KR910010169B1 - Single crystal manufacturing method of oxide titanium - Google Patents

Single crystal manufacturing method of oxide titanium Download PDF

Info

Publication number
KR910010169B1
KR910010169B1 KR1019880010653A KR880010653A KR910010169B1 KR 910010169 B1 KR910010169 B1 KR 910010169B1 KR 1019880010653 A KR1019880010653 A KR 1019880010653A KR 880010653 A KR880010653 A KR 880010653A KR 910010169 B1 KR910010169 B1 KR 910010169B1
Authority
KR
South Korea
Prior art keywords
single crystal
titanium oxide
crystal manufacturing
oxide titanium
hours
Prior art date
Application number
KR1019880010653A
Other languages
Korean (ko)
Other versions
KR900004052A (en
Inventor
김문영
장영남
Original Assignee
한국동력자원연구소
김지동
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 한국동력자원연구소, 김지동 filed Critical 한국동력자원연구소
Priority to KR1019880010653A priority Critical patent/KR910010169B1/en
Publication of KR900004052A publication Critical patent/KR900004052A/en
Application granted granted Critical
Publication of KR910010169B1 publication Critical patent/KR910010169B1/en

Links

Images

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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/14—Heating of the melt or the crystallised materials
    • 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
    • C30B29/02—Elements

Landscapes

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

Abstract

A titanium oxide single crystal is prepared by mixing titanium oxide powder having at least 99.9 % purity and 1-5 μm particle size for 2-3 hours, drying it at 50-80 deg.C, packing it into a rubber tube, moulding by the hydrostatic pressure to get a rod shape body, making 1-2 mm hole, sintering at 1200-1600 deg.C to get a rutile polycrystal, growing under the oxygen atmosphere by the floating zone method. The crystal is used for the manufacture of a semiconductor, a prism and a precious stone.

Description

산화티타늄 단결정 육성법Titanium oxide single crystal growth method

제1도는 산화티타늄 단결정 육성의 공정도.1 is a flow chart of titanium oxide single crystal growth.

본 발명은 반도체, 프리즘 및 보석용으로 활용할 수 있는 산화티타늄(TiO2) 단결정 육성법에 관한 것이다.The present invention relates to a titanium oxide (TiO 2 ) single crystal growth method that can be used for semiconductors, prisms and jewelry.

본 발명에 의한 단결정 육성법은 시간당 8㎜, ø10㎜정도 육성이 가능하나 앞으로 10-12㎜, ø115㎜의 단결정 육성도 가능할 것이며 또한 CZOCHRALSKI법에 의한 대형 단결정 육성도 적용될 것이다.The single crystal growing method according to the present invention is capable of growing about 8 mm and ø10 mm per hour, but it is also possible to grow single crystals of 10-12 mm and ø115 mm in the future, and also to grow large single crystals by the CZOCHRALSKI method.

이하 발명의 요지를 실시예적 공정을 첨부 도면에 연계시켜 상세히 설명하면 다음과 같다.DETAILED DESCRIPTION Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.

[제1공정][Step 1]

산화티타늄(1-5㎛) 고순도분말(99.9% 이상)을 계량부(1)에서 ±0.001g의 마이크로 밸런스로서 계량하고 믹싱부(2)에서 물리적 또는 화학적 방법으로 2-3시간 믹싱하면서 50-80℃로 건조시킨 다음, 패킹부(3)에서 100-120㎜ 고무관(RUBBER TUBE)에 다져넣고 프레싱부(4)에서 정수압 800-120㎏/㎠의 압력을 가해 막대기 모양으로 성형시킨 후 상단 또는 하단에 1-2㎜의 구멍을 뚫어 놓는다.Titanium oxide (1-5 μm) high purity powder (99.9% or more) was weighed as a microbalance of ± 0.001 g in the metering section 1 and mixed for 2 to 3 hours by physical or chemical method in the mixing section 2 After drying at 80 ° C, the packing part 3 was compacted in a 100-120 mm rubber tube, and the pressing part 4 was pressurized with a hydrostatic pressure of 800-120 kg / cm 2 to form a stick shape. Drill a hole of 1-2 mm at the bottom.

[제2공정][Step 2]

제1공정에서 성형된 막대기모양의 시료를 1200-1600℃의 초고온도인 신터링부(SINTERING)(5)에서 80-100분가량 1.3㎝/min의 속도로 이동시키면서 소성시키면 육성에 필요한 루타일(RUTILE)(정방정계) 다결정체를 얻을 수 있으며 이때 70-75%정도의 부피변화가 발생한다.Rutile required for growth when the rod-shaped sample formed in the first step is fired while moving at a speed of 1.3 cm / min for 80-100 minutes in the SINTERING 5, which is an ultra-high temperature of 1200-1600 ° C. (RUTILE) (Square) Polycrystals can be obtained, with volume changes of about 70-75%.

[제3공정][Step 3]

제2공정의 다결정체를 육성부(6)에서 부유대역 용융장치를 이용하여 산소분위기하에서 프로팅존(FLOATING ZONE)법에 의하여 육성하는데 종결정은 하부 샤프트축에 일치하게 위치시키고 상부 샤프트에는 소성된 시료를 매달고 약 1시간에 걸쳐 적외선 가열장치를 작동시켜 약 1850℃(할로겐 램프용량의 약66%)까지 가열하여 소성체가 용융되면 종결정과 연결시키고 용융대가 안정화되는지 확인하며 프로그래머를 이용하여 용융대와 시료의 직경이 1:1.3으로 조정한후 육성을 시작하여 미리 세트된 속도(2-8㎜/hr로 용융대를 하강시켜 재결정시킨다. 이와 같이된 본 발명의 산화티타늄 단결정 육성법은 육성할 수 있는 규격증대와 시간의 단축 또한 결함이 최소인 단결정을 육성할 수 있으므로 반도체, 프리즘 및 보석산업에 경제성 있게 공급할 수 있는 것이다.The polycrystals of the second process are grown in the growth section 6 by using a floating zone melting apparatus under a floating zone method under the FLOATING ZONE method. The seed crystals are positioned in accordance with the lower shaft axis and fired on the upper shaft. Suspend the sample and operate the infrared heater for about 1 hour and heat it to about 1850 ° C (about 66% of the halogen lamp capacity). When the fired body melts, it is connected to the seed crystals and the melter is stabilized. After the diameter of the sample is adjusted to 1: 1.3, the growth is started and the crystallization is recrystallized by lowering the melting zone at a preset speed (2-8 mm / hr. The titanium oxide single crystal growing method of the present invention can be grown. Increasing specifications and shortening the time can also foster single crystals with minimal defects, making them economically available to the semiconductor, prism and jewelry industries.

Claims (1)

산화티타늄(1-5㎛) 고순도분말(99.9% 이상)을 계량하여 2-3시간 믹싱하고 50-80℃로 건조시킨다음 고무관에 다져넣고 정수압을 가해서 막대기모양으로 성형시킨후 1-2㎜의 구멍을 뚫는 제1공정과 이를 1200-1600℃의 온도로 소성시켜 루타일 다결정체를 얻는 제2공정과 이를 부유대역 용융장치를 이용하여 산소분위기하에서 프로팅존(FLOATING ZONE)법에 의하여 육성시키는 것을 특징으로 하는 산화티타늄 단결정 육성법.Titanium oxide (1-5㎛) high purity powder (99.9% or more) was weighed and mixed for 2-3 hours, dried at 50-80 ℃ and then squeezed into a rubber tube and molded into a stick shape by applying hydrostatic pressure to 1-2mm The first process of punching and the second process of firing it at a temperature of 1200-1600 ° C. to obtain rutile polycrystals, and the growth of these by flotation zone method under oxygen atmosphere using a floating-band melting apparatus. Titanium oxide single crystal growing method characterized by the above-mentioned.
KR1019880010653A 1988-08-22 1988-08-22 Single crystal manufacturing method of oxide titanium KR910010169B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1019880010653A KR910010169B1 (en) 1988-08-22 1988-08-22 Single crystal manufacturing method of oxide titanium

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1019880010653A KR910010169B1 (en) 1988-08-22 1988-08-22 Single crystal manufacturing method of oxide titanium

Publications (2)

Publication Number Publication Date
KR900004052A KR900004052A (en) 1990-03-27
KR910010169B1 true KR910010169B1 (en) 1991-12-17

Family

ID=19277012

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1019880010653A KR910010169B1 (en) 1988-08-22 1988-08-22 Single crystal manufacturing method of oxide titanium

Country Status (1)

Country Link
KR (1) KR910010169B1 (en)

Also Published As

Publication number Publication date
KR900004052A (en) 1990-03-27

Similar Documents

Publication Publication Date Title
US2634554A (en) Synthetic gem production
US3912521A (en) Synthetic crystal and method of making same
KR910010169B1 (en) Single crystal manufacturing method of oxide titanium
KR920008348B1 (en) Single crystallization titanic magnesium
JP2831906B2 (en) Single crystal manufacturing equipment
EP0148946B1 (en) Method of producing a chrysoberyl single crystal
JPS6052117B2 (en) Beryl single crystal manufacturing method
KR950001794B1 (en) Production of rutile single crystal
JPS6027677A (en) Production of solid solution single crystal by floating zone melting method
KR920021749A (en) Ga-Yttrium Iron Garnet (YIGaG) Single Crystal Preparation
JPH0411513B2 (en)
KR950006635B1 (en) METHOD OF PREPARATION LiTaO3 POWDER FOR GROWING SINGLE CRYSTAL
JPH0812487A (en) Manufacturing of oxide single crystal
KR100198243B1 (en) Single crystal preparation method of mn-zn ferrite using ferrite chain
JPH06279174A (en) Production of oxide single crystal
KR950007601B1 (en) Method for preparing crystallized linbo3 powder
JPS6148498A (en) Process for preparing single crystal of alkali tantalate and crucible therefor
SU1528730A1 (en) Method of producing fine crystalline quartz
JPS61178489A (en) Production of corundum
JPS5938192B2 (en) Manufacturing method of corundum single crystal that emits starry colors
JPS5841800A (en) Preparation of strontium titanate single crystal imparted with semiconductivity
JPH0471877B2 (en)
JPS62275097A (en) Macro single crystal of barium tetratitanate and its production
JPH0571551B2 (en)
Liebertz Synthetic precious stones

Legal Events

Date Code Title Description
A201 Request for examination
E902 Notification of reason for refusal
G160 Decision to publish patent application
E701 Decision to grant or registration of patent right
GRNT Written decision to grant
FPAY Annual fee payment

Payment date: 20031215

Year of fee payment: 13

LAPS Lapse due to unpaid annual fee