CN112897528A - 一种激光烧结合成碳化硼/碳粉体材料的方法 - Google Patents

一种激光烧结合成碳化硼/碳粉体材料的方法 Download PDF

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CN112897528A
CN112897528A CN202110310128.8A CN202110310128A CN112897528A CN 112897528 A CN112897528 A CN 112897528A CN 202110310128 A CN202110310128 A CN 202110310128A CN 112897528 A CN112897528 A CN 112897528A
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laser
powder
boron carbide
energy
ball milling
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CN112897528B (zh
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曾和平
黄延伟
胡梦云
乔蔚
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Guangdong Langyan Technology Co ltd
East China Normal University
Chongqing Institute of East China Normal University
Shanghai Langyan Optoelectronics Technology Co Ltd
Yunnan Huapu Quantum Material Co Ltd
Chongqing Huapu Intelligent Equipment Co Ltd
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East China Normal University
Chongqing Institute of East China Normal University
Shanghai Langyan Optoelectronics Technology Co Ltd
Yunnan Huapu Quantum Material Co Ltd
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Abstract

本发明属于碳化硼材料制备技术领域，具体为一种激光烧结合成碳化硼/碳粉体材料的方法。将碳化硼反应原料粉末与稀土氧化物粉末进行高能球磨均匀混合，使用压片机将混合均匀的粉末压制成片状，放置于激光工作台固定，控制激光光斑大小、功率、烧结时间等工艺参数进行激光烧结，选用少量或微量的稀土氧化物作为激光催化激活物质，使激光共振激化稀土离子实现能量转移，持续激光能量的供应，使激化离子发生再激化以及多步级联反应和能量转移，从而诱导混合原料发生高温固相反应，生成碳化硼/碳材料，本发明方法激光能量输入低，反应快速，碳化硼的含量高，具有较好耐磨特性，且该制备方法原料利用率高，节能环保，适合大面积工业化生产。

Description

一种激光烧结合成碳化硼/碳粉体材料的方法
技术领域
本发明属于碳化硼基材料制备技术领域，具体涉及一种激光烧结合成碳化硼/碳粉体材料的方法。
背景技术
碳化硼(B4C)，别名黑钻石，是已知最硬的三种材料之一（其他两种为金刚石、立方相氮化硼），具有密度小，强度大，高温稳定性以及化学稳定性优良等特点，用于轻质装甲与避弹衣中。此外，碳化硼可吸收大量中子而不形成任何放射性同位素，因此它在核能发电厂里是很理想的中子吸收剂。与金刚石和立方氮化硼相比，碳化硼制造容易、成本低廉，因而使用更加广泛，在磨削、研磨、钻孔等方面可取代价格昂贵的金刚石。但传统制备方法所合成的B4C粉体由于客观因素，粒度不均匀、杂质含量高, 尤其表现为颗粒粗大、形貌单一,使B4C的优异性能难以充分发挥, 严重限制其应用。研究表明相对于传统B4C粉体, 高纯度、低维度、粒度均匀的B4C粉体能有效改善B4C材料烧结性能, 提高其断裂韧性。因此, 制备含量高、尺寸均匀、小粒径、高长径比的B4C粉体更有意义。
碳化硼制备技术的选择是影响最终产品质量的关键，目前主要通过碳热还原合成法制备碳化硼，虽然该方法是当前工业制备碳化硼的主要途径，但其制备过程的电弧温度过高，大量待反应粉体会以气态形式损失，造成原料利用率较低；炉区温差过大，炉中心部位的温度(2200～2500℃)可能会超过B4C的熔点(2350℃)，使其发生包晶分解，析出游离C与其他高硼化合物，而远离炉中心区的温度偏低, 使反应不完全进行, 残留待反应物，造成所制备的碳化硼纯度不高。除此之外，合成碳化硼还有以下方法：1. 元素直接合成。该方法利用单质硼与碳直接化学反应生成碳化硼，虽然该方法所制备的碳化硼纯度高，但其化学反应放热小，生成的碳化硼会阻碍硼与碳进一步扩散，所以需要更高的反应温度与更长的制备周期，此外原料单质硼价格高，造成制备成本较高；2. 化学气相沉积。该方法通常以含硼和含碳气体作为硼源和碳源，高温下在衬底表面发生化学反应制备碳化硼，虽然该方法污染小，制备的碳化硼纯度高，且可满足特殊形貌要求，但设备昂贵，前期投入高，工艺复杂，产率低，难以满足大批量生产需求；3. 自蔓延高温合成。该方法又称燃烧合成，利用反应物间高化学反应热的自加热与自传导过程在碳管炉中合成碳化硼，采用燃烧合成法虽可快速、低能耗地得到粒度较小的碳化硼，但其制备过程在密闭环境且温度较高，导致反应过程与产物形貌难以控制, 产物粒度分布不均匀。综上所述，发明一种工艺简单、能耗低、污染小、周期短的碳化硼制备方法是必要的。
本发明利用激光烧结技术，通过调节反应原料的配比、催化活性元素、激光的输入能量、烧结时间与光斑尺寸来控制反应过程。待反应粉体经激光辐照、激活稀土离子，产生高能量以催化反应物，诱导发生高温固相反应，激光能量的持续供应激发更多的稀土离子敏化以及发生多步级联反应，实现在低能耗下制备碳化硼/碳粉体材料。
此法所制备的碳化硼/碳粉体的特性如厚度、结晶度、晶格类型、晶格大小均可通过调节激光功率、烧结时间与光斑尺寸直接控制。此种技术具有工艺流程简单，装置简单，环境要求不苛刻，合成周期短，原料利用率高等特点。预计可运用于工业生产大规模制备碳化硼基材料。
发明内容
本发明的目的在于提出一种激光烧结合成碳化硼/碳粉体材料的方法，具有工艺简单、能耗低、污染少、周期短等特点。
本发明提供了一种激光烧结合成碳化硼/碳粉体材料的方法，其特征在于,步骤如下：（1）向反应原料粉末中添加稀土氧化物粉末，使稀土元素离子吸收部分激光能量并实现能量的转移和原料的级联反应；
（2）混合稀土氧化物的原料经高能球磨均匀混合后，使用压片机将混合均匀的粉末压制成片状，放置于激光工作台固定，进行激光烧结，激光共振激化稀土敏化离子，实现能量转移，持续激光能量的供应，使激化离子发生再激化以及多步级联反应和能量转移，从而诱导混合原料发生高温固相反应，生成碳化硼。
优选的，步骤（1）所述稀土氧化物粉末包括15种镧系元素氧化物，以及与镧系元素化学性质相似的钪（Sc）和钇（Y）共17种元素的氧化物，诱导反应原料发生高温固相反应，生成碳化硼成分。
优选的，步骤（1）所述反应原料为硼源和碳源原料，硼源包括硼酸（H3BO3）、氧化硼（B2O3），碳源包括并不限于石墨粉、蔗糖、葡萄糖、石墨烯片，步骤（2）所述高能球磨混合，球磨时采用聚氨酯球磨罐，以无水乙醇、丙酮或去离子水等作为媒质，球磨转速范围为300-400rpm，球磨时间在8-36小时，球磨后使用鼓风干燥箱干燥并研磨成粉，研磨后的粉末粒径在45~150µm，便于最终生成高纯度的碳化硼。
优选的，所述步骤（2）中混合稀土氧化物的原料可根据实际需要，进行造粒以得到微观颗粒尺寸更小的、致密度更高的原料，造粒过程如下：以PVA（聚乙烯醇）等有机胶质材料为粘结剂溶质，以去离子水为溶剂，使用磁力搅拌器配置质量分数为1%的粘结剂，以质量比1：1加入混合均匀的粉料中，进行研磨4小时后造粒，过筛，筛子目数为100-325目，将过筛后的粉料使用压片机压制成片状，进行激光辐照排粘，此过程也可以采取其他方式如管式炉保温排粘，提高碳化硼纯度。
优选的，所述粘结剂溶质包括并不限于PVA、甲氧基硅烷、聚氨酯、硅酮。
优选的，所述步骤（2）中进行烧结的混合粉末的状态可以是片状（使用粉末压片机）也可以是粉末状（采用同步送料法）。
优选的，所述步骤（2）中激光烧结过程，可以在真空、空气、氮气、氧气或氩气中的一种或几种中进行，激光光斑大小可以根据样品尺寸进行调节，敏化离子在激光作用下产生能量共振吸收，将能量进一步传递给反应物；激光烧结所选激光器可以是气体激光器、固体激光器、半导体二极管激光器、燃料激光器、光纤激光器、自由电子激光器或二极管泵浦固体激光器，激光功率100-3000W。
本发明的有益效果是：
以稀土元素Yb的氧化物Yb2O3，按照摄入质量分数0%、1%、3%、5%，分别计算称取相应质量的三种原料，作为原材料跟氧化硼和碳粉（按摩尔比B:C=4：7）进行高能球磨混合，球磨转速为300rpm，以乙醇为球磨媒质，充分均匀混合得到原料混合物粉末，将球磨得到的混合物粉末在100℃烘箱里烘干、研磨，过筛，筛子目数为325目，以粉末粒径在45~150µm为宜，然后利用压片机将过筛后的粉末压制成片状，放置于激光工作台夹具上进行烧结，激光波长980nm，激光烧结功率2700W，光斑直径7*7mm，烧结时间3-60s，使原料混合物发生激光激活自蔓延高温固相反应，生成碳化硼。所得碳化硼具有纯度高、晶粒细小、材料致密、耐磨性能好等特征，适合用于轻质装甲、避弹衣等军工用品中，所涉及的激光烧结激活自蔓延生长技术具有工艺简单、成本低廉、快速高效、环保污染小、能耗低等特点，适合大规模工业化应用。
附图说明
图1 低功率长时间激光烧结形貌与XRD图谱
图2 不同Yb2O3含量激光烧结形貌与XRD图谱
图3 不同激光功率烧结形貌与XRD图谱
图4 激光功率为1700W时在不锈钢衬底上烧结的碳化硼/碳混合粉体。
具体实施方式
下面通过具体实施例进一步描述本发明：
实施例1，以B:C比为4:7，稀土元素Yb的氧化物Yb2O3，按照摄入质量分数0%、1%、3%、5%，分别计算称取相应质量的B2O3、石墨粉和Yb2O3，充分均匀混合得到原料混合物粉末，将球磨得到的混合物粉末在100℃烘箱里烘干、研磨，将研磨后的原料进行造粒研磨以得到微观颗粒尺寸更小的、致密度高的生成物，造粒过程如下：以PVA等有机胶质材料为粘结剂溶质，以去离子水为溶剂，配置质量分数为1% 的粘结剂，分两到三次加入混合均匀的粉料中，进行研磨4小时，过筛，筛子目数为100-325目，以粉末粒径在45~150µm为宜，然后利用压片机将过筛后的粉末压制成片状，放入马弗炉进行排粘（升温速率1℃/min，升温至500℃，保温2h），排粘后的试样放置于激光工作台夹具上进行烧结，激光波长980nm，激光烧结功率2600W，光斑直径7*7mm，使原料混合物发生激光激活自蔓延高温固相反应，激光作用时间3-60s。
实施例2，以B:C比为4:7，稀土元素Yb的氧化物Yb2O3，按照摄入质量分数0%，分别计算称取相应质量的H3BO3、石墨粉和Yb2O3，作为原材料进行高能球磨混合，球磨转速为300rpm，球磨时间12h，以乙醇为球磨媒质，充分均匀混合得到原料混合物粉末，将球磨得到的混合物粉末在100℃烘箱里烘干、研磨，将研磨后的原料进行造粒研磨以得到微观颗粒尺寸更小的、致密度高的生成物，造粒过程如下：以PVA等有机胶质材料为粘结剂溶质，以去离子水为溶剂，配置质量分数为1% 的粘结剂，分两到三次加入混合均匀的粉料中，进行研磨4小时，过筛，筛子目数为100-325目，以粉末粒径在45~150µm为宜，然后利用压片机将过筛后的粉末压制成片状，放入马弗炉进行排粘（升温速率1℃/min，升温至500℃，保温2h），排粘后的试样放置于激光工作台夹具上进行烧结，激光波长980nm，激光烧结功率500W，光斑直径7*7mm，烧结时间60s。图1是低功率长时间激光烧结形貌与XRD图谱。
实施例3，以B:C比为4:1，稀土元素Yb的氧化物，按照摄入质量分数1%、3%、5%，分别计算称取相应质量的B2O3、蔗糖和Yb2O3，将三种原料进行高能球磨混合，以乙醇为球磨媒质，球磨转速300rpm，时间12h，充分均匀混合得到原料混合物粉末，将球磨得到的混合物粉末在100℃烘箱里烘干、研磨、过筛，筛子目数为100-325目，以粉末粒径在45~150µm为宜，然后利用压片机将过筛后的粉末压制成片状，放置于激光工作台夹具上进行烧结，激光波长980nm，激光功率2200W，光斑直径7*7mm，烧结时间3s。图2是不同Yb2O3含量激光烧结形貌与XRD图谱.
实施例4，以B:C比为4:1，稀土元素Yb的氧化物Yb2O3，按照摄入质量分数3%，分别计算称取相应质量的B2O3、葡萄糖和Yb2O3，作为原材料进行高能球磨混合，球磨转速为300rpm，球磨时间12h，以乙醇为球磨媒质，充分均匀混合得到原料混合物粉末，将球磨得到的混合物粉末在100℃烘箱里烘干、研磨，过筛，筛子目数为100-325目，以粉末粒径在45~150µm为宜，然后利用压片机将过筛后的粉末压制成片状，放置于激光工作台夹具上进行激光烧结，激光波长980nm，激光功率1800W，光斑直径7*7mm，使原料混合物发生激光激活自蔓延高温固相反应，激光作用时间3s。图3是不同激光功率烧结形貌与XRD图谱。
实施例5，以B:C比为4:7，稀土元素Yb的氧化物Yb2O3，按照摄入质量分数0%、1%、3%、5%，分别计算称取相应质量的B2O3、石墨粉和Yb2O3，充分均匀混合得到原料混合物粉末，将球磨得到的混合物粉末在100℃烘箱里烘干、研磨，将研磨后的原料进行造粒研磨以得到微观颗粒尺寸更小的、致密度高的生成物，造粒过程如下：以PVA等有机胶质材料为粘结剂溶质，以去离子水为溶剂，配置质量分数为1% 的粘结剂，分两到三次加入混合均匀的粉料中，进行研磨4小时，过筛，筛子目数为100-325目，以粉末粒径在45~150µm为宜，然后利用压片机将过筛后的粉末压制成片状，放入马弗炉进行排粘（升温速率1℃/min，升温至500℃，保温2h），排粘后的试样放置于激光工作台夹具上进行烧结，激光波长980nm，激光烧结功率1700W，光斑直径7*7mm，使原料混合物发生激光激活自蔓延高温固相反应，激光作用时间3-60s。图4 为激光功率为1700W时在不锈钢衬上烧结的碳化硼/碳混合粉体的SEM图。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。

Claims (7)

1.一种激光烧结合成碳化硼/碳粉体材料的方法，其特征在于,步骤如下：（1）向反应原料粉末中添加稀土氧化物粉末，使稀土元素离子吸收部分激光能量并实现能量的转移和原料的级联反应；
（2）混合稀土氧化物的原料经高能球磨均匀混合后，使用压片机将混合均匀的粉末压制成片状，放置于激光工作台固定，进行激光烧结，激光共振激化稀土敏化离子，实现能量转移，持续激光能量的供应，使激化离子发生再激化以及多步级联反应和能量转移，从而诱导混合原料发生高温固相反应，生成碳化硼。
2.根据权利要求1所述的一种激光烧结合成碳化硼/碳粉体材料的方法，其特征在于：步骤（1）所述稀土氧化物粉末包括15种镧系元素氧化物，以及与镧系元素化学性质相似的钪（Sc）和钇（Y）共17种元素的氧化物，诱导反应原料发生高温固相反应，生成碳化硼成分。
3.根据权利要求1所述的一种激光烧结合成碳化硼/碳粉体材料的方法，其特征在于：步骤（1）所述反应原料为硼源和碳源原料，硼源包括硼酸（H3BO3）、氧化硼（B2O3），碳源包括并不限于石墨粉、蔗糖、葡萄糖、石墨烯片，步骤（2）所述高能球磨混合，球磨时采用聚氨酯球磨罐，以无水乙醇、丙酮或去离子水等作为媒质，球磨转速范围为300-400rpm，球磨时间在8-36小时，球磨后使用鼓风干燥箱干燥并研磨成粉，研磨后的粉末粒径在45~150µm，便于最终生成高纯度的碳化硼。
4.根据权利要求1所述的一种激光烧结合成碳化硼/碳粉体材料的方法，其特征在于：所述步骤（2）中混合稀土氧化物的原料可根据实际需要，进行造粒以得到微观颗粒尺寸更小的、致密度更高的原料，造粒过程如下：以PVA（聚乙烯醇）等有机胶质材料为粘结剂溶质，以去离子水为溶剂，使用磁力搅拌器配置质量分数为1%的粘结剂，以质量比1：1加入混合均匀的粉料中，进行研磨4小时后造粒，过筛，筛子目数为100-325目，将过筛后的粉料使用压片机压制成片状，进行激光辐照排粘，此过程也可以采取其他方式如管式炉保温排粘，提高碳化硼纯度。
5.根据权利要求4所述的一种激光烧结合成碳化硼/碳粉体材料的方法，其特征在于：所述粘结剂溶质包括并不限于PVA、甲氧基硅烷、聚氨酯、硅酮。
6.根据权利要求1所述的一种激光烧结合成碳化硼/碳粉体材料的方法，其特征在于：所述步骤（2）中进行烧结的混合粉末的状态可以是片状（使用粉末压片机）也可以是粉末状（采用同步送料法）。
7.根据权利要求1所述的一种激光烧结合成碳化硼/碳粉体材料的方法，其特征在于：所述步骤（2）中激光烧结过程，可以在真空、空气、氮气、氧气或氩气中的一种或几种中进行，激光光斑大小可以根据样品尺寸进行调节，敏化离子在激光作用下产生能量共振吸收，将能量进一步传递给反应物；激光烧结所选激光器可以是气体激光器、固体激光器、半导体二极管激光器、燃料激光器、光纤激光器、自由电子激光器或二极管泵浦固体激光器，激光功率100-3000W。
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