CN107759228B - 一种六方氮化硼陶瓷的凝胶注模成型方法 - Google Patents
一种六方氮化硼陶瓷的凝胶注模成型方法 Download PDFInfo
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Abstract
本发明涉及一种六方氮化硼陶瓷的凝胶注模成型方法,包括以下步骤:步骤一、将六方氮化硼粉体原料进行热压烧结以获得烧结体;步骤二、将步骤一所述烧结体经破碎和球磨工艺,获得六方氮化硼粉体;步骤三、将步骤二所述六方氮化硼粉体进行胶注模成型,制备六方氮化硼陶瓷坯体。本发明的方法使六方氮化硼颗粒的形状由片状变为类球状,改善了六方氮化硼颗粒在水中的分散效果,解决了现有六方氮化硼陶瓷凝胶注模成型中的固相含量低,流动性差的问题,有效提高了浆料固相含量并获得流动性较好的浆料,从而使近净成形制备六方氮化硼陶瓷成为可能,避免或减少后加工工序,进而降低六方氮化硼陶瓷的生产成本。
Description
技术领域
本发明涉及陶瓷材料制备成型技术领域,尤其涉及一种六方氮化硼陶瓷的凝胶注模成型方法。
背景技术
六方氮化硼陶瓷由于具有热导率高、热膨胀系数小、抗热震性好、耐高温、耐腐蚀和电绝缘性能好等优点,在电子、冶金、化工、航空航天等领域有着广泛的应用前景。
传统的六方氮化硼陶瓷制备工艺为将六方氮化硼粉体和烧结助剂一起热压烧结,再进行机械加工,得到六方氮化硼陶瓷制品。虽然六方氮化硼陶瓷是软质材料,但加工工序会增加生产周期和成本,而且产生粉尘污染。
凝胶注模成型是一种陶瓷近净成形技术,制备的陶瓷产品不需要或者需要极少的后加工,能大大降低生产周期和成本。目前常见的凝胶注模成型用溶剂为水。片状六方氮化硼陶瓷颗粒由于颗粒之间错动非常困难,因此难以在水中分散,在凝胶注模成型中表现为浆料固相含量低,流动性差,限制了凝胶注模成型技术在六方氮化硼陶瓷产品领域的应用。
发明内容
鉴于上述的分析,本发明提供一种六方氮化硼陶瓷的凝胶注模成型方法,解决了现有六方氮化硼陶瓷凝胶注模成型中的固相含量低,流动性差的问题,从而使近净成形制备六方氮化硼陶瓷成为可能,避免或减少后加工工序,进而降低六方氮化硼陶瓷的生产成本。
本发明的目的主要是通过以下技术方案实现的:
一种六方氮化硼陶瓷的凝胶注模成型方法,所述方法包括以下步骤:
步骤一、将六方氮化硼粉体原料进行热压烧结以获得烧结体;
步骤二、将步骤一所述烧结体经破碎和球磨工艺,获得六方氮化硼粉体;
步骤三、将步骤二所述六方氮化硼粉体进行胶注模成型,制备六方氮化硼陶瓷坯体。
进一步地,所述步骤一具体为,将六方氮化硼粉体原料直接进行热压烧结,或将六方氮化硼粉体干压成型后进行热压烧结;烧结温度为1700~1900℃,烧结压力为15~30MPa,保压时间为30~120min。
为了保证六方氮化硼颗粒在加热加压的条件下发生一定程度的烧结,即晶粒长大和烧结颈形成,进而改变颗粒形状,需要选择合适的烧结工艺对六方氮化硼原料进行热压烧结处理。适当的热压烧结工艺能够改变六方氮化硼的片状结构,且烧结后获得的烧结体更加容易破碎,从而获得各向同性的氮化硼材料。
进一步地,步骤二中所述球磨工艺为,球磨转速为100~200r/min,球磨时间为10~30h,球磨介质为无水乙醇或去离子水。
进一步地,所述步骤二还包括干燥过筛工艺,其中筛网目数为80~200目。
为了得到粒度适宜的六方氮化硼粉体,需要选择合适的筛网目数对粉体进行过筛,保证六方氮化硼粉体的粒度适于在水中分散,进而有利于后续凝胶注模过程中浆料的形成。
进一步地,所述步骤三具体为,将步骤二所述六方氮化硼粉体与烧结助剂、分散剂、水混合球磨后,调节pH值,得到六方氮化硼陶瓷浆料,所述浆料真空除泡后加入引发剂球磨,在球磨后的浆料中加入催化剂并搅拌均匀,注入模具,经加热固化、脱模、干燥,得到六方氮化硼坯体。
进一步地,所述步骤三中,六方氮化硼粉体与烧结助剂、分散剂、水混合后球磨时间为8~24h,采用氨水和稀盐酸调节pH值,得到六方氮化硼陶瓷浆料,所得浆料真空除泡10~50min后加入引发剂球磨8~15h,然后在浆料中加入催化剂并搅拌均匀,将浆料注入模具,在55~85℃条件下加热固化20~50min后脱模,然后干燥24~36h,得到六方氮化硼坯体。
适当的加热固化温度和时间可以保证浆料完全固化而又不过于干燥,从而有利于脱模,干燥时间过短会影响陶瓷坯体的强度,时间过长又会导致坯体开裂,因此需要将加热温度设置在55~85℃条件下,干燥时间为24~36h。
进一步地,调节pH值后所得的六方氮化硼陶瓷浆料固相含量为50~60vol%。
进一步地,所述分散剂为聚乙烯吡咯烷酮、聚丙烯酸、四甲基氢氧化铵、聚乙二醇中的至少一种。
本发明采用的分散剂体系针对热压烧结后的六方氮化硼粉体,此粉体虽然为类球状的颗粒团聚体,但颗粒表面仍然是疏水性结构,因此需要选择合适的分散剂,使六方氮化硼表面由疏水性变为亲水性,分散剂的选取原则主要基于两种分散稳定机理:静电效应机理和空间效应机理。聚丙烯酸和四甲基氢氧化铵属于离子型分散剂,易溶于水,表面张力小,不仅产生空间位阻而且产生静电斥力,具有良好的分散性,聚乙烯吡咯烷酮和聚乙二醇属于非离子型分散剂,吸附在六方氮化硼颗粒表面形成一层高分子保护膜,使六方氮化硼表面由疏水性变为亲水性,同时在空间上起到了阻隔颗粒相互碰撞防止团聚的作用,从而增强了六方氮化硼在水中的分散稳定性。
进一步地,所述分散剂的质量为陶瓷粉体质量的1~6%。
为了保证粉体能在水中稳定分散,需要加入一定量的分散剂,但分散剂过多则会导致分散剂形成胶束,反而阻碍粉体分散,因此需要将分散剂的质量限制在陶瓷粉体质量的1~6%范围内,既能保证粉体的分散效果,又不会形成胶束阻碍粉体分散。
进一步地,所述六方氮化硼粉体原料的粒径为D50=0.2~3μm,纯度98%以上。
本发明有益效果如下:
本发明提供一种六方氮化硼陶瓷的凝胶注模成型方法,将六方氮化硼原料粉体进行热压烧结,并对六方氮化硼烧结体破碎、球磨后过筛处理,获得六方氮化硼粉体再进行凝胶注模工艺,通过优化工艺参数,制备六方氮化硼陶瓷坯体。传统六方氮化硼陶瓷的制备工艺需要后加工工艺,增加生产周期和成本,凝胶注模成型工艺是一种近净成形工艺,制备的陶瓷产品不需要或者需要极少的后加工,但普通六方氮化硼粉体由于片状结构,在水中分散困难。本发明采用将六方氮化硼粉体热压烧结然后破碎球磨的方法使六方氮化硼颗粒的形状由片状变为类球状,改善了六方氮化硼颗粒在水中的分散效果,解决了现有六方氮化硼陶瓷凝胶注模成型中的固相含量低,流动性差的问题,有效提高了浆料固相含量并获得流动性较好的浆料,从而使近净成形制备六方氮化硼陶瓷成为可能,避免或减少后加工工序,进而降低陶瓷的生产成本。
本发明的其他特征和优点将在随后的说明书中阐述,并且,部分可从说明书中变得显而易见,或者通过实施本发明而了解。本发明的目的和其他优点可通过在所写的说明书以及权利要求书中所特别指出的结构来实现和获得。
具体实施方式
下面结合实施例一起用于阐释本发明的原理。
本发明提供一种六方氮化硼陶瓷的凝胶注模成型方法,该方法包括如下步骤:
(1)将六方氮化硼粉体或干压成型后的六方氮化硼坯体装入石墨模具内进行热压烧结,烧结温度1700~1900℃,压力15~30MPa,保压时间30~120min,烧结制度的选取原则是保证六方氮化硼颗粒在加热加压的条件下发生一定程度的烧结,即晶粒长大和烧结颈形成,进而改变颗粒形状。
(2)将步骤(1)所得六方氮化硼烧结体破碎、球磨后过筛,筛网目数80~200目,筛网目数的选取原则是保证六方氮化硼粉体的粒度适于在水中分散。
(3)将步骤(2)所得六方氮化硼粉体与烧结助剂、分散剂、水混合后球磨8~24h,用氨水和稀盐酸调节浆料的pH值,pH值根据六方氮化硼粉体的Zeta电位值决定,然后得到固相含量50~60vol%的六方氮化硼陶瓷浆料,所得浆料真空除泡10~50min后加入引发剂球磨8~15h,然后在浆料中加入催化剂后搅拌均匀,确认浆料中无明显气泡后将浆料注入模具,55~85℃加热固化20~50min后脱模,适当的加热温度和时间可以保证浆料完全固化但不过于干燥,从而有利于脱模,然后将坯体干燥24~36h,干燥时间过短会影响坯体强度,时间过长会导致坯体开裂,干燥后得到六方氮化硼坯体。所用分散剂为聚乙烯吡咯烷酮、聚丙烯酸、四甲基氢氧化铵、聚乙二醇中的一种或几种,其质量为六方氮化硼粉体质量的1~6%,分散剂加入量的选取依据是保证粉体能在水中稳定分散,过多会导致分散剂形成胶束,反而阻碍粉体分散。
普通六方氮化硼粉体呈各向异性的片状,比表面积大(7.648m2·g-1),与水的润湿性差,导致在水中分散困难。经过热压烧结后的六方氮化硼粉体比表面积(3.659m2·g-1)较普通六方氮化硼小。适当的热压烧结工艺改变了六方氮化硼的片状结构,且烧结后容易破碎,从而获得各向同性的氮化硼材料。经过破碎、球磨和过筛获得的六方氮化硼有许多类球状团聚颗粒,这种团聚不容易在水中被破坏,从而有利于稳定分散。
本发明采用的分散剂体系针对热压烧结后的六方氮化硼粉体,此粉体虽然为类球状的颗粒团聚体,但颗粒表面仍然是疏水性结构,分散剂的选取原则主要基于两种分散稳定机理:静电效应机理和空间效应机理。聚丙烯酸和四甲基氢氧化铵属于离子型分散剂,易溶于水,表面张力小,不仅产生空间位阻而且产生静电斥力,具有良好的分散性,聚乙烯吡咯烷酮和聚乙二醇属于非离子型分散剂,吸附在六方氮化硼颗粒表面形成一层高分子保护膜,使六方氮化硼表面由疏水性变为亲水性,同时在空间上起到了阻隔颗粒相互碰撞防止团聚的作用,从而增强了六方氮化硼在水中的分散稳定性。
本发明的优点在于,传统六方氮化硼陶瓷的制备工艺需要后加工工艺,增加生产周期和成本,凝胶注模成型工艺是一种近净成形工艺,制备的陶瓷产品不需要或者需要极少的后加工,但普通六方氮化硼粉体由于片状结构,在水中分散困难,采用将六方氮化硼粉体热压烧结然后破碎球磨的方法使六方氮化硼颗粒的形状由片状变为类球状,改善了六方氮化硼颗粒在水中的分散效果,有效提高了浆料固相含量并获得流动性较好的浆料,从而使近净成形制备六方氮化硼陶瓷成为可能,避免或减少后加工工序,从而降低生产成本。
实施例
1.六方氮化硼原料粒度D50=0.2~3μm,纯度98%以上;凝胶注模成型所用化学试剂均为分析纯。
2.将六方氮化硼粉料装入石墨模具,置于热压烧结炉中烧结。烧结制度为10℃/min升温至1850℃,加压20MPa,保温保压60min,随后卸压随炉冷却,烧结气氛为氩气。
3.将得到的六方氮化硼烧结体在颚式破碎机中破碎后装入球磨罐中,通过行星球磨机进行球磨,球磨介质为无水乙醇,磨球为氧化锆,球磨转速150r/min,球磨时间15h。将球磨后的浆料干燥后过80目筛,得到六方氮化硼粉体。
4.将600g步骤3得到的六方氮化硼粉体和适量烧结助剂、20g聚丙烯酸和260g水混合,用氨水和稀盐酸调节浆料的pH值,球磨10h后真空脱泡30min,得到固相含量50vol%的陶瓷浆料;在浆料中加入6g过硫酸铵后球磨10h;将2g四甲基乙二胺加入浆料中,搅拌5min后注入塑料模具;将模具置于60℃的烘箱中加热35min后脱模;脱模后的坯体在80℃的烘箱中干燥24h,得到干燥后的六方氮化硼坯体。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。
Claims (6)
1.一种六方氮化硼陶瓷的凝胶注模成型方法,其特征在于,所述方法包括以下步骤:
步骤一、将六方氮化硼粉体原料进行热压烧结以获得烧结体;将六方氮化硼粉体原料直接进行热压烧结,或将六方氮化硼粉体干压成型后进行热压烧结;烧结温度为1700~1900℃,烧结压力为15~30MPa,保压时间为30~120min;
步骤二、将步骤一所述烧结体经破碎和球磨工艺,获得六方氮化硼粉体;球磨转速为100~200r/min,球磨时间为10~30h,球磨介质为无水乙醇或去离子水;
步骤三、将步骤二所述六方氮化硼粉体进行胶注模成型,制备六方氮化硼陶瓷坯体;
所述步骤三具体为,将步骤二所述六方氮化硼粉体与烧结助剂、分散剂、水混合球磨后,调节pH值,得到六方氮化硼陶瓷浆料,所述浆料真空除泡后加入引发剂球磨,在球磨后的浆料中加入催化剂并搅拌均匀,注入模具,经加热固化、脱模、干燥,得到六方氮化硼坯体;
六方氮化硼粉体热压烧结然后破碎球磨的方法使六方氮化硼颗粒的形状由片状变为类球状;
所述分散剂为聚乙烯吡咯烷酮、聚丙烯酸、四甲基氢氧化铵、聚乙二醇中的至少一种;聚丙烯酸和四甲基氢氧化铵属于离子型分散剂,聚乙烯吡咯烷酮和聚乙二醇属于非离子型分散剂。
2.根据权利要求1所述六方氮化硼陶瓷的凝胶注模成型方法,其特征在于,所述步骤二还包括干燥过筛工艺,其中筛网目数为80~200目。
3.根据权利要求1所述六方氮化硼陶瓷的凝胶注模成型方法,其特征在于,所述步骤三中,六方氮化硼粉体与烧结助剂、分散剂、水混合后球磨时间为8~24h,采用氨水和稀盐酸调节pH值,得到六方氮化硼陶瓷浆料,所得浆料真空除泡10~50min后加入引发剂球磨8~15h,然后在浆料中加入催化剂并搅拌均匀,将浆料注入模具,在55~85℃条件下加热固化20~50min后脱模,然后干燥24~36h,得到六方氮化硼坯体。
4.根据权利要求1或2所述六方氮化硼陶瓷的凝胶注模成型方法,其特征在于,调节pH值后所得的六方氮化硼陶瓷浆料固相含量为50~60vol%。
5.根据权利要求4所述六方氮化硼陶瓷的凝胶注模成型方法,其特征在于,所述分散剂的质量为陶瓷粉体质量的1~6%。
6.根据权利要求1-3,5中任一项所述六方氮化硼陶瓷的凝胶注模成型方法,其特征在于,所述六方氮化硼粉体原料的粒径为D50=0.2~3μm,纯度98%以上。
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