Ảnh hưởng của việc sấy lên từ tính của vật liệu composite Ba₁-ₓLaₓFe₁₂O₁₉/polyaniline

Nội dung text: Ảnh hưởng của việc sấy lên từ tính của vật liệu composite Ba₁-ₓLaₓFe₁₂O₁₉/polyaniline

1. 94 Tran Ngo, Tran Nguyen Tien / Tạp chí Khoa học và Công nghệ Đại học Duy Tân 02(45) (2021) 94-102 02(45) (2021) 94-102 Effect of drying on magnetic properties of Ba1-xLaxFe12O19/polyaniline composites Ảnh hưởng của việc sấy lên từ tính của vật liệu composite Ba1-xLaxFe12O19/polyaniline Tran Ngoa,c*, Tran Nguyen Tienb,c Trần Ngọa,c*, Trần Nguyên Tiếnb,c aCenter for Materials Science, Institute of Research and Development, Duy Tan University, Da Nang 550000, Vietnam aTrung tâm Khoa học Vật liệu, Viện Nghiên cứu và Phát triển Công nghệ Cao, Đại học Duy Tân, Đà Nẵng bCenter for Advanced Chemistry, Institute of Research and Development, Duy Tan University, Da Nang, 550000, Vietnam bTrung tâm Hóa học Tiên tiến, Viện Nghiên cứu và Phát triển Công nghệ Cao, Đại học Duy Tân, Đà Nẵng cFaculty of Natural Sciences, Duy Tan University, Da Nang, 550000, Vietnam cKhoa Khoa học Tự nhiên, Đại học Duy Tân, Đà Nẵng (Ngày nhận bài: 17/03/2021, ngày phản biện xong: 24/03/2021, ngày chấp nhận đăng: 29/03/2021) Abstract Composites of Ba1-xLaxFe12O19/polyaniline were successfully prepared. By using X-ray diffractometer, the secondary phase of α-Fe2O3 was detected besides the main phase of Ba1-xLaxFe12O19. Phase percentage of α-Fe2O3 increased with the increase of La doping concentration. Lattice parameters, a and c, of the main phase were decreased with respect to the increase of the La doping concentration, x. The decrease of a and c could be attributed to the substitution of small 3+ 2+ ionic of La to the larger one of Ba . The effects of drying on magnetic properties of Ba1-xLaxFe12O19/polyaniline composites were studied in two cases: un-dried and dried composites. All the magnetic parameters such as saturation magnetization, remanent magnetization, coercivity, magnetocrystalline anisotropy, magnetocrystalline anisotropy constant, and magnetocrystalline anisotropy field of the dried composites were lower than the undried ones. This change would affect the microwave absorbing properties of the composites. Keywords: Hexaferrite; polyaniline; composite; magnetic properties. Tóm tắt Chúng tôi đã chế tạo thành công vật liệu composite của Ba1-xLaxFe12O19/polyaniline và tiến hành khảo sát cấu trúc bằng máy tán xạ phổ tia X. Bên cạnh pha chính của Ba1-xLaxFe12O19, phổ tán xạ tia X còn ghi nhận sự xuất hiện của pha phụ α-Fe2O3. Tỉ lệ phần trăm của pha phụ α-Fe2O3 tăng khi nồng độ pha tạp La tăng lên. Các thông số mạng a và c của pha chính giảm khi nồng độ La tăng lên. Điều này có thể là do sự thay thế của một ion có bán kính nhỏ (La3+) cho một ion có bán kính hơn (Ba2+). Ảnh hưởng của việc sấy lên tính chất từ của vật liệu composite cũng đã được khảo sát. Để tiến hành khảo sát này, vật liệu composite ban đầu được chia thành hai lô: lô 1 được giữ nguyên sau khi chế tạo (gọi là “không sấy”) và lô 2 được đem đi nung ở 170C (gọi là “sấy”). Thông số từ thu được từ hai lô composite thể hiện sự khác nhau lớn. Tất cả các giá trị của từ độ bão hòa, từ dư, lực kháng từ, tính dị hướng từ, hằng số dị hướng từ và trường *Corresponding Author: Tran Ngo; Center for Materials Science, Institute of Research and Development, Duy Tan University, Da Nang 550000, Vietnam; Faculty of Natural Sciences, Duy Tan University, Da Nang, 550000, Vietnam. Email: tranngo@duytan.edu.vn
2. Tran Ngo, Tran Nguyen Tien / Tạp chí Khoa học và Công nghệ Đại học Duy Tân 02(45) (2021) 94-102 95 dị hướng từ của “sấy” composite luôn thấp hơn “không sấy” composite. Sự thay đổi về từ tính này sẽ có ảnh hưởng đến tính chất hấp thụ sóng viba của composite. Từ khóa: Hexaferrite; polyaniline; composite; tính chất từ. 1. Introduction second and third approaches by substituting La to Ba site of BaM and composites with PANI, Barium M-type hexaferrite (BaFe12O19, BaM) and strontium M-type hexaferrite respectively. (SrFe12O19, SrM) belong to the hexaferrite In order to fabricate composites, we firstly family which includes six types: M-, W-, Y-, Z, prepared Ba1-xLaxFe12O19 compounds with x = U-, and X-types. M-type hexaferrite has 0–0.5. Then, the compounds were carefully simplest formula and could be described as mixed with PANI to get the composites. BaO/SrO + 6·Fe2O3. BaM is an important hard Finally, we mixed the composites with a binder, magnetic material based on its excellent epoxy, to prepare toroidal devices. Magnetic characteristics such as: uniaxial loss which comes from magnetic properties of magnetocrystalline anisotropy, high composites play an important role to the permeability, high saturation magnetization microwave absorption properties. While, the (Ms), high coercivity (Hc), and good chemical drying could lead to changes of magnetic stability [1]. BaM is also a promising material properties which were motivated us to carry out for microwave absorbing due to a magnetic loss this work. In this work, we report the effects of which is mainly produced by a natural drying on magnetic properties of composites of resonance [2]. However, there are some Ba1-xLaxFe12O19/polyaniline which have disadvantages that could limit the microwave divided into two batches: the first batch was as- absorbing applications of BaM such as low prepared composites (named as un-dried dielectric constant [3], large magnetocrystalline composites) and the second batch was dried at anisotropy field, Ha = 17 kOe, and high 170°C for 30 min (named as dried composites) ferromagnetic resonance frequency, fr = 47.6 2. Experimental details GHz [4]. La doping BaFe12O19 (Ba1-xLaxFe12O19, In order to improve the application La-BaM, x = 0–0.5) compounds were prepared capability, researchers have been attempting to by a co-precipitation method followed by heat improve dielectric loss and reduce treatment at 900°C for 3 h in a box furnace. ferromagnetic resonance frequency. There were High-purity chemicals of Ba(NO3)2, La2O3, and several approaches that have been studied such Fe(NO3)39H2O (purchased from Sigma- as combining BaM with other soft magnetic Aldrich) were used as precursors. The detailed materials [5-7], preparing compound of BaM preparation process was reported in Ref. [17]. with high dielectric constant materials (carbon PANI was prepared from a mono-aniline [8], reduced graphene oxide [9], polyaniline solution using the polymerization method (PANI) [10], MoS2 [3], Ti3SiC2 [11], and which was presented in Ref. [18]. In order to carbon nanotubes (CNTs)/multi-walled CNTs prepare the composites, La-BaM samples were [12, 13]), and changing Ha and Ms to get mixed with PANI by the weight ratio of sample desiring fr by using cationic substitution [1, 2, and PANI being La-BaM/PANI = 9/1. After 14-16]. In order to improve the microwave that, the composite of La-BaM/PANI was absorption properties of BaM, we combined the mixed with 15 wt% epoxy. The composites
3. 96 Tran Ngo, Tran Nguyen Tien / Tạp chí Khoa học và Công nghệ Đại học Duy Tân 02(45) (2021) 94-102 were divided into two batches: one batch was peaks. The decreasing of a and c could be dried in a dryer at 170°C for 30 min which attributed to the substitution of a small ion 3+ 2+ named as dried-composites; the other one was (rLa = 1.172 Å) for a larger ion (rBa = 1.49 kept as-prepared and named as un-dried Å) [20]. The decreasing of a and c also proved composites. Crystal structure of composites that La was not replaced for Fe in BaFe12O19 was studied by XRD (Rigaku, Miniflex model) hexaferrites. If so, a and c would be increased working with a Cu-K radiation source ( = with respect to the increasing of La doping 3+ 3+ 1.54056 Å). Magnetic properties of the concentration because ionic radii of Fe (rFe 3+ 3+ composites were studied by using the vibrating = 0.785 Å) is smaller the one of La (rLa = sample magnetometer (VSM, LakeShore, 1.172 Å) [20]. We also found similar results in model 7404) with the applied field can be the studies of La doping BaM M-type [21, 22], varied in the range of 0–10 kOe. La doping SrCo2W W-type [23], and La doped BaCo Z Z-type [17] hexaferrites. The increase 3. Results and Discussion 2 of secondary phase of α-Fe2O3 could be XRD patterns of dried-composites at room attributed to the generation of Fe2+ to keep the temperature were presented in Fig. 1. PANI charge balance basing on equation Ba2+ + Fe3+ was crystallized in a bulk-type sample with La3+ + Fe2+ [17]. This equation meant that some peaks in the range of 20–28° [19]. the more La3+ was introduced to the BaM, the Meanwhile, Ba1-xLaxFe12O19 samples were more Fe2+ was generated in the BaM. The same crystallized into the M-type hexagonal structure phenomenon could be found in the work of P. which belongs to the P63/mmc space group. Mariño-Castellanos et. al. with La-doping Because of the very low-intensity PANI peaks, concentration up to 60% [22]. there was almost no trace of PANI in the XRD patterns of Ba1-xLaxFe12O19/polyaniline composites. Compared to the standard pattern of BaM hexaferrites, our composites showed some peaks of secondary phase which belonged to α-Fe2O3. The percentage of impurity phase increased with respect to the La doping concentration from 3.76% for x = 0 to 37.21% for x = 0.5. We also calculated lattice parameters, a and c, and volume cell, V, of the dried-composites for M-type hexaferrite phase. Both of the a and c decreased when La doping concentration increased: a decreased from 5.893 Å for x = 0 to 5.889 Å for x = 0.5; while Figure 1. XRD patterns of Ba1-xLaxFe12O19/polyaniline c decreased from 23.218 Å for x = 0 to 23.114 composites. The asterisks show the secondary phase of Å for x = 0.5. Therefore, V consequently α-Fe2O3. decreased from 698.369 Å3 to 694.988 Å3 when Figure 2 shows the all room-temperature x increased from 0 to 0.5. The variations of a, c, M(H) hysteresis loops of Ba1- and V mainly depended on the La-substitution xLaxFe12O19/polyaniline composites. The due to low intensity of polyaniline XRD pattern undried composites were represented in solid-
4. Tran Ngo, Tran Nguyen Tien / Tạp chí Khoa học và Công nghệ Đại học Duy Tân 02(45) (2021) 94-102 97 symbol-loops and the dried composites were 2 could be divided into two groups. The first plotted in opened-symbol loops. In order to group included x = 0.1 (Fig. 2(b)), x = 0.3 (Fig. have a visual look, we plotted the undried and 2(d)), and x = 0.5 (Fig. 2(f)) which showed dried composites in separate figures for each similar shapes between un-dried and dried sample. Obviously, all the M(H) loops of our composites. The second group included x = 0 samples have a shape similar to that of other (Fig. 2(a)), x = 0.2 (Fig. 2(c)), and x = 0.4 (Fig. M-type ferro/ferrimagnets [14, 16, 24-26]. 2(e)) which have bent and shrunk in the center Values of coercivity (Hc), remanent parts of the loops. The values of Hc and Mr magnetization (Mr), and Ms of all undried could be determined from intercepts of the composites were higher than that of dried ones. loops with x- and y-axes, respectively. The Compared to the shape of loops between values of Hc and Mr have been listed in Table 1 undried- and dried-composites, six plots in Fig. and Table 2. Figure 2. M(H) loops for undried (solid-symbol loops) and dried (opened-symbol loops) composites of Ba1- xLaxFe12O19/polyaniline with (a) x = 0, (b) x = 0.1, (c) x = 0.2, (d) x = 0.3, (e) x = 0.4, and (f) x = 0.5, respectively. Table 1. Experimental values obtained from analyzing M(H) hysteresis loops for undried composites of Ba1-xLaxFe12O19/polyaniline at room temperature. Sample H M M b H K c r s M /M a 1 (undried) (kOe) (emu/g) (emu/g) r s (106 Oe2) (kOe) (105 erg/cm3) x = 0 5.06 32.04 58.35 0.55 8.175 11.073 3.231 x = 0.1 4.91 32.52 58.86 0.55 8.019 10.967 3.228 x = 0.2 5.20 32.61 59.04 0.55 8.096 11.020 3.253 x = 0.3 4.52 29.99 54.83 0.55 7.970 10.934 2.998 x = 0.4 4.78 28.08 51.78 0.54 8.092 11.017 2.852 x = 0.5 5.37 23.72 43.53 0.54 8.293 11.153 2.428 In order to compare the Hc tendency of concentration, as shown in Fig. 3. Obviously, undried and dried composites, we plotted Hc Hc values of the undried composites higher than curves as a function of La-doping that of dried ones for all doping concentration.
5. 98 Tran Ngo, Tran Nguyen Tien / Tạp chí Khoa học và Công nghệ Đại học Duy Tân 02(45) (2021) 94-102 In detailed, the Hc values for undried emu/g for x = 0.5. Compared between undoped composites decreased for first doping (x = 0.1), and doped composites, drying reduced the Mr then increased for x = 0.2, then decreased to values with the reduction in the range of 3–11%. lowest value with x = 0.3, and rose up for x = 0.4 and reached highest value for x = 0.5. The case of Hc values for dried composites were a bit simple: Hc increased for x = 0.1, then decreased for higher doping (x = 0.2–0.4), then increased for x = 0.5 composites. The lowest and highest values of Hc for dried composites were found for x = 0.4 and 0.5, respectively. The variation of Hc could be partly attributed to the present of α-Fe2O3 and spin canting. In contrary to Hc, tendency of Mr values were simple (shown by red curves in Fig. 4). Figure 3. H curves as a function of La-doping For undried composites, the Mr slightly c concentration for undried (solid-symbol curve) increased from 32.04 emu/g for x = 0, to 32.52 and dried (opened-symbol curve) composites of emu/g for x = 0.1, to 32.61 emu/g for x = 0.2 Ba1-xLaxFe12O19/polyaniline. then decreased for higher doping concentration to lowest value as Mr = 23.72 emu/g for x = 0.5. Table 2. Experimental values obtained from In the case of dried composites, the Mr analyzing M(H) hysteresis loops for dried increased from 30.63 emu/g for x = 0 to 31.47 composites of Ba1-xLaxFe12O19/polyaniline at emu/g for x = 0.1, then decreased for higher room temperature. doping concentration down to Mr = 21.69 Sample H M M b H K c r s M /M a 1 (dried) (kOe) (emu/g) (emu/g) r s (106 Oe2) (kOe) (105 erg/cm3) x = 0 4.22 30.63 57.13 0.54 8.209 11.097 3.170 x = 0.1 4.86 31.47 56.82 0.55 7.955 10.924 3.103 x = 0.2 4.64 29.92 54.74 0.55 8.001 10.955 2.999 x = 0.3 4.23 28.74 52.45 0.55 7.741 10.775 2.826 x = 0.4 3.79 24.91 46.49 0.54 7.980 10.941 2.543 x = 0.5 5.03 21.69 39.77 0.55 7.996 10.952 2.178 From Fig. 2, we could observe that the where a’ is inhomogeneities (approximately hysteresis loops were not saturated in the equal to zero) and b is magnetocrystalline applied magnetic field range of 0–10 kOe. anisotropy. The second term of χH is the high- Therefore, the Ms could be obtained from the field differential susceptibility related to the hysteresis loop by employing the “Law of spontaneous magnetization of magnetic approach to saturation (LAS)” method. The domains and active in high temperature LAS is defined as [27]: analysis. Equation (1) could be shortened to the following equation: , (1)
6. Tran Ngo, Tran Nguyen Tien / Tạp chí Khoa học và Công nghệ Đại học Duy Tân 02(45) (2021) 94-102 99 , (2) particles existed in undried and dried composites of Ba1-xLaxFe12O19/polyaniline. In this work, Eq. (2) was used to fit the M(H) data at high field of H = 7–10 kOe. The values of Ms were plotted in Fig. 4 by black curves. For undried composites, Ms slightly increased from 58.35 emu/g for x = 0 to 58.86 emu/g for x = 0.1, to 59.04 emu/g for x = 0.2, then decreased for higher doping concentration. While, the Ms values of dried composites decreased when La concentration increased. Similar to Mr values, the Ms values of dried composites were lower than undried composites with reduction of 2–10 %. The decreasing of Mr Figure 4. Ms and Mr curves as a function of La-doping 2+ concentration for undried (solid-symbol curves) and Ms was caused by the replacement of Ba and dried (opened-symbol curves) composites of 3+ by La , as well as by the presence of the Ba1-xLaxFe12O19/polyaniline. secondary phase. Due to the substitution of Ba2+ by La3+, the ionic state of Fe reduced from By using LAS, we also determined Fe3+ to Fe2+ which might decrease the strength magnetocrystalline anisotropy, b, from the of the Fe3+–O–Fe3+ double-exchange slope of fitting line of magnetization where interactions. In addition, the weakening of slope is a product of b and Ms. The b values of magnetization could be attributed to spin undried and dried composites were shown in canting [15, 28]. On the other hand, the the top plot of Fig. 5. The curves of b have secondary phase of hematite (α-Fe2O3) is similar tendency to the curves of Hc for undried antiferromagnetic which could also be a composites. Compare the b curves between contributor to the reduction of Ms and Mr undried and dried composites, the b values of values. We also calculated the squareness ratio undried composites were higher than the dried Mr/Ms of undried and dried composites (listed ones except x = 0 composite. The K1 values of in Table 1 and Table 2). Considering the Mr/Ms undried and dried composites also calculated ratio, the following phenomena was through the following expression: determined: (i) Mr/Ms < 0.5: there is a dominance of the magnetostatic interaction , (3) between particles; (ii) Mr/Ms = 0.5: there is a With b and Ms obtained above, we have dominance of randomly oriented non- calculated the values of Ha and K1, listed in interacting particles under coherent rotation; Table 1 and Table 2. From Eq. (3), we could and (iii) 0.5 < Mr/Ms < 1: exchange coupling clearly observe that Ha is directly proportion to between particles takes place [29]. In our b. Therefore, the Ha has the variation work, Mr/Ms values were in the range of 0.54– tendencies similar to that of b, as shown in the 0.55, proving the exchange coupling between bottom plot of Fig. 5.
7. 100 Tran Ngo, Tran Nguyen Tien / Tạp chí Khoa học và Công nghệ Đại học Duy Tân 02(45) (2021) 94-102 Figure 5. (top) Magnetocrystalline anisotropy, b, and (bottom) magnetocrystalline anisotropy field, Ha, curves as a function of La-doping concentration for undried (solid-symbol curves) and dried (opened-symbol curves) composites of Ba1-xLaxFe12O19/polyaniline. While, the K1 values which calculated Ms, Mr, Hc, b, Ha, and K1 of the dried composites through Eq. (3) showed the similar tendencies were smaller than the undried ones. This the that of Ms curves, as shown in Fig. 6. phenomenon could be attributed to the changes Overall, all the magnetic parameters such as in the density of composites after drying. Figure 6. Magnetocrystalline anisotropy constant, K1, curves as a function of La-doping concentration for undried (solid-symbol curve) and dried (opened-symbol curve) composites of Ba1-xLaxFe12O19/polyaniline. 4. Conclusion presence of impurity phase of α-Fe2O3. The The undried and dried composites of phase percentage of α-Fe2O3 increased with Ba1-xLaxFe12O19/polyaniline were successfully respect to the increase of La doping prepared. The structural properties of dried concentration. Magnetic properties of composites studied by XRD which showed the Ba1-xLaxFe12O19/polyaniline composites were
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