KH-560改性SiO2绝缘薄膜的制备及性能研究

doi:10.15541/jim20210085

摘要/Abstract

摘要：

软磁合金是新一代质子/重离子同步加速器加速器的核心材料,在其表面涂覆绝缘涂层可有效降低高频涡流损耗。同时,高温热处理(~600 ℃)可有效减少软磁合金冷压成形产生的缺陷和位错而引起的内部残余应力。因此,软磁合金用绝缘涂层还需满足耐高温要求。SiO₂涂层是最常见的无机涂层材料,具有良好的绝缘性能和耐高温性能。本工作在植酸催化TEOS+MTES制备硅溶胶的基础上,加入硅烷偶联剂KH-560进一步提高硅溶胶的成膜性能,系统研究了KH-560对SiO₂涂层结构与性能的影响,并系统分析了KH-560提高SiO₂涂层性能的机理。研究表明,添加适量的KH-560可有效提高薄膜的稳定性和成膜性。特别是当KH-560添加量为0.04 mol时,SiO₂涂层质量最好,SiO₂-0.04 KH涂层表现出最佳的耐腐蚀性和电绝缘性。在100 V时,SiO₂-0.04 KH涂层的方块电阻仍保持2.95×10¹¹Ω/□。综上,本研究利用植酸催化和KH-560改性协同作用制备出高质量的SiO₂涂层,涂层具有良好的耐高温和优异的绝缘性能。

关键词: 软磁合金, SiO₂涂层, 方块电阻, 溶胶-凝胶法

Abstract:

Soft magnetic alloy is the core material of the proton/heavy ion accelerator. To reduce the eddy current loss at high frequencies, the insulating coating needs to be coated on the surface of soft magnetic alloy, and to be followed-up heat treatment (~600 ℃) to lower the residual stress from defects and dislocations produced in the cold forming process of soft magnetic alloys. Therefore, the insulation coating for soft magnetic alloy should meet the requirement of high-temperature resistance. SiO₂ is one of the most common inorganic coating materials, which has good insulation performance and temperature resistance, so it is especially suitable for high-temperature insulation coating. In this work, fabrication process of SiO₂ insulating coating was systematically studied. The silane coupling agent 3-glycidyloxypropyltrimethoxysilane (KH-560) was added to the phytic acid-catalyzed tetraethyl orthosilicate (TEOS) and methyltriethoxysilane (MTES) sol to improve the film-forming property. Effect of KH-560 on structure and property of SiO₂ coating was analyzed in detail. The results showed that the stability and the film-forming property were improved effectively via adding a reasonable amount of KH-560. When adding amount of KH-560 is 0.04 mol, the as-preared SiO₂ coating exhibites excellent film-forming characteristics, corrosion resistance and electrical insulation with sheet resistance of 2.97×10¹¹ Ω/□ at 100 V.

Key words: soft magnetic alloy, SiO₂ coating, sheet resistance, Sol-Gel method

中图分类号:

TQ174

杨丛纲, 米乐, 冯爱虎, 于洋, 孙大志, 于云. KH-560改性SiO₂绝缘薄膜的制备及性能研究[J]. 无机材料学报, 2021, 36(12): 1343-1348.

YANG Conggang, MI Le, FENG Aihu, YU Yang, SUN Dazhi, YU Yun. Synthesis and Performance of KH-560 Modified SiO₂ Insulation Coating[J]. Journal of Inorganic Materials, 2021, 36(12): 1343-1348.

图/表 6

参考文献 18

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Sample	E_corr/V (vs. SEC)	I_corr/(A·cm^-2)	R_p/(Ω·cm²)	PE/%
Raw soft magnetic alloy	-0.973	4.0982×10^-5	552.31	-
SiO₂-0.01 KH	-0.182	7.398×10^-6	8559.9	81.95
SiO₂-0.02 KH	-0.150	3.4603×10^-7	6519.6	99.16
SiO₂-0.03 KH	-0.065	3.1833×10^-7	22077	99.22
SiO₂-0.04 KH	-0.007	2.9071×10^-7	76910	99.29

Sample	E_corr/V (vs. SEC)	I_corr/(A·cm^-2)	R_p/(Ω·cm²)	PE/%
Raw soft magnetic alloy	-0.973	4.0982×10^-5	552.31	-
SiO₂-0.01 KH	-0.182	7.398×10^-6	8559.9	81.95
SiO₂-0.02 KH	-0.150	3.4603×10^-7	6519.6	99.16
SiO₂-0.03 KH	-0.065	3.1833×10^-7	22077	99.22
SiO₂-0.04 KH	-0.007	2.9071×10^-7	76910	99.29

Sample		Sheet resistance at 10 V/(Ω/□)	Sheet resistance at 50 V/(Ω/□)	Sheet resistance at 100 V/(Ω/□)
SiO₂-0.01 KH	1	2.33×10⁹	3.66×10⁸	2.92×10⁸
	2	8.68×10⁸	4.58×10⁸	7.56×10⁸
	3	1.59×10⁹	5.85×10⁸	2.61×10⁸
	Average	1.60×10⁹	4.70×10⁸	4.36×10⁸
SiO₂-0.02 KH	1	1.82×10¹⁰	4.92×10¹⁰	8.88×10⁹
	2	4.55×10¹⁰	3.70×10¹⁰	4.40×10⁹
	3	2.19×10¹⁰	2.71×10¹¹	1.71×10¹¹
	Average	2.85×10¹⁰	1.19×10¹¹	6.14×10¹⁰
SiO₂-0.03 KH	1	8.71×10¹⁰	1.25×10⁹	2.21×10⁹
	2	4.17×10¹⁰	6.55×10¹⁰	6.52×10⁹
	3	5.68×10¹⁰	8.58×10⁹	6.02×10⁹
	Average	6.19×10¹⁰	2.51×10¹⁰	4.92×10⁹
SiO₂-0.04 KH	1	8.62×10¹⁰	2.81×10¹¹	4.51×10¹⁰
	2	3.33×10¹¹	4.52×10¹⁰	2.76×10¹¹
	3	1.91×10¹¹	1.56×10¹⁰	5.70×10¹¹
	Average	2.03×10¹¹	1.14×10¹¹	2.97×10¹¹

Sample		Sheet resistance at 10 V/(Ω/□)	Sheet resistance at 50 V/(Ω/□)	Sheet resistance at 100 V/(Ω/□)
SiO₂-0.01 KH	1	2.33×10⁹	3.66×10⁸	2.92×10⁸
	2	8.68×10⁸	4.58×10⁸	7.56×10⁸
	3	1.59×10⁹	5.85×10⁸	2.61×10⁸
	Average	1.60×10⁹	4.70×10⁸	4.36×10⁸
SiO₂-0.02 KH	1	1.82×10¹⁰	4.92×10¹⁰	8.88×10⁹
	2	4.55×10¹⁰	3.70×10¹⁰	4.40×10⁹
	3	2.19×10¹⁰	2.71×10¹¹	1.71×10¹¹
	Average	2.85×10¹⁰	1.19×10¹¹	6.14×10¹⁰
SiO₂-0.03 KH	1	8.71×10¹⁰	1.25×10⁹	2.21×10⁹
	2	4.17×10¹⁰	6.55×10¹⁰	6.52×10⁹
	3	5.68×10¹⁰	8.58×10⁹	6.02×10⁹
	Average	6.19×10¹⁰	2.51×10¹⁰	4.92×10⁹
SiO₂-0.04 KH	1	8.62×10¹⁰	2.81×10¹¹	4.51×10¹⁰
	2	3.33×10¹¹	4.52×10¹⁰	2.76×10¹¹
	3	1.91×10¹¹	1.56×10¹⁰	5.70×10¹¹
	Average	2.03×10¹¹	1.14×10¹¹	2.97×10¹¹

KH-560改性SiO₂绝缘薄膜的制备及性能研究

Synthesis and Performance of KH-560 Modified SiO₂ Insulation Coating

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