KR20050054122A - 자외선 원자층 증착법을 이용한 박막 제조 방법 - Google Patents
자외선 원자층 증착법을 이용한 박막 제조 방법 Download PDFInfo
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- KR20050054122A KR20050054122A KR1020030087448A KR20030087448A KR20050054122A KR 20050054122 A KR20050054122 A KR 20050054122A KR 1020030087448 A KR1020030087448 A KR 1020030087448A KR 20030087448 A KR20030087448 A KR 20030087448A KR 20050054122 A KR20050054122 A KR 20050054122A
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/407—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
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Abstract
본 발명은 저온에서 자외선 원자층 증착법을 이용한 박막 제조 방법에 관한 것으로, 기판이 로딩된 챔버 내로 제1 반응물의 기체를 펄스 형태로 주입하여 기판 표면에 제1 반응물을 화학 흡착시킨 후 상기 챔버 내로 불활성 기체를 펄스 형태로 주입하여 1차로 퍼지하고, 이어서 상기 기판 위로 자외선을 조사하면서 챔버 내로 제2 반응물의 기체를 펄스 형태로 주입하여 상기 제1 반응물 상에 화학 흡착시켜 반응시킨 후 불활성 기체로 2차 퍼지하여 원자층 단위의 박막을 형성한다. 이와 같은 본 발명에 의하면, 원자층 증착과정에서 자외선을 조사하여 원자층 형성의 화학 반응을 촉진시켜 기존 원자층 증착 공정보다 저온에서의 증착 속도를 증대시키고 단차 피복성, 막의 균일도 및 기판 표면과 박막 사이의 결합력을 증가시킴으로써 고품위의 나노 두께 박막을 제조할 수 있고, 박막 제조 공정의 시간과 비용 절감의 효과를 가져올 수 있다.
Description
본 발명은 박막 제조 방법에 관한 것으로, 특히 저온에서 높은 증착 속도를 나타내고 막의 균일도 및 기판 표면과 박막 사이의 결합력을 증가시키며 단차 피복성(step coverage)이 우수한 자외선 원자층 증착법(UV-Enhanced Atomic Layer Deposition: 이하, "자외선 ALD"라고 함)을 이용한 박막 제조 방법에 관한 것이다.
최근, 반도체 소자의 고집적화에 따라 집적회로를 구성하고 있는 구조의 크기가 나노미터(nanometer) 수준으로 미세화 되고 있어, 이와 관련된 반도체 제조 과정에서 미세 패터닝된 구조의 매립이나 도포를 위한 박막 형성 공정에 있어서 기존의 CVD(Chemical Vapor Deposition) 공정보다 단차 피복성이 향상된 박막 제조 공정이 필요하게 되었다. 이에 기존 CVD 공정을 대체하는 방법으로 새롭게 부각되고 있는 것이 원자층 증착법(Atomic Layer Deposition: 이하, "자외선 ALD"라고 함)을 이용한 공정이다. 또한, 센서, 초소형 기계 및 신촉매 등 나노기능소자를 제작하는 과정에서도 여러 가지 물질들의 박막을 나노미터 수준에서 제조하고 조절하는 박막 제조 공정이 중요한 기술을 차지하고 있어, 이들 분야에서도 ALD 공정이 적용될 수 있다.
기존의 CVD 공정은 여러 반응 기체를 반응로에 혼합 주입하여 반응시켜 화학 반응을 통해 원하는 물질의 박막을 증착하는 기술이다. 그러나, 이러한 CVD 공정은 탄소나 산소 등 불순물에 의한 오염이 크고, 고온에서의 기상 반응에 의한 입자(particle) 생성 및 확산(diffusion)에 의해 표면 특성이 매끄럽지 못하게 되 는 단점이 있다. 또한, 기체 상태에서 원료들 사이의 반응, 원료의 분해, 표면 반응과 확산, 박막의 성장 등 여러 가지 복잡한 과정이 동시에 일어나기 때문에 공정 변수의 제어가 정밀하지 않아 다단계 박막을 나노급(nano scale)으로 성장시키는 데 어려움이 있다. 그리고, 주로 고온에서 수행되어야 하므로 반도체 기판 위에 형성되어 있는 열에 약한 다른 일부 소자들이 열적 손상을 받을 수 있는 문제점이 있고, 고온에서 박막 형성이 매우 빠르게 진행되므로 나노급 박막 형성에 있어 막두께의 조절이 어려운 문제점이 있다.
상기한 기존 CVD공정의 단점을 극복하기 위해 최근 제시되는 ALD공정은 기판 표에서 반응물질의 표면 포화 반응(surface saturated reaction)에 의한 화학적 흡착(chemisorption)과 탈착(desorption) 과정을 이용하여 단원자층을 형성하는 방법으로, 원자층 수준에서 막 두께의 제어가 가능한 박막 증착 방법이다.
여러 반응물을 혼합하여 챔버 내로 공급하여 반응을 진행시키는 기존 CVD 공정과 달리 ALD공정은 한 번에 하나의 반응 기체를 주입하게 되고 각각의 반응 기체 주입 단계 사이에 퍼지 또는 펌핑과정을 도입하여 미반응물 및 부산물을 제거하여 단원자층 단위로 적층하여 박막을 형성하는 공정이다.
각 반응물의 주입 단계에서 기판 표면에서만 화학적 흡착과 화학 반응이 일어나 하나의 원자층이 완전히 형성될 때까지 다른 표면 반응이 일어나지 않아 원자층 형성의 제어가 용이하다. 따라서, 불순물 혼입과 결함(defect) 생성의 억제가 가능하며 CVD 공정보다 낮은 온도에서 다양한 원료 기체를 사용하여 박막을 제조할 수 있으며, 궁극적으로 100% 단차 피복성을 나타내어 복잡한 모양을 가지는 기판에서도 균일한 두께를 갖는 고품질의 박막의 증착이 가능하다.
그러나, 기존 ALD공정의 가장 큰 단점은 저온에서 진행되는 경우 증착속도가 느리다는 것이며, 또한 퍼지나 펌핑 단계에서 물리 흡착된 미반응물과 부산물을 제거하는 단계에서 이들을 잘 제거하지 못하여 박막의 균일도와 순도가 떨어지는 문제점이 있다.
따라서, 본 발명은 상기한 기존 ALD공정의 문제점을 해결하기 위한 것으로, ALD 과정에서 자외선을 조사하여 원자층 형성의 화학 반응을 촉진시켜 기존 ALD 공정보다 저온에서의 증착 속도를 증대시키고 막의 균일도 및 기판 표면과 박막 사이의 결합력을 증가시킬 수 있는 박막 제조 방법을 제공하는 것을 목적으로 한다.
상기한 기술적 과제를 달성하기 위하여, 본 발명의 자외선 ALD를 이용한 박막 제조 방법은 (가) 챔버 내에 기판을 로딩하고 제1 반응물의 기체를 펄스 형태로 주입하여 기판 표면에 화학 흡착시켜 제1 반응물의 층을 형성하는 단계, (나) 상기 챔버 내로 불활성 기체를 펄스 형태로 주입하여 1차 퍼지하는 단계, (다) 상기 기판 위로 자외선을 조사하면서 챔버 내로 제2 반응물의 기체를 펄스 형태로 주입하여 상기 제1 반응물 층에 제2 반응물을 화학 흡착시켜 두 반응물의 화학 반응에 의하여 원자층 단위의 박막을 형성하는 단계, (라) 상기 챔버 내로 불활성 기체를 펄스 형태로 주입하여 2차 퍼지하는 단계를 포함하여 이루어지는 것을 특징으로 한다.
본 발명에서 개시하는 자외선 ALD를 이용한 박막 제조 방법은 ALD 과정에서 제1 반응물이 화학 흡착되어 있는 기판 위로 자외선(UV)을 조사(irradiation)하면서 동시에 제2 반응물 펄스 형태로 주입하여, 자외선에 의해 두 반응물간의 화학 반응 및 미반응물이나 불순물들을 분해가 광촉매적으로(photocatalytically) 촉진될 수 있다. 즉, 자외선이 기판이나 기판에 흡착되어 있는 반응물에 의해 흡수되면 반응물이 활성화되어 반응성이 증가하여 제1 반응물과 제2 반응물 간의 화학 반응이 촉진되어 증착 속도가 증가된다.
특히, 실리콘이나 TiO2와 같은 반도체들은 자외선을 흡수하여 광촉매의 역할을 할 수 있어, 저온에서 자외선 ALD를 이용하여 실리콘 기판에서 TiO2 박막을 제조하는 경우 반응물들 간의 화학 반응 및 기판 표면과 반응물 간의 화학 결합 반응이 광촉매적으로 촉진될 수 있다.
따라서, 기존의 ALD 공정에 비해 훨씬 낮은 온도에서 증착이 가능하며 실온에서도 빠른 속도로 증착이 가능할 수 있어 제조된 박막의 균일도 증가 및 ALD의 최대 장점인 탁월한 단차 피복성을 확보할 수 있다.
본 발명의 자외선 ALD 공정을 이용한 박막 제조 방법은 상기 (가), (나), (다) 및 (라) 단계를 반복적으로 수행하여 박막의 두께를, 예를 들면 10~1000Å 범위에서 원하는 데로 조절할 수 있다.
상기 (다) 단계에서 조사되는 자외선의 파장은 200nm~300nm으로 한다. 상기 기판은 실리콘웨이퍼, 유리판, 또는 용융실리카로 구성될 수 있다.
이하, 첨부된 도면을 참조하여 본 발명에 따라 기판 위에 박막을 형성하는 방법을 상세하게 설명한다.
도 1은 본 발명에 따른 자외선 원자 증착법을 이용한 박막 제조 공정을 나타내는 흐름도이다.
구체적으로, 먼저 깨끗하게 세정하여 건조시킨 기판을 챔버에 로딩 시킨 후 챔버를 일정한 온도와 압력으로 유지한다(스텝 10). 여기에서, 상기 챔버 내의 공정 온도는 20℃~100℃로 유지하고, 공정 압력은 0.1mTorr~50Torr 범위에서 일정하게 유지되도록 챔버를 계속 펌핑하여 이후의 모든 공정을 진행한다.
이어서, 상기 챔버 내로 제1반응물의 기체를 일정한 펄스의 형태로 주입하여 기판 위에 화학 흡착하도록 한 후(스텝 11), 아르곤(Ar)과 같은 불활성 기체를 역시 펄스 형태로 주입하여 1차 퍼지하여 기판에 흡착되지 않거나 물리 흡착된 제1반응물을 제거한다(스텝 12). 이 때, 기판 위에 제1 반응물의 단원자층(monolayer)이 형성된다.
다음에, 상기 챔버 내의 기판 위로 석영 창(quartz window)을 통하여 자외선을 조사하면서 동시에 제2 반응물의 기체를 챔버 내로 일정한 펄스의 형태로 주입하여 기판 위의 제1 반응물 단원자층에 화학 흡착시켜 제1 반응물과 화학 반응을 일으키도록 하여 원자층이 형성되도록 한다(스텝 13). 이어서, 아르곤(Ar)과 같은 불활성 기체를 펄스 형태로 주입하여 2차 퍼지하여 기판에 흡착되지 않거나 미반응 또는 물리 흡착된 제2 반응물과 불순물을 제거한다(스텝 14).
다음에, 상기한 바와 같은 원자층 형성 단계 즉, 제1 반응물 주입단계, 1차 퍼지 단계, 제2 반응물 주입 단계 및 2차 퍼지 단계를 포함하여 이루어지는 공정 주기(cycle)를 반복 수행하여(스텝 15) 적정 두께의 박막을 형성한다.
상기한 제1 반응물, 불활성 기체, 제2 반응물 각각의 주입 펄스 시간은 0.1초~40초 범위로 일정하게 유지한다(도 2).
본 발명의 자외선 ALD공정은 저온에서 반응성을 향상시켜 증착속도를 증대시키기 위한 목적으로 사용하는 경우에 적용이 가능하다. 예를 들어 단원자 박막, 단원자 산화물, 복합 산화물, 단원자 질화물 또는 복합 질화물 등의 박막 제조에 적용할 수 있다. 상기 단원자 산화물은 MgO, Al2O3, SiO2, TiO2, SnO2, ZnO 또는 ZrO2을 들 수 있다.
이하, 실시예에 의해 본 발명을 보다 상세히 설명하고자 한다. 이러한 실시예는 본 발명을 예시하기 위한 것으로 이에 의하여 본 발명의 범위가 제한되지 아니한다.
[실시예 1]
실리콘웨이퍼 기판 상에 TiO
2
박막의 제조
자외선 ALD를 이용하여 25℃에서 실리콘웨이퍼 기판 위에 TiO2 박막을 제조하였다.
먼저, 깨끗하게 세정하여 건조시킨 실리콘 기판을 챔버에 로딩 시킨 후 챔버의 공정 온도를 25℃로 유지하고, 공정 압력은 0.3Torr로 일정하게 유지되도록 챔버를 계속 펌핑하면서 이후의 모든 공정을 진행하였다. 이어서, 상기 챔버 내로 Ti(i-OPr)4 기체를 1~5초의 펄스로 주입한 후 아르곤을 50sccm으로 5초의 펄스로 주입하여 1차 퍼지하였다. 다음에, 상기 챔버 내의 기판 위로 자외선(600W Xe-램프, 미국 Oriel사 제품)을 조사하면서 동시에 H2O 기체를 챔버 내로 1~8초의 펄스 형태로 주입한 후, 아르곤 기체를 15초의 펄스 형태로 주입하여 2차 퍼지하였다.
이 때, Ti(i-OPr)4와 H2O 각각의 펄스 시간을 변화시키면서 얻어진 TiO2 박막의 320nm에서의 흡광도를 측정하여 그 증착 정도를 확인하였는 데, Ti(i-OPr)4와 H2O 펄스 시간이 각각 2초, 5초 이상에서 증착비가 포화되었다.
다음에, Ti(i-OPr)4와 H2O 각각의 펄스 시간을 각각 2초와 5초로 고정시킨 후 상기한 공정을 1 주기(cycle)로 하여 25~300 주기를 반복하여 TiO2 박막을 형성하였다.
주기의 반복 횟수에 따른 TiO2 박막의 두께를 터널링전자현미경(TEM: Tunneling Electron Microscope)으로 측정하였는 데, 공정 주기의 반복에 따라 박막의 두께는 계속 증가하였으며, 증착 속도는 1.2Å/주기로 얻어졌다(도 3).
[실시예 2]
실리콘웨이퍼 기판 상에 ZrO2 박막의 제조
상기 실시예 1과 같은 방법으로 자외선 ALD를 이용하여 실리콘 기판 위에 ZrO2 박막을 제조하였다. 반응물로는 Zr(t-0Bu)4와 H2O를 사용하였고, Zr(t-0Bu)
4와 H2O 펄스 시간을 각각 1~10초로 하였으며, 1차와 2차 퍼지 과정에서 아르곤 기체는 50sccm으로 각각 30초의 펄스 형태로 주입하였다.
이 때, Zr(t-0Bu)4와 H2O 각각의 펄스 시간을 변화시키면서 얻어진 ZrO2 박막의 두께를 엘립소메트리법(elipsometry)으로 측정하였는데, Zr(t-0Bu)4와 H2O 펄스 시간이 둘 다 5초 이상에서 증착비가 포화되었다.
다음에, Zr(t-0Bu)4와 H2O 각각의 펄스 시간을 각각 5초로 고정시킨 후 25~300 주기의 공정을 반복하여 ZrO2 박막을 형성하였다.
주기의 반복 횟수에 따른 형성된 ZrO2 박막의 두께를 터널링전자현미경(TEM)으로 측정하였는 데, 공정 주기의 반복에 따라 박막의 두께는 계속 증가하였으며, 증착 속도는 3.5Å/주기로 얻어졌다(도 4).
[비교예 1]
자외선 ALD와 기존 ALD 공정에 의해 제조된 TiO2 박막의 비교
자외선 ALD와 기존 ALD 공정을 비교하기 위해, 실시예 1과 같은 방법으로 25℃에서 300 주기의 공정 반복으로 얻어진 TiO2 박막과 자외선을 사용하지 않고 기존의 ALD 공정을 이용하여 75~350℃에서 300 주기의 공정 반복으로 얻어진 TiO2 박막을 제조하였다.
두 공정에서 얻어진 박막의 두께를 TEM으로 측정하여 공정 주기의 반복에 따른 두께의 변화와 증착 속도를 비교하였다(도 5). 두 박막의 표면 성상 (morphology)을 분석, 비교하기 위하여 AFM (Atomic Force Microscope; 원자힘 현미경)을 이용하여 각각의 AFM 사진을 얻었다(도 6).
또한, 기판 표면과 박막과의 결합력(adhesion)을 측정하기 위해 상기의 두 박막에 대하여 스크래치 실험(scratch test)을 수행하였다. 박막에 탐침을 이용하여 하중(load)을 가하면서 박막이 파괴되는 순간의 음향(acoustic emission)을 탐지하여 임계하중(critical load)을 측정하였다(도 7). 이 때 각각의 박막은 공정 주기를 1000회 반복하여 제조되었다.
도 5에 나타낸 바와 같이, 300℃ 이하에서 수행된 기존 ALD 공정의 증착속도는 25℃에서 수행된 자외선 ALD 공정보다 훨씬 느리게 나타났다. 자외선 ALD를 이용한 TiO2 박막 제조에 있어 25℃에서의 증착속도가 350℃에서 수행된 기존 ALD 공정의 증착 속도와 같았다. 결과적으로, 저온에서 수행되는 자외선 ALD 공정의 증착속도가 기존의 고온 ALD 공정보다 훨씬 빠름을 알 수 있다.
도 6에 나타낸 바와 같이, 자외선 ALD를 이용하여 25℃에서 제조된 TiO2 박막과 기존 ALD를 이용하여 350℃에서 제조된 박막의 AFM 사진을 비교해 보면, 자외선 ALD 공정에 제조된 TiO2 박막의 표면이 기존 ALD 공정을 이용해 제조된 박막보다 훨씬 매끄럽고 조밀함을 확인할 수 있다. 기존 ALD 공정은 고온에서 수행되어 박막 표면에서 확산(diffusion)이나 엉김(aggregation) 현상이 일어나기 때문에 표면의 거칠기(roughness)가 증가하는 문제점이 있음을 확인하였다. 이 결과로부터, 본 발명의 자외선 ALD공정은 상온에서도 수행될 수 있어 기존 ALD 공정의 이러한 문제점들을 극복하여 저온에서 고품질의 박막을 제조할 수 있음을 알 수 있다.
도 7에 나타낸 바와 같이, 스크래치 실험 결과를 보면 25℃에서 자외선 ALD공정에 의해 제조된 TiO2 박막은 하중이 14N 정도 될 때까지 실리콘 기판 표면과 박막 사이에 균열이 일어나지 않았으나, 기존 ALD를 이용하여 350℃에서 제조된 TiO2 박막은 4N 정도에서 벌써 실리콘 기판 표면과 박막 사이에 균열이 일어나 박막이 파괴되어 실리콘 기판이 드러나기 시작함을 알 수 있다. 이 결과로부터 자외선 ALD 공정에 의해 제조된 박막이 기판 표면과 더욱 강하게 결합되어 있음을 알 수 있다.
[비교예 2]
자외선 ALD와 기존 ALD 공정에 의해 제조된 ZrO2 박막의 비교
자외선 ALD와 기존 ALD 공정을 비교하기 위해, 실시예 2와 같은 방법으로 25℃에서 300 주기의 공정 반복으로 얻어진 ZrO2 박막과 자외선을 사용하지 않고 기존의 ALD 공정을 이용하여 100~350℃에서 300 주기의 공정 반복으로 얻어진 ZrO2 박막을 제조하였다.
두 공정에서 얻어진 박막의 두께를 TEM으로 측정하여 공정 주기의 반복에 따른 두께의 변화와 증착 속도를 비교하였으며(도 8), 두 박막의 표면 성상을 분석, 비교하기 위해 각각의 AFM 사진을 얻었다(도 9).
또한, 기판 표면과 박막과의 결합력(adhesion)을 측정하기 위해 상기의 두 박막에 대하여 비교예 1과 같은 방법으로 스크래치 실험(scratch test)을 수행하였다. 이 때 각각의 박막은 공정 주기를 1000회 반복하여 제조되었다.
도 8에 나타낸 바와 같이, 280℃ 이하에서 기존 ALD 공정의 증착속도는 25℃에서의 자외선 ALD 공정보다 훨씬 느리게 나타났다. 자외선 ALD를 이용한 ZrO2 박막 제조에 있어 25℃에서의 증착속도가 기존 ALD 공정에 있어 300℃에서의 증착 속도와 같았다. 결과적으로, 저온에서 자외선 ALD 공정의 증착속도가 기존의 고온 ALD공정보다 훨씬 빠름을 알 수 있다.
도 9에 나타낸 바와 같이, 자외선 ALD를 이용하여 25℃에서 제조된 ZrO2 박막과 기존 ALD를 이용하여 300℃에서 제조된 ZrO2 박막의 AFM 사진을 비교해 보면, 자외선 ALD 공정에 제조된 ZrO2 박막의 표면이 기존 ALD 공정을 이용해 제조된 ZrO2 박막보다 훨씬 매끄럽고 조밀함을 확인하였다.
스크래치 실험 결과, 25℃에서 자외선 ALD공정에 의해 제조된 ZrO2 박막은 30N 정도까지 실리콘 기판 표면과 박막 사이에 균열이 일어나지 않았으나, 기존 ALD를 이용하여 300℃에서 제조된 ZrO2 박막은 4N 정도에서 벌써 실리콘 기판 표면과 박막 사이에 균열이 일어나 실리콘 기판이 드러나기 시작하였다. 이 결과로부터 자외선 ALD 공정에 의해 제조된 박막이 기판 표면과 더욱 강하게 결합되어 있음을 알 수 있다.
[비교예 3]
자외선 ALD와 기존 ALD 공정에 의해 제조된 박막의 단차피복성 비교
트렌치의 깊이가 2㎛, 넓이가 100nm인 실리콘 트렌치웨이퍼(trench wafer)를 기판으로 사용하여 그 표면에 실험예 2의 방법으로 25℃에서 공정 주기를 100회 반복하여 자외선 ALD를 이용하여 ZrO2 박막을 형성하였다. 비교를 위해 300℃에서 실리콘 트렌치웨이퍼 표면에 자외선을 조사하지 않는 기존 ALD를 이용하여 공정 주기를 100회 반복하여 ZrO2 박막을 형성하였다. 각 박막을 FE-SEM(Field Emission Scanning Electron Microscope, 전계방출주사전자현미경)으로 분석하여 실리콘 기판의 트렌치에 증착된 박막의 상태를 비교하였다(도 10).
도 10에 도시된 바와 같이, 300℃에서 기존 ALD 공정에 의해 ZrO2 박막을 증착한 경우 기판의 트렌치 내부보다 트렌치 입구에 ZrO2 박막이 두껍게 형성되어 전체적으로 불균일하게 ZrO2 박막이 형성되었다. 반면에, 25℃에서 자외선 ALD 공정에 의한 경우 트렌치 입구와 내부에 균일하게 ZrO2 박막이 형성되었음을 확인할 수 있다. 이러한 결과는 본 발명에 따른 저온 자외선 ALD 공정이 기존 ALD 공정보다 우수한 단차 피복성(step coverage)을 나타냄을 알 수 있다.
본 발명은 원자층 증착과정에서 자외선을 조사하여 원자층 형성의 화학 반응을 촉진시켜 기존 원자층 증착 공정보다 저온에서의 증착 속도를 증대시키고, 단차 피복성, 막의 균일도 및 기판과 박막 간의 결합력을 증가시킴으로써 고품위의 나노 두께 박막을 제조할 수 있고, 박막 제조 공정의 시간과 비용 절감의 효과를 가져올 수 있다.
도 1은 본 발명에 의한 자외선 원자 증착법을 이용한 박막 제조 공정을 나타내는 흐름도이다.
도 2는 본 발명에 의한 자외선 원자층 증착법을 이용한 박막 제조 방법에 있어서 기본 공정 주기(cycle)를 나타낸 도면이다.
도 3은 본 발명의 실험예 1에 의한 TiO2 박막 제조에 있어서 공정 주기(cycle)의 반복에 따른 박막 두께의 변화를 나타낸 그래프이다.
도 4는 본 발명의 실험예 2에 의한 ZrO2 박막 제조에 있어서 공정 주기(cycle)의 반복에 따른 박막 두께의 변화를 나타낸 그래프이다.
도 5는 본 발명의 비교예 1에 있어서 박막 제조 공정의 온도 변화에 따른 TiO2 박막들의 두께 변화를 비교하여 도시한 그래프이다.
도 6a와 6b는 본 발명의 비교예 1에 의해 제조된 TiO2 박막들의 표면 성상(morphology)을 나타내는 원자힘 현미경(Atomic Force Microscope, AFM) 사진들을 도시한 도면들이다.
도 7a와 7b는 본 발명의 비교예 1에 의해 제조된 TiO2 박막들의 실리콘 기판 표면과의 결합력을 측정하기 위한 스크래치 실험(scratch test)결과를 나타낸 도면들이다.
도 8은 본 발명의 비교예 2에 있어서 박막 제조 공정의 온도 변화에 따른 ZrO2 박막들의 두께 변화를 비교하여 도시한 그래프이다.
도 9a와 9b는 본 발명의 비교예 2에 의해 제조된 ZrO2 박막들의 표면 성상을 나타내는 AFM 사진들을 도시한 도면들이다.
도 10은 본 발명의 비교예 3에 의한 실리콘 트렌치웨이퍼 기판에 형성된 ZrO2 박막들의 FE-SEM(Field Emission Scanning Electron Microscope, 전계방출주사전자현미경) 사진을 도시한 도면들이다.
Claims (8)
- (가) 챔버 내에 기판을 로딩하고 제1 반응물의 기체를 펄스 형태로 주입하여 기판 표면에 화학 흡착시켜 제1 반응물의 단원자층을 형성하는 단계;(나) 상기 챔버 내로 불활성 기체를 펄스 형태로 주입하여 1차 퍼지하는 단계;(다) 상기 기판 위로 자외선을 조사하면서 챔버 내로 제2 반응물의 기체를 펄스 형태로 주입하여 상기 제1 반응물의 층에 제2 반응물을 화학 흡착시켜 두 반응물의 화학 반응에 의하여 원자층 단위의 박막을 형성하는 단계; 및(라) 상기 챔버 내로 불활성 기체를 펄스 형태로 주입하여 2차 퍼지하는 단계를 포함하여 이루어지는 것을 특징으로 하는 자외선 원자층 증착법을 이용한 박막 제조 방법.
- 제1항에 있어서, 상기 (가), (나), (다) 및 (라) 단계를 반복적으로 수행하여 박막의 두께를 조절하는 것을 특징으로 하는 자외선 원자층 증착법을 이용한 박막 제조 방법.
- 제1항에 있어서, 상기 챔버 내의 공정 온도는 20℃~100℃, 공정 압력은 0.1mTorr~50Torr 범위에서 일정하게 유지하는 것을 특징으로 하는 자외선 원자층 증착법을 이용한 박막 제조 방법.
- 제1항에 있어서, 각 단계의 공정 시간을 0.1초~40초 범위로 하는 것을 특징으로 하는 자외선 원자층 증착법을 이용한 박막 제조 방법.
- 제1항에 있어서, 상기 (다) 단계에서 조사되는 자외선의 파장은 200nm~300nm인 것을 특징으로 하는 자외선 원자층 증착법을 이용한 박막 제조 방법.
- 제1항에 있어서, 상기 기판은 실리콘웨이퍼, 용융 실리카, 유리판 중 어느 하나 인 것을 특징으로 하는 자외선 원자층 증착법을 이용한 박막 제조 방법.
- 제1항에 있어서, 상기 박막은 단원자 박막, 단원자 산화물, 복합 산화물, 단원자 질화물 및 복합 질화물로 이루어진 일군에서 선택된 어느 하나로 형성되는 것을 특징으로 하는 자외선 원자층 증착법을 이용한 박막 제조 방법.
- 제7항에 있어서, 상기 단원자 산화물은 TiO2, SnO2, ZnO 및 ZrO2로 이루어진 일군에서 선택된 어느 하나인 것을 특징으로 자외선 원자층 증착법을 이용한 박막 제조 방법.
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