CN111855724B - 一种等轴钛铝枝晶微观组织形貌的直接显示方法 - Google Patents
一种等轴钛铝枝晶微观组织形貌的直接显示方法 Download PDFInfo
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Abstract
本发明提供一种等轴钛铝枝晶微观组织形貌的直接显示新方法。该方法避免了传统等轴枝晶微观组织形貌显示需用抛光与腐蚀、或者偏光的基本过程，直接将该方法生长的等轴钛铝枝晶放置于扫描电子显微镜下进行非破坏性观察，获得具有三维立体形态的等轴枝晶微观组织形貌，充分展示等轴钛铝枝晶微观组织形貌形成的生长过程特性。本发明提供一种等轴钛铝枝晶微观组织形貌的直接显示新方法，其显示尺度为微观层次，所得组织形貌图像生动、逼真，具有非破坏、非损伤的技术特点与优势。
Description
技术领域
本发明涉及金属及金属基复合材料制备技术领域，特别涉及一种等轴钛铝枝晶微观组织形貌的直接显示新方法。
背景技术
在金属及金属基复合材料制备技术领域，通常需要对金属及金属基复合材料的相组成和微观组织包括凝固组织进行观察和分析，为进一步调整制备工艺技术提供参考和依据。在这一过程中，传统的方法和技术是去制备透射电镜样品、扫描电镜样品、光学显微镜样品等，在这些样品的制备过程中需要对其进行机械抛光或者化学抛光，然后选用合适的化学腐蚀试剂对抛光的金属面进行化学腐蚀，使其呈现出易于成像和观察的微观凹凸等。本发明提供一种等轴钛铝枝晶微观组织形貌的直接显示新方法，与传统技术方法相比，具有非破坏、非损伤的技术特点与优势。
发明内容
本发明的目的是：提供一种等轴钛铝枝晶微观组织形貌的直接显示新方法，与传统技术方法相比，避免了化学腐蚀破坏与损伤原始样品的缺点，实现了等轴钛铝枝晶放置于扫描电子显微镜下进行非破坏性的直接观察。本发明的技术设想原理是：充分利用钛铝反应生成的片状化合物及其反应时产生的热量，将钛铝蒸汽沉积于钛铝反应生成的片状化合物上，获得具有三维立体形态的等轴钛铝枝晶微观组织形貌，用于直接微观组织形貌的观察。
基于上述原理，实现本发明的技术方案是：
(a) 将微纳量级钛粉与铝粉按比例混合均匀后盛装于由石墨坩埚(外坩埚，坩埚盖上开一直径2mm—5mm小孔)和氧化铝坩埚(内坩埚)套成的双坩埚中；
(b) 将物料装入碳管炉抽至高真空(10-3Pa量级)，将坩埚加热至1100℃—1200℃保温1—2小时；
(c) 炉温自然冷却至室温，由钛铝反应热产生的钛铝蒸汽沉积于由钛铝反应生成的片状钛铝化合物上，长大形成等轴钛铝枝晶微观组织形貌。
本发明的主要创造性在于：充分利用了钛铝反应的热量产生钛铝蒸汽，利用反应生成的片状钛铝化合物做沉积基底，避开了等轴钛铝枝晶微观组织形貌观察前的破坏性腐蚀。与现有技术相比本发明的主要优点如下：该方法避免了化学腐蚀破坏与损伤原始样品的缺点，实现了等轴钛铝枝晶放置于扫描电子显微镜下进行非破坏性的直接观察，所得组织形貌图像生动、逼真，具有非破坏、非损伤的技术特点与优势。
具体实施方式
实施实例1：
(a) 将颗粒尺寸为30微米—60微米的钛粉按体积比为10%与纯水混合，球磨48小时；
(b) 将球磨后的钛粉浆料置入真空烘箱中干燥，并按比例与铝粉混合；
(c) 将混合粉末装入由碳坩埚和氧化铝坩埚套成的双坩埚中，用碳管炉抽至高真空；
(d) 将物料加热至1200℃保温1小时；
(e) 将炉温自然冷却至室温，取出样品；
经过扫描电镜形貌观察表明：所制备的样品微观组织形貌图像生动、逼真，是具有三维立体形态的等轴钛铝枝晶组织形貌特征, 能谱测试表明其成份为钛、铝，见附图(a)。
实施实例2：
(a) 将颗粒尺寸为30微米—60微米的钛粉按体积比为10%与纯水混合，球磨72小时；
(b) 将球磨后的钛粉浆料置入真空烘箱中干燥，并按比例与铝粉混合；
(c) 将混合粉末装入由碳坩埚和氧化铝坩埚套成的双坩埚中，用碳管炉抽至高真空；
(d) 将物料加热至1100℃保温1小时；
(e) 将炉温自然冷却至室温，取出样品；
经过扫描电镜形貌观察表明：所制备的样品微观组织形貌图像生动、逼真，是具有三维立体形态的等轴钛铝枝晶组织形貌特征, 能谱测试表明其成份为钛、铝，见附图(b)。
附图说明：
图1为用扫描电镜直接观察实例1所看到的等轴钛铝枝晶微观组织形貌；
图2为用扫描电镜直接观察实例2所看到的等轴钛铝枝晶微观组织形貌。
Claims (1)
1.一种等轴钛铝枝晶微观组织形貌的直接显示新方法，其特征在于(a) 将适量微纳量级钛粉与铝粉按比例混合均匀后盛装于由外坩埚和内坩埚套成的双坩埚中，外坩埚为石墨坩埚，内坩埚为氧化铝坩埚，外坩埚盖上开一直径为2mm—5mm的小孔，用碳管炉抽真空后，将坩埚加热至1100℃—1200℃保温1—2小时；(b) 在炉温自然冷却至室温的过程中，将由钛铝反应热产生的少量钛铝蒸汽沉积于由钛铝反应生成的片状钛铝化合物上，长大形成等轴钛铝枝晶微观组织形貌。
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| ES2309710T3 (es) * | 2004-01-15 | 2008-12-16 | Element Six Limited | Procedimiento para revestir abrasivos. |
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