CN107022161B - 一种用于超声传导的水凝胶材料及其制备方法 - Google Patents
一种用于超声传导的水凝胶材料及其制备方法 Download PDFInfo
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Abstract
一种用于超声传导的水凝胶材料及其制备方法,属于水凝胶功能材料技术领域。其中所述的水凝胶材料是由以聚乙烯醇,聚乙烯吡咯烷酮,海藻酸钠,聚丙烯酸钠,氯化钙,单宁,亚硝酸盐,三乙醇胺,聚乙二醇,丙二醇,甘油、磷酸和水等原料制备的原料液,通过高能射线辐照合成方法制得。通过本发明所公开的制备方法制得的水凝胶材料具有良好的声学传导性能,并且具有良好的拉伸强度,韧性,弹性模量和耐疲劳性等机械性能,能够应用于超声无损检测等多种领域,具有超声耦合效果好、机械强度高、抗老化、防锈蚀、使用便利、安全等特点。
Description
技术领域
本发明涉及一种用于超声传导的水凝胶材料及其制备方法,属于水凝胶功能材料技术领域。
技术背景
超声耦合材料在多个领域有着广泛且重要的应用。比如在超声检测及治疗过程中,需将耦合剂涂抹于皮肤表面,使超声发生探头与皮肤紧密结合,避免超声波在传导过程中损失,而影响检测结果及治疗效果。工业上使用超声波进行探伤作业,检测各种金属材料及铸件、复合材料、塑料制品、精密工件等的加工精度,确认其内部是否存在裂隙、缺陷、伤痕等。超声探伤中需要使用导声材料作为超声探头和被测物之间的超声传导介质,实现界面间的耦合,即排除探头与被测物间的空气,使超声波能有效地传入被测物,达到有效检测的目的。
目前常用的用于工业超声探伤的耦合材料为水,膏状耦合剂,有机玻璃和透声橡胶。水浸法是常用的超声探伤检测方法,即将待测器件置于水中检测,但在实际应用中,由于此方法必须浸入水中,无法用于尺寸过大、材质不能接触水或易锈蚀的器件。通过涂抹膏状耦合剂虽然能够实现大尺寸器件的超声无损检测,但由于其为不定型态,在检测过程中容易二次产生气泡,影响检测结果,且使用后需要清除,残留的耦合剂还存在锈蚀和腐蚀器件的风险。有机玻璃的声波传导性能优良,但是机械强度高,对于表面粗糙和不规则曲面等特殊部位使用时,不能与待测器件紧密结合,从而影响检测结果。透声橡胶的声波传导性能相对适中,但是透声橡胶的机械强度和弹性模量太高,在拉伸移动时,会有颗粒状橡胶脱落,因此使用不便利性差。固态水凝胶材料作为一种新兴材料,具有良好的超声传导性能,是一种优秀的超声传导材料。目前已有专利报导(一种医用超声耦合剂贴片的制备方法,专利公开号CN 105056257 A),将固态的水凝胶材料用于医用超声耦合,但由于水凝胶材料机械强度差,在受到较大的作用力后,容易破碎,因此无法应用于工业超声无损检测。
发明内容
为解决现有用于超声无损检测的耦合材料所存在的技术缺陷,本发明公开了一种具备优良声学性能的水凝胶材料及制备方法,该制备方法制备的水凝胶材料具有优良力学性能和声传导性能,其声传导性能与水接近,同时具有良好的拉伸强度,弹性模量和耐疲劳性,能够解决现有技术方案的技术缺陷。
本发明采用的技术方案是:一种用于超声传导的水凝胶材料,所述水凝胶材料采用包括高分子骨架成分、增韧剂、增弹剂、防锈剂、保湿剂、水的原料制得原料液;所述高分子骨架成分为聚乙烯醇和聚乙烯吡咯烷酮,聚乙烯醇用量占原料液质量百分比2%-15%,聚乙烯吡咯烷酮用量占原料液质量百分比2%-5%;所述增韧剂为单宁及由氧化钙、磷酸、氢氧化钠原位反应制得的羟基磷灰石;其中单宁用量为原料液质量百分比0.1%-0.4%,用于制得羟基磷灰石的氧化钙用量为原料液质量百分比0.14%-1.4%,磷酸为原料液质量百分比0.1%-1%,氢氧化钠用量为原料液质量百分比0.024%-0.24%;所述增弹剂为海藻酸钠、聚丙烯酸钠的中一种或两种的混合物;其中海藻酸钠用量为原料液质量百分比0.2%-3%,聚丙烯酸钠用量为原料液质量百分比0.05%-0.5%;所述防锈剂为三乙醇胺、亚硝酸钠中的一种或两者的混合物,其中三乙醇胺用量为原料液质量百分比0.5%-3.5%,亚硝酸钠用量为原料液质量百分比0.1%-1%;所述保湿剂为聚乙二醇、丙二醇、甘油中的一种或以上两种或三种原料的混合物,其中聚乙二醇用量为原料液质量百分比2%-20%,丙二醇用量为原料液质量百分比1%-5%,甘油用量为原料液质量百分比1%-5%。
所述的一种用于超声传导的水凝胶材料的制备方法步骤如下:
步骤1、按所述质量百分比准备水凝胶材料的原料;
步骤2、将聚乙烯醇、聚乙烯吡咯烷酮、海藻酸钠和聚丙烯酸钠制成水溶液;
步骤3、制备原位合成的羟基磷灰石,配制氧化钙水溶液,加入步骤2水溶液中,持续加热搅拌,依次加入磷酸、氢氧化钠和三乙醇胺;
步骤4、向步骤3中,加入单宁和亚硝酸盐;
步骤5、向步骤4中加入聚乙二醇、丙二醇和甘油后,制得的原料液经真空脱泡后待用;
步骤6、制得的原料液通过包括γ射线、高能X射线、电子束的高能射线辐照合成方法制得水凝胶材料。
本发明的有益效果是:
1、这种水凝胶材料具有良好的声学传导性能。其声速与水接近,在1500-1700m/s之间,声阻抗率在1.5-1.6x106pa.s/m之间,衰减常数小于0.6Np/m,达到优良透声橡胶的水平,使其成为非常优秀的声波传导介质材料。
2,水凝胶材料具有良好的力学性能,拉伸强度达到3-5MPa,使水凝胶材料具有可加工性能,弹性模量为2-4 MPa,韧性达500-1000 J/m2,确保水凝胶材料的拉伸和形变过程中不容易断裂,提供操作便利性。水凝胶材料具有良好的耐疲劳性,反复拉伸100次,在第3次后,弹性模量几乎无变化,确保水凝胶材料可以长时间反复使用。
3,水凝胶材料的表面和内部的pH值均为7.0-8.0,三乙醇胺,磷酸酯和亚硝酸钠的加入防止锈蚀金属。水凝胶材料的缺口敏感性与有机玻璃相比相对较低,不容易发生断裂,降低在使用过程中磨损对于水凝胶材料强度的影响,保证其在使用过程中的完整性。
上述优良的性能使水凝胶材料可以广泛应用于工业超声探伤和医用理疗检测等领域。该水凝胶材料的安全性、便利性大幅提高了作为超声耦合材料的使用性。同时,该水凝胶材料的合成、加工方法,具备可生产性,可以大量的满足多样化的材料需求。
具体实施方式
以下是本发明的具体实施例,所述的实施例是用于描述本发明,而不是限制本发明。
实例1:将15g聚乙烯醇,5g聚乙烯吡咯烷酮,3g海藻酸钠,0.5g聚丙烯酸钠,和38.96g水加入到三口烧瓶中,加热至温度为95℃,搅拌制得均匀的水溶液,持续加热搅拌,加入1.4g氧化钙,待氧化钙全部溶解,依次加入1mL浓磷酸,反0.24g氢氧化钠和3.5g三乙醇胺。待搅拌均匀后,加入0.4g单宁,1g亚硝酸钠,20g聚乙二醇,5g丙二醇和5g丙三醇,当溶液搅拌均匀后倒出,使用真空脱泡处理。得到无气泡高分子水溶液。将制得的高分子水溶液进行涂布处理。使用电子加速器进行高能射线照射,照射剂量为5kgy,制得水凝胶材料。
实例2-8的制备方法与实例1类似,具体原料配比如下表所示:
实例1-8的各种组分配比表
实施例2-8所采用的高能射线辐照合成装置及辐照剂量如下表:
从实例1-8制备的水凝胶材料中,每种配比随机选取5个,测试水凝胶材料的声学性能和力学性能。结果如下表所示:
从实例1-8制备的水凝胶材料中,每种配比随机选取5个,进行防锈蚀测试,将样品置于铸铁铁板,标记位置,存放24小时后,把样品从铁板取下,记录随着时间的增加,标记位置是否存在锈蚀。结果如下表:
上述结果表明:
1、本发明的水凝胶材料的声学传导性能与水接近,超声传导效果良好,可以作为超声传导介质使用。
2、本发明水凝胶材料的拉伸强度,弹性模量和韧性良好,可加工成任意立体结构,可以在不规则曲面等特殊部位上使用,按压和移动。
3、本发明水凝胶材料中加入多种防锈剂,使用过后,随着时间延长,金属没有发生锈蚀,减少水凝胶材料锈蚀金属风险。
Claims (2)
1.一种用于超声传导的水凝胶材料,其特征是:所述水凝胶材料采用包括高分子骨架成分、增韧剂、增弹剂、防锈剂、保湿剂、水的原料制得原料液;所述高分子骨架成分为聚乙烯醇和聚乙烯吡咯烷酮,聚乙烯醇用量占原料液质量百分比2%-15%,聚乙烯吡咯烷酮用量占原料液质量百分比2%-5%;所述增韧剂为单宁及由氧化钙、磷酸、氢氧化钠原位反应制得的羟基磷灰石;其中单宁用量为原料液质量百分比0.1%-0.4%,用于制得羟基磷灰石的氧化钙用量为原料液质量百分比0.14%-1.4%,磷酸为原料液质量百分比0.1%-1%,氢氧化钠用量为原料液质量百分比0.024%-0.24%;所述增弹剂为海藻酸钠、聚丙烯酸钠中的一种或两种的混合物;其中海藻酸钠用量为原料液质量百分比0.2%-3%,聚丙烯酸钠用量为原料液质量百分比0.05%-0.5%;所述防锈剂为三乙醇胺、亚硝酸钠中的一种或两者的混合物,其中三乙醇胺用量为原料液质量百分比0.5%-3.5%,亚硝酸钠用量为原料液质量百分比0.1%-1%;所述保湿剂为聚乙二醇、丙二醇、甘油中的一种或以上两种或三种原料的混合物,其中聚乙二醇用量为原料液质量百分比2%-20%,丙二醇用量为原料液质量百分比1%-5%,甘油用量为原料液质量百分比1%-5%。
2.根据权利要求1所述的一种用于超声传导的水凝胶材料的制备方法,其特征是:所述原料液制备步骤如下:
步骤1、按所述质量百分比准备水凝胶材料的原料;
步骤2、将聚乙烯醇、聚乙烯吡咯烷酮、海藻酸钠和聚丙烯酸钠制成水溶液;
步骤3、制备原位合成的羟基磷灰石,配制氧化钙水溶液,加入步骤2水溶液中,持续加热搅拌,依次加入磷酸、氢氧化钠和三乙醇胺;
步骤4、向步骤3中,加入单宁和亚硝酸盐;
步骤5、向步骤4中加入聚乙二醇、丙二醇和甘油后,制得的原料液经真空脱泡后待用;
步骤6、制得的原料液通过包括γ射线、高能X射线、电子束的高能射线辐照合成方法制得水凝胶材料。
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