CN108033802A - 基于凝胶注模3d打印的纤维增强陶瓷异型件成型方法 - Google Patents

基于凝胶注模3d打印的纤维增强陶瓷异型件成型方法 Download PDF

Info

Publication number
CN108033802A
CN108033802A CN201711360018.2A CN201711360018A CN108033802A CN 108033802 A CN108033802 A CN 108033802A CN 201711360018 A CN201711360018 A CN 201711360018A CN 108033802 A CN108033802 A CN 108033802A
Authority
CN
China
Prior art keywords
ceramic
fiber reinforced
reinforced ceramic
fiber
special
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
CN201711360018.2A
Other languages
English (en)
Inventor
崔雨潇
林彬
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.)
Tianjin University
Original Assignee
Tianjin University
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 Tianjin University filed Critical Tianjin University
Priority to CN201711360018.2A priority Critical patent/CN108033802A/zh
Publication of CN108033802A publication Critical patent/CN108033802A/zh
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00Processes of additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00Materials specially adapted for additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00Products made by additive manufacturing
    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10Shaped 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
    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/14Shaped 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 silica
    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48Shaped 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
    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/583Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/624Sol-gel processing
    • C04B35/803
    • C04B35/806
    • 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
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5216Inorganic
    • C04B2235/522Oxidic
    • 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
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5216Inorganic
    • C04B2235/524Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • 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
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54Particle size related information
    • C04B2235/5418Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • 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
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54Particle size related information
    • C04B2235/5418Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
    • 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
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602Making the green bodies or pre-forms by moulding
    • C04B2235/6026Computer aided shaping, e.g. rapid prototyping
    • 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
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/606Drying

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)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

一种基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,包括:将陶瓷粉体、纤维材料、和助烧剂和聚丙烯酰胺交联剂溶液充分混合;将陶瓷粉体、纤维材料、和助烧剂和过硫酸铵引发剂溶液充分混合;将上述含有交联剂和引发剂的陶瓷泥料分别由两条管路供给混流管充分混合,由3D打印机的打印头挤出;打印头按照异型件的截面数据运动,在交联剂和引发剂的聚合反应作用下,陶瓷浆料凝固成型,获得陶瓷异型件坯体;在数控加工中心上对陶瓷异型件坯体进行表面修整;进行脱脂和烧结,获得纤维增强陶瓷异型件。使用该方法可以避免3D打印技术中的光固化或加热等复杂的复杂工艺,实现表面质量优良,近净尺寸的纤维增强陶瓷异型件的快速制造。

Description

基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法
技术领域
本发明涉及一种纤维增强陶瓷异型件成型方法。特别是涉及一种基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法。
背景技术
工程陶瓷材料由于其优秀的机械性能、透波性能以及生物相容性等,在国防、空天、智能终端以及医疗等领域得到了广泛应用。然而由于其脆性较大,抗机械和热冲击性能不佳,工程陶瓷在上述领域的应用还有待进一步扩展。通过向陶瓷基体中添加纤维,增强陶瓷的强度和韧性,受到了研究人员的广泛关注。目前,纤维编织体增强陶瓷应用较多,在一定程度上改善了工程陶瓷的抗冲击性能,然而其纤维编织工艺复杂,制备周期偏长,导致其成本极高。短纤维增强陶瓷无需复杂的纤维编织工艺,制备相对简单,可望取代纤维编织体增强陶瓷。不仅如此,上述领域应用的工程陶瓷零件外形多为不规则曲面,常规方法制备的陶瓷工件还需要进行去除量很大的磨削修形工作,对工程陶瓷材料造成了很大的浪费。
3D打印技术又称增材制造技术,是一种新兴先进制造技术。3D打印技术以金属、陶瓷和塑料等为材料,通过材料的逐层打印,可以实现快速成型,无需设计开发模具,因此可以缩短产品的设计和生产周期,大幅降低研制成本。3D打印技术收到世界范围内的广泛重视,但是目前打印材料种类有待进一步丰富,并且常规3D打印成型的材料性能较差,打印质量有待进一步提高。陶瓷材料的直接成型技术是3D打印技术的研究热点和重要发展方向。光固化或熔融沉积成型可以将增强纤维和陶瓷泥料进行打印并制备成陶瓷坯体,但是需要额外的光固化或者加热装置,工艺较为复杂。此外,对于工程陶瓷而言,其特定的陶瓷粉体属于瘠性材料,粘度、塑性和分散性较差,导致其无法直接用于3D打印。
发明内容
本发明所要解决的技术问题是,提供一种无需额外光固化或者加热工艺的基于凝胶注模 3D打印的纤维增强陶瓷异型件成型方法。
本发明所采用的技术方案是:一种基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,包括如下步骤:
1)将陶瓷粉体材料和增强纤维材料混合后,在球磨机中搅拌混合均匀,得到纤维增强陶瓷材料;
2)配制聚丙烯酰胺溶液,并向聚丙烯酰胺溶液中分别加入润湿分散剂和消泡剂,然后将获得的纤维增强陶瓷材料以及助烧剂加入所述的溶液中,在分散机中混合均匀,获得纤维增强陶瓷交联剂泥料;
3)配制过硫酸铵溶液,并向过硫酸铵溶液中加入润湿分散剂和消泡剂,然后将获得的纤维增强陶瓷材料以及助烧剂加入所述的溶液中,在分散机中混合均匀,获得纤维增强陶瓷引发剂泥料;
4)使用三维建模软件设计异型件的3D模型,并将3D模型转换为分层路径文件,导入 3D打印机;
5)将步骤2)和步骤3)获得的纤维增强陶瓷交联剂泥料和纤维增强陶瓷引发剂泥料由两条管路供给混流管充分混合,混合后的陶瓷泥料供给打印头,气泵通入压缩气体,提供均匀压强,打印头将混合后的陶瓷泥料均匀挤出;
6)打印头根据分层路径文件按照异型件的3D模型当前层的轮廓数据进行平面二维运动,陶瓷泥料在聚丙烯酰胺和过硫酸铵的聚合反应作用下凝固,形成当前轮廓截面;
7)完成异型件的3D模型当前层的轮廓数据后,打印头上升一个分层的厚度;
8)重复步骤5)至步骤7),直至异型件坯体打印完成;
9)将打印完成的异型件坯体置于烘箱内,保持温度在40-60℃,保温24-48小时;
10)在数控加工中心上对陶瓷异型件坯体进行表面修整,改善表面质量;
11)将步骤10)获得的异型件坯体进行脱脂和烧结,获得纤维增强陶瓷异型件。
步骤1)中所述的陶瓷粉体的粒径为0.5-2μm;纤维材料的直径为2-4μm,长度为20-40μm。
步骤1)中所述的纤维增强陶瓷材料中陶瓷粉体材料和增强纤维材料的质量比为4-9:1。
步骤2)中所述的聚丙烯酰胺溶液的质量分数为1%;。
步骤2)中所述的润湿分散剂和消泡剂的加入质量分别为聚丙烯酰胺溶液质量的1%。
步骤3)中所述的过硫酸铵溶液的质量分数为1%;润湿分散剂和消泡剂的加入质量分别为过硫酸铵溶液质量的1%。
步骤2)和步骤3)中所述的助烧剂是氧化铝、氧化钾和氧化硼中的一种以上,所述的助烧剂的质量分数为纤维增强陶瓷材料的0.5%。
所述的纤维增强陶瓷交联剂泥料和纤维增强陶瓷引发剂泥料的固含量均为70-75%。
步骤6)中由纤维增强陶瓷交联剂泥料和纤维增强陶瓷引发剂泥料混合的陶瓷泥料发生聚合反应凝固的时间为1-5分钟。
步骤1)中所述的陶瓷粉体材料为石英、氧化锆、氧化铝、氮化硼和氮化硅中的一种或多种;所述的增强纤维材料为石英纤维、高硅氧纤维、氮化硅纤维和氮化硼纤维中的一种或多种。
本发明的基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,避免了3D打印技术中常用的光固化和加热等复杂工艺,将带有交联剂和引发剂的陶瓷泥料快速充分混合后挤出打印,利用交联聚合反应实现陶瓷泥料的快速凝固,从而获得具有良好韧性和高强度的纤维增强陶瓷异型件坯体,明显简化了3D打印工艺,促进3D打印技术在陶瓷异型天线罩成型中的应用。本发明采用无毒的聚丙烯酰胺为交联剂,明显提高了凝胶注模工艺的安全性。本发明适用于多种成分的纤维增强陶瓷异型件的快速成型,脱脂烧结后可获得具有良好强度、韧性和表面质量的异型天线罩工件,无需开发模具,避免了常规纤维增强陶瓷异型件制备周期长,加工去除余量大的问题,可以显著降低生产成本。
具体实施方式
下面结合实施例对本发明的基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法做出详细说明。
本发明的基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,包括如下步骤:
1)将陶瓷粉体材料和增强纤维材料混合后,在球磨机中搅拌混合均匀,得到纤维增强陶瓷材料;其中,
所述的陶瓷粉体材料为石英、氧化锆、氧化铝、氮化硼和氮化硅中的一种或多种;所述的增强纤维材料为石英纤维、高硅氧纤维、氮化硅纤维和氮化硼纤维中的一种或多种;
所述的陶瓷粉体的粒径为0.5-2μm;纤维材料的直径为2-4μm,长度为20-40μm;
所述的纤维增强陶瓷材料中陶瓷粉体材料和增强纤维材料的质量比为4-9:1。
2)配制聚丙烯酰胺溶液,并向聚丙烯酰胺溶液中分别加入润湿分散剂和消泡剂,然后将获得的纤维增强陶瓷材料以及助烧剂加入所述的溶液中,在分散机中混合均匀,获得纤维增强陶瓷交联剂泥料;其中,
所述的聚丙烯酰胺溶液的质量分数为1%;
所述的润湿分散剂和消泡剂的加入质量分别为聚丙烯酰胺溶液质量的1%。
纤维增强陶瓷交联剂泥料的固含量均为70-75%。
3)配制过硫酸铵溶液,并向过硫酸铵溶液中加入润湿分散剂和消泡剂,然后将获得的纤维增强陶瓷材料以及助烧剂加入所述的溶液中,在分散机中混合均匀,获得纤维增强陶瓷引发剂泥料;其中,
所述的过硫酸铵溶液的质量分数为1%;所述的润湿分散剂和消泡剂的加入质量分别为过硫酸铵溶液质量的1%。
所述的纤维增强陶瓷引发剂泥料的固含量为70-75%。
在上述步骤2)和步骤3)中所述的助烧剂是氧化铝、氧化钾和氧化硼中的一种以上,所述的助烧剂的质量分数为纤维增强陶瓷材料的0.5%。
4)使用三维建模软件设计异型件的3D模型,并将3D模型转换为分层路径文件,导入 3D打印机;所述的三维建模软件是CAD或UG或Solidworks等。
5)将步骤2)和步骤3)获得的纤维增强陶瓷交联剂泥料和纤维增强陶瓷引发剂泥料由两条管路供给混流管充分混合,混合后的陶瓷泥料供给打印头,气泵通入压缩气体,提供均匀压强,打印头将混合后的陶瓷泥料均匀挤出;
6)打印头根据分层路径文件按照异型件的3D模型当前层的轮廓数据进行平面二维运动,陶瓷泥料在聚丙烯酰胺和过硫酸铵的聚合反应作用下凝固,形成当前轮廓截面;由纤维增强陶瓷交联剂泥料和纤维增强陶瓷引发剂泥料混合的陶瓷泥料发生聚合反应凝固的时间为1-5 分钟。
7)完成异型件的3D模型当前层的轮廓数据后,打印头上升一个分层的厚度;
8)重复步骤5)至步骤7),直至异型件坯体打印完成;
9)将打印完成的异型件坯体置于烘箱内,保持温度在40-60℃,保温24-48小时;
10)在数控加工中心上对陶瓷异型件坯体进行表面修整,改善表面质量;
11)将步骤10)获得的异型件坯体进行脱脂和烧结,获得纤维增强陶瓷异型件。
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。
实施例1
1)使用Solidworks软件设计异型件的3D模型,并将3D模型转换为分层路径文件,导入3D打印机;
2)将粒径为2μm的石英陶瓷粉体和直径4μm,长40μm的石英纤维按质量比9:1倒入球磨机中,再加入质量分数1%的氧化硼作为助烧剂,搅拌混合均匀,得到石英纤维增强石英陶瓷材料;
3)配制质量分数1%的聚丙烯酰胺溶液,并向聚丙烯酰胺溶液中分别加入质量分数分别为1%的润湿分散剂和消泡剂,将石英纤维增强石英陶瓷材料按照固液质量比7:3加入上述溶液,在分散机中混合均匀,获得固含量为70%的石英纤维增强石英陶瓷交联剂泥料;
4)配制质量分数1%的聚丙烯酰胺溶液,并向过硫酸铵溶液中加入质量分数分别为1%的润湿分散剂和消泡剂,将石英纤维增强石英陶瓷材料按照固液质量比7:3加入上述溶液,在分散机中混合均匀,获得固含量为70%的石英纤维增强石英陶瓷引发剂泥料;
5)将步骤3)和步骤4)获得的石英纤维增强石英陶瓷交联剂泥料和石英纤维增强石英陶瓷引发剂泥料由两条管路供给混流管充分混合,混合后的陶瓷泥料供给打印头,气泵通入压缩气体,提供均匀压强,打印头将混合后的陶瓷泥料均匀挤出;
6)打印头根据分层路径文件按照异型件的3D模型当前层的轮廓数据进行平面二维运动,陶瓷泥料在聚丙烯酰胺和过硫酸铵的聚合反应作用下凝固,形成当前轮廓截面;由石英纤维增强石英陶瓷交联剂泥料和石英纤维增强石英陶瓷引发剂泥料混合的陶瓷泥料发生聚合反应凝固的时间为5分钟;
7)完成异型件的3D模型当前层的轮廓数据后,打印头上升一个分层的厚度;
8)重复步骤5)至步骤7),直至异型件坯体打印完成;
9)将打印完成的异型件坯体置于烘箱内,保持温度在40℃,保温24小时;
10)在数控加工中心上对陶瓷异型件坯体进行表面修整,改善表面质量;
11)将步骤10)获得的异型件坯体进行脱脂和烧结,获得石英纤维增强石英陶瓷异型件。
实施例2
1)使用Solidworks软件设计异型件的3D模型,并将3D模型转换为分层路径文件,导入3D打印机;
2)、将粒径为0.5μm的氮化硼陶瓷粉体和直径2μm,长20μm的氮化硅纤维按质量比4:1 倒入球磨机中,再加入质量分数1%的氧化铝作为助烧剂,搅拌混合均匀,得到氮化硅纤维增强氮化硼陶瓷材料;
3)配制质量分数1%的聚丙烯酰胺溶液,并向聚丙烯酰胺溶液中分别加入质量分数分别为1%的润湿分散剂和消泡剂,将氮化硅纤维增强氮化硼陶瓷材料按照固液质量比7:3加入上述溶液,在分散机中混合均匀,获得固含量为70%的氮化硅纤维增强氮化硼陶瓷交联剂泥料;
4)配制质量分数1%的聚丙烯酰胺溶液,并向过硫酸铵溶液中加入质量分数分别为1%的润湿分散剂和消泡剂,将氮化硅纤维增强氮化硼陶瓷材料按照固液质量比7:3加入上述溶液,在分散机中混合均匀,获得固含量为70%的氮化硅纤维增强氮化硼陶瓷引发剂泥料;
5)将步骤3)和步骤4)获得的氮化硅纤维增强氮化硼陶瓷交联剂泥料和氮化硅纤维增强氮化硼陶瓷引发剂泥料由两条管路供给混流管充分混合,混合后的陶瓷泥料供给打印头,气泵通入压缩气体,提供均匀压强,打印头将混合后的陶瓷泥料均匀挤出;
6)打印头根据分层路径文件按照异型件的3D模型当前层的轮廓数据进行平面二维运动,陶瓷泥料在聚丙烯酰胺和过硫酸铵的聚合反应作用下凝固,形成当前轮廓截面;由氮化硅纤维增强氮化硼陶瓷交联剂泥料和氮化硅纤维增强氮化硼陶瓷引发剂泥料混合的陶瓷泥料发生聚合反应凝固的时间为1分钟;
7)完成异型件的3D模型当前层的轮廓数据后,打印头上升一个分层的厚度;
8)重复步骤5)至步骤7),直至异型件坯体打印完成;
9)将打印完成的异型件坯体置于烘箱内,保持温度在60℃,保温48小时;
10)在数控加工中心上对陶瓷异型件坯体进行表面修整,改善表面质量;
11)、将步骤10)获得的异型件坯体进行脱脂和烧结,获得氮化硅纤维增强氮化硼陶瓷异型件。

Claims (10)

1.一种基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,其特征在于,包括如下步骤:
1)将陶瓷粉体材料和增强纤维材料混合后,在球磨机中搅拌混合均匀,得到纤维增强陶瓷材料;
2)配制聚丙烯酰胺溶液,并向聚丙烯酰胺溶液中分别加入润湿分散剂和消泡剂,然后将获得的纤维增强陶瓷材料以及助烧剂加入所述的溶液中,在分散机中混合均匀,获得纤维增强陶瓷交联剂泥料;
3)配制过硫酸铵溶液,并向过硫酸铵溶液中加入润湿分散剂和消泡剂,然后将获得的纤维增强陶瓷材料以及助烧剂加入所述的溶液中,在分散机中混合均匀,获得纤维增强陶瓷引发剂泥料;
4)使用三维建模软件设计异型件的3D模型,并将3D模型转换为分层路径文件,导入3D打印机;
5)将步骤2)和步骤3)获得的纤维增强陶瓷交联剂泥料和纤维增强陶瓷引发剂泥料由两条管路供给混流管充分混合,混合后的陶瓷泥料供给打印头,气泵通入压缩气体,提供均匀压强,打印头将混合后的陶瓷泥料均匀挤出;
6)打印头根据分层路径文件按照异型件的3D模型当前层的轮廓数据进行平面二维运动,陶瓷泥料在聚丙烯酰胺和过硫酸铵的聚合反应作用下凝固,形成当前轮廓截面;
7)完成异型件的3D模型当前层的轮廓数据后,打印头上升一个分层的厚度;
8)重复步骤5)至步骤7),直至异型件坯体打印完成;
9)将打印完成的异型件坯体置于烘箱内,保持温度在40-60℃,保温24-48小时;
10)在数控加工中心上对陶瓷异型件坯体进行表面修整,改善表面质量;
11)将步骤10)获得的异型件坯体进行脱脂和烧结,获得纤维增强陶瓷异型件。
2.根据权利要求1所述的基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,其特征在于,步骤1)中所述的陶瓷粉体的粒径为0.5-2μm;纤维材料的直径为2-4μm,长度为20-40μm。
3.根据权利要求1所述的基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,其特征在于,步骤1)中所述的纤维增强陶瓷材料中陶瓷粉体材料和增强纤维材料的质量比为4-9:1。
4.根据权利要求1所述的基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,其特征在于,步骤2)中所述的聚丙烯酰胺溶液的质量分数为1%;。
5.根据权利要求1所述的基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,其特征在于,步骤2)中所述的润湿分散剂和消泡剂的加入质量分别为聚丙烯酰胺溶液质量的1%。
6.根据权利要求1所述的基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,其特征在于,步骤3)中所述的过硫酸铵溶液的质量分数为1%;润湿分散剂和消泡剂的加入质量分别为过硫酸铵溶液质量的1%。
7.根据权利要求1所述的基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,其特征在于,步骤2)和步骤3)中所述的助烧剂是氧化铝、氧化钾和氧化硼中的一种以上,所述的助烧剂的质量分数为纤维增强陶瓷材料的0.5%。
8.根据权利要求1所述的基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,其特征在于,所述的纤维增强陶瓷交联剂泥料和纤维增强陶瓷引发剂泥料的固含量均为70-75%。
9.根据权利要求1所述的基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,其特征在于,步骤6)中由纤维增强陶瓷交联剂泥料和纤维增强陶瓷引发剂泥料混合的陶瓷泥料发生聚合反应凝固的时间为1-5分钟。
10.根据权利要求1所述的基于凝胶注模3D打印的纤维增强陶瓷异型件成型方法,其特征在于,步骤1)中所述的陶瓷粉体材料为石英、氧化锆、氧化铝、氮化硼和氮化硅中的一种或多种;所述的增强纤维材料为石英纤维、高硅氧纤维、氮化硅纤维和氮化硼纤维中的一种或多种。
CN201711360018.2A 2017-12-15 2017-12-15 基于凝胶注模3d打印的纤维增强陶瓷异型件成型方法 Pending CN108033802A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711360018.2A CN108033802A (zh) 2017-12-15 2017-12-15 基于凝胶注模3d打印的纤维增强陶瓷异型件成型方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711360018.2A CN108033802A (zh) 2017-12-15 2017-12-15 基于凝胶注模3d打印的纤维增强陶瓷异型件成型方法

Publications (1)

Publication Number Publication Date
CN108033802A true CN108033802A (zh) 2018-05-15

Family

ID=62099487

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711360018.2A Pending CN108033802A (zh) 2017-12-15 2017-12-15 基于凝胶注模3d打印的纤维增强陶瓷异型件成型方法

Country Status (1)

Country Link
CN (1) CN108033802A (zh)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109482886A (zh) * 2019-01-07 2019-03-19 吉林大学 一种3d打印陶瓷与纤维复合增强铝基材料的制备方法
CN110451979A (zh) * 2019-08-19 2019-11-15 上海应用技术大学 一种具有双贯穿型孔洞的网眼多孔陶瓷的制备方法
CN111925193A (zh) * 2020-07-17 2020-11-13 长沙理工大学 细晶氧化铝陶瓷的3d打印制备方法
CN112374903A (zh) * 2020-12-21 2021-02-19 山东蓝合智能科技有限公司 一种用于氧化锆陶瓷3d打印材料的制备方法
CN112500026A (zh) * 2020-12-04 2021-03-16 西安交通大学 光固化用短切石英纤维增强氧化硅陶瓷膏料及其制备方法
CN113698226A (zh) * 2021-09-23 2021-11-26 景德镇陶瓷大学 一种高强度多孔陶瓷的制备方法及其制得的产品
CN115073195A (zh) * 2022-06-05 2022-09-20 西北工业大学 用于3d打印雷达天线罩的氮化硅晶须增强氮化物复合材料及制备和打印方法
CN115073171A (zh) * 2022-06-29 2022-09-20 清华大学深圳国际研究生院 一种适用于光固化成型加工的ltcc生料带材料、ltcc基板及其制备方法和应用
WO2023273504A1 (zh) * 2021-06-30 2023-01-05 Oppo广东移动通信有限公司 壳体及其制备方法和电子设备

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104493952A (zh) * 2015-01-06 2015-04-08 彭晓领 陶瓷梯度材料的凝胶注模3d打印制备方法
CN106278335A (zh) * 2016-08-05 2017-01-04 西安交通大学 一种纤维定向增韧陶瓷基复合材料涡轮叶片的制造方法
US20170081500A1 (en) * 2015-09-17 2017-03-23 3Dbotics, Inc. Material system and method for fabricating refractory material-based 3d printed objects
CN106927847A (zh) * 2017-02-27 2017-07-07 西安交通大学 一种基于3d打印技术的纤维增强陶瓷基复合材料成形方法及装置

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104493952A (zh) * 2015-01-06 2015-04-08 彭晓领 陶瓷梯度材料的凝胶注模3d打印制备方法
US20170081500A1 (en) * 2015-09-17 2017-03-23 3Dbotics, Inc. Material system and method for fabricating refractory material-based 3d printed objects
CN106278335A (zh) * 2016-08-05 2017-01-04 西安交通大学 一种纤维定向增韧陶瓷基复合材料涡轮叶片的制造方法
CN106927847A (zh) * 2017-02-27 2017-07-07 西安交通大学 一种基于3d打印技术的纤维增强陶瓷基复合材料成形方法及装置

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109482886A (zh) * 2019-01-07 2019-03-19 吉林大学 一种3d打印陶瓷与纤维复合增强铝基材料的制备方法
CN110451979A (zh) * 2019-08-19 2019-11-15 上海应用技术大学 一种具有双贯穿型孔洞的网眼多孔陶瓷的制备方法
CN111925193A (zh) * 2020-07-17 2020-11-13 长沙理工大学 细晶氧化铝陶瓷的3d打印制备方法
CN112500026A (zh) * 2020-12-04 2021-03-16 西安交通大学 光固化用短切石英纤维增强氧化硅陶瓷膏料及其制备方法
CN112500026B (zh) * 2020-12-04 2021-11-30 西安交通大学 光固化用短切石英纤维增强氧化硅陶瓷膏料及其制备方法
CN112374903A (zh) * 2020-12-21 2021-02-19 山东蓝合智能科技有限公司 一种用于氧化锆陶瓷3d打印材料的制备方法
WO2023273504A1 (zh) * 2021-06-30 2023-01-05 Oppo广东移动通信有限公司 壳体及其制备方法和电子设备
CN113698226A (zh) * 2021-09-23 2021-11-26 景德镇陶瓷大学 一种高强度多孔陶瓷的制备方法及其制得的产品
CN115073195A (zh) * 2022-06-05 2022-09-20 西北工业大学 用于3d打印雷达天线罩的氮化硅晶须增强氮化物复合材料及制备和打印方法
CN115073171A (zh) * 2022-06-29 2022-09-20 清华大学深圳国际研究生院 一种适用于光固化成型加工的ltcc生料带材料、ltcc基板及其制备方法和应用
CN115073171B (zh) * 2022-06-29 2023-08-08 清华大学深圳国际研究生院 一种适用于光固化成型加工的ltcc生料带材料、ltcc基板及其制备方法和应用

Similar Documents

Publication Publication Date Title
CN108033802A (zh) 基于凝胶注模3d打印的纤维增强陶瓷异型件成型方法
CN107043259B (zh) 一种反应烧结碳化硅陶瓷激光选区烧结成型方法
CN106278201B (zh) 一种直接成型3d陶瓷打印用瘠性陶瓷粉体浆料及其制备方法和应用
CN107353036B (zh) 一种基于增材制造技术的多孔氮化硅陶瓷、其制备方法及其应用
CN104526838B (zh) 陶瓷3d打印成型的方法
CN108069706A (zh) 一种基于3d打印技术的纤维增强陶瓷薄壁件的成型方法
CN111233485B (zh) 基于高固含量硅系浆料3d打印直写成型复杂结构陶瓷的方法
CN106278335B (zh) 一种纤维定向增韧陶瓷基复合材料涡轮叶片的制造方法
CN105269654A (zh) 碳化硅反射镜的3d打印制备方法
CN106495699A (zh) 一种SLS技术与PIP技术相结合制备高强度耐高温SiC陶瓷导弹头外壳的方法
US5678162A (en) Mold useful for injection molding of plastics, and methods of production and uses thereof
CN105541336A (zh) 一种碳化硼/碳化硅陶瓷整板及其制备方法与应用
CN107032826B (zh) 一种空心氧化铝球/碳化硅增强铜基复合材料的制备方法
CN113880559A (zh) 一种基于光固化成形的难固化陶瓷的制备方法及产品
CN103643067A (zh) 一种纳米级碳化硅增强金属基复合材料及其制备方法
CN109482886A (zh) 一种3d打印陶瓷与纤维复合增强铝基材料的制备方法
CN103553632A (zh) 一种致密化氮化硅陶瓷材料的制备方法
CN108017378A (zh) 一种水性氧化铝基3d打印坯体方法及其成型方法
CN115894041A (zh) 一种粉末挤出3d打印成型反应烧结碳化硅陶瓷的制备方法
CN109108288B (zh) 一种粉末注射成形制备空心球金属基轻质复合材料的方法
Wang et al. Near‐net shape forming of advanced ceramics
CN105175851B (zh) 一种精密铸造蜡及其制备方法和用途
CN116813354B (zh) 一种原位制备氮化硅陶瓷的方法、制得的氮化硅陶瓷及其应用
CN110627506B (zh) 一种结合3D打印制备Cf/SiC晶舟的方法
CN107033532A (zh) 一种掺氮化硼纳米片及氮化铝纳米颗粒的3d打印用改性abs和pp材料及其制备方法

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
RJ01 Rejection of invention patent application after publication

Application publication date: 20180515

RJ01 Rejection of invention patent application after publication