Process parameters of the SRO, SRN and SRN/SRO films deposited by LPCVD and thickness of the sample after thermal annealing.
Luminescent silicon‐rich dielectric materials have been under intensive research due to their potential applications in optoelectronic devices. Silicon‐rich nitride (SRN) and silicon‐rich oxide (SRO) films have been mostly studied because of their high luminescence and compatibility with the silicon-based technology. In this chapter, the luminescent characteristics of SRN and SRO films deposited by low‐pressure chemical vapor deposition are reviewed and discussed. SRN and SRO films, which exhibit the strongest photoluminescence (PL), were chosen to analyze their electrical and electroluminescent (EL) properties, including SRN/SRO bilayers. Light emitting capacitors (LECs) were fabricated with the SRN, SRO, and SRN/SRO films as the dielectric layer. SRN‐LECs emit broad EL spectra where the maximum emission peak blueshifts when the polarity is changed. On the other hand, SRO‐LECs with low silicon content (~39 at.%) exhibit a resistive switching (RS) behavior from a high conduction state to a low conduction state, which produce a long spectrum blueshift (~227 nm) between the EL and PL emission. When the silicon content increases, red emission is observed at both EL and PL spectra. The RS behavior is also observed in all SRN/SRO‐LECs enhancing an intense ultraviolet EL. The carrier transport in all LECs is analyzed to understand their EL mechanism.
- silicon‐rich dielectrics
- conduction mechanisms
The use of photonic signals instead of electrons to transmit information through an electronic circuit is an actual challenge. Unfortunately, it is well known that bulk silicon (Si) is an indirect bandgap semiconductor, making it an inefficient light emitter. Therefore, great efforts have been taken to obtain highly luminescent Si‐based materials in order to get Si‐based photonic devices, especially a light emitting device [1–3]. Such circumstances have led to explore new options for converting silicon into a luminescent material. Si nanoparticles (Si‐nps) embedded in a dielectric material as silicon‐rich oxide (SRO) or silicon‐rich nitride (SRN) show a prominent photoluminescence (PL) emission in red and blue‐green region, respectively [4–10]. Thus, SRN or SRO films have been considered as promising candidates for emissive materials due to their potential applications in Si‐based optoelectronic devices, and their fully compatibility with the complementary metal‐oxide‐semiconductor (CMOS) processes [11–16].
Two main strategies have been explored: those that focus on the intrinsic emission from the matrix, either through emissions from defects or by the presence of Si‐nps. The second one focus on extrinsic emission, which is produced by doping the material (usually introducing rare earth ions) [3, 17].
The most common strategy to obtain intrinsic emission is through silicon nanostructures, which significantly increase the emission due to the quantum confinement effect (QCE) [5, 18]. Furthermore, the dependence on the size of the Si‐nps on the forbidden gap width allows that the emission can be adjusted in the visible and the red‐near infrared region of the electromagnetic spectrum . Several studies have reported both red and near infrared electroluminescence (EL) SRO which is mainly attributed to the recombination of excitons in Si‐nps [20, 21]. On the other hand, the emission of green or blue light has been attributed to defects associated with oxygen [22, 23]. Some studies have reported that red (620 nm) EL emission could be attributed to non‐bridging oxygen hole center (NBOHC) defects whose origin has been corroborated by the fact that the peak position does not change if the film is excited with different energies .
Another alternative to obtain intrinsic light emission is through an ordered structure of Si‐nps by a superlattice, which is formed by the alternating of SRO and SiO2 nano‐films. Red or near infrared emission has been observed in these structures and has been related to both excitonic recombination taking place in confined states within Si‐nps or relaxation of hot electrons [25, 26].
Intrinsic emission has been also observed in SRN films [27–31]. For example, an orange emission at 600 nm was observed at room temperature and has been related to the electron‐hole pairs’ recombination within Si‐nps . Also, green emission has been observed in nitrogen‐rich silicon nitride, which was attributed to radiative recombination in localized states related to Si‐O . Some other authors have shown significant improvement of the green emission intensity using oxidized silicon‐rich nitride . Also, when a silicon nitride film is implanted with Si ions, violet and green‐yellow emission bands are observed, giving rise to an intense white EL emission . The violet band was related with the presence of defects states related to silicon dangling bonds (=Si0 or centers K0) located near the middle of the forbidden gap of silicon nitride and defect states related to the unit Si–Si= located near the edge of the valence band, while the green‐yellow band was attributed to the transition from the =Si0 state to nitrogen dangling bonds (=N–) in the tails of valence bands.
Red‐near infrared EL (800 nm) has been reported in superlattices combining SRN and SiO2 films and explained by the bipolar recombination of electron‐hole pairs in Si‐nps present within the SRN films . A yellow EL emission has been reported when an SRO film instead of SiO2 layer is used in the multilayer structure . All of these promising results have proved the first implemented all‐silicon‐based photonic device . Nevertheless, despite all these promising results in luminescent silicon‐based materials, the improvement of the efficiency of the light emitting devices is still necessary.
This chapter shows a review about our experience on the PL and EL properties of SRN and SRO films deposited by low‐pressure chemical vapor deposition (LPCVD). The effect of the combination of the SRN and SRO luminescent properties is also analyzed as an SRN/SRO structure. A study about the composition, structural, optical, and electro‐optical properties of these films will be discussed. The study also includes the analysis of the charge transport mechanism through the SRO, SRN, and SRN/SRO films to understand their electroluminescence behavior and its correlation with the different luminescent centers (LCs) within the active material.
2. Experimental procedure
In this chapter, SRN, SRO, and SRN/SRO films were deposited in a homemade LPCVD hot‐wall reactor. In these silicon‐rich dielectrics materials, the Si content was controlled by a ratio of partial pressure of reactant gases;
The SRN films were deposited on N‐type ((100)‐oriented) Si wafers with a resistivity of 1–5 Ω‐cm at 750°C using ammonia (NH3) and 5% nitrogen (N2)‐diluted silane (SiH4) as the reactant gases by the ratio
|Sample name||Pressure of gases (Torr)||Time (min)||Thickness (nm)|
|SRO||M20||20||0.53||0.80||12||55.72 ± 5.0|
|M30||30||0.80||0.80||15||64.00 ± 3.4|
|SRN||N5||5||0.22||0.85||10||102.83 ± 3.62|
|N20||20||0.85||0.85||15||112.67 ± 6.19|
|N80||80||2.00||0.50||13||66.93 ± 2.12|
|SRN/SRO||B20||80||1.08||0.41||4||16.32 ± 1.54|
|20||0.53||0.80||15||55.72 ± 5.0|
|B30||80||1.08||0.41||4||16.32 ± 1.54|
|30||0.80||0.80||15||64.00 ± 3.4|
After deposition, SRN, SRO and SRN/SRO samples were thermally annealed at 1100°C under nitrogen atmosphere conditions for 180 min.
For electrical and electroluminescence studies, light emitting capacitive (LEC) structures were fabricated. For SRN‐LECs, a transparent 300‐nm thick fluorine‐doped tin oxide SnO2:F (FTO) film was deposited onto the surface of the SRN by ultrasonic spray pyrolysis. Square‐shaped patterns with 1 mm2 area were defined by a photolithography process step to act as gate contact. For SRO‐LECs, ~400‐nm thick semitransparent n+ polycrystalline silicon (poly) gate was deposited onto the SRO film surface by LPCVD. After a photolithography process step, square‐shaped gates of 4 mm2 area were defined. For SRN/SRO‐LECs, ~300‐nm thick indium tin oxide (ITO) film was deposited by RF sputtering onto the surface of the films as gate contact. Square‐shaped patterns with area of 1 mm2 were defined by a photolithography process step to act as anode gate contact. Approximately 700‐nm thick aluminum (Al) film was evaporated onto the backside of the silicon substrates as cathode contact in all of the LECs. A thermal annealing process at 460°C in N2 atmosphere for 20 min was used to form the ohmic contact.
The thickness of thermally annealed SRO and SRN films was measured with a Gaertner L117 ellipsometer with a 70° incident laser with wavelength of 632.8 nm and is also shown in Table 1. Chemical bonding characteristics was analyzed by means of Fourier transform infra‐red spectroscopy (FTIR) with a Brucker V22 equipment in the 4000–350 cm-1 range with a resolution of 5 cm-1. The PL spectra were measured with a Fluoromax 3 of Horiba Jobin Yvon. The samples were excited using a 300 nm radiation, and the PL emission signal was collected from 400 to 900 nm with a resolution of 1 nm. The depth analysis profile of thermally annealed SRN, SRO, and SRN/SRO films was analyzed by means of X‐ray photoelectron spectroscopy (XPS) Escalab 250Xi of Thermo Scientific equipment, with an Al K
The composition of SRN and SRO films play an important role in order to understand their luminescence, electrical, and electro‐optical properties. In this sense, some techniques such as FTIR and XPS spectroscopies have been used.
3.1. Silicon‐rich nitride (SRN) film
The Si‐N bonds of SRN films were determined by FTIR measurements. Figure 1(a) shows the IR spectra measured from SRN films with
IR peaks at 460 and 840 cm-1 ascribed to Si-N wagging and stretching modes, respectively, were observed for all samples [35–37]. An IR band appears at 1080 cm-1 after thermal annealing, being more evident in the N80 sample. The presence of this peak has been observed before and attributed to a reordering in the films toward a‐Si3N4 bonding configuration [38, 39]. Nevertheless, it could be related to the Si–O stretching mode due the oxygen incorporation in the samples.
In order to comprehend the stoichiometry and the presence of some oxygen into the SRN films, analysis of their composition was performed by means of XPS. Figure 1(b) shows information about the chemical composition of the thermally annealed SRN samples. The inset of Figure 1(b) exhibits the depth profile composition of the thermally annealed
3.2. Silicon‐rich oxide (SRO) film
The Si–O bonds of SRO films were also determined by FTIR measurements. The IR spectra measured from SRO films with
Figure 2(b) exhibits the depth profile composition of the thermally annealed SRO films. Mean silicon content values of 41.85 ± 1.1 and 39.98 ± 0.8 at.% were obtained for the SRO films with
The presence of the Si0 peak in the Si2p XPS signal correlates well with the presence of silicon nanocrystal observed by high‐resolution transmission electron microscopy (HRTEM, not shown here) in the M20 film. HRTEM reveals Si nanocrystals with an average size (and density) of 2.91 ± 0.40 nm (8.66 x 1011 cm-2) .
3.3. Silicon‐rich nitride/silicon‐rich oxide (SRN/SRO) bilayer
The Si–N and Si–O bonds of SRN/SRO bilayers with
As shown in Figure 3(a), the shoulder from ~1100 to ~1300 cm-1 was observed in both samples (M20 and B20) and it was attributed to Si–O stretching out of phase . The IR peak at 610 cm-1 observed in the SRO monolayer (M20) disappeared for the bilayer (B20) and it could be related to the nitrogen incorporation within the SRO that creates Si–N–O–Si bridges. The presence of these bridges decreased the quantity of strained bonds and Si dangling bonds at the SiO2/Si‐np interface . The SRN/SRO film with
Figure 3(b) showed the depth profile composition of the thermally annealed SRO monolayer and SRN/SRO bilayer, both with
4.1. Silicon‐rich nitride (SRN) film
The PL spectra of SRN films before and after thermal annealing are shown in Figure 4. The PL intensity was normalized to the thickness of each SRN film. The as‐deposited SRN film with
The PL band of the SRN films blueshifts after thermal annealing, particularly for
PL bands between 380 and 600 nm (2.0–3.2 eV) have been observed before in SRN films, and they have been ascribed to the radiative recombination of carriers in band tail states, which are related to defect energy levels within the gap of amorphous silicon nitride [61–64]. Therefore, the PL bands emitted by the SRN films from this work can be explained by the excitation of different defects as discussed in the study of Cabañas‐Tay et al. . As observed in Figure 4(a), the as‐deposited SRN films emit at 590, 580, and 490 nm, whereas the thermally annealed films emit at 580, 540, and 420 nm for
Some studies have shown that electronic transition related with K0 centers to =Si–O–Si states are observed when oxygen is incorporated in the SRN film [65, 66]. The presence of oxygen in SRN films creates a gap state of Si–O above the VBM, giving rise to the 485 nm (~2.55 eV) emission. The XPS analysis demonstrated that SRN films contain oxygen, being the higher concentration for
In summary, the analysis of the PL emission observed in the SRN films before and after thermal annealing indicates that it could be mainly originated from the radiative recombination via luminescent Si dangling bonds, N dangling bonds, and Si–O bonds existing in the silicon nitride matrix.
4.2. Silicon‐rich oxide (SRO) film
Figure 5 shows the normalized PL spectra of SRO films before and after thermal annealing. The as‐deposited SRO film with
The PL emitted by M30 exhibit a significant redshift of the main peak after thermal annealing as shown in Figure 5(a). Nevertheless, when the silicon content is increased (M20), the PL band appears mainly at the red side of the spectrum. The redshift of the main PL peak (after thermal annealing) has been widely observed and ascribed to the agglomeration of silicon excess and a subsequent silicon nanoparticle formation as a result of thermal annealing process [67–71]. Nevertheless, some point defects are also present within the SRO films. It is widely accepted that violet‐blue (400–460 nm), green (520), and even red (630) emission bands, obtained from the deconvolution of the PL spectrum , can be related with oxygen defect centers (ODC), E’δ (SiSi=Si) and NBOHC defects, respectively [67–71]. The E’δ center is one of the at least four different E’ centers , which comprises an unpaired spin delocalized over five silicon atoms and suggest the presence of very small Si‐nps in the films.
4.3. Silicon‐rich nitride/silicon‐rich oxide (SRN/SRO) bilayers
In previous studies, it has been reported that the combination of Si3N4/SRO structure improves luminescent emission properties [73, 74]. Previous studies have also shown that a Si3N4‐SRO bilayer structure improves the operation of light‐emitting devices, such as a reduced leakage current, a reduced electric field on the oxide layer, and results an improvement in efficiency and a longer device life [73–76]. In this chapter, the effect of a SRN film on a SRO film (SRN/SRO bilayers) on their optical properties is analyzed. SRN films, deposited by LPCVD with
Figure 6 shows the PL spectra of SRN/SRO bilayers with
For the SRN film (N80), PL bands at about ~420, 505, and 680 nm were identified, which are related to electronic transitions from the K0 centers to the VBM, K0 centers to =Si–O–Si, and states of defects nitrogen (N02), respectively . For the SRO film with
As observed in Figure 6(b), the SRO monolayer with
In summary, it is observed that the emission intensity in the blue and green bands (~420 and 505 nm) is improved when a SRN/SRO bilayer is formed compared to SRO monolayers, being higher when a
SRN, SRO, and SRN/SRO films exhibit intense and visible photoluminescence. In this section, luminescent characteristics of the samples are present but under electrical excitation.
5.1. Silicon‐rich nitride (SRN)‐LECs
Figure 7 shows the EL spectra of the light emitting capacitors using the as‐deposited SRN film with
On the other hand, at reverse bias (RB), the EL spectrum changes and now three main emission bands are observed at around 600, 680, and 780 nm, as observed in Figure 7(b). Namely, the maximum emission band blueshifts when the polarity is changed from RB to FB. The EL bands at 600, 680, and 780 nm also remains at the same wavelength when the voltage is increased indicating the EL emission is also produced by defects. These EL bands have been ascribed to electronic transitions from the K0 centers to valence band tail states [58, 77]. The EL emission for all the SRN‐LECs in both polarities is through shine dots as shown in the inset of Figure 7(a) and (b). The device's area is covered with more shine dots when the current increases. The EL emission composed by shining spots is attributed to the formation of a finite number of preferential conductive paths within the SRN films, which connect the top and bottom electrodes, as discussed in the study of Cabañas‐Tay et al. .
Negligible spectral shift is observed between the EL at forward bias and PL spectra of SRN films with
5.2. Silicon‐rich oxide (SRO)‐LECs
The presence of defects including the Si‐nps, either crystalline or amorphous, and their density and size in silicon‐rich dielectric materials affect clearly the current transport, and therefore the EL, as in the SRO case. Figure 8 shows J‐E curves of SRO‐LECs with
Once the current fluctuations disappear, through the electrical annealing, the current behavior stabilized (see I–V curve marked as M30‐after in dark blue line, Figure 8) and EL on the whole area (WA EL) was observed at higher electric fields. On the other hand, the electrical behavior of SRO‐LEC with
Figure 9 shows the EL spectra from the SRO‐LECs. Blue EL in the whole area was observed with
5.3. Silicon‐rich nitride/silicon‐rich oxide (SRN/SRO)‐LECs
Figure 10 shows the J(E) characteristic and the EL spectra of SRN/SRO‐LECs at forward bias considering the substrate like reference. SRN/SRO‐LECs show a high current state (HCS) at low electric fields, and then after the applied voltage increases, the current is switched to a LCS, as shown in Figure 10(a). The resistive switching in the B20 bilayer occurs at a lower electric field (~2 MV/cm) compared to the B30 bilayer. When SRN/SRO‐LECs, both with
After current switching, in the LCS (>20V), the EL spectra changes, as observed in Figure 10(c). Also, a narrow (width of 7 ± 0.6 nm) and highly intense UV EL peaks appear at ~250, 270, 285, 305, 325, and 415 nm. A narrow blue EL peak with the highest intensity is observed at ~450 nm. All EL peaks remain at the same wavelength as the current increases. The red EL band observed in the HCS is still present at the LCS, but with a slight redshift and with a low intensity. The emission intensity of the blue EL is about 20 times higher than the red emission. The EL emission is observed as luminescent blue‐violet dots randomly distributed on the surface of the contact, as shown in the insets of Figure 10(c).
Figure 10(d) shows the EL emission of the SRN/SRO‐LEC with
Four narrow UV EL peaks have been reported at 293.78, 316.10, 403.07, and 444.82 nm, with an average width at half peak of 4 nm, in ITO/Y2O3/Ag EL devices. This emission was attributed to the characteristic radiation of indium ions . However, as the best of our knowledge, narrow UV EL peaks in silicon rich dielectric materials have not been reported before. The most intense EL peaks emitted by the present SRN/SRO‐LECS (~305, 325, 415, and 450 nm) are very similar to those obtained in reference , but displaced ~10 nm toward longer wavelengths. Thus, they could have a similar origin; however, a deeper analysis of these narrow emission bands needs to be done.
6. Conduction mechanisms
The origin of the EL emission from the SRO, SRN, and SRN/SRO‐LECs can be determined by identifying the charge transport mechanism that takes place within the different silicon‐rich dielectric materials as discussed below.
6.1. Silicon‐rich nitride (SRN)‐LECs
Figure 11 shows the J(E) dependency for the SRN‐LECs with
6.2. Silicon‐rich oxide (SRO)‐LECs
Figure 12 shows the experimental J‐E data from SRO‐LECs with
The trap energy was estimated to be
On other hand, the P‐F conduction fits well the charge transport in SRO‐LECs with
6.3. Silicon‐rich nitride/silicon‐rich oxide (SRN/SRO)‐LECs
When the SRN/SRO bilayer structure is used as active layer in LECs, several charge transport mechanisms are present, as observed in Figure 13. For the SRN/SRO‐LEC with
The average distance between traps (
The SRN/SRO‐LECs with
In summary, the conduction mechanism in the region of low electric fields at HCS is hopping for SRN/SRO bilayers. It was observed that when the nitrogen content in the SRO layer increases, the average distance between defects also increases either due to the defects passivation or due to the reduction of the Si‐nps size. In the region of high electric fields at low conduction, both TAT and P‐F mechanisms take place simultaneously. The trap depth, obtained by the TAT fit, was ~2.1 eV from the minimum of the conduction band for both bilayers (B20 and B30), which relates to the location of the centers K0 in SRN film.
The compositional, structural, optical, and electro‐optical properties of SRO, SRN films as well as combination of SRN/SRO bilayers deposited by LPCVD were studied. The EL of the SRN‐LECs showed a broad emission spectrum where the maximum peak blueshifts when the polarity changed from reverse to forward bias. The EL spectrum was nearly similar to that of PL when LECs were forwardly biased and the silicon excess was increased. Analyzing the current‐voltage characteristics, it was found that TAT was the main carrier transport mechanism in SRN films in both biases, where typical EL was observed. In SRO films, it was demonstrated that the silicon content affects the luminescence centers density obtaining the EL emission at lower electric field as the silicon excess increased. SRO with
This work has been partially supported by the project CONACyT‐180992. The authors acknowledge technicians Pablo Alarcon, Armando Hernández, and Victor Aca from INAOE and Luis Gerardo Silva from CIMAV.
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