Fe2O3对原位制备SiCw/SiC太阳能储热陶瓷的结构与性能的影响

doi:10.15541/jim20180580

摘要/Abstract

摘要：

为调控SiC_w/SiC复相陶瓷中原位生长SiC晶须的生长发育和形貌, 以提高SiC复相储热陶瓷的性能, 在CF0配方(SiC 69.31wt%, AlN 20.30wt%, Si 10.39wt%)的基础上添加0.5wt%~2.0wt% Fe₂O₃作为催化剂。研究了Fe₂O₃对晶须形貌、生长机制及SiC复相陶瓷结构与性能的影响。研究结果表明, 引入Fe₂O₃后晶须生长机制由气-固机理转变为气-液-固机理。Fe₂O₃添加量通过调节C元素在Fe-Si熔球中的溶解度, 与烧成温度共同调控晶须形貌。经1500 ℃烧成的CF4(2.0wt% Fe₂O₃)样品性能最佳, 晶须直径50~100 nm, 长度1~6 μm, 其体积密度、抗折强度、比热容分别为2.19 g/cm ³、45.08 MPa、0.95 J/(g·K) (25 ℃), 热导率达18.15 W/(m·K) (25 ℃), 相比于未添加Fe₂O₃的样品增加了169%。气-液-固机理生长的SiC晶须缺陷少、直径大, 可有效降低晶须-基体传输势垒, 具有更好的热学性能。

关键词: Fe₂O₃, SiC晶须, SiC_w/SiC复相陶瓷, 太阳能储热

Abstract:

In order to improve solar thermal storage properties of the SiC_w/SiC composite ceramics, in-situ growth and morphology of SiC whiskers (SiC_w) were controlled by adding catalyst Fe₂O₃(0.5wt%-2.0wt%) on the basis of formula CF0 (SiC 69.21wt%, AlN 20.30wt%, Si 10.39wt%). Effect of Fe₂O₃ on morphology of SiC_w as well as growth mechanism and properties of SiC composite ceramics were analyzed. Results indicated that SiC_w growth mechanism changed from vapor-solid to vapor-liquid-solid after adding Fe₂O_3. The addition of Fe₂O₃via adjusting solubility of C element into Fe-Si droplets, as well as firing temperature jointly controlled morphology of SiC_w. The sample CF4 (Fe₂O₃ 2.0wt%) fired at 1500 ℃ with whiskers diameter of 50-100 nm and 1-6 μm in length obtained optimal performance, the bulk density, bending strength, heat capacity and thermal conductivity were 2.19 g/cm ³, 45.08 MPa, 0.95 J/(g·K) (25 ℃), 18.15 W/(m·K) (25 ℃), respectively. The value of thermal conductivity increased by 169% compared to the sample without Fe₂O₃. The few defects and large-diameter of whisker grown by vapor-liquid-solid mechanism could improve thermal properties by reducing the matrix-whisker thermal barrier.

Key words: Fe₂O₃, SiC whiskers, SiC_w/SiC composite ceramics, solar thermal energy storage

中图分类号:

TQ174

徐晓虹, 田江洲, 吴建锋, 张乾坤, 金昊, 杜怿鑫. Fe₂O₃对原位制备SiC_w/SiC太阳能储热陶瓷的结构与性能的影响[J]. 无机材料学报, 2019, 34(10): 1103-1108.

XU Xiao-Hong, TIAN Jiang-Zhou, WU Jian-Feng, ZHANG Qian-Kun, JIN Hao, DU Yi-Xin. Fe₂O₃ on In-situ Synthesized SiC_w/SiC Composite Ceramics for Solar Thermal Energy Storage[J]. Journal of Inorganic Materials, 2019, 34(10): 1103-1108.

图/表 9

图1 CF系列样品的物理性能与烧成温度的关系曲线图

Fig. 1 Relationships between physical properties and firing temperatures of the samples CF

图2 经1500 ℃烧成的CF系列样品的XRD图谱

Fig. 2 XRD patterns of the samples CF fired at 1500 ℃

图3 经不同温度烧成的CF4样品的XRD图谱

Fig. 3 XRD patterns of the sample CF4 fired at different temperatures

图4 经1550 ℃烧成的CF0样品的断面SEM照片

Fig. 4 SEM morphologies of fractured surface of the sample CF0 fired at 1550 ℃

图5 经1500 ℃烧成的CF系列样品的断面SEM照片

Fig. 5 SEM morphologies of fractured surface of the samples CF fired at 1550 ℃ (a) CF1; (b) CF2; (c) CF3; (d) CF4

图6 经不同烧成温度的CF4样品断面SEM照片

Fig. 6 SEM morphologies of fractured surface of the sample CF4 fired at different temperatures (a) 1475 ℃; (b) 1525 ℃; (c) 1550 ℃; (d) 1575 ℃

图7 经1500 ℃烧成的CF4样品的二次电子像与指定点能谱图

Fig. 7 Secondary electron image and EDS patterns of the sample CF4 fired at 1500 ℃

表1 指定点能谱分析结果

Table 1 EDS analysis results of selected spots

Spot	C/at%	O/at%	Al/at%	Si/at%	Fe/at%
1	44.54	7.12	2.54	44.74	1.06
2	50.40	9.29	1.51	38.43	0.37

表2 样品的热物理性能测试结果

Table 2 Experimental results of thermal physical properties of the samples

Sample No.	Testing temperature/℃	Thermal diffusivity/ (mm²·s^-1)	Heat capacity/ (J·g^-1·K^-1)	Thermal conductivity/ (W·m^-1·K^-1)
CF0	25	3.87	0.81	6.74
CF0	300	2.25	1.10	5.62
CF4	25	8.812	0.95	18.15
CF4	300	5.513	1.23	14.69

参考文献 27

[1]	PY X, CALVET N, OLIVES R et al. Recycled material for sensible heat based thermal energy storage to be used in concentrated solar thermal power plants.J. Sol. Energy Eng, 2011,133(8):31008-31017.
[2]	MULLER-STEINHAGEN H . Concentrating solar thermal power. Phil. Trans. R. Sci. A, 2013,371(1996):1-20.
[3]	KURAVI S, TRAHAN J, GOSWAMI D Y et al. Thermal energy storage technologies and systems for concentrating solar power plants.Prog. Energy Combust. Sci, 2013,39(4):285-319.
[4]	ROMERO M ,GONZÁLEZ-AGUILAR J. Solar thermal CSP technology. Energy Environ., 2014,3(1):42-59.
[5]	LAO X B, XU X H, WU J F et al. Effect of silicon on properties of Al₂O₃-SiC_w composite ceramics in-situ synthesized by aluminium- assisted carbothermal reduction of coal series kaolin for solar thermal storage. J. Alloys Compd., 2017,692:825-832.
[6]	XU X H, RAO Z G, WU J F et al. In-situ synthesis and thermal shock resistance of cordierite/silicon carbide composites used for solar absorber coating. Sol. Energy Mater. Sol. Cells, 2014,130:257-263.
[7]	KIM K J, KIM Y, LIM K et al. Electrical and thermal properties of SiC-AlN ceramics without sintering additives. J. Eur. Ceram. Soc., 2015,35(10):2715-2721.
[8]	ZHANG C, YAO X M, LI Y S et al. Effect of AlN addition on the thermal conductivity of pressureless sintered SiC ceramics. Ceram. Int., 2015,41(7):9107-9114.
[9]	KARAMIAN E, MONSHI A, BATAILLE A et al. Formation of nano SiC whiskers in bauxite-carbon composite materials and their consequences on strength and density. J. Eur. Ceram. Soc., 2011,31(14):2677-2685.
[10]	XU X H, LAO X B, WU J F et al. Synthesis and characterization of Al₂O₃/SiC composite ceramics via carbothermal reduction of aluminosilicate precursor for solar sensible thermal storage. J. Alloys Compd., 2016,662:126-137.
[11]	CHEN Y, WANG C G, GAO R R et al. Research of the preparation technology for the SiC whisker. J. Inorg. Mater., 2013,28(7):757-762.
[12]	MILEWSKI J V, GAC F D, PETROVIC J J et al. Growth of beta-silicon carbide whiskers by the VLS process, J. Mater. Sci., 1985,20(4):1160-1166.
[13]	陈肇友 . 化学热力学与耐火材料. 北京: 冶金工业出版社, 2005: 494-496.
[14]	HAO H S, XU L H, LIU M , et al. Synthesis of O'-SiAlON/SiC by using non-traditional resources: Yangtze river sand. Mater. Sci. Forum., 2009, 610- 613:267-273.
[15]	MA B Y, LI Y, XU L B et al. In-situ synthesis of(O′+β)-Sialon/mullite composite materials. J. Northeast Univ., 2011,32(1):102-105.
[16]	XU X W, LIANG H, LI X L et al. In situ synthesis and phase analysis of low density O'-sialon based multiphase ceramics. Rare Met., 2010,29(2):214-219.
[17]	LI Z, SHI T J, TAN D X . Long β-Silicon carbide necklace-like whiskers prepared by carbothermal reduction of wood flour/silica/phenolic composite. J. Am. Ceram. Soc., 2010,93(10):3499-3503.
[18]	LI X W, QU D L, LI Z J et al. Study on the thermodynamics and characterization of synthesizing SiC whiskers. J. Synth. Cryst., 2013,42(10):2160-2163.
[19]	CAO L Z, LIU X, ZHAO J Q et al. Synthesis and photoluminescence of the branching silicon carbide nanowires. Physica E, 2012,46(9):57-60.
[20]	LI X W, QU D L, LI Z J et al. Effect of catalysts on synthesis of silicon carbide whiskers with silica sol. Bull. Chin. Ceram. Soc., 2014,33(3):593-595.
[21]	CHEN Y Q, ZHANG K, MIAO B et al. Temperature dependence of morphology and diameter of silicon nanowires synthesized by laser ablation. Chem. Phys. Lett., 2002,358(5/6):396-400.
[22]	YANG G Y, WU R B, GAO M X et al. SiC crystal growth from transition metal silicide fluxes. Cryst. Res. Technol., 2007,42(5):445-450.
[23]	VAKIFAHMETOGLU C, PIPPEL E, WOLTERSDORF J et al. Growth of one-dimensional nanostructures in porous polymer-derived ceramics by catalyst-assisted pyrolysis. Part 1: Iron catalyst. J. Am. Ceram. Soc., 2010,93(4):959-968.
[24]	WANG F Q, YAN L S, HAO Z B et al. In-situ preparation of SiC whiskers on C/C-SiC composite surface by catalytic chemical vapor deposition. Mater. Mech. Eng., 2011,35(10):98-102.
[25]	BI J Y, GU Y Z, ZHANG Z C et al. Core-shell SiC/SiO₂ whisker reinforced polymer composite with high dielectric permittivity and low dielectric loss. Mater. Des., 2016,89:933-940.
[26]	奚同庚 . 无机材料热物性学.上海: 上海科学技术出版社, 1981: 92-121.
[27]	HASSELMAN D P H, DONALDSON K Y, THOMAS JR J R . Thermal conductivity of vapor-liquid-solid and vapor-solid silicon carbide whisker-reinforced lithium aluminosilicate glass-ceramic composites. J. Am. Ceram. Soc., 1996,79(3):742-748.

Fe₂O₃对原位制备SiC_w/SiC太阳能储热陶瓷的结构与性能的影响

Fe₂O₃ on In-situ Synthesized SiC_w/SiC Composite Ceramics for Solar Thermal Energy Storage

RichHTML

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

图/表 9

参考文献 27

相关文章 15

编辑推荐

Metrics

本文评价

[1]	张文进, 申倩倩, 薛晋波, 李琦, 刘旭光, 贾虎生. 具有高度有序氧空位的α-Fe₂O₃纳米带的制备及光电催化水氧化性能研究[J]. 无机材料学报, 2021, 36(12): 1290-1296.
[2]	陈旸, 王成国, 高冉冉, 朱波. SiC晶须制备工艺的研究[J]. 无机材料学报, 2013, 28(7): 757-762.
[3]	邓洪贵, 金双玲, 何星, 詹亮, 乔文明, 凌立成. 以Fe₂O₃为原料通过水热–高温煅烧法合成LiFePO₄/C纳米复合材料及其电化学性能研究[J]. 无机材料学报, 2012, 27(9): 997-1002.
[4]	宋军, 马振叶, 李成, 吴如军. 不同晶态纳米Fe₂O₃的盐控合成[J]. 无机材料学报, 2010, 25(7): 780-784.
[5]	黄祥卉,陈振华. γ-Fe₂O₃/SiO₂纳米复合粉体的制备[J]. 无机材料学报, 2005, 20(3): 685-691.
[6]	凌律巍,吴文彪,江东亮,谭寿洪,黄政仁. SiC晶须在Mullite浆料中的分散特性及流变学表征[J]. 无机材料学报, 2001, 16(6): 1084-1088.
[7]	古绪鹏,陈同云,吴鹏生. 有机膦复合添加剂应用在碱法制备α-FeOOH过程中[J]. 无机材料学报, 2001, 16(5): 961-964.
[8]	邱春喜,姜继森,赵振杰,杨燮龙. 固相法制备α-Fe₂O₃纳米粒子[J]. 无机材料学报, 2001, 16(5): 957-960.
[9]	牛新书,徐荭. 乙二醇甲醚体系中α-Fe₂O₃纳米晶制备与结构分析[J]. 无机材料学报, 2001, 16(2): 243-248.
[10]	李巧玲,魏雨,李琳. 纺锤形α-Fe₂O₃成核前水解机理的研究[J]. 无机材料学报, 2000, 15(6): 1093-1096.
[11]	贾振斌,魏雨,王洪敏. 纳米相铁红粒子的液相制备[J]. 无机材料学报, 2000, 15(5): 926-928.
[12]	叶枫,周玉,雷廷权,杨觉明,张立同. SiC_w/BAS复合材料的显微结构及力学性能的研究[J]. 无机材料学报, 2000, 15(3): 516-520.
[13]	莫茂松,敖自华,王弘,沈瑜生. 钛掺杂的α-Fe₂O₃-K₂O纳米湿敏陶瓷结构与性能研究[J]. 无机材料学报, 2000, 15(3): 521-526.
[14]	韩晓斌,黄丽,回峥. 微波水解法制备针形α-Fe₂O₃纳米粒子[J]. 无机材料学报, 1999, 14(4): 669-673.
[15]	许钫钫,温树林,大学NORDBERG L-O. 不同气氛下烧结的α-Sialon/SiC_(w)复合材料[J]. 无机材料学报, 1998, 13(3): 320-326.