CN106729969A - 一种二氧化锆多孔生物骨修复支架的挂浆方法 - Google Patents
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Abstract
本发明涉及生物陶瓷支架材料的制备方法。一种二氧化锆多孔生物骨修复支架的挂浆方法,该方法包括以下的步骤:1)聚氨酯泡沫模型材料预处理,提高材料的亲水性和粘附性能;2)在聚氨酯泡沫模型材料上挂浆,所述的挂浆包括2~4次,第一次挂浆,浆料中ZrO2粉体的质量百分比为55~70%;挂浆后置于室温下自然干燥;然后放入烘箱中,在 100~120℃条件下烘干,使水分质量分数降至1%以下;以后每次挂浆ZrO2粉体的质量百分比相对于前一次挂浆减少1%~5%,挂浆后以相同的方法干燥并烘干。采用该方法挂浆后二氧化锆多孔生物骨修复支架经过烧结制备的二氧化锆多孔生物骨修复支架抗压及抗弯强度大,孔隙率高,孔径大小合适,能与宿主骨牢固结合,不会产生明显的异物反应,生物相容性好。
Description
技术领域
本发明涉及生物陶瓷支架材料的制备方法。
背景技术
由于创伤、炎症、肿瘤的外科治疗所导致的骨缺损特别是大段骨缺损,是除了由骨折所致的骨不连外,引起功能丧失并影响生活质量的主要原因。目前传统自体松质骨移植是治疗局部骨缺损的金标准。但是其存在不可否认的局限性,如供骨区损伤,术后并发症和治疗费用等问题,更重要的是来源与数量有限。异体骨移植则不受形状与数量的限制,可达到即时的骨量要求,其骨愈合过程与传统的长段自体移植骨基本类似。但是异体骨经各种灭菌处理后缺乏自身成骨作用,骨愈合过程缓慢且多存在不同程度的排斥反应,因此效果不佳。
随着生物材料科学的兴起,以生物材料来制作移植替代物的组织工程学正在不断的发展。因此,组织工程骨修复骨缺损也成为当前研究热点。
骨组织工程支架材料是指能与成骨细胞结合并能置入生物体的材料,它是组织工程化骨的最基本构架。植入体内后,支架材料与宿主组织接触部分发生化学结合,能长期发挥功能,而不至于在界面处发生松动与破坏。理想的骨组织工程支架材料应具备以下条件:良好的组织相容性和良好的表面活性,有利于细胞的粘附,并为细胞在其表面生长、增殖和分泌基质提供良好的微环境;具有可塑性,可被加工成所需的形状,并有一定的机械强度,在置入体内后的一定时间内仍可保持其形状,使新形成的组织具有一定的外形;具有三维立体结构,材料必须是高度多孔的,类似泡沫状,孔隙率应达到80%以上,具有较大的内表面积,一方面有利于细胞的植入粘附,另一方面有利于细胞营养成分的渗入和细胞代谢产物的排除。
目前,骨组织工程支架材料主要分为三类:生物衍生材料、陶瓷材料和高分子材料。生物衍生材料具有抗原性,特别是植体较大时,常常会引起剧烈的免疫排斥反应。羟基磷灰石是最主要的陶瓷材料,它是骨的无机成分。合成的羟基磷灰石具有良好的生物活性和生物相容性,具有较高的骨结合能力。但是由于它的力学性能较差,无法满足多数生物体内植入的生物力学要求。而高分子材料应用过程中,根据生物医用材料的要求,支架材料植入体内后,应尽量避免其与宿主骨之间的炎性反应,以保证植入材料的长期安全性。RoelKuijer等人对聚酯共聚物的支架材料研究表明,不管支架上是否种细胞,植入兔体内后均有部分支架与宿主骨之间出现感染症状。
因此,我们通过干铺-烧结方法制备出ZrO2多孔生物骨修复支架。为骨缺损治疗提供一种孔隙率高、抗压强度大、韧性强的生物陶瓷人工骨支架材料。
发明内容
本发明针对上述问题,本发明的目的提供一种二氧化锆多孔生物骨修复支架的挂浆方法,采用该方法挂浆后二氧化锆多孔生物骨修复支架经过烧结制备的二氧化锆多孔生物骨修复支架抗压及抗弯强度大,孔隙率高,孔径大小合适,能与宿主骨牢固结合,不会产生明显的异物反应,生物相容性好。
为了实现上述的目的,本发明采用了以下的技术方案:
一种二氧化锆多孔生物骨修复支架的挂浆方法,该方法包括以下的步骤:
1)聚氨酯泡沫模型材料预处理,提高材料的亲水性和粘附性能;
2)在聚氨酯泡沫模型材料上挂浆,所述的挂浆包括2~4次,第一次挂浆,浆料中ZrO2粉体的质量百分比为55~70%;挂浆后置于室温下自然干燥;然后放入烘箱中,在 100~120℃条件下烘干,使水分质量分数降至1%以下;以后每次挂浆ZrO2粉体的质量百分比相对于前一次挂浆减少1%~5%,挂浆后以相同的方法干燥并烘干。
作为优选,步骤1)中将有机聚氨酯泡沫材料采用50~70℃、10~20wt% 氢氧化钠溶液浸泡 3.0~4.0 h,用清水反复揉搓2~4遍,晾干;再以表面活性剂继续对有机聚氨酯泡沫体材料进行表面处理,最后用5% PVA浸泡20~30h后干燥。
作为优选,步骤2)中第一次挂浆的浆料按质量百分比计包括以下的组分:
ZrO2粉体 55~70%
聚乙烯醇 0.2~1.0%
羧甲基纤维素 0.2~1.0%
硅溶胶 8~15%
聚丙稀酸铵 0.2~1.2%。
作为优选,步骤2)中第一次挂浆的浆料按质量百分比计包括以下的组分:
ZrO2粉体 60~65%
聚乙烯醇 0.2~1.0%
羧甲基纤维素 0.2~1.0%
硅溶胶 8~15%
聚丙稀酸铵 0.2~1.2%。
作为优选,步骤2)第一次挂浆以后每次挂浆ZrO2粉体的质量百分比相对于前一次挂浆减少1%~5%,其他成分不变。
作为优选,步骤2)中挂浆制浆前ZrO2粉体进行预烧处理,处理温度在30℃至800℃之间时升温速度为2℃/min,800℃至1250℃之间时升温速度为4℃/min,升温至 1250℃后保温4h完成粉体预处理。
作为优选,步骤2)中浆料的制备过程如下:对原料进行完全混合研磨后,采用粉球质量比1:2,转速300r/min的高速球磨机研磨3h以制取浆料,然后先将一定量去离子水和硅溶胶搅拌10 min,加入CMC 和消泡剂辛醇,ZrO2粉体,再搅拌3 h,等待挂浆。
本发明针对现有生物陶瓷支架一旦孔隙率增高就难以满足对人工骨抗压强度和韧性要求这一缺陷,以纳米二氧化锆作为生物骨修复支架,从而为骨缺损治疗提供一种孔隙率高、抗压强度大、韧性强的生物陶瓷人工骨支架。采用该方法挂浆后二氧化锆多孔生物骨修复支架经过烧结制备的二氧化锆多孔生物骨修复支架由于孔隙率高,孔径大小合适,抗压强度大、韧性强,而且骨组织易于长入,融合速度快,与宿主骨牢固结合,不会产生明显的异物反应,生物相容性好,本发明生物陶瓷既可用于骨组织损伤修复,还可以用于体外细胞培养。
附图说明
图1为本发明具体实施方式泡沫陶瓷人工椎体尺寸图。
图2为本发明具体实施方式泡沫陶瓷人工椎体超景深图片。
图3为本发明具体实施方式术后12周椎体标本及X片。
具体实施方式
下面以犬腰椎椎体HA/ZrO2生物陶瓷支架材料作为实例对本发明进行详细的说明。
1.1 模型有机泡沫材料预处理
采用聚氨酯作为泡沫模型材料,由于聚氨酯材料存在网络间膜,而间膜的存在使浆料很难进入泡沫体模型内部,将造成堵孔、浆料无法均匀分布、烧结后的泡沫陶瓷的空隙率和力学性能较差。故需先将膜打通,使有机体泡沫形成三维网状结构。另外,有机泡沫模型存在亲水性较差、润湿角小故浆料不易吸附。为改善泡沫体模型材料的挂浆性能,需要进行预处理。将有机聚氨酯泡沫材料切割为高24cm、半径9cm半圆柱型大小,采用60℃、15wt% 氢氧化钠溶液浸泡 3.5 h,用清水反复揉搓3遍,晾干备用。处理后的有机聚氨酯泡沫材料由于被碱液腐烛,表面粗糙度明显增加,故使其亲水性和粘附性能有所改善。再以表面活性剂继续对有机聚氨酯泡沫体材料进行表面处理,最后用5% PVA浸泡24h后干燥。
1.2 ZrO2粉体、浆料的制备
采用箱式电阻炉对粉体进行预烧处理,处理温度在30℃至800℃之间时升温速度为2℃/min,800℃至1250℃之间时升温速度为4℃/min,升温至 1250℃后保温4h完成粉体预处理。浆料制备采用添加剂配比:聚乙烯醇(PVA)、羧甲基纤维素(CMC)的含量均为0.5%,加入10% 硅溶胶,聚丙稀酸铵(PAA-NH4)的含量为0.6%。首次挂浆加入ZrO2的质量分数为60%,故整体浆料固相率约为60%。对原料进行完全混合研磨后,采用粉球质量比1:2,转速300r/min的高速球磨机研磨3h以制取浆料,然后先将一定量去离子水和硅溶胶搅拌10 min,加入CMC和消泡剂辛醇,ZrO2粉体,再搅拌3 h,等待挂浆。将挂浆过程中有机泡沫内部多余浆料通过挤压法去除,保证其通孔率。再将试样置于室温下18h~24 h后自然干燥。然后放入烘箱中,在 110℃条件下烘干12 h,使水分质量分数降至1%以下。然后进行第二次研磨、挂浆,采用同样添加剂配比,但加入ZrO2粉料的质量分数降至57%,使整体浆料固相率降至57%。第二次起使用离心挂浆法,即先将未处理有机泡沫材料放入离心管底部,以便于隔离甩出的浆料,再将浸泡好的含浆料有机泡沫放入,1500r/min离心1min。经过相同工艺烘干后行第3次挂浆,第3次同样采用前两次添加剂配比,但ZrO2粉料质量分数为54%,整体浆料固相率调整至54%。
1.3 ZrO2陶瓷的烧结
对上述挂浆后预制体试样采用了三段式烧结工艺进行烧结,分别为(1)烘干阶段:在室温至100℃时,升温速度为2℃/min,目的使预制体试样内残余的水分挥发。(2)挥发阶段:在100℃至200℃时,控制升温速度为1℃/min,在200至500℃时,控制升温速度在1℃/2min,升温至500℃时,保温1h,后升温到500至750℃时,控制升温速度为2℃/3min,升温至750℃后,保温1h,后升温到750至1200℃时,控制升温速度为2℃/min。(3)高温焙烧阶段:后持续烧结温度保持在3℃/min,到达1550℃的最高烧结温度后,再保温3h并随炉冷却。得到高24cm、半径9cm半圆柱型纯ZrO2人工椎体。
1.4 在纯ZrO2泡沫陶瓷人工椎体表面浸涂HA 梯度涂层
采取两步法浸涂法涂覆梯度HA涂层。第一次浸涂浆料配比为:ZrO2粉体31.1%、HA粉体13.3%,磷酸乙酯1.4%,乙基纤维素0.2%,双蒸水53%。先将HA粉体加热至800℃后保温2h预处理,再将上述原料在50℃热水中混合,并搅拌5h。将烧结出的纯ZrO2泡沫陶瓷人工椎体浸入浆料,等完全浸透后取出,甩去多余浆料。100℃烘干5h,再加热到900℃保温5h,最后加热到1250℃保持1h。第二次浸涂浆料配比为:ZrO2粉体3.9%,HA粉体35.5%,磷酸乙酯1.4%,乙基纤维素0.2%,双蒸水58%,配置好浆料后重复上述步骤。得到HA/ZrO2梯度复合泡沫陶瓷人工椎体。
上述制备的HA/ZrO2梯度复合泡沫陶瓷人工椎体的具体数据为平均抗压强度14.28 MPa,平均孔隙率80.95%,体外细胞毒性试验(MTT)(—)。
Claims (7)
1.一种二氧化锆多孔生物骨修复支架的挂浆方法,其特征在于该方法包括以下的步骤:
1)聚氨酯泡沫模型材料预处理,提高材料的亲水性和粘附性能;
2)在聚氨酯泡沫模型材料上挂浆,所述的挂浆包括2~4次,第一次挂浆,浆料中ZrO2粉体的质量百分比为55~70%;挂浆后置于室温下自然干燥;然后放入烘箱中,在 100~120℃条件下烘干,使水分质量分数降至1%以下;以后每次挂浆ZrO2粉体的质量百分比相对于前一次挂浆减少1%~5%,挂浆后以相同的方法干燥并烘干。
2.根据权利要求1所述的一种二氧化锆多孔生物骨修复支架的挂浆方法,其特征在于:步骤1)中将有机聚氨酯泡沫材料采用50~70℃、10~20wt% 氢氧化钠溶液浸泡 3.0~4.0 h,用清水反复揉搓2~4遍,晾干;再以表面活性剂继续对有机聚氨酯泡沫体材料进行表面处理,最后用5% PVA浸泡20~30h后干燥。
3.根据权利要求1所述的一种二氧化锆多孔生物骨修复支架的挂浆方法,其特征在于步骤2)中第一次挂浆的浆料按质量百分比计包括以下的组分:
ZrO2粉体 55~70%
聚乙烯醇 0.2~1.0%
羧甲基纤维素 0.2~1.0%
硅溶胶 8~15%
聚丙稀酸铵 0.2~1.2%。
4.根据权利要求1所述的一种二氧化锆多孔生物骨修复支架的挂浆方法,其特征在于步骤2)中第一次挂浆的浆料按质量百分比计包括以下的组分:
ZrO2粉体 60~65%
聚乙烯醇 0.2~1.0%
羧甲基纤维素 0.2~1.0%
硅溶胶 8~15%
聚丙稀酸铵 0.2~1.2%。
5.根据权利要求3或4所述的一种二氧化锆多孔生物骨修复支架的挂浆方法,其特征在于步骤2)第一次挂浆以后每次挂浆ZrO2粉体的质量百分比相对于前一次挂浆减少1%~5%,其他成分不变。
6.根据权利要求1或2或3所述的一种二氧化锆多孔生物骨修复支架的挂浆方法,其特征在于步骤2)中挂浆制浆前ZrO2粉体进行预烧处理,处理温度在30℃至800℃之间时升温速度为2℃/min,800℃至1250℃之间时升温速度为4℃/min,升温至 1250℃后保温4h完成粉体预处理。
7.根据权利要求3或4所述的一种二氧化锆多孔生物骨修复支架的挂浆方法,其特征在于步骤2)中浆料的制备过程如下:对原料进行完全混合研磨后,采用粉球质量比1:2,转速300r/min的高速球磨机研磨3h以制取浆料,然后先将一定量去离子水和硅溶胶搅拌10min,加入CMC 和消泡剂辛醇,ZrO2粉体,再搅拌3 h,等待挂浆。
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