CN102317233A - 碳质耐火材料及其制造方法以及高炉炉底或侧壁 - Google Patents
碳质耐火材料及其制造方法以及高炉炉底或侧壁 Download PDFInfo
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 14
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
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- LCDFWRDNEPDQBV-UHFFFAOYSA-N formaldehyde;phenol;urea Chemical group O=C.NC(N)=O.OC1=CC=CC=C1 LCDFWRDNEPDQBV-UHFFFAOYSA-N 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
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- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 1
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- 239000010959 steel Substances 0.000 description 1
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- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供一种碳质耐火材料及其制造方法，该碳质耐火材料可在不使碳质耐火材料的耐铁水腐蚀性、耐铁水渗透性等高炉炉底耐火材料所必备的特性降低的情况下，进一步提高耐火材料的机械强度，从而抑制了热应力导致的裂纹的生成，该碳质耐火材料的特征在于，其是通过在总计为100质量％的耐火原料中加入有机粘合剂，在对所得到的混合物混炼后进行成型，然后在非氧化性气氛中烧成而得到的，其中，所述耐火原料含有60～85质量％的由焙烧无烟煤、煅烧焦炭、天然石墨或人造石墨中的1种或2种以上构成的碳质原料、5～15质量％的耐火性金属氧化物、4～15质量％的金属硅及2～10质量％的碳黑。
Description
技术领域
本发明涉及作为非氧化性气氛的窑炉、特别是高炉炉底部及炉底侧壁部的内衬耐火材料使用的碳质耐火材料(碳黑)。
背景技术
近年来的非氧化气氛的窑炉、例如高炉等在推进大型化的同时，操作过于严格化，由于高压操作、微粉煤吹入操作等，内衬耐火材料损伤的因素在增加。
另一方面，特别是在高炉中，为了抑制高额的初期投资，希望其长寿命化。严重影响这样的高炉寿命的因素是高炉浇口杯的侧壁部和炉底部的内衬材料的耐久性。作为这些部位的内衬材料，一直使用碳质耐火材料。即作为内衬材料使用的碳质耐火材料的耐久性的提高可为高炉的寿命延长带来直接的效果。
因而，以前为了谋求高炉耐用寿命的延长，就碳质耐火材料的配合、制造条件、使用方法等，提出了多种提案。
例如，在专利文献1中公开了下述的高炉用碳质耐火材料的制造方法：通过在焦粉中对将金属硅微粉配合在碳质集料(也称为骨料)中而得到的成型体进行烧成，通过与存在于成型体气孔内的N2或CO气体反应，在气孔内生成Si-O-N系的晶须，使铁水渗入的1μm以上的气孔减小，从而减少铁水或气体向气孔内的渗入。
此外，在专利文献2中，公开了下述方法：通过在普通的耐火原料中添加Al、Si等金属粉末，金属碳化物、金属氧化物的生成带来的体积膨胀导致组织致密化，抑制氧化性气体及熔渣向耐火材料组织内的侵入，从而提高耐氧化性、耐腐蚀性。
另外，在专利文献3中，公开了下述方法：通过在含碳的不定形耐火材料中添加含有Al-Mg及Al-Si合金的沥青颗粒和碳黑，在基质中形成晶须网，从而提高热强度、耐磨性。
在专利文献4中，公开了为抑制高炉出铁口封闭用填充材料(泥材)的耐熔渣性及热强度的降低，作为降低了SiO2系材料的使用的泥材，在组合含有碳材料、氧化铝超微粉、作为金属粉的铝和硅或铝的集料中添加有机结合材料而得到的高炉出铁口封闭用碳系填充材料，还公开了采用碘吸收量小的碳黑作为碳材料的一部分。
在专利文献5、6中，公开了为使耐熔渣性和耐熔损性平衡，含有碳、氧化铝、金属硅，并含有碳化钛、金属钛、氮化钛、碳氮化钛中的1种以上的碳质耐火材料。即，氧化铝在碳质耐火材料中的添加对于耐熔损性是有效的，有助于降低消耗速度，但如果过剩地添加则使耐熔渣性降低，因此从使耐熔损性和耐熔渣性平衡的观点出发，将氧化铝的添加量控制在不使耐熔渣性降低的程度，通过添加金属钛、钛化合物来确保耐熔渣性的不足部分。
此外，在专利文献5、6中，作为适合高炉浇口杯的侧壁部和炉底部的内衬材料的碳质耐火材料，公开了在含有碳质原料、氧化铝微粉、金属硅微粉，并含有钛粉末、氮化钛粉末及碳氮化钛粉末中的1种以上的混合物中加入有机粘合剂，在将该混合物混炼、成型后在非氧化性气氛中烧成而得到的碳质耐火材料。
现有技术文献
专利文献
专利文献1：日本特公昭58-43350号公报
专利文献2：日本特开平7-291712号公报
专利文献3：日本特开2003-73175号公报
专利文献4：日本特开2000-247755号公报
专利文献5：日本专利第3593101号
专利文献6：WO01/074738号
发明内容
发明所要解决的课题
如上所述，高炉内的内衬耐火材料损伤的因素在增加，作为高炉内的内衬碳质耐火材料损伤的原因，可列举出因增碳在铁水中的熔化、铁水向气孔中侵入而产生的破坏、碱或锌蒸气的侵入和反应造成的裂纹的生成、热应力造成的裂纹的生成等。
可是，在专利文献1中，只公开了通过减小碳质耐火材料组织内的1μm以上的气孔直径来抑制铁水渗透，对于为了抑制热应力造成的裂纹的生成而提高耐火材料的机械强度，既没有记载，也没有暗示。
此外，专利文献2及3的目的在于，通过添加金属粉末，在耐火材料组织内生成金属氧化物、晶须等，从而提高耐氧化性、耐腐蚀性、耐磨性、热强度。公开了金属粉末的添加量为1～2wt％左右的数据，但根据本发明人的研究，判明：在金属粉末的添加量为1～2wt％左右时，晶须等的反应生成物量不充分，在作为高炉炉底部的内衬耐火材料使用时，耐火材料的机械强度不足，存在不能抑制热应力造成的裂纹的生成的问题。
专利文献4的泥材作为封闭用填充剂在不烧成的情况下填充使用，并在填充后进行烧成、硬化。为了确保填充性添加有比较多的树脂剂，在烧成、硬化时残留大的气孔，机械强度低，难以确保对于构成高炉炉底及侧壁的足够的强度。此外，由于作为封闭剂使用，因此需要在低温区体现出强度，例如，为了体现来自600℃的温度区的强度，必须添加金属铝。因此，在烧成时由Al和C生成Al4C3，但在Al4C3的生成时，夺取周围的C，显微组织变化，导致品质降低，因此作为构成高炉炉底及侧壁的耐火材料是不优选的。
关于专利文献5、6，尽管通过添加金属钛或钛化合物而使耐熔渣性及耐熔损性优良，但是不能说对于构成高炉炉底及侧壁具备足够的机械强度。
此外，专利文献5、6的碳质耐火材料尽管在降低铁水熔化造成的消耗方面优异，但是作为耐火材料的机械强度不能说是充分的。
本发明是为解决上述的现有技术的问题点而提出的，其目的在于，提供一种碳质耐火材料及其制造方法以及高炉炉底或侧壁，该碳质耐火材料可在不使碳质耐火材料的耐铁水腐蚀性、耐铁水渗透性等高炉炉底耐火材料所必备的特性降低的情况下，进一步提高耐火材料的机械强度，从而抑制了热应力导致的裂纹的生成。
用于解决课题的手段
为解决上述课题，本发明人等研究了以往采用的碳质耐火材料中碳黑及金属硅的配合量，从而实现了碳质耐火材料的高强度化。
(1)一种碳质耐火材料，其特征在于，其是通过在总计为100质量％的耐火原料中加入有机粘合剂，在对所得到的混合物混炼后进行成型，然后在非氧化性气氛中烧成而得到的，其中，所述耐火原料含有60～85质量％的由焙烧无烟煤、煅烧焦炭、天然石墨或人造石墨中的1种或2种以上构成的碳质原料、5～15质量％的耐火性金属氧化物、4～15质量％的金属硅及2～10质量％的碳黑。
(2)根据权利要求1所述的碳质耐火材料，其特征在于，在所述耐火原料中进一步含有20质量％以下的碳化钛或金属钛。
(3)根据权利要求1或2所述的碳质耐火材料，其特征在于，所述耐火性金属氧化物是氧化铝。
(4)一种高炉炉底或侧壁，其特征在于，其通过内衬权利要求1或2所述的碳质耐火材料而形成。
(5)一种高炉炉底或侧壁，其特征在于，其通过内衬(3)所述的碳质耐火材料而形成。
(6)一种碳质耐火材料的制造方法，其特征在于，配合含有60～85质量％的由焙烧无烟煤、煅烧焦炭、天然石墨或人造石墨中的1种或2种以上构成的碳质原料、5～15质量％的耐火性金属氧化物、4～15质量％的金属硅及2～10质量％的碳黑的耐火原料以使其总计为100质量％，在该耐火原料中加入有机粘合剂后对所得到的混合物进行混炼，然后进行成型并将所得的成型体埋没在焦粉中，在1200～1300℃的非氧化性气氛中进行烧成。
(7)根据(6)所述的碳质耐火材料的制造方法，其特征在于，在所述耐火原料中进一步配合20质量％以下的碳化钛或金属钛。
(8)根据(6)或(7)所述的碳质耐火材料的制造方法，其特征在于，所述耐火性金属氧化物是氧化铝。
发明的效果
根据本发明，可制造在维持高炉炉底耐火材料所必备的特性即耐铁水渗透性及耐铁水腐蚀性与以往材料同等的特性的同时、机械强度高的碳质耐火材料。所以，通过将本发明的碳质耐火材料用作高炉炉底部的内衬耐火材料，能够抑制增碳在铁水中的熔化及铁水向气孔中的侵入，同时还能抑制热应力导致的裂纹的生成。
附图说明
图1是比较例3的碳质耐火材料的断口的场致发射型扫描电子显微镜的观察照片。
图2是本发明例5的碳质耐火材料的断口的场致发射型扫描电子显微镜的观察照片。
图3是本发明例6的碳质耐火材料的断口的场致发射型扫描电子显微镜的观察照片。
图4是表示碳黑添加量与SiC晶须平均直径的关系的一个例子的图。
具体实施方式
以下，参照附图对本发明的优选的实施方式进行详细说明。
本发明人等新发现：通过在含有金属Si的碳质耐火材料中以最佳量添加碳黑，能够促进在烧成中生成于气孔内的SiC晶须的生长，能够使得到的碳质耐火材料高强度化，从而完成了本发明。以下进行详细说明。
如上所述，本发明的碳质耐火材料是通过在总计为100质量％的耐火原料中加入有机粘合剂，在对所得到的混合物混炼后进行成型，然后在非氧化性气氛中烧成而得到的，其中，所述耐火原料含有60～85质量％的由焙烧无烟煤、煅烧焦炭、天然石墨或人造石墨中的1种或2种以上构成的碳质原料、5～15质量％的耐火性金属氧化物、4～15质量％的金属硅及2～10质量％的碳黑。
对于由焙烧无烟煤、煅烧焦炭、天然石墨或人造石墨中的1种或2种以上构成的碳质原料，在低于60质量％时导热率不足，如果超过85质量％则得到的耐火材料的气孔直径过大，耐铁水渗透性降低，因此规定为60质量％～85质量％。
对于耐火性金属氧化物的含量，在低于5质量％时耐铁水性不足，如果超过15质量％则耐熔渣性及导热性降低，因此规定为5～15质量％。
这里，成为原料的耐火性金属氧化物例如氧化铝优选为微粉。通过添加微粉状的耐火性金属氧化物、氧化铝，能够降低碳质耐火材料表面的碳露出比表面积，因而对铁水的耐腐蚀性提高。其粒径的上限没有特别的规定，但从充分获得上述效果的观点出发，优选74μm以下。另一方面，粒径的下限值也没有特别的规定，但为了避免妨碍烧成时在内部发生的气体的旁路，粒径优选为1μm以上。
此外，在本发明的碳质耐火材料中，耐火性金属氧化物具有1000℃以上的熔点，是直到达到熔点都具有机械强度的氧化金属，对其没有特别的限定，但作为耐火性金属氧化物，除了氧化铝以外，优选锆石、氧化镁、莫来石、尖晶石、硅石、氧化锆、氧化铪等高耐火性金属氧化物。通过添加这些微粉，对铁水的耐腐蚀性可得到与添加氧化铝时相同的效果，正如申请人的日本特公昭56-18559号中所记载的。
再有，进一步优选为容易形成微粉、且成本也廉价的氧化铝。
在金属硅的含量低于4质量％时，SiC晶须在气孔内不能充分生成，因此气孔细分化的效果不足，铁水渗透性降低。此外，即使充分添加后述的碳黑，生成的晶须量也少，因此几乎得不到提高强度的效果。另一方面，如果超过15质量％，则残留未反应的金属硅，使耐腐蚀性降低，因此规定为4～15质量％。作为金属硅的含量的下限值，从由气孔内更可靠地生成SiC晶须的观点出发，更优选规定为8质量％。
此外，成为原料的金属硅优选是微粉。通过添加微粉状的金属硅，与碳黑的反应性提高，促进晶须生长。其粒径的上限没有特别的限定，但为了防止残留未反应的金属硅，优选最大粒径为74μm以下。另一方面，粒径的下限值也没有特别的限定，但为了避免妨碍烧成时在内部发生的气体的旁路，优选最小粒径为1μm以上。再有，微粉状的金属硅的粒径例如能够采用激光散射衍射式粒径分布测定装置来测定。
再有，如果金属铝存在于耐火原料内，则该金属铝在碳黑烧成中与周围的碳反应结合，成为碳化铝。此时夺取周围的碳，因此显微组织变化，导致品质下降。由此得出，需要尽量不使金属铝混入耐火原料中。
本发明的特征在于进一步含有2～10质量％的碳黑。
在碳黑低于2质量％时，上述金属硅含量即使在适当的范围，由于生成的晶须量少，也几乎得不到相对于以往的碳质耐火材料的强度提高效果。另一方面，如果超过10质量％，则容易残存未反应的碳黑，得到的碳质耐火材料的气孔率上升，使机械强度降低。所以，将碳黑含量规定为2～10质量％。
附带说明一下，本发明人等对碳黑的添加量作了多种变化并进行了研究，结果发现以下倾向：直到5质量％，随着碳黑添加量的增大，耐火材料的强度也提高，但如果进一步增加碳黑添加量，则耐火材料的强度略有降低。即，在碳黑添加量为4～6质量％时，耐火材料的强度达到峰值，与以往的碳质耐火材料相比较，可得到大约25％的强度提高效果。所以，在以耐火材料的强度的最大化为目标时，优选将碳黑添加量规定为4～6质量％。
添加的碳黑粒子因粒径小而对其上限值没有特别的规定，但随着变为小粒径，比表面积增大，与金属硅微粉的反应性提高，因此优选将平均粒径规定为300nm以下。
另一方面，关于碳黑粒子的平均粒径的下限值没有特别的规定，但从操作上的观点出发，优选30nm以上。再有，可将碳黑粒子的平均粒径规定为例如通过用电子显微镜观察求出的算术平均粒径。
此外，在进一步加强化耐铁水性时，作为耐火原料，优选进一步含有20质量％以下的碳化钛或金属钛(参照专利文献6)。
如果超过20质量％，则耐铁水性的效果没有变化，而且机械加工变得困难。另一方面，对下限没有特别的规定，只要含有就可发挥提高耐铁水性的效果，但为了更可靠地享受其效果，优选含有5质量％以上。
此外，添加的碳化钛或金属钛优选是微粉。粒径越小越促进保护层在耐火材料工作面的生成，增碳熔化造成的损耗越减轻，因此从实用的观点出发，优选规定为35μm以下。但是，尽管其粒径的下限没有特别的规定，但是从操作上的观点出发，优选1μm以上。通过在上述耐火原料中加入有机粘合剂，对它们进行混炼、成型，在非氧化性气氛中烧成，可得到本发明的碳质耐火材料。
这里，作为有机粘合剂，优选采用含有碳成分的煤焦油沥青、酚醛树脂等。
此外，关于混炼、成型、烧成，通常可用熟知的方法实施。但是，在烧成时，由于以碳质原料为对象，因此需要在非氧化性气氛中烧成，此外，关于烧成温度，能够例示在通常进行的1200～1300℃左右实施。
本发明的强度提高的机理的详情虽不清楚，但认为与作为添加原料而含有的金属硅微粉和碳黑的添加具有密切的关系。
将焙烧无烟煤或人造石墨等混合作为碳集料，进而在其中加入金属硅微粉和有机粘合剂并进行混炼，在成型成规定形状的块后，将该块埋没在焦粉中，向其中送入加热空气，加热到大约1300℃进行烧成。于是，大部分的金属硅与碳集料反应，形成SiC。
此外，面朝气孔内表面的金属硅的一部分与气孔中的氧结合，形成SiO2(式1)，该SiO2进一步与其它金属硅结合，形成SiO气体(式2)。
Si(s)+O2(g)→SiO2(s) (式1)
SiO2(s)+Si(s)→2SiO(g) (式2)
另外，面朝气孔内表面的碳也与气孔中的氧反应，形成CO气体(式3)。
C(s)+1/2O2→CO(g) (式3)
通过这些生成的SiO气体和CO气体的反应，在气孔内生成SiC晶须(式4)。
SiO(g)+3CO(g)→SiC(s)+2CO2(g) (式4)
再有，供于(式4)的反应的CO气体不仅包含由(式3)生成的CO气体，还包括在使用环境下从周边供给的CO气体。
当在该反应体系中存在碳黑时，碳黑的比表面积与含有的人造石墨等其它碳集料相比非常大，因此与这些碳集料的碳源相比化学反应性非常高，因而促进(式3)的反应，SiC晶须向气孔内的生成即(式4)的反应更显著化，如后述的实施例所示，发展到SiC晶须直径增大。其结果是，认为本碳质耐火材料的机械强度增大。
此外，本发明的碳质耐火材料的制造方法只要是在上述耐火原料中加入有机粘合剂，然后进行混炼、成型，在非氧化性气氛中烧成的方法即可，但在非氧化性气氛中烧成成型体时，从成本等方面考虑，优选以将成型体埋没在焦粉中的状态下将成型体加热，在1200～1300℃的非氧化性气氛中烧成的方法。作为成型体的加热方法，可列举例如通过加热的空气使重油等燃料燃烧，利用通过该燃烧达到高温的燃烧气体将加热炉的炉壁加热，利用来自炉壁的传热将埋没在设置于加热炉中的焦粉中的成型体加热的方法。烧成时间可根据耐火原料的配合比等适宜设定，例如，在非氧化性气氛下，用两周左右升温到最高到达温度为1250℃而进行烧成，然后，将最高到达温度保持两日左右，由此能够制造所希望的碳质耐火材料。
如上所述，本发明的碳质耐火材料具有良好的耐铁水渗透性及耐铁水腐蚀性，而且机械强度高，因此优选用作高炉炉底部或高炉炉底侧壁部的内衬材料。由此，能够抑制增碳向铁水的熔化及铁水向气孔中的侵入，而且还能够抑制热应力导致的裂纹的发生，能够减少内衬材料的损伤，谋求延长高炉的寿命。
实施例
以下，采用实施例更具体地说明本发明。
按照表1所示的配合，按后述的步骤，得到本发明例1～9及比较例1～6的碳质耐火材料。
采用人造石墨作为碳质原料。此外，作为耐火性金属氧化物的氧化铝及氧化锆(ZrO2)采用平均粒径为3～4μm的氧化铝微粉及氧化锆(ZrO2)微粉，作为金属硅采用粒径为74μm以下的金属硅微粉。此外，作为碳黑采用平均粒径为50nm的碳黑。另外，作为有机粘合剂，采用以质量比计为3∶2混合酚醛树脂和煤焦油沥青而成的粘合剂。
此外，作为制造耐火材料的步骤，相对于表1所示的耐火原料的总计100质量％，以外加计(100质量％内不包含下述成分的含量)加入19质量％的上述有机粘合剂，用加压捏和机混炼，将混炼物在大约20MPa的压力下入模成型，成型为大约55×100×200mm尺寸的块。将该块埋没在焦粉中，采用通过加热的空气使重油燃烧形成的燃烧气体，在非氧化性气氛中(CO气体气氛中)，用两周升温到1250℃进行烧成，得到表1所示的各碳质耐火材料。再有，表1所示的原料组成的单位为质量％(只外加有机粘合剂)。
对于得到的各碳质耐火材料，为了评价机械强度，切割加工成25×25×160mm的棱柱状，通过在室温下进行三点弯曲试验，进行了抗弯强度的比较。再有，三点弯曲试验按照JIS R7212，通过用2个辊支撑棱柱状试验片，从上部中央用1个辊施加载荷，根据直到破坏的最大载荷和支点间距离等算出抗弯强度来进行。
从抗弯强度试验后的残余样品切割加工成9×9×18mm的棱柱状，利用水银压入法调查了气孔率。再有，关于利用水银压入法的气孔率的测定，将试样装入可进行真空处理的容器中，在用水银覆盖试样后，对水银整体施加压力，从而将水银压入试样的气孔中，测定此时施加的压力和侵入的水银容积的关系。
此外，通过加压渗透试验观察铁水的渗透情况。加压渗透试验的试验条件为：在将得到的各碳质耐火材料加工成坩埚形状后，将大约1550℃的铁水倒入坩埚样品中，然后将该坩埚样品内部在高温气氛中利用0.5MPa的氩气加压4小时。然后，保持将铁水装入坩埚的状态进行缓冷，在坩埚内的铁水凝固后切断坩埚样品，通过X射线透射观察来目视确认有无铁水向耐火材料渗透，从而评价铁水的渗透性。
此外，关于本发明例5、8及9的碳质耐火材料，通过铁水耐腐蚀性评价试验求出了侵蚀率。试验条件是，将得到的碳质耐火材料加工成20mmΦ×180mm的圆柱状，在氩气气氛下在大约1550℃的铁水中浸渍1小时。通过测定浸渍前后的样品直径，从下式求出侵蚀率。
另外，将比较例3及本发明例5、6的碳质耐火材料切割成7×7×10mm的长方体，通过切割其长边中央部使断口露出。采用场致发射型扫描电子显微镜(FE-SEM)对这些断口进行观察，对生成于耐火材料气孔内的SiC晶须实施比较。图1～3中示出观察照片。
基于该观察照片，测定任意30根SiC晶须的粗度，如图4所示，对SiC晶须直径(任意30根SiC晶须的平均直径)相对于碳黑添加量的关系进行整理。
(含有碳黑的效果)
由表1发现，相对于没有添加碳黑的比较例1～5，添加了碳黑的比较例6及本发明例1～9有抗弯强度上升的倾向。但是，比较例6由于金属硅微粉少到3质量％，因此抗弯强度只有稍微上升。
特别是，在金属硅微粉为8质量％的条件下，添加了5质量％的碳黑的本发明例5及9相对于没有添加碳黑的比较例3，抗弯强度上升最大，大约为39％。
(含有金属硅的效果)
由表1得出，在添加了5质量％以上的金属硅微粉的比较例2～5及本发明例1～9中，没有发现铁水渗透，而在添加了3质量％的金属硅微粉的比较例1、6中确认了铁水的渗透。但是，比较例2～5没有添加碳黑，因而抗弯强度低。该结果表明，通过使晶须生长并填充在气孔内，耐腐蚀性提高。
(含有TiC的效果)
由表1得知，添加了TiC的本发明例8显示5.0％的侵蚀率，相对于没有添加TiC的本发明例5及9，具有大约2倍的铁水耐腐蚀性。
以下，得知：即使在本发明例5及9中也具有充分的铁水耐腐蚀性，在本发明例8中具有非常优异的铁水耐腐蚀性。此外，由上述碳质耐火材料断口的FE-SEM观察照片(图1～3)判明：在金属硅微粉为8质量％的条件下，相对于没有添加碳黑的比较例3，在添加了碳黑的本发明例5及6中，SiC晶须生长，SiC晶须直径也变粗。
图4中示出碳黑添加量与SiC晶须平均直径的关系，未添加碳黑的比较例3的晶须直径大约为23nm，而添加了5质量％的碳黑的本发明例5中大约为40nm，另外在添加了8质量％的碳黑的本发明例6中为80nm，观察到伴随着碳黑添加量的增大，SiC晶须直径也增大的倾向。
因此，相对于未添加碳黑，通过添加5质量％的碳黑可促进生成于气孔内的SiC晶须的生长，通过使SiC晶须直径增大，使组织致密化，因而认为机械强度提高。
但是，在添加8质量％以上的碳黑时，尽管SiC晶须直径进一步增大，但是容易残留未反应的碳黑，使气孔率上升，因此认为机械强度降低。所以，需要将碳黑添加量规定在2～10质量％的范围内，但在以最大的抗弯强度为目标时，优选配合5质量％左右。
如以上所述，通过添加碳黑，促进组织内生成的SiC晶须的生长，结果气孔率降低，机械强度上升，但是在金属Si添加量为3质量％的没有充分添加的情况下，SiC晶须的生长不充分，确认铁水渗透。即如本发明，确认在提高了机械强度、且铁水没有渗透的碳质耐火材料中，添加所希望量的金属硅微粉和所希望量的碳黑是重要的。
以上，对本发明的优选的实施方式进行了说明，当然本发明并不限定于上述例子。显而易见，只要是本领域技术人员，就可在权利要求书记载的范畴内想到各种变更例或修正例，这些变更例或修正例当然也应理解为属于本发明的技术范畴。
Claims (8)
1.一种碳质耐火材料，其特征在于，其是通过在总计为100质量％的耐火原料中加入有机粘合剂，在对所得到的混合物混炼后进行成型，然后在非氧化性气氛中烧成而得到的，其中，所述耐火原料含有60～85质量％的由焙烧无烟煤、煅烧焦炭、天然石墨或人造石墨中的1种或2种以上构成的碳质原料、5～15质量％的耐火性金属氧化物、4～15质量％的金属硅及2～10质量％的碳黑。
2.根据权利要求1所述的碳质耐火材料，其特征在于，在所述耐火原料中进一步含有20质量％以下的碳化钛或金属钛。
3.根据权利要求1或2所述的碳质耐火材料，其特征在于，所述耐火性金属氧化物是氧化铝。
4.一种高炉炉底或侧壁，其特征在于，其通过内衬权利要求1或2所述的碳质耐火材料而形成。
5.一种高炉炉底或侧壁，其特征在于，其通过内衬权利要求3所述的碳质耐火材料而形成。
6.一种碳质耐火材料的制造方法，其特征在于，配合含有60～85质量％的由焙烧无烟煤、煅烧焦炭、天然石墨或人造石墨中的1种或2种以上构成的碳质原料、5～15质量％的耐火性金属氧化物、4～15质量％的金属硅及2～10质量％的碳黑的耐火原料以使其总计为100质量％，在该耐火原料中加入有机粘合剂后对所得到的混合物进行混炼，然后进行成型并将所得的成型体埋没在焦粉中，在1200～1300℃的非氧化性气氛中进行烧成。
7.根据权利要求6所述的碳质耐火材料的制造方法，其特征在于，在所述耐火原料中进一步配合20质量％以下的碳化钛或金属钛。
8.根据权利要求6或7所述的碳质耐火材料的制造方法，其特征在于，所述耐火性金属氧化物是氧化铝。
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| JP2009033979 | 2009-02-17 | ||
| PCT/JP2010/052801 WO2010095757A1 (ja) | 2009-02-17 | 2010-02-17 | 炭素質耐火物及びその製造方法、並びに、高炉炉底又は側壁 |
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| US (1) | US8889062B2 (zh) |
| EP (1) | EP2399879B1 (zh) |
| JP (1) | JP5539201B2 (zh) |
| KR (1) | KR101213658B1 (zh) |
| CN (1) | CN102317233A (zh) |
| BR (1) | BRPI1008931B1 (zh) |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924103A (zh) * | 2012-11-22 | 2013-02-13 | 四川广汉士达炭素股份有限公司 | 一种炭砖及其制造方法与应用 |
| CN103570365A (zh) * | 2012-08-10 | 2014-02-12 | 宝山钢铁股份有限公司 | 一种高炉炉缸碳砖与热电偶的粘合剂及其填充方法 |
| CN106715329A (zh) * | 2014-09-29 | 2017-05-24 | 贝克休斯公司 | 碳复合材料和制造方法 |
| US10300627B2 (en) | 2014-11-25 | 2019-05-28 | Baker Hughes, A Ge Company, Llc | Method of forming a flexible carbon composite self-lubricating seal |
| US11148950B2 (en) | 2014-11-13 | 2021-10-19 | Baker Hughes, A Ge Company, Llc | Reinforced composites, methods of manufacture, and articles therefrom |
| CN114728852A (zh) * | 2019-12-10 | 2022-07-08 | 黑崎播磨株式会社 | 耐火材料 |
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|---|---|---|---|---|
| CN102317233A (zh) * | 2009-02-17 | 2012-01-11 | 新日本制铁株式会社 | 碳质耐火材料及其制造方法以及高炉炉底或侧壁 |
| PL2527773T3 (pl) * | 2011-05-27 | 2017-09-29 | Sgl Carbon Se | Materiał ogniotrwały na wewnętrzną wykładzinę wielkiego pieca, uzyskany przez połowiczną grafityzację mieszaniny zawierającej C i Si |
| FR2977578B1 (fr) * | 2011-07-06 | 2013-07-05 | Produits Refractaires | Procede de fabrication de carbure de silicium |
| CN108002379B (zh) * | 2017-12-15 | 2021-02-12 | 吉林市巨邦炭素有限公司 | 一种增加炭黑循环使用次数的方法 |
| KR102368375B1 (ko) | 2020-06-09 | 2022-02-28 | (주)건일산업 | 실리콘 잉곳 성장로 Spill Tray용 내화단열재의 제조방법 |
| KR102368368B1 (ko) | 2020-06-09 | 2022-03-02 | (주)건일산업 | 실리콘 잉곳 성장로 Spill Tray용 내화단열재 |
| TWI745186B (zh) * | 2020-12-01 | 2021-11-01 | 中國鋼鐵股份有限公司 | 廢棄耐火材料之回收再利用方法 |
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- 2010-02-17 US US13/138,416 patent/US8889062B2/en active Active
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| CN103570365A (zh) * | 2012-08-10 | 2014-02-12 | 宝山钢铁股份有限公司 | 一种高炉炉缸碳砖与热电偶的粘合剂及其填充方法 |
| CN103570365B (zh) * | 2012-08-10 | 2015-04-01 | 宝山钢铁股份有限公司 | 一种高炉炉缸碳砖与热电偶的粘合剂 |
| CN102924103A (zh) * | 2012-11-22 | 2013-02-13 | 四川广汉士达炭素股份有限公司 | 一种炭砖及其制造方法与应用 |
| CN106715329A (zh) * | 2014-09-29 | 2017-05-24 | 贝克休斯公司 | 碳复合材料和制造方法 |
| US10315922B2 (en) | 2014-09-29 | 2019-06-11 | Baker Hughes, A Ge Company, Llc | Carbon composites and methods of manufacture |
| CN106715329B (zh) * | 2014-09-29 | 2020-12-11 | 贝克休斯公司 | 碳复合材料和制造方法 |
| US11148950B2 (en) | 2014-11-13 | 2021-10-19 | Baker Hughes, A Ge Company, Llc | Reinforced composites, methods of manufacture, and articles therefrom |
| US10300627B2 (en) | 2014-11-25 | 2019-05-28 | Baker Hughes, A Ge Company, Llc | Method of forming a flexible carbon composite self-lubricating seal |
| CN114728852A (zh) * | 2019-12-10 | 2022-07-08 | 黑崎播磨株式会社 | 耐火材料 |
| CN114728852B (zh) * | 2019-12-10 | 2023-06-09 | 黑崎播磨株式会社 | 滑动喷嘴板用耐火材料 |
Also Published As
| Publication number | Publication date |
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| BRPI1008931B1 (pt) | 2020-04-14 |
| JPWO2010095757A1 (ja) | 2012-08-30 |
| EP2399879B1 (en) | 2017-04-05 |
| EP2399879A1 (en) | 2011-12-28 |
| US20110298166A1 (en) | 2011-12-08 |
| US8889062B2 (en) | 2014-11-18 |
| JP5539201B2 (ja) | 2014-07-02 |
| WO2010095757A1 (ja) | 2010-08-26 |
| KR101213658B1 (ko) | 2012-12-18 |
| EP2399879A4 (en) | 2012-08-08 |
| BRPI1008931A2 (pt) | 2018-01-16 |
| KR20110111423A (ko) | 2011-10-11 |
| PL2399879T3 (pl) | 2017-09-29 |
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