CN108373331B - MoS2/SiC/Cf复合陶瓷材料及其制成的滚动体 - Google Patents
MoS2/SiC/Cf复合陶瓷材料及其制成的滚动体 Download PDFInfo
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Abstract
一种MoS2/SiC/Cf复合陶瓷材料及其制成的滚动体，涉及陶瓷材料领域，将MoS2、松香、硅烷偶联剂按比例匀混合，制成MoS2壳核结构粉体；再将SiC粉体、松香、硅烷偶联剂和上述均MoS2壳核结构粉体匀混合，制成MoS2/SiC壳核结构复合粉体。再将MoS2/SiC壳核结构复合粉体分散于甲基硅油中，形成分散液，并置于模具中，离心成型MoS2/SiC/Cf球形素坯，最后真空烧结制备出高韧性、自润滑的MoS2/SiC/Cf复合陶瓷滚动体。该滚动体可用于陶瓷轴承和滑块。本发明制成的复合陶瓷材料性能优异，且带自润滑功能。
Description
技术领域
本发明涉及陶瓷材料领域，详细讲是一种带自润滑功能，性能优异的MoS2/SiC/Cf复合陶瓷材料及其制成的滚动体。
背景技术
我们知道，陶瓷轴承由于具有优异的耐高温、耐磨、质轻、离心力小等特点，在高温、腐蚀、高转速等苛刻环境下具有不可替代的优势，因此主要应用于核电高温转子、航空发动机、海水高压泵等特殊领域。
目前常用的陶瓷滚动体制备方法有：凝胶注模法、热等静压、注射成型等。凝胶注模法是利用凝胶溶液作为粘结剂，将陶瓷粉体、分散剂、脱模剂等分散在凝胶剂中，搅拌混合，然后在模具内注入陶瓷浆料，静置成型，干燥后烧结。其缺点在于制备的陶瓷滚动体含有气泡，致密度低，内部气泡难以检测，使用时容易开裂。热等静压法是将陶瓷粉体混合后直接放入模具，热压成型，成型过程相对简单，致密度大大提高。其缺点在于热等静压对陶瓷粉体要求较高，高熔点陶瓷粉体难以热等静压成型，且制造成本极高，生产效率较低，难以批量化规模生产；在处理期间产生挥发性气体，从而产生泡沫，再经过干燥和烧成制得多孔陶瓷。注射成型法是将陶瓷粉体、分散剂、塑化剂等分散于溶剂中，通过螺杆注塑机注射到模具中成型；其缺点在于制备的陶瓷滚动体成分不均匀、气孔率高、断裂韧性低。
发明内容
本发明的目的是解决上述现有技术的不足，提供一种具有自润滑功能，性能优异的MoS2/SiC/Cf复合陶瓷材料及其滚动体制备方法。
一种MoS2/SiC/Cf复合陶瓷材料，其特征在于其由原材料MoS2、SiC、Cf、粘结剂、偶联剂和硅油制成，其中原材料MoS2、SiC、Cf、粘结剂、偶联剂和硅油的用量按质量份配比如下：MoS210份、SiC8-15份、Cf7-13份、粘结剂6-15份、偶联剂3-9份、硅油16-60份。
本发明中所述的粘结剂选用松香、高熔点石蜡，偶联剂选用硅烷偶联剂，硅油选用甲基硅油。
一种MoS2/SiC/Cf复合陶瓷材料的制备方法，其特征在于包括如下步骤：
a、按质量份配比选取MoS2粉体10份、粘结剂5-8份、偶联剂2-5份，均匀混合，静置至少2h，制成MoS2壳核结构粉体待用；
b、按质量份配比选取SiC粉体10份、粘结剂2-5份、偶联剂1-3份，均匀混合，至少静置5h，制成SiC壳核结构粉体待用；
c、将MoS2壳核结构粉体和SiC壳核结构粉体按比例1:0.8-1.5混合均匀，制成MoS2/SiC壳核结构复合粉体待用；
d、将MoS2/SiC壳核结构复合粉体分散于甲基硅油中，制成MoS2/SiC壳核结构复合粉体质量浓度为40-65%的MoS2/SiC壳核结构复合粉体悬浮分散液待用；
e、将Cf制备成密度为0.3-0.5 g/cm3的Cf多孔预制体。
f、将MoS2/SiC壳核结构复合粉体悬浮分散液中的固态物质（MoS2包覆SiC粉体及其粘连的松香、硅烷偶联剂和甲基硅油）注入到Cf多孔预制体内，形成材料素坯；
g、将材料素坯置于真空炉中，在1050-1150℃下烧结1.5-3h，随炉冷却后取出，即得到MoS2/SiC/Cf复合陶瓷材料。本方法成型效率高，工艺简单。
本发明的MoS2/SiC/Cf复合陶瓷材料也可以采用凝胶注模法、热等静压、注射成型等现有制备方法制备。
一种MoS2/SiC/Cf复合陶瓷材料制成的滚动体，其特征在于由如下步骤加工而成：：
a、按质量份配比选取MoS2粉体10份、粘结剂5-8份、偶联剂2-5份，均匀混合，静置至少2h，制成MoS2壳核结构粉体待用；
b、按质量份配比选取SiC粉体10份、粘结剂2-5份、偶联剂1-3份，均匀混合，至少静置5h，制成SiC壳核结构粉体待用；
c、将MoS2壳核结构粉体和SiC壳核结构粉体按比例1:0.8-1.5加入球磨机内、在90-130℃下球磨混合均匀，制成MoS2/SiC壳核结构复合粉体待用；
d、将MoS2/SiC壳核结构复合粉体分散于甲基硅油中，制成MoS2/SiC壳核结构复合粉体质量浓度为40-65%的MoS2/SiC壳核结构复合粉体悬浮分散液待用；
e、将碳纤维（块）短切（纤维长度20-45mm）、针刺制备成密度为0.3-0.5 g/cm3的滚动体形状（球形、圆柱形或圆台形））的Cf多孔预制体；
f、将Cf多孔预制体置于离心注入模具中，向离心注入模具中加入MoS2/SiC壳核结构复合粉体悬浮分散液，离心机工作、带动离心注入模具做离心运动，将MoS2/SiC壳核结构复合粉体悬浮分散液中的固体（MoS2包覆SiC粉体及其粘连的松香、硅烷偶联剂和甲基硅油）注入到滚动体形状的Cf多孔预制体内，形成滚动体素坯；
g、将滚动体素坯置于真空炉中，在1050-1150℃下烧结1.5-3h，随炉冷却后取出精磨，即得到MoS2/SiC/Cf复合陶瓷滚动体。
本发明中使用离心注入模具将MoS2/SiC壳核结构复合粉体悬浮分散液中的固态物质（MoS2包覆SiC粉体及其粘连的松香、硅烷偶联剂和甲基硅油）注入到Cf多孔预制体内。所述的离心注入模具包括滚动体模具和加料漏斗，滚动体模具为设有与滚动体形状相同的置入腔的外壳体，滚动体模具一侧设有将置入腔与加料漏斗下端（水平）连通的注入管。外壳体为分体式外壳体，Cf多孔预制体置入滚动体模具中，Cf多孔预制体置的形状与外壳体内的置入腔形状相同，体积为置入腔内体积的0.9-0.99倍。
本发明中以加料漏斗下端为圆心的同一圆周上均布有至少两个滚动体模具。工作时，离心机带动离心注入模具以加料漏斗轴线为旋转中线转动，将加料漏斗内的MoS2/SiC壳核结构复合粉体悬浮分散液中的固态物质注入到Cf多孔预制体内。
本发明制的MoS2/SiC/Cf复合陶瓷滚动体硬度为HRC>120，断裂韧性KIC: 25-30MPam1/2, 摩擦系数0.2-0.25。空气气氛下850oC没有明显氧化。且滚动体具有自润滑特征，MoS2具有自润滑作用，使用过程不需要添加润滑油或润滑脂。
附图说明
图1是本发明中离心注入模具的结构示意图。
图2是本发明制得的球形的MoS2/SiC/Cf复合陶瓷材料的滚动体实物图。
图3是图2中的MoS2/SiC/Cf复合陶瓷材料滚动体的扫描电镜形貌图。
具体实施方式
一种MoS2/SiC/Cf复合陶瓷材料，其特征在于其由原材料MoS2、SiC、Cf、粘结剂、偶联剂和硅油制成，其中原材料MoS2、SiC、Cf、粘结剂、偶联剂和硅油的用量按质量份配比如下：MoS210份、SiC8-15份、Cf7-13份、粘结剂6-15份、偶联剂3-9份、硅油16-60份。所述的粘结剂选用松香、高熔点石蜡中的一种，偶联剂选用硅烷偶联剂，硅油选用甲基硅油。MoS2/SiC/Cf成分解释：MoS2为二硫化钼、SiC为碳化硅、Cf为碳纤维。
一种MoS2/SiC/Cf复合陶瓷材料的制备方法，其特征在于包括如下步骤：
a、将MoS2研磨粉碎至1000-1500目，按质量份配比选取MoS2粉体10份、粘结剂5-8份、偶联剂2-5份，均匀混合，室温下静置至少2h，制成MoS2壳核结构粉体待用；
b、按质量份配比选取300-500目的SiC粉体10份、粘结剂2-5份、偶联剂1-3份，均匀混合，室温下静置至少5h，制成SiC壳核结构粉体待用；
c、将MoS2壳核结构粉体和SiC壳核结构粉体按比例1:0.8-1.5加入球磨机内、在90-130℃下球磨混合均匀，制成MoS2/SiC壳核结构复合粉体待用；
d、将MoS2/SiC壳核结构复合粉体分散于甲基硅油中，制成MoS2/SiC壳核结构复合粉体质量浓度为40-65%的MoS2/SiC壳核结构复合粉体悬浮分散液待用；
e、将Cf制备成密度为0.3-0.5 g/cm3的Cf多孔预制体。
f、使用离心注入模具将MoS2/SiC壳核结构复合粉体悬浮分散液中的固态物质（MoS2包覆SiC粉体及其粘连的松香、硅烷偶联剂和甲基硅油）注入到Cf多孔预制体内，形成材料素坯；
g、将材料素坯置于真空炉中，在1050-1150℃下烧结1.5-3h，随炉冷却后取出，即得到MoS2/SiC/Cf复合陶瓷材料。
所述的离心注入模具包括成型模具和加料漏斗，成型模具为设有与置入腔的外壳体，成型模具一侧设有将置入腔与加料漏斗下端水平连通的注入管。外壳体为分体式外壳体，Cf多孔预制体置入成型模具中，Cf多孔预制体置的形状与外壳体内的置入腔形状相同，体积为置入腔内空间体积的0.9-0.99倍。离心注入模具进一步改进，以加料漏斗下端为圆心的同一圆周上均布有至少两个成型模具。工作时，离心机带动离心注入模具以加料漏斗轴线为旋转中线转动，将加料漏斗内的MoS2/SiC壳核结构复合粉体悬浮分散液中的固态物质注入到Cf多孔预制体内。本方法成型效率高，工艺简单，所需时间短，生产效率高，生产成本低。
本发明的MoS2/SiC/Cf复合陶瓷材料也可以采用凝胶注模法、热等静压、注射成型等现有制备方法制备。
实施例1
一种MoS2/SiC/Cf复合陶瓷材料制成的滚动体，由如下步骤加工而成：
a、按质量份配比选取1000目MoS2粉体10份、粘结剂5份、偶联剂2份，均匀混合，室温下静置2h，制成MoS2壳核结构粉体待用；
b、按质量份配比选取300目的SiC粉体10份、粘结剂2份、偶联剂1份，均匀混合，室温下静置5h，制成SiC壳核结构粉体待用；
c、将MoS2壳核结构粉体和SiC壳核结构粉体按比例1:0.8加入球磨机内、在90℃下球磨混合均匀，制成MoS2/SiC壳核结构复合粉体待用；
d、将MoS2/SiC壳核结构复合粉体分散于甲基硅油中，制成MoS2/SiC壳核结构复合粉体质量浓度为40%的MoS2/SiC壳核结构复合粉体悬浮分散液待用；
e、将碳纤维块短切（纤维长度20mm）、针刺制备成密度为0.3g/cm3的球形的Cf多孔预制体；
f、将球形的Cf多孔预制体置于离心注入模具中，向离心注入模具中加入MoS2/SiC壳核结构复合粉体悬浮分散液，离心机转速8000rpm下工作、带动离心注入模具做离心运动，将MoS2/SiC壳核结构复合粉体悬浮分散液中的固体（MoS2包覆SiC粉体及其粘连的松香、硅烷偶联剂和甲基硅油）注入到球形的Cf多孔预制体内，离心1h后形成球形的滚动体素坯；取出滚动体素坯；
g、将滚动体素坯置于真空炉中，在1050℃下烧结1.5h，随炉冷却后取出精磨，即得到MoS2/SiC/Cf复合陶瓷滚动体。
实施例2
一种MoS2/SiC/Cf复合陶瓷材料制成的滚动体，由如下步骤加工而成：
a、按质量份配比选取1200目MoS2粉体10份、粘结剂7份、偶联剂4份，均匀混合，常温下静置3h，制成MoS2壳核结构粉体待用；
b、按质量份配比选取400目的SiC粉体10份、粘结剂4份、偶联剂2份，均匀混合，常温下静置8h，制成SiC壳核结构粉体待用；
c、将MoS2壳核结构粉体和SiC壳核结构粉体按比例1:1加入球磨机内、在120℃下球磨混合均匀，制成MoS2/SiC壳核结构复合粉体待用；
d、将MoS2/SiC壳核结构复合粉体分散于甲基硅油中，制成MoS2/SiC壳核结构复合粉体质量浓度为55%的MoS2/SiC壳核结构复合粉体悬浮分散液待用；
e、将碳纤维块短切（纤维长度35mm）、针刺制备成密度为0.42g/cm3的圆柱形的Cf多孔预制体；
f、将圆柱形Cf多孔预制体置于离心注入模具中，向离心注入模具中加入MoS2/SiC壳核结构复合粉体悬浮分散液，离心机在转速9000rpm下工作、带动离心注入模具做离心运动，将MoS2/SiC壳核结构复合粉体悬浮分散液中的固体（MoS2包覆SiC粉体及其粘连的松香、硅烷偶联剂和甲基硅油）注入到圆柱形状的Cf多孔预制体内，离心1.5h后形成圆柱形的滚动体素坯；取出滚动体素坯；
g、将滚动体素坯置于真空炉中，在1100℃下烧结1.5h，随炉冷却后取出精磨，即得到MoS2/SiC/Cf复合陶瓷滚动体。
实施例3
一种MoS2/SiC/Cf复合陶瓷材料制成的滚动体，由如下步骤加工而成：
a、按质量份配比选取1500目MoS2粉体10份、粘结剂8份、偶联剂5份，均匀混合，常温下静置4h，制成MoS2壳核结构粉体待用；
b、按质量份配比选取500目的SiC粉体10份、粘结剂5份、偶联剂3份，均匀混合，常温下静置10h，制成SiC壳核结构粉体待用；
c、将MoS2壳核结构粉体和SiC壳核结构粉体按比例1:1.5加入球磨机内、在130℃下球磨混合均匀，制成MoS2/SiC壳核结构复合粉体待用；
d、将MoS2/SiC壳核结构复合粉体分散于甲基硅油中，制成MoS2/SiC壳核结构复合粉体质量浓度为65%的MoS2/SiC壳核结构复合粉体悬浮分散液待用；
e、将碳纤维块短切（纤维长度45mm）、针刺制备成密度为0.5g/cm3的圆台形的Cf多孔预制体；
f、将圆台形Cf多孔预制体置于离心注入模具中，向离心注入模具中加入MoS2/SiC壳核结构复合粉体悬浮分散液，离心机在转速15000rpm下工作、带动离心注入模具做离心运动，将MoS2/SiC壳核结构复合粉体悬浮分散液中的固体（MoS2包覆SiC粉体及其粘连的松香、硅烷偶联剂和甲基硅油）注入到圆台形状的Cf多孔预制体内，离心1.5h后形成圆台形的滚动体素坯；取出滚动体素坯；
g、将滚动体素坯置于真空炉中，在1150℃下烧结1.5h，随炉冷却后取出精磨，即得到MoS2/SiC/Cf复合陶瓷滚动体。
本发明中使用离心注入模具将MoS2/SiC壳核结构复合粉体悬浮分散液中的固态物质（MoS2包覆SiC的粉体及其粘连的松香、硅烷偶联剂和甲基硅油）注入到Cf多孔预制体内，所述的离心注入模具的结构如图1所示，包括滚动体模具3和加料漏斗1，滚动体模具3为设有与滚动体形状相同的置入腔的外壳体，滚动体模具3一侧设有将置入腔与加料漏斗1下端水平连通的注入管2。外壳体为分体式外壳体，Cf多孔预制体置入滚动体模具中，Cf多孔预制体置的形状与外壳体内的置入腔形状相同，体积为置入腔内空间体积的0.9-0.99倍。所述的离心注入模具以加料漏斗下端为圆心的同一圆周上均布有至少两个滚动体模具；工作时，离心机带动离心注入模具以加料漏斗轴线为旋转中线转动，将加料漏斗内的MoS2/SiC壳核结构复合粉体悬浮分散液中的固态物质注入到Cf多孔预制体内。
本发明的MoS2/SiC/Cf复合陶瓷滚动体硬度为HRC>120，断裂韧性KIC: 25-30MPam1/2, 摩擦系数0.2-0.25。空气气氛下850oC没有明显氧化。本发明实施例2制成的球形MoS2/SiC/Cf复合陶瓷滚动体的实物图如图2所示，从图3中可以看出，本发明制得的MoS2/SiC/Cf复合陶瓷材料的表面光滑、致密性高。本发明的滚动体具有自润滑特征，使用过程不需要添加润滑油或润滑脂。本发明制得的MoS2/SiC/Cf复合陶瓷材料和MoS2/SiC/Cf复合陶瓷滚动体性能优异，且具有自润滑功能。本发明的加工方法具有成型效率高，工艺简单，所需时间短，生产效率高，生产成本低等优点。
Claims (1)
1.一种MoS2/SiC/Cf复合陶瓷材料制成的滚动体，其特征在于由如下步骤加工而成：
a、按质量份配比选取1000-1500目MoS2粉体10份、粘结剂5-8份、偶联剂2-5份，均匀混合，静置至少2h，制成MoS2壳核结构粉体待用；
b、按质量份配比选取300-500目SiC粉体10份、粘结剂2-5份、偶联剂1-3份，均匀混合，至少静置5h，制成SiC壳核结构粉体待用；
c、将MoS2壳核结构粉体和SiC壳核结构粉体按比例1:0.8-1.5加入球磨机内、在90-130℃下球磨混合均匀，制成MoS2/SiC壳核结构复合粉体待用；
d、将MoS2/SiC壳核结构复合粉体分散于甲基硅油中，制成MoS2/SiC壳核结构复合粉体质量浓度为40-65%的MoS2/SiC壳核结构复合粉体悬浮分散液待用；
e、将碳纤维块短切、针刺制备成密度为0.3-0.5 g/cm3的球形、圆柱形或圆台形滚动体形状的Cf多孔预制体；
f、将Cf多孔预制体置于离心注入模具中，向离心注入模具中加入MoS2/SiC壳核结构复合粉体悬浮分散液，离心机工作、带动离心注入模具做离心运动，将MoS2/SiC壳核结构复合粉体悬浮分散液中的固体注入到滚动体形状的Cf多孔预制体内，形成滚动体素坯；
g、将滚动体素坯置于真空炉中，在1050-1150℃下烧结1.5-3h，随炉冷却后取出精磨，即得到MoS2/SiC/Cf复合陶瓷滚动体。
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