Quantrain x50 Module 10 Sample Preparation

Confidential

Quantrain x50Module 10

Sample Preparation3-2010

place photo here

2

Sample Prep Basics• Specimen characteristics

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

3

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)

:

4

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

5

Volatile Materials

• Some samples become volatile under the electron beam

6

Heat Sensitivity

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

7

Electrical Charging

Internal charge builds charge cloud

--

-

-- -

8

Metal Coating

• Coating creates an electrical path to ground

-

9

Metal Coating

Plasma

Target molecules

-

10

Metal Coating

Plasma

Coating Thickness

Note thin film-

11

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

12

Mounting Media• Aluminium stub

13

Mounting Media

• Aluminium or carbon stub

14

Mounting Media• Aluminium or carbon stub• Copper cup

15

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

17

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)

18

Mounting Methods

• Adhesives

19

Mounting Methods• Adhesives

• Double sided tape

20

Mounting Methods• Adhesives• Double sided tape

• Metallic tapes

21

Mounting Methods• Adhesives• Double sided tape• Metallic tapes

• Wax or oil based to be avoided

22

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

23

Basic Preparation Techniques

• FracturesMetals

24

Basic Preparation Techniques• Fractures

MetalsNon-metals

25

Basic Preparation Techniques• Fractures

MetalsNon-metals

• SectionsHard samples- cross sections

26

Integrated Circuit Cross Section

• Chemical etching

27

Preparation Techniques

• Fracturesmetalsnon-metals

• Sectionshard samples- cross sections(cont..)

28

Preparation Techniques• Fractures

metalsnon-metals

• Sectionshard samples- cross sections

Soft samples- cross/thin sections

29

Preparation Techniques (Cont.)• Dispersions

Wet

30

Preparation Techniques (Cont.)

• DispersionsWetDilution

32

Preparation Techniques (Cont.)

• DispersionsWetDilutionPipette

33

Preparation Techniques (Cont.)

• DispersionsWetDilutionPipetteAtomize

34

Preparation Techniques (Cont.)• Dispersions

WetDilutionPipetteAtomizeSandwich

35

Preparation Techniques (Cont.)

• DispersionsWetDilutionPipetteAtomizeSandwich

• Dry dispersions

36

Preparation Techniques (Cont.)

• DispersionsWetDilutionPipetteAtomizeSandwich

• Dry dispersionsAdhesives

37

Preparation Techniques (Cont.)

• DispersionsWetDilutionPipetteAtomizeSandwich

• Dry dispersionsAdhesivesFilters

38

Preparation Techniques (Cont.)

• Live materialInsectsPlants

39

Preparation Techniques (Cont.)

• Live MaterialInsectsPlants

• DryingFixationAir-drying

40

Preparation Techniques (Cont.)

• Live MaterialInsectsPlants

• DryingFixationAir-dryingFreeze drying

41

Preparation Techniques (Cont.)

• Live MaterialInsectsPlants

• DryingFixationAir-dryingFreeze dryingCritical Point Drying

42

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

43

Preparation Techniques (Cont.)

• ReplicasCelleous acetate sheet

44

Preparation Techniques (Cont.)

• ReplicasCelleous acetate sheetSilicone rubber (Silico-set)

45

End of Quantrain 10 sample prep.ppt

Confidential

Title slidesub-title

47 Confidential

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

Body copy goes here. Ut enim ad minim, quis nostrud exercit ulla ullamco. Duisete aute irure dolor in reprehenderit www.fei.com.•Bullet style: officia deserunt mollit anim id est laborum.

• Bullet style: Sed ut perspiciatis de laborum veleta dolorum harum.

• Bullet style: words in signature red for emphasis• Sub-bullet style: Unde omnis iste natus • Nemo enim ipsam voluptatem quia aut fugitNam libero tempore,

cumin soluta nobis est placeat facere possimus, omnis voluptas ass dolor repellendus.

•Bullet style: Excepteur sint occaecat cupidatat.

48 Confidential

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

Caption goes hereCaption goes here

49 Confidential

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

Caption goes hereCaption goes here

50 Confidential

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

Excepteur sint occaecat cupidatat non proident, sunt in culpa qui officia deserunt mollit animid est laborum.

• Sed ut perspiciatis• Unde omnis iste natus• Nemo enim ipsam voluptatem quia

voluptas sis aspernatur aut fugit

51 Confidential

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