IAB PROJECT ABSTRACT/DESCRIPTION FORM PROJECT TITLE: Synthesis and Characterization of Nano-Particles Reinforced Surface Coatings Developed by Laser Cladding for Slurry Erosion Applications. INVESTIGATORS: Eswar Yarrapareddy, Syed Hamid and Radovan Kovacevic ABSTRACT/DESCRIPTION: A nano-based material system resistant to slurry erosion has been developed by the Laser-Based

Direct Metal Deposition (LBDMD) process. The nano materials system contains 5 % tungsten

carbide (WC) nano particles which are agglomerated with Ni-Tung 60 by ball mill operation.

The erosion tests are performed on the LBDMD processed coupons using the ceramic proppant

entrained into high speed water-jet at different impingement angles. The nano-based materials

system is applied to restore the damaged oil drilling crossover tools.

PROGRESS TO DATE: The erosion tests material removal rates and the depth of penetrations are correlated to the slurry

jet impingement angle. The nano materials system exhibited better performance for slurry

erosion resistance than the monolithic Ni-Tung 60 depositions. In order to understand the effect

of the nano-WC particles influence on erosion resistance and to understand the characteristic

features of erosion surfaces, sub-surfaces and the erosion mechanisms. Different advanced

characterization tools such as SEM, TEM, FIB, and XRD are used for analysis.

BENEFITS TO MEMBERS (Achieved and Anticipated) The materials resistant to slurry erosion have potential applications in hydraulic turbines, slurry

pumps, valves, pipe-lines conveying solid and liquid particles etc. Of all, industry sectors such as

marine, oil and gas production and power generation are showing interest in this type of research

work.

MILESTONES

The better slurry erosion resistant nano materials system called 5% nano WC + Ni-Tung 60 is

developed using the Laser Based Direct Metal Deposition (LBDMD) process. This materials

system is applied to restore the damaged oil drilling crossover tools.

Synthesis and Characterization of Nano-Synthesis and Characterization of Nano-Particles Reinforced Surface CoatingsParticles Reinforced Surface Coatings

Developed by Laser Cladding for SlurryDeveloped by Laser Cladding for SlurryErosion ApplicationsErosion Applications

Eswar Yarrapareddy1

Dr. Syed Hamid2

Dr. Radovan Kovacevic1

1

11Southern Methodist UniversitySouthern Methodist University

School of EngineeringSchool of Engineering

Center for Laser-Aided ManufacturingCenter for Laser-Aided Manufacturing

Dallas, TXDallas, TX

22Halliburton Energy ServicesHalliburton Energy Services

Carrollton, TXCarrollton, TX

Presentation OutlinePresentation Outline

Introduction, Objective and Applications

LBDMD MultiFab System at SMU CLAM

Experimental for Surface Coatings and Slurry Erosion

Materials Selection and Motivation Behind the Nano materials

Microstructural Characterization using SEM, FIB, TEM and XRD

Results and Discussions

Conclusions and Future Work

Acknowledgements

2

Slurry Erosion

The progressive damage of material surface by the mixture of solid particlesin a fluid medium, which are in motion.

ObjectiveObjective Develop materials system by LBDMD process for slurry erosion resistance

ApplicationsApplications

Oil and gas drilling and pumping industries

Mineral Industries

Marine and power production industries

Ultimate GoalUltimate Goal Apply LBDMD process for developing the nano particles reinforced materialssystem resistant to slurry erosion.

Objectives & ApplicationsObjectives & Applications

3

LBDMD MultiFab SystemLBDMD MultiFab System

LBDMD MultiFab System at SMU CLAMLBDMD MultiFab System at SMU CLAMLASER:

Finer geometrical features

Smaller heat affected zone

Less porosity

Multiple material composition

Better control of material properties

WELDING:

Larger geometrical features

Higher deposition rate

Controlled heat input

Controlled deposition rate

MACHINING:

Complex geometrical features

High dimensional accuracy

High surface quality

4

Slurry mixture of water and ceramic garnet

Impingement angles 15°, 30°, 45°, 60°, 75°, 90°

Impingement Time 2-3 mins

Slurry Erosion Testing ParametersSlurry Erosion Testing Parameters

The Slurry Erosion Testing Set-up at SMU CLAMThe Slurry Erosion Testing Set-up at SMU CLAM

Shielding forthe Fixture

Test Sample

Sample Fixture

Adjustable Stage

Water-Jet Erosion MachineWater-Jet Erosion Machine Experimental Set-upExperimental Set-up

5

Material Assay 1 & 2Material Assay 1 & 2

4140 Steel, AMDRY 302 Steel, 430 NS Steel, NiTi Monolithic, WC Monolithic

Other MaterialsOther Materials

H13 Tool Steel with TiC

Fe-Cr-Si-B (Armacor M)

Continuation of WorkContinuation of Work

Fe-Cr-Si-B with ZrB2

A11-LVC Steel, Inconel 625, Ni-Tung 60 and Ni Tung FGMs

Focus for Nano Materials SystemFocus for Nano Materials System Ni-Tung FGMs exhibited the better erosion resistant than the tested materialsand hence focused for the development of nano particles reinforced materials This materials system was selected to be treated by WC-nano-particles

Previous work done at CLAM and focus for Nano MaterialsPrevious work done at CLAM and focus for Nano Materials

6

Influencing Process Parameters on Slurry ErosionInfluencing Process Parameters on Slurry Erosion

Properties of the target MaterialsProperties of the target Materials

Brittle or Ductile Materials Brittle or Ductile Materials

Microstructural and Mechanical Properties Microstructural and Mechanical Properties

Properties of impingement particlesProperties of impingement particles

Particle Shape Particle Shape

Particle Size Particle Size

Particle Density Particle Density

Concentration of the Particles Concentration of the Particles

Erosion Test ConditionsErosion Test Conditions Nature of the suspension liquid Nature of the suspension liquid

Nature of slurry flow and Velocity Nature of slurry flow and Velocity

Slurry impingement angle Slurry impingement angle

7

Materials Selection and AgglomerationMaterials Selection and Agglomeration

The materials selectedThe Micro-Powders Ni-Tung 60 (particle size 100-145 µm) Nano Powders Nano WC ( particle size 40-70 nm)

The agglomeration process

The premixed micro- and nano- particles are agglomerated inball mill for about 1 hr for about 1 pound of the material

The ceramic balls to materials ratio was kept as 2:1 weight ratio

The Motivation

The nano particles will further strengthenthe matrix and will fill the space among thelarger WC particles after deposition and willresult in the improved the erosionresistance.

WC Particle

Nano WC

8

WC nanoparticles

WC nanoparticles

NT 60 1% Nano WC + NT 60

10% Nano WC + NT 605% Nano WC + NT 60

SEM Analysis of Pre-mixed PowdersSEM Analysis of Pre-mixed Powders

WC nanoparticles

9

Deposition Profiles and Process ParametersDeposition Profiles and Process Parameters

Laser Power 350- 380 watts

Traverse Speed 8-10 mm/sec

Powder Feed Rate 8-10 g/min

Layer Height 0.43 mm

Gas Flow Rate 10-12 ft3/hr

5% Nano WC + Ni-Tung 605% Nano WC + Ni-Tung 60Ni-Tung 60Ni-Tung 60

Deposition Process ParametersDeposition Process Parameters Ni-Tung 60Ni-Tung 60

10

Homogeneous Mixture of Ni-Tung 60 after LBDMDHomogeneous Mixture of Ni-Tung 60 after LBDMD

FE SEM Microstructures for Ni-Tung 60 after LBDMDFE SEM Microstructures for Ni-Tung 60 after LBDMD

11

Measurement of Nano Particles Size LBDMDMeasurement of Nano Particles Size LBDMD

Homogeneous Mixture of Nano and Micro Size Particles after LBDMDHomogeneous Mixture of Nano and Micro Size Particles after LBDMD

12

Nano size grains

Nano size grains

5

10

15

20

25

30

35

40

45

0 15 30 45 60 75 90 105

Impingement Angle (degrees)

We

igh

t L

os

s (

mg

)

4140

Ni-Tung 60

5% nano-WC + Ni-Tung 60

Weight Loss vs. Impingement AnglesWeight Loss vs. Impingement Angles

13

0

5

10

15

20

25

30

35

40

45

50

0 30 60 90 120 150 180

Impingement Time (secs)

We

igh

t L

os

s (

mg

)

4140 Steel

Ni-Tung 60

5% Nano-WC + Ni-Tung 60

Weight Loss vs. Impingement TimeWeight Loss vs. Impingement Time

14

0

5

10

15

20

25

30

35

40

45

5 15 25 35 45 55 65

Pressure (ksi)

We

igh

t L

os

s (

mg

)

4140 Steel

Ni-Tung 60

5% nano-WC + Ni-Tung 60

Depth of Penetration vs. Impingement AngleDepth of Penetration vs. Impingement Angle

15

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

0 15 30 45 60 75 90 105

Impingement Angle (degrees)

De

pth

of

Pe

ne

tra

tio

ns

(m

m)

4140

Ni-Tung 60

5% Nano-WC + Ni-Tung 60

Weight Loss vs. Water-jet PressureWeight Loss vs. Water-jet Pressure

16

FIB analysis for 5% nano WC + NT 60FIB analysis for 5% nano WC + NT 60

Nano WC

Hypothesis for Nanoparticles reinforcement

Micro size grains

Nano size grains

Nano size grains

Micro size grains

Ni matrix

The nano size WC grains are uniformlydistributed through out the Ni- matrix and they areproviding the further reinforcement. The nano-materials system has better erosion resistance

WC Particle

17

TEM Sample Preparation using Focused Ion Beam (FIB)TEM Sample Preparation using Focused Ion Beam (FIB)

Before FIB Milling

Areas of Interest forTEM AnalysisSample Holder

18

FIB Trench

After FIB Milling

TEM Analysis for 5% nano WC + NT 60TEM Analysis for 5% nano WC + NT 60

HR TEM Bright Field image

Selective Area Diffraction Pattern(This work was done at UTD Nano Characterization Lab withthe help of Dr. Moon Kim and his grad students)

19

X-Ray Diffraction PatternsX-Ray Diffraction Patterns

20

Laser Cladding of Oil Drilling Crossover ToolLaser Cladding of Oil Drilling Crossover Tool

21

Movie

ConclusionsConclusions

22

The nano-based materials system called 5% nano-WC + Ni-Tung

60 was successfully deposited by LBDMD process.

The nano-based materials system has about 20-25% better

erosion resistance than the monolithic NI-Tung 60.

Advanced characterization tools such as SEM, TEM, FIB, and

XRD are used for the analysis.

LBDMD process is applied for the restoration of damaged oil

drilling crossover tools.

Single nozzle approach would be used for cladding in between

the groves and critical areas of oil drilling crossover tools.

Future WorkFuture Work

AcknowledgementsAcknowledgements

National Science Foundation I/UCRC

Halliburton Energy Services Inc.

Mr. Roy Beavers of SMU Geology Department for SEM support

Mr. Taehun Lee, Mr. JB Jeon, and Dr. Moon Kim of The University of

Texas at Dallas Nano Characterization lab for helping in FIB and TEM

microstructural analysis.

SMU CLAM Research Team

23

List of Relevant PublicationsList of Relevant Publications Eswar Yarrapareddy, and Radovan Kovacevic, ‘Synthesis and Characterization of Laser Based Direct

Metal Deposited Nano surface Coatings for Slurry Erosion Applications’, Submitted for the Journal of

Surfaces & Coatings technology, January, 2007.

Eswar Yarrapareddy, and Radovan Kovacevic, ‘Numerical Simulation and Characterization of Slurry

Erosion of Laser Cladded Surfaces by Using Failure Analysis Approach’, Submitted for ASM International’s

Journal of Materials Engineering and Performance, October 2006, Article # JMEP-06-03-0228 (Article in

Review).

Eswar Yarrapareddy, Srdja Zekovic, Syed Hamid and Radovan Kovacevic, ‘The Development of Ni-

Tung Functionally Graded Materials (FGMs) By Laser Based Direct Metal Deposition (LBDMD) Process for

Industrial Slurry Erosion Applications’, the Journal of Engineering Manufacture, February 2006, Article #

JEM 578 (Article in Press)

Eswar Yarrapareddy, Syed Hamid, and Radovan Kovacevic, ‘Materials System Development for

Industrial Slurry Erosion Applications by Laser Based Direct Metal Deposition (LBDMD)’, Materials Science

& Technology (MS&T) Conference 2006, October 15-19, 2006, Cincinnati, OH.

Eswar Yarrapareddy, and Radovan Kovacevic, ‘Numerical Simulation and Experimental Investigation of

Surface Coatings Built by Laser Based Direct Metal Deposition (LBDMD) Process for Industrial Slurry

Erosion Applications’, Materials Science & Technology (MS&T) Conference 2006, October 15-19, 2006,

Cincinnati, OH (poster presentation). 24

Thank you