CN115341278A - Single crystal furnace water-cooling heat shield prepared from copper or copper alloy and preparation method thereof - Google Patents

Single crystal furnace water-cooling heat shield prepared from copper or copper alloy and preparation method thereof Download PDF

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CN115341278A
CN115341278A CN202210897951.8A CN202210897951A CN115341278A CN 115341278 A CN115341278 A CN 115341278A CN 202210897951 A CN202210897951 A CN 202210897951A CN 115341278 A CN115341278 A CN 115341278A
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water
inner cylinder
conical section
annular space
section inner
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CN115341278B (en
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马明月
庾高峰
张航
李雷
宁超
王文斌
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Shaanxi Sirui Advanced Materials Co Ltd
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Shaanxi Sirui Advanced Materials Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B27/00—Single-crystal growth under a protective fluid
    • C30B27/02—Single-crystal growth under a protective fluid by pulling from a melt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
    • B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/08—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a single crystal furnace water-cooling heat shield prepared from copper or copper alloy and a preparation method thereof, and relates to the technical field of copper alloy preparation. The preparation method of the water-cooling heat shield of the single crystal furnace comprises the following steps: s1, preparing an inner cylinder and an outer cylinder; s2, preparing a flow guide passage; s3, preparing an annular space. The invention optimizes the temperature distribution in the growth process of the monocrystalline silicon, and matches with the pulling speed, thereby finally achieving the purposes of increasing the pulling speed and improving the production efficiency.

Description

Single crystal furnace water-cooling heat shield prepared from copper or copper alloy and preparation method thereof
Technical Field
The invention relates to the technical field of copper alloy preparation, in particular to a single crystal furnace water-cooling heat shield prepared from copper or copper alloy and a preparation method thereof.
Background
Monocrystalline silicon is one of the most important monocrystalline materials in the world as a key supporting material in the modern information society, and not only is the main functional material for developing computers and integrated circuits, but also the main functional material in the industries of photovoltaic power generation and utilization of solar energy and semiconductors.
The Czochralski method is the most commonly used method for producing single-crystal silicon, the growth rate of which is greatly influenced by the longitudinal temperature gradient of the crystal near the crystallization interface, and the greater the temperature gradient of the crystal near the crystallization interface, the faster the single-crystal silicon grows. Since the transformation of silicon from a liquid to a solid requires the release of a large amount of heat, increasing the longitudinal temperature gradient of the crystal near the crystallization interface is the fastest efficient way to dissipate the heat.
The single crystal furnace is necessary equipment in the process of converting polycrystalline silicon into monocrystalline silicon, and is equipment for melting polycrystalline materials such as the polycrystalline silicon and the like by using a graphite heater and the like in an inert gas environment and then growing a crystal bar by upward czochralski method. The crystal bar can be used for manufacturing dislocation-free single crystal materials. And in the process of moving the crystal bar upwards, the crystal bar needs to be cooled, so that the crystal bar is fixedly formed. The existing cooling mode is that a water-cooling heat shield is fixedly arranged at a certain height position in a single crystal furnace, cooling liquid is introduced into the water-cooling heat shield, and a crystal bar is cooled through the water-cooling heat shield when moving upwards and passing through the water-cooling heat shield.
The monocrystalline silicon can be influenced by the temperature, the pulling speed and the rotating speed, the crucible tracking speed and the rotating speed, the flow rate of protective gas and other factors in the growth process. The temperature mainly determines whether the crystal can be formed, and the speed directly influences the inherent quality of the crystal, and the influence can only be known through detection after the single crystal is pulled out. The thermal field with proper temperature distribution not only can lead the single crystal to grow smoothly, but also has higher quality; if the temperature distribution of the thermal field is not reasonable, various defects are easy to generate in the process of growing the single crystal, the quality is influenced, and even the phenomenon of crystal change can occur in serious conditions, and the single crystal can not grow.
Disclosure of Invention
Aiming at the problems, the invention provides a single crystal furnace water-cooling heat shield prepared by copper or copper alloy and a preparation method thereof.
The technical scheme of the invention is as follows:
the utility model provides an utilize single crystal growing furnace water-cooling heat shield of copper or copper alloy preparation, includes conic section urceolus and conic section inner tube that cup joints each other, the top of conic section urceolus and conic section inner tube is passed through annular flange joint, and conic section urceolus bottom is equipped with straight section urceolus, conic section inner tube bottom is equipped with straight section inner tube, straight section urceolus and straight section inner tube bottom are connected through annular lower flange, form the first annular space that is used for the water-passing between conic section urceolus and the conic section inner tube, form the second annular space that is used for the water-passing between straight section urceolus and the straight section inner tube, be equipped with annular baffle between first annular space and the second annular space, inlet tube and outlet pipe have been seted up to the upper flange bilateral symmetry,
two water inlet baffles are arranged in the first annular space and correspond to the lower part of the water inlet pipe, the water inlet baffles extend to the bottom of the first annular space, one water inlet baffle is connected with the bottom of the first annular space, the bottom of the other water inlet baffle is provided with a water inlet, a plurality of annular flow guide baffles are arranged in the first annular space, each flow guide baffle is parallel and arranged at equal intervals, each flow guide baffle is connected with one water inlet baffle and is provided with an opening, the water inlet baffles connected with two adjacent flow guide baffles are different, so that a flow guide passage which is folded and ascended is formed in the first annular space by the flow guide baffles, the flow guide baffle positioned at the lowest part is connected with the water inlet baffle provided with the water inlet, the flow guide baffle positioned at the highest part extends to the right side of the water outlet pipe and is connected with the upper flange, a water activating area is formed in the first annular space on the right side of the flow guide baffle positioned at the highest part, and a movable baffle for flow guide is arranged in the middle of the water activating area;
the inside honeycomb duct that is equipped with the spiral and descends the formula of second annular space, the top of honeycomb duct is connected with the reposition of redundant personnel mouth that is equipped with on the ring baffle that is located between two water inlet baffle, behind the honeycomb duct extension to second annular space's bottom with the inside delivery port that is equipped with of lower flange is connected.
Furthermore, the movable baffle comprises a water passing plate and a rotating plate, the water passing plate is connected with the conical section inner cylinder in a sliding mode, the rotating plate is connected with the water passing plate in a rotating mode, a sliding block is arranged on the side wall, corresponding to one side of the conical section inner cylinder, of the middle of the water passing plate, the sliding groove is formed in the side wall of the conical section inner cylinder and connected with the bottom of the sliding groove in a vertical sliding mode, the bottom of the sliding block is connected with the bottom of the sliding groove through a spring, a plurality of groups of water passing holes are arranged on the surface of the water passing plate in an equidistant mode, water baffles are arranged on the upper surface of the water passing plate corresponding to one of the two adjacent water passing holes in a sliding mode, one water passing hole is arranged on the water baffle at each group, inverted T-shaped limiting blocks are arranged on the two sides of the bottom of the water passing plate and connected with the T-shaped sliding blocks on the two sides of the upper surface of the water passing plate, the water passing plate is connected with the middle of each water passing plate through a connecting rod to enable each water baffle to slide synchronously, a sliding rod is arranged on the side wall, a sliding rod corresponding to one side of the conical section inner cylinder, the middle of the lowest water baffle is provided with the sliding rod groove, and one section inner cylinder, one section is connected with the sliding grooves, and one section of the sliding rod groove, so that one section of the sliding block is shifted to drive the sliding block to slide rod between the two adjacent water passing holes. The movable baffle is arranged, so that the flowability of cooling water in the water-activating area can be effectively improved, and the occurrence of a dead water area is avoided.
Furthermore, a rotating shaft is arranged in the middle of the side wall of one side of the water passing plate corresponding to the rotating plate, and the rotating shaft is rotatably connected with the rotating plate. Through the arrangement of the rotating shaft and the rotating plate, water flow can drive the rotating plate to rotate along the water passing plate when flowing through the rotating plate, and the flowability of cooling water is further improved.
Furthermore, it is the slope setting to cross water board and rotor plate, crosses water board and rotor plate both ends and is a section horizontal plane, crosses the water board and is located the horizontal plane upper surface of top and be equipped with be used for with upper flange bottom surface magnetism inhale the butt joint and play supplementary fixed effect's magnetic sheet, cross the water board and be located the horizontal plane lower surface of below also be equipped with be used for with in the first annular space second top the magnetic sheet of water conservancy diversion baffle magnetism inhale the butt joint and play supplementary fixed effect.
Furthermore, the water hole is 5 groups, the breakwater is 3, and each group of water hole is provided with 3 water holes. Through the setting of crossing the water hole can make the water board select to shelter from the different modes of crossing the water board in quantity that crosses the water hole under corresponding high velocity of flow and the two kinds of circumstances of low velocity of flow, thereby improved water efficiency to the mobility in running water district has been guaranteed.
The preparation method of the single crystal furnace water-cooling heat shield prepared from the copper or the copper alloy comprises the following steps:
s1, preparing an inner cylinder and an outer cylinder: selecting pure copper or copper alloy as a raw material, integrally forming a conical section outer cylinder, a conical section inner cylinder, a straight section outer cylinder and a straight section inner cylinder by spinning, carrying out solution treatment on the formed conical section outer cylinder, conical section inner cylinder, straight section outer cylinder and straight section inner cylinder, wherein the temperature of the solution treatment is 950-980 ℃, and the time of the solution treatment is 2h, and then carrying out aging treatment on the conical section outer cylinder, conical section inner cylinder, straight section outer cylinder and straight section inner cylinder after the solution treatment to obtain a complete conical section outer cylinder, conical section inner cylinder, straight section outer cylinder and straight section inner cylinder;
s2, preparing a flow guide passage: connecting a water inlet baffle and a flow guide baffle which are prefabricated by forging to the complete conical section inner cylinder obtained in the step S1 in a welding mode, reserving the position of a water activating area, and then installing a movable baffle;
s3, preparing an annular space: welding the complete conical section outer cylinder and the upper flange obtained in the step S1 with the conical section inner cylinder respectively to form a first annular space, welding and installing an annular baffle at the bottom of the first annular space, welding and installing a straight section inner cylinder below the conical section inner cylinder, welding and installing a straight section outer cylinder below the conical section outer cylinder, connecting a prefabricated forged guide pipe to the complete straight section inner cylinder obtained in the step S1 in a welding manner, and welding the complete straight section outer cylinder and a lower flange obtained in the step S1 with the straight section inner cylinder respectively to form a second annular space;
further, the welding mode is argon arc welding, gas shield welding or electron beam welding. The conical section outer cylinder, the conical section inner cylinder, the straight section outer cylinder and the straight section inner cylinder are firmly connected through welding.
Further, the copper alloy in the step S1 is CuZr, cuCrZr, cuCrNbZr or CuNi 2 And (3) Si. The heat conductivity of copper and copper alloy is about 20 times of that of stainless steel, so that the heat conduction efficiency of the water-cooling heat shield structure can be effectively improved, and the pulling efficiency of monocrystalline silicon is improved.
Furthermore, the temperature of the aging treatment in the step S1 is 395-435 ℃, and the time of the aging treatment is 2-6h. The overall strength and the thermal conductivity of the material are improved through aging treatment.
The beneficial effects of the invention are:
(1) According to the water-cooling heat shield of the single crystal furnace, water cooling is enabled to extend from the middle part to the two ends of the water-cooling heat shield through the method of upper conical section cooling and lower straight section cooling, the cooling effect is better, the temperature distribution in the growth process of monocrystalline silicon is optimized and matched with the pulling speed, and the purposes of increasing the pulling speed and improving the production efficiency are finally achieved.
(2) According to the water-cooling heat shield of the single crystal furnace, the water-activating area and the movable baffle plate arranged in the water-activating area are arranged, so that the circulation of cooling water can be improved, the occurrence of a dead water area is effectively avoided, the water-passing plate on the movable baffle plate can be adjusted to shield a certain number of water-passing holes so as to select different modes according to different cooling water flow rates, a part of the water-passing holes are shielded at a low flow rate, all the water-passing holes are opened at a high flow rate, and meanwhile, the rotation of the rotating plate is matched to dredge the cooling water flowing through the water-activating area, so that the smoothness of water flow is ensured, and the generation of the dead water area and the generation of gasification phenomena are further avoided.
(3) According to the preparation method of the water cooling and heating screen of the single crystal furnace, copper or copper alloy is adopted as a raw material to be integrally formed, so that the strength of the water cooling and heating screen is improved, a stainless steel product is replaced to improve the heat conduction rate of the water cooling and heating screen structure, meanwhile, the water cooling and heating screen has good high temperature resistance, can bear high service temperature in the single crystal furnace, has the heat conductivity which is nearly 20 times of that of stainless steel, can effectively improve the heat conduction efficiency of the water cooling and heating screen structure, improves the pulling efficiency of monocrystalline silicon, reduces the hardness through solid solution treatment, facilitates subsequent shape correction treatment, and improves the overall strength and the heat conductivity of materials through aging treatment.
Drawings
FIG. 1 is a schematic view of the whole structure of a water cooling and heating screen of a single crystal furnace according to the present invention;
FIG. 2 is a schematic view of the internal structure of the first annular space at one side of the water inlet pipe of the water cooling and heating screen of the single crystal furnace of the present invention;
FIG. 3 is a schematic view of the internal structure of the first annular space at one side of the movable baffle of the water cooling and heating shield of the single crystal furnace;
FIG. 4 is a schematic view of the internal structure of the first annular space at one side of the water outlet pipe of the water cooling and heating screen of the single crystal furnace according to the present invention;
FIG. 5 is a schematic view of the internal structure of the first annular space and the second annular space at one side of the movable baffle of the water cooling and heating screen of the single crystal furnace;
FIG. 6 is a schematic structural view of a movable baffle plate of the water-cooling heat shield of the single crystal furnace of the invention;
FIG. 7 is a top view of a movable baffle plate of a water-cooling heat shield of the single crystal furnace after a water baffle plate slides;
FIG. 8 is a schematic view of the bottom structure of a movable baffle plate after a rotating plate of a water-cooling heat shield of the single crystal furnace rotates;
FIG. 9 is a schematic view of a sliding connection structure of a water baffle and a water passing plate of the water-cooling heat shield of the single crystal furnace of the invention;
FIG. 10 is a flow chart of the preparation method of the water-cooling heat shield of the single crystal furnace of the invention.
Wherein, 1-conical section outer cylinder, 2-conical section inner cylinder, 21-chute, 22-sliding rod groove, 3-upper flange, 31-water inlet pipe, 32-water outlet pipe, 4-straight section outer cylinder, 5-straight section inner cylinder, 6-lower flange, 61-water outlet, 7-first annular space, 71-water inlet baffle, 72-water inlet, 73-flow guide baffle, 74-opening, 75-flow guide passage, 76-water active area, 8-second annular space, 81-annular baffle, 82-flow guide pipe, 83-flow split port, 9-movable baffle, 91-water passing plate, 911-water passing hole, 912-T type groove, 92-rotating plate, 93-sliding block, 931-spring, 94-water blocking plate, 941-limiting block, 95-connecting rod, 96-sliding rod, 97-rotating shaft and 98-magnetic sheet.
Detailed Description
Example 1
As shown in figures 1 and 5, a single crystal furnace water-cooling heat shield prepared by copper or copper alloy comprises a conical section outer cylinder 1 and a conical section inner cylinder 2 which are mutually sleeved, the tops of the conical section outer cylinder 1 and the conical section inner cylinder 2 are connected through an annular upper flange 3, the bottom of the conical section outer cylinder 1 is provided with a straight section outer cylinder 4, the bottom of the conical section inner cylinder 2 is provided with a straight section inner cylinder 5, the bottoms of the straight section outer cylinder 4 and the straight section inner cylinder 5 are connected through an annular lower flange 6, a first annular space 7 for water passing is formed between the conical section outer cylinder 1 and the conical section inner cylinder 2, a second annular space 8 for water passing is formed between the straight section outer cylinder 4 and the straight section inner cylinder 5, an annular baffle 81 is arranged between the first annular space 7 and the second annular space 8, and water inlet pipes 31 and water outlet pipes 32 are symmetrically arranged at two sides of the upper flange 3,
as shown in fig. 2-5, two water inlet baffles 71 are arranged in the first annular space 7 and below the water inlet pipe 31, the water inlet baffles 71 extend to the bottom of the first annular space 7, one water inlet baffle 71 is connected with the bottom of the first annular space 7, a water inlet 72 is arranged at the bottom of the other water inlet baffle 71, 9 annular flow guide baffles 73 are arranged in the first annular space 7, each flow guide baffle 73 is parallel and equidistantly arranged, each flow guide baffle 73 is connected with one water inlet baffle 71 and has an opening 74 with the other water inlet baffle 71, the water inlet baffles 71 connected with the two adjacent flow guide baffles 73 are different, so that the flow guide baffles 73 form a flow guide passage 75 which is folded upwards in the first annular space 7, one flow guide baffle 73 positioned at the lowest position is connected with the water inlet baffle 71 provided with the water inlet 72, one flow guide baffle 73 positioned at the highest position extends to the right side of the water outlet pipe 32 and is connected with the upper flange 3, a live water area 76 is formed in the first annular space 7 at the right side of the one flow guide baffle 73 at the highest position, and a live water area 76 is provided with a movable baffle 9 for guiding is arranged in the middle part;
as shown in fig. 5, a spirally descending guide pipe 82 is arranged in the second annular space 8, the upper part of the guide pipe 82 is connected with a flow dividing port 83 arranged on the annular baffle 81 between the two water inlet baffles 71, and the guide pipe 82 extends to the bottom of the second annular space 8 and then is connected with a water outlet 61 arranged in the lower flange 6;
as shown in fig. 6-9, the movable baffle 9 comprises a water passing plate 91 slidably connected to the tapered inner cylinder 2 and a rotating plate 92 rotatably connected to the water passing plate 91, a rotating shaft 97 is provided at the middle of the side wall of the corresponding side of the water passing plate 91 and the rotating plate 92, the rotating shaft 97 is rotatably connected to the rotating plate 92, a slider 93 is provided at the side wall of the middle of the water passing plate 91 corresponding to the tapered inner cylinder 2, the slider 93 is slidably connected to the chute 21 provided at the side wall of the tapered inner cylinder 2 up and down, the bottom of the slider 93 is connected to the bottom of the chute 21 through a spring 931, 5 groups of water passing holes 911 arranged at equal intervals are provided on the surface of the water passing plate 91, a water baffle 94 is slidably provided on the upper surface of the water passing plate 91 corresponding to one group of the water passing holes 911 in two adjacent groups of water passing holes 911, the water baffle 94 is provided every group of water passing holes 911, the water baffle 94 is provided with 3 water passing holes 911 in each group, two sides of the bottom of the water baffle plate 94 are provided with inverted T-shaped limiting blocks 941, the limiting blocks 941 are slidably connected with T-shaped grooves 912 arranged on two sides of the upper surface of the water passing plate 91, the middle part of each water baffle plate 94 is connected through a connecting rod 95 for enabling each water baffle plate 94 to slide synchronously, the side wall of the middle part of the water baffle plate 94 positioned at the lowest part, which corresponds to one side of the conical section inner cylinder 2, is provided with a sliding rod 96, the sliding rod 96 is slidably connected with a sliding rod groove 22 arranged on the side wall of the conical section inner cylinder 2, one section of the upper part of the sliding rod groove 22 deviates to the position of the sliding groove 21, so that the sliding rod 96 after deviation drives the water baffle plate 94 to slide to the position between two adjacent groups of water passing holes 911, the water passing plate 91 and the rotating plate 92 are both arranged obliquely, two ends of the water passing plate 91 and the rotating plate 92 are both horizontal planes, the magnetic sheets 98 which are used for magnetically butting with the bottom surface of the upper flange 3 and playing an auxiliary fixing role are arranged on the upper surface of the water passing plate 91, the lower surface of the horizontal plane below the water passing plate 91 is also provided with a magnetic sheet 98 which is magnetically connected with the second flow guide baffle 73 above the first annular space 7 and plays a role in auxiliary fixing.
Example 2
This embodiment is substantially the same as embodiment 1, except that: the water holes 911 and the water deflectors 94 are provided in different numbers.
The water holes 911 are 7 groups, the water baffles 94 are 4, and each group of water holes 911 is provided with 4 water holes 911.
Example 3
This embodiment is substantially the same as embodiment 1, except that: the number of the baffle plates 73 is different.
In the first annular space 7, 10 annular deflector baffles 73 are provided.
Example 4
Based on the preparation method of the single crystal furnace water-cooling heat shield prepared by using copper or copper alloy in the embodiment 1, as shown in fig. 10, the method comprises the following steps:
s1, preparing an inner cylinder and an outer cylinder: selecting pure copper as a raw material, integrally forming a conical section outer cylinder 1, a conical section inner cylinder 2, a straight section outer cylinder 4 and a straight section inner cylinder 5 by spinning, carrying out solution treatment on the formed conical section outer cylinder 1, the conical section inner cylinder 2, the straight section outer cylinder 4 and the straight section inner cylinder 5 at the temperature of 960 ℃, wherein the solution treatment time is 2h, then carrying out aging treatment on the conical section outer cylinder 1, the conical section inner cylinder 2, the straight section outer cylinder 4 and the straight section inner cylinder 5 after the solution treatment to obtain a complete conical section outer cylinder 1, the conical section inner cylinder 2, the straight section outer cylinder 4 and the straight section inner cylinder 5, wherein the aging treatment temperature is 400 ℃, and the aging treatment time is 4h;
s2, preparing a flow guide passage 75: connecting a water inlet baffle 71 and a flow guide baffle 73 which are forged and prefabricated to the complete conical section inner cylinder 2 obtained in the step S1 in a welding mode, wherein the welding mode is argon arc welding, the position of a water activating area 76 is reserved, and then installing a movable baffle 9, wherein the distance between the upper part and the lower part of the flow guide baffle 73 is 30mm, and the depth of the flow guide baffle 73 is 30mm;
s3, preparing an annular space: welding the complete conical section outer cylinder 1 and the upper flange 3 obtained in the step S1 with the conical section inner cylinder 2 respectively to form a first annular space 7, welding and installing an annular baffle plate 81 at the bottom of the first annular space 7, welding and installing a straight section inner cylinder 5 below the conical section inner cylinder 2, welding and installing a straight section outer cylinder 4 below the conical section outer cylinder 1, connecting a prefabricated forged guide pipe 82 to the complete straight section inner cylinder 5 obtained in the step S1 in a welding manner, and welding the complete straight section outer cylinder 4 and the lower flange 6 obtained in the step S1 with the straight section inner cylinder 5 respectively to form a second annular space 8.
Example 5
This embodiment is substantially the same as embodiment 4, except that:
s1, preparing an inner cylinder and an outer cylinder: the method comprises the steps of selecting a CuZr copper alloy as a raw material, integrally forming a conical section outer cylinder 1, a conical section inner cylinder 2, a straight section outer cylinder 4 and a straight section inner cylinder 5 through spinning, carrying out solution treatment on the formed conical section outer cylinder 1, the conical section inner cylinder 2, the straight section outer cylinder 4 and the straight section inner cylinder 5 at the temperature of 950 ℃ for 2h, and carrying out aging treatment on the conical section outer cylinder 1, the conical section inner cylinder 2, the straight section outer cylinder 4 and the straight section inner cylinder 5 after the solution treatment to obtain the complete conical section outer cylinder 1, the conical section inner cylinder 2, the straight section outer cylinder 4 and the straight section inner cylinder 5, wherein the temperature of the aging treatment is 395 ℃ and the time of the aging treatment is 6h.
Example 6
This embodiment is substantially the same as embodiment 4, except that:
s1, preparing an inner cylinder and an outer cylinder: the method comprises the steps of selecting CuCrZr copper alloy as a raw material, integrally forming a conical section outer cylinder 1, a conical section inner cylinder 2, a straight section outer cylinder 4 and a straight section inner cylinder 5 through spinning, carrying out solution treatment on the formed conical section outer cylinder 1, the conical section inner cylinder 2, the straight section outer cylinder 4 and the straight section inner cylinder 5 at the temperature of 980 ℃ for 2h, and then carrying out aging treatment on the conical section outer cylinder 1, the conical section inner cylinder 2, the straight section outer cylinder 4 and the straight section inner cylinder 5 after the solution treatment to obtain the complete conical section outer cylinder 1, the conical section inner cylinder 2, the straight section outer cylinder 4 and the straight section inner cylinder 5, wherein the temperature of the aging treatment is 435 ℃, and the time of the aging treatment is 2h.
Example 7
This embodiment is substantially the same as embodiment 4, except that:
CuCrNbZr copper alloy is selected as a raw material, and the welding mode is gas shielded welding.
Example 8
This embodiment is substantially the same as embodiment 4, except that:
choose to useCuNi 2 The Si-copper alloy is used as a raw material, and the welding mode is electron beam welding.
The working principle is as follows:
when the single crystal furnace water-cooling heat shield working principle of the invention is briefly explained below, taking embodiment 1 as an example, when the required cooling temperature is low, firstly, a low-temperature mode is selected, that is, the cooling water has a low flow rate, at this time, the cooling water in the first annular space 7 enters the water-activating zone 76 through the water inlet pipe 31, the water inlet baffle 71, the water inlet 72 and the flow guide passage 75 and flows out of the water outlet pipe 32, the magnetic sheet 98 below the water passing plate 91 is butted with the flow guide baffle 73 at the low flow rate, 3 water passing holes 911 are shielded by 3 water blocking plates 94, the flow rate is controlled while the water flow is ensured, the rotating plate 92 rotates to play a certain flow guide role, and the cooling water in the water-activating zone 76 is ensured to continuously flow;
meanwhile, cooling water in the second annular space 8 flows through the diversion pipe 82 from the diversion port 83 and flows out of the water outlet 61, and cold water is extended from the middle part of the water-cooling heat shield to the two ends by the method of upper conical section cooling and lower straight section cooling, so that the cooling effect is better;
when the required cooling temperature rises and the flow rate of cooling water needs to be increased, the cooling water with high flow rate enters the water activating area 76 at the moment, the water passing plate 91 is pushed to rise, the sliding block 93 slides upwards along the sliding groove 21, the sliding rod 96 slides upwards along the sliding rod groove 22, the sliding rod 96 moves towards one side of the sliding groove 21 while sliding, the water baffle 94 slides on the surface of the water passing plate 91, the water passing hole 911 is not blocked by the water baffle 94, the water passing flow is increased, and the problem of gasification caused by uneven vertical flow rate is solved.
Examples of the experiments
The properties of the water-cooling heat shields of the single crystal furnaces prepared in examples 4 to 8 were measured and compared with those of a conventional 316 stainless steel as comparative examples, and the results of the comparison are shown in table 1.
TABLE 1 Water-Cooling Heat Shielding Performance of Single Crystal furnace of examples and comparative examples
Figure BDA0003769785410000101
As can be seen from comparison of the table 1, compared with the conventional stainless steel material, the copper or copper alloy material selected by the invention is obviously improved in various properties, wherein the comprehensive properties of the single crystal furnace water-cooling heat shield prepared from the CuCrZr alloy in the embodiment 6 are optimal.

Claims (9)

1. The utility model provides an utilize single crystal growing furnace water-cooling heat shield of copper or copper alloy preparation, its characterized in that, including conical section urceolus (1) and conical section inner tube (2) that cup joint each other, the top of conical section urceolus (1) and conical section inner tube (2) is connected through annular upper flange (3), and conical section urceolus (1) bottom is equipped with straight section urceolus (4), conical section inner tube (2) bottom is equipped with straight section inner tube (5), straight section urceolus (4) and straight section inner tube (5) bottom are connected through annular lower flange (6), forms first annular space (7) that are used for crossing water between conical section urceolus (1) and the conical section inner tube (2), forms second annular space (8) that are used for crossing water between straight section urceolus (4) and the straight section inner tube (5), be equipped with ring baffle (81) between first annular space (7) and second annular space (8), inlet tube (31) and outlet pipe (32) have been seted up to upper flange (3) bilateral symmetry,
two water inlet baffles (71) are arranged in the first annular space (7) corresponding to the lower part of the water inlet pipe (31), the water inlet baffle plates (71) extend to the bottom of the first annular space (7), one water inlet baffle plate (71) is connected with the bottom of the first annular space (7), a water inlet (72) is formed in the bottom of the other water inlet baffle plate (71), a plurality of annular flow guide baffle plates (73) are arranged in the first annular space (7), each flow guide baffle plate (73) is arranged in parallel and at equal intervals, each flow guide baffle plate (73) is connected with one water inlet baffle plate (71) and an opening (74) is reserved between the other water inlet baffle plate (71), the water inlet baffle plates (71) connected with the two adjacent flow guide baffle plates (73) are different, so that the flow guide baffle plates (73) form a flow guide passage (75) which is folded back and rises in the first annular space (7), one flow guide baffle plate (73) positioned at the lowest position is connected with the water inlet baffle plate (71) provided with the water inlet (72), one flow guide baffle plate (73) positioned at the highest position extends to the right side of the water outlet pipe (32) and then is connected with the upper flange (3), and the first annular space (7) positioned at the right side of the flow guide baffle plate (73) at the highest position forms a water moving area (76), a movable baffle (9) for guiding flow is arranged in the middle of the water activating area (76);
the inside honeycomb duct (82) that is equipped with the spiral and descends the formula of second annular space (8), the top of honeycomb duct (82) is connected with reposition of redundant personnel mouth (83) that are equipped with on annular baffle (81) that are located between two water baffles (71), honeycomb duct (82) extend to behind the bottom of second annular space (8) with delivery port (61) that lower flange (6) inside was equipped with are connected.
2. The single crystal furnace water-cooling heat shield prepared from copper or copper alloy according to claim 1, wherein the movable baffle (9) comprises a water passing plate (91) slidably connected with the conical section inner cylinder (2) and a rotating plate (92) rotatably connected with the water passing plate (91), a slide block (93) is arranged on the side wall of the middle part of the water passing plate (91) corresponding to one side of the conical section inner cylinder (2), the slide block (93) is slidably connected with the side wall of the conical section inner cylinder (2) up and down, the bottom of the slide block (93) is connected with the bottom of the slide groove (21) through a spring (931), a plurality of groups of water passing holes (911) are arranged on the surface of the water passing plate (91) in an equidistant way, a water baffle plate (94) is slidably arranged on the upper surface of the water passing plate (91) corresponding to one group of water passing holes (911) in two adjacent groups of water passing holes (911), one water passing hole (94) is arranged on the water passing plate (94), a limit block (941) of the bottom of the water passing plate (94) in an inverted T shape is arranged on two sides of the bottom of the water passing plate (94), the water passing plate (94) is arranged on the side wall of each group of the water passing hole (941) corresponding to the water passing plate (91) and a connecting rod (94), one side of the water passing plate (94) is synchronously connected with the water passing plate (94) through a connecting rod (912) which is arranged on the side of the inner cylinder (94), and one side of the inner cylinder (96) which is connected with the inner cylinder (95) which is arranged on the side wall of the sliding connection rod (94), the sliding rod (96) is in sliding connection with a sliding rod groove (22) formed in the side wall of the conical section inner cylinder (2), one section of the upper portion of the sliding rod groove (22) deviates to the position of the sliding groove (21), and the deviated sliding rod (96) drives the water baffle (94) to slide to the position between the two adjacent groups of water holes (911).
3. The single crystal furnace water-cooling heat shield made of copper or copper alloy according to claim 2, wherein a rotating shaft (97) is arranged in the middle of the side wall of the water passing plate (91) on the side corresponding to the rotating plate (92), and the rotating shaft (97) is rotatably connected with the rotating plate (92).
4. The single crystal furnace water-cooling heat shield prepared from copper or copper alloy according to claim 2, wherein the water passing plate (91) and the rotating plate (92) are both arranged obliquely, both ends of the water passing plate (91) and the rotating plate (92) are a section of horizontal plane, a magnetic sheet (98) which is magnetically butted with the bottom surface of the upper flange (3) and plays an auxiliary fixing role is arranged on the upper surface of the horizontal plane above the water passing plate (91), and a magnetic sheet (98) which is magnetically butted with a second diversion baffle plate (73) on the upper part in the first annular space (7) and plays an auxiliary fixing role is also arranged on the lower surface of the horizontal plane below the water passing plate (91).
5. The single crystal furnace water-cooling heat shield made of copper or copper alloy according to claim 2, wherein the water through holes (911) are 5 groups, the water baffle plate (94) is 3, and each group of water through holes (911) is provided with 3 water through holes (911).
6. The method for preparing the water-cooling heat shield of the single crystal furnace by using the copper or the copper alloy according to any one of claims 1 to 5, comprising the following steps:
s1, preparing an inner cylinder and an outer cylinder: selecting pure copper or copper alloy as a raw material, integrally forming a conical section outer cylinder (1), a conical section inner cylinder (2), a straight section outer cylinder (4) and a straight section inner cylinder (5) by spinning, carrying out solution treatment on the formed conical section outer cylinder (1), conical section inner cylinder (2), straight section outer cylinder (4) and straight section inner cylinder (5), wherein the temperature of the solution treatment is 950-980 ℃, the time of the solution treatment is 2h, and then carrying out aging treatment on the conical section outer cylinder (1), conical section inner cylinder (2), straight section outer cylinder (4) and straight section inner cylinder (5) after the solution treatment to obtain a complete conical section outer cylinder (1), conical section inner cylinder (2), straight section outer cylinder (4) and straight section inner cylinder (5);
s2, preparing a flow guide passage (75): connecting a water inlet baffle (71) and a flow guide baffle (73) which are prefabricated by forging to the complete conical section inner cylinder (2) obtained in the step S1 in a welding mode, reserving the position of a water activating area (76), and then installing a movable baffle (9);
s3, preparing an annular space: welding the complete conical section outer cylinder (1) and the upper flange (3) obtained in the step S1 with the conical section inner cylinder (2) respectively to form a first annular space (7), welding and installing an annular baffle (81) at the bottom of the first annular space (7), welding and installing a straight section inner cylinder (5) below the conical section inner cylinder (2), welding and installing a straight section outer cylinder (4) below the conical section outer cylinder (1), connecting a prefabricated forged guide pipe (82) to the complete straight section inner cylinder (5) obtained in the step S1 in a welding mode, and welding the complete straight section outer cylinder (4) and the lower flange (6) obtained in the step S1 with the straight section inner cylinder (5) respectively to form a second annular space (8).
7. The method for preparing the water-cooling heat shield of the single crystal furnace prepared from the copper or the copper alloy according to claim 6, wherein the welding mode is argon arc welding, gas shielded welding or electron beam welding.
8. The method for preparing the water-cooling heat shield of the single crystal furnace prepared from the copper or the copper alloy according to claim 6, wherein the copper alloy in the step S1 is CuZr, cuCrZr, cuCrNbZr or CuNi 2 Si。
9. The method for preparing the water-cooling heat shield of the single crystal furnace by using the copper or the copper alloy as claimed in claim 6, wherein the temperature of the aging treatment in the step S1 is 395-435 ℃, and the time of the aging treatment is 2-6h.
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Publication number Priority date Publication date Assignee Title
US3076443A (en) * 1958-06-19 1963-02-05 Mitchell Engineering Ltd Heat exchanger
CN208717464U (en) * 2018-07-19 2019-04-09 浙江晶阳机电有限公司 A kind of water cooling heat shielding structure of single crystal growing furnace
CN210151239U (en) * 2019-06-20 2020-03-17 宁夏旭樱新能源科技有限公司 But quick assembly disassembly formula is water-cooling heat shield and single crystal growing furnace for monocrystalline silicon preparation
CN211522367U (en) * 2019-12-27 2020-09-18 杞县东磁新能源有限公司 Water-cooling heat shield structure of single crystal furnace
CN214736220U (en) * 2021-04-15 2021-11-16 陕西斯瑞新材料股份有限公司 Novel water-cooling exchanger based on monocrystalline silicon smelting

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3076443A (en) * 1958-06-19 1963-02-05 Mitchell Engineering Ltd Heat exchanger
CN208717464U (en) * 2018-07-19 2019-04-09 浙江晶阳机电有限公司 A kind of water cooling heat shielding structure of single crystal growing furnace
CN210151239U (en) * 2019-06-20 2020-03-17 宁夏旭樱新能源科技有限公司 But quick assembly disassembly formula is water-cooling heat shield and single crystal growing furnace for monocrystalline silicon preparation
CN211522367U (en) * 2019-12-27 2020-09-18 杞县东磁新能源有限公司 Water-cooling heat shield structure of single crystal furnace
CN214736220U (en) * 2021-04-15 2021-11-16 陕西斯瑞新材料股份有限公司 Novel water-cooling exchanger based on monocrystalline silicon smelting

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