CN210314563U - Device for preparing polycrystalline silicon target material by chemical vapor deposition method - Google Patents
Device for preparing polycrystalline silicon target material by chemical vapor deposition method Download PDFInfo
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- CN210314563U CN210314563U CN201921111045.0U CN201921111045U CN210314563U CN 210314563 U CN210314563 U CN 210314563U CN 201921111045 U CN201921111045 U CN 201921111045U CN 210314563 U CN210314563 U CN 210314563U
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Abstract
The utility model relates to a device for preparing polycrystalline silicon target material by chemical vapor deposition. The device comprises a furnace body, a steel cover, a chassis, a metal pipe, a first graphite electrode and a second graphite electrode; the furnace body is a steel cylinder, the top of the furnace body is provided with a steel cover, the bottom of the furnace body is provided with a steel chassis, and the furnace body is sealed by the steel cover and the steel chassis; a tail gas outlet is arranged in the center of the chassis; the upper surface surrounds gas outlet annular evenly distributed has 4 ~ 10 second graphite electrodes, installs adjustable draw-in groove on every second graphite electrode, and the bottom of the metal pipe of perpendicular installation is fixed to the draw-in groove internal fixation, and the bottom and the second graphite electrode electricity of metal pipe are connected. The utility model comprehensively considers the structures of the sputtering sources of the chemical vapor deposition method and the magnetron sputtering method to obtain the polycrystalline silicon target material directly jointed on the substrate tube.
Description
Technical Field
The utility model relates to a polycrystalline silicon target technical field, concretely relates to device of chemical vapor deposition preparation polycrystalline silicon target.
Background
The polycrystalline silicon target material is used as an elemental sputtering source which is easy to excite, low in cost and large in yield, is used in a magnetron sputtering device to prepare silicon-related films, and has important application in the information industry and the energy industry.
The target material is used as a main consumable material of the magnetron sputtering coating process, and is related to the quality and the cost of coating. At present, the main preparation methods of the polycrystalline silicon target material are a powder metallurgy method and a directional solidification method. The method comprises the following steps of (1) crushing raw material silicon into powder by a powder metallurgy method, and sintering after compression molding to obtain a polysilicon target material with a preset shape; the directional solidification method is to melt raw material silicon, perform directional solidification to obtain polycrystalline silicon ingots, and then perform cutting to prepare the polycrystalline silicon target material. Both of them need to be reprocessed on the basis of raw material silicon so as to obtain the polycrystalline silicon target material, which causes more production process flows, complex process, more consumed manpower and material resources and increased cost. How to produce a polysilicon target material with high utilization rate at low cost and high efficiency is a problem which needs to be solved urgently at present.
Chemical Vapor Deposition (CVD) is a process for producing a solid deposit by chemical reaction of gaseous substances on a high-temperature substrate, and is widely used for refining of semiconductor raw materials, production of high-quality semiconductor single crystal films (epitaxial growth films), growth of polycrystalline films, amorphous films, and formation of single crystal and amorphous insulating films. It roughly comprises the following processes: 1. the raw material gas (reaction gas) reaches the surface of the substrate; 2. the reaction gas is absorbed by the surface of the substrate; 3. diffusion of the reactant gas to the substrate surface; 4. reaction and nucleation occur on the surface of the substrate; 5. diffusion of the product from the surface into the matrix; 6. the gas by-product diffuses from the inside to the outside through the substrate surface and leaves the surface.
In order to improve the production efficiency of the polycrystalline silicon target, the utility model provides a novel device for preparing the polycrystalline silicon target by a chemical vapor deposition method, which aims to prepare the high-purity and high-utilization polycrystalline silicon target with low cost and high efficiency.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a device for preparing polysilicon target material by chemical vapor deposition method aiming at the defects of the prior art. The device introduces a metal tube during preparation, and the metal tube is used as a heat carrier in a chemical vapor deposition method to deposit polycrystalline silicon; and then as a conductive cathode substrate tube in magnetron sputtering, because the outer surface of the conductive cathode substrate tube is already deposited with polycrystalline silicon, the steps of firstly preparing a polycrystalline silicon ingot, then carrying out cutting processing to obtain a polycrystalline silicon target material and then combining the target material and the substrate tube in the prior art are omitted. The utility model comprehensively considers the structures of the sputtering sources of the chemical vapor deposition method and the magnetron sputtering method to obtain the polycrystalline silicon target material directly jointed on the substrate tube.
The technical proposal adopted by the utility model for solving the technical problems is that,
a device for preparing a polycrystalline silicon target by a chemical vapor deposition method comprises a furnace body, a steel cover, a chassis, a metal tube, a first graphite electrode and a second graphite electrode;
the furnace body is a steel cylinder, the top of the furnace body is provided with a steel cover, the bottom of the furnace body is provided with a steel chassis, and the furnace body is sealed by the steel cover and the steel chassis;
a tail gas outlet is arranged in the center of the chassis; 4-10 second graphite electrodes are uniformly distributed on the upper surface in an annular mode around the air outlet, an adjustable clamping groove is mounted on each second graphite electrode, the bottom end of a vertically-mounted metal tube is fixed in each clamping groove, and the bottom end of the metal tube is electrically connected with the second graphite electrodes;
on the chassis, two sides of each second graphite electrode are respectively provided with an air inlet pipe;
the furnace body comprises a furnace body barrel, a first graphite electrode, a second graphite electrode, a metal tube, a second graphite electrode, a horizontal moving plate, a first graphite electrode, an adjustable clamping groove, a metal tube and a second graphite electrode, wherein the number of the vertical sliding grooves is the same as that of the second graphite electrode;
the first graphite electrode and the second graphite electrode have different polarities;
the position of the horizontal moving plate can be adjusted in the vertical direction along the sliding groove;
the air inlet pipes on the base plate are all arranged on the radial connecting line of the second graphite electrode and the air outlet;
the SiHC13The purity of the gas is 99.999999%; the purity of the hydrogen is 99.9999%;
the specified thickness is preferably 2-20 mm;
the metal pipe is a molybdenum pipe, a stainless steel pipe or a titanium pipe;
the size of the metal pipe is preferably 100-300 mm in outer diameter, 90-290 mm in inner diameter and 150-1500 mm in height.
The utility model discloses a substantive characteristics do:
the prior art generally comprises the steps of growing a polycrystalline silicon ingot by directional solidification, then cutting the silicon ingot to obtain a silicon target, and then jointing the silicon target and a cathode substrate pipe in magnetron sputtering. The utility model discloses in, the metal pipe that introduces in the reduction furnace is as the heat carrier in the chemical vapor deposition method earlier, deposits polycrystalline silicon, is the electrically conductive cathode substrate pipe in the magnetron sputtering again, has directly grown one deck polycrystalline silicon target on cathode substrate pipe in other words, and simple and convenient has improved production efficiency widely.
The utility model has the advantages that:
1. the production efficiency is high. The utility model discloses a metal pipe is as the heat carrier of chemical vapor deposition in-process, directly at metal outside of tubes surface deposit polycrystalline silicon, realizes the direct forming of polycrystalline silicon column target, need not to carry out secondary growth and subsequent cutting process to raw materials silicon and handles. The production steps of polycrystalline silicon ingot casting, cutting processing, substrate tube jointing and the like are saved, the production procedures are reduced, and the production efficiency is improved.
2. The target material has high purity. The purity of the polycrystalline silicon target material obtained by chemical vapor deposition is high and is more than 99.9999 percent.
3. The crystal grain orientation of the target material is consistent, and the crystal grains are uniform. The film grown by the chemical vapor deposition method can obtain a polycrystalline film with a columnar structure under the condition of high nucleation rate on the surface of the substrate, and can ensure the consistency of the performance of the film.
4. The target material is firmly combined with the metal tube. Because the polycrystalline silicon target material is directly deposited on the outer surface of the substrate metal tube, the cylindrical target material and the cylindrical substrate tube do not need to be jointed together by using an adhesive material such as indium or tin and the like as in the preparation of a traditional magnetron. Further, since atoms between the silicon target material and the metal tube are also diffused mutually, the adhesion is good.
5. The metal tube can be recycled. After the polycrystalline silicon target material is deposited on the metal tube, a magnetic box, a refrigerant circulating device, a rotary driving device and the like are additionally arranged in the metal tube, and the metal tube can be used as a sputtering source. After the use is finished, the metal tube can be reused in a reduction furnace as a heat carrier deposition target material through acid washing or alkali washing.
6. The operation is simple. The metal pipe is used as a heat carrier, preheating and high-voltage breakdown are not needed during heating, common electrical equipment is used, and the operation is simple.
7. The cost is low. Because common electrical equipment is used and production procedures are reduced, the consumption of manpower and material resources in the production process is reduced, and the cost is reduced.
Drawings
Fig. 1 is a schematic radial cross-sectional view of a reducing furnace structure used in the method for growing a polycrystalline silicon target according to the present invention.
Fig. 2 is a schematic view of the bottom plate of the reduction furnace used in the method for growing the polycrystalline silicon target according to the present invention.
In the figure, 1 is a steel cover, 2 is a horizontal moving plate, 3 is a first graphite electrode, 4 is a furnace body, 5 is a metal tube, 6 is an air outlet, 7 is a second graphite electrode, 8 is an air inlet tube, and 9 is a chassis.
Detailed Description
The present invention will be further described with reference to the following examples and accompanying drawings, which are not intended to limit the scope of the claims of the present application.
The structure of the reducing furnace used in the method for growing the polycrystalline silicon target material of the present invention is shown in fig. 1 and 2. The reducing furnace comprises a furnace body 4, a steel cover 1, a chassis 9, a metal pipe 5, a first graphite electrode 3 and a second graphite electrode 7;
the furnace body 4 is a steel cylinder, the top of the furnace body is provided with a steel cover 1, the bottom of the furnace body is provided with a steel chassis 9, and the furnace body 4 is sealed by the steel cover and the steel chassis;
a tail gas outlet 6 is arranged in the center of the chassis 9; the upper surface is uniformly distributed with 8 second graphite electrodes 7 annularly around the gas outlet 6, each second graphite electrode 7 is provided with an adjustable clamping groove, the bottom end of a metal tube 5 which is vertically arranged is fixed in each clamping groove, and the bottom end of the metal tube 5 is electrically connected with the second graphite electrode 7;
an air inlet pipe 8 is arranged on the chassis 9 at two sides of each second graphite electrode 7; the air inlet pipes 8 are all arranged on the radial connecting line of the second graphite electrode 7 and the air outlet 6;
the furnace body 4 is characterized in that 8 longitudinal sliding grooves are formed in the cylinder wall of the upper part of the cylinder body, one end of a horizontal moving plate 2 is fixed in the sliding grooves of the cylinder wall, the other end of the horizontal moving plate is positioned right above a second graphite electrode and is provided with a first graphite electrode 3, an adjustable clamping groove is also formed in the first graphite electrode 3, the top end of a metal tube 5 is fixed in the clamping groove, and the top end of the metal tube 5 is electrically connected with the first graphite electrode 3;
the number of the horizontal moving plates 2 is 8, the distribution positions of the horizontal moving plates correspond to the second graphite electrodes 7, and the horizontal moving plates can be adjusted in the vertical direction along the sliding grooves;
the first graphite electrode 3 and the second graphite electrode 7 have different polarities and are respectively connected with the anode and the cathode of a power supply, and the projection positions are overlapped;
the method for preparing the polycrystalline silicon target material by the chemical vapor deposition method comprises the following steps:
firstly, filling hydrogen into a reduction furnace in advance, switching on a power supply, electrically heating a metal pipe 5 to 1050-1100 ℃, and reacting high-purity SiHC13Spraying a mixed gas consisting of gas and high-purity hydrogen at the speed of 10-250 m/s through an air inlet pipe 8, feeding the mixed gas into a reduction furnace, opening an air outlet 6, keeping the pressure intensity in the reduction furnace constant at 0.1-0.2 MPa, and carrying out chemical vapor deposition reaction on the outer surface of a metal pipe 5 to generate polycrystalline silicon;
wherein the molar ratio SiHC1 in the mixed gas3Gas: hydrogen gas＝1：3～5；
And step two, discharging the residual tail gas through a gas outlet 6 while performing the hydrogen reduction reaction in the step one, collecting, separating, purifying and purifying to obtain H2、SiHC13Gas, which is reused as raw material of the reactor;
and thirdly, reacting for 2-20 hours, stopping the furnace when the polycrystalline silicon is deposited to the specified thickness, taking out the metal tube 5 deposited with the polycrystalline silicon, and performing later-stage processing treatment on the surface of the polycrystalline silicon to obtain the polycrystalline silicon target directly jointed on the substrate metal tube 5.
After obtaining the polysilicon target material bonded on the substrate metal tube 5, according to the prior art, a magnetic box is inserted into the metal tube 5, a magnet unit is assembled in the magnetic box, and a refrigerant circulating device and a rotation driving device are additionally installed to obtain a magnetron which can be used as a sputtering source for magnetron sputtering.
The SiHC13The purity of the gas is 99.999999%; the purity of the hydrogen gas was 99.9999%.
The metal tube is a molybdenum tube, a stainless steel tube or a titanium tube.
The size of the metal pipe is preferably 100-300 mm in outer diameter, 90-290 mm in inner diameter and 150-1500 mm in height.
The specified thickness is preferably 2-20 mm.
Example 1
The thickness (difference between the inner radius and the outer radius) of the cylindrical target material required by the product designed by the method of the embodiment is 6mm, the length is 1000mm, the inner diameter of the cylindrical target material is equal to the outer diameter of the metal tube, and the molybdenum metal tube 5 adopted by the embodiment has the outer diameter of 100mm, the inner diameter of 90mm and the length of 1020 mm.
The diameter of the furnace body 4 is 1200 mm; the diameter of the air inlet pipe 8 is 13 mm; the diameter of the air outlet 6 is 100 mm;
the method for growing the polycrystalline silicon target comprises the step of reducing high-purity SiHC1 by hydrogen3The process of recovering tail gas and taking out the metal tube deposited with the polycrystalline silicon comprises the following specific steps:
firstly, filling hydrogen into a reduction furnace in advance, switching on a power supply, electrically heating a molybdenum metal pipe to 5-1100 ℃, and adding commercial high-purity (purity 99.999999%) SiHC13And 99.9999% pure hydrogen in a mass ratio of 1: 5, spraying the mixture through an air inlet pipe 8 at a speed of gradually increasing 95m/s from the beginning to 104m/s at the end, feeding the mixture into a reduction furnace, opening an air outlet 6, maintaining the pressure in the reduction furnace at 0.1MPa, and carrying out chemical vapor deposition reaction on the outer surface of a molybdenum metal pipe 5 heated to 1100 ℃ to generate polycrystalline silicon. To ensure a deposition rate of 1mm/h, SiHC1 was applied over 6h3The gas flow rate is gradually and linearly increased from 142kg/H to 157kg/H, H2The flow rate was gradually increased linearly from 10kg/h to 12 kg/h.
Secondly, the residual tail gas is discharged through a gas outlet 6 while the first step hydrogen reduction reaction is carried out, and then H is obtained through separation, purification and purification2、SiHC13Can be reused as raw material of the reactor.
And thirdly, under the condition that the deposition rate is 1mm/h, stopping the furnace when the polycrystalline silicon is deposited to the thickness of 6mm after reacting for 6 hours. The molybdenum metal tube 5 with the deposited polysilicon is taken out, and the polysilicon surface is subjected to post-processing (such as grinding and polishing) to obtain the polysilicon target directly bonded on the molybdenum substrate metal tube 5.
After obtaining the polysilicon target material bonded to the molybdenum substrate metal tube 5, a magnet box is inserted into the molybdenum substrate metal tube 5, a magnet unit is assembled in the magnet box, and a refrigerant circulating device and a rotation driving device are additionally installed to obtain a magnetron which can be used as a sputtering source for magnetron sputtering. (the steps of inserting a magnetic box, obtaining a magnetron, etc. are known in the art, and reference may be made specifically to the patent "CN 201680012047-rotary cathode unit for magnetron sputtering device")
The specification of the polycrystalline silicon target product obtained by the method of the embodiment is as follows:
purity of the polycrystalline silicon target material: 99.9999 percent
Conductivity type: p or N
Impurity content: (Al/Ca/Fe/As/Mo/Sb) < 0.1. mu.g/g
Surface roughness: ra <1.6 μm
The analysis of chemical components in the data is carried out according to the regulation of GB/T245782-.
It can be seen from the above embodiment that the utility model discloses directly regard as the heat carrier among the chemical vapor deposition method with the molybdenum tube, deposit polycrystalline silicon, regard it as the electrically conductive cathode substrate pipe in the magnetron sputtering again, because of its surface has already deposited polycrystalline silicon, so saved polycrystalline silicon ingot casting, cutting process, the step of joint substrate pipe. The polycrystalline silicon target material is directly deposited on the molybdenum tube, so that the production procedures are reduced, the production efficiency is improved, and the cost in the production process is reduced.
The utility model discloses the nothing is mentioned the part and is applicable to prior art.
Claims (2)
1. A device for preparing polycrystalline silicon target by a chemical vapor deposition method is characterized in that the device is a reduction furnace and comprises a furnace body, a steel cover, a chassis, a metal tube, a first graphite electrode and a second graphite electrode;
the furnace body is a steel cylinder, the top of the furnace body is provided with a steel cover, the bottom of the furnace body is provided with a steel chassis, and the furnace body is sealed by the steel cover and the steel chassis;
a tail gas outlet is arranged in the center of the chassis; 4-10 second graphite electrodes are uniformly distributed on the upper surface in an annular mode around the air outlet, an adjustable clamping groove is mounted on each second graphite electrode, the bottom end of a vertically-mounted metal tube is fixed in each clamping groove, and the bottom end of the metal tube is electrically connected with the second graphite electrodes;
on the chassis, two sides of each second graphite electrode are respectively provided with an air inlet pipe;
the furnace body comprises a furnace body barrel, a first graphite electrode, a second graphite electrode, a metal tube, a second graphite electrode, a horizontal moving plate, a first graphite electrode, an adjustable clamping groove, a metal tube and a second graphite electrode, wherein the number of the vertical sliding grooves is the same as that of the second graphite electrode;
the first graphite electrode and the second graphite electrode have different polarities.
2. The apparatus according to claim 1, wherein the gas inlet tube of the base is located on a radial line connecting the second graphite electrode and the gas outlet.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110257909A (en) * | 2019-07-16 | 2019-09-20 | 河北工业大学 | A kind of chemical vapour deposition technique prepares the method and device thereof of polycrystalline silicon target |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110257909A (en) * | 2019-07-16 | 2019-09-20 | 河北工业大学 | A kind of chemical vapour deposition technique prepares the method and device thereof of polycrystalline silicon target |
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