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Quantrain x50Module 10

Sample Preparation3-2010

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Sample Prep Basics• Specimen characteristics

-volatile materials- heat sensitivity- electron beam sensitivity-electrical charging

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Some general preparation rules for optimum imaging

• 1. Place powders or small particles directly onto a carbon coated stub or use a conductive adhesive. Move sample away from lower lens during pump down

• 2. Metal or carbon coat filters before use.3. Use (conductive) silicon wafers instead of glass if a smooth surface is needed 4. Use a conductive tape to hold down samples.5. Lightly coat (about 2 nm) the sample (with a metal)

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Special Importance of Mounting Media for Non-conductive Specimens• Aluminium

• Carbon• Copper• Mounting adhesives• Double-sided tape• Metallic tapes• Wax or oil based mounting media

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Volatile Materials

• Some samples become volatile under the electron beam

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Heat Sensitivity

• The electron beam can generate heat to ‘burn’ or melt a sample

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Electrical Charging

Internal charge builds charge cloud

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Metal Coating

• Coating creates an electrical path to ground

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Metal Coating

Plasma

Target molecules

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Metal Coating

Plasma

Coating Thickness

Note thin film-

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Sample Prep Basics• Secure the sample

- carbon paint (isopropyl based)

• Determine if coating is possible/necessary- conductivity is the key- low voltage may be a solution- ESEM is the solution

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Mounting Media• Aluminium stub

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Mounting Media

• Aluminium or carbon stub

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Mounting Media• Aluminium or carbon stub• Copper cup

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Mounting Media• Aluminium or carbon stub• Copper cup• Analytical mounts

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What to Avoid !!!

• Carbon and double sided tape is not stable (for hi-res..)

• Constantly expanding, absorbing, swelling, etc• Contamination of sample and chamber

- finger prints- oily sputter system- has sample been in a dirty SEM?- Sitting around absorbing gas

• Silver paint (blows up leaving silver particles everywhere)

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Mounting Methods

• Adhesives

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Mounting Methods• Adhesives

• Double sided tape

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Mounting Methods• Adhesives• Double sided tape

• Metallic tapes

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Mounting Methods• Adhesives• Double sided tape• Metallic tapes

• Wax or oil based to be avoided

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Other Mounting Adhesives • Gold paint• Silver paint• Carbon paint• Colloidal carbon• Carbon tabs• Microstik

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Basic Preparation Techniques

• FracturesMetals

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Basic Preparation Techniques• Fractures

MetalsNon-metals

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Basic Preparation Techniques• Fractures

MetalsNon-metals

• SectionsHard samples- cross sections

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Integrated Circuit Cross Section

• Chemical etching

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Preparation Techniques

• Fracturesmetalsnon-metals

• Sectionshard samples- cross sections(cont..)

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Preparation Techniques• Fractures

metalsnon-metals

• Sectionshard samples- cross sections

Soft samples- cross/thin sections

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Preparation Techniques (Cont.)• Dispersions

Wet

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Preparation Techniques (Cont.)

• DispersionsWetDilution

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Preparation Techniques (Cont.)

• DispersionsWetDilutionPipette

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Preparation Techniques (Cont.)

• DispersionsWetDilutionPipetteAtomize

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Preparation Techniques (Cont.)• Dispersions

WetDilutionPipetteAtomizeSandwich

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Preparation Techniques (Cont.)

• DispersionsWetDilutionPipetteAtomizeSandwich

• Dry dispersions

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Preparation Techniques (Cont.)

• DispersionsWetDilutionPipetteAtomizeSandwich

• Dry dispersionsAdhesives

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Preparation Techniques (Cont.)

• DispersionsWetDilutionPipetteAtomizeSandwich

• Dry dispersionsAdhesivesFilters

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Preparation Techniques (Cont.)

• Live materialInsectsPlants

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Preparation Techniques (Cont.)

• Live MaterialInsectsPlants

• DryingFixationAir-drying

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Preparation Techniques (Cont.)

• Live MaterialInsectsPlants

• DryingFixationAir-dryingFreeze drying

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Preparation Techniques (Cont.)

• Live MaterialInsectsPlants

• DryingFixationAir-dryingFreeze dryingCritical Point Drying

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Critical Values of CPD Fluids

• FLUID FORMULA CRITICAL TEMP. (°C) CRITICAL PRESSURE (Atm)• water H2O 374.0 217.7• carbon dioxide CO2 31.1 72.9• nitrous oxide N2O 36.5 71.7• freon CClF3 28.9 38.2

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Preparation Techniques (Cont.)

• ReplicasCelleous acetate sheet

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Preparation Techniques (Cont.)

• ReplicasCelleous acetate sheetSilicone rubber (Silico-set)

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End of Quantrain 10 sample prep.ppt

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Sample Page HeaderSubhead: if used, should be sized to 24

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Sample App Photo PageSubhead: if used, should be sized to 24

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Sample App Photo PageDark background to be used if images are light

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Sample Product PageSubhead: if used, should be sized to 24

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Color Guidelines

Accent ColorsSupporting Tones

Signature Colors

RGB 238, 88, 7

RGB 176, 26, 36

RGB 208, 208, 208

RGB 161, 161, 161

RGB 113, 113, 113

RGB 130, 160, 99

RGB 102, 125, 136

RGB 171, 151, 33

RGB 149, 130, 115