CN107175747B - 强度、颜色均匀过渡的牙科氧化锆修复材料及其制备方法 - Google Patents
强度、颜色均匀过渡的牙科氧化锆修复材料及其制备方法 Download PDFInfo
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 158
- 239000000463 material Substances 0.000 title claims abstract description 36
- 230000008439 repair process Effects 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000007704 transition Effects 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 57
- 238000003825 pressing Methods 0.000 claims abstract description 29
- 238000005520 cutting process Methods 0.000 claims abstract description 22
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 235000015895 biscuits Nutrition 0.000 claims abstract description 7
- 239000000919 ceramic Substances 0.000 claims description 32
- 238000004040 coloring Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000011960 computer-aided design Methods 0.000 claims description 5
- 229910052573 porcelain Inorganic materials 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims 1
- 238000005299 abrasion Methods 0.000 abstract description 7
- 238000000748 compression moulding Methods 0.000 abstract description 2
- 239000003086 colorant Substances 0.000 description 8
- 230000001055 chewing effect Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000033001 locomotion Effects 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000011351 dental ceramic Substances 0.000 description 1
- 210000004268 dentin Anatomy 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
本申请公开了一种强度、颜色均匀过渡的牙科氧化锆修复材料及其制备方法,该制备方法包括以下步骤:(1)按照每层强度由高到低,颜色由深到浅的顺序将着色氧化锆粉体倒进干压模具中干压成型;(2)干压成型后再进行冷等静压成型;(3)冷等静压成型后进行预烧结,得到素胚;(4)对素胚采用CAD/CAM切削加工,最后进行终烧结,得到牙科氧化锆修复材料。本发明采用多种不同强度的着色氧化锆粉体分层压制成型,制备强度、颜色均匀过渡的牙科氧化锆修复材料,可使修复体自切端到颈部强度逐渐增加,减小了对邻牙和对颌牙的磨损,而且颈部强度高可以做长桥修复。
Description
技术领域
本公开一般涉及牙科领域,具体涉及强度、颜色均匀过渡的牙科氧化锆修复材料及其制备方法。
背景技术
陶瓷材料凭借优秀的仿真美观效果和生物相容性,成为替代天然牙硬组织的主要材料之一,其中氧化锆陶瓷是目前最受青睐的选择,随着牙科氧化锆材料制备工艺的提高,其透明度,颜色等性能已经达到美观需求,然而由于氧化锆的基本力学参数与天然牙之间有很大的差异,特别是硬度和弹性模量明显大于牙釉质,氧化锆陶瓷修复体与天然牙在咀嚼运动的过程中,产生摩擦磨损,过度的磨损可能造成天然牙损伤。天然牙的磨耗是一个自然过程,但是天然牙的过度磨损可以引起机体自身器官的损伤。因此减少在使用过程中氧化锆修复体对天然牙的磨损是临床应用中迫切需要解决的问题。
中国专利申请公布号为CN 105622096A,名称为“彩色渐变氧化锆材料及其制备方法”的专利,涉及的氧化锆材料包括底层、中间层和外层三层结构,所述的制备方法是将纳米氧化锆粉体、氧化铁、氧化铒分别按不同的配比进行混合,然后依次将其置于模腔的不同位置,经干压成型、冷等静压成型、预烧结、切削和二次烧结,得到彩色渐变氧化锆材料。
中国专利申请公布号为CN 104844200A,名称为“多种氧化物掺杂的渐变色氧化锆牙科修复体及其制备方法”,其由三种牙科氧化锆陶瓷混合粉体ABC中的一种以上与粉体D在各个瓷层按不同质量分数混合再叠加而成,三种混合粉体分别为ErO2、CeO2、Fe2O3掺杂氧化锆瓷粉原料,粉体D为无掺杂氧化锆瓷粉原料
申请公布号为CN 105584161A,名称为“透光性渐变彩色氧化锆材料及其制备工艺”,涉及一种透光性渐变彩色氧化锆材料及其制备工艺,属于牙科用陶瓷材料技术领域。所述的透光性渐变彩色氧化锆材料,包括由下而上依次设置的底层、中间层A、中间层B、中间层C和上层五层结构,分别由3Y-TZP、(3.5~4.5)Y-PSZ及(4.5~6)Y-PSZ三种粉料与着色剂按不同的质量配比制备而成。
现有技术中基本都是对氧化锆的颜色和透度进行研究,虽然提高了氧化锆牙科修复体材料的美观性能,但却忽视了氧化锆牙科修复体在咀嚼运动的过程中,对邻牙及对颌牙损伤的问题。
发明内容
鉴于现有技术中的上述缺陷或不足,期望提供一种在咀嚼运动的过程中,减少对邻牙及对颌牙损伤的强度、颜色均匀过渡的牙科氧化锆修复材料及其制备方法。
为了实现上述目的,本发明采取的技术方案是:
一种强度、颜色均匀过渡的牙科氧化锆修复材料的制备方法,包括以下步骤:
(1)按照每层强度由高到低,颜色由深到浅的顺序将着色氧化锆粉体倒进干压模具中干压成型;
(2)干压成型后再进行冷等静压成型;
(3)冷等静压成型后进行预烧结,得到素胚;
(4)对素胚采用CAD/CAM切削加工,最后中进行终烧结,得到牙科氧化锆修复材料;
第一瓷层选用的着色氧化锆粉体强度为300-800MPa;相邻两瓷层的着色氧化锆粉体强度差为20-200MPa,所述牙科氧化锆修复材料自切端到颈部强度逐渐增加,颜色自切端到颈部逐渐加深;
每种强度的着色氧化锆粉体均包含满足国际比色标准VITA16色比色板颜色的A、B、C和D四个色系;其中,A色系颜色范围为A0.1-A4,B色系颜色范围为B0.1-B4,C色系颜色范围为C0.1-C4,D色系颜色范围为D0.1-D4;当其中一瓷层的色系确定后,其余瓷层将选用此色系并遵循颜色自切端到颈部逐渐加深的规律。
本发明还提供一种按照上述的制备方法制备得到的强度、颜色均匀过渡的牙科氧化锆修复材料。
与现有技术相比,本发明的有益效果是:
本发明采用多种不同强度的着色氧化锆粉体分层压制成型,制备强度、颜色均匀过渡的牙科氧化锆修复材料,可使修复体自切端到颈部强度逐渐增加,减小了对邻牙和对颌牙的磨损,而且颈部强度高可以做长桥修复。另外,颜色上也实现了自切端到颈部逐渐加深,均匀过渡,使修复体颜色更加的接近天然牙,本发明中尤其阐述了满足国际比色标准VITA16色比色板颜色的具体配色方法。
具体实施方式
下面结合实施例对本申请作进一步的详细说明。可以理解的是,此处所描述的具体实施例仅仅用于解释相关发明,而非对该发明的限定。
需要说明的是,在不冲突的情况下,本申请中的实施例及实施例中的特征可以相互组合。
本发明提供一种强度、颜色均匀过渡的牙科氧化锆修复材料的制备方法,包括以下步骤:
(1)按照每层强度由高到低,颜色由深到浅的顺序将着色氧化锆粉体倒进干压模具中干压成型;
(2)干压成型后再进行冷等静压成型;
(3)冷等静压成型后进行预烧结,得到素胚;
(4)对素胚采用CAD/CAM(计算机辅助设计/计算机辅助制造)切削加工,最后中进行终烧结,得到牙科氧化锆修复材料。
本发明不仅可以满足临床上对氧化锆修复体颜色的要求,而且其颈部到切端强度逐渐降低,可大大减少咀嚼运动过程中对邻牙及对颌牙的损伤,使氧化锆修复体在力学性能和颜色上更好的匹配天然牙。
优选地,牙科氧化锆修复材料的瓷层数为6-8层。
层数越多,相邻两层的颜色差值越小,修复体颜色过渡越自然,但是层数越多对生产技术的要求越高,本发明在综合两方面因素的情况下,选择6-8层的层数范围,即保证了颜色的自然过渡,又利于生产。
进一步地,当第一瓷层为切端时,所述第一瓷层选用的着色氧化锆粉体强度为300-800MPa;相邻两瓷层的着色氧化锆粉体强度差为20-200MPa,所述牙科氧化锆修复材料自切端到颈部强度逐渐增加,颜色自切端到颈部逐渐加深。
本发明可根据患者口内牙齿的磨耗情况,适当调节各瓷层的强度范围,因天然牙釉质和牙本质强度并没有很高,因此,为了与天然牙齿相匹配,修复体切端强度不需要太高,考虑有时可能需要承受很大的咬合力,可以适当的增大切端强度,因此,各瓷层合理的强度设计可以使修复体更好的模拟天然牙,在功能上也做到匹配。
本发明制备方法简单易行,制备的牙科氧化锆牙科修复体的强度分布特征大大降低了修复体对邻牙及对颌牙的磨损。
所述第一瓷层的着色氧化锆粉体的质量百分含量为15-25%,中间相邻两瓷层的着色氧化锆粉体的质量百分含量之差为0±2%,所述最后一瓷层的着色氧化锆粉体的质量百分含量为18-55%。
中间相邻两瓷层指第一瓷层和最后一瓷层之间的中间瓷层,在中间瓷层中限定每个相邻的瓷层着色氧化锆粉体的含量不同,存在0±2%的质量百分差。
本发明第一瓷层为切端,位于顶端,顶端的强度最低,可以大大降低修复体对邻牙及对颌牙的磨损,适当的增加第一层的厚度,可以使修复体颜色效果更加自然。最后一层为基底层,位于颈部,强度最高,可使修复体在咀嚼过程中承受更大的咬合力而不会发生颈缘部位折断和损坏。增大基底层的厚度,可以进一步提高修复体的疲劳寿命,对于跨度较大的长桥修复体,基底层厚度越大,修复体疲劳寿命越长。
进一步地,每种强度的着色氧化锆粉体均包含满足国际比色标准VITA16色比色板颜色的A、B、C和D四个色系;其中,A色系颜色范围为A0.1-A4,B色系颜色范围为B0.1-B4,C色系颜色范围为C0.1-C4,D色系颜色范围为D0.1-D4;当其中一瓷层的色系确定后,其余瓷层将选用此色系并遵循颜色自切端到颈部逐渐加深的规律。
参见表一,本发明A色系颜色粉体与白色氧化锆粉体按照不同的质量分数比例混合成同一色系不同颜色的粉体,按照粉体添加的比例进行颜色深浅的区分,如A色系颜色粉体添加的重质量百分含量为1%,白色氧化锆粉体的重质量百分含量为99%,颜色记为A0.1,A色系颜色粉体添加的重质量百分含量为10%,白色氧化锆粉体的重质量百分含量为90%,颜色记为A1,A色系颜色粉体添加比例为40%,颜色记为A4,A色系颜色粉体添加的重质量百分含量为15%,颜色记为A1.5。
同理,将A色系颜色粉体替换为B色系颜色粉体,通过改变B色系颜色粉体添加的质量分数,得到B色系的一系列颜色粉体,可得到B0.1-B4相同色系的不同颜色。
同理,将A色系颜色粉体替换为C色系颜色粉体,通过改变C色系颜色粉体添加的质量分数,得到C色系的一系列颜色粉体,可得到C0.1-C4相同色系的不同颜色。
同理,将A色系颜色粉体替换为D色系颜色粉体,通过改变D色系颜色粉体添加的质量分数,得到D色系的一系列颜色粉体,可得到D0.1-D4相同色系的不同颜色。
优选地,所述干压成型压力为3-15MPa,时间为5-30s。
优选地,所述冷等静压成型压力为80-270MPa,保压60-200s。
优选地,所述预烧结的温度为800-1100℃,时间为90-180min。
优选地,所述终烧结的温度为1450-1550℃,时间为60-180min。
选用本发明的上述温度和压力,可以提高修复体的致密度,提高切削加工性能,终烧结后的修复体透度高,颜色自然。
本发明还提供一种按照上述的制备方法制备得到的强度、颜色均匀过渡的牙科氧化锆修复材料。
下面通过具体实施例对本发明做进一步的说明:
实施例1
一种强度、颜色均匀过渡的牙科氧化锆修复材料的制备方法,包括以下步骤:
(1)按照每层强度由高到低,颜色由深到浅的顺序将着色氧化锆粉体倒进干压模具中干压成型,干压成型压力10MPa,压制时间15s;
(2)干压成型后再进行冷等静压成型,冷等静压成型压力180MPa,保压150s;
(3)冷等静压成型后进行预烧结,得到素胚,预烧结的温度为1000℃,时间为150min;
(4)对素胚采用CAD/CAM切削加工,最后中进行终烧结,得到牙科氧化锆修复材料,终烧结的温度为1530℃,时间为120min。
实施例2
一种强度、颜色均匀过渡的牙科氧化锆修复材料的制备方法,包括以下步骤:
(1)按照每层强度由高到低,颜色由深到浅的顺序将着色氧化锆粉体倒进干压模具中干压成型,干压成型压力15MPa,压制时间5s;
(2)干压成型后再进行冷等静压成型,冷等静压成型压力270MPa,保压60s;
(3)冷等静压成型后进行预烧结,得到素胚,预烧结的温度为800℃,时间为180min;
(4)对素胚采用CAD/CAM切削加工,最后中进行终烧结,得到牙科氧化锆修复材料,终烧结的温度为1450℃,时间为60min。
实施例3
一种强度、颜色均匀过渡的牙科氧化锆修复材料的制备方法,包括以下步骤:
(1)按照每层强度由高到低,颜色由深到浅的顺序将着色氧化锆粉体倒进干压模具中干压成型,干压成型压力3MPa,压制时间30s;
(2)干压成型后再进行冷等静压成型,冷等静压成型压力120MPa,保压200s;
(3)冷等静压成型后进行预烧结,得到素胚,预烧结的温度为1100℃,时间为60min;
(4)对素胚采用CAD/CAM切削加工,最后中进行终烧结,得到牙科氧化锆修复材料,终烧结的温度为1550℃,时间为180min。
表一 颜色标记
以下为各实施例中强度与对应颜色的关系,颜色与层数对应关系,强度与层数的对应关系,及最后强度、颜色、层数三者之间的对应关系。
表二 强度及对应颜色
表三 颜色与层数的组合关系
实施例 | 颜色以6层为例 |
实施例1 | A0.1、A0.3、A0.5、A0.6、A0.8、A1 |
实施例2 | A0.5、A0.6、A0.8、A1、A1.5、A2 |
实施例3 | A0.8、A1、A1.5、A2、A2.5、A3 |
实施例4 | A1、A1.5、A2、A2.5、A3、A3.5 |
实施例5 | A1.5、A2、A2.5、A3、A3.5、A4 |
实施例6 | B0.1、B0.3、B0.5、B0.6、B0.8、B1 |
实施例7 | B0.5、B0.6、B0.8、B1、B1.5、B2 |
实施例8 | B0.8、B1、B1.5、B2、B2.5、B3 |
实施例9 | B1.5、B2、B2.5、B3、B3.5、B4 |
实施例10 | C0.1、C0.3、C0.5、C0.6、C0.8、C1 |
实施例11 | C0.5、C0.6、C0.8、C1、C1.5、C2 |
实施例12 | C0.8、C1、C1.5、C2、C2.5、C3 |
实施例13 | C1.5、C2、C2.5、C3、C3.5、C4 |
实施例14 | D0.5、D0.6、D0.8、D1、D1.5、D2 |
实施例15 | D0.8、D1、D1.5、D2、D2.5、D3 |
实施例16 | D1.5、D2、D2.5、D3、D3.5、D4 |
表四 颜色与层数的组合关系
实施例 | 颜色以7层为例 |
实施例17 | A0.3、A0.5、A0.6、A0.8、A1、A1.5、A2 |
实施例18 | A0.6、A0.8、A1、A1.5、A2、A2.5、A3 |
实施例19 | A0.8、A1、A1.5、A2、A2.5、A3、A3.5 |
实施例20 | A1、A1.5、A2、A2.5、A3、A3.5、A4 |
实施例21 | B0.3、B0.5、B0.6、B0.8、B1、B1.5、B2 |
实施例22 | B0.6、B0.8、B1、B1.5、B2、B2.5、B3 |
实施例23 | B1、B1.5、B2、B2.5、B3、B3.5、B4 |
实施例24 | C0.1、C0.3、C0.5、C0.6、C0.8、C1 |
实施例25 | C0.3、C0.5、C0.6、C0.8、C1、C1.5、C2 |
实施例26 | C0.6、C0.8、C1、C1.5、C2、C2.5、C3 |
实施例27 | C1、C1.5、C2、C2.5、C3、C3.5、C4 |
实施例28 | D0.6、D0.8、D1、D1.5、D2、D2.5、D3 |
实施例29 | D1、D1.5、D2、D2.5、D3、D3.5、D4 |
表五 颜色与层数的组合关系
表六 强度与层数的组合关系
表七 强度与层数的组合关系
表八 强度与层数的组合关系
本发明同一实施例的每层固定强度,可以对应不同色系的颜色,比如:
表九 强度、层数、颜色结合,可以列举很多实施例,例如:
表十 强度、层数、颜色结合,可以列举很多实施例,例如:
表十一 强度、层数、颜色结合,可以列举很多实施例,例如:
表十二 层数与各层氧化锆着色粉体质量百分含量的组合关系
表十三 层数与各层氧化锆着色粉体质量百分含量的组合关系
表十四 层数与各层氧化锆着色粉体质量百分含量的组合关系
本发明实施例4-实施例41中各实施例的干压成型、冷等静压成型、预烧结与终烧结的各参数及未注明的其他参数与实施例1相同。
以上描述仅为本申请的较佳实施例以及对所运用技术原理的说明。本领域技术人员应当理解,本申请中所涉及的发明范围,并不限于上述技术特征的特定组合而成的技术方案,同时也应涵盖在不脱离所述发明构思的情况下,由上述技术特征或其等同特征进行任意组合而形成的其它技术方案。例如上述特征与本申请中公开的(但不限于)具有类似功能的技术特征进行互相替换而形成的技术方案。
Claims (8)
1.一种强度、颜色均匀过渡的牙科氧化锆修复材料的制备方法,其特征在于,包括以下步骤:
(1)按照每层强度由高到低,颜色由深到浅的顺序将着色氧化锆粉体倒进干压模具中干压成型;
(2)干压成型后再进行冷等静压成型;
(3)冷等静压成型后进行预烧结,得到素胚;
(4)对素胚采用CAD/CAM(计算机辅助设计/计算机辅助制造)切削加工,最后进行终烧结,得到牙科氧化锆修复材料;
第一瓷层选用的着色氧化锆粉体强度为300-800MPa;相邻两瓷层的着色氧化锆粉体强度差为20-200MPa,所述牙科氧化锆修复材料自切端到颈部强度逐渐增加,颜色自切端到颈部逐渐加深;
每种强度的着色氧化锆粉体均包含满足国际比色标准VITA16色比色板颜色的A、B、C和D四个色系;其中,A色系颜色范围为A0.1-A4,B色系颜色范围为B0.1-B4,C色系颜色范围为C0.1-C4,D色系颜色范围为D0.1-D4;当其中一瓷层的色系确定后,其余瓷层将选用此色系并遵循颜色自切端到颈部逐渐加深的规律。
2.根据权利要求1所述的制备方法,其特征在于,所述牙科氧化锆修复材料的瓷层数为6-8层。
3.根据权利要求2所述的制备方法,其特征在于,所述第一瓷层的着色氧化锆粉体的质量百分含量为15-25%,中间相邻两瓷层的着色氧化锆粉体的质量百分含量之差为0±2%,所述最后一瓷层的着色氧化锆粉体的质量百分含量为18-55%。
4.根据权利要求1-3任一项所述的制备方法,其特征在于,所述干压成型压力为3-15MPa,时间为5-30s。
5.根据权利要求4所述的制备方法,其特征在于,所述冷等静压成型压力为80-270MPa,保压60-200s。
6.根据权利要求5所述的制备方法,其特征在于,所述预烧结的温度为800-1100℃,时间为90-180min。
7.根据权利要求6所述的制备方法,其特征在于,所述终烧结的温度为1450-1550℃,时间为60-180min。
8.一种根据权利要求1-7任一项所述的制备方法制备得到的强度、颜色均匀过渡的牙科氧化锆修复材料。
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US20180327319A1 (en) | 2018-11-15 |
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