CN109081697A - 一种制备B4C/SiC复合陶瓷粉的方法 - Google Patents
一种制备B4C/SiC复合陶瓷粉的方法 Download PDFInfo
- Publication number
- CN109081697A CN109081697A CN201810984547.8A CN201810984547A CN109081697A CN 109081697 A CN109081697 A CN 109081697A CN 201810984547 A CN201810984547 A CN 201810984547A CN 109081697 A CN109081697 A CN 109081697A
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- Prior art keywords
- composite ceramic
- powder
- sic
- boron carbide
- prepared
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- 239000002131 composite material Substances 0.000 title claims abstract description 60
- 239000000919 ceramic Substances 0.000 title claims abstract description 59
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 title claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 73
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 43
- INAHAJYZKVIDIZ-UHFFFAOYSA-N Boron carbide Chemical compound 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B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 239000003638 reducing agent Substances 0.000 claims abstract description 24
- KGBXLFKZBHKPEV-UHFFFAOYSA-N Boric acid Chemical compound 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OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004327 boric acid Substances 0.000 claims abstract description 20
- 229910003465 moissanite Inorganic materials 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000004064 recycling Methods 0.000 claims abstract description 9
- 239000002893 slag Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims abstract description 3
- 238000003723 Smelting Methods 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound 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- 230000001939 inductive effect Effects 0.000 claims description 9
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[O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N Boron trioxide Chemical compound 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- 241001417490 Sillaginidae Species 0.000 description 1
- 238000005296 abrasive Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000005039 chemical industry Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
本发明属于碳化硼复合陶瓷的制备领域，公开了一种制备B4C/SiC复合陶瓷粉的方法；(1)先将碳质还原剂破碎成粉料；(2)将破碎好的碳质还原剂粉，硼酸粉和碳化硅粉按一定的配比进行配料、混料、并压制成球团，再将球团进行烘干；(3)将球团放入加热炉内进行高温冶炼制备碳化硼复合陶瓷粗粉；(4)将得到的粗粉破碎并进行分级除杂；(5)得到的渣粉进行回收再利用，碳化硼复合陶瓷精粉用于制作碳化硼复合陶瓷烧结原料。本发明与传统电弧炉冶炼相比，提高了原料的利用率，显著地降低了生产成本和能耗；直接在配制B4C的原料中添加SiC相比于在B4C中添加SiC明显地改善了碳化硼复合陶瓷的力学性能；本工艺可以降低环境污染，减少高温气体排放。
Description
技术领域
本发明属于碳化硼复合陶瓷的制备领域，涉及一种制备B4C/SiC复合陶瓷粉的方法。
背景技术
碳化硼，分子式为B4C，为灰黑色粉末，是最硬的人造磨料之一。碳化硼具有硬度高(莫氏硬度9.36)、耐磨性好、密度小(2.52g/cm3)、熔点高(2450℃)、热电性能低(室温140s/m)、耐酸碱性强和中子吸收能力强等优异特性，被广泛应用在机械研磨、耐火材料、工程陶瓷、核工业和军事等不同领域。
复合材料通常具有不同材料相互取长补短的良好综合性能。复合材料兼具有两种或两种以上材料的特点，能改善单一材料的性能，如提高强度、增加韧性、抗冲击抗疲劳性能和改善化学稳定性、介电性能等。作为高温结构材料用的陶瓷复合材料，主要用于宇航，军工等部门。此外，在机械、化工、电子技术等领域也广泛采用各种陶瓷复合材料。
传统的电弧炉冶炼碳化硼材料存在许多不足之处，如弧区温度高，冶炼温度不均匀，不可控；硼酸挥发损失严重；气体排放量高；氧化硼粘度高，阻碍了气体的及时排出，不利于碳化硼的生成，同时增加了炉况的复杂性和处理难度。鉴于存在的这些不足之处进行改善，直接向冶炼原料中加入少量添加剂SiC粉实现改善传统冶炼工艺的目的。
Si与C和B性能接近，在元素周期表的位置毗邻，由相似相容原理推断，以Si作为烧结助剂，肯定会对B4C的烧结起到特殊作用。碳化硅具有各种优异的性能，如超硬耐磨、高热导率和机械强度、低热膨胀系数、耐化学腐蚀、高温稳定性(直到2500℃的分解温度)、有用的电阻特性等。碳化硅是所有非氧化物陶瓷中抗氧化性能最好的一种，因此碳化硅作为一种结构材料被广泛应用于各个领域。
发明内容
针对传统电弧炉冶炼存在不足的问题，本发明提出了一种制备B4C/SiC复合陶瓷粉的方法，采用直接在碳化硼原料中添加碳化硅烧结成B4C/SiC复合陶瓷粉，基于复合陶瓷的优势、Si系添加剂本身的优良性能，直接在原料中加入添加剂比原位反应生成的冶炼产物存在的优势，使得该方法与传统制备B4C/SiC复合陶瓷的原料(B4C粉、SiC粉)简单机械混合相比较，B4C与SiC在微观尺度上结合更紧密，具有更高的反应活性，更有助于烧结致密化。
本发明的具体技术方案为：
一种制备B4C/SiC复合陶瓷粉的方法，包括如下步骤：
(1)将碳质还原剂破碎成粉料；
(2)将硼酸粉、碳质还原剂粉、SiC粉按照重量比为：硼酸粉45～85％、SiC粉3～20％、其余为碳质还原剂粉的比例进行配料，并加少量水进行混料，然后在压球机上压制成团块；
(3)将压制好的团块湿料进行烘干；
(4)将已烘干的团块放入加热炉内进行高温冶炼成碳化硼复合陶瓷粗粉；所述加热炉为感应炉、电弧炉、矿热炉或电阻炉中的一种；
(5)将碳化硼复合陶瓷粗粉进行破碎，并进行分级和除杂得到碳化硼复合陶瓷精粉；
(6)将渣粉进行回收再利用。
进一步地，上述的碳质还原剂粉为石油焦、石墨、木炭、活性炭中的一种或两种以上，其中，占原料的重量百分比为石油焦0～35％，石墨0～25％，木炭0～30％，活性炭0～35％。
进一步地，上述步骤(1)所述的碳质还原剂破碎的粒度不大于1cm。
进一步地，上述步骤(2)所述的压制球团的压力为5～40Mpa,，保压时间10～60s，团块的直径大小为5～35mm。
进一步地，上述步骤(2)中加水量为配料后原料重量的5％。
进一步地，上述步骤(3)所述的烘干的温度控制在50～120℃，烘干时间为5～15h。
进一步地，上述步骤(4)所述的高温冶炼过程中温度控制在1000～2500℃，冶炼时间控制在10～120min。
上述步骤(4)中感应炉、电阻炉的升温速率可调。
与现有冶炼技术相比，本发明的优点是：
(1)先将原料破碎成0～1cm的粒度，既保证了原料配料混料后的分散性和均匀性，同时也增加了原料的比表面积，提高原料的反应活性；
(2)通过将混合料压制成团，并进行烘干，增加了原料的相互接触面积，显著减少了原料的扬尘损失和硼酸在炉子内的高温挥发损失，为实现和保证原料配料比在炉外和炉内的准确控制奠定了基础；
(3)采用了不同炉子进行冶炼，明显改善了炉内不同区域温度的均匀性，这些都是生产高品质碳化硼复合陶瓷粉的必要条件。
(4)采用了直接在原料中添加碳化硅的方法，可以改善传统原位反应的不足。
在本发明的生产方法中，不仅原料利用率高，生产成本低，节约了能源，而且生产的碳化硼复合陶瓷粉纯度高、硬度高、断裂韧性好、致密度高，完全可以满足碳化硼复合陶瓷烧结的原料需求，此外，原料挥发较少，极大降低了粉尘污染，改善了车间环境。
附图说明
图1为本发明实施例1的一种制备B4C/SiC复合陶瓷粉的方法的XRD图。
图2为本发明实施例1的一种制备B4C/SiC复合陶瓷粉的方法的SEM图。
图3为本发明的一种制备B4C/SiC复合陶瓷粉的方法的新型冶炼工艺的流程图。
具体实施方式
本发明实施例中采用硼酸原料的纯度≥99.0％。
实施例1
1、将碳质还原剂进行研磨，筛分；
2、将硼酸粉、碳质还原剂粉、SiC粉按照一定的重量比进行配料：硼酸77％，石墨5％，石油焦5％，木炭3％，活性炭7％，然后在配好的原料中加入3％的Al2O3。
3、将混好的料在压球机上压制成10mm厚的团块；
4、将压制好的团块湿料进行烘干，烘干温度为60℃，烘干时间为8h；
5、将已烘干的团块放入感应炉内进行高温冶炼，冶炼温度为1300℃，冶炼时间为100min，制备成碳化硼复合陶瓷粗粉；
6、将碳化硼复合陶瓷粗粉进行破碎，并进行分级和除杂，得到碳化硼复合陶瓷精粉；
7、将渣粉进行回收再利用。
从上图1和图2可以看出，所冶炼的产物主要为碳化硼和碳化硅，同时还会剩余一定量的碳。通过在生成碳化硼的原料中添加碳化硅使得所冶炼产物中碳化硼和碳化硅能够有效的结合在一起，提高了陶瓷粉的烧结活性，进而便于后续烧结制备B4C/SiC复合陶瓷。
实施例2
1、将碳质还原剂进行研磨，筛分；
2、将硼酸粉、碳质还原剂粉、SiC粉按照一定的重量比进行配料：硼酸60％，石墨8％，石油焦8％，木炭5％，活性炭9％，然后在配好的原料中加入10％的SiC。
3、将混好的料在压球机上压制成15mm厚的团块；
4、将压制好的团块湿料进行烘干，烘干温度为80℃，烘干时间为11h；
5、将已烘干的团块放入感应炉内进行高温冶炼，冶炼温度为1600℃，冶炼时间为80min，制备成碳化硼复合陶瓷粗粉；
6、将碳化硼复合陶瓷粗粉进行破碎，并进行分级和除杂，得到碳化硼复合陶瓷精粉；
7、将渣粉进行回收再利用。
实施例3
1、将碳质还原剂进行研磨，筛分；
2、将硼酸粉、碳质还原剂粉、SiC粉按照一定的重量比进行配料：硼酸45％，石墨12％，石油焦20％，活性炭3％，然后在配好的原料中加入20％的SiC。
3、将混好的料在压球机上压制成25mm厚的团块；
4、将压制好的团块湿料进行烘干，烘干温度为100℃，烘干时间为6h；
5、将已烘干的团块放入感应炉内进行高温冶炼，冶炼温度为2100℃，冶炼时间为40min，制备成碳化硼复合陶瓷粗粉；
6、将碳化硼复合陶瓷粗粉进行破碎，并进行分级和除杂，得到碳化硼复合陶瓷精粉；
7、将渣粉进行回收再利用。
实施例4
1、将碳质还原剂进行研磨，筛分；
2、将硼酸粉、碳质还原剂粉、SiC粉按照一定的重量比进行配料：硼酸55％，石墨7％，石油焦3％，木炭20％，然后在配好的原料中加入15％的SiC。
3、将混好的料在压球机上压制成25mm厚的团块；
4、将压制好的团块湿料进行烘干，烘干温度为100℃，烘干时间为6h；
5、将已烘干的团块放入感应炉内进行高温冶炼，冶炼温度为2300℃，冶炼时间为30min，制备成碳化硼复合陶瓷粗粉；
6、将碳化硼复合陶瓷粗粉进行破碎，并进行分级和除杂，得到碳化硼复合陶瓷精粉；
7、将渣粉进行回收再利用。
实施例5
1、将碳质还原剂进行研磨，筛分；
2、将硼酸粉、碳质还原剂粉、SiC粉按照一定的重量比进行配料：硼酸80％，石油焦10％，然后在配好的原料中加入10％的SiC。
3、将混好的料在高压压球机上压制成20mm厚的团块；
4、将压制好的团块湿料进行烘干，烘干温度为120℃，烘干时间为6h；
5、将已烘干的团块放入感应炉内进行高温冶炼，冶炼温度为1900℃，冶炼时间为40min，制备成碳化硼复合陶瓷粗粉；
6、将碳化硼复合陶瓷粗粉进行破碎，并进行分级和除杂，得到碳化硼复合陶瓷精粉；
7、将渣粉进行回收再利用。
实施例6
1、将碳质还原剂进行研磨，筛分；
2、将硼酸粉、碳质还原剂粉、SiC粉按照一定的重量比进行配料：硼酸85％，石墨5％，石油焦5％，然后在配好的原料中加入5％的SiC。
3、将混好的料在压球机上压制成15mm厚的团块；
4、将压制好的团块湿料进行烘干，烘干温度为80℃，烘干时间为11h；
5、将已烘干的团块放入感应炉内进行高温冶炼，冶炼温度为1700℃，冶炼时间为80min，制备成碳化硼复合陶瓷粗粉；
6、将碳化硼复合陶瓷粗粉进行破碎，并进行分级和除杂，得到碳化硼复合陶瓷精粉；
7、将渣粉进行回收再利用。
Claims (10)
1.一种制备B4C/SiC复合陶瓷粉的方法，其特征在于，包括如下步骤：
(1)将碳质还原剂破碎成粉料；
(2)将硼酸粉、碳质还原剂粉、SiC粉按照重量比为：硼酸粉45～85％、SiC粉3～20％、其余为碳质还原剂粉的比例进行配料，并加少量水进行混料，然后在压球机上压制成团块；
(3)将压制好的团块湿料进行烘干；
(4)将已烘干的团块放入加热炉内进行高温冶炼成碳化硼复合陶瓷粗粉；所述加热炉为感应炉、电弧炉、矿热炉或电阻炉中的一种；
(5)将碳化硼复合陶瓷粗粉进行破碎，并进行分级和除杂得到碳化硼复合陶瓷精粉；
(6)将渣粉进行回收再利用。
2.根据权利要求1所述的一种制备B4C/SiC复合陶瓷粉的方法，其特征在于，所述的碳质还原剂粉为石油焦、石墨、木炭、活性炭中的一种或两种以上，其中，占原料的重量百分比为石油焦0～35％，石墨0～25％，木炭0～30％，活性炭0～35％。
3.根据权利要求1所述的一种制备B4C/SiC复合陶瓷粉的方法，其特征在于，步骤(1)所述的碳质还原剂破碎的粒度不大于1cm。
4.根据权利要求1或2或3所述的一种制备B4C/SiC复合陶瓷粉的方法，其特征在于，步骤(2)所述的压制球团的压力为5～40Mpa,，保压时间10～60s，团块的直径大小为5～35mm。
5.根据权利要求1或2或3所述的一种制备B4C/SiC复合陶瓷粉的方法，其特征在于，步骤(2)中加水量为配料后原料重量的5％。
6.根据权利要求1或2或3所述的一种制备B4C/SiC复合陶瓷粉的方法，其特征在于，步骤(3)所述的烘干的温度控制在50～120℃，烘干时间为5～15h。
7.根据权利要求1或2或3所述的一种制备B4C/SiC复合陶瓷粉的方法，其特征在于，步骤(4)所述的高温冶炼过程中温度控制在1000～2500℃，冶炼时间控制在10～120min。
8.根据权利要求4所述的一种制备B4C/SiC复合陶瓷粉的方法，其特征在于，步骤(4)所述的高温冶炼过程中温度控制在1000～2500℃，冶炼时间控制在10～120min。
9.根据权利要求5所述的一种制备B4C/SiC复合陶瓷粉的方法，其特征在于，步骤(4)所述的高温冶炼过程中温度控制在1000～2500℃，冶炼时间控制在10～120min。
10.根据权利要求6所述的一种制备B4C/SiC复合陶瓷粉的方法，其特征在于，步骤(4)所述的高温冶炼过程中温度控制在1000～2500℃，冶炼时间控制在10～120min。
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