KR960006246B1 - Process for the preparation of plzt thin film using seed layer - Google Patents

Process for the preparation of plzt thin film using seed layer Download PDF

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KR960006246B1
KR960006246B1 KR1019930025439A KR930025439A KR960006246B1 KR 960006246 B1 KR960006246 B1 KR 960006246B1 KR 1019930025439 A KR1019930025439 A KR 1019930025439A KR 930025439 A KR930025439 A KR 930025439A KR 960006246 B1 KR960006246 B1 KR 960006246B1
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이준성
노광수
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한국과학기술원
천성순
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Abstract

The method of fabricating a PLZT thin film using sol-gel process includes the steps of forming a seed layer by using a PLZT coating solution having a first composition and drying it, forming a thin film with a PLZT coating solution having a second composition on the PLZT thin film having the first composition and drying it, and heat-treating the dried thin film.

Description

씨앗층을 이용한 PLZT 박막의 제조방법Manufacturing method of PLZT thin film using seed layer

제1도는 씨앗층을 사용하지 않은 PLZT(9.5/65/35) 박막의 SEM 사진.1 is a SEM photograph of a PLZT (9.5 / 65/35) thin film without a seed layer.

제2도는 씨앗층으로 사용되는 PLZT(15.5/40/60) 박막의 SEM 사진.2 is a SEM photograph of a PLZT (15.5 / 40/60) thin film used as a seed layer.

제3도는 씨앗층(PLZT(15.5/40/60))을 사용한 PLZT(9.5/65/35) 박막의 SEM 사진.3 is a SEM photograph of a PLZT (9.5 / 65/35) thin film using a seed layer (PLZT (15.5 / 40/60)).

제4도는 씨앗층을 사용하지 않은 PLZT(9.5/65/35) 박막과 씨앗층을 사용한 PLZT(9.5/65/35) 박막의 XRD 그래프.4 is an XRD graph of PLZT (9.5 / 65/35) thin film without seed layer and PLZT (9.5 / 65/35) thin film using seed layer.

제5도는 씨앗층을 사용하지 않은 PLZT(9.5/65/35) 박막과 씨앗층을 사용한 PLZT(9.5/65/35) 박막의 투과성 측정 그래프.5 is a graph of permeability measurement of PLZT (9.5 / 65/35) thin film without seed layer and PLZT (9.5 / 65/35) thin film using seed layer.

본 발명은 PLZT(Pb1-xLax(ZryTi1-y(1-x/4O3; 란탄산납-지르콘산납-티탄산납) 박막의 제조방법에 관한 것으로, 특히 씨앗층(seeding layer)을 사용하여 PLZT 박막을 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a PLZT (Pb 1-x La x (Zr y Ti 1-y ( 1-x / 4 O 3 ; lead lanthanum-lead zirconate-lead titanate)) thin film, in particular a seed layer To a PLZT thin film.

PLZT는 PZT(PbTiO3ㆍPbZrO3; 티탄산납ㆍ지르콘산납)에서 Pb의 일부를 La로 치환한 것으로서 광전자 분야에서 광전 소자로서 널리 사용된다.PLZT replaces a part of Pb with La in PZT (PbTiO 3 .PbZrO 3 ; lead titanate and lead zirconate) and is widely used as an optoelectronic device in the optoelectronic field.

이차 전광 효과(Quadratic electrooptic effect) 응용을 목적으로 하는 PLZT의 La/Zr/Ti 조성 비율은 8.5/65/35.9/65/35, 9.5/65/35이라는 것이 공지되어 있다. PLZT의 상(相)에는 강유전성(ferroelectric)을 나타내는 페르보스카이트상(perovskite phase)과 상유전성(paraelectric)을 나타내는 파이로클로로상(pyrochlorephase)이 있는데, 이차 전광 특성은 PLZT가 페르보스카이트상으로 이루어진 경우에만 일어나는 현상이므로,100%의 페르브스카이트상으로 이루어진 박막을 제조하는 것이 요구되어 왔다. 세라믹 물질의 소결 공정은 헥생성 공정과 생성된 핵에서부터 입자가 성장하는 공정으로 구분할 수 있는데 PLZT 박막의 경우에는 핵생성 활성화 에너지(activation energy)가 입자 성장 활성화 에너지보다 매우 크기 때문에 핵생성 과정이 전체 공정을 좌우한다. 또한, 페르보스카이트상은 파이로클로로상보다 높은 활성화 에너지를 갖기 때문에, 저온소결시 먼저 파이로클로로상으로 생성되는데, 이점이 100%의 페르보스카이트상으로 이루어진 박막을 얻기 어러운 가장 큰 이유이다.It is known that the La / Zr / Ti composition ratios of PLZT for the purpose of secondary electrooptic effect applications are 8.5 / 65 / 35.9 / 65/35 and 9.5 / 65/35. The phases of PLZT include a perovskite phase with ferroelectricity and a pyrochlore phase with paraelectricity. Since the phenomenon occurs only when made, it has been required to produce a thin film made of 100% perovskite phase. The sintering process of ceramic material can be divided into hex generation process and particle growth process from the nucleus generated. In the case of PLZT thin film, the nucleation process is performed as the nucleation activation energy is much larger than the particle growth activation energy. It depends on the process. In addition, since the pervoskate phase has a higher activation energy than the pyrochloro phase, it is first formed as a pyrochloro phase upon low temperature sintering, which is the biggest reason why it is difficult to obtain a thin film composed of 100% of perovskite phase. .

단일상의 세라믹 박막을 얻기 위하여 씨앗층을 사용하는 방법들은 공지되어 있다. 예를 들면, 밀러(K.T.Miller)와 라지(F. Large)가 저술한 "Highly Oriented Thin Films of Cubic Zirconis on Sapphire through Grain Growth Seeding", J. Mater, Res., Vol. 6, 2387, (1991)에는 Al2O3단결정 위에 ZrO2를 입힌 후 제1차 열처리를 행하여 씨앗층을 형성하고, 그후 씨앗층 위에 다시 ZrO2를 입힌 후 제2차 열치리를 행하여 최종적으로 ZrO2박막을 얻는 방법이 개시되어 있다. 또한, 코우크(C.K. Kowk)와 데수(S.B. Desu)가 저술한 "Low Temperature Perovskite Formation of Lead Zirconate Titanate Thin Films by Seeding process", J. Mater, Res., Vol. 8, 339, (1993)에는 사파이어 단결정 위에 PbTiO3를 입힌 후 제1차 열처리를 행하여 씨앗층을 형성하고, 그 후 씨앗층 위에 PZT(Zr/Ti=53/47)를 입힌 후 제2차 열치리를 행하여 최종적으로 PZT 박막을 얻는 방법이 개시되어 있다.Methods of using seed layers to obtain single phase ceramic thin films are known. See, for example, "Highly Oriented Thin Films of Cubic Zirconis on Sapphire through Grain Growth Seeding" by KTMiller and F. Large, J. Mater, Res., Vol. 6, 2387, and (1991), ZrO 2 is coated on Al 2 O 3 single crystals, and then subjected to a first heat treatment to form a seed layer. Then, ZrO 2 is coated on the seed layer again, followed by secondary thermal treatment. A method of obtaining a ZrO 2 thin film is disclosed. In addition, "Low Temperature Perovskite Formation of Lead Zirconate Titanate Thin Films by Seeding process" by CK Kowk and SB Desu, J. Mater, Res., Vol. 8, 339, (1993), PbTiO 3 is coated on the sapphire single crystal, followed by a first heat treatment to form a seed layer, and then a PZT (Zr / Ti = 53/47) is applied on the seed layer, followed by a second heat. A method of finally obtaining a PZT thin film by performing control is disclosed.

그러나, 상기 공지된 방법은 2회의 열치리 공정을 거치므로 박막의 제조공정이 복잡할 뿐만 아니라, 제1차 열처리 공정에 의하여 제조된 씨앗층이 열처리시 발생되는 입자들에 의하여 오염되고 그 입자들이 박막의 균열을 유도하므로 실제 응용하기에 어려운 문제점이 있었다. 또한 상기 공지된 방법은 단결정을 사용하므로 가격이 상당히 비싸다는 문제점도 있었다.However, since the known method undergoes two thermal treatment processes, not only the manufacturing process of the thin film is complicated, but also the seed layer produced by the first heat treatment process is contaminated by the particles generated during the heat treatment, and the particles Inducing a crack in the thin film has a problem that is difficult to practical application. In addition, the known method uses a single crystal, so there is a problem that the price is quite expensive.

본 발명은 이러한 단점을 제거하기 위한 것으로서, 본 발명의 목적은 씨앗층을 이용하여 저온에서 1회의 열치러만으로 100%의 페르보스카이트상으로 이루어진 PLZT 박막을 제조하고자 함에 있다.The present invention is to eliminate this drawback, the object of the present invention is to produce a PLZT thin film consisting of 100% of the pervoskite phase by only one heat treatment at low temperature using a seed layer.

본 발명의 목적은 또한 저렴한 비용으로 전기적 특성이 우수하고 투과성이 향상된 PLZT 박막을 제조하고자 함에 있다.An object of the present invention is also to produce a PLZT thin film having excellent electrical properties and improved permeability at low cost.

본 발명의 전술한 목적은 솔-젤(sol-gel)공정을 이용하여 PLZT 박막을 제조하는 경우 씨앗층으로 불균일헥 생성 자리(heterogeneous uncleation site)를 제공하고 1회 열처리하는 것에 의하여 달성된다.The above object of the present invention is achieved by providing a heterogeneous uncleation site as a seed layer and heat treatment once when producing a PLZT thin film using a sol-gel process.

이하 첨부된 도면을 참조하여 종래 기술과 본 발명의 실시예를 상세히 설명한다. 후술하는 실시예는 솔-젤 공정을 이용하여 PLZT 박막을 제조하는 것에 관한 것으로 기판으로는 ITO(indium thin oxide)가 코팅된 유리(상품명:Corning 7059 glass)를 사용하였다.Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings. An example to be described later relates to manufacturing a PLZT thin film using a sol-gel process, and a glass (trade name: Corning 7059 glass) coated with indium thin oxide (ITO) was used as a substrate.

(실시예 1)(Example 1)

실시예 1은 종래 기술과 마찬가지로 씨앗층을 사용하지 않고 PLZT 박막을 제조하는 것이다.Example 1 is to produce a PLZT thin film as in the prior art without using a seed layer.

먼저, PLZT(9.5/65/35)의 조성을 갖는 코팅 용액을 조제하였다. 기판을 세척한 다음, 이 기판에 상기 PLZT(9.5/65/35) 코팅 용액을 떨어뜨린 후, 기판을 3000rpm으로 30초 동안 회전시켜 박막을 형성하였다. 그 결과 얻은 박막을 350℃에서 5분간 건조하였다. 상기 PLZT(9.5/65/35) 용액의 코팅 및 건조 공정을 9회 반복하였다.First, a coating solution having a composition of PLZT (9.5 / 65/35) was prepared. After the substrate was washed, the PLZT (9.5 / 65/35) coating solution was dropped on the substrate, and the substrate was rotated at 3000 rpm for 30 seconds to form a thin film. The resulting thin film was dried at 350 ° C. for 5 minutes. The coating and drying process of the PLZT (9.5 / 65/35) solution was repeated nine times.

건조된 PLZT(9.5/63/35) 박막을 650℃ 의 노내에 직접 집어넣기(direct insertion)하여 1시간 동안 유지시켜 소결시켰다.The dried PLZT (9.5 / 63/35) thin film was directly inserted into a furnace at 650 ° C., held for 1 hour, and sintered.

(실시예 2)(Example 2)

PLZT(15.5/40/60) 및 PLZT(9.5/65/35)의 조성을 갖는 코팅 용액을 제조하였다. 기판을 세척하고, 씨앗층으로 사용될 PLZT(15.5/40/60) 코팅 용액을 기판에 떨어뜨린 후, 기판을 3000rpm으로 30초 동안 회전시켜 박막을 형성하였다. 그 결과 얻은 박막을 350℃ 에서 5분간 건조하였다.Coating solutions having compositions of PLZT (15.5 / 40/60) and PLZT (9.5 / 65/35) were prepared. The substrate was washed, a PLZT (15.5 / 40/60) coating solution to be used as the seed layer was dropped on the substrate, and the substrate was then rotated at 3000 rpm for 30 seconds to form a thin film. The resulting thin film was dried at 350 ° C. for 5 minutes.

건조된 박막 위에 PLZT(9.5/65/35) 코팅 용액을 떨어뜨린 후, 기판을 3000rpm으로 30초 동안 회전시켜 박막을 형성하였다. 그 결과 얻은 박막을 350℃에서 5분간 건조하였다. 이 때, 박막 형성 및 건조 공정을 8회 반복하였다.After dropping the PLZT (9.5 / 65/35) coating solution on the dried thin film, the substrate was rotated at 3000 rpm for 30 seconds to form a thin film. The resulting thin film was dried at 350 ° C. for 5 minutes. At this time, the thin film formation and drying processes were repeated eight times.

건조된 박막을 650℃의 로에 직접 집어넣기하여 1시간 동안 유지시켜 소결하였다.The dried thin film was put directly into a furnace at 650 ° C. and maintained for 1 hour to sinter.

제1도는 실시예 1에 의하여 제조한 PLZT(9.5/65/35) 박막의 SEM 사진이다. 즉, 씨앗층을 사용하지 않고 제조한 PLZT 박막으로서 제1도에서 지름이 5μm∼6μm 정도의 크기를 갖는 동그랗게 보이는 부분이 페르보스카이트상이고 나머지 바턍 부분이 파이로클로로상이다.1 is an SEM photograph of the PLZT (9.5 / 65/35) thin film prepared according to Example 1. FIG. That is, the PLZT thin film manufactured without using the seed layer is a pervoskite phase and a remaining portion is a pyrochloro phase in FIG. 1 having a diameter of about 5 μm to 6 μm.

제2도는 실시예 2에서 PLZT(15.5/40/60) 조성의 코팅 용액을 사용한 공정을 거친 후, 건조된 박막을 650℃의 노내에 직접 집어넣기하여 1시간 유지하여 소결한 PLZT(15.5/40/60) 박막의 SEM 사진이다. 즉,씨앗층으로 사용되는 PLZT 박막으로서 제2도는 지름이 0.2㎛∼0.3㎛ 정도되는 페르보스카이트상으로만 이루어진 PLZT 박막을 나타내고 있다.FIG. 2 shows the PLZT (15.5 / 40) sintered after the process using the coating solution of the composition PLZT (15.5 / 40/60) in Example 2, and put the dried thin film directly into the furnace at 650 ℃ for 1 hour SEM photo of the thin film. That is, the PLZT thin film used as the seed layer shows a PLZT thin film composed only of a pervoskite phase having a diameter of about 0.2 µm to 0.3 µm.

제3도는 제2실시예에 의하여 제조된 PLZT(9.5/65/35) 박막의 SEM사진이다.3 is a SEM photograph of the PLZT (9.5 / 65/35) thin film prepared according to the second embodiment.

제3도에서 볼 수 있는 바와 같이, PLZT(9.5/65/35) 박막은 지름이 0.2㎛∼0.3㎛정도인 페르보스카이트상으로만 이루어진다.As can be seen in FIG. 3, the PLZT (9.5 / 65/35) thin film consists only of a pervoskite phase with a diameter of about 0.2 μm to 0.3 μm.

제1도와 제3도를 비교하여 보면, 씨앗층을 사용하여 제조한 PLZT 박막은 씨앗층을 사용하지 않은 것에 비하여 입자의 크기가 매우 미세하고 균일하다는 것을 알 수 있다.Comparing FIG. 1 and FIG. 3, it can be seen that the PLZT thin film manufactured using the seed layer has a very fine and uniform particle size compared to the seed layer.

본 발명에서 씨앗층으로 사용한 PLZT(15.5/40/60)는 PLZT(9.5/65/35)보다 훨씬 낮은 온도의 열처리공정을 거쳐도 파이로클로로상은 전혀 나타나지 않고 페르보스카이트상만 나타나며, 또한 입자크기도 미세하고 균일하다. 따라서, 씨앗층이 PLZT(9.565/35)가 반응이 일어나기 전에 미리 작고 균일한 페르보스카이트상을 만들어 PLZT(9.5/65/35)가 페르보스카이트상으로 성장할 수 있는 헥생성 자리를 마련하여 준다.PLZT (15.5 / 40/60) used as the seed layer in the present invention is a pyrochloro phase does not appear at all, but only a pervoskite phase, even after the heat treatment process at a much lower temperature than PLZT (9.5 / 65/35) The size is also fine and uniform. Thus, the seed layer creates a small, uniform pervosky phase before PLZT (9.565 / 35) reacts, thus providing a hexogenic site for PLZT (9.5 / 65/35) to grow into pervosky phase. .

제4도는 씨앗층을 사용하지 않았을 때와 사용했을 때의 PLZT(9.5/65/35) 박막의 XRD 분석 결과이다. 제4도에서 ''PY"로 표시된 부분은 파이로클로로상을 나타내고, ''ITO"로 표시된 부분은 기판의 ITO 막을 나타낸다. 즉, 씨앗층을 사용하지 않은 경우에는 파이로클로로상이 관측되었지만 씨앗층을 사용한 졍우에는 전혀 파이로클로로상이 관측되지 않았다. 이러한 사실은 제1도 및 제3도의 SEM 분석 결과를 지지하여준다.4 shows the results of XRD analysis of PLZT (9.5 / 65/35) thin films with and without seed layers. In FIG. 4, the portion labeled 'PY' represents the pyrochloro phase, and the portion labeled 'ITO' represents the ITO film of the substrate. That is, the pyrochloro phase was observed when the seed layer was not used, but the pyrochloro phase was not observed at all when the seed layer was used. This fact supports the results of SEM analysis in FIGS. 1 and 3.

제5도는 씨앗층을 사용하지 않는 것과 사용한 PLZT(9.5/65/35) 박막의 투광성 측정 데이타이다. 제5도에서 알 수 있는 바와 같이, 씨앗층을 사용한 시편은 사용하지 않은 시편보다 20% 정도 투광성이 높다.5 is light transmission measurement data of a PLZT (9.5 / 65/35) thin film without using a seed layer. As can be seen in Figure 5, the specimen using the seed layer is about 20% higher light transmittance than the unused specimen.

이상과 같이 본 발명에 의한 PLZT 박막은 패르보스카이트상으로만 이루어지고 입자 크기가 미세하고 균일하여 이차 전광 효과의 응용에 적합하며, 특히 투광성이 향상되어 차세대 광전 소자로 사용하기에 적합하다.As described above, the PLZT thin film according to the present invention is formed only in the parvoscatite phase and has a fine and uniform particle size, which is suitable for the application of the secondary electroluminescent effect, and particularly, it is suitable for use as a next-generation photoelectric device due to improved light transmittance.

앞에서는 특정한 실시예를 들어 본 발명을 설명하였지만, 본 발명 분야에서 통상의 지식을 가진 자는 본발명의 범위내에서 다양한 변형 및 응용을 가할 수 있다는 사실을 알 수 있으므로, 본 발명은 상기 실시예만 한정되는 것이 아니다.While the present invention has been described with reference to specific embodiments, it will be appreciated by those skilled in the art that various modifications and applications can be made within the scope of the present invention. It is not limited.

Claims (3)

솔-젤 방법을 이용하여 PLZT 박막을 제조하는 방법에 있어서, 제1의 조성을 갖는 PLZT 코팅 용액으로 씨앗층을 형성한 후 건조시키는 단계와, 상기 제1의 조성을 갖는 PLZT 박막 위에 제2의 조성을 갖는 PLZT 코팅 용액으로 박막을 형성한 후 건조시키는 단계 및 건조된 박막을 열처리하는 단계를 포함하는것을 특징으로 하는 PLZT 박막의 제조방법.A method for producing a PLZT thin film using a sol-gel method, comprising: forming a seed layer with a PLZT coating solution having a first composition and drying the seed layer, and having a second composition on the PLZT thin film having the first composition Forming a thin film with a PLZT coating solution, and then drying and drying the dried thin film method of producing a PLZT thin film. 제1항에 있어서, 상기 제1 조성의 PLZT는 La/Zr/Ti 비율이 15.5/40/60이고, 제2조성의 PLZT는 La/Zr/Ti 비율이 9.5/65/35인 것인 PLZT 박막의 제조방법.The PLZT thin film according to claim 1, wherein the PLZT of the first composition has a La / Zr / Ti ratio of 15.5 / 40/60, and the PLZT of the second composition has a La / Zr / Ti ratio of 9.5 / 65/35. Manufacturing method. 제1항에 있어서, 상기 열처리 단계는 650℃에서 1시간 동안 행하는 것인 PLZT 박막의 제조방법.The method of claim 1, wherein the heat treatment is performed at 650 ° C. for 1 hour.
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