CN106086998B - 一种钛烤瓷义齿的电泳沉积-激光熔覆复合加工方法 - Google Patents
一种钛烤瓷义齿的电泳沉积-激光熔覆复合加工方法 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
- C23C28/042—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material including a refractory ceramic layer, e.g. refractory metal oxides, ZrO2, rare earth oxides
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Abstract
本发明公开了一种钛烤瓷义齿的电泳沉积‑激光熔覆复合加工方法。该加工方法首先采用电泳沉积的方法在牙科纯钛及钛合金表面沉积一定厚度的瓷层,然后采用激光熔覆的方法将瓷层熔覆到牙科纯钛及钛合金上,从而制备出牙科纯钛及钛合金烤瓷义齿。预计该方法将解决烤瓷义齿加工过度依赖人工涂覆、重复性差的缺点,在钛烤瓷义齿加工过程中得到广泛应用。
Description
技术领域
本发明属于生物材料技术领域,具体涉及一种钛烤瓷义齿的电泳沉积-激光熔覆复合加工方法。
背景技术
牙科烤瓷材料自临床应用以来,由于其良好的生物相容性、耐磨耐腐蚀性以及色泽自然逼真等优点,已成为治疗牙缺失的最主要方法。牙科纯钛及钛合金由于其不含对人体有害的镍元素与铍元素,不易过敏,已被广泛用到口腔领域。牙科纯钛及钛合金烤瓷牙相比镍铬烤瓷牙,耐腐蚀性更高、生物相容性更好,不易出现黑色牙龈或者牙龈出血的现象,安全可靠且价格较低,逐渐替代镍铬合金烤瓷牙成为非贵金属烤瓷的首选。
牙科纯钛烤瓷瓷层有粘结瓷、遮色瓷、体瓷和釉质瓷等,目前其制作的一般流程为人工刷涂瓷粉构筑瓷层,并经烧结熔覆在金属基底表面。在金属基底上制备涂层的方法主要有涂覆-烧结法、等离子喷涂法和电泳沉积烧结法等。涂覆-烧结法作为一种传统的制备瓷层的工艺,具有工艺简单,成本低廉等优点;缺点是手工涂覆复现性差,涂层厚度难以控制,易造成表面瓷层不均匀,难于实现连续生产等。等离子喷涂工艺的优点是不会改变基体全局的热处理性质,零件无变形;高温度的等离子焰流,可将各种喷涂材料加热到熔融状态,从而制备得到多种性能的喷涂层;其工艺稳定,涂层质量高。缺点是等离子喷涂设备昂贵,难以在复杂的金属基底上实现瓷层尺寸的精度控制。
电泳沉积工艺是一种非线性涂层工艺,可以在形状复杂的基体上制备出均匀涂层。电泳沉积是电泳和沉积两个过程的综合,配合调节沉积电压,可实现不同成分的颗粒在基体上先后沉积或共同沉积,从而获得组成和孔结构呈梯度变化的涂层坯体。其优点是操作方便、工艺过程易于控制;所需设备简单、工艺成本低;可连续生产,又可间歇操作;料液可循环利用,无污染物排放;可通过控制工艺参数在较大范围内控制涂层的组成、厚度和微观结构,在多层材料的制备方面具有独特的优势。另外,电泳沉积可避免采用高温涂敷引起的相变和脆裂。因牙齿形状特殊,将该工艺结合激光熔覆工艺或常规烧结工艺,可实现金属烤瓷义齿的规模生产。
由电泳沉积所制得的涂层仅为较紧密堆积的坯体,涂层与基体结合强度很低,通过激光熔覆可增强涂层与基体的结合,同时也使坯体本身致密化。梯度涂层中无明显的界面,从而使热应力得到了缓和,提高了涂层的结合强度和稳定性。这是其它涂覆工艺结合热处理所不能比拟的。
专利[CN1834306]提出了一种在钛或纯钛及钛合金表面电泳沉积羟基磷灰石涂层的制备方法,以质子型的正丁醇和非质子型的氯仿混合溶剂为分散介质,添加少量的三乙醇胺加速HAp颗粒的荷电过程,在医用钛或纯钛及钛合金表面电泳沉积HAp涂层,该工艺具有稳定性高、沉积时间短、工艺简单和结合强度高等特点。
激光熔覆是近年来迅速发展的一种材料制备手段,在激光高能量作用下,熔覆层被快速加热、熔化,在表面制备的涂层与合金界面形成牢固的冶金与化学结合,可以保证涂层和基体的结合强度。专利[CN 101053677A]提出了一种梯度生物活性陶瓷涂层及其制备方法与产品应用,采用宽带激光熔覆技术,优化了各梯度涂层的成分及比例,所制备的生物活性陶瓷涂层裂纹和孔洞少,硬度高,韧性好,生物活性和生物相容性大大提高。专利[CN102676981A]提出了一种钛及纯钛及钛合金表面激光制备氮化钛梯度涂层的方法,在钛及钛合金表面得到厚度为50-200μ m的氮化钛梯度涂层,表面硬度、耐磨性和耐蚀性较基体显著提高,并解决了普通激光气体氮化易产生裂纹、表面粗糙度大、氮化层树枝晶晶粒粗大的问题。
专利[CN 103833350 A] 提出了一种激光制备钛酸钙铝电子功能陶瓷的材料及方法,用宽带二氧化碳激光直接烧结制得钛酸钙铝电子功能陶瓷,激光烧结法耗能少,烧结时间极短(1.5秒左右),制得的钛酸钙铝陶瓷产品晶粒细小,无气孔,致密度高。专利[CN1654433A] 提出了激光熔覆制备梯度生物活性陶瓷涂层的材料及涂层的制法,所涉及的生物活性陶瓷涂层由铁粉与复合陶瓷粉制备而成,这种新的涂层材料能在钛合金表面形成生物活性陶瓷涂层,得到的产品生物活性好,不发生排异反应。文献[应用激光,2014, 34(6):487–493.] 研究了钛合金表面激光制备生物陶瓷梯度涂层,通过涂层成分设计与激光熔覆梯度制备方法,在Ti6Al4V合金基体上制备生物陶瓷梯度涂层。
目前尚未有采用电泳沉积与激光熔覆相结合的方法加工钛烤瓷义齿的报道,将电泳沉积-激光熔覆复合加工技术引入钛烤瓷义齿制备过程具有重要的应用意义。本发明的目的是开发一种钛烤瓷义齿的电泳沉积-激光熔覆复合加工方法,首先采用电泳沉积的方法在牙科纯钛及钛合金表面沉积一定厚度的瓷层,然后采用激光熔覆的方式将瓷层熔覆到牙科纯钛及钛合金上,从而制备出牙科纯钛及钛合金烤瓷义齿,此方法可解决烤瓷义齿加工过度依赖人工涂覆、重复性差的缺点。
发明内容
针对现有技术的不足,本发明的目的是提供一种钛烤瓷义齿的电泳沉积-激光熔覆复合加工方法,该加工方法操作方便、工艺过程易于控制;料液可循环利用,无污染物排放;所需设备简单、工艺成本低,可连续生产。
为解决现有技术问题,本发明采取的技术方案:
一种钛烤瓷义齿的电泳沉积-激光熔覆复合加工方法,采用电泳在牙科纯钛及钛合金基底材料表面沉积瓷层,然后采用激光熔覆将瓷层熔覆到牙科纯钛及钛合金上,即得牙科纯钛及钛合金烤瓷义齿。
作为改进的是,所述钛合金基底材料是Ti6Al4V合金。
作为改进的是,所述电泳在牙科纯钛及钛合金基底材料表面沉积瓷层中用的阳极是经过喷砂预处理的牙科纯钛及钛合金基底材料,阴极是铂片或石墨电极,电泳液体是烤瓷粉加入到有机溶剂和水混合的分散介质中,并添加三乙醇胺后,超声波振荡制备成悬浮液,电压为5V~100V,时间为30秒钟~30分钟,电极间距为1 cm~5 cm。
作为改进的是,所述的烤瓷粉为维他钛瓷粉、则武钛瓷粉、登士柏或钛瓷粉,烤瓷粉在分散介质中的浓度为3g/L~200g/L;三乙醇胺在分散介质中的浓度为1g/L~20g/L。
作为改进的是,所述有机溶剂和水的体积比为5:95~95:5;所述有机溶剂为乙醇、甲醇、丙酮、丙醇或异丙醇。
作为改进的是,所述的激光熔覆的工艺参数为:激光功率50-500 W,扫描速度5-100 mm/min,离焦量0-15 mm,扫描间距0.1-0.5 mm。
有益效果
本发明加工方法操作方便、工艺过程易于控制;料液可循环利用,无污染物排放;所需设备简单、工艺成本低,可连续生产,实现烤瓷义齿的规模生产。
具体实施方式
下面通过实施例详述本发明。
实施例1
.将70mL的乙醇和30mL水进行混合,分别加入0.5g的三乙醇胺和2.0g的维他(Vita Titankeramik)钛瓷粉进行分散,经磁力搅拌、超声波振荡制备成悬浮液。
.牙科纯钛基底冠用砂纸打磨并经过喷砂预处理后,用丙酮、去离子水、乙醇分别超声清洗,干燥备用。在电泳沉积体系中牙科纯钛及钛合金基底冠作为阳极,铂片电极为阴极,电泳沉积电压60V,电极间的距离2 cm,电泳沉积时间15分钟。待沉积完毕后,取出试样置于电热鼓风干燥箱中,于60℃干燥8h。
III、采用激光熔覆将瓷层熔覆到牙科纯钛及钛合金基底上,即得牙科纯钛及钛合金烤瓷义齿,其中,激光熔覆的具体工艺参数为:激光功率150 W,扫描速度25 mm/min,离焦量5 mm,扫描间距0.2 mm。
实施例2
.将60mL的甲醇和40mL水进行混合,分别加入0.3g的三乙醇胺和1.5g的则武(Super Porcelain Ti-22)瓷粉进行分散,经磁力搅拌、超声波振荡制备成悬浮液。
.牙科钛合金基底冠用砂纸打磨并经过喷砂预处理后,用丙酮、去离子水、乙醇分别超声清洗,干燥备用。在电泳沉积体系中牙科钛钼合金基底冠作为阳极,铂片电极为阴极,电泳沉积电压80V,电极间的距离3 cm,电泳沉积时间20分钟。待沉积完毕后,取出试样置于电热鼓风干燥箱中,于60℃干燥8h。
III、采用激光熔覆的方法将瓷层熔覆到牙科纯钛及钛合金上,即得牙科纯钛及钛合金烤瓷义齿,其中,激光熔覆的具体工艺参数为:激光功率100 W,扫描速度20 mm/min,离焦量7 mm,扫描间距0.15 mm。
实施例3
.将50mL的丙醇和50mL水进行混合,分别加入0.8g的三乙醇胺和3.0g的登士柏(Dentsply,Tibond)钛瓷粉进行分散,经磁力搅拌、超声波振荡制备成悬浮液。
.牙科钛钨合金基底冠用砂纸打磨并经过喷砂预处理后,用丙酮、去离子水、乙醇分别超声清洗,干燥备用。在电泳沉积体系中牙科钛钨合金基底冠作为阳极,铂片或石墨电极为阴极,电泳沉积电压30V,电极间的距离1 cm,电泳沉积时间10分钟。待沉积完毕后,取出试样置于电热鼓风干燥箱中,于60℃干燥8h。
III、采用激光熔覆的方法将瓷层熔覆到牙科纯钛及钛合金上,即得牙科纯钛及钛合金烤瓷义齿,其中,激光熔覆的具体工艺参数为:激光功率80 W,扫描速度15 mm/min,离焦量8 mm,扫描间距0.1 mm。
实施例4
.将40mL的丙酮和60mL水进行混合,分别加入1.2 g的三乙醇胺和5.0g的维他(Vita Titankeramik)钛瓷粉进行分散,经磁力搅拌、超声波振荡制备成悬浮液。
.牙科纯钛及钛合金基底冠用砂纸打磨并经过喷砂预处理后,用丙酮、去离子水、乙醇分别超声清洗,干燥备用。在电泳沉积体系中牙科纯钛及钛合金基底冠作为阳极,铂片电极为阴极,电泳沉积电压60V,电极间的距离1.5 cm,电泳沉积时间12分钟。待沉积完毕后,取出试样置于电热鼓风干燥箱中,于60℃干燥8h。
III、采用激光熔覆的方法将瓷层熔覆到牙科纯钛及钛合金上,即得牙科纯钛及钛合金烤瓷义齿,其中,激光熔覆的具体工艺参数为:激光功率240 W,扫描速度35 mm/min,离焦量10 mm,扫描间距0.3 mm。
实施例5
.将30mL的异丙醇和70mL水进行混合,分别加入1.8g的三乙醇胺和10.0g的则武(Super Porcelain Ti-22)进行分散,经磁力搅拌、超声波振荡制备成悬浮液。
.牙科钛钼合金基底冠用砂纸打磨并经过喷砂预处理后,用丙酮、去离子水、乙醇分别超声清洗,干燥备用。在电泳沉积体系中牙科钛钼合金基底冠作为阳极,铂片电极为阴极,电泳沉积电压20V,电极间的距离1.5 cm,电泳沉积时间15分钟。待沉积完毕后,取出试样置于电热鼓风干燥箱中,于60℃干燥8h。
III、采用激光熔覆的方法将瓷层熔覆到牙科纯钛及钛合金上,即得牙科纯钛及钛合金烤瓷义齿,其中,激光熔覆的具体工艺参数为:激光功率360 W,扫描速度50 mm/min,离焦量15 mm,扫描间距0.2 mm.
实施例6
.将20mL的乙醇和80mL水进行混合,分别加入0.6g的三乙醇胺和4.0g的登士柏(Dentsply,Tibond)钛瓷粉进行分散,经磁力搅拌、超声波振荡制备成悬浮液。
.牙科纯钛及钛合金基底冠瓷粉用砂纸打磨并经过喷砂预处理后,用丙酮、去离子水、乙醇分别超声清洗,干燥备用。在电泳沉积体系中牙科纯钛及钛合金基底冠作为阳极,铂片电极为阴极,电泳沉积电压20V,电极间的距离1cm,电泳沉积时间20分钟。待沉积完毕后,取出试样置于电热鼓风干燥箱中,于60℃干燥8h。
III、采用激光熔覆的方法将瓷层熔覆到牙科纯钛及钛合金上,即得牙科纯钛及钛合金烤瓷义齿,其中,激光熔覆的具体工艺参数为:激光功率400 W,扫描速度60 mm/min,离焦量15 mm,扫描间距0.15 mm。
Claims (4)
1.一种钛烤瓷义齿的电泳沉积-激光熔覆复合加工方法,其特征在于:采用电泳在牙科纯钛及钛合金基底材料表面沉积瓷层,然后采用激光熔覆将瓷层熔覆到牙科纯钛及钛合金上,即得牙科纯钛及钛合金烤瓷义齿;具体步骤如下:步骤1,将烤瓷粉加入有机溶剂和水混合的分散介质中,并添加三乙醇胺,超声波振荡制成的悬浮液;步骤2,牙科纯钛及钛合金基底材料经过喷砂预处理后,用丙酮、去离子水、乙醇分别超声清洗,干燥备用,再通过电泳反应在预处理后的牙科纯钛及钛合金基底材料上沉积瓷层,阴极为铂片电极;步骤3,采用激光熔覆的方法,将瓷层熔覆到牙科纯钛及钛合金上,即得钛烤瓷义齿;步骤2中所述电泳沉积电压为5~100V;电泳沉积时间为10min、12min、15min或20min;电极间距为1 ~ 5 cm;所述钛合金基底材料是Ti6Al4V合金;所述烤瓷粉为维他钛瓷粉、则武钛瓷粉、登士柏钛瓷粉中的任一种。
2.根据权利要求1所述的钛烤瓷义齿的电泳沉积-激光熔覆复合加工方法,其特征在于,步骤1中所述烤瓷粉在分散介质中的浓度为3~200g/L,所述三乙醇胺在分散介质中的浓度为1~20g/L。
3.根据权利要求1所述的钛烤瓷义齿的电泳沉积-激光熔覆复合加工方法,其特征在于,有机溶剂和水的体积比为5:95 ~95:5,所述有机溶剂为乙醇、甲醇、丙酮、丙醇或异丙醇中任一种。
4.根据权利要求1所述的钛烤瓷义齿的电泳沉积-激光熔覆复合加工方法,其特征在于,步骤3中所述的激光熔覆的具体工艺参数为:激光功率50-500W,扫描速度5-100mm/min,离焦量0-8或15mm,扫描间距0.1-0.5mm。
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