CN106380186A - 一种陶瓷材料的制备方法 - Google Patents

一种陶瓷材料的制备方法 Download PDF

Info

Publication number
CN106380186A
CN106380186A CN201510895338.2A CN201510895338A CN106380186A CN 106380186 A CN106380186 A CN 106380186A CN 201510895338 A CN201510895338 A CN 201510895338A CN 106380186 A CN106380186 A CN 106380186A
Authority
CN
China
Prior art keywords
preparation
ceramic material
colloid mixture
material according
zta
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510895338.2A
Other languages
English (en)
Inventor
蒋宏凯
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201510895338.2A priority Critical patent/CN106380186A/zh
Publication of CN106380186A publication Critical patent/CN106380186A/zh
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C04B35/111—Fine ceramics
    • C04B35/117—Composites
    • C04B35/119—Composites with zirconium oxide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3229—Cerium oxides or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Materials For Medical Uses (AREA)

Abstract

本发明公开了一种陶瓷材料的制备方法，通过改进粉料制备工艺，及烧结控制，引发应力诱导相变增韧改善ZTA材料的力学性能，得到的ZTA陶瓷材料耐磨性能优异，材料体积磨损率可以达到1.32×10-6 mm3/Nm，更适用于人工关节。

Description

一种陶瓷材料的制备方法
技术领域
本发明涉及一种陶瓷材料制备，具体涉及一种人工关节用ZTA陶瓷材料及其制备方法。
背景技术
人工关节是矫形外科领域在二十世纪取得的最重要的进展之一，现有的金属/金属、金属/聚乙烯、陶瓷/聚乙烯、金属/陶瓷人工关节磨损率高,会产生各种各样的磨屑，特别是聚乙烯磨屑会引起生物反应,导致骨吸收而引起移植体松动。无菌性移植体松动是矫形外科医生现在遇到的最大难题。陶瓷/陶瓷人工关节磨损率低，是一种很有希望的配对组合。目前用于人工关节的陶瓷材料主要是Al203和Y-TZP，但Al203由于强度低,撞击和应力集中会导致关节破坏，因而用于青年人的关节替换还需要进一步的改进。尽管Y-TZP的抗弯强度和断裂韧性较好，但Y-TZP的低温老化越来越引起科学家们的关注。Ce-TZP与Y-TZP相比，有更高的抗低温老化特性，对于整形外科应用Ce-TZP/Al203(ZTA)结合了氧化铝和氧化锆两者的优势，比单相具有更高的可靠性。
发明内容
为解决现有技术存在的问题，本发明提供一种人工关节用ZTA陶瓷材料的制备方法。
本发明解决其技术问题的解决方案是：一种陶瓷材料的制备方法，包括以下步骤
(1)采用共沉淀法制备Zr(OH)4和Ce(OH)4混合胶体，然后在混合胶体中添加纳米氧化铝粉料；
(2)等静压成型；
(3)常压空气气氛烧结，所述烧结温度为1300-1600℃烧结时，先常温升温至800℃，保温2h，然后在升温至1300-1600℃，保温烧成。
作为本发明技术方案的进一步改进，所述步骤1)中，混合胶体中，Ce(OH)4的含量为5-15mol％。
作为本发明技术方案的进一步改进，所述步骤1)中，所述氧化铝占氧化物总量的60-80mol％。
作为本发明技术方案的进一步改进，所述步骤1)中，所述氧化铝的平均粒度为100-500nm。
作为本发明技术方案的进一步改进，所述烧结保温时间为2-4h。
本发明的有益效果是：本发明通过改进粉料制备工艺，及烧结控制，引发应力诱导相变增韧改善ZTA材料的力学性能，得到的ZTA陶瓷材料耐磨性能优异，材料体积磨损率可以达到1.32×10-6mm3/Nm，更适用于人工关节。
具体实施方式
以下将结合实施例对本发明的构思、具体结构及产生的技术效果进行清楚、完整的描述，以充分地理解本发明的目的、特征和效果。显然，所描述的实施例只是本发明的一部分实施例，而不是全部实施例，基于本发明的实施例，本领域的技术人员在不付出创造性劳动的前提下所获得的其他实施例，均属于本发明保护的范围。
实施例1
一种陶瓷材料的制备方法，包括以下步骤
(1)配置Zr0Cl2和Ce(N03)3溶液，然后加入氨水，调节PH＝10，得到Zr(OH)4和Ce(OH)4混合胶体，水洗过滤得到混合胶体沉淀，其中Ce(OH)4的含量为7mol％，然后加入乙醇，配置浓度为30g/L的乙醇溶液，加入旋转蒸发仪，按照氧化铝摩尔百分数为氧化物总摩尔数的60％，称取平均粒径为100nm的氧化铝纳米粉体，同样配置为30g/L的乙醇溶液，加入旋转蒸发仪，旋转蒸发24h，然后过滤，80℃烘干，得到ZTA陶瓷粉料。
(2)将步骤)(1)中得到的陶瓷粉料，加入1wt％的乙二醇作为粘结剂，造粒，等静压成型得到样条。
(3)将样条在常压空气气氛烧结，首先160min升温至800℃，然后保温120min，然后80min内升温至1440℃，温4h后自然降温至室温。
实施例2
一种陶瓷材料的制备方法，包括以下步骤：
(1)配置Zr0Cl2和Ce(N03)3溶液，然后加入氨水，调节PH＝9，得到Zr(OH)4和Ce(OH)4混合胶体，水洗过滤得到混合胶体沉淀，其中Ce(OH)4的含量为11mol％，然后加入乙醇，配置浓度为25g/L的乙醇溶液，加入旋转蒸发仪，按照氧化铝摩尔百分数为氧化物总摩尔数的70％，称取平均粒径为220nm的氧化铝纳米粉体，同样配置为30g/L的乙醇溶液，加入旋转蒸发仪，旋转蒸发20h，然后过滤，80℃烘干，得到ZTA陶瓷粉料。
(2)等静压成型；将步骤)(1)中得到的陶瓷粉料，加入1wt％的乙二醇作为粘结剂，造粒，等静压成型得到样条。
(3)将样条在常压空气气氛烧结，首先160min升温至800℃，然后保温120min，然后95min内升温至1560℃，保温3h后自然降温至室温。
实施例3
一种陶瓷材料的制备方法，包括以下步骤
(1)配置Zr0Cl2和Ce(N03)3溶液，然后加入氨水，调节PH＝9，得到Zr(OH)4和Ce(OH)4混合胶体，水洗过滤得到混合胶体沉淀，其中Ce(OH)4的含量为15mol％，然后加入乙醇，配置浓度为25g/L的乙醇溶液，加入旋转蒸发仪，按照氧化铝摩尔百分数为氧化物总摩尔数的80％，称取平均粒径为500nm的氧化铝纳米粉体，同样配置为30g/L的乙醇溶液，加入旋转蒸发仪，旋转蒸发30h，然后过滤，80℃烘干，得到ZTA陶瓷粉料。
(2)将步骤)(1)中得到的陶瓷粉料，加入1wt％的乙二醇作为粘结剂，造粒，等静压成型得到样条。
(3)将样条在常压空气气氛烧结，首先160min升温至800℃，然后保温120min，然后100min内升温至1600℃，保温2h后自然降温至室温。
对上述实施1-3采用的性能测试方法如下：
(1)密度采用阿基米德排水法，室温18℃；
(2)抗弯强度采用GB/T6569-2006精细陶瓷弯曲强度试验方法；
(3)硬度采用GB/T16534-2009精细陶瓷室温硬度试验方法；
(4)耐磨性能万能摩擦磨损实验机，37℃的SBF溶液中。
测试结果见下表：
项目 实施例1 实施例2 实施例3
密度g/cm3 3.9871 4.0455 3.9308
抗弯强度MPa 414 439 390
维氏硬度GPa 15.9 17.1 16.6
耐磨性能×10-6mm3/Nm 1.74 1.32 2.86
以上对本发明的较佳实施方式进行了具体说明，但本发明创造并不限于所述实施例，熟悉本领域的技术人员在不违背本发明精神的前提下还可作出种种的等同变型或替换，这些等同的变型或替换均包含在本申请权利要求所限定的范围内。

Claims (5)

1.一种陶瓷材料的制备方法，其特征在于，包括以下步骤
1)采用共沉淀法制备Zr(OH)­4和Ce(OH)­4混合­胶体，然后在混合­胶体中添加纳米氧化铝粉料；
2)等静压成型；
3)常压空气气氛烧结，所述烧结温度为1300-1600℃。
2.根据权利要求1所述的陶瓷材料的制备方法，其特征在于：所述步骤1）中，混合胶体中，Ce（OH）4的含量为5-15mol%。
3.根据权利要求1所述的陶瓷材料的制备方法，其特征在于：所述步骤1）中，所述氧化铝占氧化物总量的60-80mol%。
4.根据权利要求1所述的陶瓷材料的制备方法，其特征在于：所述步骤1）中，所述氧化铝的平均粒度为100-500nm。
5.根据权利要求1所述的陶瓷材料的制备方法，其特征在于，所述烧结保温时间为2-4h。
CN201510895338.2A 2015-12-07 2015-12-07 一种陶瓷材料的制备方法 Pending CN106380186A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510895338.2A CN106380186A (zh) 2015-12-07 2015-12-07 一种陶瓷材料的制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510895338.2A CN106380186A (zh) 2015-12-07 2015-12-07 一种陶瓷材料的制备方法

Publications (1)

Publication Number Publication Date
CN106380186A true CN106380186A (zh) 2017-02-08

Family

ID=57916529

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510895338.2A Pending CN106380186A (zh) 2015-12-07 2015-12-07 一种陶瓷材料的制备方法

Country Status (1)

Country Link
CN (1) CN106380186A (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109987947A (zh) * 2019-04-19 2019-07-09 中国科学院上海硅酸盐研究所 利用原位应力诱导相变同步优化氧化铝涂层导热与力学性能的方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1593371A (zh) * 2004-06-28 2005-03-16 李石保 一种牙科修复体的制备方法
CN1709826A (zh) * 2005-05-30 2005-12-21 东北大学 一种Al2O3/ZrO2(Y2O3)纳米复合陶瓷刀具材料及其制备方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1593371A (zh) * 2004-06-28 2005-03-16 李石保 一种牙科修复体的制备方法
CN1709826A (zh) * 2005-05-30 2005-12-21 东北大学 一种Al2O3/ZrO2(Y2O3)纳米复合陶瓷刀具材料及其制备方法

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
李家驹主编: "《陶瓷工艺学》", 30 June 2006, 中国轻工业出版社 *
王迎军: "《生物医用陶瓷材料》", 31 October 2010, 华南理工大学出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109987947A (zh) * 2019-04-19 2019-07-09 中国科学院上海硅酸盐研究所 利用原位应力诱导相变同步优化氧化铝涂层导热与力学性能的方法

Similar Documents

Publication Publication Date Title
CN109704781A (zh) 一种氮化硅纳米带气凝胶及其制备方法
CN108530041A (zh) 一种高纯高强氧化铝陶瓷及其低温制备方法
CN101730672A (zh) 陶瓷材料
CN102286896A (zh) 一种具有净化空气功能吸附纸的制备方法
CN107986744B (zh) 一种耐高温气凝胶复合绝热毡及其制备方法
CN102503404B (zh) 一种低温烧结钙锶锂钐钛微波介质陶瓷的制备方法
CN104671826A (zh) 一种多孔氧化铝陶瓷、制备方法及其应用
CN106380186A (zh) 一种陶瓷材料的制备方法
CN103623466A (zh) 一种功能化的介孔生物玻璃多孔支架及其制备方法以及应用
CN104387112A (zh) 一种陶瓷纤维增强的陶瓷膜支撑体的制备方法
CN1284744C (zh) 堇青石和莫来石质耐热陶瓷材料
CN115838277A (zh) 一种环保抗菌日用陶瓷及其制备方法
CN1974448B (zh) 溶胶-凝胶生物活性玻璃纤维的制备方法
CN106966597B (zh) 一种用于低温烧成调湿陶瓷砖的增白釉料及其制备方法
CN115011176A (zh) 一种抗菌复合材料、其制备方法和包括其的锅具
CN104294071B (zh) 一种低温玻璃相增强的SiCp/Cu复合材料及其制备方法
CN104402516A (zh) 一种耐高温、低导热、柔性微孔硅酸钙绝热材料制备方法
CN105948700B (zh) 一种韧性高的日用陶瓷及其制备方法
CN101798214A (zh) (Na1/2Bi1/2)TiO3/BaTiO3陶瓷介质材料及其电容器的制备方法
CN108992702A (zh) 一种多孔纳米氧化物改性壳聚糖医用水凝胶敷料的制备方法
CN108212202A (zh) 浸渍挤出式分子筛脱硝催化剂及其制备方法
CN112778016A (zh) 一种牙科陶瓷材料及其制备方法和应用
CN107793138B (zh) 一种氧化铝陶瓷
Liu et al. Physicochemical properties and in vitro biocompatibility of a hydraulic calcium silicate/tricalcium aluminate cement for endodontic use
CN107129282A (zh) 一种陶瓷材料及其制备方法

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20170208

RJ01 Rejection of invention patent application after publication