CN114573332A - 一种牙科用多层色烤瓷坯体及其制备方法 - Google Patents

一种牙科用多层色烤瓷坯体及其制备方法 Download PDF

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CN114573332A
CN114573332A CN202210364065.9A CN202210364065A CN114573332A CN 114573332 A CN114573332 A CN 114573332A CN 202210364065 A CN202210364065 A CN 202210364065A CN 114573332 A CN114573332 A CN 114573332A
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田念华
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Abstract

本发明涉及一种牙科用多层色烤瓷坯体的制备方法,包括如下步骤:制备N种不同颜色的单色烤瓷粉体,N≥3;其中,每一种单色烤瓷粉体的制备过程包括:将牙本质瓷粉、半透明牙釉质瓷粉、透明牙釉质瓷粉按不同比例混合后研磨,得到某一单色烤瓷粉体;在每一种单色烤瓷粉体中加入5‑6%的纯水,搅拌呈均匀团聚状,然后两次压制得到多层色烤瓷预成型坯体;再将多层色烤瓷预成型坯体进行热处理,得到多层色烤瓷坯体。本发明的方法所制备的多层色烤瓷坯体,替代传统手工上瓷,具有渐变多层色体系。

Description

一种牙科用多层色烤瓷坯体及其制备方法
技术领域
本发明涉及牙科材料领域,特别涉及一种牙科用多层色烤瓷坯体及其制备方法。
在烤瓷牙工艺中全是手工上瓷,手工上瓷的义齿颜色层次更加丰富,透明度可高达78%,颜色通透自然,仿真度高;但是由于手工制作,导致产品质量不稳定,劳动效率低,生产成本高。
烤瓷粉是传统义齿制作的代表材料,氧化锆块则是数字化义齿制作的代表材料。用数字化替代传统工艺,是一项重大的技术革命,是对传统的颠覆。1980年代,德国著名的VITA公司发明了 In-Ceram技术,全瓷冠的强度得到了很大的提高,并很快应用于临床。现在随着材料科学和计算机技术的发展,CAD-CAM技术被应用于假牙的制作,氧化锆全瓷义齿加工已越来越普遍。氧化锆牙具有良好的韧性、可加工性、耐磨并能够阻射X线,不仅提高制作速率,还能提高义齿尺寸、细节的准确度;但是比对天然牙齿,氧化锆全瓷义齿的力学强度太高,对对应的上(下)颌有过载伤害,长期使用存在牙龈受损害的风险(氧化锆义齿强度为800-1100Mpa,人的自然牙约为50-110Mpa);其颜色通常也比较死板,切端通透感不足,切端透光率最高约49%,仿真效果较差,而且氧化锆烧制温度高(1540-1560℃),需要配置专用电炉,增加了工艺过程和生产成本。
发明内容
为解决传统手工上瓷步骤繁琐、技术要求高,而氧化锆义齿颜色死板、切端不通透、力学强度太高对自然牙造成磨损的问题,本发明提供一种牙科用多层色烤瓷坯体的制备方法,技术方案如下:
一种牙科用多层色烤瓷坯体的制备方法,其特征在于包括如下步骤:
a)制备N种不同颜色的单色烤瓷粉体,N≥3;其中,每一种单色烤瓷粉体的制备过程包括:
将牙本质瓷粉、半透明牙釉质瓷粉、透明牙釉质瓷粉按不同比例混合后研磨,得到某一单色烤瓷粉体;其中牙本质瓷粉重量百分比为20-100%,半透明牙釉质瓷粉重量百分比为0-25%、透明牙釉质瓷粉重量百分比为0-70%;
b)在每一种单色烤瓷粉体中加入5-6%的纯水,搅拌呈均匀团聚状,然后先将一种搅拌后的单色烤瓷粉体加入到压片机的干压模具中,压平后再加入另一种搅拌后的单色烤瓷粉体,直至N种不同颜色的加水搅拌后的单色烤瓷粉体全部加入到压片机的干压模具中,压制制得干压坯体;再将干压坯体放入等静压机进行坯体等静压压制得到多层色烤瓷预成型坯体,其中,压片机干压压制时压力为80-100Mpa;等静压机压制时压力为200-250MPa;
c)将步骤b)所制备的多层色烤瓷预成型坯体进行热处理,得到多层色烤瓷坯体,其中,热处理的温度为550℃-600℃;保温时间为1小时-3小时。
上述所述牙本质瓷粉的制备过程如下:将77-85%钾长石、1-4%三氧化二铝、4-8%-二氧化硅、 1-3%氧化钾、1-4%氧化钠、0.5-2%氧化钙、0.5-1%氧化锆、1-3%氧化硼混合,经二次煅烧、粉碎、球磨获得粒径200目下粉体,再进行配色制作而成,其中第一次煅烧1350℃,第二次煅烧1230℃。
上述所述半透明牙釉质瓷粉的制备过程如下:将77-85%钾长石、1-4%三氧化二铝、4-8%-二氧化硅、1-3%氧化钾、1-4%氧化钠、0.5-2%氧化钙、0.5-1%氧化锆、1-3%氧化硼混合,经二次煅烧、粉碎、球磨获得粒径200目下无色半透明粉体,其中第一次煅烧1450℃,第二次煅烧1270℃。
上述所述透明牙釉质瓷粉的制备过程如下:将77-85%钾长石、1-4%三氧化二铝、4-8%-二氧化硅、1-3%氧化钾、1-4%氧化钠、0.5-2%氧化钙、0.5-1%氧化锆、1-3%氧化硼混合,经二次煅烧、粉碎、球磨,获得粒径200目下无色透明粉体,其中第一次煅烧1490℃,第二次煅烧1300℃。
上述所述牙本质瓷粉、半透明牙釉质瓷粉、透明牙釉质瓷粉重量比为1:0:0。
上述所述步骤a)中研磨时间为1小时。
另外,本发明还提供了一种由上述方法制备的牙科用多层色烤瓷坯体。
采用本发明的方法所制备的多层色烤瓷坯体,替代传统手工上瓷,具有渐变多层色体系。本发明中所说的颜色及透明度参数,通过调整牙本质瓷粉、半透明牙釉质瓷粉、透明牙釉质瓷粉的比例, 通过调整烤瓷块的层数实现牙科修复体的颜色渐变以及透明度渐变,提高牙科修复体的柔润性、仿真度和切端通透感,同时兼顾牙科修复体所需的硬度要求以及美学要求。
本发明多层色烤瓷坯体成份为三氧化二铝(AL2O3)、二氧化硅(SiO2)、氧化钾(K2O)、氧化钠(Na2O)、氧化钙(CaO)、氧化锆(ZrO)、氧化硼(B2O3),其理化性能、生物相容性和美学效果,接近人的自然牙。
当牙本质瓷、半透明牙釉质瓷、透明牙釉质瓷重量比为1:0:0时,是义齿颈部的不透明深色部分,由颈部往切端方向,透明度逐渐增加,呈渐变效果。
本发明的制备方法不加入有机或无机化学试剂,仅加入5-6%的纯水压制后热处理进行固化,不需要排胶工序,无化学试剂残余,无有机物分解排放,与环境友好。
具体实施方式
下面将结合具体实施例对本发明的技术方案进行描述,所描述的实施例仅仅是本发明一部分实 1)施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
牙科用多层色烤瓷坯体的制备方法,包括如下步骤:
a)制备N种不同颜色的单色烤瓷粉体,N≥3;其中,每一种单色烤瓷粉体的制备过程包括:
将牙本质瓷粉、半透明牙釉质瓷粉、透明牙釉质瓷粉按不同比例混合后研磨1小时,得到某一单色烤瓷粉体;其中牙本质瓷粉重量百分比为20-100%,半透明牙釉质瓷粉重量百分比为0-25%、透明牙釉质瓷粉重量百分比为0-70%;
b)在每一种单色烤瓷粉体中加入5-6%的纯水,搅拌呈均匀团聚状,然后先将一种搅拌后的单色烤瓷粉体加入到压片机的干压模具中,压平后再加入另一种搅拌后的单色烤瓷粉体,直至N种不同颜色的加水搅拌后的单色烤瓷粉体全部加入到压片机的干压模具中压制,制得干压坯体;再将干压坯体放入等静压机进行坯体等静压压制得到多层色烤瓷预成型坯体,其中,第一次在压片机按 80-100Mpa压力下干压压制;第二次在等静压机按200-250MPa压力下等静压压制;
c)将步骤b)所制备的多层色烤瓷预成型坯体进行热处理,得到多层色烤瓷坯体,其中,热处理的温度为550-600℃;保温时间为1-3小时。
其中,N值越大,代表压制层数越多,最终制得的多层烤瓷坯体的渐变性与美学效果越好,但是相应的多层烤瓷坯体的成本也会越高;但是N值越小,则难以体现渐变的特点,而影响美学效果。实际应用中,N值的大小可以由本领域技术人员确定。
采用上述热处理方法,使得各单色烤瓷粉体在一定的温度下结合成型,提高烤瓷材料的强度,方便运输和使用。
在实际应用中,混合可以采用本领域常用的球磨机进行球磨混合。需要说明的是,本发明所用的热处理设备等均为本领域常用的设备,能实现本发明的目的即可,本发明在此不进行限定。
原料制备:
制备牙本质瓷粉:将81%钾长石、3.5%三氧化二铝、5.2%二氧化硅、2%氧化钾、3.5%氧化钠、 1.8%氧化钙、0.8%氧化锆、2.2%氧化硼混合,经二次煅烧、粉碎、球磨获得粒径200目下粉体,再进行配色制作而成,其中第一次煅烧1350℃,第二次煅烧1230℃。所述配色根据人的自然牙色来配制,按传统烤瓷粉配色方法进行制作。
制备半透明牙釉质瓷粉:将81%钾长石、3.5%三氧化二铝、5.2%二氧化硅、2%氧化钾、3.5%氧化钠、1.8%氧化钙、0.8%氧化锆、2.2%氧化硼混合,经二次煅烧、粉碎、球磨获得粒径200目下无色半透明粉体,其中第一次煅烧1450℃,第二次煅烧1270℃。
制备透明牙釉质瓷粉:将81%钾长石、3.5%三氧化二铝、5.2%二氧化硅、2%氧化钾、3.5%氧化钠、1.8%氧化钙、0.8%氧化锆、2.2%氧化硼混合,经二次煅烧、粉碎、球磨,获得粒径200目下无色透明粉体,其中第一次煅烧1490℃,第二次煅烧1300℃。
实施例1
根据表1中粉体1-6的配方,将各物料混合球磨均匀后,即可制备出6种不同颜色的单色烤瓷粉体(即粉体1-6);在每一种单色烤瓷粉体中加入5%的纯水,搅拌呈均匀团聚状,然后先将粉体1 加入到干压模具中,压平后再加入粉体2,压平后再加入粉体3,直至6种粉体全部加入到干压模具中,其中,每层粉体厚度为2mm,在80Mpa压力下进行第一次压制,在200MPa的压力下进行第二次等静压压制预成型,得到得到多层烤瓷预成型坯体;然后对多层烤瓷预成型坯体进行热处理,处理温度为550℃,保温时间为1小时,即可得到具有六层颜色渐变的多层烤瓷坯体。
表1、6种不同颜色的单色烤瓷粉体的配方及工艺参数
原料及工艺 粉体1 粉体2 粉体3 粉体4 粉体5 粉体6
牙本质瓷粉 20% 45% 65% 90% 100% 100%
半透明牙釉质瓷粉 10% 15% 25% 10% - -
透明牙釉质瓷粉 70% 40% 10% - - -
原料/磨球 1/2 1/2 1/2 1/2 1/2 1/2
球磨时间/h 1 1 1 1 1 1
注:表1中的各成份含量为重量百分比,原料/磨球为重量比。
实施例2
与实施例1区别在于在每一种单色烤瓷粉体中加入6%的纯水。
实施例3
与实施例1区别在于在100Mpa压力下进行第一次压制。
实施例4
与实施例1区别在于在250MPa的压力下进行第二次等静压压制预成型。
实施例5
与实施例1区别在于对多层烤瓷预成型坯体进行热处理,处理温度为600℃。
实施例6
与实施例1区别在于热处理保温时间为3小时。
实施例7
根据表2中粉体1-5的配方,将各物料混合球磨均匀后,即可制备出5种不同颜色的单色烤瓷粉体(即粉体1-5);在每一种单色烤瓷粉体中加入5%的纯水,搅拌呈均匀团聚状,然后先将粉体1 加入到干压模具中,压平后再加入粉体2,压平后再加入粉体3,直至5种粉体全部加入到干压模具中,其中,每层粉体厚度为2.5mm,在80Mpa压力下进行第一次压制,在200MPa的压力下进行第二次等静压压制预成型,得到得到多层烤瓷预成型坯体;然后对多层烤瓷预成型坯体进行热处理,处理温度为550℃,保温时间为1小时,即可得到具有五层颜色渐变的多层烤瓷坯体。
表2、5种不同颜色的单色烤瓷粉体的配方及工艺参数
Figure BDA0003585139620000031
Figure BDA0003585139620000041
注:表2中的各成份含量为重量百分比,原料/磨球为重量比。
实施例8
与实施例7区别在于在每一种单色烤瓷粉体中加入6%的纯水。
实施例9
与实施例7区别在于在100Mpa压力下进行第一次压制。
实施例10
与实施例7区别在于在250MPa的压力下进行第二次等静压压制预成型。
实施例11
与实施例7区别在于对多层烤瓷预成型坯体进行热处理,处理温度为600℃。
实施例12
与实施例7区别在于热处理保温时间为3小时。
力学性能测试
分别测定实施例1-12所制备的多层烤瓷坯体的挠曲强度,见表3。
表3实施例1-12制备的多层烤瓷坯体的性能
实施例 烧结后挠曲强度/MPa
1 265
2 262
3 274
4 287
5 293
6 289
7 259
8 266
9 276
10 290
11 295
12 284
其中,挠曲强度的测试方法参照GB 30367-2013(ISO 6872-2008,IDT)《牙科学-陶瓷材料》。
从表3中可以看出,本发明实施例制备的多层烤瓷坯体,力学性能优异。多层烤瓷坯体具有较高的强度、韧性。与氧化锆牙相比,可减小对对颌真牙的磨损。其无论在义齿加工、牙医佩戴、患者使用过程中,都可以保持良好的形态。
化学溶解性测试
测试实施例1-12制备的多层烤瓷坯体的化学溶解性,见表4。
表4
实施例 化学溶解性/μg·cm<sup>-2</sup>
1 26.56
2 26.47
3 26.50
4 26.41
5 26.58
6 26.39
7 26.52
8 26.68
9 26.54
10 26.38
11 26.46
12 26.44
生物相容性测试
测试实施例1-12制备的多层烤瓷坯体的生物相容性,见表5。
表5
检测项目 检验结果
体外细胞毒性测试 无细胞毒性
迟发型超敏反应最大剂量试验 致敏反应为阴性
口腔粘膜刺激试验 刺激指数为0
急性全身毒性 无急性全身毒性反应
亚慢性全身毒性 无临床全身毒性症状
遗传毒性 突变为阴性
从表4、5可以看出,实施例1-12制备的多层色烤瓷坯体化学稳定性高,生物相容性高,对人体健康无伤害。
多层色烤瓷坯体的应用包括如下步骤:1、使用数字化扫描仪扫描牙模和内冠,如果是金属冠需要上好遮色瓷,全瓷冠需要前期染色;2、将扫描件载入设计软件,设计牙冠形状;3、将牙冠文件载入排版软件,对牙冠进行模拟排位;4、在3D切削机上装载烤瓷盘;5、将排版文件导入3D切削机,进行数字化切削;6、将切削好的多层色烤瓷坯体与内冠结合。有两种结合方式选择:方式①牙冠单独烧结,后续进行戴冠操作;方式②内冠+牙冠结合烧结,一体成型。
以上对本发明所提供的一种数字化多层烤瓷坯体及其制备方法进行了详细介绍。本文中应用了具体实施例对本发明的原理及实施方式进行了阐述,以上实施例的说明只是用于帮助理解本发明的方法及其中心思想。应当指出,对于本领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求的保护。

Claims (7)

1.一种牙科用多层色烤瓷坯体的制备方法,其特征在于包括如下步骤:
a)制备N种不同颜色的单色烤瓷粉体,N≥3;其中,每一种单色烤瓷粉体的制备过程包括:
将牙本质瓷粉、半透明牙釉质瓷粉、透明牙釉质瓷粉按不同比例混合后研磨,得到某一单色烤瓷粉体;其中牙本质瓷粉重量百分比为20-100%,半透明牙釉质瓷粉重量百分比为0-25%、透明牙釉质瓷粉重量百分比为0-70%;
b)在每一种单色烤瓷粉体中加入5-6%的纯水,搅拌呈均匀团聚状,然后先将一种搅拌后的单色烤瓷粉体加入到压片机的干压模具中,压平后再加入另一种搅拌后的单色烤瓷粉体,直至N种不同颜色的加水搅拌后的单色烤瓷粉体全部加入到压片机的干压模具中,压制制得干压坯体;再将干压坯体放入等静压机进行等静压压制得到多层色烤瓷预成型坯体;其中,压片机干压压制时压力为80-100Mpa;等静压机压制时压力为200-250MPa;
c)将步骤b)所制备的多层色烤瓷预成型坯体进行热处理,得到多层色烤瓷坯体,所述热处理的温度为550℃-600℃;保温时间为1小时-3小时。
2.如权利要求1所述的牙科用多层色烤瓷坯体的制备方法,其特征在于所述牙本质瓷粉的制备过程如下:将77-85%钾长石、1-4%三氧化二铝、4-8%-二氧化硅、1-3%氧化钾、1-4%氧化钠、0.5-2%氧化钙、0.5-1%氧化锆、1-3%氧化硼混合,经二次煅烧、粉碎、球磨获得粒径200目下粉体,再进行配色制作而成,其中第一次煅烧1350℃,第二次煅烧1230℃。
3.如权利要求1所述的牙科用多层色烤瓷坯体的制备方法,其特征在于所述半透明牙釉质瓷粉的制备过程如下:将77-85%钾长石、1-4%三氧化二铝、4-8%-二氧化硅、1-3%氧化钾、1-4%氧化钠、0.5-2%氧化钙、0.5-1%氧化锆、1-3%氧化硼混合,经二次煅烧、粉碎、球磨获得粒径200目下无色半透明粉体,其中第一次煅烧1450℃,第二次煅烧1270℃。
4.如权利要求1所述的牙科用多层色烤瓷坯体的制备方法,其特征在于所述透明牙釉质瓷粉的制备过程如下:将77-85%钾长石、1-4%三氧化二铝、4-8%-二氧化硅、1-3%氧化钾、1-4%氧化钠、0.5-2%氧化钙、0.5-1%氧化锆、1-3%氧化硼混合,经二次煅烧、粉碎、球磨,获得粒径200目下无色透明粉体,其中第一次煅烧1490℃,第二次煅烧1300℃。
5.如权利要求1所述的牙科用多层色烤瓷坯体的制备方法,其特征在于:所述牙本质瓷粉、半透明牙釉质瓷粉、透明牙釉质瓷粉重量比为1:0:0。
6.如权利要求1所述的牙科用多层色烤瓷坯体的制备方法,其特征在于:所述步骤a)中研磨时间为1小时。
7.一种牙科用多层色烤瓷坯体,其特征在于:所述多层色烤烤瓷坯体由如权利要求1至6中任一所述的方法制备。
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