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Tribological properties of In-Situ Si 2 N 2 O-Si 3 N 4 composites

Awais Qadir

Supervisor: Prof. Dr. Ján Dusza,

Dr. Pinke Peter

(2)

Aim of the work

• To study the tribological behaviour of in-situ grown Si 2 N 2 O in Si 3 N 4 composites.

• Following parameters were studied:

 Wear Mechanism

 Coefficient of friction

24/06/2020 Semester Progress Report Jan - Jun, 2020,

Obuda University 2

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Materials Preparation

α-Si 3 N 4 Powder

Mixing with Y 2 O 3 &

Al 2 O 3

Sintering at 1500 ˚C for 3 hours

Sintering at 1700 ˚C for 3 hours

Mixing with Y 2 O 3 &

Al 2 O 3

Sintering at 1500 ˚C for 3 hours

Sintering at 1700 ˚C

Sintering at 1700 ˚C for 3 hours

Sintering at 1500 ˚C for 3 hours Mixing with

Y 2 O 3 &

Al 2 O 3

As Reference Material

10 hrs oxidized

α-Si 3 N 4

20 hrs oxidized

α-Si 3 N 4

Semester Progress Report Jan - Jun, 2020,

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Samples Details

24/06/2020 Semester Progress Report Jan - Jun, 2020,

Obuda University 4

Oxidation Time (h)

α-Si

3

N

4

(wt. %)

Y

2

O

3

(wt.

%)

Al

2

O

3

(wt. %)

SN-15/0 0 90 6 4

SN-15/10h 10 90 6 4

SN-15/20h 20 90 6 4

SN-17/0 0 90 6 4

SN-17/10h 10 90 6 4

SN-17/20h 20 90 6 4

Un-oxidized

10h oxidized

20h oxidized

10h oxidized

20h oxidized

Un-oxidized

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XRD Analysis

10 20 30 40 50 60 70 80 90

Intensity

 

SN-17/0 SN-17/10h SN-17/20h

SN-15/20h SN-15/10h

 



      

 

 



 

SN-17/20h SN-17/10h SN-17/0 SN-15/20h SN-15/10h SN-15/0

Si

3N

4

Si

3N

4

Si2N2O ZrO2 Al2O3

  

SN-15/0



Complete  to  transformation happened in case of sample sintered at 1700 C.

Phase Si

2

N

2

O appeared in samples which processed from the oxidized powders.

The amount of Si

2

N

2

O

increasing with the oxidation time or amount oxides in starting powders.

Un-oxidized

10h oxidized

20h oxidized Un-oxidized

10h oxidized

20h oxidized

Sintered @ 1700 C

Sintered @

1500 C

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What is Tribology

• Tribology = Greek word “Tribos”

Tribos = “Rubbing and Sliding”

• Tribology is a scientific study which deals with friction, lubrication and wear of contacting bodies.

• Tribological knowledge helps to improve service life, safety and reliability of interacting machine components and yields in economic benefits.

24/06/2020 Semester Progress Report Jan - Jun, 2020,

Obuda University 6

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What is Tribology and its importance?

Source: H. Czichos and M. Woydt: Introduction to Tribology and Tribological Parameters.

ASM handbook, Vol. 18, Friction, Lubrication and Wear Technology, 2017

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Impact of Tribological Issues on Global Economy

23%

77%

Energy Consumption

Tribology Remaining

24/06/2020 Semester Progress Report Jan - Jun, 2020,

Obuda University 8

Energy Consumption due to Friction and Wear

87%

13% To over come

Friction To

remanufacture the worn parts To re-manufacture

To overcome Friciton

Source: K. Holmberg and A. Erdemir, “Influence of tribology on global energy consumption, costs and emissions,” Friction, vol. 5, no. 3, pp.

263–284, Sep. 2017.

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Tribological Testing of our samples

Ball-on-disk technique

Counter part = Si

3

N

4

ball (D=5 mm) Condition = Dry sliding condition

Temperature = Room temperature (25 C) Humidity = 51%

Normal applied load = 5 N Sliding speed = 0.05 m/s Sliding distance = 1000 m.

Different types of testing techniques

Source: Source: https://www.face-kyowa.co.jp/english/en_science/en_what_friction.html

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Coefficient of Friction

24/06/2020 Semester Progress Report Jan - Jun, 2020,

Obuda University 10

0.79216

0.72682 0.73936 0.73157

0.75941

0.73298 0.80974

0.76296 0.76836

0.64664

0.72436

0.67079

SN-15/0 SN-15/10h SN-15/20h -- -- SN-17/0 SN-17/10h SN-17/20h

0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0

Samples sintered at 1700 C

C o e ffi c ie n t o f F ri c ti o n (C O F ):



Samples sintered at 1500 C

0-40 m 40-1000 m

Overall, COF of samples sintered at 1500 C was higher than that of 1700 C

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Wear Rate

1.64699E-4

1.22428E-4

1.86252E-4

2.3954E-4

3.45108E-4

2.68916E-4

SN-15/0 SN-15/10h SN-15/20h -- SN-17/0 SN-17/10h SN-17/20h

0.0 5.0x10-5 1.0x10-4 1.5x10-4 2.0x10-4 2.5x10-4 3.0x10-4 3.5x10-4

Total Wear Rate (W s): mm3Nm

Wear Rate

Samples sintered at 1500C Samples sintered at 1700C

Wear Rate of samples sintered at 1700 C was higher than that of 1500 C

Low wear rate can be attributes to the present amount alpha phase,

Alpha phase is harder and

robust than beta phase.

(12)

Stages of Wear Rate

24/06/2020 Semester Progress Report Jan - Jun, 2020,

Obuda University 12

Source: Machinability of Titanium Alloys in Drilling By Safian Sharif, Erween Abd Rahim and Hiroyuki Sasahara

Submitted: May 17th 2011Reviewed: October 12th 2011Published: March 16th 2012 DOI: 10.5772/35948

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Wear rate in Different Stages

In first 0-40 m (run-in stage), the wear rate was almost time higher than the overall wear rate.

7.62557E-4

6.39755E-4

8.04367E-4

0.00118

0.00257

0.00164

1.39788E-4

1.00873E-4

1.60498E-4 2.00542E-4 2.52321E-4

2.11934E-4

SN-15/0 SN-15/10h SN-15/20h -- SN-17/0 SN-17/10h SN-17/20h

0.0 5.0x10-4 1.0x10-3 1.5x10-3 2.0x10-3 2.5x10-3

Samples sintered at 1700C

T o ta l W e a r R a te ( W

s

): mm

3

Nm

0 - 40 m 40 -100 m

Samples sintered at 1500C

For our samples, the first

40 m of sliding is a run-in

stage

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Wear rate at every 100 m

Sintered at 1500 C Sintered at 1700 C

24/06/2020 Semester Progress Report Jan - Jun, 2020,

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0 200 400 600 800 1000

0.0 2.0x10-4 4.0x10-4 6.0x10-4 8.0x10-4

Specific Wear Rate (Ws): mm3 Nm

SN-15/0 SN-15/10h SN-15/20h

ExpDec1 Fit of Sheet1 SN-15/0 ExpDec1 Fit of Sheet1 SN-15/10h ExpDec1 Fit of Sheet1 SN-15/20h

Sliding Distance (m)

Model ExpDec1

Equation y = A1*exp(-x/t1) + y0

Reduced Chi-Sqr 9.0751E-10 2.12042E-9 3.87873E-10

Adj. R-Square 0.98319 0.95059 0.99217

Value Standard Error

SN-15/0 y0 6.63039E-5 1.36285E-5

SN-15/0 A1 9.35521E-4 5.2052E-5

SN-15/0 t1 138.20716 14.41579

SN-15/10h y0 5.03463E-5 1.91419E-5

SN-15/10h A1 8.87229E-4 9.43201E-5

SN-15/10h t1 114.28241 20.73485

SN-15/20h y0 1.1443E-4 7.79872E-6

SN-15/20h A1 0.00104 4.6521E-5

SN-15/20h t1 99.10054 7.08659

0 200 400 600 800 1000

0.0 5.0x10-4 1.0x10-3 1.5x10-3 2.0x10-3 2.5x10-3 3.0x10-3

Specific Wear Rate (W s): mm3 Nm SN-17/0

SN-17/10h SN-17/20h

ExpDec1 Fit of Sheet1 SN-17/0 ExpDec1 Fit of Sheet1 SN-17/10h ExpDec1 Fit of Sheet1 SN-17/20h

Sliding Distance (m)

Model ExpDec1

Equation y = A1*exp(-x/t 1) + y0 Reduced Chi-Sqr

2.30501E-9 9.32831E-9 3.04964E-9

Adj. R-Square 0.97795 0.9812 0.98455 Value Standard Error

SN-17/0 y0 1.41221E-4 1.85034E-5

SN-17/0 A1 0.00157 1.25797E-4

SN-17/0 t1 90.04197 10.94038

SN-17/10h y0 2.50603E-4 3.22002E-5

SN-17/10h A1 0.04485 0.11092

SN-17/10h t1 13.51229 11.30244

SN-17/20h y0 1.7767E-4 1.91966E-5

SN-17/20h A1 0.00328 3.39082E-4

SN-17/20h t1 49.09084 5.40979

Run-in 0-40 m

Steady State 40-1000 m

Run-in 0-40 m

Steady State

40-1000 m

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Wear Mechanism

SEM Image of wear track

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Conclusion

• Oxidizing the starting powders of Si 3 N 4 is successful in order to grow in-situ Si 2 N 2 O in sintered Si 3 N 4 .

• The wear rate in run-in stage is much higher than that of steady-state stage. 1000 m sliding distance is still a steady state, no catastrophic failure was observed.

• The COF is higher for the composites sintered at 1500

C and lower wear rates due to the presence of higher amount of  - Si 3 N 4 in the composite.

24/06/2020 Semester Progress Report Jan - Jun, 2020,

Obuda University 16

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Publication 2017 - 2020

1. A. Qadir, Z. Fogarassy, Z. E. Horváth, K. Balazsi, and C. Balazsi, “Effect of the oxidization of Si3N4 powder on the microstructural and mechanical properties of hot isostatic pressed silicon nitride,” Ceramics International, vol. 44, no. 12, pp. 14601–14609, Aug. 2018. (Impact Factor 2.986). https://doi.org/10.1016/j.ceramint.2018.05.081

2. Awais, Q., Balazsi, K., Balazsi, C., Ivor, M. and Dusza, J., 2020. Properties of MWCNTs added Si3N4 composites processed from oxidized silicon nitride powders. Processing and Application of Ceramics, 14(1), pp.25-31.(Impact Factor: 1.085).

https://doi.org/10.2298/PAC2001025Q

3. Qadir, A.; Pinke, P.; Dusza, J. Silicon Nitride-Based Composites with the Addition of CNTs—A Review of Recent Progress, Challenges, and Future Prospects. Materials 2020, 13, 2799. (Impact Factor 2.972)

https://doi.org/10.3390/ma13122799

4. Awais, Qadir ; Jan, Dusza ; Pinke, Péter, Tribological Behavior of Silicon Nitride and Carbon Based Filler Composites – a Review, In: Horváth, Richárd; Beke, Éva; Stadler, Róbert Gábor (eds.) Mérnöki Szimpózium a Bánkin előadásai : Proceedings of the Engineering Symposium at Bánki (ESB 2019), Budapest, Hungary : Obuda University, (2019) pp. 7-16. , 10 p

5. Tribological properties of in-situ grown Si

2

N

2

O-Si

3

N

4

composites, (In Progress)

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18

Thank You for your attention!

Köszönöm a figyelmet!

24/06/2020 Semester Progress Report Jan - Jun, 2020,

Obuda University

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