment, revolve on graphite base 4 can, need not to screw up.
Then, the silicon core 1 is inserted through the silicon core mounting hole 6 in the middle of the holder 3 and abutted against the graphite base 4, and at this time, the fastener 2 is slowly tightened, and the holding unit of the holder 3 is also fastened together while the fastener 2 is tightened, thereby fixing the silicon core 1.
Then, covering a bell jar, feeding after a series of operations, reacting trichlorosilane with hydrogen to generate deposited silicon, depositing the deposited silicon on the silicon core 1, gradually growing the silicon rod to cover the clamping body 3, combining the upper end surface of the fastening piece 2 with the silicon rod in the later growth period, and stopping the furnace after the silicon rod grows for more than 100 hours.
And finally, discharging the silicon rod, and only removing the junction layer between the silicon rod and the fastener 2.
When polycrystalline silicon is produced, the clamping body 3 plays a role in conducting electricity and clamping the silicon core 1, and the whole clamping body 3 sinks to the upper end face of the graphite base 4 to play a role in reducing carbon head materials. When trichlorosilane and hydrogen react, the generated silicon gradually deposits on the surface of the silicon core 1 and grows into a silicon rod, the upper end surface of the fastener 2 is contacted and combined with the growing silicon rod, at the moment, the problem that the clamping body 3 is coated by the silicon rod and embedded into the silicon rod is avoided, and the silicon rod and the fastener 2 are convenient to separate.
As can be seen from the above description and practice, the graphite assembly for a polysilicon reduction furnace and the use method thereof have at least the following advantages:
firstly, among the graphite subassembly, the cramping body of fixed silicon core is the formula structure that sinks, and the later stage will not be by the cladding embedding silicon rod inside, simultaneously, when silicon rod and graphite subassembly separate, will mainly form the section in the holistic last plane department of graphite subassembly, can thoroughly realize the separation of graphite accessory and silicon rod, reduce the degree of difficulty of rejecting the carbon head material simultaneously.
And secondly, the silicon rod is reduced to grow into the graphite assembly through the tight fit of the fastener and the clamping body, and the graphite assembly can be ensured to realize the effective separation of graphite and the silicon rod, so that the quality control is facilitated, and the quality control level of polycrystalline silicon is improved.
Thirdly, according to the use method of the graphite assembly, the weight ratio of the carbon head material can be effectively reduced by more than 50 percent, and further the proportion of finished polysilicon is increased, which is beneficial to improving the economic benefit.
The graphite assembly for a polycrystalline silicon reduction furnace according to the present invention is described above by way of example with reference to fig. 1 and 2. However, it will be appreciated by those skilled in the art that various modifications may be made to the graphite assembly for a polysilicon reduction furnace and the method of using the same as set forth in the above description without departing from the scope of the invention. Therefore, the scope of the present invention should be determined by the contents of the appended claims.
Claims (9)
1. A graphite assembly for a polycrystalline silicon reduction furnace, comprising:
the middle part of the clamping body is provided with a through silicon core mounting hole for fixing the silicon core;
the end face of one side of the graphite base is connected with the electrode, and the end face of the other side of the graphite base is connected with the clamping body and is abutted against the end part of one side of the silicon core;
the middle part of the fastener is provided with a fixing hole, the lower end of the fixing hole is sleeved on the graphite base, and the middle part of the fixing hole is abutted against the side face of the clamping body so as to fix the clamping body on the graphite base.
2. The graphite assembly for a polycrystalline silicon reduction furnace according to claim 1,
the side surface of the clamping body and the middle part of the fixing hole are provided with inclined contact surfaces.
3. The graphite assembly for a polycrystalline silicon reduction furnace according to claim 2,
the clamping body comprises at least two petal bodies, and a contraction joint is arranged between every two adjacent petal bodies; wherein the content of the first and second substances,
when the fixing hole is tightly abutted to the side face of the clamping body, the contraction joint is gradually reduced, and meanwhile, the size of the silicon core mounting hole is reduced.
4. The graphite assembly for a polycrystalline silicon reduction furnace according to claim 1,
the top of one side of the clamping body, which is far away from the graphite base, is a plane or a conical surface.
5. The graphite assembly for a polycrystalline silicon reduction furnace according to claim 1,
the silicon core mounting hole is a square hole, a round hole or a taper hole.
6. The graphite assembly for a polycrystalline silicon reduction furnace according to claim 1,
and one end of the graphite base is provided with a mounting groove in which the electrode can be embedded.
7. The graphite assembly for a polycrystalline silicon reduction furnace according to claim 1,
the graphite base is cylindrical, and the periphery of the graphite base is in threaded connection with the lower end of the fixing hole.
8. A method for using a graphite component for a polycrystalline silicon reduction furnace, which is applied to the graphite component for a polycrystalline silicon reduction furnace according to any one of claims 1 to 7, comprising:
fixing an electrode in an electrode hole of a chassis of a reduction furnace, and sleeving a graphite base on the electrode;
the clamping body is arranged on the graphite base, the fastening piece is sleeved on the clamping body and connected to the graphite base, meanwhile, the silicon core is inserted into the silicon core mounting hole to be abutted against the graphite base, and the fastening piece is screwed, so that the clamping body is fixedly arranged on the surface of the graphite base.
9. The method of using the graphite assembly for a polycrystalline silicon reduction furnace according to claim 8, further comprising: and after the silicon core grows, separating the silicon rod with the grown silicon core from the fastener.
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| CN202210820176.6A CN115159528A (en) | 2022-07-13 | 2022-07-13 | Graphite assembly for polycrystalline silicon reduction furnace and using method thereof |
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