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doi: 10.1038/nmat2978
Figure S1. TEM analysis of reaction mixture a.) before addition of reductant, b.)
immediately thereafter, c.) 20 minutes after addition of reductant (davg = 3.56 ± 0.59 nm),
and d.) after a standard 20h growth period (davg = 4.59 ± 1.04 nm). Histograms of the
magnesium nanocrystal sizes are also shown for the e.) 20 minute and f.) 20 hour reaction
times. These data support the burst-nucleation model hypothesized in the manuscript.
Figure S2. Histogram of the diameters of the magnesium nanocrystals present in the
70
60
Number of Particles
50
40
30
20
10
0
1 2 3 4 5 6 7 8 9 10
Diameter (nm)
independent syntheses.
composite with references (bottom) of hexagonal Mg (solid black line, JCPDS 04-0770),
cubic MgO (long dashed grey line, JCPDS 89-7746) and hexagonal Mg(OH)2 (short
dashed light grey line, JCPDS 07-0239). Mg NCs composites formed with
Mg
MgO
Mg(OH)
2
(101)
(100)
(002)
(102)
(110)
(103)
30 35 40 45 50 55 60 65
2! (degree)
calorimetry (DSC) traces of Mg NCs/PMMA composites, red solid line and dashed line,
respectively. TGA trace of pure PMMA is shown as a control (black solid line). The Mg
NCs/PMMA composite TGA trace displayed two distinct slopes: the first weight loss
from room temperature to 250 oC is attributed to the evaporation of residual solvent and
the removal of low molecular weight polymers, while the second weight loss which
plateaus around 500 oC is attributed to the degradation of the PMMA polymer matrix. In
the pure PMMA TGA trace, weight loss was complete at ~440 oC when all of the
polymer has been burned off, which corresponds closely with the TGA data obtained on
composites is thereby attributed to the pure Mg metal. Based upon this value, it is
concluded that the weight of the hydrogen storage active material (pure Mg) in the Mg
120 14
Mg-PMMA
PMMA 12
100
Mass Loss (wt. %, TGA)
10
80
8
DSC (µV)
60 6
4
40
2
20
0
0 -2
0 100 200 300 400 500 600 700
o
Temperature ( C)
Figure S6. Low loss electron energy loss spectrum (EELS) of a 50 nm MgO powder at
80kV under TEAM 0.5 (at 80 kV). MgO was stable during the 10 minutes of beam
exposure, with the largest MgO plasmon energy loss occurring at 22.3 eV. The overall
0 5 10 15 20 25 30 35
Energy Loss (eV)
measured at three different temperatures (T = 473, 523, and 573 K) and the activation
energies were determined by plotting the log of the rate constant versus 1/T.
growth. The large black circles represent the resulting curves of different kinetic
composites (initial 6 minutes); the linear fit R2 value is listed below. The small black
circles represent a linear fit to the data. Insets: MgH2 growth schematics.
equation: Diameter = 0.9λ/β*cosθ, where λ is the wavelength of the X-ray (0.154 nm)
and β is the full width at half maximum of the diffraction peak. Four samples were