CN109402724B - Non-doped and Eu2+Directional zone-melting growth device and method for doped strontium iodide crystal - Google Patents
Non-doped and Eu2+Directional zone-melting growth device and method for doped strontium iodide crystal Download PDFInfo
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- 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
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
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- 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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/08—Production of homogeneous polycrystalline material with defined structure from liquids by zone-melting
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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Abstract
The invention provides a non-doped Eu2+A directional zone-melting growth device and method for doped strontium iodide crystal, the device comprises: the device comprises a lifting support, a roller lead screw platform supported by the lifting support, a moving temperature field controlled by a stepping motor and moving relative to the roller lead screw platform, a quartz glass furnace tube fixed on the roller lead screw platform through a fixed support and transversely penetrating the moving temperature field, and a growth container arranged in the quartz glass furnace tube. The method is favorable for realizing the dynamic or real-time observation of crystal growth, can obtain the crystal in a specific direction by adopting a seed crystal inoculation process, simultaneously ensures that the top of the grown crystal is in an unrestricted state, reserves a space for the expansion of the crystal, is favorable for timely releasing the internal stress of the crystal and reducing the cracking of the crystal, and has the advantages of high growth speed, high success rate of crystal growth and excellent quality of the prepared single crystal, thereby greatly reducing the production cost of the crystal.
Description
Technical Field
The invention belongs to the field of halide crystal preparation, and particularly relates to non-doped Eu2+Doped strontium iodide (SrI)2) A device and a method for directional zone-melting growth of crystals.
Background
The scintillation crystal is a kind of optical functional crystal material which can emit ultraviolet light, visible light or infrared light under the irradiation of high-energy particles (such as X or gamma rays, etc.), and is widely applied to scientific experiments of high-energy physics, nuclear physics, astronomical physics, etc., and fields closely related to the nation and the civilian such as nuclear medicine, oil well detection, industrial CT (computed tomography), safety inspection, etc.
In 1969, U.S. Robert Hofstadter applied for Eu2+Doped strontium iodide crystals (SrI)2Eu) as a radiation detecting material, but the properties were comparable to those of Tl already commercialized due to the poor quality of the crystals produced at that time+Ion doping of NaI crystals is not advantageous and its related research subsequently falls into a silence of nearly 40 years. Until 2008, Nerine Cherepy et al prepared high quality SrI with financial support from departments such as the united states department of homeland security and energy2Eu crystal, study shows that SrI2Eu, which has a light output of 120,000 ph/MeV and is known to be the inorganic scintillator with the highest light output, has excellent energy resolution (<3%) with better energy linearity over a wider energy range. Undoped and Eu2+Doped strontium iodide as a scintillator is paid more attention to the field of inorganic scintillators, and research related to the doped strontium iodide is rapidly becoming a hotspot and frontier for inorganic scintillator research. At present, the method for growing strontium iodide crystals at home and abroad mainly adopts a Bridgman-Stockbarge method, and has the defects of complicated equipment, difficult observation of the growth process, large stress of the grown crystals, easy cracking and the like.
SrI2The melting point (538 ℃) is low, no cleavage plane exists, no phase change exists in the range from the melting point temperature to room temperature, and the growth is suitable for a melt method comprising a crucible descending method. Due to SrI2Is alkaline earth metal halide, is extremely easy to deliquesce and oxidize, and the following growth process is generally adopted internationally at present: anhydrous high-purity SrI2And EuI2The raw materials are weighed and mixed in proportion, then the mixture is loaded into a high-purity quartz crucible, the high-purity quartz crucible is sealed by melting after vacuum pumping, and crystal growth is carried out in a crucible descending furnace.
However, the crucible lowering method for growing the strontium iodide crystal has the following problems:
1) thermal expansion coefficient of quartz crucible (0.6X 10)-6℃-1) Thermal expansion coefficient (0.9-2.1X 10) with strontium iodide crystal-5℃-1) The difference is large, and during the growth process of the crystal, large stress can be accumulated in the crystal, so that the crystal is easy to crack seriously;
2) strontium iodide melt is easy to react with the quartz crucible to corrode the quartz crucible, the quartz crucible is easy to crack in the growth or cooling process, the crystal growth failure is caused, and I is caused in severe cases2The pollution of harmful substances such as steam and the like is harmful to human health;
3) strontium iodide crystals can only grow in a closed manner in a quartz crucible, cannot grow in a seed crystal seeding manner, cannot grow in a Reaction Atmosphere (RAP) technology, and cannot seriously affect the quality and performance of the crystals due to residual extremely-small amount of water and oxygen in the quartz crucible when the quartz crucible is vacuumized;
4) the growth period is longer, which is suitable for growing large-size crystals, but is not suitable for rapidly preparing the crystals.
Disclosure of Invention
Based on the defects, the invention aims to provide the non-doped Eu with high growth speed, high success rate of crystal growth, excellent quality of the prepared single crystal and greatly reduced production cost of the crystal2+Doped strontium iodide (SrI)2) A device and a method for directional zone-melting growth of crystals.
The purpose of the invention is realized as follows: the invention provides a non-doped Eu2+A directional zone-melting growth apparatus for doped strontium iodide crystals, comprising: the device comprises a lifting support, a roller lead screw platform supported by the lifting support, a moving temperature field controlled by a stepping motor and moving relative to the roller lead screw platform, a quartz glass furnace tube fixed on the roller lead screw platform through a fixed support and transversely penetrating the moving temperature field, and a growth container arranged in the quartz glass furnace tube.
The directional zone melting growth device provided by the invention adopts the transparent quartz tube as the protection cavity, can adopt the seed crystal to directionally grow the crystal, is beneficial to the dynamic and real-time observation of the crystal growth process, and has the advantages of high purity, small stress and high integrity of the grown crystal and remarkable technical advantages.
Preferably, the two ends of the quartz glass furnace tube are sealed by stainless steel flanges, and can be connected with a vacuum pump or filled with inert protective gas.
Preferably, the lifting support is provided with a plurality of lifting supports, and the growth container is horizontal or inclined at a certain angle by adjusting the height of each lifting support.
Preferably, the moving temperature field comprises: a furnace body heat-insulating layer; a heating element embedded in the furnace body heat-insulating layer; the light heat-insulating material is detachably arranged on the inner side of the furnace body heat-insulating layer; and the thermocouple is used for measuring the temperature in the moving temperature field and feeding the temperature back to the temperature control system.
Preferably, the furnace body heat-insulating layer is made of high-purity alumina light-weight polymer materials, and the heating body is a resistance wire heating body.
In another aspect of the present invention, there is provided a non-doped and Eu2+The directional zone melting growth method of the doped strontium iodide crystal comprises the following steps:
(1) fully mixing anhydrous strontium iodide and europium iodide raw materials, placing the mixture into a zone melting crucible, and placing the zone melting crucible into a quartz glass furnace tube of the directional zone melting growth device;
(2) vacuumizing the quartz glass furnace tube, or introducing inert or iodine-containing protective gas;
(3) starting a mobile temperature field;
(4) setting a control program of a stepping motor, moving the moving thermal field from one end of the quartz glass furnace tube to the other end, and then rapidly returning to the initial position to form the polycrystalline ingot.
(5) Loading the formed polycrystalline ingot into a growth container such as a growth crucible or a growth boat of a target shape, and repeating the above steps (1) to (3);
(6) setting a stepping motor control program to enable the moving temperature field to move from one end of the quartz glass furnace tube to the other end;
(7) after the crystal growth is finished, enabling the grown crystal to be in a light heat-insulating material area, and annealing in situ;
(8) and setting a cooling program to cool the crystal to room temperature so as to obtain complete crystals with the same shape as the growth container.
After the processing in the steps (1) to (4), the raw material becomes a polycrystalline ingot with transparent crystal grains with a certain size, so that the volume of the raw material can be effectively reduced and harmful impurities can be eliminated.
The method is favorable for realizing the dynamic or real-time observation of the crystal growth, and can adopt a seed crystal inoculation process to obtain the crystal in a specific direction, meanwhile, the top of the grown crystal is in an unrestricted state, so that space is reserved for the expansion of the crystal, the method is favorable for timely releasing the internal stress of the crystal and reducing the cracking of the crystal, the method has high growth speed, the success rate of the crystal growth is high, and the prepared single crystal has excellent quality, thereby greatly reducing the production cost of the crystal.
Drawings
FIG. 1 is a non-doped and Eu according to an embodiment of the present invention2+The structure schematic diagram of the doped strontium iodide crystal directional zone-melting growth device;
FIG. 2 shows undoped Eu according to an embodiment of the present invention2+The internal structure schematic diagram of a mobile temperature field in the doped strontium iodide crystal directional zone melting growth device;
1-1. step motor
1-2 roller screw rod platform
1-3. sliding block platform
1-4. liftable support
1-5 stainless steel flange
1-6. fixed support
1-7 quartz glass furnace tube
1-8 moving temperature field
2-1. thermocouple
2-2. high purity alumina light polymer material
2-3 resistance wire heating body
2-4. light thermal insulation material
2-5. light thermal insulation material
2-6 quartz glass furnace tube
2-7. crystal
2-8. melting
2-9. polycrystalline material.
Detailed Description
An embodiment of the present invention will be described in detail below with reference to the accompanying drawings.
Because the melting point of the strontium iodide crystal is lower, a transparent quartz tube can be used as a protective cavity body during directional zone-melting crystallization, thereby being beneficial to the dynamic or real-time observation of the crystal growth process; the crystal growth can be carried out in an inert or reactive atmosphere, or in vacuum; the crystal growth container can adopt a quartz crucible or a metal or graphite crucible, and because the upper part of the crucible which is horizontally placed is in an open state, the top of the grown crystal is in an unrestricted state, space is reserved for the expansion of the crystal, and the internal stress of the crystal can be released in time; during directional zone melting growth, seed crystals can be placed on one side of the crucible, and the seed crystals are used for inoculating and growing crystals, so that the success rate of crystal growth is improved, and the crystals in a specific direction can be obtained.
Based on the advantages, the invention provides non-doped Eu2+The whole structure of the doped strontium iodide crystal directional zone-melting growth device is shown in figure 1.
The device comprises a lifting support 1-4 and a roller lead screw platform 1-2 which is supported by the lifting support 1-4 and controlled by a stepping motor 1-1, wherein the rotation of the roller lead screw can drive a sliding block platform 1-3 to move back and forth, a moving temperature field 1-8 is fixed on the sliding block platform 1-3, and the moving speed is controlled by the stepping motor. Two ends of the quartz glass furnace tube 1-7 are fixed through fixing supports 1-6 fixed at two ends of the roller lead screw platform 1-2 and cross across the middle of the moving temperature field 1-8 to be used as a hearth. The growth container is arranged inside the quartz glass furnace tube 1-7.
The lifting support 1-4 is provided with a plurality of supports, for example, three supports are shown in figure 1, and the height of each support 1-4 can be adjusted to enable the growth platform to be horizontal or inclined at a certain angle.
Two ends of the quartz glass furnace tube 1-7 are sealed by stainless steel flanges 1-5, and can be connected with a vacuum pump or filled with inert protective gas.
The internal structure of the mobile thermal field 1-8 is shown in figure 2, high-purity alumina light material 2-2 is used as a furnace body heat-insulating layer, and resistance wire heating bodies 2-3 are embedded. The light heat-insulating materials 2-4 and 2-5 are detachably arranged on the inner side of the heat-insulating layer of the furnace body. The temperature is measured by the thermocouple 2-1 and fed back to the temperature control system.
The widths of the melting zone and the crystallization zone can be adjusted by changing the thickness and length of the light heat-insulating materials 2-4 and 2-5, and a temperature field and a temperature gradient suitable for crystal growth are formed.
As also shown in FIG. 2, the growth crucible containing the polycrystalline material 2-9 is placed in a quartz glass furnace tube 2-6, the proper temperature is adjusted, and the crystal growth process of converting the polycrystalline material 2-9 into the melt 2-8 and further forming the crystal 2-7 can be realized by moving the temperature field 1-8 and the growth crucible relatively.
The invention also provides non-doped Eu2+Oriented zone-melting growth method of doped strontium iodide crystal to realize high-quality non-doping and Eu2+Controllable preparation of doped strontium iodide crystal. The crystal growth process includes the following steps.
1) The anhydrous strontium iodide and europium iodide are mixed and set inside the zone melting crucible, and the zone melting crucible is set inside the quartz tube hearth of the directional zone melting growth apparatus, and the hearth may be horizontal or inclined in certain angle.
2) Starting a vacuum pump to vacuumize the quartz tube hearth, and generally keeping the vacuum degree at 1 multiplied by 10-2Pa or so, or introducing inert or iodine-containing protective gas.
3) And starting a moving temperature field serving as a heating device, so that the temperature of a melting zone is higher than the melting point by 100-200 ℃, the temperature of a preheating zone and a crystallization zone is lower than the melting point by 50-100 ℃, and the width of the melting zone is 20-100 mm.
4) And setting a control program of a stepping motor to enable the moving temperature field to move from one end of the quartz tube hearth to the other end, and then quickly returning to the initial position. Wherein the moving temperature field preferably moves at a speed of 10 to 20 mm/hr. By setting the displacement program, the process can be repeated a plurality of times.
After the steps are carried out, the raw material becomes a polycrystalline ingot with transparent crystal grains with certain size, so that the volume of the raw material can be effectively reduced and harmful impurities can be eliminated.
5) Loading a certain mass of polycrystalline ingot into a growth crucible or a growth boat with a target shape, and repeating the steps 1) to 3).
6) And setting a control program of a stepping motor to enable the moving temperature field to move from one end of the quartz hearth to the other end. Wherein the moving speed is preferably 0.1-5 mm/h, more preferably 0.1-2 mm/h.
7) After the crystal growth is finished, enabling the grown crystal to be positioned in a light heat-insulating material area, and annealing the crystal in situ at the temperature of 400-500 ℃ so as to eliminate the internal thermal stress of the crystal as much as possible;
8) and setting a temperature reduction procedure to reduce the temperature of the crystal to room temperature, so as to obtain a complete crystal with the same shape as the growth crucible or the growth boat, wherein the temperature reduction rate is preferably 5-20 ℃/hour.
The directional zone melting growth device provided by the invention adopts the transparent quartz tube as the protection cavity, can adopt the seed crystal to directionally grow the crystal, is beneficial to the dynamic and real-time observation of the crystal growth process, and the grown crystal has high purity, small stress and high integrity and has remarkable technical advantages.
The technical solution of the present invention is further illustrated by the following examples.
Example 1
Undoped SrI2The preparation process of the single crystal directional zone melting crystallization comprises the following steps:
a quartz boat with the height of 90mm, the length of 300mm, the thickness of 2.5mm and the bottom with a 90-degree cone angle is placed in a transparent quartz hearth with the inner diameter of 120mm, the length of 1500mm and the thickness of 3 mm.
1kg of SrI with the purity of more than or equal to 99.99 percent2Adding the powder into a quartz boat, starting a vacuum pump to vacuumize a quartz hearth to 1 × 10-2Pa。
And (3) taking down the light heat-insulating material in the mobile thermal field, enabling the whole quartz boat to be in a heating area, starting a heating system, heating to 200 ℃, and preserving heat for 4 hours to fully remove the adsorbed water in the raw materials.
And (3) closing the heating system, placing a light heat-insulating material in the movable thermal field heating device, adjusting the width of the melting zone to be 30mm, and enabling the melting zone to be positioned at the cone angle at the bottom of the quartz boat.
And starting a heating system, raising the temperature to 600 ℃ in the melting zone, fully melting the raw materials at the cone angle of the quartz boat, and keeping the temperature of the crystallization zone at 450 ℃.
Setting a stepping motor control program to move the melting zone from the cone angle of the quartz boat to the other end at the speed of 10mm/h, then returning to the initial position at the speed of 600mm/h, stopping for 30min, then starting to move at the speed of 10mm/h again, and repeating the process for 10 times.
Setting a control program of a stepping motor to enable a melting zone to move from a cone angle of the quartz boat to the other end at the speed of 2mm/h, enabling crystals in the quartz boat to enter a light heat-insulating material area, and setting the program to cool down to carry out in-situ annealing on the crystals, thus obtaining complete crystals with the same shape as the quartz boat.
Example 2
Eu2+Doping with SrI2The preparation process of the crystal oriented zone-melting crystallization comprises the following steps:
800g of SrI with the purity of more than or equal to 99.99 percent2Powder and 20g of EuI with purity more than or equal to 99.99%2After being uniformly mixed, the mixture is added into a platinum crucible, the diameter of the platinum crucible is 30mm multiplied by the length of the platinum crucible is 300mm, the thickness of the platinum crucible is 0.3mm, and the bottom of the platinum crucible is provided with a capillary structure; then placing the platinum crucible in a transparent quartz hearth with the inner diameter of 40mm multiplied by the length of 1500mm and the thickness of 3 mm; a layer of ceramic fiber blanket with the thickness of 2mm is arranged on the contact surface of the platinum crucible and the quartz tube to prevent the quartz tube from being locally overheated and prevent the platinum crucible from moving.
The liftable support is adjusted to enable the quartz hearth to incline by 30 degrees, and at the moment, the top end of the platinum crucible and the capillary end incline by 30 degrees, so that the whole crucible can be filled with melt.
And taking down the light heat-insulating material in the movable thermal field to enable the whole platinum crucible to be in a heating area. Starting a vacuum pump to vacuumize the quartz hearth to 1 x 10-2And Pa, starting a heating system, heating to 200 ℃, preserving heat for 4 hours, and fully removing the adsorbed water in the raw materials.
And (4) closing the heating system, and filling high-purity Ar gas into the hearth to keep the micro-positive pressure in the hearth. Then adding a light heat-insulating material in the moving temperature field, and adjusting the width of the melting zone to 30 mm.
Starting a heating system, raising the temperature to 600 ℃ in a melting zone, fully melting the raw materials in the platinum crucible, and keeping the temperature of a crystallization zone at 450 ℃.
Setting a control program of a stepping motor, moving the melting zone from the capillary structure of the platinum crucible to the other end at the speed of 10mm/h, then returning to the initial position at the speed of 600mm/h, stopping for 30min, then starting to move at the speed of 10mm/h again, and repeating the process for 15 times.
Setting a control program of a stepping motor to enable a melting zone to move from a capillary structure of a platinum crucible to the other end at a speed of 1mm/h, enabling crystals in the crucible to enter a light heat-insulating material area, setting the program to cool and carry out in-situ annealing on the crystals, and obtaining SrI2Eu crystal.
The practice of the invention is not limited to the examples described above. Many modifications and other embodiments of the invention will come to the mind of one skilled in the art having the benefit of the teachings presented in the foregoing descriptions. Accordingly, the foregoing description is by way of example only and is provided for the purpose of teaching those skilled in the art the best mode of carrying out the invention. Other structures and/or functions may be substantially modified without departing from the spirit of the present invention.
For example, the quartz boat in example 1 can be a graphite boat or a metal boat, and it is only necessary to ensure that the material does not react with strontium iodide or Eu at high temperature2+Doping strontium iodide melt to perform chemical reaction.
Or, the capillary part at the bottom of the platinum crucible in the embodiment 2 is changed into the placement of the directional seed crystal, namely, the seed crystal can be used for inoculation and growth; the size of the crucible is determined according to the size of the crystal to be grown, and the size of the vitreous silica hearth can be changed according to the size of the crucible.
Claims (4)
1. Non-doped or Eu2+A directional zone-melting growth apparatus for doped strontium iodide crystals, comprising:
a plurality of lifting brackets (1-4),
a roller screw rod platform (1-2) supported by the lifting bracket,
a moving temperature field (1-8) controlled by a stepping motor (1-1) to move relative to the roller screw platform (1-2),
a quartz glass furnace tube (1-7) which is fixed on the roller screw platform through a fixed support (1-6) and traverses the mobile thermal field (1-8), wherein two ends of the quartz glass furnace tube (1-7) are sealed by stainless steel flanges,
the growth container is arranged in the quartz glass furnace tube (1-7), and the growth container is horizontal or inclined by adjusting the height of each lifting support (1-4);
the mobile thermal field (1-8) comprises: a furnace body heat-insulating layer; a heating element embedded in the furnace body heat-insulating layer; the light heat-insulating material is detachably arranged on the inner side of the furnace body heat-insulating layer; and a thermocouple (2-1) for measuring the temperature in the moving temperature field and feeding the temperature back to the temperature control system.
2. Undoped or Eu according to claim 12+A directional zone melting growth device of doped strontium iodide crystal is characterized in that,
two ends of the quartz glass furnace tube (1-7) are sealed by stainless steel flanges and can be connected with a vacuum pump or inert protective gas is introduced.
3. Undoped or Eu according to claim 12+A directional zone melting growth device of doped strontium iodide crystal is characterized in that,
the furnace body heat-insulating layer is made of high-purity alumina light-gathering materials, and the heating body is a resistance wire heating body (2-3).
4. Non-doped or Eu2+The oriented zone melting growth method of the doped strontium iodide crystal is characterized by comprising the following steps of:
(1) placing an anhydrous strontium iodide raw material or an anhydrous strontium iodide and europium iodide raw material into a zone-melting crucible after fully mixing, and placing the zone-melting crucible into a quartz glass furnace tube of the directional zone-melting growth device according to claim 1;
(2) vacuumizing the quartz glass furnace tube, or introducing inert or iodine-containing protective gas;
(3) starting a mobile temperature field;
(4) setting a control program of a stepping motor, moving the moving temperature field from one end of the quartz glass furnace tube to the other end, and then quickly returning to the initial position to form a polycrystalline ingot;
(5) loading the formed polycrystalline ingot into a growth container with a target shape, and repeating the steps (1) to (3);
(6) setting a stepping motor control program to enable the moving temperature field to move from one end of the quartz glass furnace tube to the other end;
(7) after the crystal growth is finished, enabling the grown crystal to be in a light heat-insulating material area, and annealing in situ;
(8) and setting a cooling program to cool the crystal to room temperature so as to obtain complete crystals with the same shape as the growth container.
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