CN114808108A - Bridgman-Stockbarger method crystal growth device and application thereof - Google Patents
Bridgman-Stockbarger method crystal growth device and application thereof Download PDFInfo
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- CN114808108A CN114808108A CN202210465233.3A CN202210465233A CN114808108A CN 114808108 A CN114808108 A CN 114808108A CN 202210465233 A CN202210465233 A CN 202210465233A CN 114808108 A CN114808108 A CN 114808108A
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/003—Heating or cooling of the melt or the crystallised material
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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
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/006—Controlling or regulating
Abstract
The application provides a crystal growth device by a Bridgman method, which comprises a furnace body, a crucible, a lifting unit, a heating unit, a temperature measuring unit, a temperature collecting unit and a control unit; the lifting unit controls the lifting of the crucible in the furnace body; the furnace body can be split, so that the growth process of the crystal can be observed conveniently at any time; the heating device is arranged in the heating furnace; the furnace body comprises a high-temperature area, a gradient area and a low-temperature area; the temperature of the high-temperature area and the low-temperature area is controlled independently; the temperature measuring device detects the temperature of the crucible; the temperature acquisition unit acquires the temperature detected by the temperature measuring device; the control unit controls the lifting of the lifting unit and the heating of the heating unit. The invention overcomes the defects of high height, heavy weight, difficult observation, difficult maintenance, difficult data acquisition and the like of the crystal furnace, is convenient for preliminarily knowing the growth condition of the crystal by utilizing a small furnace body, can also be used for showing experiments, and occupies small space. The experimental period is short, and the data can be accumulated quickly. The small-size crystal growth can be carried out, and a reference is provided for the large-size crystal growth.
Description
Technical Field
The invention relates to a small Bridgman crystal growth system with multiple data acquisition, in particular to a furnace body which can be placed on a table board and can be opened and closed by adopting a simplified growth furnace body and a lifting system in cooperation. The method is suitable for the experiment that the growth has low requirements on the crystal size, but the analysis and data acquisition are needed to be carried out on the crystal growth process. Belonging to the technical field of crystal growth.
Background
The artificial crystal growth method mainly comprises a solution growth method, a hydrothermal growth method, a cosolvent method, a pulling method, a Bridgman method and the like, wherein the pulling method and the Bridgman method are the most common and important methods for preparing large single crystals and single crystals with specific shapes, and have a dominant position of unmovable shaking in the field of single crystal material growth required in modern technical applications of electronics, optics and the like. In particular, the vertical Bridgman method, also known as Bridgman method, has attracted much attention in recent years, and is a method for growing crystals from a melt. Usually, the crucible is lowered in the crystallization furnace, and the melt is crystallized from bottom to top in the crucible into a whole crystal when passing through a region with a large temperature gradient. Compared with a pulling method, the method can adopt a fully-closed or semi-closed crucible, and the components are easy to control; the crystal grown by the method is remained in the crucible, so that the method is suitable for growing large-block crystals and can grow several crystals simultaneously in one furnace. In addition, the process conditions are easy to master, and the programming and automation are easy to realize.
Traditional crucible descending system adopts syllogic structural design more, and the furnace body part divide into high-temperature region, gradient district and low temperature district, adopts the electric stove silk heating, covers integrated into one piece insulation material outward, and high low temperature district independently controls the temperature, distinguishes different shapes through the design gradient and in order to obtain the ideal temperature ladder of needs. The furnace body is arranged on a furnace plate, and the furnace plate is connected with the rack through a leveling bolt and a damping leveling cushion block. A lifting device and a rotating device are arranged below the rack. However, although the conventional Bridgman-Stockbarge method is suitable for growing large-size crystals, when the growth conditions of the crystals are searched in the early stage, the experimental period is long, data are not easy to accumulate and the observation is inconvenient, the research and development and industrialization progress of crystal materials are greatly influenced, and in addition, the following defects are also caused:
(1) the traditional crucible descending system needs a large-size heat-insulating sleeve in order to achieve the required heat-insulating effect due to low heat-insulating efficiency of heat-insulating materials, is high in installation difficulty and extremely inconvenient to maintain;
(2) the lifting mechanism requires high furnace body height, and people need to climb to high position for operation during installation, so that the operation is inconvenient;
(3) the growth furnace mostly adopts a fully-closed structure, and is not suitable for observation at high altitude.
(4) Data acquisition is difficult, the temperature in the crucible cannot be easily monitored, and large data acquisition is not facilitated;
(5) the whole crucible descending system is large in size and inconvenient to move.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a small Bridgman crystal growth system with multiple data acquisition, which has the characteristics of miniaturization, portability, mobility, easiness in modification, observability, multiple data acquisition and the like. The system is mainly used for exploring growth conditions of the early-stage crystal to grow small-size crystals, and the diameter of the crystals is below 1 inch. The furnace body adopts a nano micropore heat insulating material with small heat conductivity coefficient, and compared with the traditional aluminum silicate heat insulating material, the furnace body has light weight and good heat insulating effect. The heat insulating material is processed into a semicircular clamping groove type heater embedded in the furnace wire, the number of heating sections can be freely set, and each section is connected through a clamping groove. The furnace body is designed into a half-round shape, so that the furnace body is convenient to load and instantaneously observe during growth. An independent lifting mechanism can enable the descending pipe to move up and down, and a crystal conversion motor interface is matched to meet different requirements. The descending pipe is internally provided with a multi-head thermocouple temperature measuring device which consists of a nanometer micropore heat insulating material and a thermocouple and is manufactured by opening the molds for different crucibles.
According to one aspect of the application, a crystal growth device by a Bridgman method is provided, which comprises a furnace body, a crucible, a lifting unit, a temperature measuring unit, a temperature collecting unit and a control unit;
the lifting unit controls the crucible to lift in the furnace body;
the furnace body comprises a heat-insulating layer and a heating unit;
the heat preservation unit is used for maintaining the temperature in the furnace body;
the heating unit is used for heating the heating furnace;
the furnace body comprises a high-temperature area, a gradient area and a low-temperature area;
the high temperature area and the low temperature area are independently controlled in temperature;
the temperature measuring unit is always in contact with the outer wall of the crucible and is used for detecting the temperature of the outer wall of the crucible;
the temperature acquisition unit is used for acquiring the temperature detected by the temperature measurement unit;
the control unit controls the lifting of the lifting unit and the heating of the heating unit.
The heat-insulating layer and the heating unit are designed in an integrated mode.
The furnace body can be split for observing the growth process of the crystal.
The height of the furnace body is 50-130 cm.
The furnace body comprises n identical stacked heating furnaces;
n is 2, 3, 4, 5 or 6;
the heat-insulating layer is a nano microporous heat-insulating material.
The maximum temperature resistance of the nano microporous heat-insulating material is 1100 ℃, and the density of the nano microporous heat-insulating material is 200-320 (kg/m) 3 ) The siliceous nanometer material with small heat conductivity coefficient (0.029W/mK at 600 ℃ and 0.036W/mK at 800 ℃) can be processed into any shape by opening a mold.
The heating unit comprises a resistance wire.
The temperature measuring unit comprises a thermocouple.
In the working process of the device, the temperature acquisition unit can record the temperature value detected by the temperature measurement unit at any time.
According to another aspect of the present application, there is provided a use of the above-described Bridgman-Stockbarge crystal growing apparatus,
for growing a consistent molten compound crystal having a melting point of 500-1100 ℃;
the diameter of the consistent molten compound crystals is 10mm to 25 mm.
A small crystal growth apparatus by Bridgman method is composed of nano-class microporous insulating material, resistance wire, temp controller, thermocouple, lifting motor, screw rod, guide track of polished rod and temp recorder. The volume and the weight of the furnace body are reduced by adopting the nano micropore heat insulating material, the furnace body can be separated from the lifting system, the furnace body can be opened at 180 degrees, a plurality of thermocouple probes can be distributed on a plurality of data acquisition devices, and the probes can be in close contact with the crucible.
Specifically, the device comprises a furnace body, a lifting system, a data acquisition system and a temperature control instrument;
the furnace body is formed by stacking a plurality of identical heating furnaces, the heating furnaces are connected through clamping grooves, and the heating furnaces are made of nano microporous heat-insulating materials. The resistance wire and the temperature measuring couple are connected with the temperature controller through a binding post, and the temperature controller receives the temperature in the furnace body detected by the temperature measuring couple and controls the work of the resistance wire. And a hinge is arranged on one side of the furnace body, and the furnace body on the opposite side of the hinge can be opened so as to observe the growth condition of the crystal at any time.
The lifting system comprises a stepping motor, a lead screw, a sliding block, a guide rail and a base. The data acquisition system comprises a cup stand, a downcomer, a temperature recorder and a multi-data temperature measuring device. The lead screw and the guide rail are fixed on the base, and the sliding block can move on the guide rail. The descending tube is fixed on the cup stand and moves up and down along with the up-and-down movement of the sliding block. The down pipe is made of nano microporous heat insulation material.
The multi-data temperature measuring device comprises a temperature measuring couple, a temperature recorder and a quartz crucible. The temperature measuring couple is in contact with the quartz crucible, and the temperature recorder records the temperature measured by the temperature measuring couple.
The working process comprises the following steps:
1) a furnace body assembling stage: each heating furnace section is stacked, each section is connected through a clamping groove, the sealing is guaranteed, and an external furnace wire is connected into a binding post.
2) And (3) a furnace loading stage: the crucible filled with raw materials in advance is placed into a data acquisition device with a opened mold, and the whole device is put down in a quartz descending tube. The down pipe is connected with the lifting system through the cup stand. Controlling the downcomer to rise to a required position,
2) and (3) growth stage: and (4) heating the upper hearth and the lower hearth to the required temperature at the speed of 50-100 ℃/h, keeping the temperature near the melting point of the raw materials for 24 hours, and melting the raw materials. And setting a proper descending rate, and carrying out descending growth on the crystal. After the program growth is finished, the temperature is reduced to room temperature at 20 ℃/h.
3) And (3) data recording: the thermocouple is connected with a temperature recorder to record the initial time. The temperature was recorded continuously from the start of the batch to the end of the growth.
Drawings
FIG. 1 is a schematic view of a crystal growth apparatus of the Bridgman method described in apparatus example 1;
FIG. 2 is a sectional view of a furnace body 1 in the Bridgman crystal growth apparatus described in apparatus example 1;
FIG. 3 is a schematic view of a lifting system 2 and a data acquisition system 3 connected to the lifting system 2 in the Bridgman crystal growing apparatus described in apparatus example 1;
FIG. 4 is a sectional view of the multidata temperature measuring device 34 in the Bridgman crystal growth apparatus described in apparatus example 1.
Part numbers are as follows:
1: furnace body, 11: nano microporous thermal insulation material, 12: resistance wire, 13: temperature measurement couple, 14: terminal, 15: hinge, 2: lifting system, 21: stepping motor, 22: a screw rod, 23: slider, 24: guide rail, 25: base, 3: data acquisition system, 31: cup holder, 32: downcomer, 33: temperature recorder, 34: multiple data temperature measuring devices, 35: quartz crucible, 4: a temperature control instrument.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
Apparatus example 1
A crystal growth device by a Bridgman method is shown in figure 1, and comprises a furnace body 1, a lifting system 2, a data acquisition system 3 and a temperature controller 4;
fig. 2 is a sectional view of the furnace body 1. The furnace body is formed by stacking 4 same heating furnaces, the heating furnaces are connected through clamping grooves, and the heating furnaces are formed by nanometer microporous heat insulation materials 11. The resistance wire 12 and the temperature measuring couple 13 are connected with the temperature controller 14 through a binding post 14, and the temperature controller 14 receives the temperature in the furnace body 1 detected by the temperature measuring couple 13 and controls the work of the resistance wire 12. A hinge 15 is arranged on one side of the furnace body 1, and the furnace body on the opposite side of the hinge 15 can be opened so as to observe the growth condition of crystals at any time.
Fig. 3 is a schematic diagram of the lifting system 2 and the data acquisition system 3 connected to the lifting system 2. The lifting system comprises a stepping motor 21, a lead screw 22, a slide block 23, a guide rail 24 and a base 25. The data acquisition system comprises a cup holder 31, a down pipe 32, a temperature recorder 33 and a multi-data temperature measuring device 34. The lead screw 22 and the guide rail 24 are fixed to a base 25, and the slider 23 is movable on the guide rail 24. The down pipe 32 is fixed to the cup holder 31 and moves up and down in accordance with the up and down movement of the slider 23. The down pipe 32 is made of a nano-micro porous heat insulating material 11.
Fig. 4 is a cross-sectional view of the multiple data temperature measuring device 34. The multi-data temperature measuring device comprises a temperature measuring couple 13, a temperature recorder 33 and a quartz crucible 35. The temperature measuring couple 13 is in contact with the quartz crucible 35, and the temperature recorder records the temperature measured by the temperature measuring couple 13.
Example 1
Growing lanthanum bromide crystals
The apparatus described in apparatus example 1 was used.
The four heating furnace sections are stacked together, the middle clamping grooves are connected, and the furnace wires are connected to the binding posts. And moving the lifting system to the center of the furnace mouth and opening the furnace chamber. 1 inch lanthanum bromide crystal is selected to grow, the raw materials are 300 g in total, the lanthanum bromide crystal raw material is purchased from Sigma-Aldrich 5N grade raw material, the raw materials are evenly mixed in a glove box filled with high-purity nitrogen gas and then are put into a quartz tube, then a quartz block is used for plugging the opening of the quartz tube, then the opening of the quartz tube is sealed by epoxy resin, the glove box is taken out, and the opening of the quartz crucible is melted and sealed by oxyhydrogen flame. Then the quartz crucible 35 is put into a multi-data temperature measuring device 34, the temperature measuring thermocouple 13 is ensured to be in contact with the outer surface of the quartz crucible 35, and 5 temperature measuring probes are arranged. And (3) placing the multiple data temperature measuring device 34 into the descending pipe 32, locking the descending pipe 32 and the cup holder 31, raising the height to a required height, closing the hearth to heat and melt the materials, then cooling at a cooling rate of 1 ℃/h, enabling the lanthanum bromide melt to eliminate seed crystals growing in the C direction under the action of the seed crystals, cooling at a cooling rate of 10 ℃/h after the growth until the temperature is reduced to the room temperature, and finishing the growth of the single-crystallized crystals. And finally, opening the hearth, and taking out the quartz crucible 35 from the multi-data temperature measuring device 34.
The size of the obtained transparent single crystal is phi 25 x 70mm 3 Obtaining 5 temperature measuring points and cutting and packaging into phi 25 x 25mm 3 The energy resolution of the photoelectric peak of a Cs-137 radioactive source is 3.8 percent under 662kev when a scintillation probe formed by coupling the scintillator and a double-alkali cathode photomultiplier is tested.
Example 2
Growing barium gallium sulfide crystal
The apparatus described in apparatus example 1 was used.
The three heating furnace sections are stacked together, the middle clamping grooves are connected, and the furnace wires are connected to the wiring terminals. And moving the downcomer to the center of the furnace mouth, and opening the furnace chamber. Selecting 1 inch of barium sulfogallium crystal for growth, wherein the raw material is 250 g in total, the raw material of the barium sulfogallium crystal is purchased from Sigma-Aldrich 4N-grade elementary substance raw material, synthesizing three elementary substances of barium, sulfur and gallium at high temperature of 1100 ℃, uniformly mixing the three elementary substances in a glove box filled with high-purity nitrogen, then filling the mixture into a quartz tube, then plugging the opening of the quartz tube by a quartz block, then sealing the opening of the quartz tube by epoxy resin, taking out the glove box, and melting and sealing the opening of the quartz crucible 35 by oxyhydrogen flame. Then the quartz crucible 35 is put into a multi-data temperature measuring device 34, the temperature measuring thermocouple 13 is ensured to be in contact with the outer surface of the quartz crucible 35, and 7 temperature measuring probes are provided. And (3) putting the down pipe 32 into the multi-data temperature measuring device 34, locking the down pipe 32 and the cup holder 31, raising the height to a required height, closing the hearth to heat and melt, cooling at a cooling rate of 0.5 ℃/h, enabling the crystal to eliminate the seed crystal growing in the direction a under the action of the seed crystal by the sulfur-gallium-barium melt, cooling at a cooling rate of 10 ℃/h after the crystal grows until the temperature is reduced to the room temperature, and finishing the growth of the single crystal after the single crystallization. And finally, opening the hearth and taking out the quartz crucible from the temperature measuring device. The obtained transparent single crystal has size of phi 25 x 40mm 3 And 7 temperature measurement point whole-process data are obtained. Processing a wafer with thickness of 1mm and thickness of 4mm to 4mm, and measuring that the absorption coefficient is less than or equal to 0.1cm under the wave band of 1.06 microns -1 。
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. A crystal growth device by a Bridgman method is characterized in that,
comprises a furnace body, a crucible, a lifting unit, a temperature measuring unit, a temperature collecting unit and a control unit;
the lifting unit controls the crucible to lift in the furnace body;
the furnace body comprises a heat-insulating layer and a heating unit;
the heat preservation unit is used for maintaining the temperature in the furnace body;
the heating unit is used for heating the heating furnace;
the furnace body comprises a high-temperature area, a gradient area and a low-temperature area;
the high temperature area and the low temperature area are independently controlled in temperature;
the temperature measuring unit is always in contact with the outer wall of the crucible and is used for detecting the temperature of the outer wall of the crucible;
the temperature acquisition unit is used for acquiring the temperature detected by the temperature measurement unit;
the control unit controls the lifting of the lifting unit and the heating of the heating unit.
2. The crystal growth apparatus of claim 1, wherein the crucible is provided with a crucible having a bottom surface,
the heat-insulating layer and the heating unit are designed in an integrated mode.
3. The crystal growth apparatus of claim 1, wherein the crucible is provided with a crucible having a bottom surface,
the furnace body can be split for observing the growth process of the crystal.
4. The crystal growth apparatus of claim 1, wherein the crucible is provided with a crucible having a bottom surface,
the height of the furnace body is 50-130 cm.
5. The crystal growth apparatus of claim 1, wherein the crucible is provided with a crucible having a bottom surface,
the furnace body comprises n identical stacked heating furnaces;
and n is 2, 3, 4, 5 or 6.
6. The crystal growth apparatus of claim 1, wherein the crucible is provided with a crucible having a bottom surface,
the heat-insulating layer is a nano microporous heat-insulating material.
7. The crystal growth apparatus of claim 1, wherein the crucible is provided with a crucible having a bottom surface,
the heating unit comprises a resistance wire.
8. The crystal growth apparatus of claim 1, wherein the crucible is provided with a crucible having a bottom surface,
the temperature measuring unit comprises a thermocouple.
9. The crystal growth apparatus of claim 1, wherein the crucible is provided with a crucible having a bottom surface,
in the working process of the device, the temperature acquisition unit can record the temperature value detected by the temperature measurement unit at any time.
10. Use of the crystal growth apparatus according to any one of claims 1 to 9, wherein,
for growing consistent molten compound crystals with a melting point of 500-1100 ℃;
the diameter of the consistent molten compound crystals is 10mm to 25 mm.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017166001A1 (en) * | 2016-03-28 | 2017-10-05 | 中国科学院福建物质结构研究所 | Ba3p3o10cl single crystal growth method and crystal growth device |
| CN206666673U (en) * | 2017-04-05 | 2017-11-24 | 上海新漫晶体材料科技有限公司 | A kind of multistation crucible declines stove |
| CN206814880U (en) * | 2017-06-09 | 2017-12-29 | 厦门中烁光电科技有限公司 | The adjustable crystal growing apparatus of thermal field |
| CN113818073A (en) * | 2021-09-09 | 2021-12-21 | 河南微米光学科技有限公司 | Automatic control device and control method for growing crystal based on Bridgman method |
| CN215856440U (en) * | 2021-09-09 | 2022-02-18 | 河南微米光学科技有限公司 | Automatic control device for growing crystals based on Bridgman method |
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2022
- 2022-04-29 CN CN202210465233.3A patent/CN114808108A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017166001A1 (en) * | 2016-03-28 | 2017-10-05 | 中国科学院福建物质结构研究所 | Ba3p3o10cl single crystal growth method and crystal growth device |
| CN206666673U (en) * | 2017-04-05 | 2017-11-24 | 上海新漫晶体材料科技有限公司 | A kind of multistation crucible declines stove |
| CN206814880U (en) * | 2017-06-09 | 2017-12-29 | 厦门中烁光电科技有限公司 | The adjustable crystal growing apparatus of thermal field |
| CN113818073A (en) * | 2021-09-09 | 2021-12-21 | 河南微米光学科技有限公司 | Automatic control device and control method for growing crystal based on Bridgman method |
| CN215856440U (en) * | 2021-09-09 | 2022-02-18 | 河南微米光学科技有限公司 | Automatic control device for growing crystals based on Bridgman method |
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