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SLS and electrophysical properties of multilayer polymer structures with Ni-Cu nano additives.

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Description of initial nano powders. Selective laser sintering of separate monolayers from powder compositions: PC + nano Ni, PC + nano Cu; Compare with micro Cu ... – PowerPoint PPT presentation

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Title: SLS and electrophysical properties of multilayer polymer structures with Ni-Cu nano additives.


1
SLS and electrophysical properties of multilayer
polymer structures with Ni-Cu nano additives.
1) P.N. Lebedev Physics Institute /LPI/, Samara
branch, Russian Academy of Sciences
2) Institute of Structural Macrokinetics and
Materials Science , Russian Academy of Sciences
  • I. Shishkovsky1, Yu. Morozov2.

2
Outlines of presentation
  1. What is Rapid Prototyping Manufacturing?
  2. Why is polycarbonate with Cu and/or Ni nano
    additives ? RP roadmap, FP7 and MEMS-NEMS
    fabrication
  3. Description of initial nano powders.
  4. Selective laser sintering of separate monolayers
    from powder compositions PC nano Ni, PC nano
    Cu Compare with micro Cu
  5. Selective Laser Sintering of three dimensional
    parts from powder compositions PC nano Ni, PC
    nano Cu
  6. Scanning Electron Microcopy with Element
    Dispersive X-ray Analysis of sintered porous
    samples
  7. Qualitative X ray analysis of sintered porous
    samples
  8. Temperature dependencies of electrophysical
    properties of laser synthesized nano
    compositions
  9. Functional graded structures and 3D parts
    fabrication via SLS method from powder nano
    compositions with interleaving nickel PC
    copper
  10. Conclusions.

3
What is Rapid Prototyping Manufacturing?
Introduction
  • Combination of Computer Aid Design /CAD/
    approach, which realized in the professional
    packages ( - AUTOCAD, CATIA, Pro - Engineer, 3D
    Studio, Solid Work and etc.) with new
    high-technology of synthesis 3D part and tools
    named as-Rapid Prototyping Manufacturing, Solid
    Free Form Fabrication )

The goal of Rapid Prototyping (Selective Laser
Sintering is one from scope technique of RP) is
to be able to quickly fabricate complex-shaped,
three dimensional parts directly from powder
compositions base on CAD models.
3
3
3
4
Why is polycarbonate with Cu and/or Ni nano
additives
Background of problem
1. Kuprianov N.L., Petrov A.L., Shishkovsky I.V.
Conditions of selective laser sintering by
circuit of metal-polymer powder compositions.
//Russian Journal Fizika I himia obrabotki
materialov.- 1995.- ? 3. - p. 88-93. Shishkovsky
I.V., Kuprianov N.L. Method of manufacturing of
volume articles from powder compositions.
Application 95110182/ 02 (017874) priority from
16.06.96, 10. Patent of RF ? 2145269 log in
10.02.2000 ?.
2. Petrov A.L., Scherbakov V.I., Shishkovsky
I.V. Method of laser synthesis of volume gradient
articles. Application ? 2000120948/20, priority
from 11.08.2000. Patent of RF ? 2212982 log in
27.09.2003 ?.
3. Zubriaeva N/I/ and etc. Method of
manufacturing of oxide catalysts. Application ?
99127936/04, priority from 30.12.1999. Patent of
RF ? 2188709 log in 10.09.2002 ?.
crystalline hydrate nickel nitrate Ni(NO3)2?6H2O
5
Roadmap MEMS-NEMS in frameworks of FP7
Background of problem
Top-Down and Bottom-Up approaches
convergence in nanotechnology
MEMS-Micro-Electro-Mechanical Systems NEMS
Nano-Electro-Mechanical Systems sensors,
implants, filter, pumps, delivery systems,
actuators ant etc.
6
Initial powder materials
The nickel and copper nanoparticles were prepared
at the ISMMS of RAS by means of the levitation
jet technique . The mean size values of thus
prepared Ni particles were 27.8, 32.2, 119, and
184 nm. The Ni percentage and specific surface
area of the powders were 86.6/ 25.1 11.2/ 26.9
94.2/ 5.73 and 98.3 at. / 3.68 m2/g,
respectively (the rest of the mass was NiO). The
mean size values of Cu particles were (1.-
76-100 2.- 90-120) nm. The Ni percentage and
specific surface area of the powders were
measured (1. 96.8/3.4 2. 98.2/2.7) w. Cu
(bal., CuO) / m2/g, respectively. A
thermostable polycarbonate (PC) powder was used
as the binder. A commercially available PC powder
(LET-7 grade, Russia) had the particles size of
20-40 ?m. The starting Ni PC blend powders were
prepared in the weight ratios 11 or 12 and Cu
PC 19, 14, 37. In the case of copper,
similar powder compositions were mixed with use
of micro size Cu ( 50mm) for comparison of
sintering results.
7
Initial nano particles of nickel and copper
b)
a)
Scan electron microscopy of initial particles a)
- Ni (mean particle size 2632 nm) b) - Cu
(mean particle size 70-96 nm) .
8
SLS regime optimization for metal-polymer powder
composition ?? Cu 37, ? 11, 8.6, 6.2 W
(monolayer approach, square 10x10 mm)
Cu particle size 50 mm
Cu particle size 70 nm
9
Monolayer SLS in powder compositions ?? copper
Cu particle size 50 mm
Cu particle size 70 nm
? 8.7 W V40 mm/s Cu PC14
?8,7 W V40 mm/s, Cu PC37
?6,2 W V80 mm/s, Cu PC37
?8,7 W V80 mm/s Cu PC19
10
Three dimensional layer by - layer SLS of
porous samples from powder compositions ?? Cu,
square 10x10 mm
Cu particle size 50 mm
? 6,2 W, V 13,3 mm/s Cu PC 19
? 8,7 W , V 40 mm/s Cu PC 14
? 6,2 W, V 13,3 mm/s Cu PC 37
Cu particle size 70 nm
P 8,7 W, V 80 mm/s, Cu PC 19
P 8,7 W, V 160 mm/s, Cu PC 14
P 6,2 W, V 80 mm/s, Cu PC 37
11
Polycarbonate destruction during SLS of metal
polymer powder compositions
Density - ? (left) and intrinsic viscosity - ?
(right) of 3D sintered parts dependence vs. laser
scan velocity V. Curves 1,3 Laser powder ?
2.1 W 2,4 ? 2.9 W. Powder mixture PC Cu
91.
12
Polycarbonate destruction during SLS of metal
polymer powder composition
Logarithm dependence of sol-gel fraction S
(left, curves 1-5) and degree of cross-linked
polymer J (right, curves 6-10) vs. laser scan
velocity V. Laser power 1,7 ? 2.1 W 2,6
? 2.9 W 3-5 and 8-10 -- ? 0.7 W. Curves 3,8
polymer level 9.1 4,9 14 5,10 20
from common mass of powder mixture.
13
TGA and DTA of 3D samples after SLS on air
Curves (4-6) of TG analysis sample mass changing
W (Y axis - left) and curves (1-3) of DTG
analysis W/W0 (Y axis - right) under
different heating velocities Vh in air medium (-
?) and nitrogen (- b) vs temperature changing.
Powder composition PC Cu 91. Firm line- Vh
20 stroke-dotted 10 dashed-line - 5 0C/min.
14
TGA and DTA of 3D samples after SLS on nitrogen
Curves (4-6) of TG analysis sample mass changing
W (Y axis - left) and curves (1-3) of DTG
analysis W/W0 (Y axis - right) under
different heating velocities Vh in air medium (-
?) and nitrogen (- b) vs temperature changing.
Powder composition PC Cu 91. Firm line- Vh
20 stroke-dotted 10 dashed-line - 5 0C/min.
15
Kinetic constants of PC in MPC of different
content, determined by Kissinger method
Ln (F/TM2) Ln (nRAWmn-1/E) E/(RTM),
Where F velocity of sample heating under TGA
Tm temperature of maximum velocity mass loss
(DTA dates) E energy activation n order of
reaction A preexponential factor Wm sample
mass under moment of maximum loss .
16
Time-of-flight mass spectroscopy of secondary
ions TOF-SIMS of samples after SLS in powder
mixture nano Ni PC 1 1 low atom mass.
17
Time-of-flight mass spectroscopy of secondary
ions TOF-SIMS of samples after SLS in powder
mixture nano Ni PC 1 1 high atom mass.
Fingerprint Ions of Polycarbonate ?
18
Three dimensional layer by - layer SLS of
porous samples from powder compositions ?? Ni
21, square 10x10 mm
P 6 W, V 36.7 cm/s
Over a magnetic field
Without magnetic field
19
Scanning electron microscope investigation of
laser sintered samples from powder mixture NiPC
(1 1) ? 6 W, v 17.4 cm/s
Element Atomic Atomic Atomic
S1 S2 S3
C K 55.78 97.36 55.15
O K -- -- 6.50
Ni K 44.22 2.64 38.35
20
Scanning electron microscope investigation of
laser sintered samples from powder mixture NiPC
(1 2) P 6 W, v 17.4 cm/s under high
magnification.
Element Atomic Atomic Atomic
S1 S2 S3
C K 71.89 80.66 83.82
O K 3.42 19.18 4.24
Ni K 24.69 0.16 11.95
21
XRD patterns of laser sintered samples from Ni
PC mixtures 1 1 (1) and 1 2 (2) P 6 W,
v 17.4 cm/s. Curve (3) PC with nano additives
Cu and Ni.
22
Scanning electron microscope study of laser
sintered samples from powder mixture CuPC (3
7) ? 8.7 W, v 10 cm/s
? Cu particle size 50 mm
? Cu particle size 70 nm ?
23
XRD patterns in PC Cu system a) pure PC
without LI b) PC nano Cu 37 without LI
c-e) PC micro Cu f-h) PC nano Cu. c) P
6.2 W, v 13.3 cm/s, PC Cu 19 d)
11/20/14 e) 6.2/20/37 f) 11/20/14 g)
8.7/160/14 h) 6.2 W/80cms-1/37, respectively.
24
Temperature dependencies of real part of
dielectric permeability and a loss tangent in
laser synthesized nano composition base on Cu
PC 19 1) black circles are heating stage 2)
white circles are cooling.
?6,2 W V40 mm/s
Temperature measurements was conducted under 1
MHz frequency at exhibit of the constant voltage
displacement 40 V, in thermostats within the
temperatures range 300-400 K, by means of digital
instrument LRC E7-12 (Russia).
25
Functional graded structures and 3D parts
fabrication via SLS method from powder nano
compositions with interleaving nickel PC
copper, 10x10 mm
Earlier it has been found that giant
magnetoresistance of the multilayers is strongly
dependent on the relative amount of nickel and
cobalt present in the ferromagnetic layer.
Magnetoresistance is also strongly dependent on
the thickness of both ferromagnetic and
non-magnetic layers and increase linearly with
increasing number of interfaces. SLS process
allows to create such interleaving ferromagnetic
(Ni, Fe) and non-magnetic (Cu, PC) layers via
natural course.
Ni PC 12 5 layers, then Cu PC 14 - 5
layers
Cu PC 14, then Ni PC 12 alternation
per layer.
Ni PC 12 3 layers, then Cu PC 19 3
layers
26
SEM and EDX analysis after SLS of nano FG
structures Cu PC nano Ni PC (lateral
surface view)
Red - Ni Blue - C Green - Cu
polycarbonate
27
Conclusion
1. It was shown a principle possibility of SLS of
metal-polymer powder compositions with nano
additives Ni and/or Cu,, which ensures nano
particle sizes conservation.
2. It was shown a principle possibility of
functional graded three - dimensional parts
fabrication via the interleaving of the metal -
polymer powdered compositions with Ni and/or Cu
additives, which ensures nano particle sizes
conservation.
3. The optimal regimes of laser influence were
determined as for single monolayers as layer - by
- layer SLS process.
4. SEM with EDX analysis and X-ray qualitative
analysis of laser sintered microstructures were
shown, that practically an initial particle size
was kept. This is important for catalyst
applications.
5. Temperature dependence of the dielectric
permeability and the loss tangent in PC Cu
nanocomposite was studied. Hysteresis phenomena
were observed in the laser synthesized samples
that can be useful for MEMS-NEMS applications.
6. The sol-gel fraction content is indicated,
that complete destruction PC under laser
influence is not observed. It was optimized PC
content in metal-polymer mixture. The comparison
of our measurements with original values by the
intrinsic viscosity and the molecular weight PK
confirms this conclusion. Activation nature of
thermo-oxidation destruction substantially
decreases with an increase of the PC content, but
comparison by the absolute values shows that the
thermal degradation plays the predominant role
during SLS process. Static TOF-SIMS spectra
revealed the formation of new structures during
the SLS process.
7. Our technique can be extended for the
encapsulation of aluminium, iron, titanium,
and/or cobalt nanoparticls.
28
Thank you for the attention.
Contact address Prof. Igor V. Shishkovsky,
Laboratory of Technological Lasers, P. N.
Lebedev Physical Institute (LPI) of Russian
Academy of Science (Samara branch). Novo-Sadovaja
st. 221, 443011 Samara, Russian
Federation. Phone 7/846/3344220 Fax
7/846/3355600 E-mail shiv_at_fian.smr.ru Web page
http//www.fian.smr.ru/rp/index.htm
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