Carbonitriding of silicon using plasma focus device

Carbonitriding of silicon using plasma focus deviceS. Jabbar, I. A. Khan, and R. Ahmada�

Department of Physics, GC University, 54000 Lahore, Pakistan

M. ZakaullahDepartment of Physics, Plasma Physics Laboratory, Quaid-i-Azam University, Islamabad 45230, Pakistan

J. S. PanInstitute of Materials Research and Engineering, Agency for Science, Technology and Research (A*STAR),3 Research Link, Singapore 117602, Singapore

�Received 6 November 2008; accepted 26 January 2009; published 27 February 2009�

Carbonitride thin films have been deposited on silicon substrate by the irradiation of energeticnitrogen ions emanated from dense plasma focus device. The carbon ions are ablated by theirradiation of relativistic electrons from the insert material �graphite� placed at the anode tip. Thex-ray diffraction analysis demonstrates that a polycrystalline thin film consisting of variouscompounds such as Si3N4, SiC, and C3N4 is formed on the silicon �100� substrate. Crystallinity ofdifferent compounds decreases with the increase in angular positions �0°, 10°, and 20°�. Ramanspectroscopy shows the appearance of graphitic and disordered bands with silicon nitride and siliconcarbide indicating the formation of carbonitride. Raman spectra also indicate that broadening ofbands increases with the increase in focus deposition shots, leading to the amorphization of the thinfilm. The amorphization of the thin films depends on the ion energy flux as well as on the sampleangular position. The scanning electron microscopy exhibits the damaging of the substrate surfaceat 0° angular position. The microstructure shows the tubular shape for higher ion dose �40 focusshots�. At 10° angular position, a two phase phenomenon is observed with the ordered phase in thesolid solution. A smooth and uniform surface morphology showing a small cluster is observed for
the 20° angular position. © 2009 American Vacuum Society. �DOI: 10.1116/1.3085720�
I. INTRODUCTION

Dense plasma focus �DPF� device is emerging as a pow-erful tool for ion implantation on different types of materialssuch as conductors, semiconductors, and insulators.1–3 Thinfilms deposited using DPF can be crystalline or amorphousdepending on the energy and flux of the energetic ion beamemitted during the radial collapse phase.4 In the recent re-search of surface treatment, pulsed ion implanters have re-ceived much attention due to their simplicity and low cost.The DPF is also a simple pulsed coaxial accelerator thatmakes use of a self-generated magnetic field and confines theplasma to a very high density �1019 cm−3� and high tempera-ture �1–2 keV�.5,6 The energetic ions emitted from the focusregion are suggested for the surface treatment on materials.7

Kelly et al.8 found that a thin and well-adhered coating onmetallic samples is possible by using a metallic insert in theanode tip. Masugata et al.9 proposed the pulsed ion beamemitted from DPF for surface treatment on semiconductors.It seems very attractive especially for high melting pointsemiconductors such as silicon carbide.10

Silicon carbonitride �SiCxNy :x�y� has received a consid-erable attention as a versatile material that combines the bestproperties of silicon nitride and carbon nitride.11 SiCN hashigh hardness and enhanced oxidation and corrosion resis-tance, and these improved properties are suggested to be dueto complex covalent chemical bonding and low oxygen dif-

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381 J. Vac. Sci. Technol. A 27„2…, Mar/Apr 2009 0734-2101/2009

fusion coefficient in the amorphous structure of the siliconcarbonitride thin films.12,13 Silicon and carbon have smallradii so it is expected that the tertiary compound SiCN has awide band gap �about 3.8 eV� �Ref. 14� and high hardnessand thermal conductivity.15,16

Thin films of silicon carbonitride material have been syn-thesized using different deposition techniques such as rf in-duction plasma,17 enhanced rf magnetron sputtering,18

chemical vapor deposition,19 plasma enhanced chemical va-por deposition,20 etc. But there are some difficulties in thesynthesis of crystalline carbonitride film, which is supposedto be formed due to the following two reasons: �1� The crys-talline CN is metastable under a low pressure condition ofvapor deposition and �2� the density of active N atoms isinsufficiently high in most conventional deposition tech-niques. We reported for the first time the deposition ofc-SiCN using DPF device in this paper, demonstrating thatDPF is a good technique for the deposition of c-SiCN forvery small numbers of focus shots.

The deposited films consist of various phases such as�-Si3N4, �-SiC, and �-C3N4 on the silicon substrate. Thecharacterization of the deposited films is carried out usingx-ray diffraction �XRD�, scanning electron microscopy�SEM�, and Raman spectroscopy.

II. EXPERIMENTAL WORK

DPF device with energy up to 2.3 kJ per shot operating inthe nitrogen environment at a pressure of 1.25 mbar has been
used for ion deposition on the Si�100� surface. The carbon
381/27„2…/381/7/$25.00 ©2009 American Vacuum Society

382 Jabbar et al.: Carbonitriding of silicon using plasma focus device 382

and nitrogen ions are emitted along the axis of the coaxialaccelerator within a cone having an aperture angle varying inthe range 30°–70° depending on the ion energy, and the elec-trons are accelerated in the opposite direction toward thecentral electrode due to the induced electric field in the radialcollapse phase, which is produced due to the rapid change ininductance of the plasma column. An induced electric field isproduced in the plasma column, which accelerates the ionsand electrons towards the opposite poles of the field. Wemake use of both species by placing the target in the path ofelectrons which sputter the target, and the subsequent ionsmove toward the substrate and are deposited on the surfaceof the material. A two-dimensional schematic of the elec-trode system is shown in Fig. 1. The purity of nitrogen ionsincreases up to 91% with engraved anode.21 The depth of thehole engraved on the top of the anode is 20 mm and theanode is fitted on a 10 mm thick circular copper plate calledthe anode header. The circular T-shape graphite insert isplaced in the hole at the tip of the anode so that it covers thecopper electrode completely to avoid impurities from the an-ode material.

The samples of Si �100� are attached to the sample holder,placed at different distances from each other depending onthe angles �0°, 10°, or 20°� with respect to the anode axis atan axial position of 9 cm. A shutter is used in order to avoidthe test focus shots.

The high voltage of about +12 kV is transferred from thecapacitor bank to the electrode system via triggertron typesparkgap. When good and reproducible focusing signalsfrom the high voltage probe and the Rogowski coil on the

FIG. 1. Schematic of the Mather type plasma focus device.

TDS 500 MHz phosphor oscilloscope were obtained, the

J. Vac. Sci. Technol. A, Vol. 27, No. 2, Mar/Apr 2009

shutter was removed and the samples were exposed for treat-ment. The total procedure from the charging of the capacitorto the end of the focusing of plasma column is called “onefocus shot,” and different numbers of focus shot are taken tofind the dependence of the thin film properties on the in-creasing numbers of shots. The details of the experimentalsetup can be found in our earlier published literature.1–3

III. RESULTS AND DISCUSSION

The XRD analysis of the thin films was performed usingan X’Pert PRO MPD x-ray diffractometer using Cu K� ��=1.5406 Å� radiations. The XRD patterns of the thin filmsdeposited at 0° angular position for different numbers of fo-cus shots �10, 20, 30, and 40� are shown in Fig. 2. The newpeaks at different diffraction angles �28.3° and 56.7°� areassigned to the Si �111� and Si �311� phases,22–24 respec-tively, showing that the long range order of the Si �100�substrate is broken and new compounds such as silicon ni-tride �Si3N4�, carbon nitride �C3N4�, and silicon carbide�SiC� are identified. The formation of �-C3N4 and �-Si3N4

phases indicates the deposition of SiCN films.25

The XRD peaks identified for the �-Si3N4 phase at 0°angular position for different deposition focus shots26–31 hav-ing small shifts toward higher angles are shown in Fig. 2.These shifts show the presence of compressive stresses in thedeposited films, indicating the decrease in d values. Table Ishows that for ten focus shots, there is an increase in theobserved d values from standard d values for all phases ex-cept for the Si3N4 �3 1 8� phase. The reason for this decreasein d value for Si3N4 phase is that nitrogen atoms have largerionic radii than silicon and they enter into the lattice as in-terstitials producing the tensile stresses. But, at the sametime, relaxation in the deposited film is being produced dueto high temperature and thermal shocks, which are attributed

FIG. 2. XRD patterns of thin films at 0° angular position for different num-bers of focus shots.

to the crystal growth of compounds. Intensities of the peaks


decrease with focus shots showing the resputtering, recrys-tallization, and amorphization of the previously depositedfilm.

Different phases of �-SiC �Refs. 32 and 33� are also iden-tified from the XRD pattern. Silicon and carbon belong to thesame group of the Periodic Table and have close ionic radii.Thus the incorporation of carbon atoms decreases d values�see Table I� thereby inducing small compressive stresses.The estimated crystallite sizes of �-SiC planes are found tolie in the range of 2 to 12 nm using Debye–Scherrer for-mula. It is known that crystallite sizes of the compound aredirectly related to the film hardness.34 It has also been re-ported that for the crystallite sizes of about 70 nm,34

20 nm,35 and 10–20 nm,36 the maximum hardness is foundto be around 27, 37, and 50 GPa, respectively. Thus we cansuggest that film hardness in our case can be more than50 GPa since the crystallite sizes of the phases are smallercomparatively.

The �-C3N4 is a superhard material which has a hardnesscomparable with the hardness of diamond. During the radialcollapse phase, the temperature of the ion species reacheshundreds of eV, which is considered suitable for the forma-tion of C3N4.11 The up and down shifting in C3N4 peaksfrom the stress-free data with increasing focus shots indicatesthe presence of residual stresses �compressive and tensile� inthe films. Graphitelike carbon nitride �Gr.C3N4� has recentlyattracted much attention because it has a highly stable geom-etry. Both precursor ions of graphite and nitrogen may reactwith each other on their way and onto the substrate formingcarbon nitride.37 The peak observed at 43.3° angle may alsobe an indication of the formation of Gr.C3N4 �200�compound.38 The d values of carbon nitride compound de-creases with increasing focus shots �Table I�.

The XRD patterns of the film deposited with differentnumbers of focus shots �10, 20, 30, and 40� at 10° angular

TABLE I. List of different compounds detected from the XRD patterns alongwith the observed d values of different planes.

Differentcompounds

formed duringdeposition

Standard dvalues

�Å�

Observed d values �Å� fordifferent number of

focus shots

10 20 30 40

Si3N4 �2 1 5� 2.2853 2.2897 2.2897 2.897 2.2897Si3N4 �3 0 4� 2.0988 2.1001 2.0973 2.0931 2.0889Si3N4 �3 0 8� 1.8764 1.8786 1.8786 1.8786 1.8731Si3N4 �3 1 8� 1.6298 1.6294 1.6269 1.6269 1.6229Si3N4 �1 4 3� 1.4198 1.4246 1.4228 1.4217 1.4182SiC �1 1 1� 2.5084 2.5055 2.5055 2.5055 2.4954SiC �1 0 52� 1.9174 1.9169 1.9169 1.9134 1.9111SiC �0 1 117� 1.6079 1.6042 1.6042 1.6042 1.6004SiC �0 1 101� 1.5250 1.5241 1.5241 1.5241 1.5241SiC �1 1 33� 1.4772 1.4739 1.4739 1.4739 1.4727C3N4 �0 0 3� 3.0643 3.0601 3.0601 3.0446 3.0446C3N4 �2 2 0� 1.9082 1.9169 1.9169 1.9134 1.9082C3N4 �0 0 6� 1.5321 1.5228 1.5227 1.5261 1.5261

position are shown in Fig. 3. The peaks at angles 28.3° and

JVST A - Vacuum, Surfaces, and Films

29.3° have low intensity at 10° and ten focus shots, whereasthese are comparatively sharp and intense at 0° for ten focusshots. Their intensities increase at 20 focus shots because 10focus shots are insufficient for the good crystallization syn-thesis of these phases at 10° angular position. For 40 focusshots it decreases again, which shows the amorphization ofthe phase occurring for higher numbers of focus shots. Thereis a small shift in all peaks at higher angle for 20 focus shots,but there is no shift for 30 and 40 focus shots with respect tothe 10 focus shots. This indicates that no further relaxation ispossible with increasing focus shots, which may be due tothe appearance of �-Si3N4 �310� phase at 49.9° �Ref. 27� for30 shots. This peak disappeared at 40 focus shots due toresputtering, which may be due to more energy delivered tothe substrate. The peak at an angle of about 47.3° is resolvedinto three peaks showing the complex bonding betweenSiuN, SiuC, and CuC.27–31,33

For 20° angular position, the XRD pattern �Fig. 4� showssimilar phases as observed in Figs. 2 and 3. No considerable

FIG. 3. XRD patterns of thin film at 10° angular position for different num-bers of focus shots.

FIG. 4. XRD patterns of thin film at 20° angular position for different num-
bers of shots.


shifts are observed even for 40 focus shots. These peaksindicate that different compounds of silicon carbide, siliconnitride, and carbon nitride are formed with complex structureas expected, indicating the formation of a ternary compoundlayer of silicon carbonitride. The overall XRD analysis of thethin films deposited at 0° angular position for different focusshots shows that the nanocrystals in the films have differentphase compositions and shows the possible presence of acomplex structure in the films. The peaks with a sufficientsignal-to-noise ratio at slightly shifted angles also lead to theformation of SiCN.11

IV. RAMAN ANALYSIS

Raman spectroscopic measurements are carried out to in-vestigate the surface structure of the treated samples by ana-lyzing the phonon frequencies in a backscattering geometrywith Avantes AvaRaman microscope equipped with a con-tinuous wave diode laser of 785 nm line.

The Raman spectra for thin films of untreated and treatedsamples at 0° angular positions for different numbers of fo-cus shots �10, 20, 30, and 40� are shown in Fig. 5. For theuntreated Si �100� sample, a sharp peak is obtained at518 cm−1 and there is a decrease in the intensity after tenfocus shots and, finally, it vanishes at 40 shots. For thetreated sample at 20 focus shots, we find a small and broadspectrum in the range 1300–1700 cm−1 indicating the forma-tion of D �disorder� and G �graphite� bands centered at about1332 and 1590 cm−1, respectively, which are typical of struc-tures possessing sp2 bonding.38 The D band shows that thelong range order of the crystalline material is lost and thecarbon phase becomes glassy and both the G and D bandsbroaden.39 The spectrum is continuous and separate peaksare absent, probably due to the dangling bonds and brokenlattice symmetry.30 After 20 focus shots, the peak for crys-talline Si �100� remains no longer, and at 40 focus shots, thespectrum for D and G modes is almost absent and the prod-uct formed is generally a carbon-rich material.

For 10° angular position at different focus shots, the Ra-man spectra are shown in Fig. 6. The intensity of the peaksdecreases with increasing number of shots, which is the ef-

32

FIG. 5. Raman spectra of thin film at 0° angular position for different num-bers of shots.

fect that takes place with decreasing crystallite sizes. These


Raman shifts are more prominent than others at differentnumbers of focus shots at 20°, as shown in Fig. 6. The sameG and D modes are observed in the range 1300–1600 cm−1

centered at 1350 and 1540 cm−1. The characteristic peak dueto covalent CuN bond is prominent for 20 shots at1248 cm−1.

It was estimated that the stretching frequency of the co-valent nitrogen-carbon single bonds is in the range1212 to 1265 cm−1.40 Feng et al.41 also found a peak at about1248 cm−1 and assigned this to CuN covalent bonds. Thecharacteristic peak assigned to a covalent CwN bond at2200 cm−1 in the Raman spectra of carbon nitride films withhigher nitrogen contents is not detectable in this work,42

which may indicate that the CNx films prepared by plasmafocus device contain very small amounts of nitrogen.25 TheRaman features at about 760, 1718, and 1899 cm−1 are as-signed to the silicon carbide �SiC�.32,40,41 From the band cen-tered at 760 cm−1, it is estimated that the size of the SiCcrystal is less than or equal to 20 nm,32 and also the broadband centered at about 860 cm−1 has been observed previ-ously in nanosize SiC,42 which is considered due to the de-fects in the structure of the film. Silicon carbide is a materialthat effectively absorbs light, including the incident laserlight. The variation of the sample temperature for subsequentRaman measurements modifies the phonon feature in Ramanspectra, i.e., shifting toward lower frequencies and a sym-metric broadening with increasing temperature,43 and bothphenomena can be speculated in the Raman spectra in Fig. 6.

The Raman shift in the region 820–1100 cm−1 is alsoidentified as that of silicon nitride �SiN�. The silicon peak atabout 520 cm−1 is broadened due to the stresses and defectsin the film, and the shoulder appearing with the silicon ref-erence peak at 20 shots shows the presence of amorphousSiuSi vibrations.44

The Raman pattern for the samples placed at 20° angularposition at different focus shots is shown in Fig. 7. The sameD and G modes in broad humps at 1170–1435 cm−1 and1450–1650 cm−1 are observed. At ten focus shots the inten-sity of the silicon peak is increased and it is also shifted

FIG. 6. Raman spectra of thin film at 10° angular position for differentnumbers of shots.

toward the higher frequency, representing that the very small


uniaxial stresses produced in the sample and the increase inthe intensity of the peak may be produced due to the differ-ence in the calibration of the laser light onto the surface ofthe sample.45,46 By increasing the number of focus shots,there is an increasing symmetric broadening in the peak forsilicon which shows that defects are being produced in thesample with increasing numbers of shots and shows the pres-ence of amorphous SiuSi vibrations.32,42–44 For 40 focusshots, a sharp peak of high intensity is attributed to the crys-talline SiuN vibrations.47

V. SEM ANALYSIS

The SEM analysis of the thin film was performed using aJEOL scanning electron microscope at the Institute of Mate-rials Research and Engineering, Singapore.

The SEM micrograph for untreated sample is shown inFig. 8�a� showing that the surface of the substrate is smooth.For ten focus shots for 0° at 1000� resolution �Fig. 8�b��,

FIG. 7. Raman spectra of thin film at 20° angular position for differentnumbers of shots.

FIG. 8. SEM micrographs of different samples for ten shots for differentangular positions. �a� Micrograph of untreated sample. �b� Micrograph ofthin film at 0° angular position at 1000� resolution. �c� Micrograph of thinfilm at 0° angular position at 6000� resolution. �d� Micrograph of thin film
at 10° angular position at 6000� resolution.

equiaxed and irregularly sized grains are found and theirgrain boundaries are fine, and there is no gap between thetwo adjacent grains sharing the same boundary. In the regionbetween the grains, there is a volcanic-structure-like concen-tric ring which may be due to the dominating sputtering phe-nomenon. In some regions we can say that the film is finegrained and some precipitates are observed, while most areconcentrated near the grain boundaries. At higher resolutionin Fig. 8�c� it can clearly be seen that these precipitates con-centrate near the grain boundaries. For ten focus shots at 10°at the same resolution as shown in Fig. 8�d�, a very smoothsurface is observed with some clusters in the vicinity of thethin film. The scratches behind the cluster indicate that it isloosely bound with the surface of the film and the thrust ofthe ions coming behind fluxes of ions forced it to move alongthe surface of the material, but the overall surface is smooth.

For 30 focus shots at 0°, a thin film structure appears to belike snowflakes placed sheet by sheet on each other, asshown in Fig. 9�a�. The wide gaps between the boundariescan be observed, which shows that the grains are becomingdenser and the thickness of the film increases with increasingnumber of shots. The shining regions in the micrograph areobserved to be the phenomenon which occurs in solid solu-tions either due to extra reflection or due to diffused scatter-ing associated with several different precipitation and trans-formation phenomena.48 At 10° for 30 focus shots as shownin Fig. 9�b�, the surface seems to be totally different at alower resolution of 100 �m, showing the formation of sometubular structure which seems like the micrograph for 0° butwith higher thickness.

This may occur due to the stresses produced on the sur-face of the film resulting from the temperature gradients inthe surface of the sample. The surface damage can clearly beseen due to sputtering. In the same sample at a higher reso-

FIG. 9. SEM micrographs for different samples at 30 shots for differentangular positions. �a� Micrograph of thin film at 0° angular position at1000� resolution. �b� Micrograph of thin film at 10° angular position at100� resolution. �c� Micrograph of thin film at 10° angular position at6000� resolution. �d� Micrograph of thin film at 20° angular position at6000� resolution.

lution of 2 �m in Fig. 9�c�, the two phase mixture phenom-


enon, consisting of a solid solution and an ordered phase, isobserved. Ordered precipitates nucleated randomly near theboundaries are aligned now symmetrically as they growalong a specific soft direction in crystals48 elongated in thehorizontal and vertical positions. At 20° for 30 shots, asmooth and homogeneous surface with some clusters in thevicinity of the film is observed as shown in Fig. 9�d�.

Increasing the number of focus shots to 40 at 0° as shownin Fig. 10�a�, we observe long cylindrical tubes of about2 �m diameter. At higher resolution in Fig. 10�b�, the struc-ture is petal-like such that the sheets of petals are placed ontop of one another in which the sheet of bigger radius is inthe middle and the sheets of petals with less radius are onboth sides forming a cylindrical shape. Figure 10�c� shows arough surface of the film which may be due to the ionicbonds of SiuN, SiuC, and CuN.49 In Fig. 10�d� athigher resolution, the surface is again like snowflakes withsharp grain boundaries, which shows that the thin film de-posited is crystalline.

VI. CONCLUSION

The analysis of the treated samples shows that a thin filmof carbonitride can be deposited on Si �100� surface with ionbombardment. The results of different characterization tech-niques used for the analysis of the film are quite consistentwith each other. A systematic analysis of the XRD patternsdemonstrates that a polycrystalline thin film having differentcompounds �Si3N4, SiC, and C3N4� is formed on the surfaceof the Si �100�. For 10° and 20° angular positions, the XRDspectra show the formation of crystalline thin films. For 10°angular position, the crystallinity of the films deteriorateswith increasing ion dose. For 20° angular position, almostthe same trend in the deterioration of crystallinity of the thinfilm is observed. The XRD peaks of new compounds on Si�100� substrate indicate that the superhard material of carbonnitride is formed.

The Raman analysis of the treated samples also supportsthe XRD analysis. The G and D bonds in the Raman spectra

FIG. 10. SEM micrographs for different samples at 40 shots for differentangular positions. �a� Micrograph of thin film at 0° angular position at6000� resolution. �b� Micrograph of thin film at 0° angular position at20 000� resolution. �c� Micrograph of thin film at 10° angular position at1000� resolution. �d� Micrograph of thin film at 20° angular position at20 000� resolution.

in all the samples indicate the formation carbon nitride phase


accompanied by some other bands of silicon nitride and sili-con carbide. The broadening of the bands at higher numberof shots reveals the amorphization of the film with increasingion dose. It was found that at 10° and 20°, the extent ofamorphization of the film is lower than at 0° with increasingnumber of focus shots.

From the SEM micrographs it was found that the surfaceof the substrate has significant damage at 0° angular position.The grain size appears to decrease with increasing focusshots. For 0° angular position, the surface morphology of thefilm changes to a tubular shape at 40 shots. For 10° angularposition, two phase phenomenon is observed with the or-dered phase in the solid solution. For 20° angular position,the film seems to be quite smooth and uniform showing thepresence of some clusters.

All of the above results show that a Mather type plasmafocus device, energized by a 15 kV capacitor, is a good tech-nique for crystalline silicon carbonitride growth, which isdeposited for the first time in this work.

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Carbonitriding of silicon using plasma focus device

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