CN106752938B - 陶瓷表面密封用耐600℃高温涂层材料的制备方法 - Google Patents

陶瓷表面密封用耐600℃高温涂层材料的制备方法 Download PDF

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CN106752938B
CN106752938B CN201611123336.2A CN201611123336A CN106752938B CN 106752938 B CN106752938 B CN 106752938B CN 201611123336 A CN201611123336 A CN 201611123336A CN 106752938 B CN106752938 B CN 106752938B
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polyferrocarbosilane
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李博弘
田园
王超
曹先启
陈泽明
贾晓莹
王勃
梁西良
王文博
刘文仓
关悦瑜
王旭
张广艳
刘士琦
徐鑫
李胜
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Institute of Petrochemistry of Heilongjiang Academy of Sciences
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Abstract

陶瓷表面密封用耐600℃高温涂层材料的制备方法，它涉及一种高温涂层材料的制备方法。本发明是为了解决现有陶瓷材料由于多孔结构造成的低温易吸潮、高温热量会沿多孔结构向内部传递的问题。本方法如下：一、制备聚铁碳硅烷；二、制备乙烯基聚铁碳硅烷；三、将乙烯基聚铁碳硅烷、氮化硼、碳化硅、氮化硅和碳化硼共混，得到陶瓷表面密封用耐600℃高温涂层材料。本发明的陶瓷表面密封用耐600℃高温涂层材料其粘度为700～12000mPa·s。应用于粘接陶瓷材料剪切强度常温可达2.9MPa，200℃剪切强度常温可达2.9MPa，400℃剪切强度常温可达2.8MPa，600℃剪切强度常温可达2.5MPa，800℃剪切强度常温可达2.3MPa。本发明属于高温涂层材料的制备领域。

Description

陶瓷表面密封用耐600℃高温涂层材料的制备方法
技术领域
本发明涉及一种高温涂层材料的制备方法。
背景技术
随着航空、航天技术的发展，人们对飞行器的飞行速度提出越来越高的要求，气动加热所产生的温度越来越高，对材料的耐热性能也提出了越来越高的要求。天线罩是保证雷达系统正常工作的一种设施，目前石英陶瓷天线罩、石英纤维增强石英天线罩、高硅氧增强磷酸盐天线罩等具有使用温度高、高温透波性能好、强度高等特点的陶瓷天线罩已在国内外广泛应用。陶瓷材料为多孔结构，不仅易吸潮，而且气动加热所产生的热量会沿着材料的多孔结构迅速向内传递，造成内部电子元器件损伤而影响飞行器的精度及其他性能。因而限制了陶瓷材料在高飞行速度、高精度飞行器领域的应用范围。
发明内容
本发明的目的是为了解决现有陶瓷材料由于多孔结构造成的低温易吸潮、高温热量会沿多孔结构向内部传递的问题，提供了一种陶瓷表面密封用耐600℃高温涂层材料的制备方法。
陶瓷表面密封用耐600℃高温涂层材料的制备方法按照以下步骤进行：
一、以聚二甲基硅烷和二茂铁为原料，在250～500℃、3～18MPa、惰性气体保护下反应0.5～12h，提纯后得到粘度为800～10000mPa·s、数均分子量为400～800、分散度小于3的聚铁碳硅烷，其中二茂铁加入量为聚二甲基硅烷和二茂铁总质量的0.5％～10％；
二、将聚铁碳硅烷、四甲基四乙烯基环四硅氮烷溶于二甲苯/四氢呋喃混合溶剂中，以偶氮二异丁腈为催化剂，在温度为80～90℃的条件下反应2～8h，提纯后得到粘度为800～10000mPa·s、数均分子量为500～1600、分散度小于3的乙烯基聚铁碳硅烷；
其中聚铁碳硅烷与四甲基四乙烯基环四硅氮烷的摩尔比为1:0.05～2.5，聚铁碳硅烷与二甲苯/四氢呋喃混合溶剂的质量比为1:2～8，聚铁碳硅烷与偶氮二异丁腈的摩尔比为1:0.5～2；
三、将乙烯基聚铁碳硅烷、氮化硼、碳化硅、氮化硅和碳化硼按照1:(0～4):(0～4):(0～4):(0～4)的质量比共混，得到陶瓷表面密封用耐600℃高温涂层材料。
步骤二中所述二甲苯/四氢呋喃混合溶剂中二甲苯与四氢呋喃的体积比为1:0.8。
聚碳硅烷是一种耐高温复合材料的基体树脂，二茂铁改性聚碳硅烷提高了聚碳硅烷的耐热性，同时铁是二氧化硅的抗氧剂，可以对天线罩进行保护。聚铁碳硅烷室温为固体，难以作为陶瓷表面密封用涂层材料。将四甲基四乙烯基环四硅氮烷与聚铁碳硅烷中分子链中Si-H键反应，得到乙烯基聚铁碳硅烷，再与氮化硼、碳化硅、氮化硅、碳化硼混合，制得耐高温用于陶瓷表面密封的耐600℃高温涂层材料，其粘度为700～12000mPa·s。本发明的陶瓷表面密封用耐600℃高温涂层材料应用于粘接陶瓷材料剪切强度常温可达2.9MPa，200℃剪切强度常温可达2.9MPa，400℃剪切强度常温可达2.8MPa，600℃剪切强度常温可达2.5MPa，800℃剪切强度常温可达2.3MPa。
附图说明
图1是实验一中制备的陶瓷表面密封用耐600℃高温涂层材料的红外谱图；
图2是实验一中制备的陶瓷表面密封用耐600℃高温涂层材料180℃固化3h后TG谱图。
具体实施方式
本发明技术方案不局限于以下所列举具体实施方式，还包括各具体实施方式间的任意组合。
具体实施方式一：本实施方式陶瓷表面密封用耐600℃高温涂层材料的制备方法按照以下步骤进行：
一、以聚二甲基硅烷和二茂铁为原料，在250～500℃、3～18MPa、惰性气体保护下反应0.5～12h，提纯后得到粘度为800～10000mPa·s、数均分子量为400～800、分散度小于3的聚铁碳硅烷，其中二茂铁加入量为聚二甲基硅烷和二茂铁总质量的0.5％～10％；
二、将聚铁碳硅烷、四甲基四乙烯基环四硅氮烷溶于二甲苯/四氢呋喃混合溶剂中，以偶氮二异丁腈为催化剂，在温度为80～90℃的条件下反应2～8h，提纯后得到粘度为800～10000mPa·s、数均分子量为500～1600、分散度小于3的乙烯基聚铁碳硅烷；
其中聚铁碳硅烷与四甲基四乙烯基环四硅氮烷的摩尔比为1:0.05～2.5，聚铁碳硅烷与二甲苯/四氢呋喃混合溶剂的质量比为1:2～8，聚铁碳硅烷与偶氮二异丁腈的摩尔比为1:0.5～2；
三、将乙烯基聚铁碳硅烷、氮化硼、碳化硅、氮化硅和碳化硼按照1:(0～4):(0～4):(0～4):(0～4)的质量比共混，得到陶瓷表面密封用耐600℃高温涂层材料。
具体实施方式二：本实施方式与具体实施方式一不同的是步骤二中所述二甲苯/四氢呋喃混合溶剂中二甲苯与四氢呋喃的体积比为1:0.5～1.3。其它与具体实施方式一相同。
具体实施方式三：本实施方式与具体实施方式一或二之一不同的步骤一中在280～480℃、4～16MPa、惰性气体保护下反应1～10h。其它与具体实施方式一或二之一相同。
具体实施方式四：本实施方式与具体实施方式一至三之一不同的是步骤一中在300℃、10MPa、惰性气体保护下反应2h。其它与具体实施方式一至三之一相同。
具体实施方式五：本实施方式与具体实施方式一至四之一不同的是步骤一中二茂铁加入量为聚二甲基硅烷和二茂铁总质量的1％。其它与具体实施方式一至四之一相同。
具体实施方式六：本实施方式与具体实施方式一至五之一不同的是步骤二中在温度为88℃的条件下反应5h。其它与具体实施方式一至五之一相同。
具体实施方式七：本实施方式与具体实施方式一至六之一不同的是步骤二中聚铁碳硅烷与四甲基四乙烯基环四硅氮烷的摩尔比为1:0.5，聚铁碳硅烷与二甲苯/四氢呋喃混合溶剂的质量比为1:6，聚铁碳硅烷与偶氮二异丁腈的摩尔比为1:1。其它与具体实施方式一至六之一相同。
具体实施方式八：本实施方式与具体实施方式一至七之一不同的是步骤二中聚铁碳硅烷与四甲基四乙烯基环四硅氮烷的摩尔比为1:1。其它与具体实施方式一至七之一相同。
具体实施方式九：本实施方式与具体实施方式一至八之一不同的是步骤二中聚铁碳硅烷与二甲苯/四氢呋喃混合溶剂的质量比为1:6。其它与具体实施方式一至八之一相同。
具体实施方式十：本实施方式与具体实施方式一至九之一不同的是步骤三中将乙烯基聚铁碳硅烷、氮化硼、碳化硅、氮化硅和碳化硼按照1:4:3:2:1的质量比共混。其它与具体实施方式一至九之一相同。
采用下述实验验证本发明效果：
实验一：
陶瓷表面密封用耐600℃高温涂层材料的制备方法按照以下步骤进行：
一、以聚二甲基硅烷和二茂铁为原料，在400℃、10MPa、惰性气体保护下反应10h，提纯后得到粘度为8000mPa·s、数均分子量为860、分散度小于3的聚铁碳硅烷，其中二茂铁的添加量为9％；
二、将聚铁碳硅烷、四甲基四乙烯基环四硅氮烷溶于二甲苯/四氢呋喃混合溶剂中，以偶氮二异丁腈为催化剂，在温度为85℃的条件下反应6h，提纯后得到粘度为3900mPa·s、分子量为1240、分散度小于3的乙烯基聚铁碳硅烷；
其中低分子聚铁碳硅烷与四甲基四乙烯基环四硅氮烷的摩尔比为1:1.5，聚铁碳硅烷与二甲苯/四氢呋喃混合溶剂的质量比为1:5，低分子聚铁碳硅烷与偶氮二异丁腈的摩尔比为1:1.5；
三、将乙烯基聚铁碳硅烷、氮化硼、碳化硅、氮化硅和碳化硼按照1:2:1:2:3的质量比共混，得到陶瓷表面密封用耐600℃高温涂层材料。
步骤二中所述二甲苯/四氢呋喃混合溶剂中二甲苯与四氢呋喃的体积比为1:0.8。
将本实验制备的陶瓷表面密封用耐600℃高温涂层材料于180℃固化3h后的TG谱图如图2所示。
将本实验制备的陶瓷表面密封用耐600℃高温涂层材料粘接陶瓷材料剪切强度如表1所示。
表1
本实验制备的陶瓷表面密封用耐600℃高温涂层材料粘度如表2。
表2

Claims (10)

1.陶瓷表面密封用耐600℃高温涂层材料的制备方法，其特征在于陶瓷表面密封用耐600℃高温涂层材料的制备方法按照以下步骤进行：
一、以聚二甲基硅烷和二茂铁为原料，在250～500℃、3～18MPa、惰性气体保护下反应0.5～12h，提纯后得到粘度为800～10000mPa·s、数均分子量为400～800、分散度小于3的聚铁碳硅烷，其中二茂铁加入量为聚二甲基硅烷和二茂铁总质量的0.5％～10％；
二、将聚铁碳硅烷、四甲基四乙烯基环四硅氮烷溶于二甲苯/四氢呋喃混合溶剂中，以偶氮二异丁腈为催化剂，在温度为80～90℃的条件下反应2～8h，提纯后得到粘度为800～10000mPa·s、数均分子量为500～1600、分散度小于3的乙烯基聚铁碳硅烷；
其中聚铁碳硅烷与四甲基四乙烯基环四硅氮烷的摩尔比为1:0.05～2.5，聚铁碳硅烷与二甲苯/四氢呋喃混合溶剂的质量比为1:2～8，聚铁碳硅烷与偶氮二异丁腈的摩尔比为1:0.5～2；
三、将乙烯基聚铁碳硅烷、氮化硼、碳化硅、氮化硅和碳化硼按照1:(0～4):(0～4):(0～4):(0～4)的质量比共混，得到陶瓷表面密封用耐600℃高温涂层材料；
其中，所述氮化硼、碳化硅、氮化硅和碳化硼的用量都不为0。
2.根据权利要求1所述陶瓷表面密封用耐600℃高温涂层材料的制备方法，其特征在于步骤二中所述二甲苯/四氢呋喃混合溶剂中二甲苯与四氢呋喃的体积比为1:0.5～1.3。
3.根据权利要求1所述陶瓷表面密封用耐600℃高温涂层材料的制备方法，其特征在于步骤一中在280～480℃、4～16MPa、惰性气体保护下反应1～10h。
4.根据权利要求1所述陶瓷表面密封用耐600℃高温涂层材料的制备方法，其特征在于步骤一中在300℃、10MPa、惰性气体保护下反应2h。
5.根据权利要求1所述陶瓷表面密封用耐600℃高温涂层材料的制备方法，其特征在于步骤一中二茂铁加入量为聚二甲基硅烷和二茂铁总质量的1％。
6.根据权利要求1所述陶瓷表面密封用耐600℃高温涂层材料的制备方法，其特征在于步骤二中在温度为88℃的条件下反应5h。
7.根据权利要求1所述陶瓷表面密封用耐600℃高温涂层材料的制备方法，其特征在于步骤二中聚铁碳硅烷与四甲基四乙烯基环四硅氮烷的摩尔比为1:0.5，聚铁碳硅烷与二甲苯/四氢呋喃混合溶剂的质量比为1:6，聚铁碳硅烷与偶氮二异丁腈的摩尔比为1:1。
8.根据权利要求1所述陶瓷表面密封用耐600℃高温涂层材料的制备方法，其特征在于步骤二中聚铁碳硅烷与四甲基四乙烯基环四硅氮烷的摩尔比为1:1。
9.根据权利要求1所述陶瓷表面密封用耐600℃高温涂层材料的制备方法，其特征在于步骤二中聚铁碳硅烷与二甲苯/四氢呋喃混合溶剂的质量比为1:6。
10.根据权利要求1所述陶瓷表面密封用耐600℃高温涂层材料的制备方法，其特征在于步骤三中将乙烯基聚铁碳硅烷、氮化硼、碳化硅、氮化硅和碳化硼按照1:4:3:2:1的质量比共混。
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