CN113461421B - 一种叠层氧化锆牙科陶瓷材料及其制备方法 - Google Patents
一种叠层氧化锆牙科陶瓷材料及其制备方法 Download PDFInfo
- Publication number
- CN113461421B CN113461421B CN202110867614.XA CN202110867614A CN113461421B CN 113461421 B CN113461421 B CN 113461421B CN 202110867614 A CN202110867614 A CN 202110867614A CN 113461421 B CN113461421 B CN 113461421B
- Authority
- CN
- China
- Prior art keywords
- powder
- mixture
- layer
- screening
- mass
- 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.)
- Active
Links
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical class O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000011351 dental ceramic Substances 0.000 title claims abstract description 25
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims description 120
- 239000000203 mixture Substances 0.000 claims description 56
- 238000012216 screening Methods 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000919 ceramic Substances 0.000 claims description 18
- 238000003825 pressing Methods 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 10
- 235000015895 biscuits Nutrition 0.000 claims description 8
- 238000009694 cold isostatic pressing Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000002648 laminated material Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000007873 sieving Methods 0.000 description 9
- 238000005520 cutting process Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- 238000005336 cracking Methods 0.000 description 3
- 230000032798 delamination Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000008439 repair process Effects 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
-
- 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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/15—Compositions characterised by their physical properties
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
- A61K6/818—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising zirconium oxide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B13/00—Feeding the unshaped material to moulds or apparatus for producing shaped articles; Discharging shaped articles from such moulds or apparatus
- B28B13/02—Feeding the unshaped material to moulds or apparatus for producing shaped articles
- B28B13/0215—Feeding the moulding material in measured quantities from a container or silo
- B28B13/022—Feeding several successive layers, optionally of different materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/02—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein a ram exerts pressure on the material in a moulding space; Ram heads of special form
-
- 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
-
- 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
- C04B35/62605—Treating the starting powders individually or as mixtures
-
- 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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
- C04B35/6264—Mixing media, e.g. organic solvents
-
- 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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
-
- 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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
-
- 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
- C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
-
- 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
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/604—Pressing at temperatures other than sintering temperatures
-
- 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
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
-
- 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
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/32—Ceramic
- C04B2237/34—Oxidic
- C04B2237/345—Refractory metal oxides
- C04B2237/348—Zirconia, hafnia, zirconates or hafnates
-
- 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
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/58—Forming a gradient in composition or in properties across the laminate or the joined articles
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Epidemiology (AREA)
- Mechanical Engineering (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Composite Materials (AREA)
- Dental Preparations (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Dental Prosthetics (AREA)
Abstract
本发明属于牙科陶瓷材料技术领域，本发明公开了一种叠层氧化锆牙科陶瓷材料及其制备方法，该制备方法主要内容为粉体成型之前对不同层粉体界面进行处理，通过造粒和过筛，制备出第一、第二混合物筛选粉体，将第一混合物筛选粉体平铺在下层粉体上，第二混合物筛选粉体平铺在第一混合物筛选粉体上，然后叠加上层粉体。本发明解决了叠层氧化锆牙科陶瓷界面容易开裂的问题。所得产品不仅可以用于成形盘状坯料，还可以在预备体上成形个性化形状修复体的坯料。
Description
技术领域
本发明涉及牙科陶瓷材料技术领域，更具体的说是一种叠层牙科陶瓷材料及其制备方法。
背景技术
全瓷修复技术作为牙体缺损缺失固定修复、前牙区美容修复等口腔修复学领域的治疗方式，已在临床上得到广泛应用，越来越受到医师和患者的欢迎。氧化锆陶瓷作为全瓷修复体材料，凭借其优良的理化性能、稳定的生物相容性和良好的美观修复效果，在全球迅速普及。然而，完美的修复体除了形态、大小满足要求外，还需要有与天然牙齿接近的颜色和力学性能。未着色的氧化锆陶瓷多呈现白色或象牙白，难以满足临床对修复体色彩性的要求。为了增加氧化锆陶瓷修复体的美观效果和仿生力学性能，人们发明了颜色和强度呈梯度变化的氧化锆牙科陶瓷。
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，公开的氧化锆材料包括底层、中间层和外层三层结构。制备方法为将三种不同的氧化锆粉体依次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，最终得到氧化锆牙科陶瓷材料。
中国专利申请公布号为CN 10527228A的专利公开了一种强度、颜色均匀过渡的牙科氧化锆修复材料的制备方法。该方法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，再进行冷等静压成型，随后预烧结，得到素胚，再然后对素胚进行切削加工与终烧结，得到牙科氧化锆修复材料。
目前，彩色渐变氧化锆陶瓷材料一般都涉及到叠层氧化锆陶瓷制备技术，现有的技术中基本都是对氧化锆粉体进行分层放置于磨具中再干压成型，然后进行冷等静压。由于不同层的组分存在差异，导致烧结后容易出现分层和开裂等问题，从而增大了陶瓷块体产品的废品率，造成资源浪费和经济损失。同时，又由于界面处氧化锆陶瓷的力学性能发生突变，会降低陶瓷块体整体力学特性。
因此，如何提供一种不产生分层缺陷的氧化锆牙科陶瓷材料的制备方法成为了本领域技术人员亟需解决的问题。
发明内容
有鉴于此，本发明提供了一种叠层氧化锆牙科陶瓷材料及其制备方法，此制备方法主要解决了叠层氧化锆牙科陶瓷界面容易开裂的问题。其制备出的氧化锆陶瓷材料不仅可以用于成形盘状坯料，还可以在预备体上成形个性化形状修复体的坯料。
为了达到上述目的，本发明采用如下技术方案：
本发明提供了一种叠层氧化锆牙科陶瓷材料的制备方法，该叠层材料由多层氧化锆粉体分层压制成型，包括以下步骤：
S1、分层压制时，将10份~40份上层粉体与90份~60份下层粉体混合，得到第一混合物；
S2、分层压制时，将10份~40份下层粉体与90份~60份上层粉体混合，得到第二混合物；
S3、在第一混合物中加入酒精，使粉体潮湿，然后过两层不同目数的筛子，得到通过第一层筛子而未通过第二层筛子的第一混合物筛选粉体，其中第一层筛子目数≤50目，第二层筛子目数＞50目；
S4、在第二混合物中加入酒精，使粉体潮湿，然后过两层不同目数的筛子，得到通过第一层筛子而未通过第二层筛子的第二混合物筛选粉体，其中第一层筛子目数≤50目，第二层筛子目数＞50目；
S5、将第一混合物筛选粉体平铺在下层粉体上；
S6、将第二混合物筛选粉体平铺在第一混合物筛选粉体上；
S7、待第二混合物筛选粉体干燥后，再在第二层筛选粉体层上叠加上层粉体；
S8、干压成型后，再进行冷等静压成型，预烧结后得到素坯，对素坯进行终烧结后得到氧化锆陶瓷块体。
作为优选，所述步骤S1中将20份上层粉体与80份下层粉体混合，得到第一混合物；
作为优选，所述步骤S2中将20份下层粉体与80份上层粉体混合，得到第二混合物；
作为优选，所述步骤S3中采用喷雾法在第一混合物中加入酒精，酒精的加入量为混合物粉体质量的2%~4%；进一步优选，酒精的加入量为混合物粉体质量的3%；
作为优选，所述步骤S3中的第一层筛子的目数为30目，第二层筛的目数为200目；
作为优选，所述步骤S4中采用喷雾法在第二混合物中加入酒精，酒精的加入量为混合物粉体质量的2%~4%；进一步优选，酒精的加入量为混合物粉体质量的3%；
作为优选，所述步骤S4中的第一层筛子的目数为30目，第二层筛的目数为200目；
作为优选，所述步骤S5中的第一混合物筛选粉体的质量为下层粉体质量的2%~9%；
作为优选，所述步骤S6中的第二混合物筛选粉体的质量为上层粉体质量的2%~9%。
本发明还提供了一种按照上述叠层氧化锆牙科陶瓷材料的制备方法制备得到的叠层氧化锆牙科陶瓷材料。
本发明所应用的原理为：采用酒精加入粉体的目的是为了造粒。潮湿的粉体，经过两次过筛，得到粒径均匀的大颗粒粉体，通常情况下，其粒径均大于上下两层氧化锆粉体的粒径。经过筛选后，颗粒较大的第一混合物粉体和第二混合物粉体在后续的干压成型和冷等静压过程中，由于颗粒之间存在间隙，粉体能够彼此嵌合，且有少量的上下层粉体渗入，从而达到生成连续梯度界面的效果。
经由上述的技术方案可知，与现有技术相比，本发明的有益效果如下：
本发明通过改善界面处粉体成分分布，制备出连续梯度界面层，实现叠层氧化锆牙科陶瓷内部颜色和力学性能连续渐变，解决了叠层氧化锆牙科陶瓷界面容易开裂的问题。本发明不仅可以用于成形盘状坯料，还可以在预备体上成形个性化形状修复体的坯料，能够提高产品质量，增加经济效益。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据提供的附图获得其他的附图。
图1 附图为实施例1中得到的叠层氧化锆牙科陶瓷块切削后图片；
图2 附图为实施例2中得到的叠层氧化锆牙科陶瓷试样切削后图片；
图3 附图为实施例2中得到的叠层氧化锆牙科陶瓷试样切削后图片。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，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做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。
实施例1
2021年6月上旬，在秦皇岛某厂的三层氧化锆牙科陶瓷制备过程中，按照物理空间分为下、中、上三层，先将下层粉体放置在模型中，将10份中层粉体与90份下层粉体混合，得到混合物A1，将10下层粉体与90份中层粉体混合，得到混合物A2，采用喷雾法分别在A1和A2混合物中加入酒精，酒精质量分别为相应粉体质量的2%，混合均匀后，分别过筛30目和100目筛子，取两筛之间的粉体，得到A1筛选粉体和A2筛选粉体。称取A1筛选粉体的质量为模型组下层粉体总质量的2%，A2筛选粉体为中层粉体总质量的2%。将A1和A2筛选粉体依次平铺在下层粉体之上。静置一段时间，待粉体干燥后，再将中层粉体放在A2粉体层上。随后将10份上层粉体与90份中层粉体混合，得到混合物B1，将10中层粉体与90份上层粉体混合，得到混合物B2，采用喷雾法分别在B1和B2混合物中加入酒精，混合均匀后，分别过筛30目和100目筛子，取两筛之间的粉体，得到B1筛选粉体和B2筛选粉体。称取B1筛选粉体的质量为模型组下层粉体总质量的2%，B2筛选粉体为中层粉体总质量的2%。将B1和B2筛选粉体依次平铺在中层粉体之上。静置一段时间，待粉体干燥后，再将上层粉体放在B2粉体层上。干压成型后，再进行冷等静压成型，预烧结后得到素坯，对素坯进行终烧结后得到氧化锆陶瓷块体。随后，对陶瓷块体进行切削加工后，切削后照片如图1所示，从图中可以看出瓷块内未发现分层和开裂。
实施例2
2021年6月中旬，在秦皇岛某企业的六四层氧化锆牙科陶瓷制备过程中，按照物理空间分为一、二、三、四、五、六层，每两层之间，按照物理空间将20份上层粉体与80份下层粉体混合，得到混合物A1，将20下层粉体与80份上层粉体混合，得到混合物A2，采用喷雾法分别在A1和A2混合物中加入酒精，酒精添加量为相应粉体质量的3%，混合均匀后，分别过筛40目和120目筛子，取两筛之间的粉体，得到A1筛选粉体和A2筛选粉体。称取A1筛选粉体的质量为模型组下层粉体总质量的5%，A2筛选粉体为中层粉体总质量的5%。将A1和A2筛选粉体依次平铺在第一层粉体之上。静置一段时间，待粉体干燥后，再将第二层粉体放在A2粉体层上。六层粉体叠加完成后，干压成型，再进行冷等静压成型，预烧结后得到素坯，对素坯进行终烧结后得到氧化锆陶瓷块体。然后对陶瓷块体进行切削加工，切削后的试样如图2、图3所示，由图中可以看出该样品内部没有出现分层和开裂，表明该发明具有实用性。
Claims (2)
1.一种叠层氧化锆牙科陶瓷材料的制备方法，该叠层材料由多层氧化锆粉体分层压制成型，其特征在于，包括以下步骤：
S1、分层压制时，将10份～40份上层粉体与90份～60份下层粉体混合，得到第一混合物；
S2、分层压制时，将10份～40份下层粉体与90份～60份上层粉体混合，得到第二混合物；
S3、在第一混合物中加入酒精，然后过两层不同目数的筛子，得到通过第一层筛子而未通过第二层筛子的第一混合物筛选粉体，其中第一层筛子目数≤50目，第二层筛子目数＞50目；
S4、在第二混合物中加入酒精，然后过两层不同目数的筛子，得到通过第一层筛子而未通过第二层筛子的第二混合物筛选粉体，其中第一层筛子目数≤50目，第二层筛子目数＞50目；
S5、将第一混合物筛选粉体平铺在下层粉体上；
S6、将第二混合物筛选粉体平铺在第一混合物筛选粉体上；
S7、待第二混合物筛选粉体干燥后，再在第二混合物筛选粉体上叠加上层粉体；
S8、干压成型后，再进行冷等静压成型，预烧结后得到素坯，对素坯进行终烧结后得到氧化锆陶瓷块体；
所述步骤S3中在第一混合物中加入酒精的量为混合物粉体质量的1％～5％；
所述步骤S4中在第二混合物中加入酒精的量为混合物粉体质量的1％～5％；
所述第一混合物和第二混合物中的上层粉体与下层粉体以总质量100份计算；
所述步骤S5中的第一混合物筛选粉体的质量为下层粉体质量的1％～10％；
所述步骤S6中的第二混合物筛选粉体的质量为上层粉体质量的1％～10％。
2.权利要求1所述的叠层氧化锆牙科陶瓷材料的制备方法制备得到的叠层氧化锆牙科陶瓷材料。
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110867614.XA CN113461421B (zh) | 2021-07-30 | 2021-07-30 | 一种叠层氧化锆牙科陶瓷材料及其制备方法 |
| PCT/CN2022/097518 WO2023005435A1 (zh) | 2021-07-30 | 2022-06-08 | 一种叠层氧化锆牙科陶瓷材料及其制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110867614.XA CN113461421B (zh) | 2021-07-30 | 2021-07-30 | 一种叠层氧化锆牙科陶瓷材料及其制备方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113461421A CN113461421A (zh) | 2021-10-01 |
| CN113461421B true CN113461421B (zh) | 2022-02-01 |
Family
ID=77883311
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110867614.XA Active CN113461421B (zh) | 2021-07-30 | 2021-07-30 | 一种叠层氧化锆牙科陶瓷材料及其制备方法 |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN113461421B (zh) |
| WO (1) | WO2023005435A1 (zh) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113461421B (zh) * | 2021-07-30 | 2022-02-01 | 北京大学口腔医学院 | 一种叠层氧化锆牙科陶瓷材料及其制备方法 |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058655A (zh) * | 2013-01-18 | 2013-04-24 | 秦皇岛爱迪特高技术陶瓷有限公司 | 一种梯度透明性氧化锆牙科陶瓷及其制备方法 |
| CN103641472A (zh) * | 2013-11-14 | 2014-03-19 | 厦门惠方生物科技有限公司 | 一种制备着色半透性氧化锆预烧结体的方法 |
| CN104844200A (zh) * | 2015-04-30 | 2015-08-19 | 浙江大学 | 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 |
| CN105272228A (zh) * | 2015-11-23 | 2016-01-27 | 秦皇岛爱迪特高技术陶瓷有限公司 | 着色氧化锆粉体以及多层多色牙科陶瓷的制备方法 |
| CN105541325A (zh) * | 2015-12-22 | 2016-05-04 | 山东新华医疗器械股份有限公司 | 透光性渐变氧化锆材料及其制备方法 |
| CN105584161A (zh) * | 2015-12-22 | 2016-05-18 | 山东新华医疗器械股份有限公司 | 透光性渐变彩色氧化锆材料及其制备工艺 |
| CN105622096A (zh) * | 2015-12-22 | 2016-06-01 | 山东新华医疗器械股份有限公司 | 彩色渐变氧化锆材料及其制备方法 |
| CN109771064A (zh) * | 2019-02-27 | 2019-05-21 | 深圳市翔通光电技术有限公司 | 一种强度、透性及颜色逐层变化的义齿及其制备方法 |
| CN111348911A (zh) * | 2020-03-10 | 2020-06-30 | 上海美达义齿制作有限公司 | 一种多层透度、多层强度义齿的制备工艺 |
| WO2020178712A1 (en) * | 2019-03-04 | 2020-09-10 | 3M Innovative Properties Company | Process for producing a colored dental zirconia article |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107175747B (zh) * | 2017-05-12 | 2020-04-07 | 爱迪特（秦皇岛）科技股份有限公司 | 强度、颜色均匀过渡的牙科氧化锆修复材料及其制备方法 |
| CN108618969A (zh) * | 2018-02-06 | 2018-10-09 | 北京大学口腔医学院 | 一种仿生陶瓷牙修复体的制作方法 |
| KR102158619B1 (ko) * | 2018-08-31 | 2020-09-25 | 대전대학교 산학협력단 | 전기화학식 산소발생기를 위한 산화물 전극이 도포된 고체전해질 멤브레인 및 이의 제조방법 |
| WO2021023791A1 (de) * | 2019-08-08 | 2021-02-11 | Vita Zahnfabrik H. Rauter Gmbh & Co. Kg | Zirkondioxidrohling mit farb- und transluzenzverlauf |
| CN113461421B (zh) * | 2021-07-30 | 2022-02-01 | 北京大学口腔医学院 | 一种叠层氧化锆牙科陶瓷材料及其制备方法 |
-
2021
- 2021-07-30 CN CN202110867614.XA patent/CN113461421B/zh active Active
-
2022
- 2022-06-08 WO PCT/CN2022/097518 patent/WO2023005435A1/zh active Application Filing
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058655A (zh) * | 2013-01-18 | 2013-04-24 | 秦皇岛爱迪特高技术陶瓷有限公司 | 一种梯度透明性氧化锆牙科陶瓷及其制备方法 |
| CN103641472A (zh) * | 2013-11-14 | 2014-03-19 | 厦门惠方生物科技有限公司 | 一种制备着色半透性氧化锆预烧结体的方法 |
| CN104844200A (zh) * | 2015-04-30 | 2015-08-19 | 浙江大学 | 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 |
| CN105272228A (zh) * | 2015-11-23 | 2016-01-27 | 秦皇岛爱迪特高技术陶瓷有限公司 | 着色氧化锆粉体以及多层多色牙科陶瓷的制备方法 |
| CN105541325A (zh) * | 2015-12-22 | 2016-05-04 | 山东新华医疗器械股份有限公司 | 透光性渐变氧化锆材料及其制备方法 |
| CN105584161A (zh) * | 2015-12-22 | 2016-05-18 | 山东新华医疗器械股份有限公司 | 透光性渐变彩色氧化锆材料及其制备工艺 |
| CN105622096A (zh) * | 2015-12-22 | 2016-06-01 | 山东新华医疗器械股份有限公司 | 彩色渐变氧化锆材料及其制备方法 |
| CN109771064A (zh) * | 2019-02-27 | 2019-05-21 | 深圳市翔通光电技术有限公司 | 一种强度、透性及颜色逐层变化的义齿及其制备方法 |
| WO2020178712A1 (en) * | 2019-03-04 | 2020-09-10 | 3M Innovative Properties Company | Process for producing a colored dental zirconia article |
| CN111348911A (zh) * | 2020-03-10 | 2020-06-30 | 上海美达义齿制作有限公司 | 一种多层透度、多层强度义齿的制备工艺 |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2023005435A1 (zh) | 2023-02-02 |
| CN113461421A (zh) | 2021-10-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107175747B (zh) | 强度、颜色均匀过渡的牙科氧化锆修复材料及其制备方法 | |
| CN109414309B (zh) | 制造着色坯体的方法以及坯体 | |
| US10391671B2 (en) | Process for producing a non-dense sintered ceramic molded body having at least two layers | |
| JP5117107B2 (ja) | ブロック部材 | |
| DE60303964T2 (de) | Verstärkte keramikrestauration | |
| CN108697493B (zh) | 用于生产牙科修复体的方法 | |
| EP2313023B1 (de) | Formkörper aus formstabilisiertem material und verfahren zu seiner herstellung | |
| CN108495598A (zh) | 用于生产坯料的方法、坯料和牙科修复体 | |
| CN102285795A (zh) | 牙科复色可切削氧化锆陶瓷及制备方法 | |
| US20130180110A1 (en) | Methods for making layered dental appliances | |
| US20080064011A1 (en) | Multi-colored shaped body | |
| JP2004035332A (ja) | セラミックスブロック | |
| AU2002306555B2 (en) | Method for manufacturing a dental restoration | |
| EP2616001B1 (en) | A method of making a dental restoration | |
| WO2013127931A1 (de) | Rohling für die herstellung von zahnersatz | |
| US20160120765A1 (en) | Zirconia Dental Articles and Methods Thereof | |
| CN113461421B (zh) | 一种叠层氧化锆牙科陶瓷材料及其制备方法 | |
| KR101221026B1 (ko) | 크라운 제조방법 및 이를 이용한 크라운 | |
| DE19814762A1 (de) | Verfahren zur Herstellung von Zahnersatz unter Verwendung von Vorformen | |
| EP3900668B1 (en) | Zirconia sintered body | |
| EP4167900A2 (en) | Dental components | |
| CN112972033B (zh) | 一种义齿及其制备方法 | |
| EP3977960B1 (en) | Multi-layered zirconia dental blank with reverse layers, process for its preparation and uses thereof | |
| DE112021005253T5 (de) | Mehrschichtiger Zirkonoxid-Rohling zur zahntechnischen Verwendung mit Umkehrschichten, Verfahren zu seiner Herstellung und seine Verwendung | |
| UA112008U (uk) | Процес виготовлення цирконієвих коронок зі стабілізованого ітрієм оксиду цирконію |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240625 Address after: 066004 9 Qinhuangdao Road, Hebei economic and Technological Development Zone Patentee after: Aidite (Qinhuangdao) Technology Co.,Ltd. Country or region after: China Address before: 100081 No. 22 South Main Street, Haidian District, Beijing, Zhongguancun Patentee before: PEKING University SCHOOL OF STOMATOLOGY Country or region before: China |