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Transcript of To Start this Seminar - chemilab.comchemilab.com/mtxa/seminar/20120323/2.pdf · 4 Analysis ,...
1
Analysis , Development and Enhancement
서론서론서론서론 및및및및 기계적기계적기계적기계적 물성물성물성물성 측정측정측정측정 현황현황현황현황.(.(.(.(원리와원리와원리와원리와 응용응용응용응용))))
f|Å \Ç VâÄf|Å \Ç VâÄf|Å \Ç VâÄf|Å \Ç VâÄ
Analysis , Development and Enhancement
1. Organic Materials(Polymers)에 대한 관점
2. Vision은 깊게, Touch는 넓게.유기물질은 보이는 현상과는 다른 화학적 물리적 조성에의한 변수가 매우 다양하고, 환경(온/습도)에 의한 변화가시간에 따라 동적으로 결정됩니다.
3. 측정 기구와 측정 변수의 한계는 분명히 다르므로 측정 기구의 선택은 신중해야 합니다.
4. (사용효율/장비 가격) X 100 = 100% ?????
To Start this Seminar
2
Analysis , Development and Enhancement
MEMS(Micro Electro Mechanic System) & NEMS(Nano Electro Mechanic System)
- MEMS : Micrometer, g(mg) 수준의 길이, 하중을 조절, 측정, 구성할 수 있는 전자 기계 체계.- NEMS : Nanometer, ug(ng) 수준의 길이, 하중을 조절, 측정, 구성할 수 있는 전자 기계 체계.
NEMSNEMSNEMSNEMS
(nm, ug, ng)
MEMSMEMSMEMSMEMS
(um, g, mg)
MKS/CGS
(cm, mm, kg, g)
사용 및 요구 현황(계측 및 가공 장치 분포)
투자 및 연구 현황
NEMSNEMSNEMSNEMS
(nm, ug, ng)
MEMSMEMSMEMSMEMS
(um, g, mg)
MKS/CGS
(Ton, m, cm, mm, kg, g)
후 가공/표면가공(코팅, 증착, 점착)소재 사용 분포
2012 -> 2013 NEEDS : Machine with mks/cgs unit-> MEMS -> NEMS
Analysis , Development and Enhancement
기능성~정밀도 정밀도
Milli Micro
Nano
Micro
Milli
Kilo & Milli
정밀도<기능성
길이와 하중의 정밀도 조절 및 측정• 제품의 규격 평가 관점 : 성능 > 정밀도 > 정확도
• 학술적 평가 관점 : 성능 > 정밀도 > 정확도
소재 구성 수준에 따른 재료 및 표면 측정 장치
• 나노 소재
•의료, 바이오
•전기 전자
•제약, 의료
•반도체/디스플레이
•치공구
•자동차, 기계
•반도체
•의료
•우주항공비접촉비접촉비접촉비접촉 표면표면표면표면 측정측정측정측정
Laser
CCDSEM
접촉식접촉식접촉식접촉식 표면표면표면표면 측정측정측정측정
3차원형상차원형상차원형상차원형상
표면조도표면조도표면조도표면조도
AFM
Nano UTMHysitron(USA)
CSM(SWISS)Micro Materials(UK)
Asylum Res.(USA)Nanovea(USA)
Miniature UTMTOPTAC2000TXi(UK)RheometerDMA
microTXA
3
Analysis , Development and Enhancement
측정 요구 규격에 따른 장비의 정밀도/대상 장비
표면
특성
표면
특성
표면
특성
표면
특성
kg, m
g, cm, mm
mg, um
ug, ng, nm
재질
특성
재질
특성
재질
특성
재질
특성
kg, m
g, cm, mm
mg, um
ug, ng, nm
측정측정측정측정 요구요구요구요구 Control 신뢰성신뢰성신뢰성신뢰성
kg, cm
g, mm, um
mg, nm
ug, ng, nm, pm
측정측정측정측정 요구요구요구요구 Control 신뢰성신뢰성신뢰성신뢰성
kg, cm
g, mm, um
mg, nm
ug, ng, nm, pm
대상대상대상대상 장비장비장비장비(응력응력응력응력 조절조절조절조절 측정측정측정측정 가능가능가능가능 장비에장비에장비에장비에 한함한함한함한함)
Micrometer
표면조도측정, 3차원 형상측정
기타 비접촉 측정 장비 : SEM, TEM, Laser Vision, CCD Vision, Ultra Sonic etc.
AFM
TOPTAC2000, Texture Analyzer
Rheometer
TMA, DMA, Dilatometer
microTXA
microTXA
UTM
Nano UTM
대상대상대상대상 장비장비장비장비(응력응력응력응력 조절조절조절조절 측정측정측정측정 가능가능가능가능 장비에장비에장비에장비에 한함한함한함한함)
Analysis , Development and Enhancement
표면재질분석표면재질분석표면재질분석표면재질분석방법방법방법방법
접촉식접촉식접촉식접촉식비접촉식비접촉식비접촉식비접촉식
광학적광학적광학적광학적분석분석분석분석전기전기전기전기////전자전자전자전자특성특성특성특성 분석분석분석분석
실측영상분석실측영상분석실측영상분석실측영상분석관능분석관능분석관능분석관능분석
점탄성점탄성점탄성점탄성 측정측정측정측정 방법방법방법방법
RheometerDMATexture analyzer(Toptac Series)UTM
표면표면표면표면 조도계조도계조도계조도계3333차원차원차원차원형상측정형상측정형상측정형상측정
점착력점착력점착력점착력측정측정측정측정
표면 조성분석 방법
AFMSEMEPMA/ESCAFTIR/ATR/Image scan
microTXA
4
Analysis , Development and Enhancement
표면분석 장치
SPM(Scanning Probe Microscope )의의의의 종류종류종류종류
- AFM ( Atomic Force Microscope ) : 부도체부도체부도체부도체 시료의시료의시료의시료의 측정측정측정측정 가능가능가능가능
- STM ( Scanning Tunneling microscope ) : 최초의최초의최초의최초의 원자원자원자원자 현미경현미경현미경현미경
- MFM ( Magnetic Force Microscope ) : 시료의시료의시료의시료의 자기력자기력자기력자기력 측정측정측정측정 가능가능가능가능
- LFM ( Lateral Force Microscope ) : 시료시료시료시료 표면의표면의표면의표면의 마찰력마찰력마찰력마찰력 측정측정측정측정 가능가능가능가능
- FMM ( Force Modulation Microscope ) : 시료의시료의시료의시료의 경도경도경도경도 측정측정측정측정 가능가능가능가능
- EFM ( Electrostatic Force Microscope ) : 시료의시료의시료의시료의 전기적전기적전기적전기적 특성특성특성특성 측정측정측정측정 가능가능가능가능
- SCM ( Scanning Capacitance Microscope ) : 시료의시료의시료의시료의 capacitance 측정측정측정측정 가능가능가능가능
Analysis , Development and Enhancement
ROUGHNESS MEASURING EQUIPMENT
ROUGHNESS (거칠기) 측정은 기재의 거친 정도를 측정함으로써 기재 거칠기를 측정하는 하나의 지수로써 사용된다. 기재가 심한 거칠기를 가질 경우 그로인한 CRACK/BROKEN이 예상된다.
ROUGHNESS SPEC LIMIT : MAX 0.3 um
PRINCIPLE OF MEASUREMENT : STYLUS METHOD (CONTACT)LASER METHOD (NON-CONTACT)
MEASURING RANGES : 0.25 mm
Measure LengthL
RmaxRa
Y
Xf(x)
Ra = 1/L∫ 0L
f(x) dx
용어 정리
• Rmax (최대 높이) : 한 기준 길이 안에서 단면 곡선의 최저점으로 부터 최고점까지의 높이
• Ra (중심선 평균 거칠기) : 한 기준 길이내의 산과 골의 높이를 기준선을 중심으로 평균하여 얻어지는 값
5
Analysis , Development and Enhancement
3차원 형상 측정기 개발 현황
(출처 덕인/KRISS 측정클럽 발표 자료)
Analysis , Development and Enhancement
PDP 격벽 3D 레이저(CCD) 구조 분석 사례
KRISS 측정클럽 발표자료
6
Analysis , Development and Enhancement
I wonder if some stress applied…As a view point of Material Viscoelasticity
And very small stress have applied…
Analysis , Development and Enhancement
Principles of Rheology (cont’d.)
Introduction to Viscoelasticity
• Most materials behave such that they have a combination of viscous and elastic
responses under stress or deformation.
• Materials behave in the linear manner, as described by Hooke and Newton, only
on a small scale in stress or deformation.
Most MaterialsIdeal Solid Ideal Liquid
Hooke Newton
7
Analysis , Development and Enhancement
Dynamic Mechanical Analyser의의의의 개념개념개념개념
점탄성의 측정
Analysis , Development and Enhancement
DMA Curves for Epoxy resin
8
Analysis , Development and Enhancement
Schematic Concept
56789
10
Glassy Rubbery
Cross-linked
Temperature
A
B
C
DE
Deformation
MolecularMotion
UnstrainedState
StrainedState
E D C B AHookeanBehavior
SecondTransition
PrimaryTransition Highly Visco Elastic Flow
(rubbery)(gamma) (beta) (alpha)
Bend &StretchBonds
SideGroups
MainChain
GradualMain Chain Large
Scale MobilityChain
Slipping
Increasing
F
FSecondaryDispersion
LocalizedMotion
R. Seymour, 1971
(melt)
34
11
Crystal-crystal slip
Crystalline Polymer
Analysis , Development and Enhancement
Common changes show as:
E’E’E’E’
tan tan tan tan δδδδ
MW MWD Crosslink Density Crystallinity
9
Analysis , Development and Enhancement
• Stress or Strain is varied sinusoidally
Oscillation Experiments of Rheometer
Stimulus
Response
phase lag, δ
• Separates Elastic and Viscous effects
• The modulus and Viscosity of Oscillation experiments are called Complex ModulusComplex ModulusComplex ModulusComplex Modulus and Complex Complex Complex Complex ViscosityViscosityViscosityViscosity.
Analysis , Development and Enhancement
Linear and Non-Linear Stress-Strain Behavior of Solids
Non-Linear RegionG = f(γ)
Linear RegionG is constant
σ
GGGG
1000.00.010000 0.10000 1.0000 10.000 100.00% strain
1000
1.000
10.00
100.0
100.0
0.01000
osc.
str
ess
(Pa)
Critical Strain γc
10
Analysis , Development and Enhancement
Newtonian and Non-NewtonianBehavior of Fluids
γ
σ
ηηηη
Newtonian Regionη Independent of γ
Non-Newtonian
Region
η = f(γ)
1.0001.000E-5 1.000E-4 1.000E-3 0.01000 0.1000
shear rate (1/s)
1.000E5
10000
η η η η (P
a.s)
1.000E5
1.000
10.00
100.0
1000
10000
σσ σσ(P
a)
Analysis , Development and Enhancement
Molecular functional groups vs. Thermal behavior
• 관능기의 가지가 크면 Tg, Tm 감소 – alpha, beta, gamma, delta transition• 관능기의 입체 규칙성 증가-결정도 증가-Tg, Tm 증가
• 관능기의 2차 결합(수소결합, Van der waals, chelation, etc.)-구조적 치밀도 증가-Tg, Tm 증가
• Dipole mement 존재(-Cl, -F)-치밀도 증가
• Benzene ring 포함-Tg, Tm 급상승
분자량 vs. Thermal behavior
• 분자량이 커지면 Tg, Tm 상승
• 일정 분자량 이상에서는 Tg, Tm 감소 가능성
• 분자량 분포가 좁을수록 Tg, Tm 상승
• 분자량 분포가 넓은 이유는 저분자량 영향
• 점도는 분자량에 직접 영향
Impurity vs. Thermal behavior
• 수분, 이온, low molecules, oligomer• 상호 작용이 없이 단순히 mix되어 있는 경우-Tg, Tm 감소- 구조적 혼란
• 상호 작용 존재-치밀도 상승-seed 역할
• Critical point 존재-임계함량 이상은 Tg, Tm 감소 및 구조 파괴
11
Analysis , Development and Enhancement
공중합체의 Tm, Tg
불규칙 공중합체는 결정성 파괴로 Tm 및 결정화도 감소 → 하나의 Tg
Block 및 Graft 공중합체는 미세 상분리 → 성분중합체 각각의 Tm, Tg 가능
고분자 혼합물(blend)의 Tg
상용성이 없으면 각각의 Tg
상용성이 있으면 중간에 하나의 Tg
용매, 가소제가 혼합되면 Tg 강하
일반적으로 Tg ; 1/2 ~ 2/3 Tm
간단하고 대칭성 구조이면,
입체 규칙성이 크면,
분자간 인력 또는 결합이 강하면,
곁가지가 없고 분자량이 크면,
높은 Tm 및 결정화도
사슬의 유동성이 작을수록(방향족 사슬등)
치환기의 크기와 극성이 클수록
분자량이 클수록 (어느 한계까지)
가교도가 증가할수록
높은 Tg
Analysis , Development and Enhancement
표면에의 응력 적용
90%~
Stress
50%~60%~
80%~
50%~60%~
80%~
Applied force of Total stress
95%~50%~30%~
Creep Recovery
Elastic Viscous
Values as a results:Length, Load
[Temperature/Time & Humidity]
12
Analysis , Development and Enhancement
Basic Parameters and UnitsBasic Parameters and UnitsBasic Parameters and UnitsBasic Parameters and Units
S.I. units = c.g.s. X 10
2222Stress = Force /Area [Pa, or dyn/cm ]
σσσσ = tensile stress, ττττ = shear stressStrain = Geometric Shape Change [no units]
εεεε = tensile strain, γγγγ = shear strainStrain or Shear Rate = Velocity Gradient or d(strain)/dt [1/s]
εεεε = tensile strain rate, γγγγ = shear strain rateModulus = Stress / Strain [Pa or dyn/cm ]
E = Youngs or Tensile, G = Shear ModulusCompliance = Strain / Stress [1/Pa or cm /dyn]
Typically denoted by JViscosity = Stress /Strain Rate [Pa.s or Poise]
Denoted by ηηηη
2222
........
2222
Analysis , Development and Enhancement
Viscoelasticity DefinedViscoelasticity DefinedViscoelasticity DefinedViscoelasticity Defined
Range of Material BehaviorSolid Like ---------- Liquid Like
Ideal Solid ----- Most Materials ----- Ideal FluidPurely Elastic ----- Viscoelastic ----- Purely Viscous
Viscoelasticity: Having both viscousand elastic properties
13
Analysis , Development and Enhancement
Response for Classical ExtremesResponse for Classical ExtremesResponse for Classical ExtremesResponse for Classical Extremes
Purely ElasticResponse
Hookean Solidσ = Eε or τ = Gγ
Purely ViscousResponse
Newtonian Liquidσ = ηγ
In the case of the classical extremes, all that matters is the values of stress, strain, strain rate. The response isindependent of the loading.
Spring Dashpot
Analysis , Development and Enhancement
At short times (high frequencies) the response is solid-like
At long times (low frequencies) the response is liquid-like
THE HISTORY OF LOADING IS CRUCIAL
Response for a Viscoelastic MaterialResponse for a Viscoelastic MaterialResponse for a Viscoelastic MaterialResponse for a Viscoelastic Material
14
Analysis , Development and Enhancement
TimeTimeTimeTime----Dependent Viscoelastic Behavior:Dependent Viscoelastic Behavior:Dependent Viscoelastic Behavior:Dependent Viscoelastic Behavior:Solid and Liquid Properties of "Silly Putty"
T is short [< 1s] T is long [24 hours]
Deborah Number [De] = τ / Τ
Analysis , Development and Enhancement
Old Testament Prophetess who said :"The Mountains Flowed before the Lord"
Everything Flows if you wait long enough!
Deborah Number, De - The ratio of a characteristic relaxation time of a material (τ) to a characteristic time of the relevant deformation process ( Τ ).
De = τ/Τ
TimeTimeTimeTime----dependent Viscoelastic Behavior:dependent Viscoelastic Behavior:dependent Viscoelastic Behavior:dependent Viscoelastic Behavior:The Deborah Number
15
Analysis , Development and Enhancement
Hookean elastic solid - τ is infiniteNewtonian Viscous Liquid - τ is zeroPolymer melts processing - τ may be a few seconds
High De Solid-like behaviorLow De Liquid-like behavior
IMPLICATION: Material can appear solid-like because1) it has a very long characteristic relaxation time or2) the relevant deformation process is very fast
The Deborah NumberThe Deborah NumberThe Deborah NumberThe Deborah Number
Analysis , Development and Enhancement
Stress Relaxation ExperimentStress Relaxation ExperimentStress Relaxation ExperimentStress Relaxation Experiment
Response of Classical Extremes
time
0
time
0
stress for t>0is constant
time
0
stress for t>0 is 0
Hookean Solid Newtonian Fluid
16
Analysis , Development and Enhancement
Stress Relaxation ExperimentStress Relaxation ExperimentStress Relaxation ExperimentStress Relaxation Experiment
Response of Material
For small deformations (strains within the linear region) the ratio of stress to strain is a function of time only.
This function is a material property known as the STRESS RELAXATION MODULUS, G(t)
G(t) = σ(t)/γ
Stress decreases with timestarting at some high value and decreasing to zero.
time
0
Analysis , Development and Enhancement
Stress is applied to sample instantaneously, t1, and held constant for a specific period of time. The strain is monitored as a function of time (γ(t) or ε(t)).The stress is reduced to zero, t2, and the strain is monitored as a function of time (γ(t) or ε(t)).
Creep Recovery ExperimentCreep Recovery ExperimentCreep Recovery ExperimentCreep Recovery Experiment
Str
ess
timet1 t2
17
Analysis , Development and Enhancement
Creep Recovery ExperimentCreep Recovery ExperimentCreep Recovery ExperimentCreep Recovery Experiment
Response of Classical Extremes
– Stain for t>t1 is constant– Strain for t >t2 is 0
time
time
time
– Stain rate for t>t1 is constant– Strain for t>t1 increase with time– Strain rate for t >t2 is 0
t2t1
t1 t2t2t1
Analysis , Development and EnhancementReference: Mark, J., et.al., Physical Properties of Polymers ,American Chemical Society, 1984, p. 102.
Creep Recovery Experiment:Creep Recovery Experiment:Creep Recovery Experiment:Creep Recovery Experiment:Response of Viscoelastic Material
Creep σ> 0
timet 1 t2
RecoverableStrain
Recovery σ = 0 (after steady state)
σ/η
Strain rate decreases with time in the creep
zone, until finally reaching a steady state.
In the recovery zone, the viscoelastic fluid recoils, eventually reaching a equilibrium at some small total strain relative to the strain at unloading.
18
Analysis , Development and Enhancement
time
Recovery ZoneCreep Zone
Less Elastic
More Elastic
Creep σ > 0 Recovery σ = 0 (after steady state)
σ/η
t1 t2
Creep Recovery ExperimentCreep Recovery ExperimentCreep Recovery ExperimentCreep Recovery Experiment
Analysis , Development and Enhancement
Definition of Rheology
• Rheology is the science of flow and deformation of matter.
19
Analysis , Development and Enhancement
Geometry of Shear for RheometersGeometry of Shear for RheometersGeometry of Shear for RheometersGeometry of Shear for Rheometers
Plate & PlatePlate & PlatePlate & PlatePlate & Plate
Cone & Cone & Cone & Cone & PlatePlatePlatePlate
Concentric CylindersConcentric CylindersConcentric CylindersConcentric Cylinders
Motor applies Torque, Strain read from Optical Encoder.
TorsionTorsionTorsionTorsion
Analysis , Development and Enhancement
MotionMotionMotionMotion
Flow(Flow, Creep,
Stress Relaxation)
Oscillation Squeeze Flow/Pull Off
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Analysis , Development and Enhancement
γ = Strain γ = Strain Rate σ = Stress
Kγ = Strain Constant Kσ = Stress Constant
θ = Angular Motor Deflection M = Torquein Radians
Gc = Gravity constant = 98.07 Pascals (SI)= 980.7 dyn/cm2 (cgs)
Ω = Motor angular velocity in radians/sec.β = Cone angle in radiansH = Gap for parallel plate in mmR = Radius of plate or cone in mmR1 = Radius of concentric cylinder bob in mmR2 = Radius of concentric cylinder cup in mm
List of Symbols
Analysis , Development and Enhancement
Typical Viscosity Values (PaTypical Viscosity Values (PaTypical Viscosity Values (PaTypical Viscosity Values (Pa----s)s)s)s)
Asphalt Binder ------------------
Polymer Melt --------------------
Molasses --------------------------
Liquid Honey --------------------
Glycerol --------------------------
Olive Oil -------------------------
Water -----------------------------
Air ---------------------------------
100,000
1,000
100
10
1
0.01
0.001
0.00001
Need for Log scale
21
Analysis , Development and Enhancement
More on ViscosityMore on ViscosityMore on ViscosityMore on Viscosity
According to Isaac Newton, viscosity is constant for all times and shear-rates –Newtonian Fluids
Viscosity is dependent on Temperature and Pressure
Viscosity may not be constant – Non-Newtonian Fluids
Viscosity of Non-Newtonian fluids can depend on– Time :– Thixotropy, Rheopexy– Shear-rate :– Shear-thinning, Pseudoplasticity, Dilatency
Time-DependenceAt constant shear-rate, if viscosity
– Decreases with time - Thixotropy– Increases with time - Rheopexy
Analysis , Development and Enhancement
Non-Newtonian, Time Independent Fluids
Shear-ThinningA decrease in viscosity with increasing shear
rate. Also referred to as Pseudoplasticity.
Shear-ThickeningAn increase in viscosity with increasing shear
rate. Also referred to as Dilatancy (a special case of shear-thickening).
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Analysis , Development and Enhancement
Non-Newtonian, Time Dependent Fluids
ThixotropyA decrease in apparent viscosity with time under
constant shear rate or shear stress, followed by a gradual recovery, when the stress or shear rate is removed.
RheopexyAn increase in apparent viscosity with time under
constant shear rate or shear stress, followed by a gradual recovery when the stress or shear rate is removed. Also called Anti-thixotropy or negative thixotropy.
Reference:Barnes, H.A., Hutton, J.F., and Walters, K., An Introduction to Rheology, Elsevier Science B.V., 1989. ISBN 0-444-87469-0
Analysis , Development and Enhancement
Non-Newtonian, Time Dependent Fluids
time
Vis
cosi
ty
Thixotropic
Rheopectic
Shear Rate = Constant
23
Analysis , Development and Enhancement
TimeTimeTimeTime----Temperature Superposition PrincipleTemperature Superposition PrincipleTemperature Superposition PrincipleTemperature Superposition Principle
TTS is an EMPERICAL relationship
TTS is based on the observation that, for a single material,the curves of the viscoelastic properties, generated at different temperatures, are similar in shape when plotted againstlog time or log frequency. The Curves generated at differenttemperatures can be exactly superimposed by shiftingalong these axes.
TTS applies to stress relaxation, creep and dynamic mechanicalmeasurements
Analysis , Development and Enhancement
Time and Temperature: Two Sides of the Same CoinTime and Temperature: Two Sides of the Same CoinTime and Temperature: Two Sides of the Same CoinTime and Temperature: Two Sides of the Same Coin
(E" or G")(E' or G')
(E" or G")
(E' or G')
log Frequency
Temperature
log Time
log Time
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Analysis , Development and Enhancement
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