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Specimen Preparation for SEM investigation презентация, доклад

Содержание

Presentation programAim of SEM investigationInvestigated materialsCondition for specimens PreparationSpecimen fixationReplicaExamples

Слайды и текст этой презентации

Слайд 1Specimen Preparation for SEM investigation

prof. dr habil. ing. Włodzimierz Dudziński

Specimen Preparation  for SEM investigationprof. dr habil. ing. Włodzimierz Dudziński

Слайд 2Presentation program

Aim of SEM investigation
Investigated materials
Condition for specimens
Preparation
Specimen fixation
Replica
Examples

Presentation programAim of SEM investigationInvestigated materialsCondition for specimens PreparationSpecimen fixationReplicaExamples

Слайд 3Aim of SEM investigation
Materials are investigated for:
Mikrostructure determination (SE, BSE,

AE, EBSD – Electron Beam Selected Diffraction)

Chemical composition: (EDS, BSE,AE)

Aim of SEM investigationMaterials are investigated for:Mikrostructure determination (SE, BSE, AE, EBSD – Electron Beam Selected Diffraction)Chemical

Слайд 4Analytical SEM JEOL JSM-6610A

Analytical SEM JEOL JSM-6610A

Слайд 5 Low vacuum SEM JSM- 5800LV

Low vacuum SEM JSM- 5800LV

Слайд 6Types of specimens for SEM investigation

Four types of specimens:
1. Metalic
2.

Polymer
3. Biological
4. Geological

Types of specimens for SEM investigationFour types of specimens:1. Metalic2. Polymer3. Biological4. Geological

Слайд 7Metalic specimens
For current conductive metalic specimens any additional preparation is

not necessary.
They can be investigated like specimens for macro or

metallography research.
Specimen can be at polished or tobe at etched state.

It is only necessary to fix
the specimen with appropriate
holder.
Metalic specimensFor current conductive metalic specimens any additional preparation is not necessary.They can be investigated like specimens

Слайд 8Specimens from polymers and composites

Polymer specimens must be sputtered by

the layer of current conductive elements like: C, Au, Pt,

Cu.

Specimens from polymers and compositesPolymer specimens must be sputtered by the layer of current conductive elements like:

Слайд 9Biological specimens
Living cells, biological tissue, and some organs needs to

be specially prepared for the reason their fixation and protection

to stabilize them and to protect against the ravages of the electron beam. 








SEM image of pollen before and after graphic processing

Biological specimensLiving cells, biological tissue, and some organs needs to be specially prepared for the reason their

Слайд 10Biological specimens

Biological specimens must be:
Dried, because inside the SEM chamber

the material will be in the vacuum and therefore can

not be inserted preparations hydrated.

Sputered by current conductive material. Carbon is the best.


Biological specimensBiological specimens must be:Dried, because inside the SEM chamber the material will be in the vacuum

Слайд 11Flower petals sprinkled by gold

Flower petals sprinkled by gold

Слайд 12Samples of powder sputerred by gold

Samples of powder sputerred by gold

Слайд 13Biological specimens covered by gold

Biological specimens covered by gold

Слайд 14Specimen size
Specime sizes are limited by dimensions of SEM support

table. Typical values are:
- Diameter below 5cm,
- Highest below 2,5cm.
Typical

dimensions are: 10 x 10 x 5 mm.


Specimen sizeSpecime sizes are limited by dimensions of SEM support table. Typical values are:- Diameter below 5cm,-

Слайд 15Specimens embeding
Specimens are embeded at epoxy resin for the reason

of better mounting and correction of specimen quality.
Before mounting specimens

must be cleaned, free of dust, grease and any impurities.
Two techniques can be applied:
Hot embeding under the pressure,
Cold embeding.


Specimens embedingSpecimens are embeded at epoxy resin for the reason of better mounting and correction of specimen

Слайд 16Specimen embeding
„Cold embeding” is suitable for materials sensitive at high

temperature and pressure. Special epoxy or acryl resines are applied.
„Hot

embeding” is suitable in the case when high quality of specimen preparation, equal size, shape and short time preparation is necessary. This process is realized by special equipment, (hot temperature press pressure).
Specimen embeding„Cold embeding” is suitable for materials sensitive at high temperature and pressure. Special epoxy or acryl

Слайд 17Electrical current conductivity

Specimens analyzed by SEM methods must conduct electrical

current.

If specimen doesn’t conduct electrical current, then must be

covered by the layer of Au, Pt, C or Cu.

Such prepared specimens can be investigated at high or low vacuum.
Electrical current conductivitySpecimens analyzed by SEM methods must conduct electrical current. If specimen doesn’t conduct electrical current,

Слайд 18Specimen preparation
Cutting, to obtain dimensions limited by support table disposed

inside specimen chamber

Cleaning and degreasing of specimen surfaces

Grinding

Polishing

Etching

Specimen preparationCutting, to obtain dimensions limited by support table disposed inside specimen chamberCleaning and degreasing of specimen

Слайд 19Specimen preparation
Grinding, by using special waterproof fine grain grinding papers.


Specimen preparationGrinding, by using special waterproof fine grain grinding papers.

Слайд 20Specimen preparation
Mechanical polishing by using special velvet tissue immersed by

diamant paste or water suspension of Al2O3. Any traces of

scratches must be eliminated. Specimen surface must be brillant.

Specimen preparationMechanical polishing by using special velvet tissue immersed by diamant paste or water suspension of Al2O3.

Слайд 21Specimen preparation
Etching is the last operation necessary for microstructure visualisation.

It is realised by application chemical reagent on the surface

of polished specimen.

Specimen preparationEtching is the last operation necessary for microstructure visualisation. It is realised by application chemical reagent

Слайд 22Etching reagents

Etching reagents

Слайд 23Etching reagents

Etching reagents

Слайд 24Cross Section Polisher SM-09010

Cross Section Polisher, makes cross section
perpendicullar

to the
specimen surface. It is suitable for investigation
of multilayer structures.



Cross Section Polisher SM-09010Cross Section Polisher,  makes cross section perpendicullar to thespecimen surface.  It is

Слайд 25Cross Section Polisher SM-09010


Principle of operation

.

Cross Section Polisher SM-09010   Principle of operation.

Слайд 26Procedura przygotowania próbki

Procedura przygotowania próbki

Слайд 27Specimens cutting
Saw equipment for sample
precission cutting







Specimens cuttingSaw equipment for sampleprecission cutting

Слайд 28 Examples of SEM application
Granulated
medicine

Examples of SEM applicationGranulated medicine

Слайд 29Examples of SEM application
Paper
Cross-section

Examples of SEM applicationPaper Cross-section

Слайд 30Evaporisation / sputerring
Is realised for covering
the surface specimen
by C, Au,

Pt or Cu
at high vacuum
using special equipment.

Evaporisation / sputerringIs realised for coveringthe surface specimenby C, Au, Pt or Cuat high vacuum using special

Слайд 31Evaporation

Evaporation

Слайд 32Cathode sputtering

Cathode sputtering

Слайд 33Specimen fixation





Current conductive
plasticine
Sticky carbon discs

Specimen fixation	  Current conductive  plasticine					Sticky carbon discs

Слайд 34Specimen fixation







Double Scotch tape

Silver glue
Specimen fixation

Слайд 35Specimen fixed to the holder

Specimen fixed to the holder

Слайд 36Specimens inside the holder

Specimens inside the holder

Слайд 37Replica
The aim is to obtain direct microstructure of construction elements

without their cutting or destruction.
Advantages:
Non destructive method (without decrising the

strength of investigated elements).
Disadvantages:
The abbility to study only the outer surface layer (cannot be representative for whole volume / thickness of investigated material).
ReplicaThe aim is to obtain direct microstructure of construction elements without their cutting or destruction.Advantages:Non destructive method

Слайд 38Replica

Replica

Слайд 39Replica

Replica

Слайд 40Extraction replica

Extraction replica

Слайд 41Examples


Surface of ceramic powder

Cross section of ceramic powder
Examples   Surface of ceramic powder

Слайд 42Examples
Cross section of bone



ExamplesCross section of bone

Слайд 43Pollen of flowers

Pollen of flowers

Слайд 44Part of insect head

Part of insect head

Слайд 45Brittle fracture

Brittle fracture

Слайд 46Composite

Composite

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