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CN116200823B - Crystal growth device and cesium iodide crystal growth method - Google Patents

Crystal growth device and cesium iodide crystal growth method Download PDF

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Publication number
CN116200823B
CN116200823B CN202211576792.8A CN202211576792A CN116200823B CN 116200823 B CN116200823 B CN 116200823B CN 202211576792 A CN202211576792 A CN 202211576792A CN 116200823 B CN116200823 B CN 116200823B
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growth
crystal
crystal growth
furnace tube
seed
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CN116200823A (en
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郑霄
刘伟
陆海松
刘柱
王伟
孙磊
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Yirui New Material Technology Taicang Co ltd
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Yirui New Material Technology Taicang 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
    • C30B27/00Single-crystal growth under a protective fluid
    • C30B27/02Single-crystal growth under a protective fluid by pulling from a melt
    • 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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/12Halides
    • 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)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention belongs to the technical field of single crystal growth, and particularly relates to a crystal growth device and a cesium iodide crystal growth method. The crystal growth device is provided with a furnace shell, a heat insulation material is filled in the furnace shell, and a furnace chamber is formed in the center of the heat insulation material; the furnace chamber is internally provided with a visual furnace tube, the top of the visual furnace tube is covered with a sealing member, and the sealing member is provided with a ventilation valve for adjusting the atmosphere in the visual furnace tube; an upper heating device and a lower heating device are circumferentially arranged on the periphery of the visual furnace tube; placing a crucible in the visual furnace tube, arranging a growth mold in the crucible, wherein a vertically through middle gap is formed in the growth mold, and the upper surface of the growth mold is provided with a V-shaped notch communicated with the middle gap; the seed rod passes through the sealing piece in a sliding and sealing way, the seed rod vertically faces the V-shaped notch of the growth mould, and the lower end of the seed rod can be fixed with seed crystals for guiding the growth of crystals. The invention can rapidly crystallize in a large gradient temperature thermal field, realizes rapid growth of cesium iodide crystals, and has high crystal quality.

Description

Crystal growth device and cesium iodide crystal growth method
Technical Field
The invention belongs to the technical field of single crystal growth, and particularly relates to a crystal growth device and a cesium iodide crystal growth method.
Background
The cesium iodide thallium doped (CsI: tl) crystal has important application value in the fields of security detection, radiation detection and medical imaging.
The traditional cesium iodide crystal growth mode comprises the following steps: a crucible descending method and a pulling method. Wherein, the crucible descending method can grow cesium iodide crystals with high quality, but the growth speed is generally slower (1-3 mm/h); in the later stage of crystal growth, the gradient of a growth interface is reduced due to poor heat conduction, and the growth interface is sunken downwards, so that impurities cannot be discharged to the crucible wall and are concentrated in the central axis area of the crystal, and the tail performance of the crystal is affected. In addition, the segregation coefficient of thallium ions in cesium iodide crystals is about 0.12, which results in far-reaching difference between thallium ion concentrations at the front and rear stages of the crystals and also seriously affects light output uniformity and crystal utilization. Although the pulling method can grow cesium iodide crystals with larger size, the number of bubble impurities and the like in the crystals is large, the quality of the crystals is poor, and the concentration of doped ions is not uniform before and after the growth.
Therefore, it is of great research and practical importance to find a growth technique that uniformly distributes dopant ions in cesium iodide crystals.
Disclosure of Invention
The invention provides a crystal growth device and a cesium iodide crystal growth method. The invention aims to overcome the defects of the prior art and provide a CsI crystal growth device and a CsI crystal growth method which have the advantages of high crystallization speed, high crystal quality and uniform doping ion distribution.
A first aspect of the present invention provides a crystal growth apparatus, the apparatus comprising: a crucible for holding a raw material melt for crystal growth; a crystal growth die for guiding the flow direction of the raw material melt; and the seed rod is used for guiding the crystal to grow.
The growth mould is arranged in a crucible and fixed by a mould clamping sleeve, after raw materials in the crucible are melted, the raw material melt rises to a V-shaped notch at the top end of the growth mould from a mould slot through siphon action, and crystal growth is carried out through seed crystal traction; the seed rod can move up and down and is arranged above the growth mould; the lower part of the seed rod is provided with seed crystals for pulling the crystal to grow, the crucible is arranged in a visual furnace tube, the upper part of the crucible is provided with a sealing flange, and the furnace tube is sleeved with a resistance heating coil.
The thickness of the crystal growth is defined by the growth mold width and the width of the crystal growth is defined by the growth mold length. The width of the slit of the die is 0.3-0.8mm, and the angle of the opening is 100-150 degrees.
Further, the crystal growth mold is made of graphite or quartz, preferably made of high-purity quartz or three-high isostatic pressing graphite. The crucible is made of quartz, and the seed rod is made of molybdenum.
The device also comprises a furnace shell, wherein the furnace shell is preferably made of 304 stainless steel, and a fiber heat insulation material for further heat preservation is piled between the furnace shell and the visible furnace tube, so that heat loss in the crystal growth process is avoided.
Further, a gas release valve, an air charging valve, an observation window and a lifting sealing device for passing the seed rod are arranged on the sealing flange.
Furthermore, the seed crystal is CsI single crystal bar, the growth direction is 111, and the crystal quality can be effectively improved.
The first aspect of the invention provides a cesium iodide crystal growth method, which adopts the device to perform growth.
The method comprises the following steps:
step one: preparation of materials
The CsI feed containing the dopant was mixed.
Step two: charging material
And under a dry and clean environment, filling CsI raw materials into a crucible, adjusting the distance between a seed crystal and a die opening of a crystal growth die, and placing CsI broken grains at the crystal growth die opening as a melting point reference material.
Step three: melting crystal
Vacuumizing and filling protective gas, wherein the protective gas is Ar and N preferably 2 The method comprises the steps of carrying out a first treatment on the surface of the Heating until the material block is observed to be melted, obtaining a raw material melt, and observing a feed slot at the bottom of a V-shaped groove at the top end of the crystal growth die and a bright melt surface line.
Step four: seeding
And lowering the seed crystal to make the seed crystal contact with the V-shaped notch on the die opening of the crystal growth die until the lower end of the seed crystal contacts the molten liquid level at the bottom end of the seed crystal, then lowering the temperature, and pulling the seed crystal rod to enable the raw material melt to condense and grow on the seed crystal.
Step five: shoulder pad
After the crystal seeding is finished, the whole temperature is reduced, a shouldering stage is carried out, the lifting speed of a seed rod is maintained at the stage, the set temperature is reduced, the crystal becomes thicker and wider gradually along with the upward lifting process, and the width of the crystal is equal to the width of a growing die.
Step six: constant diameter growth
After shouldering is finished, as the seed rod is pulled, crystals grow in a constant width, namely the design width of the die; the growth rate is constant at this stage, the Gao Dila rate is increased until the melt of the raw material in the crucible is exhausted, the crystal automatically leaves the crystal growth mold, and the crystal growth is finished.
Step seven: cooling and annealing
And after the crystal growth is finished, cooling and annealing to room temperature are started.
Further, the specific steps of the first step are as follows: csI and TlI powder with the purity of 99.999% are selected as raw materials; first, 3000g CsI and 6g TlI powder were respectively added at 2X 10 -3 Baking in pa vacuum environment at 200-300 deg.C for 6-20 hr to remove adsorbed water; then weighing 2 raw materials, and uniformly mixing the weighed raw materials in a mortar under a dry and clean environment.
Further, the temperature rising rate in the third step is 60-100 ℃/h; the pulling rate in the fourth step is 3-5mm/h; in the fifth step, the speed of reducing the set temperature is 20-50 ℃/h; in the fifth step, the pulling rate is 5-18mm/h; and step seven, the cooling rate of cooling and annealing is 40-60 ℃/h.
Advantageous effects
The invention puts the raw materials into a crucible for heating and melting, the melt rises to the top end of the mould along the slit of the mould under the capillary action, the liquid level at the top of the mould is connected with a seed crystal for lifting the melt, and the melt is gradually solidified along with the cooling to grow single crystals with the same shape as the edge of the mould. The invention can rapidly crystallize in a large gradient temperature thermal field, thereby realizing rapid growth of cesium iodide crystals. The solid-liquid interface of the grown crystal is small, the crystal is not affected by the doping segregation coefficient, the crystallization speed is high, the crystal quality is high, and the grown crystal can grow according to the required size of processing.
Drawings
FIG. 1 is a schematic structural view of a crystal growth apparatus according to the present invention.
Fig. 2 is a schematic cross-sectional view of a growth mold.
Fig. 3 is a top view of a growth mold.
FIG. 4 is a schematic diagram of a sampling position.
Fig. 5 shows thallium iodide concentration and light output results.
In the figure, 1, a seed rod; 2. seed crystal; 3. growing a mould; 4. a raw material melt; 5. a crystal; 6. a crucible; 7. a visual furnace tube; 8. a lower heating device; 9. an upper heating device; 10. a heat insulating material; 11. a furnace shell; 12. a bleed valve; 13. an inflation valve; 14. and (5) sealing the flange. Detailed Description
The invention is further illustrated by the following specific examples, which are intended to illustrate the problem and to explain the invention, without limiting it.
In a first aspect, a cesium iodide crystal growth apparatus is provided.
As shown in fig. 1, the device is provided with a furnace shell 11, wherein the furnace shell 11 is preferably made of 304 stainless steel, and the furnace shell 11 is filled with a heat insulation material 10 for avoiding heat dissipation during the growth of crystals 5, and the heat insulation material 10 can be a fiber heat insulation block, preferably an alumina fiber heat insulation block; a vertical air-accommodating space, i.e., a cavity, is formed in the center of the insulating material 10.
The center of the furnace chamber is provided with a visible furnace tube 7 made of columnar transparent material so as to observe the internal condition, and the visible furnace tube 7 is preferably made of quartz material; the top of the visible furnace tube 7 is opened, and a sealing flange 14 is covered at the opening, so that a closed space is formed inside the visible furnace tube 7, and the stability of the internal growth atmosphere is kept. In order to facilitate accurate regulation and control of the atmosphere in the visual furnace tube 7, a gas release valve 12 and an inflation valve 13 are also arranged on the sealing flange 14; in addition, for the convenience of observation, a transparent observation window is provided on the sealing flange 14.
An annular space is provided between the visible furnace tube 7 and the heat insulating material 10, and heating devices surrounding the visible furnace tube 7 are arranged in the annular space and are divided into an upper section and a lower section, the lower section is marked as a lower heating device 8, the upper section is marked as an upper heating device 9, and the upper section and the lower section are used for respectively controlling the upper temperature and the lower temperature, wherein the lower heating device 8 is mainly used for heating the lower crucible 6 and raw materials in the crucible 6, and the upper heating device 9 is mainly used for heating the upper space and heating in an annealing stage. When the crystal 5 grows, the lower temperature is high, the upper temperature is low, and the upper temperature and the lower temperature are respectively controlled so as to realize a large temperature gradient and realize the rapid growth of the crystal 5.
A crucible 6 is placed in the view tube 7, the crucible 6 is used for containing the raw material melt 4 for crystal growth, and the position of the crucible 6 corresponds to the lower heating device 8. A growth mold 3 is arranged in the crucible 6 at an upper position.
As shown in fig. 2 and 3, the growth mold 3 has a slit extending downward therein, which is called a middle slit. The upper surface of the growth mould 3 is provided with an elongated V-shaped notch communicated with the middle gap. The intermediate gap is inserted into the raw material melt 4, and the raw material melt 4 is grown by crystallization from the intermediate gap up to the V-shaped notch on the upper surface of the growth mold 3 under the capillary action, so that the thickness of the grown crystal 5 is defined by the width of the V-shaped notch, and the width of the grown crystal 5 is defined by the length of the V-shaped notch. Therefore, the size of the crystal 5 can be effectively adjusted by adjusting the size of the V-shaped notch, thereby reducing the post-processing and improving the utilization rate of raw materials.
A seed rod 1 capable of moving up and down is penetrated in the center of the sealing flange 14, and sliding seal is arranged between the seed rod 1 and the sealing flange 14. The seed rod 1 vertically faces the V-shaped notch of the growth mould 3, and the seed crystal 2 is fixed at the lower part of the seed rod 1 and is used for guiding the raw material melt 4 at the V-shaped notch to grow to form crystals 5. The upper end of the seed rod 1 is connected with a driving device capable of pulling the seed rod 1 upwards, and the driving device drives the seed rod 1 to gradually upwards move along with the growth of the crystal 5, so as to guide the crystal 5 to gradually grow upwards.
In a second aspect, a cesium iodide crystal growth method is provided.
The cesium iodide crystal growth apparatus described above was used for growth. The growth mould 3 is formed by processing high-purity quartz, and the dimensions of each part of the growth mould 3 are as follows: the middle gap is 0.8mm wide, the angle of the V-shaped notch is 120 degrees, the width of the V-shaped notch is 5mm, and the length of the V-shaped notch is 100mm. The seed crystal 2 is CsI cylindrical single crystal bar grown by a descent method, phi 5mm, and the growth direction is [111].
Step one: preparation of materials
Firstly, csI and TlI raw materials are respectively in 2 multiplied by 10 -3 Baking for 12 hours at 300 ℃ in a Pa vacuum environment, and removing water adsorbed in the raw materials; then, 3000g CsI and 6g TlI were weighed, and the weighed materials were uniformly mixed in a dry and clean environment using a mortar.
Step two: charging material
Under the dry and clean environment, the raw materials are filled into a crucible 6, the distance between the bottom of a seed crystal 2 and the plane of a V-shaped notch of a mould of a growth mould 3 is adjusted to be more than or equal to 2cm, and CsI broken crystal grains are placed at the V-shaped notch of the growth mould 3 to serve as melting point reference materials.
Step three: melt material
The visual furnace tube 7 is vacuumized, then protective gas Ar is filled to 0.1Mpa, the two heating areas are heated to 100 ℃/h, the raw materials in the crucible 6 can be observed to be melted from the observation window of the sealing flange 14 to form a raw material melt 4, broken crystal grains at the upper part of the V-shaped notch at the top end of the growth die 3 are melted, and a bright melt surface line is visible at the middle gap.
Step four: seeding
The seed crystal 2 was lowered to bring the seed crystal 2 close to the V-shaped notch of the growth mold 3 until the lower end of the seed crystal contacted the melt level, and held for 5 minutes. Melting and then reducing the temperature, pulling the seed rod 1, controlling the pulling rate to be 4mm/h, and enabling the raw materials to coagulate and grow on the seed crystal 2.
Step five: shoulder pad
And after seeding is completed, a shouldering stage is carried out, the pulling speed is higher than the seeding speed and lower than the constant diameter growth pulling speed, and the cooling slope is 20 ℃/h. The crystal 5 becomes thicker and wider gradually along with the upward pulling process until the width reaches the width of the corresponding growth mold 3, and the temperature reduction is stopped at this time to continue pulling.
Step six: constant diameter growth
After shouldering, as the seed rod 1 is pulled, flaky crystals 5 grow at a constant width of 100 mm; the growth rate is constant at this stage, the Gao Dila rate is kept to 12mm/h until the raw material in the crucible 6 is exhausted, the crystal 5 automatically leaves the mold, and the crystal growth is finished.
Step seven: cooling and annealing
After the crystal growth is finished, the temperature of the crystal 5 is kept for 24 hours at 480 ℃ in an annealing area at the upper part, and then the temperature is reduced to room temperature, wherein the temperature reduction rate is 30 ℃/h.
Step eight: taking out crystal
After the furnace chamber is cooled to room temperature, the seed rod 1 is taken out, and the crystal 5 is taken down.
Performance testing
The flaky crystals 5 obtained by growth were sampled in accordance with the regions (1) to (6) shown in fig. 4, and thallium iodide concentration and light output were measured, respectively, using ICP-MS, and light output was measured using an X-ray tube and a PD photo sensor.
The test results are shown in FIG. 5, which shows that Tl ions are uniformly distributed throughout the crystal 5, and the light transmission is substantially uniform.
The above embodiments are illustrative for the purpose of illustrating the technical concept and features of the present invention so that those skilled in the art can understand the content of the present invention and implement it accordingly, and thus do not limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.

Claims (4)

1. A cesium iodide crystal growth method characterized in that: the following crystal growth apparatus was used for growth:
the crystal growth device is provided with a furnace shell, a heat insulation material is filled in the furnace shell, and a furnace chamber is formed in the center of the heat insulation material; the furnace chamber is internally provided with a visual furnace tube, and the top of the visual furnace tube is covered with a sealing element to form a closed space inside; the sealing piece is provided with a ventilation valve for adjusting the atmosphere in the visible furnace tube;
the periphery of the visual furnace tube is circumferentially provided with heating devices which are divided into an upper section and a lower section, the lower part is marked as a lower heating device, and the upper part is marked as an upper heating device and used for controlling the upper temperature and the lower temperature respectively;
placing a crucible in the visible furnace tube for containing raw material melt for crystal growth, wherein the position of the crucible corresponds to the lower heating device;
a growth die is arranged in the crucible, a vertically through middle gap is formed in the growth die, and a V-shaped notch communicated with the middle gap is formed in the upper surface of the growth die; the middle gap is inserted into the crucible, so that the raw material melt is guided to the V-shaped groove opening by capillary action;
the seed rod passes through the sealing piece in a sliding and sealing way, the seed rod vertically faces the V-shaped notch of the growth mould, and the lower end of the seed rod can be fixed with seed crystals for guiding the growth of crystals;
the growth die is made of graphite or quartz, the width of the middle gap is 0.3-0.8mm, and the upward opening angle of the V-shaped groove opening is 100-150 degrees;
the growth method comprises the following steps:
step one: preparation of materials
Preparing a dried mixed raw material of CsI and TlI;
step two: charging material
Filling raw materials into a crucible;
step three: melt material
The protective gas is replaced by the visible furnace tube, and the temperature is raised until the raw material is melted, so as to obtain a raw material melt;
step four: seeding
Lowering the seed crystal to make the seed crystal approach the V-shaped notch of the growth mould until the lower end of the seed crystal contacts the molten liquid level, then lowering the temperature, lifting the seed rod, and condensing and growing the melt on the seed crystal;
step five: shoulder pad
Maintaining the lifting speed of the seed rod after seeding is completed, reducing the heating power to cool until the width of the crystal reaches the width of the V-shaped notch of the growth die;
step six: constant diameter growth
After shouldering is finished, increasing the lifting speed to enable the crystal to grow at a constant width, and automatically separating from a growth mould after the crystal growth is finished;
step seven: cooling and annealing
Cooling and annealing to room temperature after crystal growth is finished;
the seed crystal is a CsI single crystal bar, and the growth direction is [111];
step one, csI and TlI raw materials are respectively processed under the pressure of not more than 2 multiplied by 10 -3 Baking at 200-300 ℃ for 6-20h in Pa vacuum environment, and removing water adsorbed in the raw materials; then uniformly mixing the weighed raw materials in a dry and clean environment by using a mortar;
in the third step, heating is carried out to ensure that the heating rate of raw material melting is 60-100 ℃/h; in the fifth step, the cooling rate is 20-50 ℃/h; in the seventh step, the cooling rate of the cooling annealing is 40-60 ℃/h;
in the fourth step, the pulling rate is 3-5mm/h; in the fifth step, the pulling rate is 5-18mm/h.
2. The cesium iodide crystal growth method according to claim 1, wherein: the lower heating device is an electric heating coil set arranged around the visible furnace tube, and the upper heating device is an electric heating coil set arranged around the visible furnace tube.
3. The cesium iodide crystal growth method according to claim 1, wherein: the crucible is made of quartz, the seed rod is made of molybdenum, and the visible furnace tube is made of quartz.
4. The cesium iodide crystal growth method according to claim 1, wherein: the sealing element is a sealing flange, a deflation valve and an inflation valve are further arranged on the sealing flange, and an observation window made of transparent materials is further arranged on the sealing flange.
CN202211576792.8A 2022-12-09 2022-12-09 Crystal growth device and cesium iodide crystal growth method Active CN116200823B (en)

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