CN106116614A - 再结晶碳化硅辊棒的制备方法 - Google Patents

再结晶碳化硅辊棒的制备方法 Download PDF

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CN106116614A
CN106116614A CN201610512648.6A CN201610512648A CN106116614A CN 106116614 A CN106116614 A CN 106116614A CN 201610512648 A CN201610512648 A CN 201610512648A CN 106116614 A CN106116614 A CN 106116614A
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麦鹤瀛
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Foshan Yeston Black Carbon Materials Ltd By Share Ltd
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Abstract

本发明公开了一种再结晶碳化硅辊棒制备方法，制备过程包括如下步骤，(1)选用不同粒级的SiC粉按比例称量，加入适量水及羧甲基纤维素，均匀混合，得混合料；(2)将上述混合料加入模具中挤压成型，获得辊棒坯体；(3)将所述辊棒坯体置于烧结炉中烧结采用充填惰性气体以隔绝空气并形成保护气氛；烧结温度达到1950℃～2400℃，保温1小时；继续升温至2800℃，保温60‑80min，断电后自然冷却至室温。相比于同类型的产品，具有良好的高温强度，抗热震性能，抗氧化性能和可导热性能，使用寿命长，性能更加优越。

Description

再结晶碳化硅辊棒的制备方法
技术领域
本发明涉及材料制备技术领域，尤其是涉及一种再结晶碳化硅制品的辊棒的制备方法。
背景技术
再结晶碳化硅制品因其具有独特的耐高温、耐腐蚀、抗氧化、导热快、强度高、蓄热小、寿命长及低热膨胀系数等优势而被广泛应用于航空航天、冶金化工、能源、环保等多个领域，然而在恶劣的高温及热冲击条件下使用使其性能降低、寿命变短，再结晶碳化硅辊棒即是其一种利用，而目前的再结晶碳化硅辊棒大部分是直接使用一定颗粒级的碳化硅微粉，与碳混合后成型生坯，然后在高温下渗硅部分硅与碳反应，生成碳化硅与胚体中的碳化硅结合，达到烧结的目的。中国专利申请名称为一种再结晶碳化硅制品及其制备方法、申请公布号为CN105645963A、申请公布日为2016.06.08、申请号为2016100188804的发明公开了一种再结晶碳化硅制品及其制备方法，再结晶碳化硅制品的原料由质量份数为60～70份碳化硅粗粉、30～40份碳化硅细粉、1～3份碳化硼粉、2～6份生物质糖和1～3份成型助剂组成，碳化硅粗粉的粒径为20～150微米，碳化硅细粉的粒径为0.3～2微米；碳化硼粉的粒径为0.3～2微米；制备方法步骤如下：将生物质糖溶于水得糖水溶液；将碳化硅细粉、碳化硼粉混合均匀，再加入糖水溶液，得混合湿细粉；将碳化硅粗粉、混合湿细粉和成型助剂混合均匀，加水捏炼成可塑泥料；将可塑泥料经真空挤制成型和微波干燥后烧结，出炉后得再结晶碳化硅制品。上述虽然能提高一定有性能，但碳化硅颗粒制品中仍含有较多游离硅的存在，大约含有8-15％的游离硅，其使用温度低于1400℃，最佳使用温度不超过1300℃，超过这个温度制品的强度硬度耐腐蚀性，抗氧化性大幅度下降，导致产品变形氧化开裂断裂，难以满足使用的需求。
发明内容
本发明的目的就是为了解决现有技术之不足而提供的一种不仅具有良好的高温强度，抗热震性能，抗氧化性能和可导热性能，使用寿命长的再结晶碳化硅辊棒的制备方法。
发明是通过如下技术方案来达到上述目的的：
再结晶碳化硅辊棒的制备过程包括如下步骤，
(1)选用不同粒级的SiC粉按比例称量，加入适量水及羧甲基纤维素，均匀混合，得混合料；
其中粗颗粒(245-255μm)的SiC的含量所占比例为40-60％，90-100μm目的碳化硅粉末25％-35％，1μm碳化硅粉末10％-20％；
羧甲基纤维素0.2％～5％；
上述组份的含量总和为100％；
(2)将上述混合料加入模具中挤压成型，获得辊棒坯体；
(3)将所述辊棒坯体置于烧结炉中，在所述坯体的两端连接上石墨电极，并在接有石墨电极的辊棒坯体外围密封采用充填惰性气体以隔绝空气并形成保护气氛；
(4)将两石墨电极通电，利用坯体的导电性实施自身加热烧结，使烧结温度达到1950℃～2400℃，保温1～2小时；
(5)调节所述制品两端的电压，以每小时不超过80℃的速度，使制品继续升温至2800℃，保温60-80min，断电后自然冷却至室温。
进一步地，所述粗颗粒(245-255μm)的SiC的含量中wt％，SiC 99.6
SiO2 0.12 Fe2O3<0.03 free Si<0.01 free C<0.05
90-100μm目的碳化硅含量中wt％，SiC 99.5
SiO2 0.16 Fe2O3<0.05free Si<0.01 free C<0.05
1μm目的碳化硅含量中wt％，SiC 99.2
SiO2 0.05 Fe2O3<0.05free Si<0.01 free C<0.05
进一步地，粗颗粒(245-255μm)的SiC为250μm，其所占比例为50％；
在R-SiC材料的表面涂覆一层与热膨胀指数匹配且氧化扩散系数低的涂层，来提高材料的抗氧化性能。
本发明采用上述技术解决方案所能达到的有益效果是：
采用本发明方法制备的该再结晶碳化硅辊棒的导热系数达120～150W/m·K，抗弯强度达120～140MPa，抗热震性好，使用寿命比普通再结晶碳化硅制品提高了30～50％，其具有1650℃的高温负载能力，广泛用于制造氧化铝陶瓷、工程技术陶瓷、磁性材料、粉末冶金、耐火材料及其它特种陶瓷制品在高温和高氧化环境下的辊道窑，该产品性能特点：
△良好高温荷重性能
△优良的导热性能和耐热性能
△良好的抗氧化性能
△优良的耐酸碱性能
△优良的抗热震性能
△使用寿命长。
具体实施方式
以下结合具体实施例对本技术方案作详细的描述。
制备过程包括如下步骤，
(1)选用三种不同粒级的SiC粉按比例称量，加入适量水及羧甲基纤维素，均匀混合，得混合料；三种不同粒级的SiC粉含量重量比如下：所述粗颗粒250μm的SiC的含量中wt％，SiC 99.6
SiO2 0.12Fe2O3<0.03 free Si<0.01 free C<0.05
95μm目的碳化硅含量中wt％，SiC 99.5
SiO2 0.16Fe2O3<0.05 free Si<0.01 free C<0.05
1μm目的碳化硅含量中wt％，SiC 99.2
SiO2 0.05Fe2O3 <0.05free Si<0.01 free C<0.05
其中粗颗粒250μm的SiC的含量所占比例为50％，95μm目的碳化硅粉末32％，1μm碳化硅粉末17％；
羧甲基纤维素1％；
(2)将上述混合料加入模具中通过100t挤压机挤压成型，获得辊棒坯体；
(3)将所述辊棒坯体置于烧结炉中，在所述坯体的两端连接上石墨电极，并在接有石墨电极的辊棒坯体外围密封采用充填惰性气体以隔绝空气并形成保护气氛；
(4)将两石墨电极通电，利用坯体的导电性实施自身加热烧结，使烧结温度达到1950℃～2400℃，保温1小时；
(5)调节所述制品两端的电压，以每小时不超过80℃的速度，使制品继续升温至2800℃，保温80min，断电后自然冷却至室温。
在R-SiC材料的表面涂覆一层与热膨胀指数匹配且氧化扩散系数低的涂层，来提高材料的抗氧化性能。
实验表明粗碳化硅(SiC)颗粒的加入对再结晶碳化硅陶瓷(R-SiC)抗热震性能的影响；通过不同温度下热震(水淬试验)后测试不同配方样品的残余强度来评价其抗热震性能,并测试了R-SiC陶瓷在30～1200℃的平均线膨胀系数,通过SEM分析了材料的显微结构及热震损伤机制。结果表明:随着粗SiC颗粒(250μm)含量的提高,R-SiC陶瓷的密度、临界热震温差均先升后降；含有50％250μm SiC颗粒陶瓷的密度最大,为2.60g·cm～(-3),线膨胀系数最小,为4.60×10～(-6)/℃,抗热震性能最好,其临界热震温差达395℃；250μm SiC颗粒的引入使得R-SiC在热震过程中产生大量的微裂纹,能够迅速吸收存储在材料中的弹性应变能,从而提高其抗热震性能。
随着粗SiC颗粒(245-255μm)含量的提高,R-SiC陶瓷的密度、临界热震温差均先升后降；含有50％250μm SiC颗粒辊棒的密度最大,为2.60g·cm～(-3),线膨胀系数最小,为4.60×10～(-6)/℃,抗热震性能最好,其临界热震温差达395℃；250μm SiC颗粒的引入使得R-SiC在热震过程中产生大量的微裂纹,能够迅速吸收存储在材料中的弹性应变能,从而提高其抗热震性能。
实验中，我们发现，当两种不同粒级SiC颗粒的比例达到＝65:35时，R-SiC体积密度最大，当成型压力为100MPa、成型水分为6wt％、CMC含量为2wt％时，生坯试样表面光整，容易脱模，且烧成后体积密度最高为2.54g/cm3；当烧成温度为2400℃时，可获得SiC颗粒间结合很好，且抗弯强度高达64MPa的R-SiC陶瓷材料。
以上所述的仅是本发明的优选实施方式，应当指出，对于本领域的普通技术人员来说，在不脱离本发明创造构思的前提下，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。

Claims (5)

1.一种再结晶碳化硅辊棒的制备方法，特征在于，它包括如下步骤，
(1)选用不同粒级的SiC粉按比例称量，加入适量水及羧甲基纤维素，均匀混合，得混合料；
其中粗颗粒的SiC的含量所占比例为40-60％，其颗粒径为245-255μm，90-100μm的碳化硅粉末25％-35％，1μm碳化硅粉末10％-20％；
羧甲基纤维素0.2％～5％；
上述组份的含量总和为100％；
(2)将上述混合料加入模具中挤压成型，获得辊棒坯体；
(3)将所述辊棒坯体置于烧结炉中，在所述坯体的两端连接上石墨电极，并在接有石墨电极的辊棒坯体外围密封采用充填惰性气体以隔绝空气并形成保护气氛；
(4)将两石墨电极通电，利用坯体的导电性实施自身加热烧结，使烧结温度达到1950℃～2400℃，保温1～2小时；
(5)调节所述制品两端的电压，以每小时不超过80℃的速度，使制品继续升温至2800℃，保温60-80min，断电后自然冷却至室温。
2.根据权利要求1所述的再结晶碳化硅辊棒制备方法，其特征在于，所述粗颗粒的SiC的含量中wt％，SiC 99.6 SiO2 0.12Fe2O3<0.03free Si<0.01free C<0.05；
90-100μm目的碳化硅含量中wt％，SiC 99.5 SiO2 0.16Fe2O3<0.05free Si<0.01freeC<0.05；
1μm目的碳化硅含量中wt％，SiC 99.2 SiO2 0.05Fe2O3<0.05free Si<0.01free C<0.05。
3.根据权利要求1或2所述的再结晶碳化硅辊棒制备方法，其特征在于，粗颗粒的SiC为250μm，其所占比例为50％。
4.根据权利要求1或2所述的再结晶碳化硅辊棒制备方法，其特征在于，在R-SiC材料的表面涂覆一层与热膨胀指数匹配且氧化扩散系数低的涂层。
5.根据权利要求1或2所述的再结晶碳化硅辊棒制备方法，其特征在于，所述粗颗粒SiC的含量与90-100μm的碳化硅粉末比例为：65：35。
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