a SciTechnol journal Research Article
Kumar and Kailas, Res Rep Metals 2017, 1:4
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Research and Reports on
Metals
International Publisher of Science,
Technology and Medicine
Evolution of In-Situ Nano-Pores
during Friction Stir Processing
of Polymer Derived Ceramic
Reinforced Metal Matrix
Composites
Ajay Kumar P
1
* and Satish V. Kailas
2
Abstract
Nano-porous ceramics have potential applications as diverse as
biomedical implants, catalysis, and armors. This work shows that in-
situ Nano-porous Polymer Derived Ceramics (PDC) can be produced
in Metal Matrix Composites (MMCs) using solid state Friction Stir
Processing (FSP). Direct insertion of cross-linked polymer into the
metal by FSP in solid state is a signifcant step toward inserting
different chemistry of polymer precursors to generate a variety
of in-situ porous structures in Polymer Derived (PD)-MMC. The
PDC route is an effcient and cost effective way to produce SiCN-
based PD-MMC and tailored pore architecture suitable for high
temperature applications. Microstructural observations indicate a
uniform distribution of ~100 nm size pores in the ceramic phase
after pyrolysis.
Keywords
Polymer derived ceramics; Porous materials; Friction Stir
Processing; Metallic composites
*Corresponding author: Ajay Kumar P, Department of Materials Science
and Engineering, University of Wisconsin-Milwaukee-53201 WI, USA, E-mail:
ajaykumarmech85@gmail.com
Received: December 13, 2017 Accepted: December 25, 2017 Published:
December 30, 2017
Introduction
Polymer Derived Ceramics (PDCs) represent a unique class of
high-temperature stable materials synthesized directly by the thermal
decomposition of polymers. PD silicon carbonitride (Si-C-N)
ceramics are candidate materials for high temperature structural
and functional applications in the form of fbers [1], protective
coatings [2], fber and particulate-reinforced composites [3]. In air,
they are stable up to 1500
o
C. Te synthesis of the materials involves
cross-linking and/or pyrolysis of suitable organo-silicon precursor
polymers in inert atmosphere, leading to ceramics with high purity,
controlled structure and chemical composition [4]. Fabrication of the
non-oxide Polymer Derived Porous Ceramics (PDPC) via the method
of PDC is a novel technique. Furthermore, PDPC can be synthesized
at a temperature as low as 1000
o
C free of any additives, and cost-
efcient manners which cannot be performed by the powder-route
technique. Porous ceramics possess number of favorable properties
which combine the merits of ceramics and porous materials such as
light weight, low density, low thermal conductivity, low dielectric
constant, thermal stability, high specifc strength, high specifc surface
area, high porosity, high permeability, high wear resistance, and high
resistance to chemical attack [5].
FSP has successfully evolved as an alternative technique for
fabricating MMCs [6]. FSP depends on the standards of Friction Stir
Welding (FSW) [7]. In FSW, a rotating tool with a pin and a shoulder
are inserted into the material to be joined and traversed along the line
of the joint. Te friction between the tool and the work piece resulting
in localized heating that sofens and plasticizes the material. In the
FSP of MMCs, the material undergoes intense plastic deformation
resulting in the mixing of ceramic particles and the metal. FSP also
results in signifcant grain refnement [8] and has also been used to
homogenize the microstructure of Nano composites [9].
Our previous published work reported the fabrication of in-
situ Nano PD-MMC by Friction Stir Processing (FSP) [10]. In this
paper, a unique method of producing in-situ Nano porous PDC in
solid state using FSP has been introduced. We report the evolution
of in-situ Nano pores/cracks in PDC particles when SiCN cross-
linked polymer was reinforced in copper metal matrix during multi-
pass FSP. Tis method difers from the conventional methods used
for producing porous ceramics and nobody has reported as per the
author’s knowledge. Te pores developed in PDC particles have been
micro structurally characterized in detail to understand the pore
distribution and its morphology.
Experimental Procedure
A commercially available product, KDT Ceraset Polysilazane
20 (VL20) owned by Kion Corporation was used as the polymeric
precursor for preparation of SiCN ceramics. Te VL20 is a versatile
liquid thermosetting resin. Tis polymer contains repeated units
of silicon and nitrogen atoms which are bonded in an alternating
sequence. Te matrix material selected in the present study is pure
copper (99.9%). SiCN cross linked polymer powder, having angular
shaped particles with an average size of 10μm is used as reinforcement
[10]. Te powder is a cross-linked polymer having a density of ~1.0
gcm
−3
. Grooves (3 mm x 4 mm) were cut and holes (ϕ=3 mm) were
drilled into a 6 mm thick copper plate and were flled with the above
mentioned polymer powder. Four passes of FSP were carried out on
a fve-axis friction stir welding machine (BiSS - ITW, Bangalore) on
the groove at a tool rotation speed of 1500 rpm and traverse speed of
25 mm/min. A frustum shaped threaded Densimet tool with shoulder
diameter, pin diameter and pin length of 25 mm, 6 mm and 5 mm,
respectively was used. A tool tilt angle of 3
o
was used. Te processed
plate was then pyrolysed at 800 °C in mufe furnace for 30 min to
convert polymer into ceramic [10].
Te samples were carefully polished using standard methods and
ground with SiC abrasive papers through 3000 grit. Ten the samples
were polished with alumina slurry and fnally with diamond paste
using polishing machine. Ultrasonic cleaning was done for all samples
to make the surface of the specimen free from dust/abrasive particles
and preferably free of oxide layers. Samples were characterized using
Scanning Electron Microscopy (SEM) (Sirion, Model VL 30FEG) with
Energy Dispersive Spectroscopy (EDS) and Transmission Electron
Microscopy (TEM, F-30).