CN111855724A - 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
- Publication number
- CN111855724A CN111855724A CN202010529025.6A CN202010529025A CN111855724A CN 111855724 A CN111855724 A CN 111855724A CN 202010529025 A CN202010529025 A CN 202010529025A CN 111855724 A CN111855724 A CN 111855724A
- Authority
- CN
- China
- Prior art keywords
- titanium
- aluminum
- crucible
- microstructure morphology
- equiaxed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 18
- 210000001787 dendrite Anatomy 0.000 title claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- -1 titanium-aluminum compound Chemical class 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 230000006378 damage Effects 0.000 abstract description 10
- 230000007797 corrosion Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000005498 polishing Methods 0.000 abstract description 3
- 230000001066 destructive effect Effects 0.000 abstract description 2
- 230000010287 polarization Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000000498 ball milling Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000002905 metal composite material Substances 0.000 description 3
- 239000011156 metal matrix composite Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
Landscapes
- Chemical & Material Sciences (AREA)
- Immunology (AREA)
- Biochemistry (AREA)
- Pathology (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
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，其关键技术特征在于(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，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。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010529025.6A CN111855724B (zh) | 2020-06-11 | 2020-06-11 | 一种等轴钛铝枝晶微观组织形貌的直接显示方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010529025.6A CN111855724B (zh) | 2020-06-11 | 2020-06-11 | 一种等轴钛铝枝晶微观组织形貌的直接显示方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111855724A true CN111855724A (zh) | 2020-10-30 |
| CN111855724B CN111855724B (zh) | 2023-10-24 |
Family
ID=72986548
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010529025.6A Active CN111855724B (zh) | 2020-06-11 | 2020-06-11 | 一种等轴钛铝枝晶微观组织形貌的直接显示方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111855724B (zh) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5108983A (en) * | 1989-11-21 | 1992-04-28 | Georgia Tech Research Corporation | Method for the rapid deposition with low vapor pressure reactants by chemical vapor deposition |
| US20070157525A1 (en) * | 2004-01-15 | 2007-07-12 | Egan David P | Method for coating abrasives |
| CN101029376A (zh) * | 2007-04-12 | 2007-09-05 | 北京科技大学 | Fe基非晶纳米晶喷涂粉末及其氩气雾化制备方法 |
| CN110702497A (zh) * | 2019-09-09 | 2020-01-17 | 中国航发北京航空材料研究院 | 一种预测金属表面裂纹萌生位置或扩展方向的方法 |
-
2020
- 2020-06-11 CN CN202010529025.6A patent/CN111855724B/zh active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5108983A (en) * | 1989-11-21 | 1992-04-28 | Georgia Tech Research Corporation | Method for the rapid deposition with low vapor pressure reactants by chemical vapor deposition |
| US20070157525A1 (en) * | 2004-01-15 | 2007-07-12 | Egan David P | Method for coating abrasives |
| CN101029376A (zh) * | 2007-04-12 | 2007-09-05 | 北京科技大学 | Fe基非晶纳米晶喷涂粉末及其氩气雾化制备方法 |
| CN110702497A (zh) * | 2019-09-09 | 2020-01-17 | 中国航发北京航空材料研究院 | 一种预测金属表面裂纹萌生位置或扩展方向的方法 |
Non-Patent Citations (9)
| Title |
|---|
| 刘玉芬;钱建刚;黄巍;: "AZ91D镁合金前处理工艺对化学镀镍的影响", 材料保护, no. 06 * |
| 杨曜源等: "化学气相沉积法生长透明硒化锌多晶", 《硅酸盐学报》 * |
| 杨曜源等: "化学气相沉积法生长透明硒化锌多晶", 《硅酸盐学报》, no. 08, 26 August 2004 (2004-08-26) * |
| 杨道媛等: "透明MgAl_2O_4晶须的制备与表征", 《硅酸盐通报》 * |
| 杨道媛等: "透明MgAl_2O_4晶须的制备与表征", 《硅酸盐通报》, 15 August 2009 (2009-08-15), pages 74 - 77 * |
| 段红娟等: "温度和气氛对合成镁铝尖晶石纤维的影响", 《人工晶体学报》 * |
| 段红娟等: "温度和气氛对合成镁铝尖晶石纤维的影响", 《人工晶体学报》, no. 11, 15 November 2013 (2013-11-15) * |
| 钦兰云等: "激光沉积修复ZL114A铝合金的组织及力学性能", 《稀有金属材料与工程》 * |
| 钦兰云等: "激光沉积修复ZL114A铝合金的组织及力学性能", 《稀有金属材料与工程》, no. 06, 15 June 2017 (2017-06-15) * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111855724B (zh) | 2023-10-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1289389C (zh) | 含有磷酸铝组合物的材料以及磷酸铝组合物 | |
| Adamov et al. | Electrical and structural properties of thin gold films obtained by vacuum evaporation and sputtering | |
| CN107641751B (zh) | 一种MoNbCrVTi难熔高熵合金及其制备方法 | |
| CN108706965B (zh) | 一种氧化铟镓锌管状靶材的短流程制备方法 | |
| CN108447773A (zh) | 石墨烯单晶薄膜及其制备方法 | |
| FR2837217A1 (fr) | Revetement composite de mosi2-si3n4 et son procede de fabrication | |
| CN113652593A (zh) | 一种MoxNbTayTiV高熵合金及其制备方法 | |
| Yokota et al. | Fabrication of metallic fibers with high melting point and poor workability by unidirectional solidification | |
| Eremeev et al. | Progress with multi-cell Nb3Sn cavity development linked with sample materials characterization | |
| CN107236989B (zh) | 一种五元稀土硼化物单晶热阴极材料及其制备方法 | |
| CN111855724A (zh) | 一种等轴钛铝枝晶微观组织形貌的直接显示方法 | |
| Sure et al. | Microstructural characterization and chemical compatibility of pulsed laser deposited yttria coatings on high density graphite | |
| CN111855723B (zh) | 一种粗大铝胞状晶组织形貌的直接三维显示方法 | |
| CN105714370A (zh) | 一种大量制备锡晶须的方法 | |
| CN111499377B (zh) | 一种压电陶瓷及其制备方法 | |
| CN116462517B (zh) | 一种利用熔盐法在石墨基体上制备氮化硅涂层的方法 | |
| JP2002068896A (ja) | 窒化物単結晶製造方法及び製造装置 | |
| Jiang et al. | Preparation of dense films of crystalline ZrO2 by intense pulsed‐electron‐beam ablation | |
| JP5509411B2 (ja) | 細胞培養観察方法、細胞培養観察用炭素基板およびその製造方法 | |
| CN105441877A (zh) | 电阻式热蒸发制备铁磁性材料Fe3Si薄膜的工艺 | |
| Guo et al. | Effects of Dy on the microstructure and spallation failure of the alumina scales grown on NiAl | |
| Kamitsuji et al. | Direct observation of crystallization of amorphous Mg-bearing silicate grains into Mg (forsterite) | |
| CN108624853A (zh) | 一种铁尾矿微晶玻璃薄膜及其制备方法与应用 | |
| He et al. | Effect of substrate temperature on the microstructure and properties of Be2C films: Aim to advance its applications as ICF ablator | |
| CN113387683A (zh) | 一种锂钴锰氧化物靶材及其制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |