KR20070024884A - Method for the preparation of zinc oxide single crystal - Google Patents

Method for the preparation of zinc oxide single crystal Download PDF

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KR20070024884A
KR20070024884A KR1020050080465A KR20050080465A KR20070024884A KR 20070024884 A KR20070024884 A KR 20070024884A KR 1020050080465 A KR1020050080465 A KR 1020050080465A KR 20050080465 A KR20050080465 A KR 20050080465A KR 20070024884 A KR20070024884 A KR 20070024884A
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zinc oxide
mineralizer
single crystal
reactor
solution
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Korean (ko)
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이영국
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한국화학연구원
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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
    • 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
    • C30B29/16—Oxides
    • 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
    • C30B19/00—Liquid-phase epitaxial-layer growth
    • C30B19/10—Controlling or regulating
    • C30B19/106—Controlling or regulating adding crystallising material or reactants forming it in situ to the liquid
    • 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
    • C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
    • C30B31/04—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor by contacting with diffusion materials in the liquid state

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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

A method for fabricating a zinc oxide single crystal is provided to increase the growth rate of a zinc oxide single crystal by adding NH4Cl to a conventional solution used to be utilized as a mineralizer. Under the existence of a mixed hydrothermal solution including KOH, LiOH and NH4Cl as a mineralizer, a zinc oxide single crystal is formed by a hydrothermal method while using a zinc oxide powder sintering material and a zinc oxide seed crystal. After the zinc oxide powder sintering material is installed in the lower part of a reactor and the zinc oxide seed crystal is installed in the upper part of the reactor, a mineralizer solution is filled in the reactor. The upper part of the reactor is heated to a temperature of around 330~350 deg.C, and the lower part of the reactor is heated to a temperature of 350~370 deg.C.

Description

산화아연 단결정의 제조방법 {METHOD FOR THE PREPARATION OF ZINC OXIDE SINGLE CRYSTAL}Production method of zinc oxide single crystal {METHOD FOR THE PREPARATION OF ZINC OXIDE SINGLE CRYSTAL}

본 발명은 산화아연 단결정의 성장에 있어서 성장 속도의 이방성을 제어하여 <100> 방향으로의 성장을 증가시킬수 있는 산화아연 단결정의 제조방법에 관한 것으로, 보다 상세하게는 기존의 KOH와 LiOH으로 이루어진 혼합용액에 NH4Cl를 첨가한 용액을 광화제로서 사용함으로써 산화아연 벌크(bulk) 단결정을 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a zinc oxide single crystal that can increase the growth in the <100> direction by controlling the anisotropy of the growth rate in the growth of the zinc oxide single crystal, more specifically, a mixture consisting of conventional KOH and LiOH A method of producing a zinc oxide bulk single crystal by using a solution obtained by adding NH 4 Cl to a solution as a mineralizer.

산화아연 단결정은 태양전지의 투명 전극, 표면 탄성파 소자, 산화물 반도체 등의 분야에 사용되는 유용한 물질이다.Zinc oxide single crystal is a useful material used in fields such as transparent electrodes, surface acoustic wave devices, and oxide semiconductors of solar cells.

일반적으로 수열법에 의한 산화아연 단결정의 제조시 광화제로서 KOH와 LiOH의 혼합수용액을 사용하는데, 이 때 결정이 주로 <001> 방향으로만 성장하기 때문에 <001> 방향에 대한 <100> 방향의 성장속도의 비가 0.1 이하에 불과하여 벌크 단결정을 얻기 어렵다는 문제점이 있다.In general, a mixed aqueous solution of KOH and LiOH is used as a mineralizer in the production of a zinc oxide single crystal by hydrothermal method. In this case, since the crystal grows mainly in the <001> direction, the <100> direction relative to the <001> direction is used. There is a problem that it is difficult to obtain a bulk single crystal because the growth rate ratio is only 0.1 or less.

산화아연은 최근 청색 및 자외 영역에서의 LED (light emitting diode) 소자 제조에 널리 이용되는데 기존의 소자 제조에서는 사파이어 단결정 기판을 이용한 이종 에피탁시(hetero-epitaxy) 기술을 사용함으로써 성장된 박막의 내부에 결함이 많이 존재하여 제조된 소자의 발광 효율이 떨어지는 문제점이 있었다. Zinc oxide has recently been widely used in the manufacture of light emitting diode (LED) devices in the blue and ultraviolet regions. In conventional device fabrication, zinc oxide has been grown by using hetero-epitaxy technology using a sapphire single crystal substrate. There is a problem in that the luminous efficiency of the device manufactured due to the presence of a large number of defects.

이러한 문제점을 해결하는 방법으로 산화아연 단결정 기판을 사용한 동종 에피탁시(homo-epitaxy) 기술이 최근 개발되고 있으나 산화아연의 (001) 방향 성장 속도가 느려 대형의 단결정 기판을 구하기 어려운 문제점이 있다.A homo-epitaxy technique using a zinc oxide single crystal substrate has been recently developed as a method of solving such a problem, but there is a problem that it is difficult to obtain a large single crystal substrate due to the slow growth rate of (001) direction of zinc oxide.

이에 본 발명자들은 a 축 방향의 크기가 작은 주상형의 종자결정을 사용하면서도 결정 성장속도의 이방성을 제어함으로써 <100> 방향으로의 성장을 증가시킬 수 있는 산화아연 벌크 단결정의 제조방법을 개발하기 위해 계속 연구를 진행한 결과, 기존에 광화제로서 사용되는 KOH와 LiOH의 혼합수용액에 NH4Cl를 첨가함으로써 <100> 방향의 성장을 증가시킬 수 있음을 발견하여 본 발명을 완성하였다.Accordingly, the present inventors have developed a method for producing a zinc oxide bulk single crystal capable of increasing growth in the <100> direction by controlling anisotropy of crystal growth rate while using seed crystals having a columnar seed having a small size in the a-axis direction. As a result of further research, the present invention was found to be able to increase the growth in the <100> direction by adding NH 4 Cl to a mixed aqueous solution of KOH and LiOH, which is used as a mineralizer.

본 발명의 목적은 산화아연의 벌크(bulk) 단결정 제조시, <100> 방향의 성장을 증가시킬 수 있는 산화아연 단결정의 제조방법을 제공하는 것이다.It is an object of the present invention to provide a method for preparing zinc oxide single crystals which can increase the growth in the <100> direction when producing bulk single crystals of zinc oxide.

상기 목적을 달성하기 위해, 본 발명에서는 광화제로서 KOH, LiOH 및 NH4Cl 의 혼합 수열 용액의 존재 하에 산화아연 분말 소결체 및 산화아연 종자결정을 사용하여 수열법에 의해 산화아연 단결정을 제조하는 방법을 제공한다.In order to achieve the above object, in the present invention, a method for producing a zinc oxide single crystal by hydrothermal method using a zinc oxide powder sintered body and zinc oxide seed crystals in the presence of a mixed hydrothermal solution of KOH, LiOH and NH 4 Cl as a mineralizer. To provide.

이하 본 발명을 상세하게 설명한다.Hereinafter, the present invention will be described in detail.

본 발명에 따른 산화아연 단결정 제조방법은 광화제로 사용되던 기존의 용액에 NH4Cl을 첨가하여 산화아연 단결정의 성장 속도를 증대시킴을 특징으로 한다.The zinc oxide single crystal production method according to the present invention is characterized by increasing the growth rate of the zinc oxide single crystal by adding NH 4 Cl to the existing solution used as a mineralizer.

본 발명에 따르면, 광화제로서 KOH, LiOH 및 NH4Cl 함유 수열 용액을 사용하는데, 각 성분의 농도는 예를 들면 1 내지 4 M KOH, 0.5 내지 1.5 M LiOH 및 0.5 내지 1 M NH4Cl 로 하는 것이 적합하다. 광화제 용액은 KOH 수용액에 LiOH 및 NH4Cl을 첨가함으로써 얻을 수 있다.According to the invention, hydrothermal solutions containing KOH, LiOH and NH 4 Cl are used as mineralizers, the concentration of each component being for example 1 to 4 M KOH, 0.5 to 1.5 M LiOH and 0.5 to 1 M NH 4 Cl. It is appropriate. The mineralizer solution can be obtained by adding LiOH and NH 4 Cl to an aqueous KOH solution.

본 발명에 따른 산화아연 단결정의 제조 방법은, 구체적으로 산화아연 분말 소결체를 오토클레이브 (autoclave) 형태 반응기의 하단에 장착하고 산화아연 종자 결정은 상기 반응기의 상단에 장착한 다음, 상기 반응기에 광화제 용액을 채우고, 반응기를 밀봉한 다음, 상단부는 약 330 내지 350℃, 하단부는 350 내지 370℃로 승온하고 유지시킴으로써 수행할 수 있다. 이 때 반응기의 압력은 대략 350-400 기압으로 유지한다.In the method for producing a zinc oxide single crystal according to the present invention, specifically, the zinc oxide powder sintered body is mounted at the bottom of an autoclave type reactor, and the zinc oxide seed crystal is mounted at the top of the reactor, and then the mineralizer is added to the reactor. After filling the solution and sealing the reactor, the upper end may be performed by raising and maintaining the temperature at about 330 to 350 ° C and the lower part to 350 to 370 ° C. At this time, the pressure of the reactor is maintained at approximately 350-400 atmospheres.

이때, 상기 광화제 용액은 산화아연 분말을 약 5 내지 10 g/ℓ의 농도로 광화제 용액에 첨가한 후 예를 들면 60 내지 70 ℃로 가열함으로써 산화아연이 포화된 용액 형태로 사용하는 것이 반응기 벽면 위의 자발 핵생성에 의한 결석 현상을 억제시킬 수 있으므로 바람직하다. In this case, the mineralizer solution is used to add zinc oxide powder to the mineralizer solution at a concentration of about 5 to 10 g / ℓ and then heated to 60 to 70 ℃ for use in the form of a zinc oxide saturated solution It is preferable because it can suppress the stones due to spontaneous nucleation on the wall surface.

본 발명의 단결정 제조방법은 결정이 주상형이나 판상형에 관계없이 사용될수 있는 방법으로서, <100> 방향으로의 성장 속도를 기존의 방법에 비해 최소한 5배 이상 증가시킬 수 있다.The single crystal production method of the present invention is a method in which the crystal can be used irrespective of the columnar shape or the plate shape, and can increase the growth rate in the <100> direction at least five times as compared to the conventional method.

이하, 본 발명을 하기 실시예에 의거하여 좀더 상세하게 설명하고자 한다. 단, 하기 실시예는 본 발명을 예시하기 위한 것일 뿐, 본 발명의 범위가 이들 만으로 제한되는 것은 아니다.Hereinafter, the present invention will be described in more detail based on the following examples. However, the following examples are only for illustrating the present invention, and the scope of the present invention is not limited thereto.

실 시 예 1Example 1

산화아연 분말을 내경 10mm의 몰드를 이용하여 펠렛트(pellet) 모양으로 만든 다음1000℃에서 2 시간 동안 소결시켜 얻은 소결체 50g을 바스켓에 넣어 은으로 내자된 내용적 200cc의 오토클레이브(autocave)의 하단부(원료용해부)에 창착 하였다. 그 위에 개공도 10%의 대류조절판을 얹은 다음, 오토클레이브의 상단부(결정육성부)에 <001> 방향의 판상 산화아연 종자결정을 장착하였다.Zinc oxide powder was pelletized using a mold having an internal diameter of 10 mm, and then 50 g of a sintered body obtained by sintering at 1000 ° C. for 2 hours was put in a basket. Founded in (dissolve raw material). A convection control plate having a porosity of 10% was placed thereon, and then plate-shaped zinc oxide seed crystals in the <001> direction were mounted on the upper portion (crystal growth portion) of the autoclave.

3M KOH 수용액에 LiOH 및 NH4Cl를 첨가하여 3M KOH, 1M LiOH 및 0.5M NH4Cl가 되도록 혼합용액을 조제한 후 여기에 5g/ℓ의 산화아연 분말을 첨가하고 80℃로 가열한 다음 거름종이로 걸렀다. 이 용액을 충진율 80%에 맞춰 채취하여 상기 오토클레이브에 채운 다음, 밀봉하고 상단부 350℃, 하단부 370℃로 승온한 수 20일간 유지시켜 결정을 육성하였다. 육성이 끝난 후 결정을 회수하여 X-선 분말회절도로 육성된 결정이 산화아연 단결정임을 확인하였다.LiOH and NH 4 Cl were added to the 3M KOH aqueous solution to prepare a mixed solution to be 3M KOH, 1M LiOH and 0.5M NH 4 Cl, and then 5 g / L zinc oxide powder was added thereto, and heated to 80 ° C. Filtered. The solution was collected at 80% filling rate, filled in the autoclave, sealed, and maintained for 20 days in which the temperature was raised to 350 ° C. at the top and 370 ° C. at the lower end to grow crystals. After the growth was completed, the crystals were recovered, and it was confirmed that the crystals grown by X-ray powder diffraction were zinc oxide single crystals.

실 시 예 2Example 2

광화제 용액 중 NH4Cl의 농도를 1 M로 하는 것을 제외하고는 상기 실시예 1과 동일한 방법으로 산화아연 단결정을 제조하였다.Zinc oxide single crystals were prepared in the same manner as in Example 1, except that the concentration of NH 4 Cl in the mineralizer solution was 1 M.

실 시 예 3 Example 3

성장온도를 상단부 330℃, 하단부 350℃로 하는 것을 제외하고는 상기 실시 예 1과 동일한 방법으로 산화아연 단결정을 제조하였다.Zinc oxide single crystals were prepared in the same manner as in Example 1, except that the growth temperature was set to 330 ° C. at the top and 350 ° C. at the bottom.

비 교 예 1Comparative Example 1

광화제로서 NH4Cl를 첨가하지 않은 KOH와 LiOH만의 혼합 용액을 사용하는 것을 제외하고는 상기 실시예 1과 동일한 방법으로 산화아연 단결정을 제조하였다.Zinc oxide single crystals were prepared in the same manner as in Example 1, except that KOH and LiOH mixed solutions without NH 4 Cl were used as the mineralizer.

비 교 예 2Comparative Example 2

광화제로서 NH4Cl를 첨가하지 않은 KOH와 LiOH만의 혼합 용액을 사용하는 것을 제외하고는 상기 실시예 3과 동일한 방법으로 산화아연 단결정을 제조하였다. As mineralizer Zinc oxide single crystals were prepared in the same manner as in Example 3, except that KOH and LiOH mixed solutions without NH 4 Cl were used.

상기 실시예 및 비교예에서의 단결정 성장 결과를 하기 표 1에 나타내었다.The results of single crystal growth in Examples and Comparative Examples are shown in Table 1 below.

Figure 112005048581937-PAT00001
Figure 112005048581937-PAT00001

상기 표에서 보듯이, <001> 방향의 성장속도는 실시예 및 비교예가 모두 비슷하였으나, <100> 방향의 성장속도는 광화제에 NH4Cl를 첨가한 실시예의 경우 비교예에 비하여 약 8 내지 9배 증가하였음을 알 수 있다.As shown in the above table, the growth rate in the <001> direction was similar in both the examples and the comparative examples, but the growth rate in the <100> direction was about 8 to about 8 compared to the comparative example in the case of adding NH 4 Cl to the mineralizer. 9 times increase.

본 발명의 산화아연 단결정 제조방법에 따르면, <100> 방향의 성장속도가 기존의 것에 비해 8배 이상 증가된 산화아연 단결정을 제조할 수 있다.According to the zinc oxide single crystal production method of the present invention, it is possible to produce a zinc oxide single crystal in which the growth rate in the <100> direction is increased by 8 times or more.

Claims (6)

광화제로서 KOH, LiOH 및 NH4Cl을 포함하는 혼합 수열 용액의 존재 하에 산화아연 분말 소결체 원료 및 산화아연 종자 결정을 사용하여 수열법에 의해 산화아연 단결정을 제조하는 방법.A method for producing a zinc oxide single crystal by hydrothermal method using a zinc oxide powder sintered raw material and zinc oxide seed crystals in the presence of a mixed hydrothermal solution containing KOH, LiOH and NH 4 Cl as mineralizers. 제 1 항에 있어서, The method of claim 1, 광화제 중의 각 성분의 농도가 KOH 1 내지 4 M, LiOH 0.5 내지 1.5 M 및 NH4Cl 0.5 내지 1 M 범위임을 특징으로 하는 방법.Wherein the concentration of each component in the mineralizer ranges from KOH 1 to 4 M, LiOH 0.5 to 1.5 M and NH 4 Cl 0.5 to 1 M. 제 1 항에 있어서,The method of claim 1, 광화제로서 산화아연이 포화된 용액을 사용함을 특징으로 하는 방법.A method characterized by using a saturated solution of zinc oxide as a mineralizer. 제 3 항에 있어서,The method of claim 3, wherein 산화아연이 포화된 광화제 용액이, 산화아연 분말을 광화제 용액에 5 내지 10 g/l 범위의 농도로 넣고 60 내지 70 ℃ 범위로 가열함으로써 제조된 것임을 특징으로 하는 방법.And a zinc oxide saturated mineralizer solution is prepared by putting zinc oxide powder in a mineralizer solution at a concentration ranging from 5 to 10 g / l and heating to a range from 60 to 70 ° C. 제 1 항에 있어서,The method of claim 1, 산화아연 분말 소결체를 반응기의 하단에 장착하고 산화아연 종자 결정을 상기 반응기의 상단에 장착한 다음, 상기 반응기에 광화제 용액을 채우고, 상단부는 약 330 내지 350℃, 하단부는 350 내지 370℃로 승온하는 것을 포함함을 특징으로 하는 방법.The zinc oxide powder sintered body was mounted at the bottom of the reactor and the zinc oxide seed crystals were mounted at the top of the reactor, and then the mineralizer solution was filled in the reactor. Method comprising the step of: a. 제 5 항에 있어서,The method of claim 5, 반응기의 압력을 350 내지 400 기압으로 유지함을 특징으로 하는 방법.The pressure of the reactor is maintained at 350 to 400 atmospheres.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102127802A (en) * 2011-03-18 2011-07-20 山东大学 Method for growing zinc oxide monocrystalline under hydrothermal condition by utilizing mineralizer
CN104032374A (en) * 2014-05-16 2014-09-10 浙江大学 Preparation method of lead titanate/zinc oxide composite nanostructure on flexible substrate

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102127802A (en) * 2011-03-18 2011-07-20 山东大学 Method for growing zinc oxide monocrystalline under hydrothermal condition by utilizing mineralizer
CN102127802B (en) * 2011-03-18 2013-01-02 山东大学 Method for growing zinc oxide monocrystalline under hydrothermal condition by utilizing mineralizer
CN104032374A (en) * 2014-05-16 2014-09-10 浙江大学 Preparation method of lead titanate/zinc oxide composite nanostructure on flexible substrate
CN104032374B (en) * 2014-05-16 2016-09-28 浙江大学 The preparation method of lead titanates/zinc oxide composite nanostructure in a kind of flexible substrates

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