#2

Hong-Sub Lee
Basic Experiment for Materials
(Basic of electronics and materials)
Assistant Professor,
Department of Advanced Materials Engineering for
Information and Electronics, Kyung Hee University
e-mail: h.s.lee@Khu.ac.kr

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Thin Film Deposition:
- Thermal Evaporation
- Atomic Layer Deposition (ALD)

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 Thin Film Deposition

박막제조 기술은 과학기술의 기반이 되는 기술이며 따라서 많은 연구가 박막을 이용하여 이루어지고 있다.
박막제조 기술은 모재의 성능을 향상시키거나 모재에 부가적인 기능을 부여하는 표면처리 기술에 바탕을 두고
있다.
표면처리는 크게 박막제조와 표면개질로 구분되는데 박막제조는 모재의 표면 에 다른 물질을 코팅하는 것을
의미하며 표면개질은 이온빔 조사 등을 통해 모재의 표면을 변화시켜 성능을 향상 시키는 기술을 의미한다.
박막제조 기술 중 진공증착은 물리증착(Physical Vapor Deposition; PVD)과 화학증착(Chemical Vapor Deposition;
CVD)으로 구분되는데 1950년대 이후 전자기 재료를 중심으로 응용이 시작되어 비약적인 발전을 이루었으며
현재는 반도체나 디스플레이를 비롯한 각종 소재의 표면처리에 다양하 게 응용되고 있다.
진공증착 공정 연구는 주로 피막의 조직제어 연구가 주를 이루었는데, 1980년대까지는 증착변수(기판온도,
증착 압력)에 의한 조직제어 연구가 활발히 이루어져 소위 조직대 모델(Structure Zone Model; SZM)이 완성되었다.

Ex: TiO2 표면개질

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 Thin Film Growth

• Thin film deposition

• Physical vapor deposition
• Thermal evaporation
• E-beam evaporation
• Sputter deposition
• Pulsed laser deposition
• Chemical vapor deposition
• Chemical Vapor Deposition
• Atomic Layer Deposition
• Chemical solution deposition (spin coating)

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 Structure Zone Model (SZM) of Thornton
박막의 형성 과정은 과포화 증기로부터 물질의 물리적인 응축현상이며, 응축은 가스 상에서 액체 혹은 고체상으로의
변화를 의미함. 열역학적으로 응축이 일어나기 위해서는 가스 상에서 박막물질의 분압이 그 온도에서 응축상 내의 증
기압 보다 높거나 같아야 함. 그러나 이 조건은 응축이 같은 물질의 기판 위나 이미 박막 물질이 응축된 기판 위에서 일
어날 경우에만 성립된다. 일반적으로 기판은 박막물질과 다른 화학적 성질을 가지며, 이러한 조건 하에서는 가스 원자
들이 기판 위에 흡착 되었으나 아직 다른 흡착원자들과 결합되지 않은 상태가 고려되어야 한다. 응축은 흡착된 원자들
의 결합을 통한 작은 입자덩어리들의 형성에 의해 시작된다. 이 입자 덩어리들을 nuclei라 부르며, 이 입자덩어리들의
형성 과정을 핵생성(nucleation) 이라 한다.

일반적으로 핵생성과 성장은 박막형성동안 동시에

일어난다. Nuclei의 형성은 흡착원자(adatom)들이
re-evaporation 되기 전에 표면에서 충분히 확산되어
nucleus에 도달할 수 있어야 할 뿐 아니라, 안정적인
nuclei가 형성된 후, 기판 위에 형성된 island의
형성을 야기하기 위해 충분한 표면 이동도가
요구됨. 박막의 용융온도 Tm에 대한 기판온도 Ts

출처: https://www.bnl.gov/nsls2/sciOps/chemSci/growth.asp Semicon.

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 Structure Zone Model (SZM) of Thornton

• Zone 1 (Ts/Tm＜0.3) : 흡착원자의 표면 확산이

무시 될 수 있기 때문에 대부분의 입사이온들
은 박막의 높은 위치에 흡착, tapered column 과
column들 사이의 공간들로 구성되며, column은
빈약한 결정성을 갖거나, 비정질이다.

• Zone 2 (0.3＜Ts/Tm＜0.5) : 흡착원자들의 표면

확산이 충분히 높기 때문에 뚜렷한 grain
boundary를 가진 columnar, platelet, whisker
grain들로 이루어지며, grain size는 Ts/Tm의 증
가와 함께 증가하는 경향을 보여준다.

• Zone 3 (Ts/Tm>0.5): 구조의 성장은 grain 내에서

흡착원자의 확산이 박막성장의 중요한 구조로
작용하며, 낮은 결함밀도를 가진 큰 grain들로
구성된다. Zone Ⅲ 구조의 박막은 높은 온도에
서 재 결정화에 의해 응력에 자유로우며 낮은
잔류응력 및 매우 매끈한 표면을 가지는 박막
• Zone T 구조는 zone 1의 구조와 비슷한 defected column등으로 구성 되지만, 이 성장된다.
column들 사이와 column내에 매우 적은 수의 공간들을 포함. Semicon.
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 Comparison of typical thin film deposition technology

Physical vapor deposition

Pulse laser deposition (PLD)

Molecular beam epitaxy (MBE)
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 Vacuum
진공 영역 진공도 범위 적용되는 공정 진공펌프의 기종
저진공 건식 로터리 베인 펌프,
대기압 ~ 1 Torr 진공성형, 진공포장
Rough Vacuum 급유식 로터리 베인 펌프
중진공 다단식 로타리 베인 펌프, 루츠펌프, 피스
1 Torr ~ 10-3 Torr 진공건조, 진공함침, 진공증류, 진공소결
Fine Vacuum 톤 펌프
고진공 확산펌프, 터보 분자 펌프,
10-3 Torr ~10-7 Torr 진공코팅, 전자 현미경
High Vacuum 흡착펌프, 저온 냉각 펌프,
초고진공 물리 실험 장치 터보 분자 펌프, 저온 냉각펌프,
10-7 Torr 이하
Ultra-High Vacuum (ex: X-ray photoemission spectroscopy) 확산펌프 , 흡착 펌프

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PVD vacuum system

Chamber

Rotary
pump

Turbo
pump

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 Evaporation

• Load the source material to be deposited Substrate

Film
(evaporant) into the container (crucible)
• Heat the source to high temperature
• Source material evaporates Evaporant
• Evaporant vapor transports to and Impinges Vapor
on the surface of the substrate
• Evaporant condenses on and is adsorbed by Current
Crucible (energy source)
the surface

출처: https://www.mrsec.harvard.edu/education/ap298r2004/Erli%20chenFabrication%20II%20-%20Deposition-1.pdf Semicon.

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 Deposition rate

Mass Deposition Rate per unit area of source surface: Substrate

 M  2 cos θ cos ϕ 1 (P (T ) − P )
Rm = Cm   r
 
e
T
r2
θ ϕ

Pe

Source (K-Cell)

출처: https://www.mrsec.harvard.edu/education/ap298r2004/Erli%20chenFabrication%20II%20-%20Deposition-1.pdf Semicon.

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 Uniform Coating

출처: https://www.mrsec.harvard.edu/education/ap298r2004/Erli%20chenFabrication%20II%20-%20Deposition-1.pdf Semicon.

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https://youtu.be/qIn8vPIKV54 Semicon.
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 Uniformity on a Flat Surface

출처: https://www.mrsec.harvard.edu/education/ap298r2004/Erli%20chenFabrication%20II%20-%20Deposition-1.pdf Semicon.

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 Uniformity Requirement on a Flat Surface

출처: https://www.mrsec.harvard.edu/education/ap298r2004/Erli%20chenFabrication%20II%20-%20Deposition-1.pdf Semicon.

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 Heating Method – Thermal (Resist Heater)

Molybdenum or Tungsten boat

Cr coated Tungsten Rod

출처: https://www.mrsec.harvard.edu/education/ap298r2004/Erli%20chenFabrication%20II%20-%20Deposition-1.pdf Semicon.

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 Heating Method – e-Beam Heater

e-
Electron Beam

Crucible Magnetic Field

Focusing
Aperture
Evaporant Evaporant (beam focusing
& positioning)

Cathode Filament

Advantage of E-Beam Evaporation:

Water Cooled Rotary Copper Hearth
(Sequential Deposition) Very low container contamination

출처: https://www.mrsec.harvard.edu/education/ap298r2004/Erli%20chenFabrication%20II%20-%20Deposition-1.pdf Semicon.

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 Comparison

Stoichiometrical Problem of Evaporation

• Compound material breaks down at high temperature
• Each component has different vapor pressure, therefore different deposition
rate, resulting in a film with different stoichiometry compared to the source

출처: https://www.mrsec.harvard.edu/education/ap298r2004/Erli%20chenFabrication%20II%20-%20Deposition-1.pdf Semicon.

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 Typical Boat/Crucible Material

출처: https://www.mrsec.harvard.edu/education/ap298r2004/Erli%20chenFabrication%20II%20-%20Deposition-1.pdf Semicon.

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 Comparison between Evaporation and Sputtering

출처: https://www.mrsec.harvard.edu/education/ap298r2004/Erli%20chenFabrication%20II%20-%20Deposition-1.pdf Semicon.

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 Thin Film Deposition

• Thin film deposition

• Physical vapor deposition
• Sputter deposition
• Thermal evaporation
• E-beam evaporation
• Pulsed laser deposition
• Chemical vapor deposition
• Chemical Vapor Deposition
• Atomic Layer Deposition
• Chemical solution deposition (spin coating)

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 Definition of ALD

• ALD is a method of applying thin films to various substrates with atomic scale
precision.
• Similar in chemistry to chemical vapor deposition (CVD), except that the ALD
reaction breaks the CVD reaction into two half-reactions, keeping the precursor
materials separate during the reaction.
• ALD film growth is self-limited and based on surface reactions, which makes
achieving atomic scale deposition control possible.
• By keeping the precursors separate throughout the coating process, atomic layer
thickness control of film grown can be obtained as fine as atomic/molecular scale
per monolayer.
• Introduced in 1974 by Dr. Tuomo Suntola and co-workers in Finland to improve the
quality of ZnS films used in electroluminescent displays.
• Recently, it turned out that ALD method also produces outstanding dielectric layers
and attracted semiconductor industries for making High-K dielectric materials.

Ref: "Atomic Layer Deposition," Wikipedia: The Free Encyclopedia, Wikimedia Foundation, 24 April 06.
<http://en.wikipedia.org/wiki/Atomic_Layer_Deposition>.

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 ALD Process and Equipment

• Releases sequential precursor gas pulses to

deposit a film one layer at a time on the
substrate.
• The precursor gas is introduced into the process chamber and produces a
monolayer of gas on the wafer surface. A second precursor of gas is then
introduced into the chamber reacting with the first precursor to produce a
monolayer of film on the wafer surface.
Two fundamental mechanisms:
 Chemisorption saturation process
 Sequential surface chemical reaction process
• Example: ALD cycle for Al2O3 deposition
• Since each pair of gas pulses (one cycle) produces exactly one monolayer
of film, the thickness of the resulting film may be precisely controlled by the
number of deposition cycles.

Ref: A. Knop–Gericke, "Preparation of Model Systems by Physical Methods," a lecture given at Modern Methods in Heterogeneous
Catalysis Research Lecture Series, Fritz Haber Institute of the Max Planck Society. 24 April 06.
<http://w3.rz-berlin.mpg.de/%7Ejentoft/lehre/catalysis0405.html>.
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 ALD Process and Equipment

• Releases sequential precursor gas pulses to deposit a film one layer at a time.

• A first precursor gas is introduced into the process

chamber and produces a monolayer of gas on the
wafer surface. Then a second precursor of gas is
introduced into the chamber reacting with the first
precursor to produce a monolayer of film on the
wafer surface.
Two fundamental mechanisms:
 Chemisorption saturation process
 Sequential surface chemical reaction process
• Example: ALD cycle for Al2O3 deposition
• Since each pair of gas pulses (one cycle) produces exactly one monolayer of film, the
thickness of the resulting film may be precisely controlled by the number of deposition
cycles.

Ref: A. Knop–Gericke, "Preparation of Model Systems by Physical Methods," a lecture given at Modern Methods in Heterogeneous
Catalysis Research Lecture Series, Fritz Haber Institute of the Max Planck Society. 24 April 06.
<http://w3.rz-berlin.mpg.de/%7Ejentoft/lehre/catalysis0405.html>.
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 ALD Process and Equipment

• Releases sequential precursor gas pulses to deposit a film one layer at a time.
• A first precursor gas is introduced into the process chamber and produces a monolayer of
gas on the wafer surface. Then a second precursor of gas is introduced into the chamber
reacting with the first precursor to produce a monolayer of film on the wafer surface.
Two fundamental mechanisms:
 Chemisorption saturation process
 Sequential surface chemical reaction process

• Example: ALD cycle for Al2O3 deposition (Step 1a)

Diethyl zinc

Trimethylaluminum
(TMA)
Ref: "Atomic Layer Deposition," Cambridge Nano Tech Inc., 24 April 06. <http://www.cambridgenanotech.com/>.
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 ALD Process and Equipment

• Releases sequential precursor gas pulses to deposit a film one layer at a time.
• A first precursor gas is introduced into the process chamber and produces a monolayer of
gas on the wafer surface. Then a second precursor of gas is introduced into the chamber
reacting with the first precursor to produce a monolayer of film on the wafer surface.
Two fundamental mechanisms:
 Chemisorption saturation process
 Sequential surface chemical reaction process

• Example: ALD cycle for Al2O3 deposition (Step 1b)

Ref: "Atomic Layer Deposition," Cambridge Nano Tech Inc., 24 April 06. <http://www.cambridgenanotech.com/>.
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 ALD Process and Equipment

• Releases sequential precursor gas pulses to deposit a film one layer at a time.
• A first precursor gas is introduced into the process chamber and produces a monolayer of
gas on the wafer surface. Then a second precursor of gas is introduced into the chamber
reacting with the first precursor to produce a monolayer of film on the wafer surface.
Two fundamental mechanisms:
 Chemisorption saturation process
 Sequential surface chemical reaction process

• Example: ALD cycle for Al2O3 deposition (Step 1c)

Ref: "Atomic Layer Deposition," Cambridge Nano Tech Inc., 24 April 06. <http://www.cambridgenanotech.com/>.
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 ALD Process and Equipment

• Releases sequential precursor gas pulses to deposit a film one layer at a time.
• A first precursor gas is introduced into the process chamber and produces a monolayer of
gas on the wafer surface. Then a second precursor of gas is introduced into the chamber
reacting with the first precursor to produce a monolayer of film on the wafer surface.
Two fundamental mechanisms:
 Chemisorption saturation process
 Sequential surface chemical reaction process

• Example: ALD cycle for Al2O3 deposition (Step 2a)

Ref: "Atomic Layer Deposition," Cambridge Nano Tech Inc., 24 April 06. <http://www.cambridgenanotech.com/>.
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 ALD Process and Equipment

• Releases sequential precursor gas pulses to deposit a film one layer at a time.
• A first precursor gas is introduced into the process chamber and produces a monolayer of
gas on the wafer surface. Then a second precursor of gas is introduced into the chamber
reacting with the first precursor to produce a monolayer of film on the wafer surface.
Two fundamental mechanisms:
 Chemisorption saturation process
 Sequential surface chemical reaction process

• Example: ALD cycle for Al2O3 deposition (Step 2b)

Ref: "Atomic Layer Deposition," Cambridge Nano Tech Inc., 24 April 06. <http://www.cambridgenanotech.com/>.
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 ALD Process and Equipment

• Releases sequential precursor gas pulses to deposit a film one layer at a time.
• A first precursor gas is introduced into the process chamber and produces a monolayer of
gas on the wafer surface. Then a second precursor of gas is introduced into the chamber
reacting with the first precursor to produce a monolayer of film on the wafer surface.
Two fundamental mechanisms:
 Chemisorption saturation process
 Sequential surface chemical reaction process

• Example: ALD cycle for Al2O3 deposition (Step 2c)

Ref: "Atomic Layer Deposition," Cambridge Nano Tech Inc., 24 April 06. <http://www.cambridgenanotech.com/>.
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 ALD Process and Equipment
https://www.youtube.com/watch?v=XMda8TXLIFk
• Releases sequential precursor gas pulses to deposit a film one layer at a time.
• A first precursor gas is introduced into the process chamber and produces a monolayer of
gas on the wafer surface. Then a second precursor of gas is introduced into the chamber
reacting with the first precursor to produce a monolayer of film on the wafer surface.
Two fundamental mechanisms:
 Chemisorption saturation process
 Sequential surface chemical reaction process

• Example: ALD cycle for Al2O3 deposition (after 3 cycles)

Ref: "Atomic Layer Deposition," Cambridge Nano Tech Inc., 24 April 06. <http://www.cambridgenanotech.com/>.
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 ALD Process and Equipment

• Releases sequential precursor gas pulses to deposit a film one layer at a time.
• A first precursor gas is introduced into the process chamber and produces a monolayer of gas
on the wafer surface. Then a second precursor of gas is introduced into the chamber
reacting with the first precursor to produce a monolayer of film on the wafer surface.
Two fundamental mechanisms:
 Chemisorption saturation process
 Sequential surface chemical reaction process
• Example: ALD cycle for Al2O3 deposition

• Since each pair of gas pulses

(one cycle) produces exactly one
monolayer of film, the thickness
of the resulting film may be
precisely controlled by the
number of deposition cycles.

Step coverage and deposition rate Vs.

Ref: "Technology Backgrounder: Atomic Layer Deposition," IC Knowledge LLC, 24 April 06. deposition technique.
<www.icknowledge.com/misc_technology/Atomic%20Layer%20Deposition%20Briefing.pdf>.

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 ALD Process and Equipment

Four main types of ALD reactors

• Closed system chambers (most common)
 The reaction chamber walls are designed to effect the transport of
the precursors.

Schematic of
a closed ALD
system

Ref: "Technology Backgrounder: Atomic Layer Deposition," IC Knowledge LLC, 24 April 06.
<www.icknowledge.com/misc_technology/Atomic%20Layer%20Deposition%20Briefing.pdf>.

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 ALD Process and Equipment

(N2 gas)

One cycle [1] [1]

Acceptable
temperature range
for deposition.

Process Temperature [1]

1 "Technology Backgrounder: Atomic Layer Deposition," IC Knowledge LLC, 24 April 06.
<www.icknowledge.com/misc_technology/Atomic%20Layer%20Deposition%20Briefing.pdf>.
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ALD Process and Equipment

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 ALD Applications

• High-K dielectrics for CMOS

• Reduces leakage current

• Uniformity
• Step coverage
• Growth rate

Candidates for High-K dielectrics

Film Precursors
Al2O3 Al(CH)3, H2O or O3
HfO2 HfCl4 or TEMAH, H2O
ZrO2 ZrCl4, H2O
Ref: "Intel's High-k/Metal Gate Announcement," Intel® Corporation. 26 April, 06.
<http://www.intel.com/technology/silicon/micron.htm#high>.

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 Scaling Challenges - Aspect Ratio

Cell Capacitor Structure at 1x nm DRAM

A/R “60”

A/R “6”

~70m
Lotte World DRAM
Source : WILEY-VCH Verlag GmbH & Co
Tower Cell

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 ALD Applications

• High-K dielectrics for CMOS

• Semiconductor memory (DRAM)

• Cu interconnect barrier
• Deposition in porous structures

All these applications take

advantage of uniformity,
conformal step coverage,
precise thickness control
of deposited films, which
can be achieved by ALD
deposition method.
Step coverage and deposition rate Vs.
deposition technique.
Ref: "Technology Backgrounder: Atomic Layer Deposition," IC Knowledge LLC, 24 April 06.
<www.icknowledge.com/misc_technology/Atomic%20Layer%20Deposition%20Briefing.pdf>.

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 ALD Character

• Uniformity ?
• Step coverage ?
• Growth rate ?
• Hydrogen doping ?
• Precursor dependency ?

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Photolithography

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 Lithography

• 설계된 도면에 맞춰 원판 mask 를 제작하고 mask에 빛을 조사하여 기판위에 도포한 감광제에

정확한 크기로 정확한 위치에 패턴을 형성하는 공정기술
• 반도체 공정 중 가장 정밀을 요하는 공정 (가장 고가의 장비)
• Lithography 종류
• Photolithography (UV) : high throughput Motto of Lithography
• Extreme ultraviolet (EUV) lithography  Faster (throughput),
• e-beam lithography  Smaller (integration),
 More accurate (Size/position control)
• x-ray lithography
• Ion beam lithography

Glass or quartz Positive PR

UV
photomask
Substrate
Chrome

Substrate Substrate Substrate

Negative PR

Cleaning Photoresist coating Align & exposure Development Substrate

& soft bake
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 Lithography
Mask aligner

Spin coater Hot plate

- Photoresist (PR)
- Developer Glass or quartz Positive PR
- PR remover UV
photomask
Substrate
Chrome

Substrate Substrate Substrate

Negative PR

Cleaning Photoresist coating Align & exposure Development Substrate

& soft bake
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 Cleanroom

Clean room 등급 (class)

1. English system:
공기 중 청정실의 입방 피트 당 0.5㎛ 또는 그 이상의 크기를 갖는 particle 수
예) Class 100 청정실 (English system)은 100 particles/ft3
2. Metric system : 공기 중 청정실의 입방 미터 당 0.5㎛ 또는 그 이상의 크기를 갖는particle 수, 로그(log)로 나타냄
예) Class M 3.5 청정실(metric system)은 103.5 또는 3500 particles/m3
Semicon.
KHU Mater.
Charact.
Photolithography 공정 시 particle의 문제점

Semicon.
KHU Mater.
Charact.
 박막 패턴

Etch-back Lift-off

PR의 두께는 박막의 두께보다 3배 이상이어야 함

Semicon.
KHU Mater.
Charact.
 Etching
습식 식각 (wet etching) 건식 식각 (dry etching)
방법 화학적 반응 (용액) 물리적, 화학적 반응 (gas)
환경/장비 대기, bath 진공, chamber
장점 1) 저비용, 쉬운과정 1) 정확성이 좋다
2) 식각속도 (etch rate) 빠름 2) 미세 패터닝 가능
3) 선택비 (selectivity) 좋음
단점 1) 비교적 정확성이 안좋음 1) 고비용, 어려운 과정
2) 웨이퍼 오염 위험 (화학물질) 2) 낮은 처리량 (low throughput)
3) PR 밑부분 식각 3) 선택비 (selectivity) 나쁨

방향성

등방성 etching 이방성 etching

그림출처: IT CookBook, 현대 반도체 소자 공학 Semicon.

KHU Mater.
Charact.
 Dry etching
 Plasma etch (chemical etch)
Plasma를 생성하는 과정에서 나오는 radical을 사용하여 etching하는 것으로 화학반응이 일어나서 dry
chemical etching, plasma etching이라 함. 화학 반응이기 때문에 등방성 etching이 일어나고 전기적
damage가 없음. 높은 selectivity를 가지며 높은 etch rate를 가짐.

 Sputter etch (physical etch)

Plasma를 생성하면서 만들어진 Ar 이온을 이용하여 식각 대상의 표면을 때려 뜯어내는 방식으로 ion
milling 이라고도 함. Physical etching 으로 이방성을 띄며 selectivity와 etch rate이 낮음.

 Reactive ion etching (RIE, chemical & physical etching)

Dry etch 에서 chemical 방식과 physical 방식을 혼합하여 사용하는 방식-> RIE
Physical etch의 장점인 이방성과 chemical etch의 장점인 selectivity와 etch rate 가 높다는 것을 혼합한
방법으로 두 종류의 방식 중 비율을 조절하여 특성에 대해서 선택적으로 고를 수 있음.
Isotropic과 selectivity, etch rate는 서로 trade off 관계에 있음.
Semicon.
KHU Mater.
Charact.
 SiO2

• SiO2 층은 mask로 사용될 수 있음

• Drain, source의 n+ 또는 p+ 영역 형성 시

Implantation

[그림 3-1] 실리콘 소자 제조 공정에서 몇 가지 기본 단계. (a) 실리콘 산화,

(b) 선택적 산화물 제거, (c) 도펀트 원자 주입, (d) 실리콘 내부로 도펀트 원자 확산

그림출처: IT CookBook, 현대 반도체 소자 공학 Semicon.

KHU Mater.
Charact.
 Photolithography process

Hexa Methyl Di Silazane (HDMS)

or bake (125oC ~ 200oC)

Light intensity & time

RPM & time temperature & time

temperature & time temperature & time Semicon.

KHU Mater.
Charact.
 Exposure

음영인쇄법 (Shadow printing) 접촉인쇄법 (Contact printing)

노광 방법 근접인쇄법 (Proximity printing)
투사형인쇄법 (Projection printing)

Step-and-repeat printing

projection

Semicon.
KHU Mater.
Charact.