Influence of Boron Nitride Nanoparticles in the Electrical And

Materials Express

Inﬂuence of boron nitride nanoparticles in the electrical and photoconduction characteristics of planar boron nitride-graphene oxide composite layer

Harith Ahmad1, 2, ∗ and Tamil Many K. Thandavan1 1Photonics Research Centre, Faculty of Science, University of Malaya, 50603 Kuala Lumpur, Malaysia 2Visiting Professor at the Department of Physics, Faculty of Science and Technology, Airlangga University, Surabaya 60115, Indonesia Article

ABSTRACT IP: 192.168.39.211 On: Mon, 27 Sep 2021 01:54:43 Copyright: American Scientific Publishers A modified Hummer’s method is used to obtainDelivered a photoconducting by Ingenta material based on boron nitride (BN)– graphene oxide (GO) composite layer. The proposed silver/BN–GO/silver Schottky photodetector was fabricated using a drop-casting technique and electron beam evaporation. It was characterized using field emission scanning electron microscopy, energy dispersive X-ray spectroscopy, Raman spectroscopy, and Fourier-transform infrared spectroscopy. The confine element composition of boron, nitrogen, carbon, and oxygen showed excellent photoconduction toward laser wavelength of 650 nm and output power of 0.7 mW. The dark and illuminated current–voltage characteristics were used to determine the ideality factor and barrier height, which inevitably simplified the transport mechanism in the device. The reported ideality factor of 2.58 suggests the charge transport at the junction and formation of non-amorphous BN–GO composite layer. Keywords: Photodetector, Boron Nitride, Graphene Oxide, Ideality Factor, Barrier Height, Visible.

1. INTRODUCTION Their properties such as high mechanical and thermal The rapid growth of new functional two-dimensional (2D) stability and large piezoelectric constant incorporated in materials has attracted considerable interest in photocon- quantum wells, modulation-doped heterointerfaces, and duction technology due to their usefulness primarily in heterojunction structures provide access to wider spectral defense, sensors, health, and weather forecast systems.1 regions for optoelectronic devices.3 However, these mate- In addition, III-nitride-based materials such as gallium rials have lattice mismatch and thermal incompatibility nitride (GaN), aluminium nitride (AlN), and indium nitride with most substrates. Given these limitations, researchers (InN) have been widely used as ternary and quaternary have shifted their attention to boron (B)-based nitride III-nitride structures due to their bandgaps of 6.2, 3.4, and materials. Boron nitride (BN) has exceptional hexagonal 0.7 eV, respectively. These materials enable the bandgap and cubic forms (hBN and cBN)1 4 similar to the struc- to be tuned, allowing for wide-spectrum absorption from ture and properties of graphite and diamond,5 respec- 2 the deep ultraviolet (UV) region to whole visible range. tively. It can be synthesized in nanostructures with various morphologies for solar-blind deep UV photodetection.6 7 ∗Author to whom correspondence should be addressed. The bandgap of BN is similar to that of diamond Email: [email protected] and can be modulated even lower than 2.0 eV through

Mater. Express, Vol. 9, No. 3, 2019 265 Materials Express Inﬂuence of boron nitride nanoparticles in the electrical and photoconduction Ahmad and Thandavan

modified synthesis techniques.8 Deposition of electrodes 2. EXPERIMENTAL DETAILS using electron beam deposition with cBN in between 2.1. Materials and Method the electrodes shows peak responsivity at 180 nm owing The prepared BN–GO composite material was used as the to the high homogeneity of electric field between the main source for the conversion of light signal into electri- electrodes.9 Plasma-enhanced chemical vapor deposition cal signal. The GO was prepared using a modified Hum- enables sulfur doping in cBN lattices, decreasing the mer’s method.26 27 The preparation of GO involved two bandgap to 4.78 eV.10 hBN with similar physical, struc- steps: (i) pre-oxidation of graphite flakes and (ii) further tural, and isoelectrical analogy of graphene enables syn- oxidation of the pre-oxidized graphite. Oxidizing solvents

thetization with NSs such as nanosheets, nanotubes, and (100 mL of 98% sulfuric acid (H2SO4) and 15 mL of 11 12 nanorods compared with cBN NSs. 68% nitric acid (HNO3)) were mixed with 5.0 g of Mesh Surface modification or functionalization of large sur- 7-graphite flakes to form pre-oxidized graphite flakes. The face area of graphene13 with 2D materials is highly mixture was stirred thoroughly for 60 min at 200 rpm in promising due to the low cost of maintenance, high effi- an ice bath. In the second step, the pre-oxidized graphite ciency and speed, and good photosensitivity linearity in flakes were further oxidized using 15 g of potassium 14 15 wide light intensity range. Graphene and graphene permanganate (KMnO4) under constant stirring at 40 C oxide (GO) have direct bandgap between 0 eV and 1 eV for 30 min at 200 rpm. Then, 50 mL of 10% hydro- that can be chemically tuned to facilitate light-, humidity-, gen peroxide (H2O2) was mixed into the final solution to and sound-sensitive polarizers16 and allow the absorp- reduce excessive oxidation of pre-oxidized graphite flakes. tion of infrared (IR) photons for photodetection.17 GO is At this stage, the active oxidizing species of manganate well-known and ideal material as it possesses carboxyl and (Mn2O7−) were eliminated by H2O2. Finally, the mixture hydroxyl functional groups18 for multifunctional struc- was centrifuged at 15000 rpm for 30 min to obtain the GO ture with 2D materials.19 20 Functionalizing GO with BN supernatant. can maximize the structural and thermal properties of GO BN solution was prepared by dispersing 100 mg of BN powder in 50 mL of deionized water, which was then son- and maintain its optical properties. 21 Simulation studies icated for 5 h at room temperature. The solution was fur- on graphene–BN photodetector coupled with an optical ther centrifuged at 5000 rpm for 30 min to collect pure mode of a Si waveguide showIP: maximum 192.168.39.211 responsivity On: of Mon, 27 Sep 2021 01:54:43 BN supernatant. The collected BN supernatant was further 0.36 AW−1 and high speed operationCopyright: with a 3 American dB cut- Scientific Publishers Delivered bysonicated Ingenta for another 2 h before mixing with GO super- off at 42 GHz.22 The bandgap of GO can also be tuned natant obtained using the modified Hummer’s method at from 2.7 eV to 1.15 eV by using fructose.23 Recently, volume ratio of 0.2:1. The BN–GO liquid base material

Article Huang et al. explored carbon-based 2D carbon nitride was further ultrasonicated for 6 h at 40 Cinordertobe nanosheets (CNNs) that show superior electron mobility drop-casted on SiO2/Si substrate for a fast drying process. and high speciﬁc surface area with more surface active This process would allow for strong adhesion between the sites. CNNs can be incorporated with 0D carbon nan- BN–GO composite layer and the Ag source and drain elec- odots, metal atoms, and semiconductor nanoparticles to trodes deposited using the electron beam evaporation sys- enhance the photocatalytic performance.24 Huang et al. tem. Initially, the Si was thermally oxidized to SiO2 with demonstrated that graphitic carbon nitride heterojunction 1500 nm thickness at temperatures of 800 C–1200 C. photoactive nanocomposites can be used for environ- This deposited SiO2 layer acts as a dielectric layer and mental protection and clean energy and show excellent avoids direct contact of the BN–GO composite layer and stability in the presence of organic pollutants under illumi- Ag electrodes with Si substrate.28 Thus, the photocon- nation and decomposition features of abundant hydroxyl duction is purely due to the BN–GO composite layer can radical. 25 be determined. Then, 1.0 L of BN–GO solution was

In this work, a planar BN–GO-based photodetector dropped on the SiO2/Si substrate once the temperature was utilized using a low-cost drop-casting technique and reached 550 C. Initially, the temperature of the substrate modiﬁed Hummer’s method. Current–voltage (I–V )char- was set to decrease at a rate of 1 C/s from an initiated acteristics of the fabricated metal–semiconductor–metal- temperature of 650 C. structured Ag/BN–GO/Ag Schottky photodetector were evaluated to simplify the transport mechanism in the 2.2. Characterizations device. The efﬁciency of BN nanoparticles in the bulk The I–V characteristics of the photodetector under GO layer was effective as the photoconduction in the GO laser/light illumination were characterized using a Keithley bulk layer was not easily achieved. Thus, based on the 2410 SourceMeter unit as shown in Figure 1. Under the calculated ideality factor and barrier height of the BN– illumination of red laser source wavelength at 650 nm, the GO composite layer, the generation of electron–hole (e–h) photoresponsivity of the planar BN–GO composite pho- pairs under the illumination of red laser at 650 nm was todetector was determined using a Yokogawa DLM2054 evaluated. mixed signal oscilloscope.

266 Mater. Express, Vol. 9, 2019 Inﬂuence of boron nitride nanoparticles in the electrical and photoconduction Materials Express Ahmad and Thandavan

distribution of BN nanoparticles in the BN–GO composite layer.

3.2. Raman and FTIR Analysis Figure 4(a) shows the Raman scattering spectrum of the BN–GO composite layer measured at room temperature. The Si peak at 521 cm−1 was attributed to the penetra- tion of Raman green laser 532 nm through the drop-casted Fig. 1. I–V measurement setup of planar BN–GO composite layer on BN–GO composite layer. A sharp and intense peak was SiO2/Si substrate. observed at 1355 cm−1 associated to the high-frequency E 29 intrinsic 2g tangential vibration mode of hBN. This 3. RESULTS AND DISCUSSION peak overlapped with the D band of the GO layer, which 3.1. FESEM and EDX Analysis shows a defective C structure due to incorporation of BN The morphological and elemental compositions in the fab- nanoparticles. A low intense peak at 1585 cm−1 indicated ricated BN–GO composite layer were obtained using a the G band of GO, which is attributed to the characteris- Quanta 450 FEG scanning electron microscope. A forma- tics of C sp2 in-plane vibration.30 However, another low tion of a glossy GO layer covering the bright nanoparti- intense peak at 823 cm−1 (Fig. 4(a)) was ascribed to out- cles of BN can be observed in Figure 2. The glossy GO of-plane radical buckling mode, where B and N atoms layer covered the whole area of the SiO2/Si substrate. BN were moving radially inward or outward. The functional nanoparticles in the composite layer were found to be less groups attached to the BN–GO composite material were than 500 nm in size, suggesting that the ultrasonication evaluated using a Thermo Nicolet 5ZDX Fourier-transform process separated the powdered BN into nanoparticles. infrared spectroscopy (FTIR) analyzer over a transmit- − To distinguish the conﬁne distribution of elements, tance mode range of 400–4000 cm 1 at a resolution of 4cm−1. The FTIR spectrum of the BN–GO composite

energy dispersive X-ray (EDX) spectroscopy was con- Article ducted. Figures 3(a) and (b) show the EDX scanned area (Fig. 4(b)) exhibits stretching modes at 610, 1200, 1675, − and spectrum, respectively. The large scanned area exhib- and 3450 cm 1, which confirm the presence of BN, BN–O, IP: 192.168.39.211 On: Mon, 27 Sep 2021 01:54:43 31 ited B, N, C, O, and Si elements inCopyright: the BN–GO American com- ScientificC O, and Publishers B–OH functional groups, respectively. posite layer fabricated on the SiO2/Si substrate,Delivered and the by Ingenta detailed composition of elements is shown in Table I. The 3.3. I–V Characteristics EDX spectrum showed the distribution of B, C, N, and To signify the effect of BN nanoparticles in photocon- O elements with weight (wt) percentages of 23.00, 19.79, duction, I–V measurement was carried out on bare GO 30.02, and 25.36, respectively. Identification of Si ele- (without BN nanoparticles) layer that was drop-casted on ment indicates that the composite layer was thinly formed SiO2/Si substrate consisting of Ag electrodes. The results to allow sufficient X-ray to reach SiO2 surface penetrat- showed no profound photoconduction in the bulk GO ing through the fabricated BN–GO composite layer. High layer. However, the I–V characteristics of Ag/BN–GO/Ag counts per second (cps) of O element indicated success- measured at room temperature showed significant changes ful bonding with C and Si. Although the B element had asshowninFigure5. low cps (Fig. 3(b)), it had 23 wt%, indicating profound A well-defined Schottky characteristic was also revealed between the Ag contacts and the drop-casted BN–GO composite material. Such characteristic is best described by the thermionic emission theory, which can be used to analyze the transport mechanism in the BN–GO composite layer. According to this theory, the generated current can be expressed as Eq. (1), which is also known as the basic cell equation in the dark. I = I eqV /kT − 0 1(1) I 0 indicates dark saturation current that can be expressed as

I = AA∗T 2e−qb /kT 0 (2) V is the voltage across the Ag source and drain electrodes through the BN–GO composite layer, k is the Boltzmann constant (1.38 × 10−23 m2s−2kgK−1, T is the Fig. 2. FESEM image of fabricated BN–GO composite layer on absolute room temperature (273.15 K), q is the elec- −19 SiO2/Si substrate. tronic charge (1.6 × 10 C), A is the device active area

Mater. Express, Vol. 9, 2019 267 Materials Express Inﬂuence of boron nitride nanoparticles in the electrical and photoconduction Ahmad and Thandavan

(a) (b)

Fig. 3. (a) EDX scanned area and (b) spectrum of BN–GO composite material on SiO2/Si substrate.

(9 mm2,andA∗ is the effective Richardson constant of of BN nanoparticles led to few defects in the GO bulk −2 −2 BN (0.0020 Am K . b and are the barrier height material. 32 y I and ideality factor, respectively, which need to be eval- Based on the -intercept, 0 was calculated as 94 and uated. In this measurement, V was greater than 100 mV; 86 nA for dark current and red laser illumination at thus, the term “−1” in Eq. (1) was neglegible. The reduced 650 nm, respectively. Moreover, the occurrence of barrier version of Eq. (1) could be rearranged as Eq. (3) to deter- inhomogeneity and surface states in the BN–GO compos- I mine the ideality factor and reverse saturation current ( 0). ite layer have provided multiple current pathways in the 36 D q q interface. Thus, the density of surface states ( s is best lnI = lnI + V = (3) estimated from Eq. (4): 0 kT kT × slope − i 1 BN The ideality factor is best estimatedIP: 192.168.39.211 using the dark On:I–V Mon, 27 Sep 2021 01:54:43Ds = − (4) t q2 Wq2 curve at the intermediate current range,Copyright: where theAmerican shunt Scientific Publishers i resistance and series resistance are negligible. Thus,Delivered the by Ingenta where i and ti are the dielectric constant and thickness ideality factor was determined from the slope of the linear of the interfacial layer, respectively. Given that the BN region of lnI against V as shown in Figures 6(a) and (b). Article nanoparticles seem to be incorporated into the GO bulk The ideality factors of the device were found to be dif- layer and exposed to air, the dielectric constant and thick- ferent, approximately 2.58 and 3.81 for dark current and ness are assumed to be permittivity of free space and red laser illumination at 650 nm, respectively. These val- W 5 Å, respectively. BN and are relative dielectric con- ues are slightly greater than the ideal values of a Schottky stants of BN and depletion width, which are assumed to diode, which are 1 and 2 for low and high voltages, be 4.5o and 160 nm, respectively. The calculated ide- 33 respectively. This was caused by the charge trans- ality factor values of 2.58 and 3.81 for the dark current port through junction due to thermionic emission. Under and red laser illumination at 650 nm exhibited estimated laser irradiation at 650 nm, greater thermionic emission density of surface states of 1.083 × 1036 and 1.781 × increased the ideality factor from 2.58 to 3.81. However, 1036 states/m2/eV, respectively. The barrier height was cal- these ideality factors are far lower than the reported 5.1.34 35 culated from Eq. (2), which was rearranged as and 10.4, suggesting the formation of non-amorphous nature of epitaxial BN–GO composite layer on SiO /Si kT AA∗T 2 2 b = due to rapid heating on the hotplate. Furthermore, these q ln I (5) 0 ideality factors also indicated that the random distribution where kT /q is a constant of 0.02586 V. The barrier heights Table I. Detailed element composition in BN–GO composite material of Schottky behavior photodetector were estimated to be 0.2474 and 0.2497 eV for dark current and red laser illu- on SiO2/Si substrate. mination at 650 nm, respectively. Element Line type wt% wt% sigma Atomic % The sensitivity of the fabricated photodetector was cal- BKseries2300 073 2811 culated based on the ratio of differences of photocurrent CKseries1979 049 2177 and dark current to dark current.20 The sensitivity of the NKseries3002 0 56 28 32 device toward red laser wavelength at 650 nm was eval- OKseries2536 042 2094 Si K series 183 008 086 uated accordingly as the DC bias voltage ranged from − Total: 10000 10000 3.0 V to 3.0 V. The device exhibited high sensitivity or ON/OFF ratio in percentage with DC bias ranging from

268 Mater. Express, Vol. 9, 2019 Inﬂuence of boron nitride nanoparticles in the electrical and photoconduction Materials Express Ahmad and Thandavan

(a) 20000 (b) hBN 18000

16000 G band D band 14000 Si

Intensity (a.u) 12000 823 cm–1

10000

8000 600 800 1000 1200 1400 1600 1800 2000 Wavenumber (cm–1)

Fig. 4. (a) Raman spectrum and (b) FTIR spectrum of planar BN–GO composite layer on SiO2/Si substrate.

−0.5 V to 0.5 V, which shows peak sensitivity of 6119% important figure of merit is responsivity, which is defined I P dependent on low DC bias voltage at 0.2 V (Fig. 7(a)). as the ratio of ph to incident power ( i and can be <− > R = I /P 38 I However, DC bias 1Vand 1 V showed low sensi- expressed as ph i. ph represents the differences tivity range of 100% to 800%. between the measured photocurrent and dark current. The An important figure of merit that needs to be evaluated BN–GO composite layer exhibited higher responsivity of is external quantum efficiency (EQE), which expresses the 6.5 mAW−1 in the forward bias region compared with −1 number of electrons detected per incident photon and is the negative bias region (0.3 mAW . The enhancement Article calculated as follows: EQE = hcR/e,whereh, c, e,and in responsivity was found to be approximately 2067% at are the Planck constant (6.63 × 10−34 m2kgs−1, speed the forward bias region compared with the negative bias − IP: 192.168.39.211 On: Mon, 27 Sep 2021 01:54:43 of light (3.0 × 108 ms 1, charge ofCopyright: an electron American (1.6 × Scientificregion. Publishers 10−19 C), and illuminated laser wavelenth, respectively.Delivered37 by IngentaBased on the I–V curve, 1.53×1013 electrons were cre- The forward bias region of the EQE curve (inset in ated at 2.7 V. This is due to illumination, wherein some Fig. 7(b)) shifted to the left, meaning that at 0 voltage, the electrons diffused from BN nanoparticles to GO or some device has profound increase of photocurrent (23.32 nA, were swept from GO to BN nanoparticles in the depletion which is 3450%). The number of e–h pairs generated or transition region. The presence of BN nanoparticles in per incident photon increased linearly for voltage rang- the BN–GO composite layer altered the bandgap of GO, ing from 1.4 V to 2.7 V (Fig. 7(b)). At 2.7 V, the EQE which enabled the absoprtion of photons of the red laser was 0.0125, indicating that the generation of 0.0125 signal at 650 nm. This led to the generation of e–h pairs and electrons was triggered by the incident photon. Another photocurrent in the device.

(a) 6µ Red laser 650 nm 2µ 832n 6µ Dark current 1E-6 306n 113n 41n 5µ 1E-7 15n 6n 2n 1E-8 758p y-intercept = –16.18 4µ ln current (A) 279p slope = 14.99 103p

Logscale (A) 1E-9 38p Dark current 3µ 14p (b) 6µ 1E-10 2µ Current (A) 2µ 832n 306n 1E-11 113n –3 –2 –1 0 1 2 3 1µ 41n Voltage (V) 15n 6n y-intercept = -16.27 ln current (A) 0 2n slope = 10.15 758p Red laser 650 nm

–2.5 –2.0 –1.5 –1.0 –0.5 0.0 0.5 1.0 1.5 2.0 2.5 –3 –2 –1 0 1 2 3 Voltage (V) Voltage (V)

Fig. 5. I–V characteristics of BN–GO composite under illumination Fig. 6. I–V characteristics in ln scale for (a) dark current and (b) of red laser 650 nm and inset in logscale current. under illumination at red laser 650 nm.

Mater. Express, Vol. 9, 2019 269 Materials Express Inﬂuence of boron nitride nanoparticles in the electrical and photoconduction Ahmad and Thandavan

0.014 (a) (b) 0.01 6000 Red laser 650 nm (0.2,6119.0) Red laser 650 nm 0.012 5000 0.001 0.010

(0.0,3451.0) 1E-4 4000

0.008 Log EQE

1E-5 3000 0.006 EQE

1E-6 Sensitivity (%) 2000 0.004 –3 –2 –1 0 1 2 3 Voltage (V) 0.002 1000 1.4-2.7 V 0.000 0 –3 –2 –1 0 1 2 3 –3 –2 –1 0 1 2 3 Voltage (V) Voltage (V)

–1 0.005

0.004

0.003

0.002

Responsivity (AW 0.3 mAW–1 0.001

0.000 IP: 192.168.39.211 On: Mon, 27 Sep 2021 01:54:43 Copyright:–3 American –2 –1 Scientific 0 Publishers 1 2 3 Delivered byVoltage Ingenta (V)

Fig. 7. Distribution of (a) sensitivity, (b) EQE and (c) responsivity of BN–GO composite layer and the inset is EQE in logscale. Article

3.4. Temporal Response 90% to 10%, which were measured for pulsed laser at The response speed of the planar Ag/BN–GO/Ag photode- 650 nm with various frequencies. Figure 8 shows the tem- tector is an important merit to be evaluated for the fabri- poral response of the device at frequency modulation of cated device. The rise time duration for photoresponsivity 1 Hz. The measured rise time of 30 s was faster than increased from 10% to 90%, and fall time decreased from the fall time (268 s). This is due to the attainment of saturation. This allows for the production of highly ener- Rise Time=2.99251E-5 Fall Time=2.68081E-4 gized e–h pairs that are responsible for the generation of Rise Range=0.00464 Fall Range=0.00478 photocurrent. 0.018

0.016 4. CONCLUSION

0.014 An Ag/BN–GO/Ag Schottky photodetector was success- fully fabricated using the modiﬁed Hummer’s method 0.012 and drop-casting technique. EDX spectroscopy conﬁrmed the presence of B, N, O, and C elements. Furthermore, 0.010 −1

Response (V) Raman peaks at 1355 and 1585 cm also conﬁrmed the incorporation of BN with GO in the photoconduct- 0.008 ing material. FTIR analysis veriﬁed the establishment of 0.006 BN, C C, BN–O, and B–OH bonding in the BN–GO composite material. The ideality factor, barrier height, –1.0 –0.8 –0.6 –0.4 –0.2 0.0 0.2 0.4 0.6 0.8 1.0 and density of surface states were determined based on Time (s) the thermionic emission theory. Excellent photoconduc- Fig. 8. Temporal response of planar BN–GO composite photodetector tion toward red laser at 650 nm with low ideality fac- under illumination of red laser 650 nm. tor value indicated the profound occurrence of charge

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Received: 2 November 2018. Revised/Accepted: 4 February 2019.

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