JP2017186600A - Manufacturing method of alloy and alloy powder - Google Patents
Manufacturing method of alloy and alloy powder Download PDFInfo
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本発明は、互いに熱拡散しやすい金属Ａと金属Ｃの合金及びその製造方法に関する。 The present invention relates to an alloy of metal A and metal C that easily diffuses to each other and a method for manufacturing the same.
合金の製造方法として、溶解法、固相−液相反応法、固相−固相反応法、メカニカルミリング法が知られている。 As a method for producing an alloy, a melting method, a solid-liquid phase reaction method, a solid-solid phase reaction method, and a mechanical milling method are known.
特許文献１においては、メカニカルミリング法によりＭｇ−Ｓｉ合金を製造している。メカニカルミリング法は、硬質Ｃｒ鋼容器にステンレス製ボールを入れ、さらに配合粉末を入れて容器を振動あるいは回転させることによって、容器内の粉末を混合あるいは粉砕して合金化して合金を製造する方法である。メカニカルアロイング装置として、振動ボールミル、遊星型ボールミル、転動型ボールミル、回転子挿入型ボールミルを挙げることができる。 In Patent Document 1, an Mg—Si alloy is manufactured by a mechanical milling method. The mechanical milling method is a method in which a stainless steel ball is placed in a hard Cr steel container, and further mixed powder is added and the container is vibrated or rotated to mix or pulverize the powder in the container to form an alloy. is there. Examples of the mechanical alloying device include a vibration ball mill, a planetary ball mill, a rolling ball mill, and a rotor insertion type ball mill.
特許文献２においては、ホットプレス法、熱間等方圧プレス法（ＨＩＰ）、放電プラズマ焼結法（ＳＰＳ）、熱間圧延法、熱間押出法、熱間鍛造法などの熱処理によってＭｇ−Ｓｉ合金を製造している。 In Patent Document 2, Mg— is applied by heat treatment such as hot pressing, hot isostatic pressing (HIP), spark plasma sintering (SPS), hot rolling, hot extrusion, hot forging, and the like. Si alloy is manufactured.
また、特許文献３においては固相−固相反応法によってＭｇ２Ｓｉ合金を製造している。 In Patent Document 3, an Mg 2 Si alloy is manufactured by a solid-solid reaction method.
金属Ａは融点がＴｆｕｓ（Ａ）で沸点がＴｖａｐ（Ａ）であり、金属Ｃは融点がＴｆｕｓ（Ｃ）で沸点がＴｖａｐ（Ｃ）であるとする。金属Ａの融点Ｔｆｕｓ（Ａ）が金属Ｃの融点Ｔｆｕｓ（Ｃ）とほぼ等しい場合には溶解法による合金製造は問題ない。しかしながら、金属Ｃの融点Ｔｆｕｓ（Ｃ）が金属Ａの沸点Ｔｖａｐ（Ａ）より高い場合には、金属Ａ−金属Ｃの合金を溶解法によって製造しようとすると、大気圧においては金属Ａの蒸発量が極めて大きくなり、金属Ａ−金属Ｃの合金の組成を制御するのが困難である。加圧炉中で金属Ａと金属Ｃを加熱溶解することによって金属Ａの蒸発を抑えることができるが、製造コストが高くなる。したがって、金属Ｃの融点Ｔｆｕｓ（Ｃ）が金属Ａの沸点Ｔｖａｐ（Ａ）より高い場合には、溶融法による金属Ａ−金属Ｃの合金の製造は、組成制御が困難であるとともに製造コストが高くなる。 Metal A has a melting point of Tfus (A) and a boiling point of Tvap (A), and metal C has a melting point of Tfus (C) and a boiling point of Tvap (C). When the melting point Tfus (A) of the metal A is substantially equal to the melting point Tfus (C) of the metal C, there is no problem in manufacturing the alloy by the melting method. However, when the melting point Tfus (C) of the metal C is higher than the boiling point Tvap (A) of the metal A, if an alloy of metal A and metal C is to be produced by the melting method, the amount of evaporation of the metal A at atmospheric pressure Becomes extremely large, and it is difficult to control the composition of the metal A-metal C alloy. Evaporation of the metal A can be suppressed by heating and melting the metal A and the metal C in a pressure furnace, but the manufacturing cost increases. Therefore, when the melting point Tfus (C) of the metal C is higher than the boiling point Tvap (A) of the metal A, the production of the metal A-metal C alloy by the melting method is difficult to control the composition and the production cost is high. Become.
また、溶融法により得られる合金はバルク状であるので、合金粉末とするためにはバルク状の合金を粉砕しなければならない。粉砕することによって、不純物が混入して合金の純度が低下するおそれがあるとともに製造コストが高くなり問題である。 In addition, since the alloy obtained by the melting method is in a bulk form, the bulk form alloy must be pulverized to obtain an alloy powder. By pulverizing, impurities may be mixed and the purity of the alloy may be lowered, and the manufacturing cost is increased, which is a problem.
メカニカルミリング法によって金属Ａ−金属Ｃの合金を作成しようとすると、容器の材料やボールの材料が剥離し、金属Ａ−金属Ｃの合金中に不純物として混入する。したがって、メカニカルミリング法による金属Ａ−金属Ｃの合金の製造は、得られる金属Ａ−金属Ｃの合金中に容器の材料やボールの材料が混入しやすく、純度が低く、均一な組成を得るのが困難であり問題である。 When an alloy of metal A-metal C is prepared by the mechanical milling method, the material of the container and the material of the ball are peeled and mixed as impurities in the alloy of metal A-metal C. Therefore, in the manufacture of the metal A-metal C alloy by the mechanical milling method, the container material and the ball material are easily mixed in the obtained metal A-metal C alloy, and the purity is low and a uniform composition is obtained. Is difficult and problematic.
特許文献３に開示されている固相−固相反応法によって金属Ａ−金属Ｃの合金を作成しようとすると、溶解法による上記の問題やメカニカルミリング法による上記の問題はないが、酸化物が生成しやすく、均一な組成を得ることができず問題である。酸化物により固相中の原子または分子の拡散が妨害され物質拡散速度が大幅に低下したためと考えられる。 When an alloy of metal A and metal C is prepared by the solid phase-solid phase reaction method disclosed in Patent Document 3, there is no problem described above due to the dissolution method or mechanical milling method. It is a problem that it is easy to produce and a uniform composition cannot be obtained. This is probably because the diffusion of atoms or molecules in the solid phase was hindered by the oxide, and the material diffusion rate was greatly reduced.
したがって、本発明により解決しようとする課題は、酸化物が生成しにくく、均一な組成を得ることができる固相−固相反応法による金属Ａ−金属Ｃの合金粒子の製造方法を提供することにある。
本発明の別の課題は、粒子径が均一な金属Ａ−金属Ｃの合金粒子を提供することにある。
Therefore, the problem to be solved by the present invention is to provide a method for producing metal A-metal C alloy particles by a solid-solid reaction method, which is difficult to produce oxides and can obtain a uniform composition. It is in.
Another object of the present invention is to provide metal A-metal C alloy particles having a uniform particle diameter.
当該課題は、請求項１に記載の第１の本発明、すなわち、互いに熱拡散しやすい金属Ａ及び金属Ｃについて、金属Ａの粉末又は金属Ａの水素化合物の粉末と金属Ｃの粉末を均一に混合した後に、当該混合物を黒鉛るつぼ内に収納し、真空排気した直後に、金属Ａの融点より低く、かつ、金属Ｃの融点より低い温度で熱処理して、均一組成の合金粉末を得る合金の製造方法によって、達成される。 The subject is the first aspect of the present invention according to claim 1, that is, the metal A and the metal C that are easily thermally diffused with each other, and the metal A powder or the metal A hydrogen compound powder and the metal C powder are uniformly distributed. After mixing, the mixture is stored in a graphite crucible and immediately after being evacuated, heat treatment is performed at a temperature lower than the melting point of metal A and lower than the melting point of metal C to obtain an alloy powder having a uniform composition. This is achieved by the manufacturing method.
互いに熱拡散しやすい金属Ａと金属Ｃの例として、Ａｌ−Ｂｅ、Ａｌ−Ｓｉ、Ａｌ−Ｔｉ、Ａｌ−Ｆｅ、Ａｌ−Ｎｉ、Ａｌ−Ｃｕ、Ａｌ−Ｍｇ、Ａｌ−Ａｇ、Ａｌ−Ｖ、Ｂｅ−Ｓｉ、Ｂｅ−Ｃｕ、Ｂｅ−Ａｕ、Ｂｅ−Ａｇ、Ｃｒ−Ｓｉ、Ｃｒ−Ｗ、Ｃｏ−Ｓｉ、Ｃｏ−Ｎｉ、Ｃｏ−Ｐｄ、Ｃｕ−Ａｕ、Ｃｕ−Ｓｉ、Ｃｕ−Ｍｏ、Ｃｕ−Ｎｉ、Ｃｕ−Ｎｂ、Ｃｕ−Ａｇ、Ｃｕ−Ｖ、Ａｕ−Ｓｉ、Ａｕ−Ｎｉ、Ｍｇ−Ｎｉ、Ｍｇ−Ｓｉ、Ｍｎ−Ｓｉ、Ｍｏ−Ｎｂ、Ｍｏ−Ｓｉ、Ｍｏ−Ｐｄ、Ｍｏ−Ｐｔ、Ｍｏ−Ｔａ、Ｍｏ−Ｗ、Ｎａ−Ｓｉ、Ｔｉ−Ｃｒ、Ｔｉ−Ｆｅ、Ｔｉ−Ｎｉ、Ｔｉ−Ｃｕ、Ｔｉ−Ｎｂ、Ｔｉ−Ｍｏ、Ｔｉ−Ｐｄ、Ｔｉ−Ｔａ、Ｔｉ−Ｗ、Ｔｉ−Ｐｔ、Ｔｉ−Ｓｉ、Ｔｉ−Ｕ、Ｗ−Ｃｕ、Ｗ−Ｓｉ、Ｆｅ−Ｎｉ、Ｆｅ−Ｃｕ、Ｆｅ−Ｚｒ、Ｆｅ−Ｎｂ、Ｆｅ−Ｐｄ、Ｆｅ−Ｓｉ、Ｆｅ−Ｔａ、Ｆｅ−Ｗ、Ｆｅ−Ｕ、Ｎｉ−Ｃｕ、Ｎｉ−Ｎｂ、Ｎｉ−Ｍｏ、Ｎｉ−Ｓｉ、Ｎｉ−Ｐｄ、Ｎｉ−Ｐｔ、Ｎｉ−Ｗ、Ｎｉ−Ｕ、Ｎｂ−Ｓｉ、Ｎｂ−Ｔａ、Ｎｂ−Ｗ、Ｎｂ−Ｖ、Ｐｄ−Ｓｉ、Ｐｄ−Ｗ、Ｐｔ−Ｓｉ、Ｐｔ−Ｗ、Ａｇ−Ｓｉ、Ａｇ−Ｔｉ、Ｔａ−Ｓｉ、Ｔａ−Ｖ、Ｚｒ−Ｓｉ、Ｚｒ−Ｕ、Ｕ−Ａｌを挙げることができる。 Examples of metal A and metal C that are likely to thermally diffuse with each other include Al-Be, Al-Si, Al-Ti, Al-Fe, Al-Ni, Al-Cu, Al-Mg, Al-Ag, Al-V, Be-Si, Be-Cu, Be-Au, Be-Ag, Cr-Si, Cr-W, Co-Si, Co-Ni, Co-Pd, Cu-Au, Cu-Si, Cu-Mo, Cu- Ni, Cu-Nb, Cu-Ag, Cu-V, Au-Si, Au-Ni, Mg-Ni, Mg-Si, Mn-Si, Mo-Nb, Mo-Si, Mo-Pd, Mo-Pt, Mo-Ta, Mo-W, Na-Si, Ti-Cr, Ti-Fe, Ti-Ni, Ti-Cu, Ti-Nb, Ti-Mo, Ti-Pd, Ti-Ta, Ti-W, Ti- Pt, Ti-Si, Ti-U, W-Cu, W-Si, Fe-Ni, Fe-Cu, e-Zr, Fe-Nb, Fe-Pd, Fe-Si, Fe-Ta, Fe-W, Fe-U, Ni-Cu, Ni-Nb, Ni-Mo, Ni-Si, Ni-Pd, Ni- Pt, Ni-W, Ni-U, Nb-Si, Nb-Ta, Nb-W, Nb-V, Pd-Si, Pd-W, Pt-Si, Pt-W, Ag-Si, Ag-Ti, Ta-Si, Ta-V, Zr-Si, Zr-U, U-Al can be mentioned.
金属Ａの水素化合物の例として、ＬｉＨ、ＢｅＨ、ＮａＨ、ＭｇＨ２、ＴｉＨ２、ＣｒＨ、ＣｒＨ２、ＮｉＨ、ＣｕＨ、ＺｒＨ２、ＮｂＨ、ＮｂＨ２を挙げることができる。 Examples of the hydrogen compound of a metal A, mention may be made of LiH, BeH, NaH, MgH 2 , TiH 2, CrH, CrH 2, NiH, CuH, ZrH 2, NbH, the NbH 2.
第１の本発明の実施態様においては、請求項２に記載のように、金属Ａの粉末又は金属Ａの水素化合物の粉末と金属Ｃ粉末の混合比は、得ようとする合金の化学量論比である。 In the first embodiment of the present invention, as described in claim 2, the mixing ratio of the metal A powder or the metal A hydrogen compound powder and the metal C powder is determined by the stoichiometry of the alloy to be obtained. Is the ratio.
第１の本発明の他の実施態様においては、請求項３に記載のように、金属Ａの粉末又は金属Ａの水素化合物の粉末の純度が９９．９％以上であり、平均粒径が０．１〜１００μｍであり、金属Ｃ粉末の純度が９９．９％以上であり、平均粒径が０．１〜１００μｍである。 In another embodiment of the first aspect of the present invention, as described in claim 3, the purity of the metal A powder or the metal A hydrogen compound powder is 99.9% or more, and the average particle size is 0. 0.1 to 100 μm, the purity of the metal C powder is 99.9% or more, and the average particle size is 0.1 to 100 μm.
第１の本発明のさらに他の実施態様においては、請求項４に記載のように、１０Ｐａ以下の真空度まで真空排気する。 In still another embodiment of the first aspect of the present invention, as described in claim 4, the vacuum is evacuated to a degree of vacuum of 10 Pa or less.
当該課題は、請求項５に記載の第２の本発明、すなわち、互いに熱拡散しやすい金属Ａ及び金属Ｃについて、金属Ａの粉末又は金属Ａの水素化合物の粉末と金属Ｃの粉末を均一に混合した後に、当該混合物を黒鉛るつぼ内に収納し、真空排気した直後に、金属Ａの融点より低く、かつ、金属Ｃの融点より低い温度で熱処理して、得られる均一組成の粉末合金であって、合金粉末の平均粒径が０．０１〜１００μｍであることを特徴とする合金粉末によっても達成される。 The subject is the second aspect of the present invention according to claim 5, that is, the metal A and the metal C that are easily thermally diffused with each other, and the metal A powder or the metal A hydrogen compound powder and the metal C powder are uniformly distributed. After mixing, the mixture is stored in a graphite crucible, and immediately after being evacuated, heat treatment is performed at a temperature lower than the melting point of the metal A and lower than the melting point of the metal C. The alloy powder is also achieved by an alloy powder characterized in that the average particle diameter of the alloy powder is 0.01 to 100 μm.
市販の不活性ガスを用いず、１０Ｐａ以下の真空度まで真空排気した直後に熱拡散処理しているので、酸素分圧が低い状態で昇温、保持、冷却され、酸化物が生成しにくい。 Since the thermal diffusion treatment is performed immediately after evacuation to a vacuum degree of 10 Pa or less without using a commercially available inert gas, the oxide is not easily generated because it is heated, held and cooled in a state where the oxygen partial pressure is low.
原料として粉末状の金属Ａの水素化合物を用いる場合には、加熱によって金属Ａの水素化合物が金属ＡとＨ２に分解され、発生したＨ２によって、金属Ａ粉末の表面を覆う酸化層が還元され除去され、金属Ａ粉末の表面が活性化される。 When a powdered metal A hydrogen compound is used as a raw material, the metal A hydrogen compound is decomposed into metal A and H 2 by heating, and the generated H 2 reduces the oxide layer covering the surface of the metal A powder. And the surface of the metal A powder is activated.
そのため、熱拡散速度が遅くならず、金属Ａと金属Ｃの固相−固相反応が促進され、比較的低温度かつ比較的短時間で原料金属Ｃ粉末の中心部まで熱による金属Ａの物質移動を均等に行うことができる。その結果、本発明によって、均一な組成の金属Ａ−金属Ｃの合金粉末を製造することができる。 Therefore, the thermal diffusion rate is not slowed, the solid-solid reaction between the metal A and the metal C is promoted, and the material of the metal A is heated to the center of the raw metal C powder at a relatively low temperature and in a relatively short time. The movement can be performed evenly. As a result, according to the present invention, a metal A-metal C alloy powder having a uniform composition can be produced.
以下、金属Ｍｇと金属Ｓｉとの合金の製造の実施形態について説明する。 Hereinafter, an embodiment of manufacturing an alloy of metal Mg and metal Si will be described.
実施例１
原料として、Ｍｇ粉末及びＳｉ粉末を使用した。Ｍｇ粉末（関東金属製）の純度は９９．９％であり、平均粒径は１００μｍであった。また、金属Ｓｉ粉末（東京印刷機材トレーディング（株）製）の純度は９９．９９９９％であり、平均粒径は１μｍであった。
Example 1
Mg powder and Si powder were used as raw materials. The purity of the Mg powder (manufactured by Kanto Metals) was 99.9%, and the average particle size was 100 μm. The purity of the metal Si powder (manufactured by Tokyo Printing Equipment Trading Co., Ltd.) was 99.9999%, and the average particle size was 1 μm.
上記のＭｇ粉末３．２ｋｇと上記のＳｉ粉末１．８５ｋｇをポリ容器内に秤量して、振とうしたところ、Ｍｇ粉末とＳｉ粉末は均一に混合されていた。 When 3.2 kg of the above Mg powder and 1.85 kg of the above Si powder were weighed into a plastic container and shaken, the Mg powder and the Si powder were uniformly mixed.
図１は本実施形態において使用した製造装置の概略図である。黒鉛るつぼ１は内径φ２７５ｍｍ×高さ２８０ｍｍであり、上面の中央にガス抜き穴１１が設けられている。混合原料２を黒鉛るつぼ１内に収納した後に、高周波加熱装置４を備えた真空容器３内に水平に配置した。 FIG. 1 is a schematic view of a manufacturing apparatus used in this embodiment. The graphite crucible 1 has an inner diameter φ275 mm × height 280 mm, and a gas vent hole 11 is provided in the center of the upper surface. After the mixed raw material 2 was accommodated in the graphite crucible 1, it was placed horizontally in a vacuum vessel 3 equipped with a high frequency heating device 4.
そして、混合原料２が飛散しないように注意しながら、配管５を通じて真空ポンプ６を用いて真空容器３内を１０Ｐａまで真空排気した。 And the inside of the vacuum vessel 3 was evacuated to 10 Pa using the vacuum pump 6 through the pipe 5 while taking care not to scatter the mixed raw material 2.
１０Ｐａまで真空排気した直後に、図２に示す熱処理パターンのように、室温（Ｔｒ）から６００℃（Ｔｍａｘ）まで1時間（０〜ｔ１）かけて昇温し、６００℃（Ｔｍａｘ）で５時間（ｔ１〜ｔ２）保持し、その後、加熱電源をＯＦＦして、自然冷却した。昇温、保持、冷却の間も真空ポンプ６を用いて真空排気を続けた。 Immediately after evacuation to 10 Pa, as shown in the heat treatment pattern shown in FIG. 2, the temperature was raised from room temperature (T r ) to 600 ° C. (T max ) over 1 hour (0 to t 1 ), and 600 ° C. (T max ) For 5 hours (t 1 to t 2 ), and then the heating power supply was turned off to naturally cool. Vacuum evacuation was continued using the vacuum pump 6 during the temperature raising, holding, and cooling.
混合原料２を十分に冷却した後、真空ポンプ６を停止し大気圧に戻し、黒鉛るつぼ１を取り出し、試料粉末を得た。 After the mixed raw material 2 was sufficiently cooled, the vacuum pump 6 was stopped and returned to atmospheric pressure, the graphite crucible 1 was taken out, and a sample powder was obtained.
得られた試料粉末についてＳＥＭ像を観察した。図３、図４は得られた試料粉末の走査電子顕微鏡観察写真である。なお図４は図３の部分拡大写真である。ＳＥＭ観察の結果、試料粉末は１μｍ程度の微粒子が凝集した形態であり、原料のＳｉ粉末の平均粒径と同等であった。このことから、原料粉末の融着はほとんど生じなかったと考えられる。また、得られた試料粉末には、約５％のマグネシウムの酸化物が含まれていた。 The SEM image was observed about the obtained sample powder. 3 and 4 are scanning electron microscope observation photographs of the obtained sample powder. FIG. 4 is a partially enlarged photograph of FIG. As a result of SEM observation, the sample powder was in a form in which fine particles of about 1 μm were aggregated, and was equivalent to the average particle diameter of the raw material Si powder. From this, it is considered that the raw material powder was hardly fused. The obtained sample powder contained about 5% magnesium oxide.
さらに、得られた試料粉末の断面を作成し、Ｍｇ分布、Ｓｉ分布、Ｏ分布を測定した。図５は得られた試料粉末の断面のカラーマップデータであり、（ａ）は断面のＳＥＭ像、（ｂ）はＭｇ分布、（ｃ）はＳｉ分布、（ｄ）はＯ分布を示している。Ｍｇ分布及びＳｉ分布ともに粒子の表面から中心にわたって均等であった。このことから、得られた試料粉末の組成は粒子の表面から中心にわたって均一になっていると考えられる。 Furthermore, the cross section of the obtained sample powder was created, and Mg distribution, Si distribution, and O distribution were measured. FIG. 5 is color map data of the cross section of the obtained sample powder, (a) shows the SEM image of the cross section, (b) shows the Mg distribution, (c) shows the Si distribution, and (d) shows the O distribution. . Both the Mg distribution and the Si distribution were uniform from the surface of the particle to the center. From this, it is considered that the composition of the obtained sample powder is uniform from the surface of the particle to the center.
実施例２
原料として、Ｍｇ粉末、ＭｇＨ２粉末及びＳｉ粉末を使用した。Ｍｇ粉末（関東金属製）の純度は９９．９％であり、平均粒径は１００μｍであった。ＭｇＨ２粉末（バイオコーク技研製）の純度は９９．９％であり、平均粒径は６０μｍであった。また、金属Ｓｉ粉末（東京印刷機材トレーディング（株）製）の純度は９９．９９９９％であり、平均粒径は１μｍであった。
Example 2
Mg powder, MgH 2 powder and Si powder were used as raw materials. The purity of the Mg powder (manufactured by Kanto Metals) was 99.9%, and the average particle size was 100 μm. The purity of MgH 2 powder (manufactured by Bio Coke Giken) was 99.9%, and the average particle size was 60 μm. The purity of the metal Si powder (manufactured by Tokyo Printing Equipment Trading Co., Ltd.) was 99.9999%, and the average particle size was 1 μm.
上記のＭｇ粉末１．６ｋｇと上記のＭｇＨ２粉末１．７３ｋｇと上記のＳｉ粉末１．８５ｋｇをポリ容器内に秤量して、振とうしたところ、Ｍｇ粉末とＭｇＨ２粉末とＳｉ粉末は均一に混合されていた。 When 1.6 kg of the above Mg powder, 1.73 kg of the above MgH 2 powder and 1.85 kg of the above Si powder were weighed into a plastic container and shaken, the Mg powder, MgH 2 powder and Si powder were uniformly distributed. It was mixed.
実施例１と同様に、混合原料２を黒鉛るつぼ１内に収納した後に、高周波加熱装置４を備えた真空容器３内に水平に配置した。 In the same manner as in Example 1, after the mixed raw material 2 was stored in the graphite crucible 1, it was horizontally disposed in the vacuum vessel 3 equipped with the high-frequency heating device 4.
そして、混合原料２が飛散しないように注意しながら、配管５を通じて真空ポンプ６を用いて真空容器３内を１０Ｐａまで真空排気した。 And the inside of the vacuum vessel 3 was evacuated to 10 Pa using the vacuum pump 6 through the pipe 5 while taking care not to scatter the mixed raw material 2.
１０Ｐａまで真空排気した直後に、図２に示す熱処理パターンのように、室温（Ｔｒ）から６００℃（Ｔｍａｘ）まで３時間（０〜ｔ１）かけてゆっくりと昇温し、６００℃（Ｔｍａｘ）で５時間（ｔ１〜ｔ２）保持し、その後、加熱電源をＯＦＦして、自然冷却した。昇温、保持、冷却の間も真空ポンプ６を用いて真空排気を続けた。急速に昇温すると時間当たりの水素発生量が多くなりすぎ混合原料２が飛散しやすくなることがわかった。 Immediately after evacuating to 10 Pa, as shown in the heat treatment pattern shown in FIG. 2, the temperature was slowly raised from room temperature (T r ) to 600 ° C. (T max ) over 3 hours (0 to t 1 ), and 600 ° C. ( (T max ) for 5 hours (t 1 to t 2 ), and then the heating power supply was turned off to naturally cool. Vacuum evacuation was continued using the vacuum pump 6 during the temperature raising, holding, and cooling. It has been found that when the temperature is rapidly increased, the amount of hydrogen generated per hour increases so that the mixed raw material 2 is easily scattered.
混合原料２を十分に冷却した後、真空ポンプ６を停止し大気圧に戻し、黒鉛るつぼ１を取り出し、試料粉末を得た。 After the mixed raw material 2 was sufficiently cooled, the vacuum pump 6 was stopped and returned to atmospheric pressure, the graphite crucible 1 was taken out, and a sample powder was obtained.
得られた試料粉末についてＳＥＭ像を観察した。ＳＥＭ観察の結果、試料粉末は１μｍ程度の微粒子が凝集した形態であり、原料のＳｉ粉末の平均粒径と同等であった。このことから、原料粉末の融着はほとんど生じなかったと考えられる。また、得られた試料粉末に含まれるマグネシウムの酸化物は１％以下であった。 The SEM image was observed about the obtained sample powder. As a result of SEM observation, the sample powder was in a form in which fine particles of about 1 μm were aggregated, and was equivalent to the average particle diameter of the raw material Si powder. From this, it is considered that the raw material powder was hardly fused. Moreover, the oxide of magnesium contained in the obtained sample powder was 1% or less.
さらに、得られた試料粉末の断面を作成し、Ｍｇ分布、Ｓｉ分布、Ｏ分布を測定した。Ｍｇ分布及びＳｉ分布ともに粒子の表面から中心にわたって均等であった。このことから、得られた試料粉末の組成は粒子の表面から中心にわたって均一になっていると考えられる。 Furthermore, the cross section of the obtained sample powder was created, and Mg distribution, Si distribution, and O distribution were measured. Both the Mg distribution and the Si distribution were uniform from the surface of the particle to the center. From this, it is considered that the composition of the obtained sample powder is uniform from the surface of the particle to the center.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5350494A (en) * | 1976-10-19 | 1978-05-08 | Matsushita Electric Ind Co Ltd | Production method of resistor compound |
| JPH0297603A (en) * | 1988-10-04 | 1990-04-10 | Tdk Corp | Silicon iron alloy powder and manufacture thereof and compacting core |
| JP2000054009A (en) * | 1998-08-07 | 2000-02-22 | Yazaki Corp | Production of alloy powder and production of thermoelement using it |
| WO2003027342A1 (en) * | 2001-09-25 | 2003-04-03 | Center For Advanced Science And Technology Incubation, Ltd. | Magnesium base composite material |
| JP2012190984A (en) * | 2011-03-10 | 2012-10-04 | Hitachi Chem Co Ltd | Magnesium silicide powder, sintered compact and thermoelectric conversion element using the same, and method for producing the same |
| JP2015145512A (en) * | 2014-01-31 | 2015-08-13 | 学校法人東海大学 | Method for producing intermetallic compound particle and intermetallic compound particle |
-
2016
- 2016-04-04 JP JP2016075403A patent/JP2017186600A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5350494A (en) * | 1976-10-19 | 1978-05-08 | Matsushita Electric Ind Co Ltd | Production method of resistor compound |
| JPH0297603A (en) * | 1988-10-04 | 1990-04-10 | Tdk Corp | Silicon iron alloy powder and manufacture thereof and compacting core |
| JP2000054009A (en) * | 1998-08-07 | 2000-02-22 | Yazaki Corp | Production of alloy powder and production of thermoelement using it |
| WO2003027342A1 (en) * | 2001-09-25 | 2003-04-03 | Center For Advanced Science And Technology Incubation, Ltd. | Magnesium base composite material |
| JP2012190984A (en) * | 2011-03-10 | 2012-10-04 | Hitachi Chem Co Ltd | Magnesium silicide powder, sintered compact and thermoelectric conversion element using the same, and method for producing the same |
| JP2015145512A (en) * | 2014-01-31 | 2015-08-13 | 学校法人東海大学 | Method for producing intermetallic compound particle and intermetallic compound particle |
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