Figure 1.
The synthesis processes of LaFeO3/Fe2O3 doped with ZnO powders.
In this study, we used a natural resource, yarosite minerals, as a Fe2O3 precursor. Yarosite minerals were used for the synthesis of LaFeO3/Fe2O3 doped with ZnO via a co-precipitation method using ammonium hydroxide, which produced a light brown powder. Then, an ethanol gas sensor was prepared using a screen-printing technique and characterized using gas chamber tools at 100,200, and 300 ppm of ethanol gas to investigate the sensor's performance. Several factors that substantiate electrical properties such as crystal and morphological structures were also studied using X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM), respectively. The crystallite size decreased from about 61.4 nm to 28.8 nm after 0.5 mol% ZnO was added. The SEM characterization images informed that the modified LaFeO3 was relatively the same but not uniform. Lastly, the sensor's electrical properties exhibited a high response of about 257% to 309% at an operating temperature that decreased from 205 ℃ to 180 ℃. This finding showed that these natural resources have the potential to be applied in the development of ethanol gas sensors in the future. Hence, yarosite minerals can be considered a good natural resource that can be further explored to produce an ethanol gas sensor with more sensitive response. In addition, this method reduces the cost of material purchase.
Citation: Endi Suhendi, Andini Eka Putri, Muhamad Taufik Ulhakim, Andhy Setiawan, Syarif Dani Gustaman. Investigation of ZnO doping on LaFeO3/Fe2O3 prepared from yarosite mineral extraction for ethanol gas sensor applications[J]. AIMS Materials Science, 2022, 9(1): 105-118. doi: 10.3934/matersci.2022007
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In this study, we used a natural resource, yarosite minerals, as a Fe2O3 precursor. Yarosite minerals were used for the synthesis of LaFeO3/Fe2O3 doped with ZnO via a co-precipitation method using ammonium hydroxide, which produced a light brown powder. Then, an ethanol gas sensor was prepared using a screen-printing technique and characterized using gas chamber tools at 100,200, and 300 ppm of ethanol gas to investigate the sensor's performance. Several factors that substantiate electrical properties such as crystal and morphological structures were also studied using X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM), respectively. The crystallite size decreased from about 61.4 nm to 28.8 nm after 0.5 mol% ZnO was added. The SEM characterization images informed that the modified LaFeO3 was relatively the same but not uniform. Lastly, the sensor's electrical properties exhibited a high response of about 257% to 309% at an operating temperature that decreased from 205 ℃ to 180 ℃. This finding showed that these natural resources have the potential to be applied in the development of ethanol gas sensors in the future. Hence, yarosite minerals can be considered a good natural resource that can be further explored to produce an ethanol gas sensor with more sensitive response. In addition, this method reduces the cost of material purchase.
Many researchers are currently deliberating about gas sensors, focusing on the development of metal oxide semiconductor (MOS) gas-sensing due to its potential applications in the technology industry to monitor safety. Apart from that, it can also be employed in daily life to monitor health processes [1]. As a gas sensing material, the MOS has been developed in various forms [2], one of which is the modification of gas-sensing material by several researchers to obtain high-performance gas sensors [3,4,5,6,7]. Generally, MOSs have been used to detect harmful gases such as formaldehyde [8], toluene [9], NO2 [10], acetone [11], and ethanol [12]. Among these gases, ethanol is more widely used in daily life products, such as the food and medicine industries [13]. Ethanol easily evaporates in the air and poses considerable risks [14]. Hence, in order to ensure safety, it is crucial to develop ethanol gas sensors to monitor industrial processes.
To this date, ethanol gas sensors have been developed with various types of MOSs such as SnO2 [15], WO3 [16], Fe2O3 [17], and LaFeO3 [18]. MOS can be divided into two groups: n-type and p-type. The p-type semiconductor responds better to ethanol gases because they have excellent catalytic activity and significantly higher oxygen ion mobility [19]. The p-type semiconductor material that has been applied extensively in many ethanol gas sensors is LaFeO3 due to its high stability and tunability [20]. In addition, considerable effort has been devoted to using LaFeO3 as an ethanol-gas-sensing material due to its high resistance [21]. Also, LaFeO3 were chosen due to their good characteristics in oxidation or reduction and significant sensitive to reducing gases, such as ethanol [22].
As previously mentioned, a method of solving these problems is to modify gas-sensing materials, and in this case, by doping LaFeO3. Doping can reduce the resistance of LaFeO3 [23]. Doping is used to influence the crystal structure, morphology, and electrical properties of the material to optimize the performance of gas sensors [24], including LaFeO3-based ethanol gas sensors. Many researchers have applied this treatment and added some doping to LaFeO3 using various elements such as Mg [25], Zn [26], Ag [26,27], Cr [28], and Co [28,29]. Among these elements, Zn is rarely used even though it provides a better response in ethanol gas sensors; it was used by Chen et al. [26], who reported that Zn doping plays an important role because it can reduce the resistance even by small amounts. In addition, the presence of Zn increases the response to ethanol gases. Zn doping affects Fe2+ ions, creating oxygen vacancies and increasing the amount of electron hopping of Fe3+–Fe2+ [30]. These processes can increase the gas-sensing properties of the materials, such as the electrical properties, i.e., the response and operating temperature [31]. This shows that the influence of doping of gas-sensing material is a topic requiring further study. The LaFeO3/Fe2O3 co-doped Ca and Zn was synthesized, and found that the gas sensor performance, especially the response to detecting ethanol, had significantly improved. The response to ethanol gases increased by about 41% compared to LaFeO3/Fe2O3 without doping [32], demonstrating the potential for applying doping for improving gas sensor performance.
Based on the above, in this study, LaFeO3 modified with the addition of 0.5 mol% ZnO was synthesized for application in ethanol gas sensing based thick film that was fabricated using screen printing. The dose of 0.5 mol% ZnO doping was chosen based on the previous studies from Lai et al. [33] that using the composition of ZnO with the amount of 0.5 mol% and exhibited a good characteristics to applied as gas sensing application. Hence, in this research we used 0.5 mol% for the dosage of ZnO doping to establish the performance of LaFeO3/Fe2O3 will do better as the previous work or worse. Then, screen printing is a technology that is commonly used for thick-film fabrication, and it can produce multiple layers of the thick film [34]. The advantages of applying screen printing for gas sensing is its low cost and the easy deposition of thick-film layers [35,36]. However, a large deposition affects the gas sensor's performance. The proposed ethanol gas sensor based on modified LaFeO3/Fe2O3 with the addition of 0.5 mol% ZnO is characterized using X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), and electrical properties to determine its performance.
Extracted and purified yarosite minerals were used as the ferric oxide (Fe2O3) precursor in the preparation of LaFeO3/Fe2O3 doped with 0.5 mol% ZnO powders. The other chemicals, i.e., lanthanum chloride heptahydrate (LaCl3‧7H2O), zinc sulfate (ZnSO4), hydrochloric acid (HCl) 2.0 M, distilled water, and ammonium hydroxide (NH4OH), were of analytical grade. Then, the thick film ceramics were prepared using alumina substrate, silver paste (Ag), ethyl cellulose, and alpha-terpineol. For ethanol detection, we used 97% ethanol as the target.
The LaFeO3/Fe2O3 doped with 0.5 mol% ZnO powders is synthesized using the co-precipitation method, as illustrated in Figure 1. Firstly, 50 mol% LaCl3‧7H2O is dissolved in the distilled water. Then 49.5 mol% Fe2O3 and 0.5 mol% ZnSO4 are dissolved in the 2.0 M HCl, separately, with a magnetic stirrer at room temperature. Afterwards, each solution is produced by simultaneously mixing and stirring until it becomes homogeneous. Next, NH4OH is slowly added until the solution reaches pH = 7 and it is then left for 12 h. Next, the precipitate is filtered and dried at 100 ℃ for 6 h. Lastly, the product is calcined at 800 ℃ for 6 h until the brown light powders are produced. This experiment also synthesizes the dark brown powders of LaFeO3/Fe2O3 using the same treatment for comparison.
Firstly, each material is produced using the synthesis process, consisting of LaFeO3/Fe2O3, and its modification of 0.5 mol% ZnO doped, which are prepared using material paste. These processes are performed by mixing the synthesized materials and organic vehicles in a ratio of 7:3. First, the mixtures are manually stirred using a stainless micro spatula for about 2 h until they become homogeneous. The organic vehicle is then fabricated from a mixture of ethyl cellulose and alpha-terpineol in a ratio of 1:9.
Second, thick-film ceramics are fabricated using the screen-printing technique using alumina as the substrate, which has a thickness of about 0.5 mm and a size of 1.0 × 0.5 cm, as shown in Figure 2a. The process starts with printing the silver paste (Ag) as the material electrode is placed over the alumina substrates, as shown in Figure 2b, and fired at 600 ℃ for 10 min. Then, the material paste is printed over the silver coating, as shown in Figure 2c, and fired at 600 ℃ for 2 h.
The ethanol gas sensor based on thick-film ceramic LaFeO3/Fe2O3 and its modification with 0.5 mol% ZnO were respectively characterized in terms of crystal and morphological structure using XRD and SEM. XRD characterization was performed using a PANanalytical X'Pert Pro Series PW3040/x0 X'Pert Pro with a CuKα1 wavelength of 1.5404 × 10−10 m.
The XRD characterization was used to determine the average of crystallite size that was calculated using the Debye-Scherrer formula as shown in Eq 1 [37,38,39,40,41]. Where λ is the x-ray wavelength used in this characterization, B is the peak of full width at half-maximum (FWHM) intensity, and θ is the angle of Bragg diffraction.
| D=0.89λBcosθ | (1) |
SEM characterization was conducted using scanning electron microscopy analysis (JEOL JSM-6360LA). SEM was used to characterize the grain size of the materials. Further, the electrical properties were also considered to investigate the sensor's ethanol gas detection performance. The electrical properties were characterized using a static gas chamber as previously reported [32]. The electrical properties investigated included the responses and operating temperature of the ethanol gas sensor based on LaFeO3 and its modification. In this work, the samples were placed in a static gas chamber without ethanol gas as the ambient condition, with various ethanol gases conditions, i.e., 100,200, and 300 ppm. The output of this characterization was the resistance value of the thick film that was measured at various temperatures (from room temperature up to 215 ℃) and displayed by an ohmmeter. This process determines the resistance value. Then, the resistance value was processed and calculated using Eq 2 to obtain the response of LaFeO3/Fe2O3 and its modification with 0.5 mol% ZnO doped in ethanol detection processes [42,43,44,45,46]. Where Rg is the resistance of the gas sensor in ethanol gas and Ra is the resistance of the gas sensor in air (ambient condition or without ethanol gas).
| Response =RgRa×100% | (2) |
In this research, we reported the data accomplished in the experiment. Firstly, the synthesis process was conducted to produce the materials, LaFeO3/Fe2O3 and its modification with 0.5 mol% ZnO doped. This process produced the dark brown powders for LaFeO3/Fe2O3 and brown light powders for 0.5 mol% ZnO doped LaFeO3/Fe2O3. Then, both of the materials were characterized using XRD to determine their crystal characteristics within the results, as shown in Figure 3. This characterization also indicates the crystallite size and their effect on the performance of LaFeO3/Fe2O3 and its modification with 0.5 mol% ZnO doped as ethanol gas sensing. The crystallite size is calculated using Eq 1 and produces the results in Table 1. These results show that 0.5 mol% ZnO doped decreases the crystallite size of LaFeO3/Fe2O3.
| Material | Crystal structures | Lattice Parameters (Å) | Crystallite Size (nm) |
| LaFeO3 | cubic | 3.8977 | 61.4 |
| LaFeO3/ Fe2O3 with 0.5 mol% ZnO | cubic | 3.9516 | 28.8 |
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Furthermore, the SEM characterization was also conducted to determine the morphological properties of LaFeO3/Fe2O3 and its modification with 0.5 mol% ZnO doped. The characterization results are shown in Figure 4. These results indicate that the grain sizes of the materials are relatively similar but not uniform.
Lastly, the electrical properties characterization was conducted to determine the performance of LaFeO3/Fe2O3 and its modification with 0.5 mol% ZnO doped to detect the ethanol gases. This performance test was conducted by resistance measurement using an ohmmeter. First, the resistance measurement is conducted in the different concentrations of ethanol gases, i.e., with 100 ppm, 200 ppm, and 300 ppm. Then, the resistance value is graphically indicated as the temperature function, as shown in Figure 5.
As mentioned in Section 2.3, the resistance value obtained from the experiment was calculated using Eq 2 and produced the response of LaFeO3/Fe2O3 and its modification with 0.5 mol% ZnO doped in the processes of ethanol gas detection. The response value is shown in Figure 6. The response of LaFeO3/Fe2O3 increases from 257% to 309% at 300 ppm. Figure 6 also illustrates that the operating temperature of LaFeO3/Fe2O3 decreases from 205 ℃ to 180 ℃, caused by the 0.5 mol% ZnO doped.
In this experiment, we had been successfully synthesized the LaFeO3/Fe2O3 and its modification with 0.5 mol% ZnO doped. Then, these materials were characterized using XRD, SEM, and electrical properties.
XRD pattern shows that the materials have two phases, i.e., LaFeO3 and Fe2O3, and it has been fitted with the JCPDS No. 96-154-2033 for LaFeO3 and JCPDS No. 96-101-1241 for Fe2O3. The JCPDS number were known from the analysis process using Match 3. However, there are still other peaks in the XRD pattern, possibly caused by the impurities of yarosite minerals shown in Table 2. The impurities of the yarosite mineral have been reported by Ariyani et al. [47].
| No. | Compound | wt% |
| 1 | Fe2O3 | 91.30 |
| 2 | Al2O3 | 3.30 |
| 3 | SiO2 | 2.05 |
| 4 | TiO2 | 3.02 |
| 5 | CaO | 0.16 |
| 6 | MnO | 0.17 |
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The XRD data also inform the crystallite size, as shown in Table 1. This experiment shows that the crystallite size decreases drastically after 0.5 mol % zinc oxide is added into LaFeO3/Fe2O3. The crystallite size affects the response of a gas sensor. The smaller the crystallite size, the better the response of the gas sensor [48]. Apart from that, the other characterization conducted in this experiment is SEM. This characterization informed that 0.5 mol% ZnO doped influences the morphological structure of LaFeO3/Fe2O3. Based on Figure 4, it is found that the 0.5 mol% ZnO doped also decreases the grain size of LaFeO3/Fe2O3, and it has an effect on the materials' performance in the detecting the target, which in this research is ethanol gases.
The performance test starts with the resistance measurement of both materials, LaFeO3/Fe2O3 and its modification of 0.5 mol% ZnO doped. This process produces the graphic of resistance function to the temperature, as shown in Figure 5. It informs that the resistance increases as the ethanol gas concentration increases, confirming that LaFeO3/Fe2O3 and its modification with 0.5 mol% ZnO doped are p-type semiconductors [49]. This is strengthened by the claim that the p-type semiconductor of the gas sensor has a greater resistance in the ethanol contained solution compared to in the ambient condition [50].
Then, the resistance is calculated using Eq 2 to produce the value of the gas sensor response of LaFeO3/Fe2O3 and its modification, as shown in Figure 6. The results show that the response of the gas sensor is affected by the concentration of ethanol gas. In addition, the dopant also strongly affects the gas response, with is similar to the result reported by Gao et al. [51].
In this research, as explained in the previous section, the response of LaFeO3/Fe2O3 increases when 0.5 mol% zinc oxide is added. The modification of LaFeO3/Fe2O3 with 0.5 mol% zinc oxide produces a suitable gas-sensing material. It is known from the compares results of this study with the other studies of LaFeO3 or Fe2O3 that have been applied as ethanol gas sensors with the addition of doping as listed in Table 3. From the Table 3 were known that the type of doping was influence the response value of LaFeO3 or Fe2O3. It caused by the different characteristics of the doping. The doping can help the LaFeO3 or Fe2O3 to bind the oxygen atoms that contains in ethanol gases [52]. Therefore, Suhendi et al. [32] reported that using co-doping has a higher response than this work.
| Elements doping | Concentration (ppm) | Response | Operating temperature (℃) | Ref |
| Zn | 300 | 3.09 | 180 | This work |
| Co-doped Ca and Zn | 300 | 3.65 | 190 | [32] |
| Sr | 300 | 3.05 | 300 | [37] |
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The addition of 0.5 mol% zinc oxide also decreases the operating temperature of LaFeO3/Fe2O3, indicating that zinc oxide doping improves the characteristics of LaFeO3/Fe2O3 as a gas-sensing material. The reduce operating temperature of undoped and 0.5 mol% zinc oxide doped LaFeO3/Fe2O3 were caused by the different activation and adsorbing energies from both materials [53]. The mechanism was described by the LaFeO3 sensing processes that occurred as a result of the interaction between absorbed gas molecules in the surface of the gas sensor that change the conductivity [54]. Nonetheless, the main reason of zinc oxide doping could be reducing the operating temperature for LaFeO3/Fe2O3 is zinc oxide has high reactivity and easy adsorption of oxygen atoms which is contained in ethanol, its characteristics were help LaFeO3/Fe2O3 to capture ethanol gases molecules around the surface [52].
The sensing mechanism through which LaFeO3/Fe2O3 and its modification detect ethanol gases is explained by the adsorption and desorption of gas molecules on the surface of the thick film. When the surface of the thick film is exposed to air (without ethanol gases), the oxygen molecules are absorbed by the material's surface to produce chemisorbed oxygen. The chemisorbed oxygen catches the electrons of the conduction band (CB). These processes can be explained by the reaction shown in Eqs 3–5 [55,56,57].
| O2(gas)↔O2(ads) | (3) |
| O2(ads)+e−(CB)↔O−2(ads) | (4) |
| O−2(ads)+e−(CB)↔2O−(ads) | (5) |
When the thick-film surface is exposed to ethanol, the adsorbed oxygen reacts with ethanol by releasing the trapped electrons to the gas-sensing material, in this case, LaFeO3/Fe2O3 and its modification. These processes cause the resistance of the gas-sensing material to increase when it is exposed to ethanol gas, as shown in Figure 5. The interaction of adsorbed oxygen and ethanol can be explained in the reaction shown in Eq 6 [58].
| C2H5OH(gas)+6O−↔2CO2+3H2O+6e− | (6) |
In summary, ethanol gas sensors based on LaFeO3/Fe2O3 doped with 0.5 mol% zinc-oxide-based thick-film ceramics were produced using a screen-printing technique. We also used yarosite minerals as the Fe2O3 precursor to Indonesia's natural resources. The performance of the gas sensors was investigated using three types of characterizations, i.e., XRD to determine the crystal structure, SEM to determine the morphological structure, and electrical properties to determine the ability of the materials to detect ethanol gas. These characterizations show that yarosite minerals have the potential to be applied in ethanol gas sensors. ZnO doping reduces the crystallite size and grain size of LaFeO3/Fe2O3, causes the materials to bind the targets more easily and improves the response of ethanol gas sensors. Importantly, ZnO doping increases the response of LaFeO3/Fe2O3 to detect ethanol gases from about 257% to 309%. Lastly, the use of yarosite minerals reduces the cost of the fabrication process. Overall, the results show that doping plays an important role in improving the performance of gas-sensing materials; LaFeO3/Fe2O3 and yarosite minerals can be further explored to improve ethanol gas sensing in the future.
This work was financially supported by "Hibah Penelitian Terapan Unggulan Perguruan Tinggi Kementerian Pendidikan, Kebudayaan, Riset, dan Teknologi Republik Indonesia" research grants for the 2020 fiscal year.
The authors declare no conflict of interest.
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| 1. | Prakash Sudalaimani, Suvitha Athisayasa Rajah, Ananth Steephen, Ajay Pulavazhy, Bradha Madhavan, Perovskite oxides (LaFeO3) incorporated with reduced graphene oxide for electromagnetic interference shielding, 2024, 13, 2045-9831, 32, 10.1680/jnaen.23.00049 | |
| 2. | Hasniah Aliah, Ryan Nur Iman, Andhy Setiawan, Dani Gustaman Syarif, Asti Sawitri, Assa Prima Dasti Putri, Edi Suharyadi, Irfan Syafar Farouk, Utilization of jarosite and manganite mineral as raw material to fabricate metal-oxide composite film for gas sensor application, 2024, 848, 00092614, 141398, 10.1016/j.cplett.2024.141398 | |
| 3. | Endi Suhendi, Muhamad Taufik Ulhakim, Dani Gustaman Syarif, 2025, Chapter 1, 978-981-96-0659-7, 1, 10.1007/978-981-96-0660-3_1 | |
| 4. | Andhy SETIAWAN, Farah Aprisza SHEELMAREVAA, Muhamad Taufik ULHAKIM, Dani Gustaman SYARIF, Endi SUHENDI, Enhancing acetone gas sensor performance with cobalt oxide doping in LaFeO\(_{3}\) prepared by co-precipitation, 2025, 35, 2630-0508, e1919, 10.55713/jmmm.v35i1.1919 |
Endi Suhendi, Andini Eka Putri, Muhamad Taufik Ulhakim, Andhy Setiawan, Syarif Dani Gustaman. Investigation of ZnO doping on LaFeO3/Fe2O3 prepared from yarosite mineral extraction for ethanol gas sensor applications[J]. AIMS Materials Science, 2022, 9(1): 105-118. doi: 10.3934/matersci.2022007
| Material | Crystal structures | Lattice Parameters (Å) | Crystallite Size (nm) |
| LaFeO3 | cubic | 3.8977 | 61.4 |
| LaFeO3/ Fe2O3 with 0.5 mol% ZnO | cubic | 3.9516 | 28.8 |
DownLoad:
CSV
| No. | Compound | wt% |
| 1 | Fe2O3 | 91.30 |
| 2 | Al2O3 | 3.30 |
| 3 | SiO2 | 2.05 |
| 4 | TiO2 | 3.02 |
| 5 | CaO | 0.16 |
| 6 | MnO | 0.17 |
DownLoad:
CSV
| Elements doping | Concentration (ppm) | Response | Operating temperature (℃) | Ref |
| Zn | 300 | 3.09 | 180 | This work |
| Co-doped Ca and Zn | 300 | 3.65 | 190 | [32] |
| Sr | 300 | 3.05 | 300 | [37] |
DownLoad:
CSV
| Material | Crystal structures | Lattice Parameters (Å) | Crystallite Size (nm) |
| LaFeO3 | cubic | 3.8977 | 61.4 |
| LaFeO3/ Fe2O3 with 0.5 mol% ZnO | cubic | 3.9516 | 28.8 |
| No. | Compound | wt% |
| 1 | Fe2O3 | 91.30 |
| 2 | Al2O3 | 3.30 |
| 3 | SiO2 | 2.05 |
| 4 | TiO2 | 3.02 |
| 5 | CaO | 0.16 |
| 6 | MnO | 0.17 |
| Elements doping | Concentration (ppm) | Response | Operating temperature (℃) | Ref |
| Zn | 300 | 3.09 | 180 | This work |
| Co-doped Ca and Zn | 300 | 3.65 | 190 | [32] |
| Sr | 300 | 3.05 | 300 | [37] |
