A Review: Ultrahigh-Vacuum Technology for Electron Microscopes

555 Pages·2020·30.278 MB·English

by  Nagamitsu Yoshimura

A Review: Ultrahigh-Vacuum Technology
for Electron Microscopes
A Review: Ultrahigh-Vacuum
Technology for Electron
Microscopes
Nagamitsu Yoshimura
Retired from the Japan Electron Optics Laboratory (JEOL), Tokyo, Japan
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Contents
Abouttheauthor xxi [1-3] “Outgassingcharacteristicsof
Preface xxiii electropolishedstainlesssteel”
Acknowledgment xxv (Tohyama,Yamada,Hirohata,
Areview xxvii Yamashina,1990)
2 Samplesandexperimentalmethod 19
Part 1 3 Experimentalresultsanddiscussions 20
Reviewedpaper 25
Adsorption, desorption, diffusion,
Relatedpaper
and outgassing/pumping
[1-4] “Areviewofthestainlesssteelsurface”
(Adams,1983)
1. Microstructure and elemental
features of stainless-steel surface 7 Relatedpaper 25
Reviewedpapers
[1-1] “Outgassingcharacteristicsand 2. Characteristics of outgassing
microstructureofanelectropolished from metal surfaces 27
stainlesssteelsurface”
Quotedbook
(Yoshimura,Sato,Adachi,and
Kanazawa,1990) [1-1] “Typicalisothermsinthechemisorption
ofgasesonmetal-surfaces:equilibrium
2 Outgassingcharacteristicsofan
adsorption”(Redhead,Hobson,and
electropolishedpipewall 7
Kornelsen,1968)
A Afteraninsitubakeout 8
3 Microstructureandelementalfeatures Referencesinquotedbook 28
ofstainless-steelsurfaces 11
[1-2] “Relationsbetweenpressure,
A Microstructure 11
pumpingspeedandoutgassingrate”
B Elementalfeatures 12
(Dayton,1960)
4 Conclusion 14
Referencesinthereviewedpaper 14 2 Semiempiricalformulas 29
Reviewedpaper 14 3 Relationamongpressure,speed,and
outgassingrate 29
[1-2] “Outgassingcharacteristicsand
Referencesinthepaper 32
microstructureofa“vacuumfired”
(cid:1) Reviewedpaper 32
(1050 C)stainlesssteelsurface”
(Yoshimura,Hirano,Sato,Ando, [1-3] “Outgassingrateofcontaminatedmetal
andAdachi,1991) surfaces”(Dayton,1962)
2 Microstructureandelementalfeatures 15 2 Equationfortheoutgassingrate 32
A Microstructure 15 Referencesinthepaper 37
B Elementalfeatures 16 Reviewedpaper 37
3 Vacuumcharacteristics 16
[1-4] “Theeffectofbake-outonthedegassing
4 Conclusion 18
ofmetals”(Dayton,1963)
Referencesinthereviewedpaper 18
Reviewedpaper 18 2 Degassingtimeatconstanttemperature 38
v
vi Contents
3 Outgassingratewithvariable Referencesinthepaper 63
temperature 43 Reviewedpaper 63
Referencesinthepaper 45
[1-10] “Trueandmeasuredoutgassingrates
Reviewedpaper 45
ofavacuumchamberwithareversibly
[1-5] “Advantageofslowhigh-vacuum adsorbedphase”(Akaishi,Nagasuga,
pumpingforsuppressingexcessive andFunato,2001)
gasloadindynamicevacuationsystems”
Nomenclature 64
(Yoshimura,2009)
2 Modelingofpump-down 64
A Massconservationequations 64
1 Introduction 46
B Equilibriumandnonequilibrium
2 Transitionalphenomenaofoutgassing 46
adsorptionisotherms 65
3 Excessivegasloadjustafterswitching
overtheevacuationmode 49
3.1 Advantagesofasmallbypassvalve 49 C Measuredandtrueoutgassingrates 67
Referencesinthepaper 51 3 Comparisonbetweentheoryand
Reviewedpaper 51 experiment 68
4 Discussion 69
[1-6] “Thevariationinoutgassingratewith A Approximateexpressionofn 69
p
thetimeofexposureandpumping” B gDependenceofKandp 70
(Rogers,1964) Referencesinthepaper 70
Reviewedpaper 70
2 Analysis 51
4 Firstpump-down 52 [1-11] “Recombinationlimited
5 Secondpump-down 53 outgassingofstainlesssteel”
6 Summary 54 (Moore,1995)
Referencesinthepaper 54
1 Introduction 71
Reviewedpaper 54
2 Methodofanalysis 72
[1-7] “Reductionofstainless-steeloutgassing A MeasurementsbyHseuhandCui 72
inultra-highvacuum”(Calderand B Numericdiffusioncalculation 72
Lewin,1967) C Recombinationlimit 72
3 Resultsofanalysis 73
2 Theory 55
A Recombinationlimitedconcentration
2.1 Effectoftemperatureondegassing 55
profilesversusbaketime 73
2.2 Outgassingafteranormalbakeout 56
B Outgassingrateversustime 74
2.3 Permeationrateofatmospheric
4 Discussion 74
hydrogen 57
A Bakeefficiencyasafunctionof
2.4 High-temperaturebulkdegassing
temperature 74
insitu 58
B Vacuumfurnaceversusinsitubake
2.5 High-temperaturebulkdegassing
efficiency 74
inafurnacewithresidualhydrogen
C Uncertaintiesintheestimateof
pressure 59
outgassingrate 74
5 Summaryandconclusion 60
Referencesinthepaper 75
Referencesinthepaper 60
Reviewedpaper 75
Reviewedpaper 60
Relatedpapers
[1-8] “Estimatingthegaspartialpressuredue
todiffusiveoutgassing”(Santeler,1992) [1-12] “Lade´sorptionsousvide”
(Schram,1963)
2 Diffusiveoutgassing—Fick’slaw 61
Referencesinthepaper 62 Reviewedpaper 75
[1-9] “Modelfortheoutgassingofwaterfrom [1-13] “Hydrogenpumpingbyaustenitic
metalsurfaces”(LiandDylla,1993) stainlesssteel”(ZajecandNamenicˇ,2005)
4 Finalremarks 63 Reviewedpaper 76
Contents vii
3. Methods for measuring outgassing [1-6] “Correctionsinoutgassingrate
rates 77 measurementsbythevariable
conductancemethod”(Berman,
Reviewedpapers
Hausman,andRoth,1971)
[1-1] “Measurementofoutgassingratesfrom
2 Theory 104
materialsbythedifferentialpressurerise
3 Timeinfluence 107
method”(Yoshimura,Oikawa,and
6 Conclusion 107
Mikami,1970)
Referencesinthepaper 108
2 Principleofthedifferentialpressure-rise Reviewedpaper 108
method 77
[1-7] “Conductancemodulationmethod
Reviewedpaper 80
forthemeasurementofthepumping
[1-2] “Athree-point-pressuremethodfor speedandoutgassingrateofpumps
measuringthegas-flowratethrough inultrahighvacuum”(Terada,Okano,
aconductingpipe”(Hiranoand andTuji,1989)
Yoshimura,1986)
1 Introduction 109
1 Introduction 81 2 Conductancemodulationmethod 110
2 Three-point-pressuremethod 81 5 Discussionsandconclusion 112
A Principle 81 Referencesinthepaper 113
B Optimizationofthemeasuringsystem 83 Reviewedpaper 113
C Measurementofgas-flowrates 83
[1-8] Differentialorificemethod;“La
3 Discussion 85
de´sorptionsousvide”(Schram,1963)
4 Conclusion 88
Referencesinthepaper 89 Reviewedpaper 114
Reviewedpaper 89
[1-9] “Discussiononmethodsformeasuring
theoutgassingrate”(Yoshimura,1990)
[1-3] “Two-pointpressuremethodfor
measuringtheoutgassingrate” Reviewedpaper 115
(YoshimuraandHirano,1989)
1 Introduction 89
4. Outgassing rates of
2 Two-point-pressuremethod 90
A Principle 90 system-component materials 117
B Measurementoftheoutgassingrate 91
[1] OutgassingRatesofMetallicMaterials
C Validityoftheone-point-pressuremethod 93
Reviewedpapers
3 Measurementbytheorificemethod 94
4 Discussionandconclusion 95 [1-1] “Outgassingratesofstainlesssteeland
Referencesinthepaper 96 mildsteelafterdifferentpretreatments”
Reviewedpaper 96 (Ishimori,Yoshimura,Hasegawa,and
Oikawa,1971)
[1-4] “Speedmeasuringofiongetterpumps
bythe‘three-gauge’method” Reviewedpaper 121
(MunroandTom,1965)
[1-2] “Outgassingcharacteristicsofstainless
2 Method 96 steelandaluminumwithdifferent
3 Resultsanddiscussion 98 surfacetreatments”(Young,1969)
Referencesinthepaper 101
Referencesinthepaper 123
Reviewedpaper 101
Reviewedpaper 123
[1-5] “Orificemethodinwhichtwopumping
[1-3] “Technologyoflow-pressure
speedscanbeselected”
systems—establishmentofoptimum
1 Methodsofmeasuringoutgassingrates 101 conditionstoobtainlowdegassing
Referencesinthepaper 103 rateson316Lstainlesssteelbyheat
Reviewedpaper 103 treatments”(Nuvolone,1977)
viii Contents
Conclusion 124 [1-7] “Airbake-outtoreducehydrogenoutgassing
Referencesinthepaper 124 fromstainlesssteel”(Bernardini,Braccini,De
Reviewedpaper 124 Salvo,DiVirgilio,Gaddi,Gennai,Genuini,
Giazotto,Losurdo,Pan,Pasqualetti,
[1-4] “Treatmentofthewallmaterialsof
Passuello,Popolizio,Raffaelli,Torelli,Zhang,
extremelyhighvacuumchamberfor
Bradaschia,DelFabbro,Febbro,Ferrante,
dynamicalsurfaceanalysis”
Fidecaro,LaPenna,Mancini,Poggiani,
(Tsukui,Hasunuma,Endo,Osaka,and
Narducci,Solina,andValentini,1998)
Ohdomari,1993)
Relatedpaper 137
2 Extremelyhighvacuumsystems 125
3 Treatmentofvacuumchamberwall 125 [1-8] “Anoverviewofmethodstosuppress
4 Surfacetopography 126 hydrogenoutgassingratefromaustenitic
5 Surfacecomposition 127 stainlesssteelwithreferencetoUHVand
6 Outgassingrate 130 EXV”(IshikawaandNemanicˇ,2003)
7 Conclusion 130
Relatedpaper 138
Referencesinthepaper 131
Reviewedpaper 131 Reviewedpapers
[1-5] “Thin-wallvacuumchambersof [1-9] “Permeabilitymeasurementswithgaseous
austeniticstainlesssteel” hydrogenforvarioussteels”(Eschbach,
(Moore,1998,2001) Gross,andSchulien,1963)
[1-5-1] “Atmosphericpermeationofaustenitic 6 Summary 140
stainlesssteel”(Moore,1998) Referencesinthepaper 140
Reviewedpaper 140
2 Analysis 131
A Eschbachexperiment 131 [1-10] Vapor-pressuredata
B Extrapolationprocedure 132
[1-10-1] “Vapor-pressuredataforthemore
C Oxygeneffects 132
commonelements”(Honig,1957)
D Quantitativeeffectofhydrogen
recombinationonoutgassingand Reviewedpaper 141
permeation 133
[1-10-2] “Vapor-pressuredataforsome
E Summaryofhydrogenpermeation
commongases”(Honigand
corrections 134
Hook,1960)
F Effectofatmosphericwatervapor 134
4 Summary 134 Reviewedpaper 143
Referencesinthepaper 134
[2] OutgassingRatesofNonmetallic
Reviewedpaper 134
Materials
Relatedpaper [2-1] DatabyYoshimuraetal.(1970)and
Yoshimura(1985)
[1-5-2] “Thin-walledvacuumchambersof
austeniticstainlesssteel” [2-1-1] “Measurementofoutgassingratesfrom
(Moore,2001) materialsbydifferentialpressurerise
method”(Yoshimura,Oikawa,and
Relatedpaper 135
Mikami,1970)
[1-6] Outgassingcharacteristicsofthe
[2-1-2] “Adifferentialpressure-risemethodfor
thin-walledstainlesssteelcells
measuringthenetoutgassingrates
[1-6-1] “Outgassinginthinwallstainless ofasolidmaterialandforestimatingits
steelcells” characteristicvaluesasagassource”
(Yoshimura,1985)
Relatedpaper 136
Reviewedpapers 144
[1-6-2] “Experimentswithathin-walled
stainless-steelvacuumchamber” [2-2] DatabyDayton(1959)
Relatedpaper 137 Referencesinthepaper 149
Contents ix
Part 2
[2-3] “WatervaporpermeationthroughViton
O-ringseals”(Yoshimura,1989) Molecular-flow network 175
Referencesinthepaper 154
5. Molecular-flow conductance and
[2-4] “ThepropertiesofViton‘A’elastomers:
gas-flow patterns 179
PartV.Thepracticalapplicationof
Viton‘A’sealsinhighvacuum” [1] Molecular-flowconductance
(deCsernatonyandCrawley,1966)
Quotedbook
1 Summaryofpreviousresults 154
[1-1] “Conductanceoforifice,longtube,
2 UseofdoubleO-rings 156
andshorttube”(Roth,1990)
3 Contamination 157
4 Practicalconsiderations 158 Quotedbook 180
5 Conclusion 159
Reviewedpapers
Referencesinthepaper 159
[1-2] “MonteCarlocalculationof
[2-5] “Recentadvancesinelastomer
molecularflowratesthrougha
technologyforUHVapplications”
cylindricalelbowandpipesof
(deChernatony,1977)
othershapes”(Davis,1960)
3 Recentfluoro-elastomers:Kalrez
Reviewedpaper 182
ECD-006andVitonE60C 160
4 Conclusion 164 [1-3] “Optimizationofmolecularflow
Referencesinthepaper 164 conductance”(Levenson,Milleron,
andDavis,1960)
[2-6] “Practicalselectionofelastomer
materialsforvacuumseals” Reviewedpaper 187
(Peacock,1980)
Relatedpaper
2 Propertiesofpolymerseal
[1-4] “Areviewofthemolecularflow
materials-chemical 164
conductanceforsystemsoftubes
3 Propertiesofpolymerseal
andcomponentsandthe
materials—mechanical 165
measurementofpumpingspeed”
A Compressionset 165
(Steckelmacher,1966)
4 Outgassing 166
5 Permeation 167 Relatedpaper 188
6 Radiationdamageofsealpolymers 168
[2] Gas-flowpatterns
Referencesinthepaper 168
Reviewedpapers
CommentsinPart-1
[2-1] “Gasflowpatternsatentranceand
1 Recommendedpretreatmentsfor
exitofcylindricaltubes”
stainless-steelchamberwalls 169
2 Effectofinsitubaking 170 Reviewedpaper 191
3 Effectofunittimeexposure 170
[2-2] “Angulardistributionsofmolecular
4 Advantageofslowhigh-vacuum
fluxfromorificesofvarious
pumpingforsuppressingexcessive
thicknesses”(Nanbu,1985)
gasload 171
5 Differentialpressurerisemethodfor [2-3] “Afurtherdiscussionabout
measuringtheoutgassingratesofsample gasflowpatternsattheentrance
materials 171 andexitofvacuumchannels”
6 Three-point-pressure,two-point-pressure, (Ji-Yuan,1988)
andone-point-pressuremethods 172
2.Bladechannelsoftheturbomolecular
7 Makeuseofmild-steelforscientific
pump 192
instrumentchamber 173
Referencesinthepaper 193
x Contents
6. Total and partial pressure gauges [1-7] “Enhancedignitionofcoldcathodegauges
for ultrahigh-vacuum use 195 throughtheuseofradioactiveIsotopes”
(Welch,Smart,andTodd)
[1] Bayard(cid:3)Alpertgauge(BAG)andextractor
gauge(EG) 5 Experimenttrials 208
Reviewedpaper 210
Reviewedpapers
[1-8] “Measurementofultra-highvacuum.
[1-1] “Newhot-filamentionizationgauge
Part1.Totalpressuremeasurements”
withlowresidualcurrent”(Redhead,1966)
(Weston,1979)
4 Summaryandconclusion 196
4 Gaugecalibration 210
Referencesinthepaper 196
5 Conclusion 213
Reviewedpaper 196
Referencesinthepaper 214
[1-2] “Practicalguidetotheuseof Reviewedpaper 214
Bayard(cid:3)Alpertionizationgauges”
[1-9] “Reviewofpressuremeasurement
(Singleton,2001)
techniquesforultrahighvacua”
4 Safetyprecautions 197 (Lafferty,1971)
7 Conclusion 197
Reviewedpaper 215
Referencesinthepaper 198
[1-10] “Comparisonofhotcathodeandcold
[1-3] “Comparisonofthepressure
cathodeionizationgauges”(Peacock,
indicationofaBayard(cid:3)Alpertandan
Peacock,andHauschulz,1991)
extractorgauge”(Beeckand
Reich,1972) Reviewedpaper 216
[1-11] “Hot-cathodemagnetronionization
4 Theextractorgauge 198
gaugewithanelectronmultiplierion
5 Comparisonofpressureindicators
betweenBayard(cid:3)Alpertgaugeand detectorforthemeasurementofextreme
ultra-highvacua”(Lafferty,1963)
extractorgauge 199
Referencesinthepaper 201 Relatedpaper 217
Reviewedpaper 201
[2] Partialpressuregauges
[1-4] “Outgassingcharacteristicsofan
Reviewedpaper
electropolishedstainless-steelpipewith
anoperatingextractorionizationgauge” [2-1] “Perspectivesonresidualgasanalysis”
(Yoshimura,Hirano,Ohara,andAndo,1991) (Lichtman,1984)
2 Experiment 202 3 Currentpartialpressureanalyzers 218
Referencesinthepaper 205 A Magneticsector 218
B Quadrupole(monopole) 219
[1-5] Ioncurrentcharacteristicsof
Referencesinthepaper 221
sputter-ionpump,comparedwithan
Reviewedpaper 221
extractorgauge(EG);“Ar-pumping
characteristicsofdiode-typesputter [2-2] “Measurementofultra-highvacuum:
ionpumpwithvariousshapesof“Ti/Ta” Partialpressuremeasurements”
cathode-pairs”(Yoshimura,Ohara, (Weston,1980)
Ando,andHirano,1992)
11 Calibration 222
Reviewedpaper 206 12 Conclusion 225
Referencesinthepaper 226
[1-6] “Startingdelaysincold-cathodegauges
atlowpressures”(Kendalland [2-3] “Determinationoftheionizationgauge
Drubetsky,1996) sensitivityusingtherelativeionization
cross-section”(Nakao,1975)
8 Discussion 207
Referencesinthepaper 207 1 Introduction 226
Reviewedpaper 207 2 Sensitivityoftheionizationgauge 227