CVD Cu2O and CuO NanosystemsCharacterized by XPSDavide BarrecaISTM-CNR and INSTM - Padova University, Department of Chemistry, Via Marzolo, 1, Padova,35131, Italy

Alberto Gasparottoa� and Eugenio TondelloPadova University and INSTM, Department of Chemistry, Via Marzolo, 1, Padova, 35131, Italy

�Received 14 July 2008; accepted 24 March 2009; published 22 July 2009�

In the present investigation, X-ray photoelectron and X-ray excited Auger electron spectroscopyanalyses of the principal core levels �O 1s, Cu 2p, and Cu LMM� of Cu2O and CuO nanosystemsare proposed. The samples were obtained by chemical vapor deposition starting from a novelsecond-generation copper�II� precursor, Cu�hfa�2·TMEDA �hfa�1,1,1,5,5,5-hexafluoro-2,4-pentanedionate; TMEDA�N,N,N’,N’- tetramethylethylenediamine�, under a dry O2atmosphere. The obtained route led to pure, homogeneous and single-phase Cu�I� and Cu�II� oxidenanosystems at temperatures of 300 and 500 °C, respectively, whose chemical nature could beconveniently distinguished by analyzing the Cu 2p band shape and position, as well as by evaluatingthe Auger parameters. The samples were characterized by O/Cu atomic ratios greater than theexpected stoichiometric values, due to marked interactions with the outer atmosphere attributed totheir high surface-to-volume ratio. © 2006 American VacuumSociety. �DOI: 10.1116/11.20080701�

Keywords: Cu2O; CuO; nanosystems; CVD; X-ray photoelectron spectroscopy

Accession #s: 1052 and 1053

Technique: XPS

Host Material: #01052: Cu2Osupported nanosystem;#01053: CuO supportednanosystem

Instrument: Perkin-Elmer PhysicalElectronics, Inc. 5600ci

Major Elements in Spectra: C, O,Cu

Minor Elements in Spectra: none

Published Spectra: 8

Spectra in Electronic Record: 12

Spectral Category: technical

PACS: 8116-c, 8115Gh, 7960Jv, 6146-w, 7322-f, 6150Nw

INTRODUCTION

Cu2O and CuO are nontoxic, abundant and inexpensive p-typesemiconductors with direct bandgap values of 2.1 and 1.2 eV,respectively �Refs. 1–4�. While the former crystallizes in a cubicstructure with a lattice parameter of 4.27 Å, CuO is monoclinicwith lattice parameters of a�4.684 Å, b�3.425 Å, c�5.129 Å,and ��99.28° �Ref. 5�. To date, both copper oxides representattractive candidates for applications in various fields, includingheterogeneous catalysis, magnetic storage media, thermoelectric,photothermal and photoconductive materials, solar energy conver-sion, gas sensing devices and anodes for Li-ion batteries �Refs.1–3 and 5–11�. To this regard, a great effort has recently beendevoted to devising proper synthetic strategies to nano- orsubmicrometer-sized Cu2O and CuO systems �Refs. 2, 3, and9–13�, since it is well recognized that the size- and shape-dependent properties characterizing nanostructured materials canopen broad perspectives for the improvement of functional prop-erties in several of the above applications.

In recent years, our research group has devoted several effortsto the sol-gel synthesis of Cu-, Cu2O-, and CuO-based nanosys-tems �either thin films or composites� with tailored characteristics�Refs. 4, 13, and 14�. Based on previous results, the present workis the first part of a research project aimed at the chemical vapordeposition �CVD�/Sol-Gel development of Cu-Ti-O nanocompos-ites with tailored characteristics in view of eventual applicationsas innovative electrodes in lithium-ion batteries. Despite the useof copper oxides in these applications has already been reported�Refs. 6–8 and 15�, the use of the above nanosystems opens at-tractive perspectives for forefront research activities in the field.

As a part of the ongoing investigation, we first focused ourattention on a CVD route towards Cu-O nanosystems with tai-

a�

Author to whom correspondence should be addressed.

Surface Science Spectra, Vol. 14, 2007 1055-5269/2007/14(1)

lored structure, composition, and morphology, with the aim ofidentifying the optimal operating conditions for the preparation ofpure Cu2O and CuO samples. Cu�hfa�2·TMEDA, a complex pos-sessing favorable characteristics for CVD use, has been adoptedfor the first time as a copper molecular source. The obtainedsamples were characterized by a multitechnique approach, namelyby glancing-incidence X-ray diffraction �GIXRD�, field emission-scanning electron microscopy �FE-SEM�, Fourier transform infra-red spectroscopy �FT-IR�, X-ray photoelectron �XPS�, and X-rayexcited Auger electron �XE-AES� spectroscopies. To this regard,the combined use of XPS and XE-AES was a powerful analyticaltool in order to discriminate between copper�I� and copper�II�-containing oxides. In this contribution, relevant data pertaining totwo representative single-phase specimens deposited on Si�100�substrates are analyzed.

SPECIMEN DESCRIPTION „ACCESSION #01052, 1 OF 2…

Host Material: Cu2O

CAS Registry #: 1317-39-1

Host Material Characteristics: homogeneous; solid; polycrystal-line; semiconductor; inorganic compound; see As ReceivedCondition

Chemical Name:: copper�I� oxide

Source: sample obtained by chemical vapor deposition �CVD� onSi�100�

Host Composition: Cu, O

Form: supported nanosystem

Lot #: CuO18

Structure: The GIXRD pattern of the sample, recorded at an in-cidence angle of 0.5°, presented two signals located at 2��36.3° and 2��42.2° that could be attributed to the �111� and

�200� reflections of cubic Cu2O �cuprite� �Ref. 16�. The mean

© 2006 American Vacuum Society 41/41/11/$23.00

crystallite size was �10 nm. No appreciable preferential ori-entations were detected.

History & Significance: The synthesis of the Cu�hfa�2·TMEDAcomplex used as precursor for the Cu-O nanostructures�99.99%� has been performed based on a previous literatureprocedure �Ref. 17�.

The sample was grown in an electronic grade O2 atmo-sphere by means of a cold-wall reduced pressure CVD appa-ratus. The custom-built reaction system �Refs. 18 and 19� con-sisted of a quartz chamber, equipped with a resistively heatedsusceptor and an external reservoir for the precursor vaporiza-tion. Mass transport of the precursor vapors to the depositionzone was performed by a 100 � 1 sccm O2 flow, while asupplementary oxygen flow of 100 � 1 sccm was introducedin the vicinity of the substrate surface. The deposition wasperformed on p-type Si�100� �MEMC®, Merano, Italy� at300 °C. Prior to the experiment, the substrate wafer was de-greased in dichloromethane, rinsed in 2-propanol and finallyetched in an aqueous HF solution �2%� for 3 min, in order toremove the native oxide layer from its surface. The precursorvaporization temperature, total pressure and experiment dura-tion were set at 70 °C, 10 mbar, and 120 min, respectively. Toavoid undesired condensation phenomena, the gas lines con-necting the water and precursor reservoirs to the reactionchamber were heated to 120 °C.

The obtained specimen was homogeneous, with a pink-bluish color.

As Received Condition: as grown

Analyzed Region: same as host material

Ex Situ Preparation/Mounting: sample mounted as received witha metallic clip to grounded sample holder and introduced intothe analysis chamber through a fast entry lock system

In Situ Preparation: none

Pre-Analysis Beam Exposure: The analyzed region was exposedto X-ray irradiation for alignment for a period no longer than 5min.

Charge Control: none

Temp. During Analysis: 298 K

Pressure During Analysis: �1 � 10�7 Pa

SPECIMEN DESCRIPTION „ACCESSION #01053, 2 OF 2…

Host Material: CuO

CAS Registry #: 1317-38-0

Host Material Characteristics: homogeneous; solid; polycrystal-line; semiconductor; inorganic compound; see As ReceivedCondition

Chemical Name:: copper�II� oxide

Source: sample obtained by chemical vapor deposition �CVD� onSi�100�

Host Composition: Cu, O

Form: supported nanosystem

Lot #: CuO14

Structure: The GIXRD pattern of the sample, recorded at an in-cidence angle of 0.5°, was characterized by reflections cen-tered at 2��35.5°, 38.7° and 48.8°, related respectively to the

¯ ¯

�002�/�111�, �111� and �202� planes of monoclinic CuO �teno-

42 Surface Science Spectra, Vol. 14, 2007

rite� �Ref. 20�. The average crystallite size was �10 nm. Simi-larly to the previous specimen, no appreciable preferential ori-entations were detected.

History & Significance: The sample was deposited by CVD start-ing from Cu�hfa�2·TMEDA under an oxygen atmosphere, inthe same conditions as the previous one �see description forAccession #1052�, except for the growth temperature that waskept at 500 °C. A uniform, brown-black and opaque depositwas obtained.

As Received Condition: as grown

Analyzed Region: same as host material

Ex Situ Preparation/Mounting: sample mounted as received witha metallic clip to grounded sample holder and introduced intothe analysis chamber through a fast entry lock system

In Situ Preparation: none

Pre-Analysis Beam Exposure: The analyzed region was exposedto X-ray irradiation for alignment for a period no longer than 5min.

Charge Control: none

Temp. During Analysis: 298 K

Pressure During Analysis: �1 � 10�7 Pa

INSTRUMENT DESCRIPTION

Manufacturer and Model: Perkin-Elmer Physical Electronics,Inc. 5600ci

Analyzer Type: spherical sector

Detector: multi-channel detector, part number 619103

Number of Detector Elements: 16

INSTRUMENT PARAMETERS COMMON TO ALLSPECTRA

� Spectrometer

Analyzer Mode: constant pass energy

Throughput „T�E N…: 0

Excitation Source Window: 1.5 µm Al window

Excitation Source: Al K�

Source Energy: 1486.6 eV

Source Strength: 250 W

Source Beam Size: 25000 µm �25000 µm

Signal Mode: multichannel direct

� Geometry

Incident Angle: 9°

Source to Analyzer Angle: 53.8°

Emission Angle: 45°

Specimen Azimuthal Angle: 0°

Acceptance Angle from Analyzer Axis: 0°

Analyzer Angular Acceptance Width: 14° � 14°

� Ion Gun

Manufacturer and Model: PHI 04-303A

Cu2O and CuO Nanosystems by XPS

Energy: 3000 eV

Current: 0.4 mA/cm2

Current Measurement Method: Faraday Cup

Sputtering Species: Ar

Spot Size „unrastered…: 250 µm

Raster Size: 2000 µm � 2000 µm

Incident Angle: 40°

Polar Angle: 45°

Azimuthal Angle: 111°

Comment: differentially pumped ion gun

DATA ANALYSIS METHOD

Energy Scale Correction: For both samples, no charging phe-nomena were detected.

Recommended Energy Scale Shift: 0

Peak Shape and Background Method: After a Shirley-typebackground subtraction �Ref. 26�, peak positions and widthswere determined from a least-square fitting procedure, adopt-ing Gaussian/Lorentzian functions.

Quantitation Method: The atomic concentrations were calculatedby using sensitivity factors taken from standard PHI V5.4Asoftware. The peak areas were measured above an integratedbackground.

ACKNOWLEDGMENTS

This work was financially supported by CNR-INSTM PROMOand CARIPARO Foundation within the project “Multi-layer opti-cal devices based on inorganic and hybrid materials by innovativesynthetic strategies”. Thanks are due to Mr. Loris Calore, Dr. Rob-erta Saini �Padova University� and Mr. Antonio Ravazzolo�ISTM-CNR� for valuable help in the synthesis and characteriza-tion of the precursor compound.

REFERENCES

1. Y. C. Zhang, J. Y. Tang, G. L. Wang, M. Zhang, and X. Y.Hu, J. Cryst. Growth 294, 278 �2006�.

2. M. Yang and J. -J. Zhu, J. Cryst. Growth 256, 134 �2003�.3. X. Wang, G. Xi, S. Xiong, Y. Liu, B. Xi, Y. Yu, and Y. Qian,

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Surface Science Spectra, Vol. 14, 2007

5. D. Chauan, V. R. Satsangi, S. Dass, and R. Shrivastav, Bull.Mater. Sci. 29, 709 �2006�.

6. J. Morales, L. Sànchez, F. Martìn, J. R. Ramos-Barrado, andM. Sànchez, Thin Solid Films 474, 133 �2005�.

7. J. Morales, L. Sànchez, S. Bijani, L. Martínez, M. Gabás, andJ. R. Ramos-Barrado, Electrochem. Solid State Lett. 8, A159�2005�.

8. S. Bijani, M. Gabás, L. Martínez, J. R. Ramos-Barrado, J.Morales, and L. Sànchez, Thin Solid Films 515, 5505�2007�.

9. Y. Liu, L. Liao, J. Li, and C. Pan, J. Phys. Chem. C 111,5050 �2007�.

10. W. -T. Yao, S. -H. Yu, Y. Zhou, J. Jiang, Q. -S. Wu, L. Zhang,and J. Jiang, J. Phys. Chem B 109, 14011 �2005�.

11. M. Kaur, P. Muthe, S. K. Despande, S. Choudhury, J. B.Singh, N. Verma, S. K. Gupta, and J. V. Yakhami, J. Cryst.Growth 289, 670 �2006�.

12. U. S. Chen, Y. L. Chueh, S. H. Lai, L. J. Chou, and H. S.Shih, J. Vac. Sci. Technol. B 24, 139 �2006�.

13. L. Armelao, D. Barreca, G. Bottaro, G. Mattei, C. Sada, andE. Tondello, Chem. Mater. 17, 1450 �2005�.

14. L. Armelao, D. Barreca, M. Bertapelle, G. Bottaro, C. Sada,and E. Tondello, Mater. Res. Soc. Symp. Proc. 737, F8.27.1�2003�.

15. J. Morales, L. Sànchez, F. Martìn, J. R. Ramos-Barrado, andM. Sànchez, Electrochim. Acta 49, 4589 �2004�.

16. Pattern No. 5-667, JCPDS �2000�.17. S. Delgado, A. Muñoz, M. E. Medina, and C. J. Pastor, In-

org. Chim. Acta 359, 109 �2006�.18. D. Barreca, A. Gasparotto, C. Maragno, E. Tondello, and C.

Sada, Chem. Vap. Deposition 10, 229 �2004�.19. D. Barreca, A. Gasparotto, C. Maragno, E. Tondello, E. Bon-

tempi, L. E. Depero, and C. Sada, Chem. Vap. Deposition11, 426 �2005�.

20. Pattern No. 45-937, JCPDS �2000�.21. R. P. Vasquez, Surf. Sci. Spectra 5, 257 �1998�.22. http://srdata.nist.gov/xps23. J. F. Moulder, W. F. Stickle, and K. D. Bomben, Handbook of

X-ray Photoelectron Spectroscopy �Perkin Elmer Corpora-tion, Eden Prairie, MN, 1992�.

24. R. P. Vasquez, Surf. Sci. Spectra 5, 262 �1998�.25. D. Briggs and M. P. Seah, Practical Surface Analysis: Auger

and X-ray Photoelectron Spectroscopy �Wiley, New York,1990�.

26. D. A. Shirley, Phys. Rev. B 5, 4709 �1972�.

Cu2O and CuO Nanosystems by XPS 43

SPECTRAL FEATURES TABLE

SpectrumID # Element/

Transition

PeakEnergy„eV…

Peak WidthFWHM„eV…

Peak Area„eV-cts/s…

SensitivityFactor

Concen-tration„at. %…

PeakAssignment

01052-02 C 1s 284.8 2.0 54574 0.296 47.6 advent. surface contamination

01052-03 a O 1s 530.2 1.8 47153 0.711 17.1 lattice oxygen in Cu2O

01052-03 a O 1s 531.6 1.8 38424 0.711 13.9 Adsorbed -OH groups/carbonates

01052-04 Cu 2p3/2 932.3 1.9 ··· ··· ··· Cu�I� in Cu2O

01052-04 Cu 2p1/2 952.2 1.9 ··· ··· ··· Cu�I� in Cu2O

01052-04 Cu 2p ··· ··· 440341 5.321 21.4 Cu�I� in Cu2O

01052-05 b Cu L3M45M45 916.8 ··· ··· ··· ··· Cu�I� in Cu2O

01053-02 C 1s 284.8 2.2 6399 0.296 22.4 advent. surface contamination

01053-03 a O 1s 529.7 1.7 21485 0.711 31.4 lattice oxygen in CuO

01053-03 a O 1s 531.6 2.1 12296 0.711 17.9 Adsorbed -OH groups/carbonates

01053-04 c Cu 2p3/2 933.9 3.2 ··· ··· ··· Cu�II� in CuO

01053-04 c Cu 2p1/2 953.9 3.2 ··· ··· ··· Cu�II� in CuO

01053-04 Cu 2p ··· ··· 145385 5.321 28.3 Cu�II� in CuO

01053-05 b Cu L3M45M45 917.9 ··· ··· ··· ··· Cu�II� in CuO

a The sensitivity factor is referred to the whole O 1s signal.b The peak position is given in KE.c The BE value is referred to the most intense spin-orbit split component.

Footnote to Spectrum 01052-02: While the main C1s component was assigned to adventitious hydrocarbon contamination, the shoulderlocated at Binding Energy �BE��288.5 eV was assigned to surface carbonates �Refs. 23 and 24�, whose presence likely arose by interaction withthe outer atmosphere. The surface C 1s photoelectron signal disappeared after 5’ Ar erosion, suggesting thus that carbon presence could be

attributed to atmospheric contamination and that the precursor had a clean decomposition pattern under the adopted conditions.

Footnote to Spectrum 01052-03: The O 1s surface peak presented a rather broad shape, suggesting the coexistence of different species.Indeed, the signal was fitted by two different bands, located at BE�530.2 eV �full width at half maximum �FWHM��1.8 eV, 55.1% of the totaloxygen� and 531.6 eV �FWHM�1.8 eV, 44.9% of the total oxygen�. While the former can be unequivocally ascribed to lattice oxygen in copper�I�oxide �Refs. 1, 6, 15, and 21–23�, the attribution of the second has been the object of controversy. Many authors assigned the high BE O 1scomponents to oxygen adsorbed on copper oxides �Refs. 2, 3, 9, 10, and 12�, despite contributions from surface -OH groups and carbonatespecies could not be unambiguously ruled out �Refs. 15 and 21–23�. In particular, the presence of carbonates was confirmed by the high BEcomponent of the C 1s peak �see comment to Accession #1052-2�. As a result, the surface O/Cu atomic ratio calculated considering the overalloxygen was 1.4, an appreciably higher value than the one expected for copper�I� oxide, while the O/Cu ratio obtained taking into account the sole

O lattice component at BE�530.2 eV yielded 0.80, a closer value to that pertaining to stoichiometric Cu2O.

Footnote to Spectrum 01052-04: The Cu 2p photoelectron peak was characterized by the absence of well detectable shake-up satellites,that enabled to exclude the presence of Cu�II� in appreciable amounts, suggesting the occurrence of copper�I� oxide �d10, a closed-shell system�

as the dominant specie �Refs. 7, 8, and 25�. Indeed, the Cu 2p3/2 BE value �932.3 eV; FWHM�1.9 eV� was in agreement with previous literaturereports for Cu2O �Refs. 1, 2, 7, 8, 15, and 21�. In addition, its presence could be verified by the evaluation of the Auger alpha parameter,calculated by the sum of Cu 2p3/2 BE and the Cu LMM Auger peak kinetic energy �KE� �alpha�BE�Cu 2p3/2� KE�Cu LMM��1849.1 eV�, that

agreed to a good extent with literature values for copper�I� oxide �Refs. 1, 4, 7, 8, and 21�.

Footnote to Spectrum 01053-02: The C 1s peak tailing towards the high binding energy �BE� side was assigned to the presence of surfacecarbonates �Refs. 23 and 24� arising by interaction with the outer atmosphere. The surface C 1s photoelectron signal fell to noise level after 5’

Ar erosion, suggesting thus that the precursor had a clean decomposition pattern under the adopted conditions.

Footnote to Spectrum 01053-03: Similarly to the results reported for the Cu2O specimen �compare spectrum #1053-03�, the O 1s surfacesignal was fitted by two different bands, located at BE�529.7 eV �FWHM�1.7 eV, 63.6% of the total oxygen� and 531.6 eV �FWHM�2.1 eV,36.4% of the total oxygen�. The former was due to lattice O in CuO �Refs. 6, 14, 15, and 22–24�. As regards the second, it has been ascribed tooxygen adsorbed on copper oxides �Refs. 2, 3, 9, 10, and 12�, despite contributions from surface -OH groups and carbonate species could notbe ruled out �Refs. 14 and 21–24�. In particular, the presence of carbonates was confirmed by the high BE component of the C 1s peak �seecomments to spectra #1052-2 and 1053-2�. As a result, the surface O/Cu atomic ratio calculated considering the overall oxygen was 1.7, a highervalue than the one expected for copper�II� oxide. A similar phenomenon has already been documented for CuO films obtained by spray pyrolisis�Refs. 6 and 15�. Conversely, the O/Cu ratio obtained taking into account the sole O lattice component at BE�529.7 eV yielded 1.1, a closer

value to that pertaining to stoichiometric CuO.

Footnote to Spectrum 01053-04: The Cu 2p photoelectron peak displayed the presence of intense shake-up satellites centered at BE

44 Surface Science Spectra, Vol. 14, 2007 Cu2O and CuO Nanosystems by XPS

values ca. 9.0 eV higher than the main spin-orbit split componentsconfiguration interaction in the final state due to relaxation phenomespecies �Ref. 4, 11–13, and 25�. In addition, the presence of CuO�BE�Cu 2p3/2��933.9 eV; FWHM�3.2 eV� and the Auger alpha paratent with previous reports on copper�II� oxide �Refs. 1, 3, 6, 9, 10, 1

ANALYZER CALIBRATION TABLE

SpectrumID # Element/

Transition

PeakEnergy„eV…

Peak WidthFWHM„eV…

Peak Area„eV-cts/s…

SensitivityFactor

Concen-tration„at. %…

PeakAssignment

01054-01 a Au 4f7/2 84.0 1.4 186403 3.536 ··· metallic gold

01055-01 a Cu 2p3/2 932.7 1.6 86973 3.547 ··· metallic copper

a

The peak was acquired after Ar erosion.

GUIDE TO FIGURES

Spectrum„Accession… #

SpectralRegion

VoltageShift* Multiplier Baseline Comment #

1052-1 survey 0 0 0 1

1052-2 C 1s 0 0 0 1

1052-3 O 1s 0 0 0 1

1052-4 Cu 2p 0 0 0 1

1053-1 survey 0 0 0 2

1053-2 C 1s 0 0 0 2

1053-3 O 1s 0 0 0 2

1053-4 Cu 2p 0 0 0 2

1052-5 �NP�** Cu LMM 0 0 0 1

1053-5 �NP� Cu LMM 0 0 0 2

1054-1 �NP� Au 4f7/2 0 0 0 3

1055-1 �NP� Cu 2p3/2 0 0 0 3

* Voltage shift of the archived �as-measured� spectrum relative to the printed figure. The figure reflects the recommended energy scale correctiondue to a calibration correction, sample charging, flood gun, or other phenomenon.** �NP� signifies not published; digital spectra are archived in SSS database but not reproduced in the printed journal.1. Cu2O2. CuO

. Such satellites, that have been attributed to the occurrence of a strongna, have a diagnostic value as a fingerprint for the presence of d9 copper�II�as the dominant Cu-O phase was further confirmed by the peak positionmeter �alpha�BE�Cu 2p3/2� KE�Cu LMM��1851.8 eV�, that were consis-2, 14, 15, and 24�.

3. Calibration spectrum

Surface Science Spectra, Vol. 14, 2007 Cu2O and CuO Nanosystems by XPS 45

Accession# 01052–01

Host Material Cu2O supported nanosystem

Technique XPS

Spectral Region survey

Instrument Perkin-Elmer Physical Electronics, Inc. 5600ci

Excitation Source Al K�

Source Energy 1486.6 eV

Source Strength 250 W

Source Size 25000 µm �25000 µm

Analyzer Type spherical sector

Incident Angle 9°

Emission Angle 45°

Analyzer Pass Energy: 187.85 eV

Analyzer Resolution 1.9 eV

Total Signal Accumulation Time 101.3 s

Total Elapsed Time 111.5 s

Number of Scans 3

Effective Detector Width 1.9 eV

46 Surface Science Spectra, Vol. 14, 2007 Cu2O and CuO Nanosystems by XPS

� Accession #: 01052–02

� Host Material: Cu2O supportednanosystem

� Technique: XPS

� Spectral Region: C 1s

Instrument: Perkin-Elmer PhysicalElectronics, Inc. 5600ci

Excitation Source: Al K�

Source Energy: 1486.6 eV

Source Strength: 250 W

Source Size:25000 µm �25000µm

Analyzer Type: spherical sector

Incident Angle: 9°

Emission Angle: 45°

Analyzer Pass Energy: 58.7 eV

Analyzer Resolution: 0.6 eV

Total Signal Accumulation Time:160.8 s

Total Elapsed Time: 176.9 s

Number of Scans: 16

Effective Detector Width: 0.6 eV

Comment: See footnote below theSpectral Features Table.

� Accession #: 01052–03

� Host Material: Cu2O supportednanosystem

� Technique: XPS

� Spectral Region: O 1s

Instrument: Perkin-Elmer PhysicalElectronics, Inc. 5600ci

Excitation Source: Al K�

Source Energy: 1486.6 eV

Source Strength: 250 W

Source Size:25000 µm �25000µm

Analyzer Type: spherical sector

Incident Angle: 9°

Emission Angle: 45°

Analyzer Pass Energy: 58.7 eV

Analyzer Resolution: 0.6 eV

Total Signal Accumulation Time:160.8 s

Total Elapsed Time: 176.9 s

Number of Scans: 16

Effective Detector Width: 0.6 eV

Comment: See footnote below theSpectral Features Table.

Surface Science Spectra, Vol. 14, 2007 Cu2O and CuO Nanosystems by XPS 47

� Accession #: 01052–04

� Host Material: Cu2O supportednanosystem

� Technique: XPS

� Spectral Region: Cu 2p

Instrument: Perkin-Elmer PhysicalElectronics, Inc. 5600ci

Excitation Source: Al K�

Source Energy: 1486.6 eV

Source Strength: 250 W

Source Size:25000 µm �25000µm

Analyzer Type: spherical sector

Incident Angle: 9°

Emission Angle: 45°

Analyzer Pass Energy: 58.7 eV

Analyzer Resolution: 0.6 eV

Total Signal Accumulation Time:400.8 s

Total Elapsed Time: 440.9 s

Number of Scans: 16

Effective Detector Width: 0.6 eV

Comment: See footnote below theSpectral Features Table.

48 Surface Science Spectra, Vol. 14, 2007 Cu2O and CuO Nanosystems by XPS

Surface Science Spectra, Vol. 14, 2007

01053–01

CuO supported nanosystem

XPS

survey

Perkin-Elmer Physical Electronics, Inc. 5600ci

Al K�

1486.6 eV

250 W

25000 µm �25000 µm

spherical sector

9°

45°

187.85 eV

1.9 eV

135.1 s

148.6 s

4

1.9 eV

Accession#

Host Material

Technique

Spectral Region

Instrument

Excitation Source

Source Energy

Source Strength

Source Size

Analyzer Type

Incident Angle

Emission Angle

Analyzer Pass Energy:

Analyzer Resolution

Total Signal Accumulation Time

Total Elapsed Time

Number of Scans

Effective Detector Width

Cu2O and CuO Nanosystems by XPS 49

50 Su

� Accession #: 01053–02

� Host Material: CuO supportednanosystem

� Technique: XPS

� Spectral Region: C 1s

Instrument: Perkin-Elmer PhysicalElectronics, Inc. 5600ci

Excitation Source: Al K�

Source Energy: 1486.6 eV

Source Strength: 250 W

Source Size:25000 µm �25000µm

Analyzer Type: spherical sector

Incident Angle: 9°

Emission Angle: 45°

Analyzer Pass Energy: 58.7 eV

Analyzer Resolution: 0.6 eV

Total Signal Accumulation Time:120.6 s

Total Elapsed Time: 132.7 s

Number of Scans: 12

Effective Detector Width: 0.6 eV

Comment: See footnote below theSpectral Features Table.

� Accession #: 01053–03

� Host Material: CuO supportednanosystem

� Technique: XPS

� Spectral Region: O 1s

Instrument: Perkin-Elmer PhysicalElectronics, Inc. 5600ci

Excitation Source: Al K�

Source Energy: 1486.6 eV

Source Strength: 250 W

Source Size:25000 µm �25000µm

Analyzer Type: spherical sector

Incident Angle: 9°

Emission Angle: 45°

Analyzer Pass Energy: 58.7 eV

Analyzer Resolution: 0.6 eV

Total Signal Accumulation Time:120.6 s

Total Elapsed Time: 132.7 s

Number of Scans: 12

Effective Detector Width: 0.6 eV

Comment: See footnote below theSpectral Features Table.

rface Science Spectra, Vol. 14, 2007 Cu2O and CuO Nanosystems by XPS

S

� Accession #: 01053–04

� Host Material: CuO supportednanosystem

� Technique: XPS

� Spectral Region: Cu 2p

Instrument: Perkin-Elmer PhysicalElectronics, Inc. 5600ci

Excitation Source: Al K�

Source Energy: 1486.6 eV

Source Strength: 250 W

Source Size:25000 µm �25000µm

Analyzer Type: spherical sector

Incident Angle: 9°

Emission Angle: 45°

Analyzer Pass Energy: 58.7 eV

Analyzer Resolution: 0.6 eV

Total Signal Accumulation Time:300.6 s

Total Elapsed Time: 330.7 s

Number of Scans: 12

Effective Detector Width: 0.6 eV

Comment: See footnote below theSpectral Features Table.

urface Science Spectra, Vol. 14, 2007 Cu2O and CuO Nanosystems by XPS 51