CN116940541A - 高韧性、高强度的氮化硅球的制造方法 - Google Patents
高韧性、高强度的氮化硅球的制造方法 Download PDFInfo
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 37
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 60
- 229910052710 silicon Inorganic materials 0.000 claims description 49
- 239000010703 silicon Substances 0.000 claims description 49
- 239000006260 foam Substances 0.000 claims description 30
- 229910052582 BN Inorganic materials 0.000 claims description 19
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 19
- 230000002706 hydrostatic effect Effects 0.000 claims description 16
- 238000000465 moulding Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 15
- 238000005238 degreasing Methods 0.000 claims description 12
- 229920003023 plastic Polymers 0.000 claims description 11
- 239000004033 plastic Substances 0.000 claims description 11
- 239000011863 silicon-based powder Substances 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 8
- 238000001694 spray drying Methods 0.000 claims description 6
- 239000008188 pellet Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- 238000004806 packaging method and process Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000004378 air conditioning Methods 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
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- 238000005538 encapsulation Methods 0.000 description 1
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- 230000001590 oxidative effect Effects 0.000 description 1
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- C01B21/00—Nitrogen; Compounds thereof
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- C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
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Abstract
本发明涉及高韧性、高强度的氮化硅球的制造方法，更具体地，涉及如下的氮化硅球的制造方法：能够大幅提高氮化硅球的生产产量，在烧结时可控制与碳之间的反应，从而能够制造高强度及高韧性的氮化硅球。
Description
技术领域
本发明涉及高韧性、高强度的氮化硅球的制造方法，更具体地，涉及如下的氮化硅球的制造方法：能够大幅提高氮化硅球的生产产量，在烧结时可控制与碳的反应，从而能够制造高强度及高韧性的氮化硅球。
背景技术
陶瓷材料因密度及热膨胀率低且高硬度及耐热特性优异而适用于各种机器部件。
因这样的特性，作为在严苛条件下使用的轴承用球的材料而广泛使用陶瓷。
目前，在酸性、碱性等条件下使用的轴承用球大部分为ZrO2系、Si3N4系，作为高温及高速轴承用球，主要使用比重比较少的Si3N4系或Al2O3系。
一般的耐蚀用轴承球材料即ZrO2根据烧结温度的上升而产生3种形式的晶体结构的相变(单斜晶→正方晶→立方晶)，在烧结之后冷却时，也会产生从正方晶变成单斜晶的相变。此时，产生4％左右的体积膨胀而导致试样被破损，因此难以进行单独的烧结。
因此，为了改善烧结性，在ZrO2中，作为稳定剂添加从Y2O3、CeO2、MgO中选择的1种而使用。在此，在ZrO2中添加Y2O3的情况下，虽然机械特性优异，但耐蚀性下降，主要使用于切割工具(Cutter)类等一般的耐磨损产品，在添加CeO2或MgO的情况下，虽然耐蚀性优异，但因过度的晶粒生长，导致机械物性不足。另一方面，在Al2O3的情况下，虽然其是硬度及耐蚀性优异的经济性的材料，但强度及耐磨特性低于其他陶瓷材料Si3N4及ZrO2，因此难以用作轴承用球。
发明内容
技术课题
本发明是为了解决上述问题而研发的，本发明的目的在于提供一种能够制造用作轴承用球的高韧性、高强度的氮化硅球的氮化硅球的制造方法。
另外，本发明的另一个目的在于提供一种能够大幅提高制造产量的氮化硅球的制造方法。
解决课题的手段
为了达到上述目的，本发明提供一种氮化硅球的制造方法，其特征在于，包括如下步骤：准备硅粉末；在上述硅粉末中添加溶剂及有机粘合剂而形成浆料；对上述浆料进行热喷雾干燥而制造具备规定的粒径的颗粒(granule)；对上述颗粒加压成型而制造硅球；使上述硅球位于软质的多孔性泡沫的各个孔中；将配置有多个硅球的多孔性泡沫放入塑料袋进行真空排气而封装；将封装后的塑料袋放入静水压机而进行静水压成型；在获得上述静水压成型的硅球之后进行脱脂；及将脱脂后的硅球氮化并烧结而制造氮化硅球。
在优选的实施例中，上述多孔性泡沫为PE泡沫，各个孔形成为圆形或多边形并贯穿上述多孔性泡沫的上表面及下表面而开放，各个孔的最大宽度大于所配置的硅球的直径。
在优选的实施例中，上述多孔性泡沫为PE泡沫，各个孔形成为圆形或多边形且仅向上述多孔性泡沫的上表面开放，在各个孔的内部安装有硅球。
在优选的实施例中，在上述脱脂的过程中还包括在上述静水压成型的硅球的外表面涂布氮化硼的步骤，由此在将硅球脱脂及烧结时控制在熔炉(furnace)的内部与碳发生反应。
在优选的实施例中，上述氮化硼以浆料形态并以湿式涂布到上述静水压成型的硅球的外表面。
发明效果
本发明具备如下的优异的效果。
根据本发明的氮化硅球的制造方法，能够在多孔性泡沫中放置多个硅球之后封装而进行静水压力成型，因此具有能够大幅提高氮化硅球制造的产量的优点。
另外，根据本发明的氮化硅球的制造方法，在静水压力成型的硅球的外表面涂布氮化硼而在脱脂及烧结时可控制与碳的反应，因此具有能够制造高韧性及高强度的氮化硅球的优点。
附图说明
图1是本发明的一个实施例的氮化硅球的制造方法的流程图。
图2是例示在本发明的一个实施例的氮化硅球的制造方法中在进行静水压成型时使用的多孔性泡沫的图。
图3是示出在本发明的一个实施例的氮化硅球的制造方法中静水压成型的硅球的图。
图4是示出在本发明的一个实施例的氮化硅球的制造方法中涂布有氮化硼的硅球的图。
(符号说明)
100：氮化硅球 200：多孔性泡沫
210：孔 300：塑料袋
310：封装的塑料袋 320：静水压成型的硅球
400：涂布有氮化硼的硅球
具体实施方式
关于本发明中使用的用语，尽量选择了目前广泛使用的一般的用语，但在特定的情况下，也有由申请人任意选定的用语，在该情况下，不应单纯地考虑用语的名称，而应考虑在发明的详细的说明部分中记载或使用的意思来掌握其意思。
下面，参照附图中图示的优选的实施例而详细说明本发明的技术结构。
但是，本发明不限于在此说明的实施例，也可以其他方式具体实施。在整个说明书中，相同的符号表示相同的构成要件。
图1是本发明的一个实施例的高韧性、高强度的氮化硅球的制造方法的流程图。
参照图1，本发明的一个实施例的高韧性、高强度的氮化硅球的制造方法是制造在轴承等机器装置中为了减少接触摩擦而插入的氮化硅球的方法。
首先，准备硅粉末(S1000)。
另外，关于上述硅粉末，使用将金属硅废料(scrap)粉碎而控制杂质和粒度的硅粉末。
另外，上述硅粉末的粒度越小越好，但为了与烧结添加剂之间的混合和最终的精细化而可使用平均粒径为1μm至10μm的硅粉末。
然后，在上述硅粉末中添加溶剂及有机粘合剂而形成浆料(S2000)。
另外，对上述溶剂和有机粘合剂的种类，不作特别的限定，但作为上述溶剂，优选使用从乙醇、甲醇、异丙醇、蒸馏水及丙酮中选择的1种以上，作为上述有机粘合剂，优选使用聚乙烯醇缩丁醛(PVB)系粘合剂。
然后，将上述浆料热喷雾干燥(spray drying)而制造具备规定的粒径的颗粒(granule)(S3000)。
另外，关于进行热喷雾干燥获得的颗粒，为了使其内部不是空的或形成甜甜圈形态的颗粒，将腔的内部温度固定为120℃，将外部腔的温度固定为90℃，将雾化器(atomizer)速度规定为8,000rpm至15,000rpm。
另外，这样制造的颗粒的平均粒径为60μm至120μm，优选为80μm至120μm。
然后，将上述颗粒加压成型而制造硅球100(S4000)。
另外，关于上述加压成型的成型压力，优选设定为20kg/cm3至50kg/cm3，以在执行下面的静水压成型时，施加均匀的压力而在成型之后容易处理。
然后，使上述硅球100位于软质的多孔性泡沫200的各个孔210(S5000)。
另外，上述多孔性泡沫200为形成有彼此分开的多个孔210的PE泡沫，如图2的(b)所示，上述孔210形成为圆形或如图2的(a)所示，上述孔210形成为多边形形态。
另外，上述孔210可打孔为贯穿上述多孔性泡沫200的上表面及下表面的形态，也可以凹陷为下表面被堵住，仅向上表面开放的槽形态。
另外，上述孔210的最大宽度应大于上述硅球100的直径。
这是为了在上述硅球100位于上述孔210时使其通过且将与PE泡沫的接触最小化。
但是，需要将大小调节为在一个孔210内仅设有一个硅球100。
即，上述多孔性泡沫200起到能够放置多个硅球的夹具的作用。
另外，为了在上述多孔性泡沫200的各个孔210内设置硅球100，利用在上述多孔性泡沫200上放置多个硅球100并利用振动器而左右摇晃，由此使硅球100卡置在各个孔210内的方法。
另外，上述多孔性泡沫200的厚度应小于上述硅球100的直径，优选为上述硅球100的直径的20％至50％。
然后，将放置有上述硅球100的多孔性泡沫200放入塑料袋300而进行真空排气，由此进行封装(S6000)。
另外，关于上述塑料袋300，只要在下面说明的静水压成型中能够承受压力，则可利用任何材质或形态的塑料袋。
另一方面，本申请人以往在一个橡胶袋中放入一个硅球之后进行密封并通过静水压机进行了成型，因此产量较低，但通过利用上述多孔性泡沫200而将多个硅球一次性地封装之后进行静水压力成型，从而大幅提高了产量。
然后，将封装的塑料袋310放入静水压机而执行静水压成型(S7000)。
另外，在上述静水压成型时施加的压力优选保持200atm至400atm，施加的时间优选为30分钟至60分钟左右。
然后，如图3所示，将上述静水压成型的硅球320从塑料袋取出而得到之后经过脱脂(S9000)及烧结(S9100)过程而完成高韧性、高强度的氮化硅球的制造。
另外，上述脱脂是将以未氧化的状态包含硅粉末的有机物去除的过程，直至450℃为止，使升温速度保持在0.11℃/分钟至1℃/分钟，并在氧化环境下保持进行2小时至10小时。并未完全去除的残留碳在氮环境下，在900℃下进行1小时至10小时的脱脂。
另外，上述烧结是利用气压烧结(GPS：gas pressure sintering)方法而进行烧结及硅球的氮化的过程，直至1400℃为止，使升温速度保持在0.1℃/分钟至2℃/分钟，使氮压力保持在1.0气压至1.8气压，保持进行0.5小时至10小时。为了进行最终烧结，直至1900℃为止，使升温速度保持在1℃至5℃，使氮压力保持在9气压，保持进行1小时至10小时。
另一方面，在上述静水压成型之后，在上述脱脂工序之前可追加在上述硅球涂布氮化硼的过程(S8000)。
另外，图4表示在上述硅球涂布氮化硼的状态。
另外，关于上述氮化硼，在氮化硼粉末中添加溶剂而实现浆料化，然后将氮化硼浆料以湿式涂布到上述氮化硅球。
另外，作为上述溶剂，优选使用水。
另外，作为上述溶剂而使用水的理由如下：在进行热喷雾干燥时作为有机粘合剂而使用聚乙烯醇缩丁醛(PVB)系粘合剂，而当使用水以外的有机溶剂时，硅球表面的聚乙烯醇缩丁醛(PVB)系粘合剂熔化而与氮化硼进行反应，在该情况下，在烧结时难以实现精细化。
另外，在氮化硼浆料中，相对氮化硼粉末的水的比重为50重量％至98重量％，因为当重量比下降时，浆料的黏度变高，所涂布的厚度过于厚，在烧结时导热率低，由此导致表面和内部的结构不同，从而带来降低球的强度的影响。
另外，关于涂布氮化硼的厚度，在涂布为5μm至20μm的厚度的情况下，在烧结过程中能够抑制在硅球之间的界面上产生反应，并能够抑制表面上的粒子生长。
然后，将涂布有上述氮化硼浆料的硅球进行干燥之后执行上述脱脂工序(S9000)，并进行烧结(S9100)而完成上述高韧性、高强度的氮化硅球的制造。
另外，干燥的硅球的水分含量优选为5％以内。因为在高压的气压烧结过程中挥发的水分将装备内部的石墨发热体或在腔内部中由石墨构成的部件氧化而氧化为一氧化碳或二氧化碳，由此对装备及产品带来损坏。
这样，在对涂布了氮化硼的硅球执行脱脂及烧结时，如果不控制在熔炉(furnace)内部与碳进行反应，则碳会渗透到硅球而合成为碳化硅，从而难以制造高韧性及高强度的氮化硅球，因此良好地控制碳而防止形成碳化硅是非常重要的。
如上所述，本发明以优选的实施例为例进行了图示及说明，但本发明不限于上述的实施例，在不超出本发明的精神的范围内，本领域技术人员可进行各种变更和修改。
Claims (5)
1.一种氮化硅球的制造方法，其特征在于，包括如下步骤：
准备硅粉末；
在上述硅粉末中添加溶剂及有机粘合剂而形成浆料；
对上述浆料进行热喷雾干燥而制造具备规定的粒径的颗粒即granule；
对上述颗粒加压成型而制造硅球；
使上述硅球位于软质的多孔性泡沫的各个孔内；
将配置有多个硅球的多孔性泡沫放入塑料袋进行真空排气而封装；
将封装的塑料袋放入静水压机而进行静水压成型；
在获得上述静水压成型的硅球之后进行脱脂；及
将脱脂的硅球氮化并烧结而制造氮化硅球。
2.根据权利要求1所述的氮化硅球的制造方法，其特征在于，
上述多孔性泡沫为PE泡沫，各个孔形成为圆形或多边形并贯穿上述多孔性泡沫的上表面及下表面而开放，各个孔的最大宽度大于所配置的硅球的直径。
3.根据权利要求1所述的氮化硅球的制造方法，其特征在于，
上述多孔性泡沫为PE泡沫，各个孔形成为圆形或多边形且仅向上述多孔性泡沫的上表面开放，在各个孔的内部安装有硅球。
4.根据权利要求1至3中的任一项所述的氮化硅球的制造方法，其特征在于，
在上述脱脂的过程中还包括在上述静水压成型的硅球的外表面涂布氮化硼的步骤，由此在将硅球脱脂及烧结时控制在熔炉即furnace的内部与碳进行反应。
5.根据权利要求4所述的氮化硅球的制造方法，其特征在于，
上述氮化硼以浆料形态以湿式涂布到上述静水压成型的硅球的外表面。
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