WO2007064247A2 - Procede de croissance de cd1-xznxte, ou 0$m(f)x$m(f)1 - Google Patents

Procede de croissance de cd1-xznxte, ou 0$m(f)x$m(f)1 Download PDF

Info

Publication number
WO2007064247A2
WO2007064247A2 PCT/RU2006/000626 RU2006000626W WO2007064247A2 WO 2007064247 A2 WO2007064247 A2 WO 2007064247A2 RU 2006000626 W RU2006000626 W RU 2006000626W WO 2007064247 A2 WO2007064247 A2 WO 2007064247A2
Authority
WO
WIPO (PCT)
Prior art keywords
melt
crystal
growing
order
composition
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/RU2006/000626
Other languages
English (en)
Russian (ru)
Other versions
WO2007064247A3 (fr
Inventor
Vladimir Dmitrievich Golyshev
Michael Alexandrovich Gonik
Svetlana Viktorovna Bykova
Vladimir Borisovich Tsvetovsky
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Spp 'thermo A' Ltd
Original Assignee
Spp 'thermo A' Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Spp 'thermo A' Ltd filed Critical Spp 'thermo A' Ltd
Publication of WO2007064247A2 publication Critical patent/WO2007064247A2/fr
Publication of WO2007064247A3 publication Critical patent/WO2007064247A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/16—Heating of the molten zone
    • C30B13/18—Heating of the molten zone the heating element being in contact with, or immersed in, the molten zone

Definitions

  • the invention relates to the field of growing single crystals of Cd 1-x Zn x Te, where O ⁇ x ⁇ l, (CZT) from a melt under high pressure inert gas.
  • CZT Cd 1-x Zn x Te, where O ⁇ x ⁇ l, (CZT) from a melt under high pressure inert gas.
  • One of the most common methods for producing CZT crystals is the method of vertically directed crystallization (Bridgman method) under high inert gas pressure Ar 2-10 MPa [V. K. Komar, A. S Gerasimenko, D.P. Nalivaiko, “Cdi -x Zn x Te crystals for semiconductor X-ray and ⁇ -radiation detectors” // “Functional materials for science and texics”, Institute of Single Crystals, 2001, p.167 - 198; NN Kolespikov, A.A.
  • Analogue 2 was chosen as a prototype, since during the crystallization by the CDW method, a stationary state is faster than the Bridgman method due to the fact that the relatively small molten zone is fed by ⁇ remelted material of the original ingot. As a result, the effective distribution coefficient quickly becomes equal to 1.
  • the purpose of the invention is the development of a method for growing macro and micro-uniform low-dislocation crystals Cdi_ x Zn x Te, where O ⁇ x ⁇ l with a diameter of up to 100-150 mm.
  • the objective of the invention is to eliminate the disadvantages inherent in other methods of growing and due to the physical nature of the system.
  • the main problems during crystallization of these systems include: 1) the preferential volatilization of one of the components at high partial pressures, which leads to non-stoichiometry and, as a consequence, to constitutional hypothermia, to morphological instability of the interphase surface and to microinhomogeneity, to the appearance of precipitates and intrinsic defects , 2) the dependence of the crystallization temperature on the composition, which leads to the dependence of the shape of the interphase surface on the composition of the melt, to constitutional supercooling at n the accumulation of one of the components near the crystallization front due to segregation, 3) a high tendency to the appearance of twins and blocks, 4) the low thermal conductivity of the melt at a relatively high heat of crystallization and high thermal conductivity of the crucible walls leads to a crystallization front concave in the melt, which leads, in addition, to the transverse heterogeneity, 5) the inequality of the distribution coefficient (segregation) of the unit leads to unevenness of the longitudinal distribution of the composition and the dop
  • the volatility of the components leads to an uncertainty in the composition, and due to the influence of the composition on the crystallization temperature, there is an uncertainty in the temperature of the onset of crystallization and difficulty in seeding. Due to the uncertainty of melt supercooling during spontaneous seeding, an additional reason arises for the uncertainty of the moment of crystallization onset. Moreover, the higher the temperature of the superheat of the melt, the greater the volatility of the components. All these problems increase sharply with increasing diameter of the growing crystal, since in traditional methods it is necessary to overheat the melt to melt the system on the axis of the crucible. Due to the concavity of the crystallization front and the tendency to form blocks, many blocks and twins are formed in the ingot.
  • the composition in the longitudinal and transverse directions by immersing a special heater (OTP heater) in the melt, which divides the melt into two zones Wi and W 2 (see Fig.), While the lower zone is the growth zone, and the upper the zone acts as a feeder.
  • OTP heater special heater
  • the OTP heater is located near the interphase surface, which makes it possible to obtain low-dislocation crystals due to the creation of small temperature gradients in the radial direction and to obtain small thermoelastic stresses, provides control of the melt overheating over the entire melt volume, and also the possibility of increasing the micro-uniformity of the crystals due to the creation of weak laminar flows near the interfacial surface due to the small thickness of the melt layer near the interfacial surface and suppression of thermal convection.
  • the figure shows the installation diagram for the implementation of the described method.
  • the crucible 1 is located inside the growth chamber with a multi-section background heater (FN) 2.
  • An additional multi-section heater 3 (OTF heater) is placed inside the crucible in a sealed casing 4.
  • the OTF heater is immersed in the melt a small distance from the interface.
  • a probe 5 (TMZ) is placed along the axis of the OTF of the heater, inside which there is a temperature sensor T *. This probe is installed with the ability to move and measure the magnitude of the movement during crystallization.
  • the system of temperature sensors 6 (Tl, T2), 7 (T9, TlO) is located inside the OTF of the heater, in the bottom of the crucible 8 (TK, T4) and on the side wall of the crucible 9 (T5 - T8).
  • a charge is loaded into the conical part of the crucible, then an OTF heater is installed on it and the charge is poured on top.
  • Zones Wi and Wg are interconnected by a narrow gap ⁇ between the crucible wall and the OTF heater. The gap thickness is determined from the condition that there is no back diffusion from the Wi zone to the Wg zone> In the Wi and W 2 zones, a different initial composition is established.
  • the melt composition in the Wl zone corresponds to the liquidus composition of the grown crystal (e.g., for a crystal of the composition Cdo.sZno. 2 Te the liquidus composition Cdo. 8 sZno.isTe), the melt composition in the W2 zone corresponds to the solidus composition (Cdo.sZno.2Te).
  • the crucible is mounted on a heat sink stand 10. OTF heater is fixed motionless relative to the heater heater.
  • the proposed method is implemented as follows.
  • the vacuum is pumped out, the furnace is turned on, and at a temperature of 220-270 ° C, the chamber is filled with inert gas with the expectation that at the working temperature the gas pressure will be 80-120 atm.
  • the temperature is increased until the mixture is melted.
  • a temperature regime is established in which a melt overheat of 20-100 degrees is created in the lower zone, and an inverse temperature gradient is established in the upper zone (temperature control is carried out using temperature sensors T). In this state, the system is kept for 0.5 - 1.5 hours to stabilize the mode.
  • TMZ is used in the crystallization process. TMZ is lowered down to the moment of touching the interface.
  • the distance that TMZ passes is the height of the melt layer.
  • the temperature boundary conditions that are used to control crystallization are corrected.
  • the bottom of the OTF heater is isothermal. This leads to the fact that a one-dimensional temperature field (axial heat flux) is formed under the OTF heater.
  • the quantity h ⁇ 0.13D (crucible diameter) is always such that the temperature field on the system axis is described by one-dimensional heat transfer equations. This makes it possible to introduce computer control of the front position and crystallization rate according to the thermal model. Crystallization is controlled according to the thermal model using a high-precision computer control system (accuracy of maintaining the temperature below 0.1K).
  • the following values are kept constant: h, gradT, Ti, and growth rate.
  • the shape of the front is controlled by the radial distribution of power over the OTF heater, and near the walls of the crucible is carried out due to the redistribution of power between the FN and OTF temperature heaters
  • the temperature regime of OTF crystallization and crystallization conditions are determined by the required quality (properties) of the crystal, which in turn is determined by the purpose of the material: for optics, for substrates, or as a detector material.
  • the system is cooled according to a predetermined program.
  • the crystal is annealed at a temperature of 750-900 C.
  • Cd 1-x Zn x Te single crystals were grown, where 0 ⁇ x ⁇ 0.3, diameter 45 - 50 mm and height 70 mm, characterized by a high degree of macro and micro-uniformity. At 85-90% of the crystal length, deviations from the given composition in the volume were 0.5 at%. The average density of etching pits was

Landscapes

  • 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)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)

Abstract

L'invention concerne la croissance de monocristaux de Cd1-xZnxTe (CZT), où 0≤x≤1, à partir de masses fondues et sous pression élevée d'un gaz inerte. La croissance de cristaux s'effectue dans des conditions d'un flux thermique axial proche du front de cristallisation (procédé OTF). Le procédé OTF appliqué aux CZT présente les avantages suivants: 1) régulation de la composition en direction longitudinale par la création d'une zone d'alimentation grâce à la division des masses fondues en deux zones par une réchauffeur immergé dans les masses fondues (réchauffeur OTF); 2) régulation de la composition en direction transversale grâce à la commande, au moyen du réchauffeur OTF, de la forme de front de cristallisation; 3) commande de l'intensité de surchauffe des masses fondues grâce aux capteurs optiques montés dans le réchauffeur OTF; et 4) possibilité d'obtenir des cristaux à faible dislocation par la création de faibles courants laminaires près de la surface interfaciale. Les cristaux CZT ainsi cultivés sont caractérisés par un degré élevé de micro- et de macro-homogénéité (les déviations par rapport aux valeurs prédéterminées de la composition pour un volume donné sont < 05 at %, la densité moyenne des cavités d'attaque chimique est de 5*103*cm-2 sans recuit).
PCT/RU2006/000626 2005-12-01 2006-11-24 Procede de croissance de cd1-xznxte, ou 0$m(f)x$m(f)1 Ceased WO2007064247A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2005137297 2005-12-01
RU2005137297/15A RU2330126C2 (ru) 2005-12-01 2005-12-01 СПОСОБ ВЫРАЩИВАНИЯ Cd1-xZnxTe, где 0≤x≤1

Publications (2)

Publication Number Publication Date
WO2007064247A2 true WO2007064247A2 (fr) 2007-06-07
WO2007064247A3 WO2007064247A3 (fr) 2007-08-16

Family

ID=38092669

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/RU2006/000626 Ceased WO2007064247A2 (fr) 2005-12-01 2006-11-24 Procede de croissance de cd1-xznxte, ou 0$m(f)x$m(f)1

Country Status (2)

Country Link
RU (1) RU2330126C2 (fr)
WO (1) WO2007064247A2 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102220644A (zh) * 2011-06-08 2011-10-19 上海大学 一种提高碲锌镉晶体性能的方法
CN102230213A (zh) * 2011-06-08 2011-11-02 上海大学 碲溶剂溶液法生长碲锌镉晶体的方法
CN103911665A (zh) * 2013-01-08 2014-07-09 广东先导稀材股份有限公司 采用镀碳石英坩埚制备碲锌镉晶体过程中的除杂方法

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2434976C2 (ru) * 2009-10-07 2011-11-27 Владимир Дмитриевич Голышев СПОСОБ ВЫРАЩИВАНИЯ МЕТОДОМ ОТФ Cd1-XZnXTe, ГДЕ 0≤x≤1, ДИАМЕТРОМ ДО 150 мм
RU2633899C2 (ru) * 2015-12-21 2017-10-19 Общество с ограниченной ответственностью "КристалсНорд" Способ выращивания монокристаллов Cd1-xZnxTe, где 0≤x≤1, на затравку при высоком давлении инертного газа
CN110106555B (zh) * 2019-06-05 2020-12-04 湖南大合新材料有限公司 一种碲锌镉单晶炉及碲锌镉单晶的生长工艺

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59217700A (ja) * 1983-05-20 1984-12-07 Sumitomo Electric Ind Ltd 化合物半導体製造用部材およびその製造法
JPS60191094A (ja) * 1984-03-08 1985-09-28 Hitachi Cable Ltd Ｂνルツボの前処理方法
SU1800854A1 (ru) * 1990-02-15 1996-06-20 Всесоюзный научно-исследовательский институт синтеза минерального сырья Устройство для выращивания кристаллов

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102220644A (zh) * 2011-06-08 2011-10-19 上海大学 一种提高碲锌镉晶体性能的方法
CN102230213A (zh) * 2011-06-08 2011-11-02 上海大学 碲溶剂溶液法生长碲锌镉晶体的方法
CN102230213B (zh) * 2011-06-08 2012-08-29 上海大学 碲溶剂溶液法生长碲锌镉晶体的方法
CN102220644B (zh) * 2011-06-08 2013-04-03 上海大学 一种提高碲锌镉晶体性能的方法
CN103911665A (zh) * 2013-01-08 2014-07-09 广东先导稀材股份有限公司 采用镀碳石英坩埚制备碲锌镉晶体过程中的除杂方法

Also Published As

Publication number Publication date
RU2330126C2 (ru) 2008-07-27
WO2007064247A3 (fr) 2007-08-16
RU2005137297A (ru) 2007-06-10

Similar Documents

Publication Publication Date Title
Chu et al. Physics and properties of narrow gap semiconductors
JP5497053B2 (ja) 単結晶ゲルマニウムの結晶成長システム、方法および基板
US10443149B2 (en) Method of producing crystal
EP0261498A2 (fr) Appareillage pour le tirage de cristaux
JP3232461B2 (ja) 単結晶の成長方法
WO2008050524A1 (fr) Dispositif de production d&#39;un cristal unique et procédé de production d&#39;un cristal unique
TW201109483A (en) Systems, methods and substrates of monocrystalline germanium crystal growth
RU2434976C2 (ru) СПОСОБ ВЫРАЩИВАНИЯ МЕТОДОМ ОТФ Cd1-XZnXTe, ГДЕ 0≤x≤1, ДИАМЕТРОМ ДО 150 мм
RU2330126C2 (ru) СПОСОБ ВЫРАЩИВАНИЯ Cd1-xZnxTe, где 0≤x≤1
JP5370394B2 (ja) 化合物半導体単結晶基板
JP4830312B2 (ja) 化合物半導体単結晶とその製造方法
EP1774068B1 (fr) Procédé de formation de monocristaux par fusion
US9109299B1 (en) Solidification of high quality alloy semiconductors
RU2633899C2 (ru) Способ выращивания монокристаллов Cd1-xZnxTe, где 0≤x≤1, на затравку при высоком давлении инертного газа
RU2381305C1 (ru) СПОСОБ ВЫРАЩИВАНИЯ МОНОКРИСТАЛЛОВ ГЕРМАНИЯ ДИАМЕТРОМ ДО 150 мм МЕТОДОМ ОТФ
JP2022020187A (ja) ＦｅＧａ合金単結晶の製造方法
JP2704032B2 (ja) 化合物半導体単結晶の製造方法
RU2320791C1 (ru) Способ выращивания кристаллов и устройство для его осуществления
RU2261297C1 (ru) Способ выращивания монокристаллов из расплава методом амосова
RU2330127C2 (ru) Способ выращивания монокристаллов германия методом отф
US5476064A (en) Pull method for growth of single crystal using density detector and apparatus therefor
RU2338815C2 (ru) Способ выращивания монокристаллов-сцинтилляторов на основе иодида натрия или цезия и устройство для его реализации
JP2717685B2 (ja) チョクラルスキー法による結晶育成の方法及び装置
RU2199614C1 (ru) Способ выращивания кристаллов
JPH04144990A (ja) 結晶成長方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application
NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 06843980

Country of ref document: EP

Kind code of ref document: A2