WO2018188582A1 - 制备色阶陶瓷的方法及渐层浆料混合装置 - Google Patents

制备色阶陶瓷的方法及渐层浆料混合装置 Download PDF

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WO2018188582A1
WO2018188582A1 PCT/CN2018/082485 CN2018082485W WO2018188582A1 WO 2018188582 A1 WO2018188582 A1 WO 2018188582A1 CN 2018082485 W CN2018082485 W CN 2018082485W WO 2018188582 A1 WO2018188582 A1 WO 2018188582A1
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ceramic
filling
mixing
speed
mixing device
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PCT/CN2018/082485
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English (en)
French (fr)
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王志光
王彦雄
董国龙
潘立诚
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高雄医学大学
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof

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  • the present invention relates to a method of preparing a gradation ceramic and a grading slurry mixing apparatus.
  • the existing grading technique at least two different colors of the dyeing liquid (water salt dyeing liquid) and a ceramic block are provided; and the dyeing liquid is simultaneously and separately made from the opposite sides of the ceramic block.
  • the soaking procedure (using vacuum soaking, the soaking procedure is between 0.25 hours and 4 hours) causes the ceramic block to absorb the dyeing liquid on opposite sides.
  • the ceramic block after the immersion is taken out and subjected to a standing process.
  • the standing time of the standing process is 24 hours to 48 hours, and the ceramic block after standing is subjected to a heat drying process or a freeze drying process (alternative).
  • the dried ceramic block is subjected to a sintering process to obtain a ceramic block comprising at least two color regions, and the sintering process is performed at at least 1450 degrees Celsius for at least one hour.
  • a sintering process to obtain a ceramic block comprising at least two color regions, and the sintering process is performed at at least 1450 degrees Celsius for at least one hour.
  • zirconia ceramic materials requires cold pressure forming or hot pressure sintering to form a more complicated step, and the process equipment involves high pressure, and the high unit price requires professional operation, which is not generally known.
  • This material has to be mechanically modified after high-pressure production to be excellent in order to be used in the field of dental digital processing (CAD/CAM), bringing many conveniences to the dental industry and simplifying many traditional production steps.
  • CAD/CAM dental digital processing
  • the block material is hard, the forming time is long, the tool is worn out, and the turning process may contain cracks.
  • processing machines, milling tools, and materials are all high unit prices.
  • the remaining materials after turning are not easily reused, resulting in waste.
  • Most of the color of the porcelain block is a single color, which often results in poor aesthetics
  • the present invention is a problem in developing a new device for providing a simple and rapid material process with a color gradation as a main purpose to improve the complicated steps of a conventional process and a single color system.
  • This makes it possible to produce new mixing plants and techniques with gradation materials such as zirconia, lithium silicate, glass ceramics, nanoceramics or ceramics containing inorganic minerals.
  • gradation materials such as zirconia, lithium silicate, glass ceramics, nanoceramics or ceramics containing inorganic minerals.
  • the following problems can be solved: l, the traditional process is complicated, time-consuming, material waste and unsightly. 2, CAD / CAM processing type restrictions. 3, CAD / CAM can only be processed in a single material. 4.
  • CAD/CAM equipment and tools have high parity and high wear rate.
  • the technical features of the invention are as follows: 1.
  • the stirring and the simultaneous screw pushing function. 2 can be used with pneumatic valves to drive the push material.
  • the device of the invention is combined with the advantages of the prior invention technology--the temperature-sensing water-collecting material is combined with the ceramic material, and the water-gel material has the ability to shrink when the temperature rises, so that the sintered powder can be densified, and the principle is like the powder cold-pressure equalization ( Cold isostatic pressing; CIP) molding technology to improve the strength of the material after sintering. Therefore, the colloidal material is added to different concentrations of liquid salts, stirred by a mixing device, and matched with parameters such as stirring speed, vacuum degree, material viscosity and extrusion speed, thereby achieving a slurry material having a color-grading effect, Provide use in various fields.
  • CIP powder cold-pressure equalization
  • the invention provides a ceramic material having cold pressure equal shrinkage forming property, comprising: a temperature sensitive water gel, having a negative temperature characteristic, which increases hydrophobicity and volume shrinkage when the temperature exceeds a critical temperature; and a ceramic material The composition, wherein the ceramic material component is zirconia, lithium silicate, glass ceramic, nano ceramic or inorganic mineral-containing ceramic, wherein the temperature sensitive water gel is combined with the ceramic material component to form the cold pressure equalizing shrinkage forming. Characteristic ceramic material.
  • the viscosity, concentration and addition ratio of the temperature sensitive water gel are adjusted as needed to increase the uniform shrinkage between the powders of the ceramic material.
  • the temperature sensitive glue and the ceramic material are controlled to fill the material capacity and the extrusion time to produce a color gradation or gradient concentration when mixed.
  • the invention further provides a method for preparing ceramics having different color gradations or gradient concentrations, comprising: (a) stirring and mixing a temperature sensitive water gel with a zirconia ceramic powder to obtain a mixture; (b) different concentrations of liquid salts Adding the mixture and controlling the degree of vacuum, pressure, mixing time, mixing speed, filling speed and extrusion speed; and (c) increasing the temperature of the mixture to a critical temperature to uniformly shrink the ceramic powder of the mixture , to obtain ceramics with different color gradations or gradient concentrations.
  • the degree of vacuum, pressure, mixing time, mixing speed, and extrusion speed are achieved under controlled ranges to achieve and achieve an optimum color state.
  • the degree of vacuum is 0-90 cm/Hg ⁇ 50%
  • the pressure is 0-50 kg/cm 2 ⁇ 50%
  • the mixing time is 1-30 minutes ⁇ 50%. It is 1-900 rpm/min ⁇ 50% and the extrusion speed is 1-60 ml/min ⁇ 50%.
  • the invention further provides a gradient slurry mixing device, comprising: a filling tube for filling a filling material; an upper cover located on an upper side of the filling tube, having at least two material inlets for Filling material is filled into the filling tube; a stirring member is disposed between the upper cover and the filling tube, has a rotating motor, a rotating shaft center, which is driven by the rotating motor, and a stirrer is disposed on An end of the rotating shaft for rotating to agitate the filling material; and a material outlet end for discharging the agitated mixed material.
  • the apparatus of the present invention further includes a screw having a plurality of helical turns disposed over the axis of rotation for increasing agitation.
  • the apparatus of the present invention further includes an air intake tube disposed on the upper cover for introducing a gas.
  • the apparatus of the present invention further includes a throttle valve disposed between the filling tube and the outlet end of the material for controlling the discharge of the mixed material.
  • the filling material of the device of the present invention comprises a temperature sensitive water gel and a ceramic material component.
  • the ceramic material is zirconia, lithium silicate, glass ceramic, nano ceramic or ceramic containing inorganic minerals.
  • the apparatus of the present invention further includes a controller for regulating one or more parameters including, but not limited to, the viscosity, concentration, addition ratio, and filling of the temperature sensitive glue.
  • a controller for regulating one or more parameters including, but not limited to, the viscosity, concentration, addition ratio, and filling of the temperature sensitive glue.
  • the fill material of the device of the present invention further comprises a liquid salt.
  • Figure 1 is a schematic view of the water gel mixed with ceramic and filled into the syringe.
  • Figure 2 shows the color gradation in the inlet pipe after mixing and stirring.
  • Figure 3 is a full view of the mixing device.
  • Figure 4 is a panoramic view of the hybrid device design.
  • Figure 5 is a design diagram of the stirring rod.
  • the present invention refers to ⁇ Method for preparing porous ceramic composition by temperature sensitive water gel>, Republic of China Patent No. I411595; US Patent Publication No. US8940203 B2; ⁇ Three-dimensional laminated printing negative temperature water-sensitive mixed ceramic powder Body green body>, US Patent Provisional Case 62/263,005, Dec 4, 2015, with a new process technology for extending development materials. Therefore, the device is controlled by mixing parameters such as the material filling capacity and the extrusion time to achieve the gradation effect.
  • Specific embodiments of the present invention include: (1) adjusting the ratio of optimal mixing of the temperature sensitive water gel/ceramic powder; (2) mixing and stirring speed of the device; (3) filling speed of the mixed material of the device; (4) mixing of the device The speed at which the material is pushed out after agitation.
  • the temperature sensitive water glue is combined with the ceramic and the self-designed screw agitator is used to prepare the premixed slurry.
  • the preparation parameters are: vacuum degree: 0-90cm/Hg ( ⁇ 50% range), pressure: 0- 50kg/cm 2 (about ⁇ 50% range), mixing time: 1-30min (about 50% range), mixing speed: 1-900rpm/min ( ⁇ 50% range).
  • the flow rate of the material to be filled is 1-10 ml/min for A color material (about ⁇ 50%), 1-25 ml/min for B color material (about ⁇ 50% range), and the material speed (squeezing speed) is 1 -60 ml/min (around ⁇ 50%).
  • the negative temperature sensible water gel and the material are stirred and mixed by the device, and have a distribution of color gradation or gradient concentration.
  • the gradient slurry mixing device 10 of the present invention comprises: a filling tube 20 for filling a filling material; an upper cover 30 located on the upper side of the filling tube 20, having at least two material inlets 31, 31'
  • a stirring member 40 is disposed between the upper cover 30 and the filling tube 20, and has a rotating motor 41 and a rotating shaft 42.
  • the rotary motor 41 is driven, and an agitator 43 is disposed at the end of the rotating shaft 42 for rotating to stir the filling material; and a material outlet end 50 for discharging the agitated mixed material.
  • the apparatus 10 of the present invention further includes a screw 44 having a plurality of helical turns disposed over the axis of rotation 42 for increased agitation.
  • the apparatus 10 of the present invention further includes an air intake tube 60 disposed on the upper cover 30 for introducing a gas.
  • the apparatus 10 of the present invention further includes a throttle valve 70 disposed between the fill tube 20 and the material outlet end 50 for controlling the discharge of the mixed material.
  • the device of the present invention further includes a regulator for regulating the viscosity, concentration, addition ratio, filling material capacity, and extrusion speed of the temperature sensitive water gel, the stirring speed of the stirring member 40, and/or the filling tube 20 Vacuum degree. (As shown in Figures 3 to 5).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)

Abstract

一种具有冷均压收缩成形特性的陶瓷材料,包括一温感水胶以及一陶瓷材料成分,其中该温感水胶结合该陶瓷材料成分。一种制作具有不同色阶或梯度浓度的陶瓷的方法,包含将温感水胶与氧化锆陶瓷粉末混合、加入液体盐类,及将混合物的稳定提高到临界温度。一种渐层浆料混合装置,包括一填充管、一上盖、一搅拌构件和一材料出口端。

Description

制备色阶陶瓷的方法及渐层浆料混合装置 技术领域
本发明是关于制备色阶陶瓷的方法及渐层浆料混合装置。
背景技术
现有渐层技术中是提供至少二种不同颜色的染色液体(水盐类染色液体)及一陶瓷块体;再将所述染色液体同时且分别由所述陶瓷块体的相对二侧进行一浸泡程序(采用真空浸泡,所述浸泡程序的时间为0.25小时~4小时之间),使所述陶瓷块体相对二侧分别吸收所述染色液体。浸泡后的陶瓷块体取出并进行一静置程序,所述静置程序的时间为24小时~48小时,静置后的陶瓷块体进行一热干燥程序或一冷冻干燥程序(二择一),将干燥后的陶瓷块体进行一烧结程序,进而得一包含有至少二色区的陶瓷块体,所述烧结程序是在至少摄氏1450度中烧结至少l小时。但此等技术缺点仍属多重步骤,且制程耗时(需要浸泡、干燥、再烧结)。
目前氧化锆陶瓷材料制作均需经过冷均压成形或热均压烧结成形属较复杂步骤,且制程设备涉及高压,更属高单价仪器需有专业人员操作并非一般人可涉略。此材料须经过高压制作后机械性质改变成极佳,方可被牙科数字加工(CAD/CAM)领域应用,为牙科产业带来许多便利与简化许多传统制作步骤,不过,却也衍生出多项缺点,如制程中,软加工(Soft-matchined)的部分烧结瓷块进行车削后,其体积收缩量大(约有25%的体积收缩);而硬加工(Hard-matchined)则是所用的瓷块材料硬,成形时间长,对工具耗损大,而且车削过程可能含有裂缝(Crack)产生。除此之外,加工机器、车削工具(Milling tool)、材料均属高单价,此外,车削后的剩余材料不易再利用,进而导致浪费。而瓷块颜色大部分为单一颜色,常造成美观与仿真性不佳的情形。
发明内容
本发明是开发一新装置为材料制程提供一简单且快速并同时具有色阶为主要目的,以改善传统制程的繁杂步骤及单一色系的问题。此可制作具色阶材料,如氧化锆、硅酸锂、玻璃陶瓷、纳米陶瓷或含无机质矿物的陶瓷等的新混合搅拌装置与技术。可解决下列问题:l、传统制程繁杂、耗时、材料浪费及不美观等。2、CAD/CAM加工的型态限制。3、CAD/CAM仅能单一材料加工。4、CAD/CAM设备与工具平价及耗损率高。
本发明技术特点:1、具搅拌同时螺旋推挤功能。2、可搭配气动阀驱动推挤材料。3、具节流阀可控制出料流量。4、可制作具渐层的陶瓷浆料。
本发明的装置搭配既有的发明技术优势─温感水胶材料结合陶瓷材料,利用温度上升时水胶材料会有收缩的能力,让烧结粉体能够致密化,其原理犹如粉末冷均压(cold isostatic pressing;CIP)成型技术,提高烧结后材料强度。因此,将胶体材料加入不同浓度的液体盐类,经过混合装置搅拌,并配合相关搅拌速度、真空度、材料黏度及挤料速度等参数设定,进而达到具色阶效果的浆体原料,以提供各领域使用。
本发明提供一种具有冷均压收缩成形特性的陶瓷材料,包含:一温感水胶,具有负温感特性,其于温度越过一临界温度时,疏水性增加,体积收缩;以及一陶瓷材料成份,其中该陶瓷材料成份为氧化锆、硅酸锂、玻璃陶瓷、纳米陶瓷或含无机质矿物的陶瓷,其中该温感水胶结合该陶瓷材料成份,以形成具有该冷均压收缩成形的特性的陶瓷材料。
在一较佳实施例中,该温感水胶的黏度、浓度及添加比例依需要调整,用以提高该陶瓷材料的粉末间的均匀收缩。
在另一较佳实施例中,该温感水胶与该陶瓷材料于经搅拌混合时,控制填入材料容量及挤出时间,用以产生色阶或梯度浓度。
本发明另提供一种制作具有不同色阶或梯度浓度的陶瓷的方法,包含:(a)将温感水胶与氧化锆陶瓷粉末搅拌混合得到一混合物;(b)将不同浓度的液体盐类加入该混合物,并控制真空度、压力、混合时间、混合速度、填入速度及挤料速度;及(c)将该混合物的温度提高至一临界温度,使该混合物的陶瓷粉末之间均匀收缩,得到具有不同色阶或梯度浓度的陶瓷。
在一较佳实施例中,真空度、压力、混和时间、混和速度及挤料速度在可控制范围实施下,可使材料达到并呈现最佳色阶状态。
在另一较佳实施例中,该真空度为0-90cm/Hg±50%、该压力为0-50kg/cm 2±50%、该混合时间为1-30分钟±50%、该混合速度为1-900rpm/min±50%及该挤料速度为1-60ml/min±50%。
本发明另提供一种渐层浆料混合装置,包括:一充填管,用以充填一填入材料;一上盖,位于该充填管的上侧,具有至少二个材料入口,用以将该填入材料充填至该充填管;一搅拌构件,设置于该上盖与该充填管之间,具有一旋转马达,一旋转轴心,其是 由该旋转马达带动,及一搅拌器,设置于该旋转轴心的末端,用以旋转以搅拌该填入材料;以及一材料出口端,用以排出经搅拌的混合材料。
在一较佳实施例中,本发明的装置进而包含一螺旋器,具有复数个螺旋状圈,套设于该旋转轴心,用以增加搅拌作用。
在一较佳实施例中,本发明的装置进而包含一进气管,设置于该上盖上,用以导入气体。
在一较佳实施例中,本发明的装置进而包含一节流阀,设置于该充填管与该材料出口端间,用以控制该混合材料的排出。
在一较佳实施例中,本发明装置的该填入材料包含一温感水胶及一陶瓷材料成份。在另一较佳实施例中,该陶瓷材料成份为氧化锆、硅酸锂、玻璃陶瓷、纳米陶瓷或含无机质矿物的陶瓷。
在一较佳实施例中,本发明装置进而包含一调控器,用以调控一或复数个参数,该一或复数个参数包含但不限于该温感水胶的黏度、浓度、添加比例、填入材料容量、及挤出速度、该搅拌构件的搅拌速度及/或该充填管的真空度。
在一较佳实施例中,本发明装置的该填入材料进而包含一液体盐类。
附图说明
图1为水胶与陶瓷混合后填入针筒内的示意图。
图2为混合搅拌后流入承接管内的色阶情况。
图3为混合装置全视图。
图4为混合装置设计全景图。
图5为搅拌杆设计图。
具体实施方式
本发明可能以不同的形式来实施,并不仅限于下列文中所提及的实例。下列实施例仅作为本发明不同面向及特点中的代表。
本发明参照<以温感水胶制备含多孔性陶瓷组合物的方法>,中华民国专利证号发明第I411595号;美国专利公告号US8940203 B2;<三维积层打印负温感水胶混合陶瓷粉体的生坯体>,美国专利临时案62/263,005,Dec 4,2015,以延伸开发材料的新制程技术研究。因此,利用本装置控制填入材料容量及挤出时间等参数进行混合,以达到色阶效 果。
本发明各具体实施例包含:(1)调整温感性水胶/陶瓷粉末最佳混合的比例;(2)装置的混合搅拌速度;(3)装置的混合材料填入速度;(4)装置混合搅拌后推出材料的速度。其中温感性水胶与陶瓷结合并以自制设计的螺杆搅拌器,进行前置浆体混合搅拌制备,其制备参数:真空度:0-90cm/Hg(±50%范围左右),压力:0-50kg/cm 2(±50%范围左右),混合时间:1-30min(±50%范围左右),混合速度:1-900rpm/min(±50%范围左右)。填入材料的流量速度为A色材料1-10ml/min(±50%范围左右),B色材料1-25ml/min(±50%范围左右),而推出材料速度(挤料速度)为1-60ml/min(±50%范围左右)。负温感水胶与材料经本装置搅拌混合后,已具有色阶或梯度浓度的分布。
本发明的渐层浆料混合装置10,包括:一充填管20,用以充填一填入材料;一上盖30,位于该充填管20的上侧,具有至少二个材料入口31、31’,用以将该填入材料充填至该充填管20;一搅拌构件40,设置于该上盖30与该充填管20之间,具有一旋转马达41,一旋转轴心42,其是由该旋转马达41带动,及一搅拌器43,设置于该旋转轴心42的末端,用以旋转以搅拌该填入材料;以及一材料出口端50,用以排出经搅拌的混合材料。本发明的装置10进而包含一螺旋器44,具有复数个螺旋状圈,套设于该旋转轴心42,用以增加搅拌作用。本发明的装置10进而包含一进气管60,设置于该上盖30上,用以导入气体。本发明的装置10进而包含一节流阀70,设置于该充填管20与该材料出口端50间,用以控制该混合材料的排出。本发明装置进而包含一调控器,用以调控该温感水胶的黏度、浓度、添加比例、填入材料容量、及挤出速度、该搅拌构件40的搅拌速度及/或该充填管20的真空度。(如图3至图5所示)。
符号说明
10 渐层浆料混合装置
20 充填管
21 固定栓(固定上盖用)
22 上盖固定槽
30 上盖
31、31’ 材料入口
32 材料管
40 搅拌构件
41 旋转马达
42 旋转轴心
43 搅拌器
44 螺旋器
50 材料出口端
60. 进气管
70 节流阀
90 金属支架
91 搅拌片
92 推阀

Claims (10)

  1. 一种具有冷均压收缩成形特性的陶瓷材料,包含:
    一温感水胶,具有负温感特性,其于温度越过一临界温度时,疏水性增加,体积收缩;以及
    一陶瓷材料成份,其中该陶瓷材料成份为氧化锆、硅酸锂、玻璃陶瓷、纳米陶瓷或含无机质矿物的陶瓷,
    其中该温感水胶结合该陶瓷材料,以形成具有该冷均压收缩成形的特性的陶瓷材料。
  2. 一种制作具有不同色阶或梯度浓度的陶瓷的方法,包含:
    (a)将温感水胶与氧化锆陶瓷粉末搅拌混合得到一混合物;
    (b)将不同浓度的液体盐类加入该混合物,并控制真空度、压力、混合时间、混合速度、填入速度及挤料速度;及
    (c)将该混合物的温度提高至一临界温度,使该混合物的陶瓷粉末之间均匀收缩,得到具有不同色阶或梯度浓度的陶瓷。
  3. 如权利要求2所述的方法,其中该真空度为0-90cm/Hg±50%、该压力为0-50kg/cm 2±50%、该混合时间为1-30分钟±50%、该混合速度为1-900rpm/min±50%及该挤料速度为1-60ml/min±50%。
  4. 一种渐层浆料混合装置,包括:
    一充填管,用以充填一填入材料;
    一上盖,位于该充填管的上侧,具有至少二个材料入口,用以将该填入材料充填至该充填管;
    一搅拌构件,设置于该上盖与该充填管之间,具有一旋转马达,一旋转轴心,其是由该旋转马达带动,及一搅拌器,设置于该旋转轴心的末端,用以旋转以搅拌该等填入材料;以及
    一材料出口端,用以排出经搅拌的混合材料。
  5. 如权利要求4所述的混合装置,其进而包含一螺旋器,具有复数个螺旋状圈,套设于该旋转轴心,用以增加搅拌作用。
  6. 如权利要求4或5所述的混合装置,其进而包含一进气管,设置于该上盖上,用以导入气体。
  7. 如权利要求4-6任一所述的混合装置,其进而包含一节流阀,设置于该充填管与该 材料出口端间,用以控制该混合材料的排出。
  8. 如权利要求4-7任一所述的混合装置,其中该填入材料为一温感水胶及一陶瓷材料成份。
  9. 如权利要求4-8任一所述的混合装置,其进而包含一调控器,用以调控一或复数个参数,该一或复数个参数包含该温感水胶的黏度、浓度、添加比例、填入材料容量、及挤出速度、该搅拌构件的搅拌速度及/或该充填管的真空度。
  10. 如权利要求8所述的混合装置,其中该填入材料进一步包含一液体盐类。
PCT/CN2018/082485 2017-04-10 2018-04-10 制备色阶陶瓷的方法及渐层浆料混合装置 WO2018188582A1 (zh)

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