GLOBAL R&D CENTRE-ASIA, APOLLO TYRES LTD.,

Transcription

1 LASER DIFFRACTION TECHNIQUE: AN APPROACH TO DETERMINE AGGREGATE SIZE DISTRIBUTION OF CARBON BLACK GLOBAL R&D CENTRE-ASIA, APOLLO TYRES LTD., Tapas R. Mohanty*, Ramakrishnan S, TR.Gopalakrishnan, SKP. Amarnath, Daniele Lorenzetti, PK.Mohamed * Speaker 1

2 Contents Introduction Carbon Black Morphology Importance of ASD & Various Techniques for Measuring ASD Disc Centrifuge Photosedimentry (DCP) Laser Diffraction Technique for measuring ASD of CB Comparison between Laser Diffraction & DCP Summary & Conclusion 2

3 It s Time for a change.. 3

4 Contents Introduction Carbon Black Morphology Importance of ASD & Various Techniques for Measuring ASD Disc Centrifuge Photosedimentry (DCP) Laser Diffraction Technique for measuring ASD of CB Comparison between Laser Diffraction & DCP Summary & Conclusion 4

5 Carbon Black Morphology 5

6 Contents Introduction Carbon Black Morphology Importance of ASD & Various Techniques for Measuring ASD Disc Centrifuge Photosedimentry (DCP) Laser Diffraction Technique for measuring ASD of CB Comparison between Laser Diffraction & DCP Summary & Conclusion 6

7 PSD Vs ASD PSD ASD WHY TO MEASURE AGGREGATE SIZE DISTRIBUTION (ASD)? PSD- Particle Size Distribution : ASD- Aggregate Size Distribution 7

8 Aggregate Size Distribution Broad ASD Narrow ASD Low Tint Strength Easy to Disperse Low RR High Tint Strength Difficult to Disperse High abrasion resistance 8

9 ASD: Effect on Tyre Performance NG- CB3 NG- CB2 NG- CB1 tan δ (max.) Vs Average distance between aggregates (δaa) of CB (NR Compound) Narrow ASD blacks Vs ASTM CB Michael D. Morris, Advanced Tire Fillers, Rubber World February 2010 Florian Diehl, Werner Niedermeier and Lin Bradley, Rubber World February

10 Techniques of ASD Measurement Disc Centrifuge Photosedimentry Image Analysis Laser Diffraction Dynamic Light Scattering 10

11 Contents Introduction Carbon Black Morphology Importance of ASD & Various Techniques for Measuring ASD Disc Centrifuge Photosedimentry (DCP) Laser Diffraction Technique for measuring ASD of CB Comparison between Laser Diffraction & DCP Summary & Conclusion 11

12 Disc Centrifuge Photosedimentometry (DCP) CB sample Low sonication Add Ethanol Sonicated sample Add Surfactant High sonication Sample for analysis 12

13 ASD of standard reference blacks (SRB8) samples by DCP SRB8 A2 SRB8 B2 SRB8 C SRB8 F2 13

14 Contents Introduction Carbon Black Morphology Importance of ASD & Various Techniques for Measuring ASD Disc Centrifuge Photosedimentry (DCP) Laser Diffraction Technique for measuring ASD of CB Comparison between Laser Diffraction & DCP Summary & Conclusion 14

15 Laser Diffraction Technique: Particle Size Analyzer Measures particle size and distribution with technique using Fraunhofer and Mie scattering principles. help of laser diffraction 15

16 Sample preparation & Instrumentation H2O External sonication CB Sample + Surfactant CB Suspension Sonicated sample F. Storti and F. Balsamo, Solid Earth, 1, 25 48,

17 Core Principle Can investigate a particle with light and derive its size Low angle scattering High angle scattering Large Signal Large Particle Small signal Small Particle 17

18 Fraunhofer & Mie Theory of Diffraction of laser light Size range: 0.02μm to 2000μm Light sources: Red light: Helium neon laser Blue light: Solid state light source Detection systems: Red light: Forward scattering, side scattering, back scattering. Blue light: Wide angle forward and back scattering. 18

19 Factors Affecting ASD Measurement Sample Concentration Surfactant Concentration Sonication (Time or %) Suspension Emulsion Stable Suspension Sedimentation Flocculation 19

20 Factors Affecting ASD Measurement Laser obscuration range(%) Pump speed(rpm) Stirrer Speed(rpm) Optimisation of sample addition Laser Source Measuring Cell Laser Obscuration range ( 0-30%) 20

21 Mode of Test General Purpose Mode Multi Narrow Mode Single Narrow Mode 21

22 Data Interpretation D(v, 0.1) : Size of 10% particle D(v, 0.5): Size of 50% particle D(v, 0.9) : Size of 90%. particle Span= [d(0.9)-d(0.1)]/d(0.5) d(0.5) median d(0.1) d(0.9) D(3,2) Size um D(4,3) Span is measurement of the width of distribution. 22

23 ASD - standard reference blacks (SRB8) Colour Grade SRB8B2 SRB8C SRB8E SRB8F SRB8A2 SRB8D 23

24 Aggregate size distribution (µm) Aggregate size distribution (µm) Comparison of Aggregate size : SRB8 Particle size distribution - d (0.1) Particle size distribution - d (0.5) Aggregate size distribution (µm) A2 B2 C D Standard Black E F 0.0 A2 B2 C D Standard Black E F 1.4 Particle size distribution - d (0.9) SRB Grade Hard Blacks SRB Grade Soft Blacks 0.0 A2 B2 C D Standard Black E F 24

25 ASD ( (μm) ASD ( (μm) ASD ( (μm) ASD ( (μm) ASD ( (μm) Effect of sonication time on ASD - SRB SRB8A2 d(0.1) d(0.5) d(0.9) 10 min 15 min SRB8B2 d(0.1) d(0.5) d(0.9) 10 MIN 15 min SRB8C d(0.1) d(0.5) d(0.9) 10 min 15 min SRB8D d(0.1) d(0.5) d(0.9) 10 min 15 min SRB8F d(0.1) d(0.5) d(0.9) 10 min 15 min Note: d(0.1), d(0.5),d (0.9) values for 10 mins and 15 mins sonication time are average of 3 obs. 25

26 Effect of Sonication Time on ASD of Hard Black ( N339) 26

27 Effect of Sonication Time on ASD of Soft Blacks (N550 & N660) w.r.t. Sources *B- Source 2: C-Source 3 27

28 ASD of N134 between Sources Performance analysis of different sources Process Optimisation. Source Tint St. ASD A Broad B Narrow *A- Source 1: B-Source 2 28

29 ASD of N220 between Sources Source Tint St. ASD B Broad C Narrow *B- Source 2: C-Source 3 29

30 Overview 30

31 Contents Introduction Carbon Black Morphology Importance of ASD Measurement & Various Techniques for Measuring ASD Laser Diffraction Technique for measuring ASD of CB Disc Centrifuge Photosedimentometry (DCP) Comparison between Laser Diffraction & DCP Summary & Conclusion 31

32 Analysis of SRB 8 : Laser Diffraction Vs DCP 0.3 d(0.1) SRB8A2 d(0.1) 0.2 SRB8B d(0.9) d(0.5) d(0.9) d(0.5) d(0.1) SRB8C d(0.1) SRB8F d(0.9) d(0.5) d(0.9) d(0.5) Laser Diffraction DCP 32

33 Aggregate Size (µm) Aggregate Size (µm) Aggregate Size (µm) SRB 8 : Laser Diffraction Vs DCP Technique d(0.1) Laser Diffraction SRB8A2 SRB8B2 SRB8C SRB8F DCP 0.6 d(0.5) Laser Diffraction SRB8A2 SRB8B2 SRB8C SRB8F DCP 1.5 d(0.9) Laser Diffraction SRB8A2 SRB8B2 SRB8C SRB8F DCP 33

34 Contents Introduction Carbon Black Morphology Importance of ASD & Various Techniques for Measuring ASD Disc Centrifuge Photosedimentry (DCP) Laser Diffraction Technique for measuring ASD of CB Comparison between Laser Diffraction & DCP Summary & Conclusion 34

35 Summary & Conclusions Technique ASD of 7 ASTM grades and 6 ASTM SRB8 were measured by laser diffraction technique. The results obtained are in good agreement with the theoretical expectations. Successful dispersion of CB has been obtained by optimizing the sonication time(10 mins). The experimental values for four SRB8 (A2, B2, C& F) samples follow same trend in both the test methods. Both the test methods are based on different principles & approximations, the values will not be absolutely same. Laser diffraction technique has advantage of quite a shorter test time. 35

36 References Technique [1] David B. Blackford,Gary R. Simons : Particle Size Analysis of Carbon Black, Particle & Particle System Characterization, Volume 4, Issue 1-4, Page (1987). D.O.E.: [2] Walther W. Tscharnuter, Lily Zu, Bruce B. Weiner, William Bernt,ASTM Carbon Black Reference Materials: Particle Sizing Using a Brookhaven Instruments BI-DCP, Disc Centrifuge Photosedimentometer [3] Rubber grade carbon blacks by D. T. Norma, Manager, Product Development Witco Corporation,ConcarbDivisionHouston,Texas. [4] C. J. Stacy, P. H. Johnson and G. Kraus, Effect of Carbon Black Structure Aggregate Size Distribution on Properties of Reinforced Rubber, Rubber Chemistry and Technology,Volume. 48, Issue 4, Page (1975) D.O.E. : [5] Michael D. Morris, Advanced Tire Fillers, Rubber World February 2010 [6] Cynthia M Flanigan, Comparative study of silica, carbon black and novel fillers in tread compounds, Rubber World February 2012 [7] Flanigan C.M., Beyer L., Klekamp D., Rohweder D., Comparative study of silica, carbon black and novel fillers in tread compounds, American chemical society divison of rubber chemistry,volume 1, Page ,Meeting;180th, American Chemical Society. Rubber Division and Advanced Materials in Health Care; 2011; Akron. 36

37 References Technique [8] Effects of Filler Morphology and Loading on Tire Innerliner Permeability A Computational Study : Dr. Tyler Gruber, Dr. Charles Herd, Dr. Paul Smith, and Steve Crossley Columbian Chemicals Company [9]Weidong Wang, Charles R. Herd, Jorge A. Ayala, Carbonaceous material with broad aggregate size distribution and improved dispersibility, PatentCA C [10] F. Storti and F. Balsamo,Particle size distributions by laser diffraction: sensitivity of granular matter strength to analytical operating procedures, Solid Earth,,Volume 1,Page 25 48,(2010) [11] Florian Diehl, Werner Niedermeier and Lin Bradley, Orion Engineered Carbons, Narrow aggregate size distribution blacks for wear improvement of truck tires,rubber World February 2016 [12] Mikihito Takenaka, Analysis of structures of rubber-filler systems with combined scattering methods, Polymer Journal (2013) 45, [13] F. Storti and F. Balsamo, Particle size distributions by laser diffraction: sensitivity of granular matter strength to analytical operating procedures, Solid Earth, 1, 25 48,

38 Acknowledgement Technique The authors of this research work would like to acknowledge their sincere thanks to Mr Charles Herd, Head R&D, Columbian Carbon and his team for their valuable support. 38

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