CN108587743B - 一种磁流变胶及其制备方法 - Google Patents
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Abstract
本发明公开了一种磁流变胶及其制备方法,所述磁流变胶包括磁性颗粒、载液和与所述载液互不相溶的极性溶剂或磁流体,按照以下体积百分比组成:磁性颗粒:10~40%,载液:60~90%,极性溶剂或磁流体:0.1~10%。其具有优异的沉降稳定性和显著的磁流变效应,并且制备方法简单,成本低。
Description
技术领域
本发明涉及磁流变技术,具体涉及一种磁流变胶及其制备方法。
背景技术
现有的磁流变液是一类分散均匀的磁性颗粒悬浮体系,其在磁场下的力学响应主要由磁性颗粒的体积分数决定,但是由于颗粒与载液间存在较大的密度差,使得体系缺乏足够的稳定性,因而限制了其应用和功能。
沉降稳定性一直是制约磁流变材料应用的最主要问题,目前大多数磁流变液零场黏度较高,稳定性能不理想。若发生沉降后的磁性颗粒结块成团,即使强力搅拌,也不能使颗粒再次均匀的分散到载液中,从而使磁流变液失去应用价值。通常使用表面改性剂减少磁性粒子团聚,添加触变剂提高载液黏度,釆用高分子包覆磁性粒子降低密度,或者采用双分散磁性颗粒的方法,可以在一定程度是改善磁流变液的沉降稳定性,但是会导致屈服应力的下降或零场黏度的上升。
发明内容
本发明的目的是提供一种磁流变胶及其制备方法,其具有优异的沉降稳定性和显著的磁流变效应,并且制备方法简单,成本低。
本发明所述的磁流变胶,包括磁性颗粒、载液和与所述载液互不相溶的极性溶剂或磁流体,按照以下体积百分比组成:
磁性颗粒:10~40%,
载液:60~90%,
极性溶剂或磁流体:0.1~10%。
进一步,所述磁性颗粒为羰基铁粉或磁性铁氧体粉末,所述磁性颗粒的平均粒径为1~10μm。
进一步,所述载液为矿物油、硅油或聚α烯烃。
进一步,所述极性溶剂为去离子水、乙二醇、丙三醇、二氯甲烷和聚乙二醇中的一种或多种的组合;所述磁流体包括极性溶剂和超声分散于所述极性溶剂中的粒径为3~15nm的磁性颗粒γ-Fe2O3或Fe3O4,所述磁性颗粒γ-Fe2O3或Fe3O4在磁流体中的体积百分比为0.1~2%。
一种磁流变胶的制备方法,其包括以下步骤:
1)取适量磁性颗粒,干燥;
2)取适量极性溶剂或磁流体加入到载液中,搅拌均匀后超声破碎,得到混合液;
3)将干燥后的磁性颗粒加入到步骤2)得到的混合液中,搅拌均匀后超声波分散或球磨分散,得到悬浮胶;
4)将步骤3)得到的悬浮胶置于真空干燥箱中除气泡,即得到磁流变胶,装入干燥的塑料容器中密封即可长期保存。
进一步,所述步骤1)中干燥磁性颗粒的真空度为0.2MPa,温度为80~100℃,时间为12h。
进一步,所述步骤二中的超声破碎时间为1~5min。
进一步,所述步骤三中采用超声波分散时,超声波分散时间为3~5min,采用球磨分散时,磨球转速为250~600rpm,球磨时间为1~3h。
进一步,所述步骤4)中真空干燥箱中的真空度为0.2~0.6MPa,常温下干燥5~30min。
本发明与现有技术相比具有如下有益效果:
1、本发明通过加入与载液互不相溶的极性溶剂或磁流体,使得磁性颗粒间形成毛细液桥,进而使得磁流变液发生相转变,由液体转变为类固体,凝化形成磁流变胶,提高了沉降稳定性;
2、磁流体的加入能显著增强磁流变胶的磁流变效应,基于磁流体的毛细液桥,在磁场作用下可以提高颗粒链的导磁能力,增大了磁性颗粒间的相互作用,从而提高了磁流变胶的力学性能。
3、本发明所述的制备方法工艺流程简单,采用的原材料价格低廉,成本低,得到的磁流变胶能够广泛应用于振动控制和机械传动领域。
附图说明
图1是本发明实施例三的磁流变胶和对比样的零场黏度与剪切速率的关系曲线图,其中样品中羰基铁含量均为20vol%,磁流变胶中含有体积分数为1.2%的乙二醇;
图2:是本发明实施例四的磁流变胶和对比样的零场黏度与剪切速率的关系曲线图,其中样品中羰基铁含量均为20vol%,磁流变胶中含有体积分数为1.6%的乙二醇;
图3是本发明实施例五的磁流变胶和对比样的储能模量随磁场强度的变化曲线,其中样品中羰基铁含量均为20vol%,磁流变胶中含有体积分数为0.5%的去离子水;
图4是本发明实施例六的磁流变胶和对比样的剪切应力随剪切速率的变化曲线,其中样品中羰基铁含量均为20vol%,磁流变胶中含有体积分数为3%的磁流体,实心符号表示H=0kA/m,空心符号表示H=211kA/m;
图5是本发明实施例七的磁流变胶和对比样的储能模量随磁场强度的变化曲线,其中样品中羰基铁含量均为30vol%,磁流变胶中含有体积分数为3%的磁流体。
具体实施方式
下面结合附图和具体实施方式对本发明作详细说明。
实施例一,一种磁流变胶,包括磁性颗粒、载液和与所述载液互不相溶的极性溶剂;所述磁性颗粒、载液和极性溶剂按以下体积百分比组成:
磁性颗粒:10~40%,
载液:60~90%,
极性溶剂:0.1~10%。
所述磁性颗粒为羰基铁粉,所述羰基铁粉的平均粒径为1~10μm;所述载液为矿物油、硅油或聚α烯烃;所述极性溶剂为去离子水、乙二醇、丙三醇、二氯甲烷、聚乙二醇中的一种或多种的组合。
实施例二,一种磁流变胶,包括磁性颗粒、载液和与所述载液互不相溶的磁流体;
所述磁性颗粒、载液和磁流体按以下体积百分比组成:
磁性颗粒:10~40%,
载液:60~90%,
磁流体:0.1~10%。
所述磁性颗粒为羰基铁粉,所述羰基铁粉的平均粒径为1~10μm;所述载液为矿物油、硅油或聚α烯烃;所述磁流体包括去离子水和超声分散于所述去离子水中的粒径为3~15nm的磁性颗粒γ-Fe2O3或Fe3O4,所述磁性颗粒γ-Fe2O3或Fe3O4在磁流体中的体积百分比为0.1~2%。
实施例三,一种磁流变胶的制备方法,其包括如下步骤:
1)取12.48g羰基铁粉在真空度为0.1MPa,温度为80℃的条件下干燥12h,除去羰基铁粉表面的物理吸附水;
2)取适量的乙二醇加入到6.27mL的矿物油中,搅拌均匀后超声破碎5min,得到混合液;
3)将干燥后的羰基铁粉加入到步骤2)得到的混合液中,搅拌均匀后超声波分散5min,得到悬浮胶;
4)将步骤3)得到的悬浮胶置于真空干燥箱中除气泡,在真空度为0.2MPa,温度为25℃的条件下,除气泡10min,即得到磁流变胶,所述磁流变胶的组成为:羰基铁粉:20vol%,矿物油:78.8vol%,乙二醇:1.2vol%。
实施例四,一种磁流变胶的制备方法,其包括如下步骤:
1)取12.48g羰基铁粉在真空度为0.1MPa,温度为80℃的条件下干燥12h,除去羰基铁粉表面的物理吸附水;
2)取适量的乙二醇加入到6.27mL的矿物油中,搅拌均匀后超声破碎5min,得到混合液;
3)将干燥后的羰基铁粉加入到步骤2)得到的混合液中,搅拌均匀后球磨分散,磨球转速为300rpm,球磨时间为1h,得到悬浮胶;
4)将步骤3)得到的悬浮胶置于真空干燥箱中除气泡,在真空度为0.6MPa,温度为25℃的条件下,除气泡10min,即得到磁流变胶,所述磁流变胶的组成为:羰基铁粉:20vol%,矿物油:78.4vol%,乙二醇:1.6vol%。
实施例五,一种磁流变胶的制备方法,其包括如下步骤:
1)取12.48g羰基铁粉在真空度为0.1MPa,温度为80℃的条件下干燥12h,除去羰基铁粉表面的物理吸附水;
2)取适量的去离子水加入到6.27mL的矿物油中,搅拌均匀后超声破碎5min,得到混合液;
3)将干燥后的羰基铁粉加入到步骤2)得到的混合液中,搅拌均匀后超声波分散5min,得到悬浮胶;
4)将步骤3)得到的悬浮胶置于真空干燥箱中除气泡,在真空度为0.4MPa,温度为25℃的条件下,除气泡10min,即得到磁流变胶,所述磁流变胶的组成为:羰基铁粉:20vol%,矿物油:79.5vol%,去离子水:0.5vol%。
实施例六,一种磁流变胶的制备方法,其包括如下步骤:
1)取12.48g羰基铁粉在真空度为0.1MPa,温度为80℃的条件下干燥12h,除去羰基铁粉表面的物理吸附水;
2)制备磁流体,采用化学共沉淀法制备Fe3O4磁性颗粒,其具体步骤为;
a.将二价铁盐和三价铁盐按一定比例混合,加入沉淀剂氨水溶液搅拌,反应一段时间即得到黑色的Fe3O4胶粒沉淀,反应式为:
2FeCl3·6H2O+FeCl2·4H2O+8NH3·H2O=Fe3O4+8NH4Cl+24H2O;
b.将黑色沉淀用水洗分离后,加入HNO3溶液搅拌,然后加入Fe(NO3)3溶液煮沸,一段时间后得到γ-Fe2O3棕色沉淀物;
c.将棕色沉淀分散在柠檬酸纳水溶液中,调节温度至80℃、pH=7,进行表面处理;
d将步骤c处理后的沉淀物经溶剂洗涤和柠檬酸处理后分散于去离子水中,调节pH=7,离心1h分离较大颗粒和团聚体,制得磁流体,所述磁流体中磁性颗粒的体积分数为1%,经试验验证得到的磁流体数月内未出现沉降和相分离现象;
3)取适量的磁流体加入到6.24mL的矿物油中,搅拌均匀后超声破碎5min,得到混合液;
4)将干燥后的羰基铁粉加入到步骤3)得到的混合液中,搅拌均匀后超声波分散5min,得到悬浮胶;
5)将步骤4)得到的悬浮胶置于真空干燥箱中除气泡,在真空度为0.4MPa,温度为25℃的条件下,除气泡10min,即得到磁流变胶,所述磁流变胶的组成为:羰基铁粉:20vol%,矿物油:78vol%,磁流体:2vol%。
实施例七,一种磁流变胶的制备方法,其包括如下步骤:
1)取12.48g羰基铁粉在真空度为0.1MPa,温度为80℃的条件下干燥12h,除去羰基铁粉表面的物理吸附水;
2)制备磁流体,采用化学共沉淀法制备Fe3O4磁性颗粒,其具体步骤为;
a.将二价铁盐和三价铁盐按一定比例混合,加入沉淀剂氨水溶液搅拌,反应一段时间即得到黑色的Fe3O4胶粒沉淀,反应式为:
2FeCl3·6H2O+FeCl2·4H2O+8NH3·H2O=Fe3O4+8NH4Cl+24H2O;
b.将黑色沉淀用水洗分离后,加入HNO3溶液搅拌,然后加入Fe(NO3)3溶液煮沸,一段时间后得到γ-Fe2O3棕色沉淀物;
c.将棕色沉淀分散在柠檬酸纳水溶液中,调节温度至80℃、pH=7,进行表面处理;
d将步骤c处理后的沉淀物经溶剂洗涤和柠檬酸处理后分散于去离子水中,调节pH=7,离心1h分离较大颗粒和团聚体,制得磁流体,所述磁流体中磁性颗粒的体积分数为1%,经试验验证得到的磁流体数月内未出现沉降和相分离现象;
3)取适量的磁流体加入到6.24mL的矿物油中,搅拌均匀后超声破碎5min,得到混合液;
4)将干燥后的羰基铁粉加入到步骤3)得到的混合液中,搅拌均匀后超声波分散5min,得到悬浮胶;
5)将步骤4)得到的悬浮胶置于真空干燥箱中除气泡,在真空度为0.4MPa,温度为25℃的条件下,除气泡10min,即得到磁流变胶,所述磁流变胶的组成为:羰基铁粉:20vol%,矿物油:78vol%,磁流体:3vol%。
实施例八:对制得的磁流变胶进行对比分析:
以实施例三制得的磁流变胶为分析样一,以实施例四制得的磁流变胶为分析样二,以羰基铁粉含量为20vol%的磁流变液为对比样,通过流变仪分别测定分析样一、分析样二和对比样的零场黏度随剪切速率的变化曲线,参见图1和图2,分析样一和分析样二的黏度明显高于对比样,约高出1~2个数量级,并表现出明显的剪切稀化特征。因为乙二醇的加入,其在磁性颗粒间形成了液桥,使颗粒组装联接,在整个体系内形成团聚结构,体系黏度显著增大,在剪切作用下,颗粒间距离增大,毛细液桥作用减弱,体系黏度随之降低。体系内的磁性颗粒聚集结构使磁流变胶具有良好的沉降稳定性。
以实施例五制得的磁流变胶为分析样三,通过流变仪测定分析样三和对比样的储能模量与磁场强度的关系曲线,参见图3,分析样三的储能模量高于对比样,尤其在低磁场强度下更明显。在低磁场强度下,毛细液桥作用以及静磁作用使得磁流变胶的力学强度增大,而在高磁场下,体系的力学强度主要由静磁作用决定,此时样品储能模量相近。
以实施例六制得的磁流变胶为分析样四,通过流变仪测定分析样四和对比样在不同磁场强度下剪切应力与剪切速率的关系曲线,参见图4,在零场时,分析样四的剪切应力高于对比样的剪切应力,这是磁性颗粒的毛细凝聚形成聚集结构所致,在磁场下,分析样四的剪切应力仍高于对比样的剪切应力,这是由于磁流体在磁性颗粒链间形成液桥,增强了颗粒链的导磁能力,使得颗粒间相互作用力增强,从而增大了分析样四的剪切应力。
以实施例七制得的磁流变胶为分析样五,通过流变仪测定分析样五和对比样储能模量与磁场强度的关系曲线,参见图5,在整个磁场强度测试范围内,分析样五的储能模量高于对比样,这是由于磁性颗粒链间的磁流体液桥,增强了颗粒链的导磁能力,使得颗粒间相互作用力增强,从而增大了分析样五的储能模量。
Claims (7)
1.一种磁流变胶,其特征在于:包括磁性颗粒、载液和与所述载液互不相溶的极性溶剂或磁流体,按照以下体积百分比组成:
磁性颗粒:10~40%,
载液:60~90%,所述载液为矿物油、硅油或聚α烯烃;
极性溶剂或磁流体:0.1~10%;所述极性溶剂为去离子水、乙二醇、丙三醇和二氯甲烷中的一种或多种的组合;
所述磁流体包括极性溶剂和超声分散于所述极性溶剂中的粒径为3~15nm的磁性颗粒γ-Fe2O3或Fe3O4,所述磁性颗粒γ-Fe2O3或Fe3O4在磁流体中的体积百分比为0.1~2%。
2.根据权利要求1所述的磁流变胶,其特征在于:所述磁性颗粒为羰基铁粉或磁性铁氧体粉末,所述磁性颗粒的平均粒径为1~10μm。
3.一种根据权利要求1或2所述的磁流变胶的制备方法,其特征在于包括以下步骤:
1)取适量磁性颗粒,干燥;
2)取适量极性溶剂或磁流体加入到载液中,搅拌均匀后超声破碎,得到混合液;
3)将干燥后的磁性颗粒加入到步骤2)得到的混合液中,搅拌均匀后超声波分散或球磨分散,得到悬浮胶;
4)将步骤3)得到的悬浮胶置于真空干燥箱中除气泡,即得到磁流变胶,装入干燥的塑料容器中密封即可长期保存。
4.根据权利要求3所述的磁流变胶的制备方法,其特征在于:所述步骤1)中干燥磁性颗粒的真空度为0.2MPa,温度为80~100℃,时间为6~12h。
5.根据权利要求3或4所述的磁流变胶的制备方法,其特征在于:所述步骤二中的超声破碎时间为1~5min。
6.根据权利要求3或4所述的磁流变胶的制备方法,其特征在于:所述步骤三中采用超声波分散时,超声波分散时间为3~5min,采用球磨分散时,磨球转速为250~600rpm,球磨时间为1~3h。
7.根据权利要求3或4所述的磁流变胶的制备方法,其特征在于:所述步骤4)中真空干燥箱中的真空度为0.2~0.6MPa,常温下干燥5~30min。
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