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Atomic layer deposition of titanium phosphate on silica nanoparticles
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10.1116/1.3664097
/content/avs/journal/jvsta/30/1/10.1116/1.3664097
http://aip.metastore.ingenta.com/content/avs/journal/jvsta/30/1/10.1116/1.3664097

Figures

Image of FIG. 1.
FIG. 1.

(Color online) Depiction of the pulse sequences used.

Image of FIG. 2.
FIG. 2.

(Color online) Powder composition as a function of deposition temperature after 20 ALD cycles using the sequence (a) TiCl4-H2O-(MeO)3PO-H2O, (b) TiCl4-(MeO)3PO, and (c) TiCl4-H2O-(MeO)3PO. Elemental concentrations were determined by EDS. The balance is oxygen.

Image of FIG. 3.
FIG. 3.

(Color online) Material composition and mass recovered as a function of saturation level, as determined by mass spectrometry of the exhaust stream. All depositions consisted of 20 cycles of the sequence TiCl4-(MeO)3PO at 175 °C. The mass loaded in each case was 980 mg. Elemental concentrations were determined by EDS. The balance is oxygen.

Image of FIG. 4.
FIG. 4.

(Color online) Data from the mass spectrometer, showing the intensities of HCl+, MeCl+, H2O+, and MeO+ species detected in the exhaust stream. The deposition was done at 200 °C using the pulse sequence TiCl4-H2O-(MeO)3PO-H2O. The first four pulses are labeled; the sequence then repeats. The pulse lengths are slightly above what is needed for saturation; the H2O pulses following TiCl4 and (MeO)3PO are the same length.

Image of FIG. 5.
FIG. 5.

Comparison of P/Ti ratios obtained by EDS and XPS. The samples analyzed were deposited at 200 or 250 °C using 20 or 60 cycles. In order of increasing P/Ti ratios, the samples were deposited with the pulse sequences TiCl4-H2O-(MeO)3PO, TiCl4-H2O-(MeO)3PO-H2O (2 samples), and TiCl4-(MeO)3PO.

Image of FIG. 6.
FIG. 6.

Transmission electron microscope images of (a), (b) silica and (c), (d) silica with 60 ALD cycles titanium phosphate. The titanium phosphate was deposited at 250 °C using the sequence TiCl4-H2O-(MeO)3PO-H2O.

Image of FIG. 7.
FIG. 7.

Scanning electron microscope images of silica (a) uncoated, (b) with 20 cycles titanium phosphate, and (c) with 60 cycles titanium phosphate. The scale bar in each image is 200 nm.

Image of FIG. 8.
FIG. 8.

(Color online) (a) Surface area as a function of number of ALD cycles, as measured by the BET method. Shown are both the specific surface area (m2/g material) and the surface area of material that contains 1 g of the original silica substrate. (b) Si, Ti, and P concentrations as a function of number of deposition cycles. Cl <0.1% in all cases. Elemental concentrations were determined by EDS. The balance is oxygen. All depositions were done at 250 °C using the sequence TiCl4-H2O-(MeO)3PO-H2O.

Tables

Generic image for table
TABLE I.

Results of depositions with different pulse sequences at various saturation levels. Each deposition consisted of 20 cycles. Elemental concentrations were determined by EDS.

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/content/avs/journal/jvsta/30/1/10.1116/1.3664097
2011-12-09
2014-04-19
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752b84549af89a08dbdd7fdb8b9568b5 journal.articlezxybnytfddd
Scitation: Atomic layer deposition of titanium phosphate on silica nanoparticles
http://aip.metastore.ingenta.com/content/avs/journal/jvsta/30/1/10.1116/1.3664097
10.1116/1.3664097
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