raman spectroscopy: about chips and stress · the effect of processing parameters and materials...

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6 ©Spectroscopy Europe 2003 Spectroscopy Europe 15/2 (2003) RAMANSPECTROSCOPY Introduction Stress in microelectronics Moore’s law * dictates microelectron- ics researchers to make integrated cir- cuit (IC) devices smaller and to put them as close to each other as possible on a chip. This results in a better per- formance and a larger functionality of the chips. However, these devices also require a good electrical isolation from each other. This is in general done by the formation of a thick local oxide in the “field region” between the devices. In 1970, researchers from Philips 1 invented the so-called LOCOS (LOCal Oxidation of Silicon) technique to achieve this isolation. Using a Si 3 N 4 mask, the silicon is thermally oxidised in the nitride-free field regions. Figure 1 (left) shows a typical LOCOS struc- ture. Although LOCOS seemed a per- fect solution at that time, it came with a lot of problems, many of them related to mechanical stresses. Thermal oxida- tion of Si to SiO 2 occurs together with a 125% volume expansion. As a result, the oxide grown in the field region, called the “field oxide”, exerts large forces on the surrounding silicon. Another major drawback of this tech- nique is the so-called “bird’s beak”, caused by the lateral growth of the oxide under the nitride mask. This bird’s beak not only affects the intend- ed device length, it also introduces large local mechanical stresses in the silicon, because of volume expansion, and it also deforms the nitride film. These stresses often resulted in the generation of dislocations in the silicon, which are quite harmful for the devices (see Figure 1, right). Measuring these local stresses using known techniques such as wafer bend- ing or x-ray diffraction (XRD) was not possible at that time. The devices were too small (μm size). So, in the 1980s and beginning of the 1990s, a lot of effort was spent on simulation of the oxidation process, the LOCOS forma- tion and the induced stresses. However, this simulation process was not straightforward. The different materials had to be treated as being non-linear visco-elasto-plastic, their material parameters could change with temperature and stress, and the oxida- tion rate depended on the (changing) silicon crystal orientation. Although this seemed a mission impossible, many researchers succeeded in simulating the LOCOS process quite well. But this did not really solve the questions on stress. How large is this stress, what is the effect of processing parameters and materials used, and what is the effect of geometry? Answering these questions is why Raman spectroscopy found much greater utilisation within the micro- electronics industry. Raman spectroscopy and microelectronics Raman spectroscopy was of course already being used in the 1970s for the study of semiconductors. It allows iden- tification of the material and yields information about phonon frequencies, energies of electron states and elec- tron–phonon interaction, carrier con- centration, impurity content, composi- tion, crystal structure, crystal orienta- tion, temperature and mechanical strain. 2 Several studies on the effect of strain on the Raman signal of semiconductors were initiated in Germany by Professor Cardona’s group at the Max-Planck- Institute for Solid State Research, Stuttgart, and further investigated in detail by Professor E. Anastassakis. 3 Strain in the crystal affects the frequen- cy of the phonons, and as such the posi- tion of the Raman peak. In 1980, this property was exploited in the micro- electronics industry, but only for uni- form films: Raman spectroscopy was applied to measure the stress in silicon films on sapphire substrates. 4 In 1983, researchers from Mitsubishi Electronic Corporation in Japan used micro- Raman spectroscopy to study the recrystallisation and crystal orientation of silicon with a high spatial resolu- tion. 5,6 This work triggered Japanese researchers from Toshiba Corp. to use Raman spectroscopy for the measure- ment of local stress. 7 They applied the technique to study stress in and outside grooves etched in Si. They measured a Raman spectrum of Si at one point in between grooves with different spacing, and related the frequency differences to differences in local stresses. In 1987, the Mitsubishi group 8,9 showed that micro-Raman spec- troscopy could be used to measure mechanical stress in the Si near LOCOS structures with a spatial resolution of about 1 μm. They did not just measure at single points, but performed scans along equidistant points (1 μm) along a line, as shown in Figure 2. Once it was proved that Raman spectroscopy could be used to measure local stresses in Si devices, application of the technique became popular very Raman spectroscopy: about chips and stress Ingrid De Wolf IMEC, Kapeldreef 75, B-3001 Leuven, Belgium * Moore’s law: this is attributed to an observation in the mid-1960s made by Gordon Moore, co-founder of Intel, that the number of transistors per square inch on ICs had doubled since the technology was invented. He predicted the trend would con- tinue for the foreseeable future. Figure 1. TEM pictures showing a LOCOS structure. Left: field oxide (FO) and bird’s beak (BB) are indicated. Right: stress induced disloca- tions in the Si-substrate.

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Page 1: Raman spectroscopy: about chips and stress · the effect of processing parameters and materials used, and what is the effect of geometry? Answering these questions is why Raman spectroscopy

6 ©Spectroscopy Europe 2003 Spectroscopy Europe 15/2 (2003)

RAMANSPECTROSCOPY

IntroductionStress in microelectronics

Moore’s law* dictates microelectron-ics researchers to make integrated cir-cuit (IC) devices smaller and to putthem as close to each other as possibleon a chip. This results in a better per-formance and a larger functionality ofthe chips. However, these devices alsorequire a good electrical isolation fromeach other. This is in general done bythe formation of a thick local oxide inthe “field region” between the devices.In 1970, researchers from Philips1

invented the so-called LOCOS (LOCalOxidation of Silicon) technique toachieve this isolation. Using a Si3N4mask, the silicon is thermally oxidisedin the nitride-free field regions. Figure1 (left) shows a typical LOCOS struc-ture. Although LOCOS seemed a per-fect solution at that time, it came with alot of problems, many of them relatedto mechanical stresses. Thermal oxida-tion of Si to SiO2 occurs together witha 125% volume expansion. As a result,the oxide grown in the field region,called the “field oxide”, exerts largeforces on the surrounding silicon.Another major drawback of this tech-nique is the so-called “bird’s beak”,caused by the lateral growth of theoxide under the nitride mask. Thisbird’s beak not only affects the intend-ed device length, it also introduces largelocal mechanical stresses in the silicon,because of volume expansion, and italso deforms the nitride film. Thesestresses often resulted in the generationof dislocations in the silicon, which arequite harmful for the devices (seeFigure 1, right).

Measuring these local stresses usingknown techniques such as wafer bend-ing or x-ray diffraction (XRD) was notpossible at that time. The devices weretoo small (µm size). So, in the 1980sand beginning of the 1990s, a lot of

effort was spent on simulation of theoxidation process, the LOCOS forma-tion and the induced stresses.However, this simulation process wasnot straightforward. The differentmaterials had to be treated as beingnon-linear visco-elasto-plastic, theirmaterial parameters could change withtemperature and stress, and the oxida-tion rate depended on the (changing)silicon crystal orientation. Althoughthis seemed a mission impossible, manyresearchers succeeded in simulating theLOCOS process quite well. But thisdid not really solve the questions onstress. How large is this stress, what isthe effect of processing parameters andmaterials used, and what is the effect ofgeometry? Answering these questions iswhy Raman spectroscopy found muchgreater utilisation within the micro-electronics industry.

Raman spectroscopy andmicroelectronics

Raman spectroscopy was of coursealready being used in the 1970s for thestudy of semiconductors. It allows iden-tification of the material and yieldsinformation about phonon frequencies,energies of electron states and elec-tron–phonon interaction, carrier con-centration, impurity content, composi-tion, crystal structure, crystal orienta-tion, temperature and mechanicalstrain.2

Several studies on the effect of strainon the Raman signal of semiconductorswere initiated in Germany by ProfessorCardona’s group at the Max-Planck-Institute for Solid State Research,Stuttgart, and further investigated indetail by Professor E. Anastassakis.3

Strain in the crystal affects the frequen-cy of the phonons, and as such the posi-tion of the Raman peak. In 1980, thisproperty was exploited in the micro-electronics industry, but only for uni-form films: Raman spectroscopy wasapplied to measure the stress in siliconfilms on sapphire substrates.4 In 1983,researchers from Mitsubishi ElectronicCorporation in Japan used micro-Raman spectroscopy to study therecrystallisation and crystal orientationof silicon with a high spatial resolu-tion.5,6 This work triggered Japaneseresearchers from Toshiba Corp. to useRaman spectroscopy for the measure-ment of local stress.7 They applied thetechnique to study stress in and outsidegrooves etched in Si. They measured aRaman spectrum of Si at one point inbetween grooves with different spacing,and related the frequency differences todifferences in local stresses.

In 1987, the Mitsubishi group8,9

showed that micro-Raman spec-troscopy could be used to measuremechanical stress in the Si near LOCOSstructures with a spatial resolution ofabout 1 µm. They did not just measureat single points, but performed scansalong equidistant points (1 µm) along aline, as shown in Figure 2.

Once it was proved that Ramanspectroscopy could be used to measurelocal stresses in Si devices, application ofthe technique became popular very

Raman spectroscopy: about chipsand stress

Ingrid De WolfIMEC, Kapeldreef 75, B-3001 Leuven, Belgium

*Moore’s law: this is attributed to an observation in the mid-1960s made by GordonMoore, co-founder of Intel, that the number of transistors per square inch on ICshad doubled since the technology was invented. He predicted the trend would con-tinue for the foreseeable future.

Figure 1. TEM pictures showing a LOCOS structure. Left: field oxide(FO) and bird’s beak (BB) are indicated. Right: stress induced disloca-tions in the Si-substrate.

Page 2: Raman spectroscopy: about chips and stress · the effect of processing parameters and materials used, and what is the effect of geometry? Answering these questions is why Raman spectroscopy

quickly in microelectronics researchcentres and industry.

In IMEC (Interuniversity Micro-Electronics Center), Belgium, we startedusing this technique for the study of stressin LOCOS in 1989. This was soon fol-lowed by measurements on alternativeisolation schemes such as LOPOS(Polysilicon-buffered LOCOS) andPELOCOS (Poly-silicon encapsulatedLOCOS),10–13 shallow and deep trenchisolation,14 silicides15 and even MEMS(MicroElectroMechanical Systems),16

solder bumps and packaged chips.17 Thetechnique also evolved during theseyears. The measurements in 1989 wererather cumbersome: one had to move theX–Y stage by hand or joy-stick, focus theprobing laser beam on the sample, startthe measurement, save the data, movethe X–Y stage again etc. This took a lotof patience and time. Now, you just putthe sample at the correct position, definethe measurement area and the computerdoes it all for you: auto-focus, movingthe stage, saving the data, fitting the spec-tra etc.

Below we show some typical resultsof local stress measurements in micro-electronics structures, performed usingmicro-Raman spectroscopy. Theydemonstrate the unique possibilities andthe power of the technique for thisapplication.

Raman spectrumof silicon

Figure 3 shows a typical Raman spec-trum of crystalline silicon. The sharp,Gaussian-like lines which can also beseen in the spectrum shown in Figure 3are Rayleigh scattered plasma lines fromthe argon laser. They can be used forcalibration.

The Raman scattering frequency ofSi is at ω = 521 Rcm–1, however,mechanical strain results in a change ofthis value. By monitoring this frequen-cy at different positions on the sample,

a “strain map” can be obtained withmicrometer spatial resolution. Ramaninstruments dedicated for stress mea-surements are able to measure frequen-cy changes as small as 0.02 cm–1. For sil-icon, this corresponds with a stress sen-sitivity of about 10 MPa.

The relation between strain or stressand the Raman frequency is rathercomplex.3,11 All non-zero strain tensorcomponents influence the position ofthe Raman peak. In some cases, how-ever, the relation becomes simply lin-ear. For example, for uniaxial (σ) orbiaxial (σxx + σyy) stress in the (100)plane of silicon, this relation is:

σ (MPa) = –435 ∆ω (cm–1)or

σxx + σyy (MPa) = –435 ∆ω (cm–1)(1)

In general, compressive stress willresult in an increase of the Raman fre-quency, while tensile stress results in adecrease. However, if more complexstrain pictures are expected, such as forexample at the edge of a film, or near atrench or LOCOS structure, the relationbetween ∆ω and the strain tensor com-ponents is more complicated. In order toobtain quantitative information on thestrain in this case, some prior knowledgeof the strain distribution in the sample isrequired. In other words, one has to pre-suppose a strain model. From this model,the expected Raman shift can be calcu-lated and compared with the Ramandata, and feedback can be given to themodel. Of course, some experimentalparameters, such as the penetration depthof the laser light in the sample and thediameter of the focused laser beam on thesample have to be taken into account.

StressmeasurementsNitride lines

The first example shows results fromstress measurements on very simple

8 Spectroscopy Europe 15/2 (2003)

RAMANSPECTROSCOPY

Figure 2. Left: schematic show-ing the measurement position,Right: Raman frequency shift forLOCOS with different widths.8

Figure 3. Typical Raman spec-trum of crystalline silicon, mea-sured using the 457.8 nm line ofan argon laser. It shows the SiRaman peak and plasma linesfrom the laser.

Page 3: Raman spectroscopy: about chips and stress · the effect of processing parameters and materials used, and what is the effect of geometry? Answering these questions is why Raman spectroscopy

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structures: long Si3N4 stripes with dif-ferent widths on a silicon substrate.These nitride lines are under tensilestress due to the deposition process. Asa result, they compress the Si atoms inthe substrate under them causing com-pressive stress, and they pull at the Siatoms next to the lines, causing tensilestress. This effect is clearly seen in theRaman spectroscopy data of Figure 4.

This figure shows the measured shiftof the frequency of the Si Raman peakwhen scanning along a line across thewidth of such stripes.12 The position ofthe stripes is indicated by the lines ontop of the data. The laser is first focusedfar from the lines, where the stress canbe assumed to be zero. Next the sampleis moved, using the XY-stage, in stepsof 0.1 µm and at each position a Si-Raman spectrum, such as the oneshown in Figure 3, is recorded. ALorentzian function is fitted to each ofthese Raman peaks in order to deter-mine the frequency. The shift of thisfrequency from the stress free value,∆ω, is plotted as a function of the posi-tion on the sample where the corre-sponding spectrum was measured.Figure 4 shows that ∆ω becomes nega-tive when approaching the lines, indi-cating tensile stress (Equation 1). Whencrossing the border, ∆ω changes signvery fast to reach a maximum positivevalue under the line, near the edge,indicating compressive stress. ∆ωremains positive under the line, withsome relaxation towards the centre. Inorder to obtain an idea about the mag-nitude of the stress, one can assume uni-axial stress, σ, along the width of theline. This assumption is not too badnear the centre of the line, but it doesnot hold at the edges. A shift of ∆ω =0.2 cm–1, as measured in the siliconunder the centre of the wide nitrideline, would then correspond with acompressive stress of about –90 MPa.This stress clearly increases withdecreasing width of the Si3N4 lines. Itbecomes about –300 MPa for 2.5 µmwide lines. It is possible to obtain more

detailed information on the differentstress components by fitting a stressmodel to the Raman data.12 This wasdone for these nitride lines using the so-called analytical “edge force model”.18

The full lines in Figure 4 show theresult of a fit of this model to the µRS(micro-Raman spectroscopy) data, tak-ing into account experimental parame-ters such as probing spot diameter andpenetration depth. This procedure offitting theoretical stress models toRaman data can be used for any modeldescribing any device where Ramandata can be measured. In this way, µRScan be used to experimentally verifystress models.

SilicidesStress induced in Si by metal lines can

also be studied. Figure 5 shows theresult of a µRS scan across a Si samplewith arrays of [110] oriented 16 nmthick TiSi2 lines with decreasingpitch.19,20 The position of the TiSi2lines is indicated by the stripes onFigure 5. TiSi2 lines do give a Ramansignal, but this signal is very weak anddifficult to use for the monitoring ofstress in the lines. It can be used, how-ever, to study the phase of the TiSi2.

21

In this study, we measured the stressinduced by the silicide lines in the sili-con substrate next to the lines, and theeffect of line pitch on this stress. The

laser light could not penetrate throughthe silicide, so, no signal is obtainedfrom underneath the lines.

∆ω becomes negative near the edgeof the lines (blue circles), indicating thepresence of tensile stress in the silicon(Equation 1). In between the lines (redcircles), ∆ω remains negative. Forsmaller spacing between the lines, thisnegative value of ∆ω increases, showingthat the tensile stress in between thelines increases with decreasing spacing.From this experiment one can expectthat for a certain line spacing, this ten-sile stress might become so large that itwill trigger the formation of disloca-tions. TEM analysis of 110 nm thickTiSi2 lines showed that dislocationsindeed start to occur in the silicon whenthe spacing was equal to or smaller than1 µm.

IsolationAs mentioned in the introduction, an

important processing step is the isola-tion of active areas in Si chips. This iso-lation, through the growth of aLOCOS, or through the etching andoxide-filling of shallow or deep trench-es, is known to induce large stress in thesilicon substrate. Figure 6 show theresult of two Raman experiments per-formed during a two-dimensional scanacross a 3 µm wide square (left) and line(right) active Si isolated by PBLOCOS(Poly-buffered LOCOS). The stress istensile (∆ω < 0) near the edges andcompressive (∆ω > 0) in the centre.Notice that the tensile region is largernear the sides of the square than nearthe edges. On the other hand, the com-pressive stress is larger at the edges ofthe square and of the line than near thesides, and there is also a clear relaxationtowards the centre. These experimentsdemonstrate the stress-mapping capabil-ities of micro-Raman spectroscopy.

PackagingWhen information on the variation

of stress with depth has to be obtained,there are three possible ways to pro-

Figure 5. Shift of the silicon Raman peak, ∆ω, from the stress free fre-quency as a function of the position on 16 nm thick TiSi2 lines, spac-ing = width = 5, 3, 2 or 1 µm, on (100) Si substrate.

Figure 4. ∆ω (symbols) measured on nitride lines with different widthson Si substrate. The rectangles at the top indicate the position of thelines. See text for details.

Page 4: Raman spectroscopy: about chips and stress · the effect of processing parameters and materials used, and what is the effect of geometry? Answering these questions is why Raman spectroscopy

ceed. The first is by changing the prob-ing depth by using different wave-lengths of the exciting laser. A disad-vantage of that approach is that theRaman signal arises from the wholeprobed area. This can be minimised bymaking use of the confocality of thesystem. This works well in transparentsamples, like GaN or diamond, but isnot so useful in opaque samples such assilicon. A third way is to cleave thesample, and polish if required, and tomeasure on the cross-section. An exam-ple of this last approach is shown inFigure 7.

The packaging process of chips,including wire bonding, solder bump-ing, chip adhesion to a substrate, globtop covering etc. also introduces stress-es in the chip. These stresses are in gen-eral studied through finite element (FE)simulations, but they can in many casesalso be studied using Raman spec-troscopy. Figure 7 shows the exampleof a stress map, measured by Ramanspectroscopy on the cross-section of a Sichip that was bonded to a copper sub-strate.17 Due to the difference in ther-mal expansion coefficient between Siand Cu, this bonding induces stresses inthe silicon. One can clearly distinguishstresses introduced by both the Cu sub-strate and the solder bump on the top ofthe chip. This kind of study allows thecomparison of stress introduced by dif-ferent chip/substrate bonding processes,the effect of encapsulation of the chips,and even the effect of changes in thewire bonding process.

MEMS: pressure sensormembrane

As a last example, we discuss a µRS-experiment on the Si membrane of apressure sensor.16 This sensor wasprocessed by etching cavities in the sili-con wafer and bonding the wafer anod-ic to a glass substrate [Figure 8(a)]. Thebonding introduced a negative pressureunder the membrane, resulting in aninward deflection of about 5 µm. AµRS-system equipped with an autofo-cus module was used to scan the surfaceof the membrane. Figure 8(b) shows themechanical stress in the membrane, cal-culated from the change of the Ramanfrequency (∆ω) from its stress freevalue, assuming biaxial stress. We clear-ly find compressive stress in the centreof the membrane and tensile stress nearthe sides. The corners have very lowstresses. Similar experiments were per-formed on the underside of the mem-brane. Indeed, the µRS-techniqueallows probing of the silicon throughthe glass substrate. This makes it possi-ble to study, for example, the glass/sili-con interface.

ConclusionsMechanical stress has always been an

important concern for IC-processing

and reliability engineers. This stressoccurs at nearly all the stages of the chipdevelopment and life: during depositionof films, temperature steps, oxidegrowth, silicidation, trench filling,wafer thinning, dicing, chip bonding,chip packaging and in an environmentwith ever changing temperatures.

Mechanical stress can have direct orindirect effects on the functioning andreliability of a chip, and cause differentfailure modes, such as changes in elec-tron or hole mobility, dislocations nearLOCOS (Figure 1) or trench isolationstructures giving rise to an increasedleakage current, dislocations near densesilicide lines, fracture of MEMS, cracksin chips, breaking of solder bumps,creep in metals, stress migration etc.

S.M. Hu correctly predicted in1991:18 “Many problems of defectivedevices in silicon ICs can be traced ulti-mately to stresses that develop at variousstages of IC processing. These problemswill become more acute as IC devicesbecome more complex in geometry andmaterial mix”. The same can be said forIC packages.

It is important to control mechanicalstress induced by processing steps in ICand MEMS manufacturing and chippackaging. The stress can in many casesbe monitored using micro-Ramanspectroscopy. This technique is ratherunique in the sense that it is the onlysimple, spectroscopic, non-destructivetechnique that can offer this informa-tion. Only examples from Si deviceswere shown, but Raman spectroscopyis not restricted to Si. For example, thetechnique can also be applied to semi-conductor materials such as Ge, GaAs,GaN etc.

AcknowledgementsThe examples used in this paper came

from collaboration with different peo-ple: many thanks to Veerle Simons,Merlijn van Spengen, Chen Jian, AnnSteegen, Dave Howard, Karen Maex,Rita Rooyackers and Goncal Badenes.

RAMANSPECTROSCOPY

12 Spectroscopy Europe 15/2 (2003)

Figure 6. Shift of the silicon Raman peak, ∆ω, from the stress free fre-quency as a function of the position on 3 µm wide active square Siregion (left) and line (right) isolated by PBLOCOS.22

Figure 7. Stress in a Si chipbonded to a Cu substrate.17

Figure 8. (a) Schematic showing the membrane on glass substrate. (b)Mechanical stress in a 4 mm × 4 mm membrane measured usingRaman spectroscopy. The stress is calculated assuming biaxial stressin the membrane.16

Page 5: Raman spectroscopy: about chips and stress · the effect of processing parameters and materials used, and what is the effect of geometry? Answering these questions is why Raman spectroscopy

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