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CN107083564B - Vertical Bridgman furnace multi-component compound crystal growth equipment - Google Patents

Vertical Bridgman furnace multi-component compound crystal growth equipment Download PDF

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Publication number
CN107083564B
CN107083564B CN201710468013.5A CN201710468013A CN107083564B CN 107083564 B CN107083564 B CN 107083564B CN 201710468013 A CN201710468013 A CN 201710468013A CN 107083564 B CN107083564 B CN 107083564B
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furnace body
furnace
compound crystal
rod
heat insulation
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CN107083564A (en
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宋德鹏
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Shandong Liguan Microelectronics Equipment Co ltd
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Shandong Liguan Microelectronics Equipment Co ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/003Heating or cooling of the melt or the crystallised material
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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

Abstract

The invention discloses a vertical Bridgman furnace multi-element compound crystal growth device, which comprises a furnace body, a bracket for supporting the furnace body and a feeding mechanism for feeding into the furnace body, wherein the furnace body comprises: the inner tube is a quartz tube arranged vertically; the outer tube is a quartz tube, is nested outside the inner tube coaxially, and is spaced a given distance from the inner tube to form an intermediate space, and the surface of the outer tube is plated with a heat insulation coating; the heat insulation piece is positioned in the middle of the upper and lower directions of the middle space, the space of the inner tube positioned at the upper part of the heat insulation piece is a high-temperature area, the space positioned at the lower part of the heat insulation piece is a low-temperature area, and the area where the heat insulation piece is positioned is a gradient area; and a heater located in the intermediate space and including an upper heater for heating the high temperature region and a lower heater for heating the low temperature region. The furnace body according to the invention is relatively compact in structure and relatively small in weight.

Description

Vertical Bridgman furnace multi-component compound crystal growth equipment
Technical Field
The invention relates to a vertical Bridgman furnace multi-element compound crystal growth device.
Background
Bridgman crystal growth, also known as Bridgman-Stockbarge method, B-S for short, is a commonly used crystal growth method.
The Bridgman crystal growth method depends on a vertical Bridgman furnace, the vertical Bridgman furnace has a certain temperature gradient from top to bottom, and the experimental flow of the Bridgman crystal growth hair is as follows:
the material required for crystal growth is placed in a cylindrical crucible, the crucible is slowly lowered in a vertical Bridgman furnace under the control of a corresponding driving device, and the furnace temperature of the Bridgman furnace is controlled to be slightly higher than the melting point of the material. The resistance furnace or the high-frequency furnace can be selected according to the properties of the materials and the heating device. While passing through the heating zone, the material in the crucible is melted, and as the crucible continues to descend, the temperature at the bottom of the crucible first drops below the melting point and crystallization begins, with the crystal continuing to grow as the crucible descends. This method is commonly used to prepare alkali metal, alkaline earth metal halides and fluoride single crystals.
Typically, the background section of chinese patent document CN101220502a and its fig. 1 show the basic structure of a vertical bridgman furnace, comprising a stainless steel casing, a ceramic liner housed in the stainless steel casing and wound with heating wires for generating the required temperature gradient, and the ceramic liners at both ends are separated by ceramic cooling fins, thereby forming three furnace sections, a high temperature zone, a temperature gradient zone and a low temperature zone in this order from top to bottom, generating the required temperature gradient.
In order to effectively insulate heat, the heat insulation material needs to be filled between the shell and the liner tube, the overall radial dimension specification is relatively large, the heat insulation material still constructs a connection between the shell and the liner tube based on the filled heat insulation material, and the heat insulation effect is not good.
The technical solution claimed in the above-mentioned chinese patent document CN101220502a focuses on the construction of the temperature gradient, and the axial dimension of the vertical bridgman furnace has not been modified yet.
Fig. 1 of chinese patent document CN106480495a also shows the general structure of a vertical bridgman furnace, i.e. the furnace is sequentially configured from top to bottom into a high temperature zone, a gradient zone and a low temperature zone, and the detailed description section also shows that the furnace body can rotate, obviously if the furnace body adopts a relatively thick heat insulating material (such as heat insulating cotton), the furnace body must occupy a relatively large space during rotation, the weight of the furnace body will be relatively large, and a relatively large driving force is required.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a vertical Bridgman furnace multiple compound crystal growth apparatus having a relatively compact furnace body structure and a relatively small weight.
According to an embodiment of the present invention, there is provided a vertical Bridgman furnace multiple compound crystal growth apparatus including a furnace body, a support supporting the furnace body, and a feeding mechanism feeding into the furnace body, the furnace body including:
the inner tube is a quartz tube arranged vertically;
the outer tube is a quartz tube, is nested outside the inner tube coaxially, and is spaced a given distance from the inner tube to form an intermediate space, and the surface of the outer tube is plated with a heat insulation coating;
the heat insulation piece is positioned in the middle of the upper and lower directions of the middle space, the space of the inner tube positioned at the upper part of the heat insulation piece is a high-temperature area, the space positioned at the lower part of the heat insulation piece is a low-temperature area, and the area where the heat insulation piece is positioned is a gradient area; and
the heater is positioned in the middle space and comprises an upper heater for heating the high-temperature area and a lower heater for heating the low-temperature area.
The vertical Bridgman furnace multiple compound crystal growth apparatus described above, optionally, the thermally insulating coating is a gold coating.
Alternatively, the insulating coating is provided with a plurality of windows which are not covered by the insulating coating in the up-down direction.
Optionally, the outer wall of the inner tube is spaced apart from the inner wall of the outer tube by L, and L has the following characteristics:
L=0.866R~0.890R
wherein R is the radius of the inner tube.
Optionally, the lower end cover of the furnace body is provided with a central hole, and the upper end of a rod penetrating into the furnace body through the central hole is a container;
the rod is an output member of the feeding mechanism.
Optionally, the feeding mechanism further includes:
a linear driving mechanism whose driving direction is parallel to the axis of the lever;
and the parallel connection part is used for transversely connecting the linear driving mechanism and the rod.
Optionally, the parallel connection part is provided with a guide sleeve with an axis parallel to the rod;
correspondingly, the guide sleeve is matched, and a guide rod which is parallel to the rod and sleeved for the guide sleeve is also arranged on the rack of the linear driving mechanism and is used for guiding the parallel connection part.
Optionally, the frame of the linear driving mechanism is separated from the bracket for supporting the furnace body and is configured as an independent auxiliary bracket;
a gap is reserved between the rod and the central hole so as to avoid interference between the rod and the wall of the central hole.
Optionally, the auxiliary bracket is provided with a seat frame positioned below the furnace body and a back frame positioned at one side of the seat frame and extending upwards;
wherein, the back frame is used for the installation of sharp actuating mechanism on the auxiliary stand.
Optionally, the linear driving mechanism is a screw-nut screw mechanism, and a screw nut of the screw-nut screw mechanism is fixedly connected with the parallel connection component.
According to the embodiment of the invention, the existing single-tube structure is replaced by the double quartz tube matched with the heat-insulating cotton structure, the outer tube is provided with the heat-insulating coating, and it is understood that the heat-insulating coating is a heat-insulating structure based on the reflection principle, so that most of heat can be reflected, heat can be effectively insulated, the nested structure is far smaller than the single-tube structure matched with the heat-insulating cotton structure, the whole structure tends to be compact, and the weight is relatively light.
Drawings
FIG. 1 is a schematic diagram showing the structure of a vertical Bridgman furnace multiple compound crystal growth apparatus according to an embodiment of the present invention.
Fig. 2 is a schematic diagram of an assembly structure of the auxiliary bracket and the lifting mechanism.
FIG. 3 is a schematic view of a furnace structure.
In the figure: 1. the furnace comprises a furnace body, a lower furnace cover, a rod, a lifting mechanism, a connecting seat, a main support and an auxiliary support.
11. An inner tube 12, an upper heater 13, an outer tube 14, and a heat insulator; A. a high temperature region, a gradient region and a low temperature region.
31. The ampoule is supported.
41. And (5) a guide post.
51. And (5) guiding the sleeve.
71. Back frame, 72. Seat frame, 73. Reinforcing plate.
Detailed Description
Referring to fig. 1 of the drawings, a general structure of a vertical bridgman furnace multi-component compound crystal growth apparatus is shown, wherein a furnace body 1 is vertically arranged, namely, a process implementation of the bridgman method is realized by vertical movement.
The vertical Bridgman furnace multiple compound crystal growth apparatus shown in FIG. 1, the basic structure of which includes a furnace body 1, a main support 6 for vertically mounting the furnace body 1, the furnace body 1 needs to be stably erected so as to move the container in a vertical direction at a given speed.
The conventional feeding mechanism is to feed from top to bottom, and the inventor considers that the problem of sealing moving parts is caused by the fact that the furnace body 1 is an elongated member with a relatively large length-diameter ratio, and a certain length of operating rod is often required for feeding the container into the furnace body 1, and the rod 3 shown in fig. 1 is also an operating rod. The upper end of the furnace body 1 is provided with an upper end cover, the lower end is provided with a lower end cover, and if the operating rod extends into the furnace body 1 from the upper end, the operating rod needs to be in a matching relation with the upper end cover.
The bridgman furnace is not a vacuum furnace, and under the condition of heat convection, the heat of the high temperature area A is easy to dissipate from the upper gap, which is different from the structure shown in fig. 1, the rod 3 extends from the lower end cover of the furnace body 1, namely the lower furnace cover 2 in fig. 1, and the heat convection effect is smaller when the hot air is on the upper part. In this regard, the details will be described below, and the details will not be repeated here.
According to the embodiment of the invention, firstly, the furnace body 1 adopts a double quartz tube structure, and the quartz material can be the same as that of a quartz crucible.
The conventional structure of the furnace body 1 can be seen in the prior art documents cited in the background art, the prior furnace body 1 is usually provided with an inner tube body made of ceramic or quartz, and the inner tube body is coated with heat insulation material or heat insulation cotton, on the one hand, the whole volume is larger, and on the other hand, the heat insulation cotton is made of opaque materials, and once the heat insulation material is coated, the condition in the inner tube body, particularly, the growth condition of crystals in a quartz crucible, for example, cannot be observed.
In fig. 3, the furnace body 1 has a double-quartz tube structure, and the double-quartz tube has an inner tube 11 and an outer tube 13 which are coaxial or have relatively high coaxiality.
The inner diameter of the outer tube 13 is larger than the outer diameter of the inner tube 11, and a certain space is formed between the two, which is denoted as an intermediate space, which serves as an assembly space for the assembly of the upper heater 12 and the lower heater 15 and the heat insulator 14 in fig. 3 on the one hand, and also serves as a heat insulation space, such as the upper heater 12, for example, after the outer wall of the inner tube 11 is assembled, heating is mainly achieved by heat conduction, the specific gravity of heat radiation is relatively small, and the radial specification of the intermediate space affects the heating efficiency of the heat radiation to the outer tube 13.
Further, the surface of the outer tube 13 is coated with a heat insulating coating layer to reflect most of heat radiation, so that a good heat insulating effect can be obtained under the condition of relatively compact structure.
In contrast, the nested double-tube structure is relatively compact, and when the furnace body 1 needs to have motion, the compact and light weight is easier to realize than the traditional furnace body 1.
In regard to the heat insulation, as shown in fig. 3, there is provided a heat insulator 14 in the middle of the intermediate space in the up-down direction, so that the intermediate space is divided into three regions, i.e., a space in which the inner tube 11 is located at the upper portion of the heat insulator 14 is a high temperature region a, a space in which the inner tube is located at the lower portion of the heat insulator 14 is a low temperature region C, and a region in which the heat insulator 14 is located is a gradient region B.
The upper and lower principles are also principles of thermal convection, as are conventional Bridgman ovens.
As for the heaters, there are also two types, and are also provided in the intermediate space, including an upper heater 12 for heating the high temperature region a and a lower heater 15 for heating the low temperature region C.
The high temperature region a, the gradient region B, and the low temperature region C refer to temperature gradient regions within the inner tube 11.
With respect to the thermal barrier coating, it is only meant that a thermal barrier coating is present, which is produced by plating for the most part in the process, but not only by using a plating process, but in some applications, it may be produced by using a coating or spraying process, and the reflectivity to heat radiation may reach 87% or even higher with the development of coating technology, such as nano thermal barrier coating.
The heat insulation coating is preferably a gold coating, and the gold coating is more applied in the aerospace field, for example, the gold coating plated on the surface of a spacecraft has better reflection effect on cosmic rays and sunlight so as to protect equipment and personnel in the spacecraft. The gold plating layer has very high reflectivity which can reach more than 95 percent, and can play a good role in heat insulation.
The furnace body 1 adopts a double-quartz-tube structure, quartz belongs to transparent materials, and under the condition without a heat insulation coating, the situation in the double-quartz-tube can be clearly seen, but under the condition that the heat insulation coating is arranged, light rays can be shielded, the situation in the quartz-tube cannot be seen, and the situation in the furnace body 1 cannot be clearly seen as in the traditional furnace body 1 structure.
Unlike the prior art, which generally requires filling of insulation material between the outer and inner tubes, and cannot construct a window, in the embodiment of the present invention, since the double quartz tube is used, the construction of the window has a relatively good structural basis without filling of insulation material, and a plurality of unplated areas are left on the insulation coating to construct the window, so that an operator can observe the crystallization condition of the crystal through the window.
The coating is relatively thin, the window constructed is not necessarily large, and the viewing angle is relatively large based on the perspective effect, unlike the prior art, when the heat insulation is realized by filling the heat insulation material, a relatively large viewing range is required to be constructed. Therefore, in the condition of constructing the window, the smaller window has relatively less influence on heat insulation, unlike the structural condition of the conventional furnace body 1.
In a preferred implementation, the outer wall of the inner tube 11 is spaced apart from the inner wall of the outer tube 13 by L, and L has the following characteristics:
L=0.866R~0.890R
wherein R is the radius of the inner tube 11.
The above indicates the width of the intermediate space, or the distance between the outer wall of the inner tube 11 and the inner wall of the outer tube 13 is positively correlated with the specification of the inner tube 11, and the larger the inner tube 11, the larger the L.
Regarding the furnace body 1, as described above, the upper end of the conventional furnace body 1 has an upper end cap, and the lower end has a lower end cap, wherein the upper end cap is provided with a via hole for penetrating the operating rod of the container. Unlike the conventional furnace body 1 in the construction of the embodiment of the present invention, the rod 3 for the operation of the container, such as the ampoule holder 31 shown in fig. 2, penetrates from the lower end cap of the furnace body 1, and the lower furnace cover 2 is used for the installation of the lower end of the furnace body 1 on the main support 6, as shown in fig. 1, on the one hand. The lower furnace cover 2 is provided with a central hole, a rod penetrates into the furnace body 1 through the central hole, and the ampoule support 31 is arranged at the upper end of the rod 3.
Accordingly, the rod 3 is the output member of the feed mechanism.
Further, the feeding mechanism further includes:
a linear driving mechanism whose driving direction is parallel to the axis of the lever 3;
a flat connection for the transverse connection between the linear drive and the rod 3, such as the connection seat 5 shown in fig. 1.
The parallel connection part is used for suspending the output component of the linear driving mechanism to one side, and the parallel rod 3 and the linear driving mechanism are different from the direct connection of the rod 3 and the linear driving mechanism, so that the height of the main support 6 can be reduced, and the main support 6 is more stable.
Further, in order to improve the stability of the rod 3 when driven, the connection seat 5, as shown in fig. 1 and 2, is provided with a guide sleeve 51 having an axis parallel to the rod.
Correspondingly, the guide sleeve 51 is matched, and a guide rod 41 which is parallel to the rod 3 and sleeved for the guide sleeve 51 is further arranged on the rack of the linear driving mechanism and used for guiding the connecting seat 5, so that the connecting seat 5 runs up and down more stably.
The connecting seat 5 stably runs, so that the rod 3 is more stable, the container is relatively stable on one hand, and interference between the rod 3 and a central hole on the lower furnace cover 2 can be avoided on the other hand.
Further, the frame of the linear driving mechanism is separated from the bracket for supporting the furnace body to form an independent auxiliary bracket 7, so that the driving vibration generated by the linear driving mechanism is not directly transmitted to the main bracket 6, and the furnace body 1 is prevented from shaking.
Furthermore, a gap is reserved between the rod 3 and the central hole so as to avoid interference between the rod 3 and the central hole wall and ensure that the rod 3 is stably lifted and lowered.
Regarding the gap, due to the characteristics of the Bridgman furnace, no obvious heat convection can be generated when the furnace is heated up and cooled down, so that the furnace is different from the traditional Bridgman furnace, and the heat preservation effect is better.
Further, alternatively, the sub-bracket 7 has a seat frame 72 located below the furnace body 1, and a back frame 71 located on one side of the seat frame 72 and extending upward;
wherein the back frame 71 is used for mounting the linear driving mechanism on the auxiliary frame 71, the whole structure is relatively compact, the seat frame 72 can be positioned below the main frame 6, and the position relationship is relatively flexible under the condition that the main frame 6 is separated from the auxiliary frame 7.
Since the container needs to slowly descend in the furnace body 1, the screw pair can provide precise and relatively strong control, and therefore, preferably, the linear driving mechanism is a screw-nut screw mechanism, and a screw nut of the screw-nut screw mechanism is fixedly connected with the parallel connection component.

Claims (10)

1. The utility model provides a perpendicular Bridgman furnace polynary compound crystal growth equipment, includes furnace body, supports of supporting the furnace body to and the feeding mechanism of feeding in to the furnace body, its characterized in that, the furnace body includes:
the inner tube is a quartz tube arranged vertically;
the outer tube is a quartz tube, is nested outside the inner tube coaxially, and is spaced a given distance from the inner tube to form an intermediate space, and the surface of the outer tube is plated with a heat insulation coating;
the heat insulation piece is positioned in the middle of the upper and lower directions of the middle space, the space of the inner tube positioned at the upper part of the heat insulation piece is a high-temperature area, the space positioned at the lower part of the heat insulation piece is a low-temperature area, and the area where the heat insulation piece is positioned is a gradient area; and
the heater is positioned in the middle space and comprises an upper heater for heating the high-temperature area and a lower heater for heating the low-temperature area.
2. The vertical bridgman furnace multi-component compound crystal growth apparatus according to claim 1, wherein the heat insulating coating is a gold coating.
3. The vertical bridgman furnace multi-component compound crystal growing apparatus according to claim 1 or 2, wherein the insulating coating is provided with a plurality of windows which are not covered with the insulating coating in the up-down direction.
4. The vertical bridgman furnace multi-component compound crystal growing apparatus according to claim 1, wherein the distance between the outer wall of the inner tube and the inner wall of the outer tube is L, and L has the following characteristics:
L=0.866R~0.890R
wherein R is the radius of the inner tube.
5. The vertical bridgman furnace multiple compound crystal growing apparatus according to claim 1, wherein the lower end cap of the furnace body has a center hole, and an upper end of a rod penetrating into the furnace body through the center hole is a container;
the rod is an output member of the feeding mechanism.
6. The vertical bridgman furnace multi-component compound crystal growing apparatus of claim 5, wherein said feed mechanism further comprises:
a linear driving mechanism whose driving direction is parallel to the axis of the lever;
and the parallel connection part is used for transversely connecting the linear driving mechanism and the rod.
7. The vertical bridgman furnace multi-component compound crystal growing apparatus according to claim 6, wherein the horizontally connected member is provided with a guide sleeve having an axis parallel to the rod;
correspondingly, the guide sleeve is matched, and a guide rod which is parallel to the rod and sleeved for the guide sleeve is also arranged on the rack of the linear driving mechanism and is used for guiding the parallel connection part.
8. The vertical bridgman furnace multiple compound crystal growing apparatus according to claim 7, wherein the frame of the linear driving mechanism is separated from the frame supporting the furnace body to be constructed as a separate sub-frame;
a gap is reserved between the rod and the central hole so as to avoid interference between the rod and the wall of the central hole.
9. The vertical bridgman furnace multiple compound crystal growing apparatus according to claim 8, wherein the sub-mount has a mount below the furnace body, and a back mount located on one side of the mount and extending upward;
wherein, the back frame is used for the installation of sharp actuating mechanism on the auxiliary stand.
10. The vertical bridgman furnace multi-component compound crystal growth apparatus according to any one of claims 6 to 9, wherein the linear driving mechanism is a screw-screw mechanism, and a screw of the screw-screw mechanism is fixedly connected with the parallel connection member.
CN201710468013.5A 2017-06-20 2017-06-20 Vertical Bridgman furnace multi-component compound crystal growth equipment Active CN107083564B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109444210A (en) * 2018-12-19 2019-03-08 宝钛集团有限公司 A kind of dedicated sample heat-treatment furnace of transformation temperature test
CN110219046B (en) * 2019-05-31 2021-08-06 山东大学 A visual directional growth device and growth method for large-size bromine lead cesium single crystal

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CN1664175A (en) * 2004-12-22 2005-09-07 哈尔滨工业大学 Visible small-angle inclined region melting growth device and growth method of crystal
CN104047047A (en) * 2014-06-09 2014-09-17 北京雷生强式科技有限责任公司 Horizontal growth device and growth method of phosphorus silicon cadmium mono-crystal
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