TW201338895A - Method for fabricating alloy powder by mechanical alloying using opposed jet milling - Google Patents
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本發明是有關於製作合金的方法，特別是指一種機械合金化製作合金粉末的方法。The present invention relates to a method of making an alloy, and more particularly to a method of mechanically alloying an alloy powder.
以機械合金化製作合金粉末是一種通過高能球磨過程，使金屬粉末或合金粉末經受反覆的變形、冷焊、破碎，從而達到元素間原子水平合金化的複雜物理化學過程與技術；因為機械合金化製作合金粉末不需要高溫熔融、冷卻的常見冶金過程，而能在室溫得到均勻、精細結構的合金，因此已成為製作一般生產常規手段難以製備的合金種類，或新合金材料開發的方法。The alloying of alloy powder by mechanical alloying is a complex physical and chemical process and technology for subjecting metal powder or alloy powder to repeated deformation, cold welding and crushing through high-energy ball milling process to achieve atomic level alloying between elements; The alloy metal powder does not require a common metallurgical process of melting and cooling at a high temperature, and an alloy having a uniform and fine structure can be obtained at room temperature. Therefore, it has become a method for producing an alloy which is difficult to prepare by conventional production, or a method for developing a new alloy material.
一般來說，目前新興的儲氫材料、超導體材料、熱電材料、磁致冷材料，以及CIGS太陽能電池材料等都是採用機械合金化製作得到；例如CN101967591A號「機械合金化法製備Nb3Al超導材料的方法」專利案，揭示依序以高能球磨、粉末壓制和低溫快速燒結，以及低溫燒結和高溫合金化製作得到Nb3Al超導材料、CN1281775C號「一種鎂基儲氫材料及其機械合金化製備方法」專利案，揭示用傳統熔煉和球磨製作得到La-M-Mg系列儲氫合金材料、CN 101633985號「RE-FE-B系儲氫合金的製備方法」專利案，公開用高溫熔煉和球磨製作多相結構的RE-FE-B系儲氫合金、CN1202537C號「一種用機械合金化製備釤鐵氮永磁材料的方法」專利案，揭示用釤粉、鐵粉及具有促進滲氮作用的元素配合球磨製作釤鐵氮永磁材料、CN101786163號「高性能室溫磁致冷納米塊體材料的製備方法」專利案，揭示用球磨和放電等離子燒結製作La-Fe-Si基磁致冷材料，及CN101125367A號「一種用機械合金化製造CRW合金粉末的方法」專利案，揭示用鎢粉、鉻粉和添加總質量2%~5%過程控制劑球磨得到鉻鎢合金(CrW)粉末。In general, the emerging hydrogen storage materials, superconductor materials, thermoelectric materials, magnetic refrigeration materials, and CIGS solar cell materials are all produced by mechanical alloying; for example, CN101967591A "Mechanical alloying method for preparing Nb 3 Al super "Methods of Conducting Materials" patent case, revealing Nb 3 Al superconducting materials by high-energy ball milling, powder pressing and low-temperature rapid sintering, as well as low-temperature sintering and high-temperature alloying, CN1281775C "A magnesium-based hydrogen storage material and its machinery The patented preparation method discloses a La-M-Mg series hydrogen storage alloy material obtained by conventional smelting and ball milling, and a patent of CN 101633985 "Preparation method of RE-FE-B hydrogen storage alloy", which discloses a high temperature. Melting and ball milling to produce multi-phase structure of RE-FE-B hydrogen storage alloy, CN1202537C "A method for preparing yttrium-iron-nitrogen permanent magnet material by mechanical alloying" patent case, revealing bismuth powder, iron powder and promoting osmosis Nitrogen-based elements combined with ball milling to produce yttrium-iron-nitrogen permanent magnet materials, CN101786163 "Preparation method for high-performance room temperature magnetically cooled nano-block materials", disclosed La-Fe-Si-based magnetic refrigeration material prepared by ball milling and spark plasma sintering, and CN101125367A "A method for manufacturing CRW alloy powder by mechanical alloying" patent case, revealing the total mass of tungsten powder, chromium powder and added 2%~ A 5% process control agent was ball milled to obtain a chromium tungsten alloy (CrW) powder.
但是，目前各式機械合金化製作合金的方法普遍採用高能的研磨機或是球磨機進行機械合金化的過程，而無論是用研磨機或是球磨機，在進行機械合金化的過程中或多或少都會發生研磨介質汙染研磨物料的問題。However, at present, various methods of mechanical alloying alloys generally use a high-energy grinder or a ball mill for mechanical alloying, whether in a grinding machine or a ball mill, more or less in the process of mechanical alloying. There is a problem that the grinding media contaminates the abrasive material.
因此，本發明之目的，即在提供一種直接以氣體作為機械合金化介質，而不會產生介質汙染的以對衝式氣流研磨進行機械合金化製備合金粉末的方法。Accordingly, it is an object of the present invention to provide a method for mechanical alloying of alloy powders by controlled airflow milling using a gas as a mechanical alloying medium without causing media contamination.
於是，本發明一種以對衝式氣流研磨進行機械合金化製備合金粉末的方法，包含一反應腔準備步驟、一對撞合金化步驟，及一收集步驟。Thus, the present invention provides a method for mechanically alloying a alloy powder by countercurrent airflow milling, comprising a reaction chamber preparation step, a pair of impact alloying steps, and a collection step.
該反應腔準備步驟準備一具有一反應空間的反應腔，其中，該反應空間包括一收集部，及一相反於該收集部的撞擊開始發生部。The reaction chamber preparation step prepares a reaction chamber having a reaction space, wherein the reaction space includes a collection portion and an impact initiation portion opposite to the collection portion.
該對撞合金化步驟用一具有一第一流速的第一氣體推送一第一粉末至該撞擊開始發生部中，同時用一具有一第二流速的第二氣體相對該第一氣體推送一第二粉末使該第一粉末和第二粉末彼此高速對撞後向該收極部移動，並在對撞和移動的過程中重複發生粒子撞擊、界面合金化，而得到一合金粉末。The collisional alloying step pushes a first powder into the impact initiation portion with a first gas having a first flow rate, and simultaneously pushes a first gas with a second gas having a second flow rate. The two powders cause the first powder and the second powder to collide with each other at a high speed and then move toward the collector portion, and repeatedly collide with the particles and alloy the interface during the collision and movement to obtain an alloy powder.
該收集步驟於該收集部收集經過該合金粉末。The collecting step collects the alloy powder through the collecting portion.
本發明的目的及解決其技術問題還可採用於下技術措施進一步實現。The object of the present invention and solving the technical problems thereof can also be further implemented by the following technical measures.
較佳的，所述的以對衝式氣流研磨進行機械合金化製備合金粉末的方法還包含一再粉碎步驟，於該對撞合金化步驟後還通入氣體使該合金粉末重複發生粒子撞擊而粉碎和破碎，而得到粒徑小於原始第一粉末、第二粉末的合金粉末較佳地，該對撞合金化步驟中還選擇性地對該第一粉末和第二粉末其中至少一施加感應磁場。Preferably, the method for mechanically alloying the alloy powder by the cross-flow airflow grinding further comprises a re-pulverization step, wherein after the collision alloying step, a gas is introduced to cause the alloy powder to repeatedly pulverize and collide with the particles. Preferably, the alloy powder having a smaller particle diameter than the original first powder and the second powder is obtained, and the inversion alloying step selectively applies an induced magnetic field to at least one of the first powder and the second powder.
較佳地，該對撞合金化步驟中還選擇性地對該第一粉末和第二粉末其中至少一施加電場。Preferably, the counter-alloying step further selectively applies an electric field to at least one of the first powder and the second powder.
較佳地，該對撞合金化步驟中還選擇性地對該第一粉末和第二粉末其中至少一加溫。Preferably, at least one of the first powder and the second powder is selectively warmed in the collisional alloying step.
較佳地，該對撞合金化步驟中還選擇性地對該第一粉末和第二粉末其中至少一施加微波。Preferably, the collision alloying step further selectively applies microwaves to at least one of the first powder and the second powder.
較佳地，該對撞合金化步驟中還選擇性地對該第一氣體和第二氣體其中至少一加溫。Preferably, at least one of the first gas and the second gas is selectively heated in the collisional alloying step.
較佳地，該反應腔的反應空間成自該撞擊開始發生部向該收集部漸縮減的錐狀。Preferably, the reaction space of the reaction chamber is tapered from the impact initiation portion to the collection portion.
較佳地，該反應腔的反應空間包括多數成類球狀且彼此連通的球狀部。Preferably, the reaction space of the reaction chamber includes a plurality of spherical portions which are spherical and communicate with each other.
較佳地，該第一氣體和第二氣體是擇自下列所構成的群組：氫氣、氮氣、惰性氣體，及此等之一組合。Preferably, the first gas and the second gas are selected from the group consisting of hydrogen, nitrogen, an inert gas, and a combination thereof.
本發明之功效在於：提供一種以氣體作為載體，配合反應空間的空間體積自撞擊開始發生部向收集部漸縮減的反應腔，而以氣體推送第一、二粉末高速對撞，從而不斷發生界面合金化與碰撞粉碎的機械合金化製作合金粉末的方法，由於本發明無研磨介質，所以可以完全避免研磨介質的汙染，而得到純度高的合金粉末。The utility model has the advantages that the gas is used as a carrier, and the space volume of the reaction space is gradually reduced from the impact start portion to the reaction portion of the collecting portion, and the first and second powders are pushed by the gas at high speed, thereby continuously generating an interface. The method of mechanical alloying alloying and collision pulverization to form an alloy powder, since the present invention has no grinding medium, the contamination of the grinding medium can be completely avoided, and an alloy powder having high purity can be obtained.
有關本發明之前述及其他技術內容、特點與功效，在以下配合參考圖式之二個較佳實施例的詳細說明中，將可清楚的呈現。The above and other technical contents, features and advantages of the present invention will be apparent from the following detailed description of the preferred embodiments of the invention.
在本發明被詳細描述之前，要注意的是，在以下的說明內容中，類似的元件是以相同的編號來表示。Before the present invention is described in detail, it is noted that in the following description, similar elements are denoted by the same reference numerals.
參閱圖1與圖2，本發明一種以對衝式氣流研磨進行機械合金化製備合金粉末的方法的一第一較佳實施例，包含一反應腔準備步驟11、一對撞合金化步驟12，及一收集步驟13，用以機械合金化製作合金粉末。Referring to FIG. 1 and FIG. 2, a first preferred embodiment of a method for preparing an alloy powder by mechanical alloying by means of a cross-flow airflow polishing process comprises a reaction chamber preparation step 11, a pair of alloying step 12, and A collection step 13 is used to mechanically alloy the alloy powder.
首先進行該反應腔準備步驟11，準備一具有一反應空間21的反應腔2，其中，該反應空間21包括一收集部23，及一相反於該收集部23的撞擊開始發生部22，且該反應空間21的空間體積自該撞擊開始發生部22向該收集部23漸縮減成錐狀。First, the reaction chamber preparation step 11 is performed to prepare a reaction chamber 2 having a reaction space 21, wherein the reaction space 21 includes a collection portion 23, and an impact initiation portion 22 opposite to the collection portion 23, and the The space volume of the reaction space 21 is tapered from the impact start generating portion 22 to the collecting portion 23 to be tapered.
接著即以該對撞合金化步驟12，用具有第一流速的第一氣體推送第一粉末至該撞擊開始發生部22中，同時用具有第二流速的第二氣體相對該第一氣體推送第二粉末，使第一粉末、第二粉末彼此高速對撞後向該收集部23移動，並在對撞和移動的過程中重複發生粒子撞擊，而得到一合金粉末。Then, in the collisional alloying step 12, the first powder is pushed into the impact initiation portion 22 by the first gas having the first flow rate, and the second gas having the second flow velocity is pushed relative to the first gas. The two powders cause the first powder and the second powder to collide with each other at a high speed and then move toward the collecting portion 23, and repeatedly collide with the particles during the collision and movement to obtain an alloy powder.
最後於該收集步驟13於該收集部23收集經過產生的合金粉末。Finally, the produced alloy powder is collected in the collecting portion 23 in the collecting step 13.
參閱圖2、圖3，本發明一種以對衝式氣流研磨進行機械合金化製備合金粉末的方法的一第二較佳實施例，是與上例相似，其不同處在於還包含一再粉碎步驟14，於該對撞合金化步驟12後繼續通入氣體使合金粉末重複發生粒子撞擊而粉碎和破碎，而得到粒徑小於原始第一粉末、第二粉末的合金粉末。Referring to FIG. 2 and FIG. 3, a second preferred embodiment of the method for preparing an alloy powder by mechanical alloying by buffering airflow grinding is similar to the above example, and the difference is that a further pulverizing step 14 is further included. After the collision alloying step 12, the gas is continuously introduced to cause the alloy powder to repeatedly collide with the particles to be pulverized and crushed, thereby obtaining an alloy powder having a smaller particle diameter than the original first powder and the second powder.
另外要再說明的是，於該對撞合金化步驟12或是再粉碎步驟14中，還可選擇性地對該第一粉末和第二粉末其中至少一施加感應磁場、或是電場、或是微波而進一步提高第一粉末和第二粉末的內能，使該第一、二粉末對撞時更易發生界面合金化、粉碎和破碎；而且，施加感應磁場、或是電場、或是微波均可不藉助任何介質而直接透過反應腔2進行，所以可以不虞汙染的發生。In addition, in the collision alloying step 12 or the re-pulverizing step 14, optionally, an induced magnetic field, an electric field, or an electric field is applied to at least one of the first powder and the second powder. Microwave to further increase the internal energy of the first powder and the second powder, so that the first and second powders are more likely to undergo interface alloying, pulverization and crushing when colliding; and, the application of an induced magnetic field, an electric field, or a microwave may not Directly through the reaction chamber 2 by means of any medium, so that contamination does not occur.
此外，推送第一、二粉末的第一氣體和第二氣體可以視需要為惰性氣體，例如氬氣，僅單純作為載體，而不虞和第一、二粉末產生化學反應的氣體，或包含其他例如氫氣、氮氣等特定氣體，而同時達到氮化、滲碳、氫化，甚或氧化、還原等的固氣反應；當然，也可以改變第一、二氣體的相對吹送角度、速度，而使推送的第一、二粉末以預設的速度、碰撞角度產生最佳界面合金化、研磨，及合金計量的效果。In addition, the first gas and the second gas which push the first and second powders may be an inert gas, such as argon gas, as needed, only as a carrier, and do not react with the first or second powder to generate a chemical reaction gas, or include other, for example. a specific gas such as hydrogen or nitrogen, while at the same time achieving a solid-gas reaction of nitriding, carburizing, hydrogenation, or even oxidation, reduction, etc.; of course, it is also possible to change the relative blowing angle and speed of the first and second gases, and to push the first The first and second powders produce the best interface alloying, grinding, and alloy metering effects at a preset speed and collision angle.
參閱圖4，再者，該反應腔2的反應空間21還可以包括多數成類球狀且彼此連通的球狀部24，藉此讓第一、二粉末自該撞擊開始發生部22向該收集部23碰撞、移動的過程中，不斷地在每一球狀部24中環繞移動而發生更多次的碰撞、界面合金化。Referring to FIG. 4, further, the reaction space 21 of the reaction chamber 2 may further include a plurality of spherical portions 24 which are spherical and communicate with each other, thereby allowing the first and second powders to be collected from the impact initiation portion 22. During the collision and movement of the portion 23, it continuously moves around each of the spherical portions 24 to cause more collisions and alloying of the interface.
以下以二實驗例進一步說明本發明以對衝式氣流研磨進行機械合金化製備合金粉末的方法。Hereinafter, the method for preparing an alloy powder by mechanical alloying by a cross-flow air jet grinding will be further described in the following two experimental examples.
【實驗例一】製備鋁鈮合金粉末(Nb3Al)[Experimental Example 1] Preparation of aluminum-bismuth alloy powder (Nb 3 Al)
取1μm~5μm的純鈮粉末1040克及純鋁粉末100克，分別放入如圖1所示的反應腔2。1040 g of pure strontium powder of 1 μm to 5 μm and 100 g of pure aluminum powder were taken and placed in the reaction chamber 2 as shown in FIG.
利用電阻加熱將純鈮粉末升溫至1600℃、純鋁粉末升溫至500℃(為了避免偏析及局部熔解情形出現，鋁粉的溫度不宜超過其熔點660.45℃)、並以氬氣(Ar)作為載送氣體，將氣體速度調至200m/s，並以原料流量閥控制純鈮粉末的流量為每分鐘104克、純鋁粉末的流量為每分鐘10克，對撞時間為10分鐘，10分鐘後繼續放入氬氣進行研磨10分鐘，即可收集得到鋁鈮合金粉末(Nb3Al)。The pure tantalum powder is heated to 1600 ° C by resistance heating, and the pure aluminum powder is heated to 500 ° C (in order to avoid segregation and local melting, the temperature of the aluminum powder should not exceed the melting point of 660.45 ° C), and the argon (Ar) is used as the load. Gas is supplied, the gas velocity is adjusted to 200m/s, and the flow rate of the pure tantalum powder is controlled by the raw material flow valve to be 104 grams per minute, the flow rate of pure aluminum powder is 10 grams per minute, and the collision time is 10 minutes, after 10 minutes. The aluminum bismuth alloy powder (Nb 3 Al) was collected by continuously adding argon gas for 10 minutes.
【實驗例二】製備Cu0.7In0.3GaSe2合金粉末[Experiment 2] Preparation of Cu 0.7 In 0.3 GaSe 2 alloy powder
準備粒徑1μm~5μm的銅(Cu)粉末980克、銦(In)粉末1233克、鎵(Ga)粉末321.7克及硒(Se)粉末2415克(即依據莫耳比0.7:0.3:1:0.2的比例)，分別放入如圖1所示的反應腔2中。Prepare 980 g of copper (Cu) powder with a particle size of 1 μm to 5 μm, 1233 g of indium (In) powder, 321.7 g of gallium (Ga) powder, and 2415 g of selenium (Se) powder (ie, according to molar ratio of 0.7:0.3:1: The ratio of 0.2 is placed in the reaction chamber 2 as shown in Fig. 1, respectively.
利用電阻加熱將銅(Cu)粉末升溫至600℃，銦(In)粉末升溫至500℃，鎵(Ga)粉末昇溫至600℃，硒(Se)粉末升溫至100℃，其中因為硒(Se)的沸點為685℃，熔點為217℃，所以銅(Cu)粉末、鎵(Ga)粉末的溫度均不超過600℃，以避免硒(Se)瞬間氣化而發生***。同時配合以氬氣作為載送氣體，將氣體速度調至150m/s，並調整原料流量閥控制銅(Cu)粉末的流量為每分鐘49克、銦(In)粉末的流量為每分鐘61.6克、鎵(Ga)粉末的流量為每分鐘16.6克、硒(Se)粉末的流量為每分鐘120.3克，對撞時間為20分鐘，20分鐘後繼續放入氣體進行研磨10分鐘，冷卻可收集得到Cu0.7In0.3GaSe2合金粉末。The copper (Cu) powder is heated to 600 ° C by resistance heating, the indium (In) powder is heated to 500 ° C, the gallium (Ga) powder is heated to 600 ° C, and the selenium (Se) powder is heated to 100 ° C, wherein selenium (Se) The boiling point is 685 ° C, the melting point is 217 ° C, so the temperature of copper (Cu) powder, gallium (Ga) powder does not exceed 600 ° C, to avoid the explosion of selenium (Se) instantaneous vaporization. At the same time, argon gas is used as carrier gas, the gas velocity is adjusted to 150m/s, and the raw material flow valve is adjusted to control the flow rate of copper (Cu) powder to 49 grams per minute, and the flow rate of indium (In) powder is 61.6 grams per minute. The flow rate of gallium (Ga) powder is 16.6 grams per minute, the flow rate of selenium (Se) powder is 120.3 grams per minute, the collision time is 20 minutes, and after 20 minutes, the gas is continuously placed for grinding for 10 minutes, and the cooling can be collected. Cu 0.7 In 0.3 GaSe 2 alloy powder.
綜上所述，本發明是提出利用第一、二氣體推送欲機械合金化的第一、二粉末，使第一、二粉末高速對撞產生的機械摩擦，導致對撞的第一、二粉末產生介面合金化，並隨著粉體碰撞次數增加、粉末變細，隨之機械合金化程度也逐漸升高，而完成合金粉末的製備；由於本發明整個機械合金化的過程完全不需要研磨介質，同時還可以藉著推送的第一、二氣體完成氮化、滲碳、氫化，甚或氧化、還原等的固氣反應，所以可以完全改善現有的機械合金化的製作過程中，無法排除研磨介質的存在而會產生研磨介質汙染的問題，故確實能達成本發明之目的。In summary, the present invention proposes to use the first and second gases to push the first and second powders to be mechanically alloyed, so that the first and second powders collide with each other at high speed, resulting in collision of the first and second powders. The interface alloying is generated, and as the number of powder collisions increases, the powder becomes finer, and the degree of mechanical alloying gradually increases, and the preparation of the alloy powder is completed; since the entire mechanical alloying process of the present invention does not require grinding medium at all At the same time, it is also possible to complete the solid-gas reaction of nitriding, carburizing, hydrogenation, or even oxidation and reduction by pushing the first and second gases, so that the existing mechanical alloying process can be completely improved, and the grinding medium cannot be excluded. The existence of the grinding medium causes the problem of contamination of the grinding medium, so that the object of the present invention can be achieved.
惟以上所述者，僅為本發明之較佳實施例而已，當不能以此限定本發明實施之範圍，即大凡依本發明申請專利範圍及發明說明內容所作之簡單的等效變化與修飾，皆仍屬本發明專利涵蓋之範圍內。The above is only the preferred embodiment of the present invention, and the scope of the invention is not limited thereto, that is, the simple equivalent changes and modifications made by the scope of the invention and the description of the invention are All remain within the scope of the invention patent.
11．．．反應腔準備步驟11. . . Reaction chamber preparation step
12．．．對撞合金化步驟12. . . Collision alloying step
13．．．收集步驟13. . . Collection step
14．．．再粉碎步驟14. . . Re-grinding step
2．．．反應腔2. . . Reaction chamber
21．．．反應空間twenty one. . . Reaction space
22．．．撞擊開始發生部twenty two. . . Impact start
23．．．收集部twenty three. . . Collection department
24．．．球狀部twenty four. . . Spherical part
圖1是一流程圖，說明本發明一種以對衝式氣流研磨進行機械合金化製備合金粉末的方法的一第一較佳實施例；1 is a flow chart showing a first preferred embodiment of the present invention for preparing a alloy powder by mechanical alloying by means of a cross-flow type air jet;
圖2是一示意圖，說明本發明一種以對衝式氣流研磨進行機械合金化製備合金粉末的方法的較佳實施例的一反應腔；Figure 2 is a schematic view showing a reaction chamber of a preferred embodiment of the method for preparing an alloy powder by mechanical alloying by means of a cross-flow type air jet;
圖3是一流程圖，說明本發明一種以對衝式氣流研磨進行機械合金化製備合金粉末的方法的一第二較佳實施例；及Figure 3 is a flow chart showing a second preferred embodiment of the present invention for preparing a alloy powder by mechanical alloying by means of a cross-flow type air jet; and
圖4是一示意圖，說明本發明一種以對衝式氣流研磨進行機械合金化製備合金粉末的方法的較佳實施例的另一種態樣的反應腔。Figure 4 is a schematic view showing another aspect of the reaction chamber of a preferred embodiment of the method for mechanically alloying an alloy powder by countercurrent flow milling.
11．．．反應腔準備步驟11. . . Reaction chamber preparation step
12．．．對撞合金化步驟12. . . Collision alloying step
13．．．收集步驟13. . . Collection step
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