NGHIÊN CỨU CÁC ĐẶC TÍNH CẤU TRÚC CỦA VẬT LIỆU LAI

Bi2O3@NaBi(MoO4)2 TỔNG HỢP BẰNG PHƯƠNG PHÁP THỦY

NHIỆT

1. Phương pháp tổng hợp vật liệu

Synthesis of Bi2O3@NaBi(MoO4)2 hybrid composites (HCs) : A mixture A consisted of 0.15 g of

poly-(2-ethyl-2-oxazoline) (PEtOx, MW = 50,000) and 0.70 g of polyvinylpyrrolidone (PVP, M W

= 360,000) in 30 ml of triethylene glycol (TEG) was stirred at 90 oC under Ar gas in a three-neck

round-bottom flask until becoming a homogenous solution. At the same time, the compounds of

4 mmol of Na2MoO4.2H2O in 30 ml TEG adding 10 ml of 2 M NaOH, and 54 mmol NaBH 4 in

40 ml TEG were prepared in two separately beakers named B and C, respectively. The solution

B was added quickly into A once they all obtained the homogenous state. After the mixture was

uniform completely, the solution C was dropped slowly to it using a glass pressure-equalizing

funnel. A large amount of gas will be generated during this chemical reaction, which was kept

for 2 h since the finished drop process and cooled down to room temperature (RT)

spontaneously. A white precipitate of bipyramid Na2MoO4 was collected by centrifugation at

9,000 rpm for 10 min and washed with ethanol alternatively several times. The products were

gathered and dispersed again in 70 ml of TEG by ultrasound (solution D), which later was heated

to 180 oC in a three-neck round-bottom flask under constant magnetic stirring and Ar gas.

Meanwhile, a ready mixture called E of 4 mmol of Bi(NO3)3.5H2O in 30 mL TEG was

homogeneously prepared. We added E drop by drop using a glass pressure-equalizing funnel to

the solution D, while the temperature was maintained as a constant at 180 °C during reaction for

different reaction times (1 h and 3 h). The examined samples of Bi 2O3@NaBi(MoO4)2 HCs were

cooling to RT before collected by centrifugation for 10 min at 9,000 rpm, and washing with a
mixture of deionized water and ethanol (1:1 in volume) thrice. Next, the powder substances were

collected and dried at 70 °C in a vacuum oven for 4 h, followed by annealing for 12 h under Ar

gas at 200 °C. These powders, named as Bi2O3@NaBi(MoO4)2-1h and Bi2O3@NaBi(MoO4)2-3h,

were used for materials characterization and electrochemical measurements.

(Kèm theo sơ đồ khối mô tả các bước thí nghiệm)

2. Phương pháp xác định các đặc tính cấu trúc vật liệu

Materials characterization: The crystalline phase and component of the powder samples were

determined by powder X-ray diffraction (XRD, Bruker-AXS-D8). The electron diffraction was

investigated by transmission electron microscopy (TEM, Talos-F200X).

3. Kết quả và bàn luận

- Giải thích về cách hình thành vật liệu, viết phương trình phản ứng liên quan.

- Vẽ phổ XRD và thảo luận về các peak trong phổ XRD (kèm chỉ số hkl, và ký hiệu của

từng chất chuẩn).

- Xác định các vòng nhiễu xạ trong phổ electron diffraction tương ứng với kích thước d

của mặt (hkl) nào.

- Dựa vào phổ XRD: đánh giá sơ về khả năng tồn tại dạng amorphous hay crystalline hay

là hỗn hợp của cả amorphous và crystalline; tính d ứng với các peaks, tính kích thước hạt;

tính lattice strain; tính hằng số mạng a,b,c của Bi2O3 và NaBi(MoO4)2 .

- Tham khảo các bài báo liên quan để biết cách giải thích các peaks trong phổ XRD.