CN110981452A - 一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺 - Google Patents

一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺 Download PDF

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CN110981452A
CN110981452A CN201911294626.7A CN201911294626A CN110981452A CN 110981452 A CN110981452 A CN 110981452A CN 201911294626 A CN201911294626 A CN 201911294626A CN 110981452 A CN110981452 A CN 110981452A
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oxide
polyethylene glycol
graphene oxide
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胡宏武
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Anhui Cloud Digital Push Network Technology Co Ltd
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Abstract

本发明提供了一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,涉及陶瓷刀具技术领域,制备工艺包括以下步骤:(1)氧化石墨烯加入至无水乙醇中,加入聚乙二醇、氧化铝粉体,得粉体浆料I;(2)将无水乙醇与聚乙二醇混合,加入β‑SiC纳米颗粒和TiC晶须、烧结助剂,得粉体浆料II;(3)球磨,得复合浆料;(4)干燥、过筛,得复合粉体;(5)预压成型;(6)将预压成型的坯体进行真空热压烧结。本发明提中石墨烯、TiC晶须、β‑SiC纳米颗粒协同作用,补强增韧效果好,制备过程中各原料分散性高,制备得到的陶瓷刀具的力学性能优异,其韧性、强度高,且耐磨性好。

Description

一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺
技术领域
本发明涉及陶瓷刀具技术领域,具体涉及一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺。
背景技术
氧化铝基陶瓷刀具材料凭借其优异的性能和相对低廉的制备成本,被广泛应用于切削加工领域。Al2O3基陶瓷刀具可分为:(1)纯氧化铝陶瓷,当Al2O3在材料中的含量高达99.99%及以上时,材料呈白色,由此俗称白陶瓷。(2)氧化铝-碳化物复合陶瓷,Al2O3基体中添加碳化物后热压烧结的陶瓷便是这种类型,常见的碳化物是TiC、Mo2C、WC等。(3)氧化铝-TiC-金属复合陶瓷,在氧化铝-TiC复合陶瓷中添加金属颗粒,如Ni、Mo等,从而提高了氧化铝和碳化钛的连接强度,这类陶瓷又称为金属陶瓷。(4)晶须增韧陶瓷刀具,在基体材料中添加晶须烧制而成。典型的Al2O3-SiCw就是在Al2O3的基体中加入SiC晶须后烧制得到的。(5)梯度功能陶瓷刀具,有Al2O3-TiC梯度功能陶瓷刀具。
现代的陶瓷材料的强度、硬度高,并且在高温时仍保持优异的性能。但其断裂韧性低,脆性大,导致其抗冲击性弱,可靠性较低。因此,为了克服陶瓷材料的脆性弱点,提高其抗破坏性,增加使用可靠性,各国学者都开始致力于研究如何改善陶瓷材料的断裂韧性。材料的断裂需要能量的提供,其他形式将能量吸收就会阻止裂纹扩展。固体主要靠两种方式吸收能量:材料的变形和形成新的表面。陶瓷材料的晶体排列和键位组合是不可滑移变形的根本原因。因此可知,陶瓷材料的脆性弱点是由物质化学键性质和微观结构决定的。
氧化铝基复合陶瓷材料具有强度高、刚度高、耐摩擦和耐高温等优异性能,在切削刀具中应用广泛。陶瓷材料刀具的缺点是脆性较大,因此需要通过陶瓷增韧技术对陶瓷材料进行增韧。研究表明,对氧化铝陶瓷增韧主要有颗粒、晶须和纤维增韧三种方式,其中颗粒由于具有容易获得、生产成本低和工艺流程简单等特点,在陶瓷增韧技术中应用最多。
申请号为201610347928.6的中国专利公开了一种具有各向异性的石墨烯增韧Al2O3纳米复合陶瓷刀具材料及其制备方法。该陶瓷刀具材料是以Al2O3为基体,石墨烯纳米片为增强相,MgO、Mo和Ni为烧结助剂。该陶瓷刀具材料经石墨烯分散、复合粉体制备、干燥过筛、冷压装模和热压烧结而成。该发明所制备的石墨烯增韧Al2O3纳米复合陶瓷材料中,石墨烯增韧效果显著,且在基体中取向性明显。但是在该发明中虽然石墨烯其具有较好的增韧效果,但是石墨烯片层之间存在强的范德华力,片层之间很难实现良好的分散,从而使其增韧效果大打折扣。
发明内容
针对现有技术的不足,本发明提供一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,石墨烯、TiC晶须、β-SiC纳米颗粒协同作用,补强增韧效果好,制备过程中各原料分散性高,制备得到的陶瓷刀具的力学性能优异,其韧性、强度高,且耐磨性好。
为实现以上目的,本发明通过以下技术方案予以实现:
一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,包括以下步骤:
(1)将0.3-1份氧化石墨烯加入至无水乙醇中,机械搅拌10-15min后加入聚乙二醇,机械搅拌15-20min后加入60-75份氧化铝粉体,同时进行超声振动和机械搅拌30-40min后,得粉体浆料I;
(2)将无水乙醇与聚乙二醇混合,同时进行超声振动和机械搅拌,15-20min后加入10-16份β-SiC纳米颗粒和13-18份TiC晶须,同时进行超声振动和机械搅拌40-60min后,加入0.7-1.3份烧结助剂,同时进行超声振动和机械搅拌20-30min后,得粉体浆料II;
(3)将粉体浆料I置于球磨机中,在氮气气氛下,球磨60-70h后,加入粉体浆料II,继续在氮气气氛下球磨9-12h,得复合浆料;
(4)将经过球磨后所得复合浆料置于干燥箱中,干燥完成后过200目筛,得混合均匀的复合粉体;
(5)将复合粉体进行预压成型;
(6)将预压成型的坯体进行真空热压烧结,先以100-120℃/min的速度升温至1050-1180℃,保温10-15min,再以16-20℃/min的升温速度升温至1680-1730℃,保温20-25min,热压压力52-60MPa;之后随炉冷却至750-780℃时,通过风冷降温至240-260℃,再置于240-260℃的炉中随炉冷至室温,即得陶瓷刀具。
优选地,步骤(1)中,氧化石墨烯厚度为0.5-5nm;氧化铝为α-氧化铝,氧化铝粉体的平均粒径为200-400nm。
优选地,步骤(2)中,TiC晶须的直径为1-5μm,长径比为50-200。
优选地,步骤(2)中,β-SiC纳米颗粒由以下重量百分比成分组成:平均粒径为75-90nm的β-SiC纳米颗粒20-40%,平均粒径为10-20nm的β-SiC纳米颗粒60-80%。
优选地,步骤(2)中,烧结助剂为氧化钇、氧化镧、氧化铈、氧化镁、氧化钙中的一种或者多种。进一步优选地,烧结助剂为氧化钇、氧化镧、氧化镁按质量比1:0.5-0.8:0.2-0.3混合而成。
优选地,粉体浆料I中,聚乙二醇为聚乙二醇4000或聚乙二醇5000,聚乙二醇的含量为22-35g/L;
粉体浆料II中,聚乙二醇为聚乙二醇2000或聚乙二3000,聚乙二醇的含量为4-7g/L。
优选地,步骤(3)中,球料比为10-14:1。
优选地,步骤(4)中,干燥的温度为120-130℃。
优选地,步骤(5)中,预压压力为20-30MPa,保压时间为2-3min。
本发明的有益效果是:
本发明在陶瓷材料中加入氧化石墨烯作为增韧材料,氧化石墨烯其分散性较石墨烯好,同时通过优化的混合、研磨工艺,使氧化石墨烯在复合粉体中具有很好的分散性。后续真空热压烧结时,先快速升温至1050-1180℃,氧化石墨烯脱除含氧基团并且实现氧化石墨烯的充分剥离,从而能实现氧化石墨烯的还原从而转变成石墨烯,可有效解决石墨烯分散性差的问题,并实现很好的增韧效果,并使陶瓷刀具的强度显著增加。
在陶瓷刀具中加入适量的TiC晶须具有很好的晶须侨联、晶须拔出和裂纹偏转作用,增韧效果好,并使陶瓷刀具的强度和硬度均有所提高,但是TiC晶须在陶瓷刀具材料在真空热压烧结后晶须有分布均匀的现象,在此基础上,相应量的β-SiC纳米颗粒和还原后所得石墨烯,均可在一定程度上有效消除TiC晶须的分布各项异性,三者协同作用,补强增韧效果好,从而使综合性能更加优异。其中当β-SiC纳米颗粒由不同颗粒级别的β-SiC组成时,其效果更好。适量的TiC晶须还可使得陶瓷材料都的耐磨性和热稳定性均有显著改善,氧化铝基陶瓷中加入TiC晶须,在烧结过程中,氧化铝与TiC晶须基体界面通过化学反应生成碳氧化钛化物,TiC晶须与氧化铝界面之间的结合力加强,从而使陶瓷刀具的机械强度增加。
在制备陶瓷刀具的过程中,先将含有氧化铝粉体和氧化石墨烯的粉体浆料I进行研磨,可保证氧化石墨烯的分散性,之后再加入含有β-SiC纳米颗粒TiC晶须的粉体浆料II,即可使各原料获得均匀稳定的分散性,同时可防止TiC晶须因长时间研磨而造成机械损伤,从而使补强增韧的效果达到最佳。在烧结过程中,合理控制烧结温度、时间、升温速度,使韧性、强度提高,冷却时结合炉冷+水冷+炉冷,使陶瓷刀具组织稳定均匀,无缺陷、无应力,综合性能优异。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例,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作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:
一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,包括以下步骤:
(1)将0.7份氧化石墨烯加入至无水乙醇中,机械搅拌12min后加入聚乙二醇4000,机械搅拌20min后加入70份α-氧化铝粉体,同时进行超声振动和机械搅拌35min后,得粉体浆料I,粉体浆料I中聚乙二醇4000的含量为28g/L;
氧化石墨烯厚度为1-3nm;α-氧化铝粉体的平均粒径为300nm。
(2)将无水乙醇与聚乙二醇2000混合,同时进行超声振动和机械搅拌,18min后加入15份β-SiC纳米颗粒和15份TiC晶须,同时进行超声振动和机械搅拌50min后,加入1份烧结助剂,同时进行超声振动和机械搅拌25min后,得粉体浆料II,粉体浆料II中聚乙二醇2000的含量为5g/L;
TiC晶须的直径为1-3μm,长径比为100-150;β-SiC纳米颗粒由以下重量百分比成分组成:平均粒径为80nm的β-SiC纳米颗粒30%,平均粒径为15nm的β-SiC纳米颗粒70%;
烧结助剂为氧化钇、氧化镧、氧化镁按质量比1:0.5:0.2混合而成。
(3)将粉体浆料I置于球磨机中,在氮气气氛下,球料比为12:1,球磨65h后,加入粉体浆料II,继续在氮气气氛下球磨10h,得复合浆料;
(4)将经过球磨后所得复合浆料置于干燥箱中,干燥的温度为125℃,干燥完成后过200目筛,得混合均匀的复合粉体。
(5)将复合粉体进行预压成型,预压压力为25MPa,保压时间为2min。
(6)将预压成型的坯体进行真空热压烧结,先以115℃/min的速度升温至1100℃,保温12min,再以18℃/min的升温速度升温至1700℃,保温22min,热压压力56MPa;之后随炉冷却至760℃时,通过风冷降温至245℃,再置于245℃的炉中随炉冷至室温,即得陶瓷刀具。
实施例2:
一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,包括以下步骤:
(1)将0.5份氧化石墨烯加入至无水乙醇中,机械搅拌15min后加入聚乙二醇5000,机械搅拌18min后加入70份α-氧化铝粉体,同时进行超声振动和机械搅拌40min后,得粉体浆料I,粉体浆料I中聚乙二醇5000的含量为30g/L;
氧化石墨烯厚度为0.5-2nm;α-氧化铝粉体的平均粒径为400nm。
(2)将无水乙醇与聚乙二醇2000混合,同时进行超声振动和机械搅拌,15min后加入15份β-SiC纳米颗粒和13份TiC晶须,同时进行超声振动和机械搅拌60min后,加入0.7份烧结助剂,同时进行超声振动和机械搅拌25min后,得粉体浆料II,粉体浆料II中聚乙二醇2000的含量为4g/L;
TiC晶须的直径为1-3μm,长径比为100-150;β-SiC纳米颗粒由以下重量百分比成分组成:平均粒径为90nm的β-SiC纳米颗粒20%,平均粒径为20nm的β-SiC纳米颗粒80%;
烧结助剂为氧化钇、氧化镧、氧化镁按质量比1:0.8:0.2混合而成。
(3)将粉体浆料I置于球磨机中,在氮气气氛下,球料比为10:1,球磨60h后,加入粉体浆料II,继续在氮气气氛下球磨9h,得复合浆料。
(4)将经过球磨后所得复合浆料置于干燥箱中,干燥的温度为120℃,干燥完成后过200目筛,得混合均匀的复合粉体。
(5)将复合粉体进行预压成型,预压压力为30MPa,保压时间为2min。
(6)将预压成型的坯体进行真空热压烧结,先以120℃/min的速度升温至1120℃,保温12min,再以18℃/min的升温速度升温至1680℃,保温25min,热压压力52MPa;之后随炉冷却至780℃时,通过风冷降温至255℃,再置于255℃的炉中随炉冷至室温,即得陶瓷刀具。
实施例3:
一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,包括以下步骤:
(1)将0.3份氧化石墨烯加入至无水乙醇中,机械搅拌10min后加入聚乙二醇4000,机械搅拌15min后加入60份α-氧化铝粉体,同时进行超声振动和机械搅拌30min后,得粉体浆料I,粉体浆料I中聚乙二醇4000的含量为22g/L;
氧化石墨烯厚度为3-5nm;α-氧化铝粉体的平均粒径为200nm。
(2)将无水乙醇与聚乙二醇3000混合,同时进行超声振动和机械搅拌,20min后加入10份β-SiC纳米颗粒和18份TiC晶须,同时进行超声振动和机械搅拌40min后,加入1.3份烧结助剂,同时进行超声振动和机械搅拌20min后,得粉体浆料II,粉体浆料II中聚乙二醇3000的含量为6g/L;
TiC晶须的直径为3-5μm,长径比为50-100;β-SiC纳米颗粒由以下重量百分比成分组成:平均粒径为75nm的β-SiC纳米颗粒40%,平均粒径为10nm的β-SiC纳米颗粒60%;
烧结助剂为氧化钇、氧化镧、氧化镁按质量比1:0.5:0.3混合而成。
(3)将粉体浆料I置于球磨机中,在氮气气氛下,球料比为14:1,球磨70h后,加入粉体浆料II,继续在氮气气氛下球磨12h,得复合浆料。
(4)将经过球磨后所得复合浆料置于干燥箱中,干燥的温度为130℃,干燥完成后过200目筛,得混合均匀的复合粉体。
(5)将复合粉体进行预压成型,预压压力为20MPa,保压时间为3min。
(6)将预压成型的坯体进行真空热压烧结,先以100℃/min的速度升温至1050℃,保温10min,再以16℃/min的升温速度升温至1710℃,保温20min,热压压力58MPa;之后随炉冷却至750℃时,通过风冷降温至240℃,再置于240℃的炉中随炉冷至室温,即得陶瓷刀具。
实施例4:
一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,包括以下步骤:
(1)将1份氧化石墨烯加入至无水乙醇中,机械搅拌12min后加入聚乙二醇5000,机械搅拌20min后加入75份α-氧化铝粉体,同时进行超声振动和机械搅拌35min后,得粉体浆料I,粉体浆料I中聚乙二醇5000的含量为35g/L;
氧化石墨烯厚度为1-3nm;α-氧化铝粉体的平均粒径为300nm。
(2)将无水乙醇与聚乙二醇2000混合,同时进行超声振动和机械搅拌,18min后加入16份β-SiC纳米颗粒和15份TiC晶须,同时进行超声振动和机械搅拌50min后,加入1份烧结助剂,同时进行超声振动和机械搅拌30min后,得粉体浆料II,粉体浆料II中聚乙二醇2000的含量为7g/L;
TiC晶须的直径为2-4μm,长径比为150-200;β-SiC纳米颗粒由以下重量百分比成分组成:平均粒径为80nm的β-SiC纳米颗粒30%,平均粒径为15nm的β-SiC纳米颗粒70%;
烧结助剂为氧化铈、氧化钙按质量比1:1混合而成。
(3)将粉体浆料I置于球磨机中,在氮气气氛下,球料比为12:1,球磨65h后,加入粉体浆料II,继续在氮气气氛下球磨10h,得复合浆料。
(4)将经过球磨后所得复合浆料置于干燥箱中,干燥的温度为125℃,干燥完成后过200目筛,得混合均匀的复合粉体。
(5)将复合粉体进行预压成型,预压压力为25MPa,保压时间为2.5min。
(6)将预压成型的坯体进行真空热压烧结,先以110℃/min的速度升温至1180℃,保温15min,再以20℃/min的升温速度升温至1730℃,保温22min,热压压力60MPa;之后随炉冷却至760℃时,通过风冷降温至260℃,再置于260℃的炉中随炉冷至室温,即得陶瓷刀具。
实施例5:
一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,包括以下步骤:
(1)将0.8份氧化石墨烯加入至无水乙醇中,机械搅拌15min后加入聚乙二醇4000,机械搅拌18min后加入65份α-氧化铝粉体,同时进行超声振动和机械搅拌35min后,得粉体浆料I,粉体浆料I中聚乙二醇4000的含量为30g/L;
氧化石墨烯厚度为2-4nm;α-氧化铝粉体的平均粒径为300nm。
(2)将无水乙醇与聚乙二醇3000混合,同时进行超声振动和机械搅拌,20min后加入13份β-SiC纳米颗粒和15份TiC晶须,同时进行超声振动和机械搅拌50min后,加入1份烧结助剂氧化铈,同时进行超声振动和机械搅拌20min后,得粉体浆料II,粉体浆料II中聚乙二醇3000的含量为6g/L;
TiC晶须的直径为1-3μm,长径比为50-100;β-SiC纳米颗粒由以下重量百分比成分组成:平均粒径为80nm的β-SiC纳米颗粒35%,平均粒径为15nm的β-SiC纳米颗粒65%;
(3)将粉体浆料I置于球磨机中,在氮气气氛下,球料比为12:1,球磨65h后,加入粉体浆料II,继续在氮气气氛下球磨10h,得复合浆料;
(4)将经过球磨后所得复合浆料置于干燥箱中,干燥的温度为130℃,干燥完成后过200目筛,得混合均匀的复合粉体。
(5)将复合粉体进行预压成型,预压压力为20MPa,保压时间为3min。
(6)将预压成型的坯体进行真空热压烧结,先以110℃/min的速度升温至1090℃,保温12min,再以18℃/min的升温速度升温至1700℃,保温22min,热压压力56MPa;之后随炉冷却至760℃时,通过风冷降温至245℃,再置于245℃的炉中随炉冷至室温,即得陶瓷刀具。
实施例6:
一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,包括以下步骤:
(1)将0.8份氧化石墨烯加入至无水乙醇中,机械搅拌10min后加入聚乙二醇4000,机械搅拌20min后加入70份α-氧化铝粉体,同时进行超声振动和机械搅拌40min后,得粉体浆料I,粉体浆料I中聚乙二醇4000的含量为30g/L;
氧化石墨烯厚度为2-4nm;α-氧化铝粉体的平均粒径为320nm。
(2)将无水乙醇与聚乙二醇2000混合,同时进行超声振动和机械搅拌,15min后加入15份β-SiC纳米颗粒和15份TiC晶须,同时进行超声振动和机械搅拌55min后,加入1.1份烧结助剂,同时进行超声振动和机械搅拌25min后,得粉体浆料II,粉体浆料II中聚乙二醇2000的含量为4-7g/L;
TiC晶须的直径为3-5μm,长径比为100-150;β-SiC纳米颗粒由以下重量百分比成分组成:平均粒径为85nm的β-SiC纳米颗粒25%,平均粒径为15nm的β-SiC纳米颗粒75%;
烧结助剂为氧化钇、氧化钙按质量比3:1组成。
(3)将粉体浆料I置于球磨机中,在氮气气氛下,球料比为13:1,球磨65h后,加入粉体浆料II,继续在氮气气氛下球磨10h,得复合浆料;
(4)将经过球磨后所得复合浆料置于干燥箱中,干燥的温度为125℃,干燥完成后过200目筛,得混合均匀的复合粉体。
(5)将复合粉体进行预压成型,预压压力为22MPa,保压时间为2min。
(6)将预压成型的坯体进行真空热压烧结,先以115℃/min的速度升温至1120℃,保温12min,再以17℃/min的升温速度升温至1700℃,保温20min,热压压力58MPa;之后随炉冷却至780℃时,通过风冷降温至260℃,再置于260℃的炉中随炉冷至室温,即得陶瓷刀具。
对比例1:
一种氧化铝基陶瓷刀具的制备工艺,其步骤(1)为:将无水乙醇中加入聚乙二醇4000,机械搅拌20min后加入70份α-氧化铝粉体,同时进行超声振动和机械搅拌35min后,得粉体浆料I,粉体浆料I中聚乙二醇4000的含量为28g/L;氧化石墨烯厚度为1-3nm;α-氧化铝粉体的平均粒径为300nm。
步骤(2)、(3)、(4)、(5)、(6)同实施例1。
对比例2:
一种氧化铝基陶瓷刀具的制备工艺,其步骤(2)为:将无水乙醇与聚乙二醇2000混合,同时进行超声振动和机械搅拌,18min后加入30份β-SiC纳米颗粒,同时进行超声振动和机械搅拌50min后,加入1份烧结助剂,同时进行超声振动和机械搅拌25min后,得粉体浆料II,粉体浆料II中聚乙二醇2000的含量为5g/L;TiC晶须的直径为2-3μm,长径比为100-150;β-SiC纳米颗粒由以下重量百分比成分组成:平均粒径为80nm的β-SiC纳米颗粒30%,平均粒径为15nm的β-SiC纳米颗粒70%;烧结助剂为氧化钇、氧化镧、氧化镁按质量比1:0.5:0.2混合而成。
步骤(1)、(3)、(4)、(5)、(6)同实施例1。
对实施例1-6和对比例1-2中制备得到的陶瓷刀具进行性能测试,具体测试结果如表1所示。
表1:
Figure BDA0002320167780000121
Figure BDA0002320167780000131
由表1可知,本发明实施例1-6中制备得到的氧化石墨烯增韧氧化铝基陶瓷刀具中,石墨烯、TiC晶须、β-SiC纳米颗粒协同作用,补强增韧效果好,制备得到的陶瓷刀具的力学性能优异,其韧性、强度、硬度高。由对比例1-2可知,在不加入氧化石墨烯或TiC晶须时,对刀具的硬度、断裂性和抗弯强度均具有所降低。
以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。

Claims (10)

1.一种氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,其特征在于,包括以下步骤:
(1)将0.3-1份氧化石墨烯加入至无水乙醇中,机械搅拌10-15min后加入聚乙二醇,机械搅拌15-20min后加入60-75份氧化铝粉体,同时进行超声振动和机械搅拌30-40min后,得粉体浆料I;
(2)将无水乙醇与聚乙二醇混合,同时进行超声振动和机械搅拌,15-20min后加入10-16份β-SiC纳米颗粒和13-18份TiC晶须,同时进行超声振动和机械搅拌40-60min后,加入0.7-1.3份烧结助剂,同时进行超声振动和机械搅拌20-30min后,得粉体浆料II;
(3)将粉体浆料I置于球磨机中,在氮气气氛下,球磨60-70h后,加入粉体浆料II,继续在氮气气氛下球磨9-12h,得复合浆料;
(4)将经过球磨后所得复合浆料置于干燥箱中,干燥完成后过200目筛,得混合均匀的复合粉体;
(5)将复合粉体进行预压成型;
(6)将预压成型的坯体进行真空热压烧结,先以100-120℃/min的速度升温至1050-1180℃,保温10-15min,再以16-20℃/min的升温速度升温至1680-1730℃,保温20-25min,热压压力52-60MPa;之后随炉冷却至750-780℃时,通过风冷降温至240-260℃,再置于240-260℃的炉中随炉冷至室温,即得所述陶瓷刀具。
2.根据权利要求1所述的氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,其特征在于,所述步骤(1)中,氧化石墨烯厚度为0.5-5nm;所述氧化铝为α-氧化铝,氧化铝粉体的平均粒径为200-400nm。
3.根据权利要求1所述的氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,其特征在于,所述步骤(2)中,TiC晶须的直径为1-5μm,长径比为50-200。
4.根据权利要求1所述的氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,其特征在于,所述步骤(2)中,β-SiC纳米颗粒由以下重量百分比成分组成:平均粒径为75-90nm的β-SiC纳米颗粒20-40%,平均粒径为10-20nm的β-SiC纳米颗粒60-80%。
5.根据权利要求1所述的氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,其特征在于,所述步骤(2)中,烧结助剂为氧化钇、氧化镧、氧化铈、氧化镁、氧化钙中的一种或者多种。
6.根据权利要求5所述的氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,其特征在于,所述烧结助剂为氧化钇、氧化镧、氧化镁按质量比1:0.5-0.8:0.2-0.3混合而成。
7.根据权利要求1所述的氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,其特征在于,所述粉体浆料I中,聚乙二醇为聚乙二醇4000或聚乙二醇5000,聚乙二醇的含量为22-35g/L;
所述粉体浆料II中,聚乙二醇为聚乙二醇2000或聚乙二3000,聚乙二醇的含量为4-7g/L。
8.根据权利要求1所述的氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,其特征在于,所述步骤(3)中,球料比为10-14:1。
9.根据权利要求1所述的氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,其特征在于,所述步骤(4)中,干燥的温度为120-130℃。
10.根据权利要求1所述的氧化石墨烯增韧氧化铝基陶瓷刀具的制备工艺,其特征在于,所述步骤(5)中,预压压力为20-30MPa,保压时间为2-3min。
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CN112125653A (zh) * 2020-08-31 2020-12-25 江苏大学 一种基于3d打印制备的石墨烯陶瓷复合材料及其制备方法
CN113206353A (zh) * 2021-04-29 2021-08-03 湖北亿纬动力有限公司 一种电池模组用电芯连接板及其制备方法和用途
CN115849880A (zh) * 2022-11-29 2023-03-28 湖南圣瓷新材料有限公司 基于热压铸成型的陶瓷手臂的制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112125653A (zh) * 2020-08-31 2020-12-25 江苏大学 一种基于3d打印制备的石墨烯陶瓷复合材料及其制备方法
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