WO2021047149A1 - 适合超重力定向凝固使用的坩埚装置 - Google Patents

适合超重力定向凝固使用的坩埚装置 Download PDF

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Publication number
WO2021047149A1
WO2021047149A1 PCT/CN2020/076972 CN2020076972W WO2021047149A1 WO 2021047149 A1 WO2021047149 A1 WO 2021047149A1 CN 2020076972 W CN2020076972 W CN 2020076972W WO 2021047149 A1 WO2021047149 A1 WO 2021047149A1
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WIPO (PCT)
Prior art keywords
crucible
crucible body
cooling
positioning flange
directional solidification
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PCT/CN2020/076972
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English (en)
French (fr)
Inventor
韦华
谢亚丹
王江伟
卢士亮
林伟岸
张泽
陈云敏
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浙江大学
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Publication of WO2021047149A1 publication Critical patent/WO2021047149A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
    • B22D23/06—Melting-down metal, e.g. metal particles, in the mould
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/04—Influencing the temperature of the metal, e.g. by heating or cooling the mould
    • B22D27/045—Directionally solidified castings
    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002—Crucibles or containers for supporting the melt
    • 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
    • C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions

Definitions

  • the invention relates to the technical fields of crucible, metallurgy and directional solidification, and in particular to a crucible device suitable for supergravity directional solidification.
  • the high-pressure turbine blades are the most severe rotating parts in the engine when they work under coupled loading conditions such as high temperature, high pressure, high speed, and alternating load for a long time during service. Its reliability directly affects the performance of the whole machine. In the development of superalloys, technology has played a great role in promoting the development of superalloys.
  • Orientation and single crystal blades eliminate the transverse grain boundary or completely eliminate the grain boundary, and the crystal grows along the specific direction of [001], which increases the initial melting temperature and solution treatment window temperature, increases the number of ⁇ and refines it, greatly improving performance and improving Operating temperature.
  • almost all advanced aero-engines use single crystal superalloys.
  • the rapid solidification method widely used in industry to prepare single crystal alloys has a temperature gradient of only about 100K/cm, and a very low solidification rate, which leads to coarse solidification structure and serious segregation, which makes the performance of the material not fully utilized.
  • Crystal growth under microgravity effectively suppresses the irregular heat and mass convection caused by gravity due to the reduction of gravitational acceleration, thereby obtaining crystals with highly uniform solute distribution, but the cost is too high to be industrialized.
  • Crystal growth under high gravity strengthens buoyancy convection by increasing the acceleration of gravity.
  • the buoyancy convection increases to a certain extent, it transforms into a laminar flow state, that is, re-laminar fluidization, which also suppresses irregular heat and mass convection.
  • the forced convection of the liquid phase is caused during the accelerated rotation, which greatly changes the heat and mass transfer process and causes a significant change in the interface morphology, resulting in a significant reduction in the width of the mushy zone.
  • the rapid flow of the liquid phase causes a great increase in the temperature gradient in the liquid phase at the front of the interface, which is very conducive to the uniform mixing of liquid solutes and the growth of the flat interface of the material.
  • the dendrite growth morphology changes significantly.
  • the crystal becomes a spike-like crystal with no obvious main axis, and the spike-like crystal has a fine microstructure.
  • the key to preparing single crystal alloys under high gravity is to develop crucibles suitable for directional solidification devices under high gravity.
  • What the present invention needs to solve is to provide a special crucible structure design scheme in view of the key problem that the temperature gradient is difficult to realize in the supergravity directional solidification process.
  • the crucible design scheme provided is simple, convenient to use and high in safety.
  • the invention includes a crucible body and a central cavity, a cooling hole, a temperature gradient adjustment block, a heat radiation groove, a positioning flange block, a heat dissipation groove and a gas discharge hole arranged on the crucible body;
  • the crucible body body is a cylindrical structure ,
  • the center of the top surface of the crucible body is provided with a cylindrical blind hole as the center cavity, and the center cavity is filled with the molten metal/metal sample to be directionally solidified by high gravity;
  • the top surface of the crucible body around the center cavity is provided with multiple verticals along the circumference Through holes are used as cooling holes, a plurality of cooling holes are evenly distributed along the circumferential direction, and cooling gas is passed into the lower end of the cooling holes;
  • each cooling hole is equipped with a temperature gradient adjustment block for realizing and adjusting the temperature gradient of directional solidification, and the temperature gradient is adjusted There is a gap between the block and the wall of the cooling hole, and the temperature gradient adjustment block
  • the heat dissipation groove penetrates the outer wall of the positioning flange block, and the bottom of the heat dissipation groove penetrates the bottom surface of the positioning flange block.
  • the heat radiation groove penetrates the top surface of the crucible body axially, and the radial outer part of the heat dissipation groove penetrates the outer peripheral surface of the crucible body.
  • the crucible body is used to contain molten metal/metal sample in the directional solidification process in a supergravity environment.
  • the crucible body is made of high-strength ceramic materials.
  • the cooling gas is liquid nitrogen, compressed air, etc.
  • the temperature of the cooling gas is not higher than 5°C, and the pressure is not higher than 5Mpa.
  • the invention has the advantages of simple structure, operation scheme and high safety factor, is suitable for 1g-2500g supergravity environment, and the temperature is from room temperature to 1700°C.
  • Figure 1 is a front cross-sectional view of the crucible device
  • Figure 2 is a top view of the crucible device
  • Fig. 3 is a partial enlarged cross-sectional view of the part marked A in Fig. 1;
  • Figure 4 is a cross-sectional view of A-A in Figure 1;
  • Fig. 5 is a perspective view of the crucible device.
  • Fig. 6 is a structural diagram of a super-gravity air cooling system matched with a crucible device.
  • crucible body 25 central cavity 25-1, cooling hole 25-2, temperature gradient adjustment block 25-3, heat radiation groove 25-4, positioning flange block 25-5, heat dissipation groove 25-6, gas Drain hole 25-7.
  • the specific implementation includes a crucible body 25 and a central cavity 25-1 arranged on the crucible body 25, a cooling hole 25-2, a temperature gradient adjustment block 25-3, a heat radiation groove 25-4, and a positioning convex
  • the main body of the crucible body 25 has a cylindrical structure, and the center of the top surface of the crucible body 25 is provided with a cylindrical blind hole as the central cavity 25-1.
  • 25-1 Fill the molten metal/metal sample to be directionally solidified under high gravity;
  • the top surface of the crucible body 25 around the central cavity 25-1 is provided with a plurality of vertical through holes as cooling holes 25-2 along the circumference.
  • the holes 25-2 are evenly spaced along the circumferential direction, and cooling gas is passed into the lower end of the cooling holes 25-2; each cooling hole 25-2 is equipped with a temperature gradient adjustment block 4 for realizing and adjusting the temperature gradient of directional solidification.
  • the upper outlet is connected, and the cooling gas is introduced into the cooling hole 25-2 through the air duct.
  • the cooling hole 25-2 is a channel through which the cooling gas diffuses on the wall of the crucible, and the cooling gas is mainly used to take away heat to achieve the purpose of cooling the crucible.
  • the lower peripheral surface of the crucible body 25 is fixed with a ring-shaped projection as a positioning flange block 25-5.
  • the positioning flange block 25-5 and the crucible body 25 are integrally formed, and the positioning flange block 25 -5 is provided with a plurality of heat dissipation grooves 25-6 on the outer peripheral cylindrical surface of the lower part.
  • the number of heat dissipation grooves 25-6 is twice that of the cooling holes 25-2.
  • the heat dissipation grooves 25-6 extend radially from the inner wall of the crucible body 25
  • the outer wall of the positioning flange block 25-5 extends outward and penetrates the outer wall of the positioning flange block 25-5.
  • the bottom of the heat dissipation groove 25-6 penetrates the bottom surface of the positioning flange block 25-5; the heat dissipation groove 25-6 is in the crucible body 25 A cavity is formed at the lower end of the positioning flange block 25-5, which enhances the heat dissipation effect of the lower part of the crucible body 25, and facilitates the formation of a temperature gradient during the solidification of the crucible.
  • the positioning flange block 25-5 assists in determining the position of the crucible body 25 when installing the crucible body 25 in the heating system of the high gravity directional solidification melting and casting furnace, and prevents the crucible body 25 from shaking when the crucible body 25 is installed under high gravity.
  • the outer peripheral cylindrical surface of the crucible body 25 above the positioning flange block 25-5 is provided with a plurality of heat radiation grooves 25-4, and the plurality of heat radiation grooves 25-4 are evenly spaced along the circumferential direction.
  • the number of heat radiation grooves 25-4 is the same as the number of cooling holes 25-2.
  • the outer cylindrical surface of the crucible body 25 between two adjacent cooling holes 25-2 has a heat radiation groove 25-4.
  • the groove 25-4 axially penetrates the top surface of the crucible body 25, and the radial outer part of the heat dissipation groove 25-6 penetrates the outer peripheral surface of the crucible body 25; in actual implementation, the heat radiation groove 25-4 and the heating system of the high gravity directional solidification melting and casting furnace
  • the upper heating furnace tube, the lower heating furnace tube and the heating element are used to heat the crucible.
  • one or two small through holes are opened on the side wall of the crucible body 25 at the top surface of the positioning flange block 25-5 as gas discharge holes 25-7, if there are two gas discharge holes 25 -7 is arranged symmetrically on both sides of the side wall of the crucible body 25, the gas discharge hole 25-7 buffers the cooling hole 25-3 and the outside of the crucible body 25, and the gas discharge hole 25-7 and the cooling hole 25-3 form a cooling gas
  • the passage is used for discharging the cooling gas and at the same time preventing damage to the crucible body 25 caused by the expansion of the cooling gas at high temperature.
  • the crucible body 25 is used to hold the molten metal/metal sample during the directional solidification process in a high-gravity environment.
  • the crucible body 25 is made of high-strength ceramic materials, so that the crucible has sufficient strength and rigidity to ensure that it can work normally under high gravity after being installed in the directional melting and casting furnace.
  • the crucible material has extremely low porosity to ensure that the high-temperature melt cannot seep out of the crucible under supergravity during the directional solidification process, so that it can be conveniently and flexibly applied to various types of supergravity directional solidification melting and casting furnaces.
  • the cooling gas is liquid nitrogen, compressed air, etc.
  • the temperature of the cooling gas is not higher than 5°C
  • the pressure is not higher than 5Mpa
  • the pressure is controllable and adjustable. According to the temperature gradient requirements, the type of cooling gas can be changed.
  • the invention can be suitable for 1g-2500g supergravity environment, and the temperature is from normal temperature to 1700°C.
  • the crucible body 25 is installed in a super-gravity environment to work under super-gravity, and the direction of applying the super-gravity is downward along the axis of the crucible body 25. Specifically, it is installed in the heating system of the high-gravity directional solidification melting and casting furnace.
  • the heat generated by the heating element is radiated and transferred to the outer wall of the crucible body 25 through the heat radiation groove 25-4, and then the crucible body 25 is heated to the center cavity.
  • the metal sample in 25-1 is heated to melt the sample in the crucible.
  • the cooling gas enters the crucible body 25 from the lower end of the cooling hole 25-2, the initial temperature gradient adjustment block 25-3 is located at the bottom of the cooling hole 25-2, and the pressure of the cooling gas drives the temperature gradient adjustment Block 25-3, and flow from the gap between the temperature gradient adjustment block 25-3 and the wall of the cooling hole 25-2 to the top of the cooling hole 25-2, so that heat conduction through the wall of the cooling hole 25-2 from bottom to top
  • the central cavity 25-1 is cooled, and directional solidification is performed.
  • the temperature gradient adjustment block 25-3 is respectively affected by the weight of the supergravity, the friction between the wall of the cooling hole 25-2 and the pressure of the cooling gas during the movement of the cooling hole 25-2. There is a pressure difference between the two ends of the temperature gradient adjustment block 25-3.
  • the temperature gradient adjustment block 25-3 is in contact with the cooling hole 25 of the crucible body 25 during the movement process.
  • the friction between the wall of the hole and the pressure of the cooling gas can be combined with the temperature gradient adjustment block 25-3 to adjust and move up and down under the action of the pressure difference to achieve the temperature gradient in the supergravity directional solidification process. In this way, the temperature of the central cavity 25-1 from bottom to top can be gradually reduced and cooled, so that the metal sample that has been melted in the central cavity 25-1 gradually solidifies as needed from bottom to top, and directional solidification is realized.
  • the cooling gas After cooling and directional solidification, the cooling gas is normally discharged from the top port of the cooling hole 25-2. However, when the temperature gradient adjustment block 25-3 is blocked in the cooling hole 25-2, the pressure of the cooling gas flows from the small diameter hole of the gas discharge hole 25-7 to the outside of the crucible body 25, which prevents the pressure of the cooling gas from increasing continuously. Avoid the safety problems caused by the infinite increase of internal pressure.
  • the crucible body 25 is also connected to the intake pipe 29, the crucible support body 21, the cooling base 26, the cooling speed adjusting ring 27, the crucible body 25, the exhaust cover 28 and the exhaust pipe 30; the crucible support body 21 is placed at the bottom , A cooling base 26 is installed on the top surface of the crucible support body 21, a crucible body 25 is installed on the cooling base 26, an exhaust cover 28 is installed on the top of the crucible body 25, and a cooling system composed of a cooling speed adjusting ring 27 is fitted in the middle of the crucible body 25 to cooperate and work. .
  • the function of the crucible support body 21 is to support the pressure generated by the crucible and the heating system under supergravity.
  • the crucible support body 21 is provided with a vent pipe. The lower end of the vent pipe penetrates the outer wall of the bottom of the crucible support body 21 and is connected to one end of the air inlet pipe 29. 29 The other end is connected to the cooling gas source outside the supergravity experiment cabin through the ventilation bracket inside the supergravity experiment cabin to provide cooling gas for the cooling system;
  • the cooling base 26 is used to connect the crucible and the crucible support.
  • the upper end of the cooling base 26 is open, and the opening is provided with a lower annular groove.
  • the circumference of the lower annular groove is consistent with the circumference of the cooling hole 25-2 of the crucible body 25.
  • the lower end of the crucible body 25 It is installed in the upper opening of the cooling base 26, and the lower ends of the cooling holes 25-2 of the crucible body 25 are connected through the lower annular groove.
  • the bottom end of the cooling base 26 is provided with an air inlet through hole communicating with the lower annular groove, and the crucible support 21
  • the upper end of the vent pipe penetrates through the top surface of the crucible support body 21 and communicates with the air inlet through hole of the cooling base 26.
  • the cooling gas enters the vent pipe inside the crucible support body 21 through the air inlet pipe 29, and then enters the lower annular groove through the air inlet through hole, and then into the various cooling holes 25-2 of the crucible body 25, and then from the lower end of the cooling hole 25-2 Entering into the crucible body 25, the crucible body 25 starts to be cooled.
  • the upper opening of the cooling base 26 is provided with two inner and outer lower annular grooves.
  • the two lower annular grooves are connected and communicated.
  • a lower annular groove on the outer ring and the cooling hole 25-2 of the crucible body 25 are provided.
  • the circumference is correspondingly connected, and a lower annular groove of the inner ring is provided with an air inlet through hole.
  • the cold speed adjusting ring 27 is fixedly installed on the positioning flange block 25-5 of the crucible body 25.
  • the bottom surface of the cold speed adjusting ring 27 and the top surface of the positioning flange block 25-5 are in close contact with the top surface of the positioning flange block 25-5.
  • Supporting, one or two vertical gas collecting slots are formed on the top surface of the cooling speed adjusting ring 27.
  • the number of gas collecting slots is the same as that of the gas discharge holes 25-7 of the crucible body 25, and the top of the gas collecting slots penetrates
  • the cooling speed adjusting ring 27 communicates with the outside of the crucible body 25, and the bottom end of the gas collecting slot passes through the inner wall surface of the cooling speed adjusting ring 27 and communicates with the gas discharge hole 25-7 of the crucible body 25 to collect the gas after cooling the crucible;
  • the lower end of the exhaust cover 28 is open, and an upper annular groove is provided in the opening.
  • the circumferential size of the upper annular groove is also consistent with the circumference of the cooling hole 25-2 of the crucible body 25.
  • the lower end of the crucible body 25 is installed in the lower end opening of the exhaust cover 28,
  • the upper end of each cooling hole 25-2 of the crucible body 25 is connected through the upper annular groove to provide a gas path for the cooling gas.
  • the bottom end of the exhaust cover 28 is provided with an outlet hole communicating with the upper annular groove.
  • the through hole is connected with one end of the exhaust pipe 30 for discharging cooling gas; the other end of the exhaust pipe 30 is connected to the outside through the ventilation bracket and the slip ring of the supergravity centrifuge inside the supergravity experiment chamber to discharge the cooling gas.
  • the cooling gas that has passed through the cooling hole 25-2 of the crucible body 25 enters the upper annular groove from the top of the cooling hole 25-2, is collected in the upper annular groove, and is then discharged through the air outlet through hole.
  • the trachea 30 is discharged.
  • a boss is formed in the middle of the opening at the lower end of the exhaust cover 28, and the boss is embedded in the top of the central cavity 25-1 of the crucible body 25 to fix the crucible to prevent the crucible from shaking under high gravity.
  • the bottom of the crucible can be further cooled by the cooling base 26, and the dispersed gas is collected into the crucible cooling hole; the cooling speed adjusting ring 27 collects the cooling gas in the lower part of the crucible, and adjusts the position according to the temperature zone requirements to achieve different temperature zone requirements .

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  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
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Abstract

一种适合超重力定向凝固使用的坩埚装置，其包括坩埚本体（25）和开设在坩埚本体上的中心容腔（25-1），该坩埚本体的主体呈柱形，中心容腔灌充金属试样；中心容腔周围设多个冷却孔（25-2），每个冷却孔中均安装有温度梯度调节块（25-3），温度梯度调节块在冷却孔轴向移动；坩埚本体下部有定位凸缘块（25-5），定位凸缘块下部的外周柱面开设多个散热槽（25-6）；定位凸缘块上方的坩埚本体外周柱面开设多个热量辐射槽（25-4）；在定位凸缘块顶面处的坩埚本体侧壁开设一个或者两个小通孔作为气体排放孔（25-7），气体排放孔将冷却孔和坩埚本体外部缓冲连通。该坩埚装置解决了超重力定向凝固过程中温度梯度难实现的问题，结构简单，安全系数较高。

Description

适合超重力定向凝固使用的坩埚装置 技术领域
本发明涉及坩埚、冶金、定向凝固技术领域，尤其涉及一种适合超重力定向凝固使用的坩埚装置。
背景技术
高压涡轮工作叶片作为航空发动机和燃气轮机热端部件关键组成部分之一，服役时长期工作在高温、高压、高转速、交变负载等耦合加载条件下，是发动机中工作条件最恶劣的转动部件，其使用可靠性直接影响整机性能。在高温合金的发展过程中，工艺对高温合金的发展起着很大的推动作用。通常为了提高高温合金的综合力学性能，采用两种途径：其一是加入大量合金化元素，通过合理的热处理工艺使之产生固溶强化、沉淀强化及晶界强化等，从而保证高温合金具有从室温到高温的良好强度、表明稳定性和较好的塑性；其二是从凝固工艺入手，采用定向凝固工艺，制备晶界平行于主应力轴从而消除有害横向晶界的柱状晶高温合金或制备消除所有晶界的单晶高温合金。定向及单晶叶片由于消除横向晶界或完全消除晶界，晶体沿[001]特定方向生长，提高初熔温度及固溶处理窗口温度，增加γ数量并细化，大幅度提高了性能，提高使用温度。目前，几乎所有先进航空发动机均采用单晶高温合金。工业上广泛应用的快速凝固法制备单晶合金，其温度梯度只能达到100K/cm左右，凝固速率很低，导致凝固组织粗大，偏析严重，致使材料的性能千里没有得到充分发挥。微重力下的晶体生长，由于重力加速度减小而有效的抑制了重力造成的无规则热质对流，从而获得溶质分布高度均匀的晶体，但由于成本太高，无法工业化。超重力下的晶体生长，通过增大重力加速度而加强浮力对流，当浮力对流增强到一定程度时，就转化为层流状态，即重新层流化，同样抑制了无规则的热质对流。在加速旋转过程中造成液相强迫对流，由于极大的改变热质传输过程而引起了界面形貌的显著变化，导致糊状区宽度显著减小。液相快速流动引起界面前沿液相中的温度梯度极大的提高，非常有利于液相溶质的均匀混合和材料的平界面生长，枝晶生长形态发生显著的变化，由原来具有明显主轴的枝晶变为无明显主轴的穗状晶，穗状晶具有细密的显微组织。但超重力环境下制备单晶合金的关键是，必须研发适合超重力下定向凝固装置使用的坩埚。
发明内容
本发明需要解决的是针对上述超重力定向凝固过程中温度梯度难实现的关键难题，提供一种特殊的坩埚结构设计方案，提供的坩埚设计方案简单、使用方便、安全系数高。
本发明采用的技术方案是：
本发明包括坩埚本体和设置在坩埚本体上的中心容腔、冷却孔、温度梯度调节块、热量辐射槽、定位凸缘块、散热槽和气体排放孔；所述的坩埚本体主体为柱形结构，坩埚本体顶面中央开设有圆柱盲孔作为中心容腔，中心容腔灌充待超重力定向凝固的金属熔液/金属试样；中心容腔周围的坩埚本体顶面沿圆周开设多个垂直通孔作为冷却孔，多个冷却孔沿周向间隔均布，冷却孔下端通入冷却气体；每个冷却孔中均安装有用于实现和调节定向凝固温度梯度的温度梯度调节块，温度梯度调节块和冷却孔孔壁之间存在间隙，温度梯度调节块在冷却孔能沿轴向上下移动；坩埚本体下部周面固定有环形的凸块作为定位凸缘块，定位凸缘块下部的外周柱面开设多个散热槽，散热槽从坩埚本体主体内壁径向向外延伸定位凸缘块外壁；定位凸缘块上方的坩埚本体外周柱面开设多个热量辐射槽，多个热量辐射槽沿周向间隔均布，相邻两个冷却孔之间的坩埚本体外周柱面均有一个热量辐射槽；在定位凸缘块顶面处的坩埚本体侧壁开设一个或者两个小通孔作为气体排放孔，气体排放孔将冷却孔和坩埚本体外部缓冲连通。
所述的散热槽贯穿出定位凸缘块外壁，散热槽底部贯穿出定位凸缘块底面。
所述的热量辐射槽轴向贯穿出坩埚本体顶面，散热槽径向外侧部贯穿出坩埚本体外周面。
所述的坩埚本体用于超重力环境下定向凝固过程的金属熔液/金属试样盛装。
所述的坩埚本体采用高强陶瓷材料。
所述的冷却气体为液氮、压缩空气等，冷却气体温度不高于5℃，压力不高于5Mpa。
本发明的有益效果是：
为超重力环境下的定向凝固装置提供一种特殊的坩埚结构设计方案，能用于安装超重力的加热装置中帮助实现超重力定向凝固过程中温度梯度，帮助辅助实现解决了超重力定向凝固过程中温度梯度难实现的关键难题。
本发明具有结构简单，操作方案且安全系数较高的优点，适合1g-2500g超重力环境，温度从室温-1700℃。
附图说明
图1是坩埚装置正面剖视图；
图2是坩埚装置俯视图；
图3是图1中标A部位的局部放大剖视图；
图4是图1中A-A的剖视图；
图5是坩埚装置的立体图。
图6是与坩埚装置配合的超重力气冷系统的结构图。
图中：坩埚本体25、中心容腔25-1、冷却孔25-2、温度梯度调节块25-3、热量辐射槽25-4、定位凸缘块25-5、散热槽25-6、气体排放孔25-7。
具体实施方式
下面结合附图和实施例对本发明作进一步说明。
如图1所示，具体实施包括坩埚本体25和设置在坩埚本体25上的中心容腔25-1、冷却孔25-2、温度梯度调节块25-3、热量辐射槽25-4、定位凸缘块25-5、散热槽25-6和气体排放孔25-7；坩埚本体25主体为柱形结构，坩埚本体25顶面中央开设有圆柱盲孔作为中心容腔25-1，中心容腔25-1灌充待超重力定向凝固的金属熔液/金属试样；中心容腔25-1周围的坩埚本体25顶面沿圆周开设多个垂直通孔作为冷却孔25-2，多个冷却孔25-2沿周向间隔均布，冷却孔25-2下端通入冷却气体；每个冷却孔25-2中均安装有用于实现和调节定向凝固温度梯度的温度梯度调节块4，温度梯度调节块4和冷却孔25-2孔壁之间存在间隙，温度梯度调节块4在冷却孔25-2能沿轴向上下移动；具体实施中，冷却孔25-2和坩埚支撑座的通气管道上端出口相连，经通气管道向冷却孔25-2中通入冷却气体。冷却孔25-2为冷却气体在坩埚壁扩散的通道，主要是利用冷却气体带走热量，实现冷却坩埚的目的。
如图1和图5所示，坩埚本体25下部周面固定有环形的凸块作为定位凸缘块25-5，定位凸缘块25-5和坩埚本体25主体一体成型，定位凸缘块25-5下部的外周柱面开设多个散热槽25-6，具体实施中散热槽25-6的数量为冷却孔25-2的两倍，散热槽25-6从坩埚本体25主体内壁径向向外延伸定位凸缘块25-5外壁，并贯穿出定位凸缘块25-5外壁，散热槽25-6底部贯穿出定位凸缘块25-5底面；散热槽25-6在坩埚本体25的定位凸缘块25-5下端形成一个空腔，增强坩埚本体25下部的散热效果，有利于坩埚凝固过程中温度梯度的形成。
定位凸缘块25-5除了开设散热槽25-6下部的上部部分在超重力定向凝固 熔铸炉加热系统中安装坩埚本体25时辅助确定位置，防止超重力下坩埚本体25安装晃动。
如图1和图3所示，定位凸缘块25-5上方的坩埚本体25外周柱面开设多个热量辐射槽25-4，多个热量辐射槽25-4沿周向间隔均布，具体实施中热量辐射槽25-4的数量和冷却孔25-2的数量相同，相邻两个冷却孔25-2之间的坩埚本体25外周柱面均有一个热量辐射槽25-4，热量辐射槽25-4轴向贯穿出坩埚本体25顶面，散热槽25-6径向外侧部贯穿出坩埚本体25外周面；具体实施中，热量辐射槽25-4与超重力定向凝固熔铸炉加热系统中的上加热炉管、下加热炉管和发热体配合，用来加热坩埚。
如图2和图4所示，在定位凸缘块25-5顶面处的坩埚本体25侧壁开设一个或者两个小通孔作为气体排放孔25-7，若为两个气体排放孔25-7则在坩埚本体25侧壁两侧对称布置，气体排放孔25-7将冷却孔25-3和坩埚本体25外部缓冲连通，气体排放孔25-7与冷却孔25-3形成一个冷却气体通路，用于排放冷却气体，同时防止高温下冷却气体膨胀对坩埚本体25产生的破坏。
坩埚本体25用于超重力环境下定向凝固过程的金属熔液/金属试样盛装。
坩埚本体25采用高强陶瓷材料，使坩埚具有足够的强度和刚度，确保安装到定向熔铸炉后在超重力下能正常工作。坩埚材料具有极低的孔隙率，确保定向凝固过程中，高温熔体在超重力下不能够从坩埚中渗出，以方便灵活地适用于各种类型的超重力定向凝固熔铸炉。
冷却气体为液氮、压缩空气等，冷却气体温度不高于5℃，压力不高于5Mpa，压力可控可调。根据温度梯度要求，冷却气体类型可以改变。
本发明能适合1g-2500g超重力环境，温度从常温-1700℃。
本发明的工作过程如下：
具体实施在定向凝固过程中，是将坩埚本体25安装于超重力环境中在超重力下工作，施加超重力方向沿坩埚本体25轴向向下方向。具体是安装于超重力定向凝固熔铸炉的加热系统中。
在超重力定向凝固试验的加热阶段，在没有冷却气体通入情况下，发热体产生的热量，通过热量辐射槽25-4辐射和热传导到坩埚本体25外壁，进而加热坩埚本体25对中心容腔25-1中的金属试样进行加热，熔化坩埚中的试样。
在超重力定向凝固试验的凝固阶段，冷却气体从冷却孔25-2下端进入坩埚本体25内部，初始温度梯度调节块25-3位于冷却孔25-2的底部，冷却气体的压力推动温度梯度调节块25-3，并从温度梯度调节块25-3和冷却孔25-2孔壁之间的间隙中流经到冷却孔25-2顶部，使得由下到上通过冷却孔25-2孔壁热 传导对中心容腔25-1进行冷却，实施定向凝固。
对于凝固阶段的控制，温度梯度调节块25-3在冷却孔25-2的移动过程中分别受超重力的重量、与冷却孔25-2孔壁之间的摩擦力以及冷却气体的压力影响，温度梯度调节块25-3两端受力存在压差，通过设置超重力作用下温度梯度调节块25-3的超重量、温度梯度调节块25-3移动过程中与坩埚本体25的冷却孔25-2孔壁之间的摩擦力以及冷却气体的压力，根据需要可结合使温度梯度调节块25-3在压差作用下上下调节移动，来实现超重力定向凝固过程中的温度梯度。这样能够实现由下到上的中心容腔25-1逐渐温度降低冷却，使得在中心容腔25-1已经熔化的金属试样由下到上按照需要逐渐凝固，实现了定向凝固。
试验过程中，通过改变超重力大小、冷却气体流量、时间、温度梯度调节块的重量等措施，与超重力定向熔铸炉加热系统配合，实现不同的温度梯度要求。
冷却实施定向凝固后冷却气体正常从冷却孔25-2顶端口排出。但是当温度梯度调节块25-3在冷却孔25-2中堵塞时，冷却气体的压力从气体排放孔25-7的小径孔流通到坩埚本体25外部，避免了冷却气体的压力不断增大，避免了内部压力无限增大导致的安全问题。
具体实施中，坩埚本体25还和进气管29、坩埚支撑体21、冷却底座26、冷速调节环27、坩埚本体25、排气盖28和排气管30；坩埚支撑体21置于最底部，坩埚支撑体21顶面上安装冷却底座26，冷却底座26上安装坩埚本体25，坩埚本体25顶端安装排气盖28，坩埚本体25中部套装冷速调节环27构成的冷却系统配合连接进而工作。
坩埚支撑体21的作用是支撑坩埚和加热系统在超重力下产生的压力，坩埚支撑体21内部开设有通气管道，通气管道下端穿出坩埚支撑体21底部外壁和进气管29一端连接，进气管29另一端通过超重力实验舱内部的通气支架与超重力实验舱外的冷却气源相连，为冷却系统提供冷却气体；
冷却底座26用来连接坩埚和坩埚支撑体，冷却底座26上端开口，开口内设有下环形槽，下环形槽的圆周尺寸和坩埚本体25的冷却孔25-2圆周相一致，坩埚本体25下端安装到冷却底座26上端开口中，且通过下环形槽将坩埚本体25的各个冷却孔25-2下端连通，冷却底座26底端开有和下环形槽连通的进气通孔，坩埚支撑体21的通气管道上端穿出坩埚支撑体21顶面和冷却底座26的进气通孔连通。
冷却气体经进气管29进入坩埚支撑体21内部的通气管道，再经进气通孔进入下环形槽，进而通入到坩埚本体25的各个冷却孔25-2，进而从冷却孔25- 2下端进入坩埚本体25内部，对坩埚本体25开始进行冷却。
具体实施中，如图6所示，冷却底座26上端开口内设有内外两道下环形槽，两道下环形槽连接相通，外圈的一道下环形槽和坩埚本体25的冷却孔25-2圆周对应连通，内圈的一道下环形槽开设进气通孔。
冷速调节环27固定安装于坩埚本体25的定位凸缘块25-5上，冷速调节环27底面和定位凸缘块25-5顶面紧贴，被定位凸缘块25-5顶面承托，冷速调节环27顶面开设有一个或者两个垂直的集气槽孔，集气槽孔的数量和坩埚本体25的气体排放孔25-7数量相同，集气槽孔顶端穿出冷速调节环27和坩埚本体25外部连通，集气槽孔底端穿过冷速调节环27内圈壁面和坩埚本体25的气体排放孔25-7连通，用来收集冷却坩埚后的气体；
排气盖28下端开口，开口内设有上环形槽，上环形槽的圆周尺寸和坩埚本体25的冷却孔25-2圆周也相一致，坩埚本体25下端安装到排气盖28下端开口中，且通过上环形槽将坩埚本体25的各个冷却孔25-2上端连通，为冷却气体提供气路，排气盖28底端开有和上环形槽连通的出气通孔，排气盖28的出气通孔和排气管30的一端连通，用于排出冷却气体；排气管30另一端通过超重力实验舱内部的通气支架、超重力离心机滑环与外界相连通，将冷却气体排出。
冷却实施定向凝固后，坩埚本体25的冷却孔25-2内已经实施流经过的冷却气体从冷却孔25-2顶端进入上环形槽，收集在上环形槽中，进而经出气通孔后由排气管30排出。
具体实施中，排气盖28下端开口内的中间设置形成凸台，凸台嵌装于坩埚本体25的中心容腔25-1顶端内，能固定坩埚防止超重力作用下坩埚晃动。
试验中，进一步能够通过冷却底座26对坩埚底部冷却，并将分散气体的收集到坩埚冷却孔；冷速调整环27收集坩埚下部的冷却气体，并根据温区要求调整位置，实现不同温区要求。

Claims (6)

  1. 一种适合超重力定向凝固使用的坩埚装置，其特征在于：包括坩埚本体(25)和设置在坩埚本体(25)上的中心容腔(25-1)、冷却孔(25-2)、温度梯度调节块(25-3)、热量辐射槽(25-4)、定位凸缘块(25-5)、散热槽(25-6)和气体排放孔(25-7)；所述的坩埚本体(25)主体为柱形结构，坩埚本体(25)顶面中央开设有圆柱盲孔作为中心容腔(25-1)，中心容腔(25-1)有待超重力定向凝固的金属熔液/金属试样；中心容腔(25-1)周围的坩埚本体(25)顶面沿圆周开设多个垂直通孔作为冷却孔(25-2)，多个冷却孔(25-2)沿周向间隔均布，冷却孔(25-2)下端通入冷却气体；每个冷却孔(25-2)中均安装有用于实现和调节定向凝固温度梯度的温度梯度调节块(4)，温度梯度调节块(4)和冷却孔(25-2)孔壁之间存在间隙，温度梯度调节块(4)在冷却孔(25-2)能沿轴向上下移动；坩埚本体(25)下部周面固定有环形的凸块作为定位凸缘块(25-5)，定位凸缘块(25-5)下部的外周柱面开设多个散热槽(25-6)，散热槽(25-6)从坩埚本体(25)主体内壁径向向外延伸定位凸缘块(25-5)外壁；定位凸缘块(25-5)上方的坩埚本体(25)外周柱面开设多个热量辐射槽(25-4)，多个热量辐射槽(25-4)沿周向间隔均布，相邻两个冷却孔(25-2)之间的坩埚本体(25)外周柱面均有一个热量辐射槽(25-4)；在定位凸缘块(25-5)顶面处的坩埚本体(25)侧壁开设一个或者两个小通孔作为气体排放孔(25-7)，气体排放孔(25-7)将冷却孔(25-3)和坩埚本体(25)外部缓冲连通。
  2. 根据权利要求1所述的一种适合超重力定向凝固使用的坩埚装置，其特征在于：所述的散热槽(25-6)贯穿出定位凸缘块(25-5)外壁，散热槽(25-6)底部贯穿出定位凸缘块(25-5)底面。
  3. 根据权利要求1所述的一种适合超重力定向凝固使用的坩埚装置，其特征在于：所述的热量辐射槽(25-4)轴向贯穿出坩埚本体(25)顶面，散热槽(25-6)径向外侧部贯穿出坩埚本体(25)外周面。
  4. 根据权利要求1所述的一种适合超重力定向凝固使用的坩埚装置，其特征在于：所述的坩埚本体(25)用于超重力环境下定向凝固过程的金属熔液/金属试样盛装。
  5. 根据权利要求1所述的一种适合超重力定向凝固使用的坩埚装置，其特征在于：所述的坩埚本体(25)采用高强陶瓷材料。
  6. 根据权利要求1所述的一种适合超重力定向凝固使用的坩埚装置，其 特征在于：所述的冷却气体为液氮、压缩空气等，冷却气体温度不高于5℃，压力不高于5Mpa。
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CN110523958B (zh) * 2019-09-10 2024-02-27 浙江大学 适合超重力定向凝固使用的坩埚装置
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