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Part 5


一、介绍研究背景(background)﹑ 研究意义




一、介绍研究背景(background)﹑ 研究意义

Since the early 1960s, …has attracted much attention due to … In recent years, more and more attention has been paid


to …

…have recently evoked a lot of interest.


It is well known that …is be of great interest because …
Very recently, it was reported that …


二、阐述目前该领域的研究现状﹑存在问题﹑ 待解决的问题

Although … has been investigated extensively, very few literatures reported …
However, … have so far not been studied. Unfortunately, the current method suffers from certain limitations. though, whereas, on the other hand, but , while… Thus, there is a need to …

? ?

? ?


三、指出本文的研究内容﹑目的及其独到之处 常用句式:
? ?

In this paper, we present data on … Recently, we found that… In this paper … are discussed in detail. The present work was aimed at studying …



Herein we demonstrated that …


Part 6


The format of an experimental section should be
in accordance with the requirement of the journal you choose.


Generally, an experimental section mainly consists
three parts, that is:


Chemicals (Materials), Synthesis (preparation),
and Characterization


1.实验预备:描述实验中所需要的化学原材料、试 剂的来源、预处理和纯化; 2.实验过程:描述实验(合成)的操作步骤、方法、 条件、现象和注意事项等; 3.结果表征:描述通过什么样的仪器、测试方法或 技术手段来获得支持论文观点的有效数据(经常指


一、原材料的来源及准备(Chemicals or Materials) 1. 直接买到的药品一般需指明来源和纯度:

Amino acid (Bachem), 2-(2-aminoethyl)pyridine (Fluka) and 2hydroxypyridine (Acros) were used as received.





ZnEt2 (diethylzinc)was purchased from Aldrich and was used as received.
Amino acid 氨基酸 amine 胺 ammonia 氨 Ammonium 铵 pyridine 吡啶



一、原材料的来源及准备(Chemicals or Materials)

The starting materials were Li3PO4 (99%, Aldrich) and Fe3(PO4)· 2O (99%, Aldrich). 8H An appropriate amount of PVA (degree of polymerization 1500, Junsei) as the carbon source was added to the raw materials.
PVA is poly (vinyl alcohol) 聚乙烯醇


一、原材料的来源及准备(Chemicals or Materials)

All materials, such as potassium hexacyano-cobaltate (III) (K3Co(CN)6), zinc fluoride (ZnF2), zinc chloride (ZnCl2), zinc bromide (ZnBr2), zinc iodide (ZnI2) and tertiary butyl alcohol (tBuOH) were purchased from Aldrich and used without further purification.
fluorine-F2 chlorine —Cl2 bromine —Br2 iodine —I2


Polymerization grade of poly( tetramethylene ether glycol) (PTMEG, molecular weight =1800) was donated by BASF Korea Ltd.

一、原材料的来源及准备(Chemicals or Materials) 2. 直接购买的普通溶剂或辅助药品只需简单提及或略 过

All other materials were commercially available and used as received unless otherwise noted. All other chemicals were of analytical grade and were used as received.
化学实验中使用的药品按照纯度的不同常可以分为: industrial grade 工业级 ; analytical grade 分析级 ; spectral grade 光谱级


一、原材料的来源及准备 (Chemicals or Materials) 3. 需经纯化处理的药品一般需说明纯化方法

Bisphenol A was recrystallized from chlorobenzene. Dichloromethane was distilled prior to use and stored over molecular sieves. Molecular sieves were activated at 350oC for 10 h under N2 before use.
Chlorobenzene 氯苯;Dichloromethane 二氯甲烷;molecular sieves分子筛


Ethyl acetate was dried over K2CO3 and distilled. All solvents were freshly distilled before use.


二. 实验过程
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…was prepared by the method of … [10]. …was synthesized according to Ref. [4].


…were synthesized according to
published procedures [1].

二. 实验过程
具体的实验步骤、条件、反应等则需要详细说 明,通常有如下的小标题:

Preparation of …

c. d.

… Synthesis
Synthesis procedure Reaction of …


Synthesis of Cyclic Carbonate Monomer <小标题>
Triethylamine (84.0 g, 0.825 mol) was added dropwise

to a solution of 1,3-propanediol (29.9 g, 0.393 mol) and
ethyl chloroformate (85.4 g, 0.786 mol) in 2L of THF at 0 oC over a period of 30 min. The reaction mixture was stirred for 2h at room temperature. Precipitated triethylamine hydrochloride salt was filtered off, and the

filtrate was concentrated under vacuum. The residue
was recrystallized three times from THF-ether.
ethyl chloroformate 氯甲酸乙酯 formic acid 甲酸,蚁酸


Synthesis of trimethylene carbonate <小标题>





following a procedure described elsewhere.25 The product was recrystallized twice from

diethyl ether. White crystal was obtained in
55% yield: (mp 45°C). The 1H-NMR spectrum (4H, 4.50 ppm; 2H, 2.21 ppm) was consistent with that reported previously.25


Preparation of catalysts
A solution of ZnCl2 (220 mmol) in deionized water(115 mL) and tBuOH (21 g) is taken in the first beaker (solution 1). A solution of K3Co(CN)6 (3.15 g, 9.5 mmol) in deionized water (42 mL) is taken in the second beaker (solution 2). The third beaker contains a mixture of deionized water (1 mL), tBuOH (20 mL) and PTMEG (3.5 g) (solution 3). Solution 2 is added to solution 1 dropwise for a period of over 60 min at 50 oC with continuous stirring using a mechanical stirrer. Solution 3 is then added and the mixture is stirred for an additional 3 min. The mixture is then centrifuged(离心). The resulting catalyst (DMC-Cl) cake is dried at 60 oC under vacuum (30 inHg) to a constant weight. The catalysts using ZnF2 (DMC-F), ZnBr2 (DMC-Br) and ZnI2 (DMC-I) were prepared by similar procedures.


Synthesis of chelating resins

1.0g of PS-Cl, 1.628g of Bismuththiol I (BMT), 4.0g K2CO3 powder, and 20ml of acetone was placed in a one-neck flask. With magnetic stirring, the mixture was refluxed for 8h. The solvent acetone was distilled, and then 100ml of distilled water were added to dissolve the salts. The polymeric product was filtered and washed with distilled water, 2% solution of KOH, 1% hydrochloric acid, and finally with distilled water. The product was transferred to a Soxhlet’s extraction apparatus for reflux-extraction in 95% ethanol for 10h and then was dried under vacuum at 50℃ over 48h. Elemental analysis (%): Cl, 4.84; S, 19.51; N, 5.80. FTIR: νC=N 1381cm-1.


Preparation of Bi2Te3 Nanotubes
A mixture of 7.5 mmol tellurium powders (5 N, ?30 μm) or Na2TeO3, and 5 mmol BiCl3 were put into a 250 ml glass beaker containing 200 ml distilled water. For some samples, an organic surfactant of 0.5 g sodium dodecyl-benzenesulfonate (SDBS) was charged in the solution. Then about 2 g NaOH were added to adjust the pH value to about 13. Subsequently, 1 g NaBH4 was used as the reductant. The solution was heated to 65 oC for 48 h and stirred by a magnetic stirrer. The beaker was covered with a polyethylene film to reduce the evaporation of water during the synthesis. The resulting solid products were filtered and washed several times with distilled water and acetone, and then dried at room temperature in vacuum.

Nuclear Magnetic Resonance (NMR) Spectroscopy
? 1H-NMR

spectra were recorded on a Bruker ARX250 spectrometer at 250 MHz.
MHz megahertz 兆赫

? 1H

and 13C NMR spectra were obtained on a JEOL LA600 spectrometer using CDCl3 (containing 1% TMS as an internal reference) solvent.
CDCl3 Deuterium substituted chloroform 氘代氯仿 TMS 标准物质 四甲基硅烷 Tetramethylsilane

Infrared Spectroscopy

IR spectrometric analysis was carried out using Perkin–Elmer Paragon-1000 IR spectrometer. IR spectra (Nicolet Nexus 670 FT-IR, KBr) were used for detecting the formation of coordination bond. coordination bond 配位键 Fourier Transform-Infrared Spectroscopy (FTIR) APE 1720 FTIR spectrometer was used to obtain the spectra (16 scans, resolution 2 cm-1) of the monomer and polymers over the range from 4000 to 400 cm-1. cm-1 Wave number



Differential Scanning Calorimetry (DSC)
Differential Scanning Calorimetry (DSC) was carried out with a Perkin-Elmer DSC 7 thermal analyzer. All the samples were heated at 20 °C/min heating rate from 25 °C to 200 °C for the first scan, then cooled at 50-100 °C/min to 25 °C, and immediately heated a second time. Peak melting temperatures (Tm) and melting enthalpy ( Hm) were measured on the first scan, and glass transition temperatures (Tg) were measured on the second scan.
melting enthalpy 熔融热焓; glass transition temperatures 玻璃化转变温度

Thermal Gravimetry (TG)

In this method, differential scanning calorimetry (DSC) and thermal gravimetry(热重分析) (TG) are applied simultaneously to the sample, allowing a simultaneous measurement of changes in enthalpy and weight. The thermal scans were performed with a heating rate of 10 K/min up to a temperature of 400 oC in an argon stream.

Scanning Electron Microscopy (SEM)

Samples were then covered by an ultrathin(超薄的) layer of gold and observed with a scanning electron microscope (JSM 6400). SEM (HITACHI S-4300) was used to observe the particle morphology. Examination of the morphology of the powder was conducted(操作) by scanning electron microscopy (Hitachi S-4200) with an accelerating voltage of 3 kV.



X-ray diffraction analysis

X-ray diffraction ( 衍 射 ) (XRD) patterns of the samples were measured with a Siemens D5000 diffractometer (Cu Ka radiation). Structural parameters were determined by Rietveld analysis of diffraction patterns, using the Bruker AXS program Win-Rietveld.
Structural parameters 结构参数


The crystallographic structure of the powder was analyzed by X-ray diffraction (XRD) (Rint/Dmax-2500, Rigaku) with Cu Ka radiation.
Crystallographic structure 晶体学参数

Gel Permeation Chromatography (GPC)

Molecular weight data was obtained by gel permeation chromatography (GPC), using two PL gel columns connected to a Water 410 RI detector (Waters Corp, MA). Molecular weights and the distributions were estimated by gel permeation chromatography (GPC).
GPC gel permeation chromatography 凝胶渗透色谱


Chemical Analysis

The chemical composition(组成) of the samples (Li, Fe, and P) was determined by atomic absorption spectrometry (spectra AA 800 series, Varian) and inductively coupled plasma (ICP, Thermal Jarrell ASH).
inductively coupled plasma 感应耦合等离子体技术


The residue coating carbon content among the LiFePO4/C composites was determined on the element analysis apparatus (设备)of Vario-EL (Germany).

Mass spectrum( MS)

Matrix assisted laser desorption ionization—

time of flight (MALDI-TOF) mass analysis was
carried out on Shimadzu Kompact MALDI III spectrometer using 2,5-dihydroxy benzoic acid as matrix and THF as solvent.
Matr$L酞尩E$L酞尩遝r desorption ionization 激光解离离子化; time of flight 飞行时间;

Other technologies

XPS: X-ray photoelectron spectroscopy analysis TEM: Transmission electron microscopy

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UV-Vis: Ultraviolet-visible Spectroscopy ……


实验中需要通过一定的技术手段和预先设计 的方法来测定目标样品的物理、化学和机械 性能等, 以便于研究者了解样品的性能,从而 有可能设计成实用的产品。

Cell or battery test

The assembly of the cell was carried out in an environmentally controlled dry box. The cathode performance was investigated in terms of cyclic

voltammetry (CV 循环伏安), charge-discharge
curves, and cycle life. The CV tests were run by standard electrochemical equipment and the cycling tests by a Maccor Battery Cycler instrument.



Cycle life

Ionic conductance and capacitance measurements
Ionic conductance was measured with an electrometer setup at room temperature [25]. The electrochemical performance of the conductive hydrogel ( 水 凝 胶 ) was evaluated by cyclic voltammetry at room temperature. An Autolab Pgstat30 potentiostat/galvanostat ( 恒 压 恒 流 ) was used for electrochemical measurements.

Conductivity measurements
Conductivity measurements were made on discshaped samples by two-point and four-point d.c. methods. For two-point measurements, gold electrodes were sputtered (喷溅) on opposing(相对 的) faces of discs of ~8 mm diameter and ~1 mm thickness. Four-point conductivity measurements were made by the van der Pauw method on discs of ~8 mm diameter lapped(重叠、拍打) to ~300 μm thickness. Gold electrodes were sputtered at the perimeter (周长、 周界) of the masked discs, and a Bio-Rad HL5500PC instrument (Hercules, California, USA) was used.
μm micron 微米 d.c. method直流方式

Thermal conductivity 热导率

The thermal conductivity of the composites was measured by means of a hot plate steadystate ( 稳 态 的 ) heat flow type of thermal conductivity instrument (model NF-7) supplied by South China University of Technology as shown in Fig. 1.

Fig. 1. NF-7 thermal conductivity instrument.


Two thermocouples (热电偶)were set on the two cold faces of the test pieces, and two thermocouples were set on the two heated face of the test pieces. The temperatures and heating power were measured as soon as the heat transfer reached the steady state. All measured data were collected and recorded by a computer.

Water uptake(吸收) measurements

The swelling capability (溶胀)of hydrogels was investigated by measuring their water uptake (WU) and using Eq. (1), where Ws and Wd are the

weight of the swollen hydrogel at equilibrium(平
衡) and the weight of dry hydrogel (水凝胶), respectively.


Mechanical properties testing

The mechanical properties (机械性能)testing were performed at a relative humidity(湿度) of 50% using ISO 527 specimens (Fig. 1). The tensile tests (拉伸测试)were carried out in a 10 kN Instron machine equipped with a temperature controlled chamber(室式温控).
Instron machine 英斯特朗拉伸试验装置



The Shore A hardness test was carried out according to ISO7619 using a Zwick 7206 Hardness Tester. Sheets (薄片)of 6 mm thickness were used for hardness measurement.


Impact strength

The Izod impact test was performed using a 2 J hammer on a Universal Digital Pendulum (摆锤) Model CEAST machine in accordance to ASTM D 256-97. Specimens were soaked(浸湿) in liquid nitrogen for 1 min prior to impact testing. Izod impact test 悬臂梁式冲击试验

ASTM =American Society for Testing and Materials 系美国材料与试验协会的英文缩写。

Geometry 几何形状

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