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Organization of hydrogen energy technologies Organization of hydrogen energy technologies

trainingtraining

No. ESF/2004/2.5.0-K01-045No. ESF/2004/2.5.0-K01-045

Main organization - Lithuanian Energy Institute

Partner - Vytautas Magnus University

Ramunė Kazlauskaitė

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Report on surface profilometry measurements technique and analysis of

the experimental results

2005.2005.1010..0303 - 2005. - 2005.1010..2323Training at Poitiers UniversityTraining at Poitiers University Metallurgic Physics LaboratoryMetallurgic Physics Laboratory

FranceFrance

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Grinding with machine

Polishing with machine and

by hand

Surface profile

measurements

The purposeThe purposess of this work: of this work:

1. Specimens preparation:

• Grinding;

• Polishing;

2. Surface profile measurements:

• Used The Dektak IIA profilometer.

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Such films are not useful for further analysis because:

• its are scratching;

• have some defects;

• its are crumbled.

Fig.1 The surface of thin film

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For specimen preparation we used grinding and polishing machine, called RotoForce-1 on RotoPol-11 (Fig.2).

The main RotoForce-1 components:A – control keys and display(5-50N in 5N steps);B – lupo drip lubricator; C – release handle; D – support column; E – pressure feet; F – fastening screws and support hole.

Fig. 2 The scheme of RotoForce-1 on RotoPol-11

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Fig.3 Silicon carbide waterproof abrasive papers

Silicon carbide papers features:

• silicon carbide abrasive;

• exellent grain adhesion;

• waterproof papers backing;

• strength and resistance to  deterioration when used wet;

• ideal for finish sanding

• exellent for machine and hand rubbing;

• the grit size represents the number of holes per linear inch in a sieve screen.

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Resultants of grinding process:

Figures 4. The specimens after different grinding steps

A

D

B

C

Alloy600 specimens after different grinding step:

A - grit size P600, F=10N, t=10min;

B - grit size P800, F=10N, t=10min;

C - grit size P1200, F=10N, t=10min;

C – grit size P1200, F=10N, t=15min;

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Figure 5. Black key felt disk

Felt disk features:

• They are die cut from the finest grade of felt, woven from 100% wool.

• Felt discs have magnobase - magnetic disc, self adhesive for attachment to polishing platens (magnoplate) for use with our polishing specimens.

After grinding with silicon carbide disk we begin to polish with felt disks and diamond polishing abrasives .

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Products features:

• Diamonds products fasters way to obtain a perfect surface due to the polycrystalline properties;

• Non-setting stable suspensions with thixiotropric characteristics are ideally suited for automated systems;

• DP products are environmentally safe;

•All suspensions are non-toxic, non-combustible and water-based.

Figure 6. Implements for polishing

Implements for polishing:• DP-Lubricant red (lubricating liquid for diamond polishing);• Diamond polishing abrasives, grain size 6, 3, 1 micron;

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Resultants of polishing process:A Alloy600 specimens

after different polishing steps:A - grain size 6 µm, F=5N, t=5min;B - grain size 3 µm, F=5N, t=10min;C - grain size 1 µm, by hand F~5N, t=10min; C – grain size 1 µm, by hand F~5N, t=15 min;Figures 7. The specimens after polishing steps

C D

B

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Surface profilometry measurementsThe Dektak IIA profilometer is an instrument for measuring:

• the thickness of thin films (from 20nm to 65000 nm);

• the vertical surface profile of a sample (from 50 microns to 30mm);

The Dektak decompounds of two parts: the Dektak itself, and the computer to its left that is used to control the machine.

Figures 8. The Dektak IIA profilometer

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Fig. 9 The scheme of the Dektak IIA profilometer

Rotory stage

Focusing knob

Camera

The illuminator

Slylus

Fig. 9 The scheme of the Dektak IIA profilometer

13Fig 11.Surface profile measurement

Fig 10. Tracking forse and linearity

• Tracking force and linearity are closely connected. The linearity determines the tension with which the stylus is held.

•Dektak IIA works by gently dragging a mechanical diamond tipped stylus across a surface.

•Vertical movements of the stylus are sensed to computer, digitalized, and stored in the instruments memory.

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Surface profile after grinding with grit size P600 silicon carbid paper

-500

0

500

1000

1500

2000

2500

0

112.

2

228.

4

344.

6

460.

9

577.

1

693.

3

809.

6

925.

8

1042

1158

.3

1274

.5

1390

.7

1507

1623

.2

1739

.4

1855

.7

1971

.9

Scan length [micron]

Ro

ug

hn

ess

[An

gst

rom

]

Surface profile

Ra=330-430 Å

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Surface profile after grinding with grit size P800 silicon carbid paper

-1000

0

1000

2000

0

120.

2

240.

4

360.

7

480.

9

601.

2

721.

4

841.

6

961.

9

1082

.1

1202

.4

1322

.6

1442

.8

1563

.1

1683

.3

1803

.6

1923

.8

Scan lenght [micton]

Rou

ghne

ss

[ang

stro

m]

Surface profile

Ra=250-330 Å

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Surface profile after grinding size P1200 silicon carbid paper

-1000

-500

0

500

1000

0

120.

2

240.

4

360.

7

480.

9

601.

2

721.

4

841.

6

961.

9

1082

.1

1202

.4

1322

.6

1442

.8

1563

.1

1683

.3

1803

.6

1923

.8

Scan lenght [micron]

Rau

gh

nes

s [A

ng

stro

m]

Surface profile

Ra=180-250 Å

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Surface profile after polishing with grain size 6 micron

-400-300-200-100

0100200300400500600700800900

100011001200

0

11

2.2

22

4.4

33

6.6

44

8.8

56

1.1

67

3.3

78

5.5

89

7.7

10

10

11

22

.2

12

34

.4

13

46

.6

14

58

.9

15

71

.1

16

83

.3

17

95

.5

19

07

.8

Scan lenght [micron]

Ro

ug

hn

es

s[A

ng

str

om

]]

Surface profile

Ra=130-180 Å

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Surface profile after polishing with grain size 3 micron

-1000-800-600-400-200

0200400600800

100012001400160018002000

335

435

535.1

635.1

735.2

835.3

935.3

1035.4

1135.4

1235.5

1335.6

1435.6

1535.7

1635.7

1735.8

1835.9

1935.9

Scan lenght [micron]

Ro

ug

hn

ess [

An

gstr

om

]

Surface profile

Ra=90-130 Å

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Surface profile after polishing with grain size 1 micron

-600-500-400-300-200-100

0100200300400500

0

110.

5

221.

1

331.

6

442.

2

552.

7

663.

3

773.

8

884.

4

994.

9

1105

.5

1216

1326

.6

1437

.1

1547

.7

1658

.2

1768

.8

1879

.3

Scan lenght [micron]

Rou

ghne

ss[A

ngst

rom

]

Ra=50-90 Å

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Ra dependence on grinding and polishing steps

04080

120160200240280320360400

Abrasives grit size

Ra

[ang

stro

m]

Ra dependence ongrinding and polishingsteps

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Conclusions:

• In this work I polished substrate of Alloy 600 with grinding and polishing machine and saw that it is impossible to get more than 50Å roughness quality surface with it.

• I got structure of Alloy 600 and saw that there are homogenous grains over all surface.

• Surface profilometry measurements show, that surface roughness depend on abrasives grain sizes: it variable from 430Å to 180Å during grinding and from 180Å to 50Å during polishing.