TWI747671B - Method for manufacturing homogeneous tungsten-copper alloy - Google Patents
Method for manufacturing homogeneous tungsten-copper alloy Download PDFInfo
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本發明係有關於一種鎢銅合金粉末之製程。 The present invention relates to a manufacturing process of tungsten copper alloy powder.
鎢銅複合材料結合了鎢的高強度、高熔點、較低線膨脹係數和銅的高導電、導熱性，具有良好的導電導熱性能、耐電弧燒蝕性能、耐高溫抗氧化及抗熔焊性等特點。隨著鎢銅複合材料應用的擴展，對於緻密度和微觀組織結構等性能指標的要求也越來越高。然而，鎢和銅互不固溶，是一種典型的假合金，在燒結的過程中很難緻密。 Tungsten copper composite material combines the high strength, high melting point, low linear expansion coefficient of tungsten and the high electrical and thermal conductivity of copper. It has good electrical and thermal conductivity, arc ablation resistance, high temperature resistance, oxidation resistance, and welding resistance, etc. Features. With the expansion of the application of tungsten copper composite materials, the requirements for performance indicators such as density and microstructure are getting higher and higher. However, tungsten and copper do not dissolve in each other, which is a typical pseudo-alloy, and it is difficult to densify during the sintering process.
目前製備鎢銅複合材料的技術種類通常有熔滲法、液相活化燒結法等兩種方法。其中熔滲法是將鎢粉或移入部分銅粉的混合粉末壓製成胚塊，然後在胚塊上放置所需的銅粉(壓塊)，使銅熔化滲入到壓胚的孔隙中，形成鎢銅材料。其缺點是產品尺寸變化大，精度低，需要預留較多的加工餘量，不僅效率低，且原材料浪費較大，製造成本高。此外，該技術方法難以得到鎢銅元素均勻分散、相互包裹的鎢銅合金。另外液相活化燒結法是採用常規粉末冶金製程，即混粉、壓制和燒結。為了降低燒結溫度，在壓坯中添加了微量的例如鎳、鈷、氧化銅等燒結助劑，從而達到降低燒結溫度的效果。其缺點是合金中引入了不需要的合金元素，降低了合金的導熱率，製備得到的鎢銅合金局部會存在微孔，因此氣密性和熱導率都低於熔滲法。除了以上所提到的一些局限性或缺點，上述兩種技術方法還存在一些共同的缺陷：(1)粉末混料和燒結過程難以完全避免污染，使得合 金中的氧、氮等雜質總含量較高，阻礙了其在高真空環境的應用；(2)合金中鎢的分佈均勻性難以得到保證。 Currently, there are two methods for preparing tungsten copper composite materials: infiltration method and liquid phase activation sintering method. Among them, the infiltration method is to press the tungsten powder or the mixed powder transferred into part of the copper powder into a blank, and then place the required copper powder (brick) on the blank, so that the copper melts and penetrates into the pores of the blank to form tungsten Copper material. The disadvantage is that the product size changes greatly, the accuracy is low, and more processing allowances need to be reserved, which is not only low in efficiency, but also has a large waste of raw materials and high manufacturing costs. In addition, it is difficult to obtain a tungsten-copper alloy in which tungsten-copper elements are uniformly dispersed and wrapped in each other with this technical method. In addition, the liquid phase activation sintering method adopts the conventional powder metallurgy process, that is, powder mixing, pressing and sintering. In order to reduce the sintering temperature, a small amount of sintering aids such as nickel, cobalt, copper oxide, etc. are added to the compact to achieve the effect of reducing the sintering temperature. The disadvantage is that unnecessary alloy elements are introduced into the alloy, which reduces the thermal conductivity of the alloy. The prepared tungsten copper alloy has micropores locally, so the air tightness and thermal conductivity are lower than the infiltration method. In addition to the limitations or shortcomings mentioned above, the above two technical methods also have some common defects: (1) The powder mixing and sintering process are difficult to completely avoid pollution, which makes the combination The high total content of impurities such as oxygen and nitrogen in gold hinders its application in high vacuum environments; (2) the uniformity of tungsten distribution in the alloy is difficult to guarantee.
例如2018年2月27日中國大陸所公開之發明第CN107739862號「一種鎢銅合金材料的製備方法」，主要係將氧化銅(CuO)粉末與鎢(W)粉混合粉末進行兩次還原處理，每次還原處理後壓實壓制成型，然後破碎為粉末，再進行下一步操作；然後將得到的混合粉末製成壓坯，在壓坯上下放置銅薄片，進行燒結和初步滲銅；最後將處理後的材料置於石墨容器中，並將鎢絲編制體置於材料上，真空下熔融滲銅，即制得銅鎢觸頭材料。其係以氧化銅(CuO)粉替代誘導銅(Cu)粉、以鎢絲編織體作為骨架，不僅提高了觸頭材料的耐電弧燒損性，同時提高了其強度。 For example, the invention No. CN107739862 "A preparation method of tungsten-copper alloy material" published on February 27, 2018 in Mainland China is mainly to reduce the mixed powder of copper oxide (CuO) powder and tungsten (W) powder twice. After each reduction treatment, it is compacted and molded, then crushed into powder, and then proceeded to the next step; then the obtained mixed powder is made into a compact, and copper flakes are placed on and above the compact for sintering and preliminary copper infiltration; finally, the treatment The latter material is placed in a graphite container, and a tungsten wire woven body is placed on the material, and copper is melted in a vacuum to obtain a copper-tungsten contact material. It uses copper oxide (CuO) powder instead of induced copper (Cu) powder and a tungsten wire braid as the skeleton, which not only improves the arc burn resistance of the contact material, but also improves its strength.
又有2016年3月30日中國大陸所公開之發明第CN105441766號「高比重鎢合金及其製備方法」，主要係屬於金屬材料領域。以品質百分數計，鎢合金成分如下：鎢95.0%~99.0%，氧化鋯1.0%~5.0%，以及不可避免的雜質；製備步驟包括：(1)分別將偏鎢酸銨、硝酸鋯溶於水中，混合，混合液乾燥得粉末，粉末經煆燒、還原得到複合鎢粉；(2)複合鎢粉球磨後經壓制成型、燒結得到燒結坯料，燒結坯料脫氫處理後經變形、熱處理得到高比重鎢合金。其主要係通過液-液摻雜法在鎢基體中加入二氧化鋯(ZrO2)強化相，並採用兩段燒結工藝、脫氫處理、旋鍛處理製備鎢合金，解決了傳統鎢合金強化相分佈不均、氫脆、燒結密度不高等問題，為鎢合金在新領域的應用和發展提供了新的方向。 There is also the invention No. CN105441766 "High specific gravity tungsten alloy and its preparation method" published on March 30, 2016 in Mainland China, which mainly belongs to the field of metal materials. In terms of quality percentage, the composition of the tungsten alloy is as follows: 95.0%-99.0% tungsten, 1.0%-5.0% zirconia, and inevitable impurities; the preparation steps include: (1) Dissolve ammonium metatungstate and zirconium nitrate in water, respectively , Mixing and drying the mixed solution to obtain powder. The powder is sintered and reduced to obtain composite tungsten powder; (2) After ball milling, the composite tungsten powder is press-formed and sintered to obtain a sintered blank. After dehydrogenation treatment, the sintered blank is deformed and heat-treated to obtain a high specific gravity. Tungsten alloy. It is mainly through liquid-liquid doping method to add zirconium dioxide (ZrO2) strengthening phase to the tungsten matrix, and adopts two-stage sintering process, dehydrogenation treatment, and rotary forging treatment to prepare tungsten alloy, which solves the traditional tungsten alloy strengthening phase distribution Problems such as unevenness, hydrogen embrittlement, and low sintering density provide a new direction for the application and development of tungsten alloys in new fields.
上述專利前案均會因為鎢、銅係為熔點相差極大的二元合金，因此在常常會因為鎢、銅粉末的混合不均，造成性質的不穩定，因此燒結成為鎢銅複合材料後，其結構當然也會造成性質的不穩定，以至於影響到產品使用的局限性，這樣的局限對於日益蓬勃發展且追求穩定快速的通訊3C產業而言，無疑是一個重大的致命缺點。 The previous patents mentioned above are due to the fact that tungsten and copper are binary alloys with very different melting points. Therefore, the uneven mixing of tungsten and copper powders often causes instability in properties. Therefore, after sintering to become a tungsten-copper composite material, its Of course, the structure will also cause instability in nature, so as to affect the limitations of product use. Such limitations are undoubtedly a major fatal flaw for the increasingly vigorously developing and pursuing stable and fast communication 3C industry.
爰此，有鑑於目前習知鎢銅複合材料在製程上具有上述的缺點。故本發明提供一種勻相鎢銅合金之製造方法，包含有：製備一偏鎢酸銨溶液及一氧化銅粉末，將一偏鎢酸銨溶於水中，使其形成該偏鎢酸銨水溶液；再將該氧化銅粉末置入一析鍍空間內，然後將該偏鎢酸銨水溶液加入該析鍍空間內，使該氧化銅粉末溶入於偏鎢酸銨水溶液中，進行加熱使水分蒸發，使得一鎢會析鍍在該氧化銅粉末的表面，以形成一鎢鍍銅粉末；將該鎢鍍銅粉末置入於一還原空間內，並於該還原空間內加入一氫氣，以3℃/min升溫到500℃，持溫1小時，再以3℃/min升溫至700℃至900℃之間的還原溫度，持溫12小時後，再自然冷卻，以形成一鎢銅合金粉末。 In view of this, in view of the above-mentioned shortcomings in the manufacturing process of conventional tungsten-copper composite materials. Therefore, the present invention provides a method for manufacturing a homogeneous tungsten copper alloy, which includes: preparing an ammonium metatungstate solution and copper oxide powder, and dissolving an ammonium metatungstate in water to form the ammonium metatungstate aqueous solution; Then put the copper oxide powder into a deposition space, then add the ammonium metatungstate aqueous solution into the deposition space, dissolve the copper oxide powder in the ammonium metatungstate aqueous solution, and heat to evaporate the water. A tungsten is deposited on the surface of the copper oxide powder to form a copper-plated tungsten powder; the copper-plated tungsten powder is placed in a reduction space, and a hydrogen gas is added to the reduction space at a temperature of 3°C/ The temperature is raised to 500°C for 1 hour, and then raised to a reduction temperature between 700°C and 900°C at 3°C/min. After holding the temperature for 12 hours, it is cooled naturally to form a tungsten copper alloy powder.
上述係將220公克的該偏鎢酸銨溶於200公克的該水中，使其形成該偏鎢酸銨水溶液。 In the above system, 220 g of the ammonium metatungstate was dissolved in 200 g of the water to form the ammonium metatungstate aqueous solution.
上述將50公克的該氧化銅粉末放入該析鍍空間內，然後加入420公克的該偏鎢酸銨水溶液。 As mentioned above, 50 grams of the copper oxide powder was put into the precipitation space, and then 420 grams of the ammonium metatungstate aqueous solution was added.
上述析鍍空間內的加熱溫度係為100℃至120℃之間，加熱時間則為.5小時至2小時之間。 The heating temperature in the deposition space is between 100°C and 120°C, and the heating time is between 0.5 hours and 2 hours.
上述還原空間內的該氫氣流量係為每分鐘1公升，該鎢鍍銅粉末的添加量係為10公克至50公克。 The hydrogen flow rate in the reduction space is 1 liter per minute, and the added amount of the tungsten copper-plated powder is 10 grams to 50 grams.
上述還原溫度係為700℃、750℃、800℃、850℃或900℃。 The aforementioned reduction temperature is 700°C, 750°C, 800°C, 850°C, or 900°C.
進一步對於上述鎢銅合金粉末進行性質分析，該性質分析包含：粒徑分析、振實密度、含氧量分析、外觀觀察的其中之一或其任意組合，該粒徑分析係確認該鎢銅合金粉末全部的平均粒徑有90%≦6um，有50%≦2um，有10%≦0.8um，該振實密度係高於30%理論密度，該理論密度係為15.68g/cm3， 該含氧量需要小於3000ppm，該外觀觀察係在放大5000倍至10000倍的放大倍率範圍下看到獨立的顆粒。 The property analysis of the above-mentioned tungsten-copper alloy powder is further carried out. The property analysis includes one or any combination of particle size analysis, tap density, oxygen content analysis, and appearance observation. The particle size analysis confirms that the tungsten-copper alloy The average particle size of all powders is 90%≦6um, 50%≦2um, and 10%≦0.8um. The tap density is higher than 30% of the theoretical density, and the theoretical density is 15.68g/cm 3 . The oxygen content needs to be less than 3000 ppm, and the appearance observation system can see independent particles under the magnification range of 5000 times to 10000 times.
對於上述鎢銅合金粉末進行燒結程序，以形成一鎢銅複合材料，該燒結程序包含：模壓壓力設定為200MPa，以3℃/min升溫到500℃後，持溫1小時，再以2℃/min升溫至950℃後，持溫2小時，再以2℃/min升溫至1150℃後，持溫1小時，再以3℃/min升溫至1250℃至1280℃後，持溫1小時，再自然冷卻到室溫後取出，以形成該鎢銅複合材料。 The above-mentioned tungsten-copper alloy powder is subjected to a sintering procedure to form a tungsten-copper composite material. The sintering procedure includes: setting the molding pressure to 200MPa, raising the temperature to 500°C at 3°C/min, holding the temperature for 1 hour, and then at 2°C/min. After the temperature is raised to 950°C in min, hold the temperature for 2 hours, then at 2°C/min to 1150°C, hold the temperature for 1 hour, and then at 3°C/min to 1250°C to 1280°C, hold the temperature for 1 hour, and then After being naturally cooled to room temperature, it is taken out to form the tungsten copper composite material.
上述鎢銅複合材料的燒結性質分析包含：密度量測、導電率量測、微觀結構觀察、硬度量測的其中之一或其任意組合，該密度量測係其密度大於15g/cm3，該導電率係大於46%，該微觀結構觀察係透過掃描式電子顯微鏡進行微結構觀察，其斷面微結構係為連續式銅網包覆鎢晶粒結構，該硬度測量之其硬度值係為Hv175至325之間。 The analysis of the sintering properties of the above-mentioned tungsten-copper composite material includes one of density measurement, electrical conductivity measurement, microstructure observation, hardness measurement, or any combination thereof. The density measurement system has a density greater than 15g/cm 3 . The electrical conductivity is greater than 46%. The microstructure is observed through a scanning electron microscope. The microstructure of the section is a continuous copper mesh covered with tungsten grain structure. The hardness value of the hardness measurement is Hv175 To 325.
上述技術特徵具有下列之優點： The above technical features have the following advantages:
1.經由混拌加熱後，可將鎢均勻析鍍在氧化銅粉末之顆粒上，再透過適當的還原製程與參數控制可將鎢及銅等氧化物完全還原，以製成均勻結合的鎢銅合金粉末。 1. After mixing and heating, tungsten can be uniformly deposited on the particles of copper oxide powder, and then through appropriate reduction process and parameter control, oxides such as tungsten and copper can be completely reduced to produce uniformly combined tungsten copper Alloy powder.
2.再配合適當的燒結參數控制，燒結後可以得到完全緻密且具有均勻的連續式銅網包覆鎢晶粒的鎢銅合金網狀結構，不但機械性質良好，而且具有高導電率，可用以做為高效元件之應用。 2. With proper sintering parameter control, after sintering, a completely dense tungsten-copper alloy network structure with uniform continuous copper mesh coated with tungsten grains can be obtained, which not only has good mechanical properties, but also has high electrical conductivity, which can be used for As an application of high-efficiency components.
1:氧化銅粉末之顆粒 1: Particles of copper oxide powder
2:攪拌桶 2: Mixing barrel
21:析鍍空間 21: Analysis of plating space
22:攪拌片 22: Stirring tablets
3:馬達 3: motor
4:加熱線圈 4: heating coil
[第一圖]係為本發明實施例之製造流程圖。 [The first figure] is a manufacturing flow chart of an embodiment of the present invention.
[第二圖]係為本發明實施例之操作方塊圖。 [The second figure] is a block diagram of the operation of the embodiment of the present invention.
[第三圖]係為本發明實施例攪拌桶之構造示意圖。 [The third figure] is a schematic diagram of the structure of the mixing barrel of the embodiment of the present invention.
[第四圖]係為本發明實施例攪拌桶內攪拌片之使用示意圖。 [Fourth Figure] is a schematic diagram of the use of the stirring blade in the stirring barrel of the embodiment of the present invention.
[第五圖]係為本發明實施例進行還原程序升溫時的時間及溫度之關係示意圖。 [Fifth Figure] is a schematic diagram of the relationship between time and temperature when the temperature is raised during the reduction program in the embodiment of the present invention.
[第六圖]係為本發明實施例透過掃描式電子顯微鏡放大10000倍看到鎢銅合金粉末的獨立顆粒之金相圖。 [Figure 6] is a metallographic diagram of individual particles of tungsten-copper alloy powder seen through a scanning electron microscope at a magnification of 10000 times in an embodiment of the present invention.
[第七圖]係為本發明實施例透過掃描式電子顯微鏡放大10000倍看到鎢銅合金粉末的獨立顆粒之金相圖。 [The seventh figure] is a metallographic diagram of individual particles of tungsten copper alloy powder seen through a scanning electron microscope magnified 10000 times in an embodiment of the present invention.
[第八圖]係為本發明實施例進行燒結程序升溫時的時間及溫度之關係示意圖。 [The eighth figure] is a schematic diagram of the relationship between time and temperature during the sintering program temperature rise in the embodiment of the present invention.
[第九圖]係為本發明實施例升溫至700℃還原後鎢鍍銅粉末之外觀相片。 [Figure 9] is a photograph of the appearance of tungsten copper-plated powder after reduction at 700°C in an embodiment of the present invention.
[第十圖]係為本發明實施例升溫至750℃還原後鎢鍍銅粉末之外觀相片。 [Figure 10] is a photograph of the appearance of tungsten copper-plated powder after reduction at 750°C in an embodiment of the present invention.
[第十一圖]係為本發明實施例升溫至800℃還原後鎢鍍銅粉末之外觀相片。 [Figure eleven] is a photograph of the appearance of tungsten copper-plated powder after heating to 800°C for reduction in an embodiment of the present invention.
[第十二圖]係為本發明實施例升溫至850℃還原後鎢鍍銅粉末之外觀相片。 [Figure 12] is a photograph of the appearance of tungsten copper-plated powder after heating to 850°C for reduction in an embodiment of the present invention.
[第十三圖]係為本發明實施例升溫至900℃還原後鎢鍍銅粉末之外觀相片。 [Figure 13] is a photograph of the appearance of tungsten copper-plated powder after heating to 900°C for reduction in an embodiment of the present invention.
[第十四圖]係為本發明實施例鎢銅合金粉末在不同還原溫度下的氧含量之變化曲線圖。 [Figure 14] is a graph showing the variation of oxygen content of tungsten-copper alloy powder at different reduction temperatures in the embodiment of the present invention.
[第十五圖]係為本發明實施例鎢銅合金粉末在不同還原溫度下的X-射線繞射分析比對示意圖。 [Figure 15] is a schematic diagram of the comparison of the X-ray diffraction analysis of the tungsten copper alloy powder at different reduction temperatures in the embodiment of the present invention.
[第十六圖]係為本發明實施例鎢銅合金粉末在不同時間及不同還原溫度下的X-射線繞射分析比對示意圖。 [Figure 16] is a schematic diagram of the comparison of X-ray diffraction analysis of tungsten copper alloy powders at different times and at different reduction temperatures in the embodiments of the present invention.
[第十七圖]係為本發明實施例透過掃描式電子顯微鏡放大5000倍看到鎢銅合金粉末呈現多角型態之金相圖。 [Figure 17] is a metallographic diagram showing the polygonal shape of the tungsten-copper alloy powder through a scanning electron microscope magnified 5000 times in an embodiment of the present invention.
[第十八圖]係為本發明實施例透過掃描式電子顯微鏡放大10000倍看到鎢銅合金粉末呈現多角型態之金相圖。 [Figure 18] is a metallographic diagram showing the polygonal shape of the tungsten-copper alloy powder through a scanning electron microscope magnified 10,000 times in an embodiment of the present invention.
[第十九圖]係為本發明實施例於不同還原溫度所獲得的鎢銅合金粉末，其密度隨著燒結溫度增加的變化曲線圖。 [Figure 19] is a graph showing the density of tungsten-copper alloy powders obtained at different reduction temperatures in the examples of the present invention as the sintering temperature increases.
[第二十圖]係為本發明實施例於不同還原溫度所獲得的鎢銅合金粉末，其硬度隨著燒結溫度增加的變化曲線圖。 [Figure twentieth] is a graph showing changes in hardness of tungsten-copper alloy powders obtained at different reduction temperatures in the examples of the present invention with increasing sintering temperature.
[第二十一圖]係為本發明實施例於不同還原溫度所獲得的鎢銅合金粉末，其導電率隨著燒結溫度增加的變化曲線圖。 [Figure 21] is a graph showing the electrical conductivity of tungsten-copper alloy powders obtained at different reduction temperatures in the embodiments of the present invention as the sintering temperature increases.
[第二十二圖]係為本發明實施例還原溫度700℃的鎢銅合金粉末經最終燒結溫度1220℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Twenty-second Figure] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten copper alloy powder with a reduction temperature of 700°C at a final sintering temperature of 1220°C and a holding temperature for 2 hours in the embodiment of the present invention.
[第二十三圖]係為本發明實施例還原溫度750℃的鎢銅合金粉末經最終燒結溫度1220℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Twenty-third Figure] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten-copper alloy powder with a reduction temperature of 750°C at a final sintering temperature of 1220°C and holding the temperature for 2 hours in an embodiment of the present invention.
[第二十四圖]係為本發明實施例還原溫度800℃的鎢銅合金粉末經最終燒結溫度1220℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Twenty-fourth Figure] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten-copper alloy powder with a reduction temperature of 800°C at a final sintering temperature of 1220°C and holding the temperature for 2 hours in an embodiment of the present invention.
[第二十五圖]係為本發明實施例還原溫度850℃的鎢銅合金粉末經最終燒結溫度1220℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Figure 25] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten copper alloy powder with a reduction temperature of 850°C at a final sintering temperature of 1220°C and holding the temperature for 2 hours in the embodiment of the present invention.
[第二十六圖]係為本發明實施例還原溫度900℃的鎢銅合金粉末經最終燒結溫度1220℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Figure 26] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten copper alloy powder with a reduction temperature of 900°C at a final sintering temperature of 1220°C and a holding temperature for 2 hours in the embodiment of the present invention.
[第二十七圖]係為本發明實施例還原溫度700℃的鎢銅合金粉末經最終燒結溫度1250℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Figure 27] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten copper alloy powder with a reduction temperature of 700°C at a final sintering temperature of 1250°C and holding the temperature for 2 hours in an embodiment of the present invention.
[第二十八圖]係為本發明實施例還原溫度750℃的鎢銅合金粉末經最終燒結溫度1250℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Figure 28] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten copper alloy powder with the reduction temperature of 750°C at a final sintering temperature of 1250°C and holding the temperature for 2 hours in the embodiment of the present invention.
[第二十九圖]係為本發明實施例還原溫度800℃的鎢銅合金粉末經最終燒結溫度1250℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Figure 29] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten copper alloy powder with a reduction temperature of 800°C at a final sintering temperature of 1250°C and a holding temperature for 2 hours in the embodiment of the present invention.
[第三十圖]係為本發明實施例還原溫度850℃的鎢銅合金粉末經最終燒結溫度1250℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Figure 30] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten copper alloy powder with a reduction temperature of 850°C at a final sintering temperature of 1250°C and holding the temperature for 2 hours in an embodiment of the present invention.
[第三十一圖]係為本發明實施例還原溫度900℃的鎢銅合金粉末經最終燒結溫度1250℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Figure 31] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten copper alloy powder with a reduction temperature of 900°C at a final sintering temperature of 1250°C and holding the temperature for 2 hours in an embodiment of the present invention.
[第三十二圖]係為本發明實施例還原溫度700℃的鎢銅合金粉末經最終燒結溫度1280℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Figure 32] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten copper alloy powder with a reduction temperature of 700°C at a final sintering temperature of 1280°C and a holding temperature for 2 hours in the embodiment of the present invention.
[第三十三圖]係為本發明實施例還原溫度750℃的鎢銅合金粉末經最終燒結溫度1280℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Figure 33] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten copper alloy powder with a reduction temperature of 750°C at a final sintering temperature of 1280°C and holding the temperature for 2 hours in an embodiment of the present invention.
[第三十四圖]係為本發明實施例還原溫度800℃的鎢銅合金粉末經最終燒結溫度1280℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Thirty-fourth Figure] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten-copper alloy powder with a reduction temperature of 800°C at a final sintering temperature of 1280°C and holding the temperature for 2 hours in an embodiment of the present invention.
[第三十五圖]係為本發明實施例還原溫度850℃的鎢銅合金粉末經最終燒結溫度1280℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Figure 35] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten copper alloy powder with a reduction temperature of 850°C at a final sintering temperature of 1280°C and holding the temperature for 2 hours in an embodiment of the present invention.
[第三十六圖]係為本發明實施例還原溫度900℃的鎢銅合金粉末經最終燒結溫度1280℃、持溫2小時燒結後所獲得的斷面微結構之金相圖。 [Figure 36] is a metallographic diagram of the cross-sectional microstructure obtained after sintering the tungsten copper alloy powder with a reduction temperature of 900°C at a final sintering temperature of 1280°C and holding the temperature for 2 hours in an embodiment of the present invention.
[第三十七圖]係為本發明實施例經由850℃還原、1280℃燒結及持溫2小時之鎢銅複合材料，具有連續式銅網包覆鎢晶粒微結構之金相圖。 [Figure 37] is a metallographic diagram of the tungsten copper composite material, which has been reduced at 850°C, sintered at 1280°C, and held at temperature for 2 hours, with a continuous copper mesh-coated tungsten grain microstructure according to an embodiment of the present invention.
請參閱第一圖及第二圖所示，本發明實施例係包含有下列步驟： Please refer to the first and second figures, the embodiment of the present invention includes the following steps:
A.製備偏鎢酸銨溶液及氧化銅粉末。首先按照目標成分比例計算所需的偏鎢酸銨(Ammonium metatungstate，AMT)和氧化銅(CuO)，本發明實施例之成分目標設定為80%鎢/20%銅。首先將220公克的偏鎢酸銨溶於200公克的水中，使其形成420克的該偏鎢酸銨水溶液。再製備50公克的該氧化銅粉末。 A. Preparation of ammonium metatungstate solution and copper oxide powder. First, the required ammonium metatungstate (AMT) and copper oxide (CuO) are calculated according to the target composition ratio. The composition target in the embodiment of the present invention is set to 80% tungsten/20% copper. First, 220 grams of ammonium metatungstate was dissolved in 200 grams of water to form 420 grams of the ammonium metatungstate aqueous solution. Another 50 grams of the copper oxide powder was prepared.
B.使偏鎢酸銨析鍍於氧化銅的表面，以形成一鎢鍍銅粉末。將50公克的該氧化銅粉末之顆粒1放入一攪拌桶2的一析鍍空間21內〔如第三圖及第四圖所示〕，該攪拌桶2係可藉由一馬達3帶動旋轉，並於該攪拌桶1的內壁周緣設有複數攪拌片22，以幫助該氧化銅粉末之攪拌，可以使位於底部的該氧化銅粉末得以被翻動，同時該攪拌桶2的底部可透過加熱線圈4予以局部加熱，利用該馬達3變速與透過偏心轉動，以及內部的該攪拌片可以將粉末充分攪拌均勻。然後將420公克的該偏鎢酸銨水溶液慢慢加入該攪拌桶2內部，該氧化銅粉末會溶入於該偏鎢酸銨水溶液(化學式為(NH4)6[H2W12O40]．nH2O)中，使得該氧化銅粉末之顆粒1與偏鎢酸銨混煉均勻，藉由該加熱線圈4之加熱作用，逐步加溫使水分蒸發，加熱溫度100℃至120℃之間，加熱時間為0.5小時至2小時之間，當乾燥後該鎢則會析鍍在該氧化銅的表面，以形成該鎢鍍銅粉末。
B. Precipitate ammonium metatungstate on the surface of copper oxide to form a copper-plated tungsten powder. Put 50 grams of the copper
C.調整還原參數，將該鎢鍍銅粉末還原成為一鎢銅合金粉末。將適量的該鎢鍍銅粉末〔10公克至50公克〕置入於一氧化鋁坩鍋的一還原空間內，並於該還原空間內加入氫氣進行加熱還原，該還原空間內的氫氣流量係為1公升/min。以3℃/min升溫到500℃，持溫1小時，再以3℃/min分別升溫至700℃、750℃、800℃、850℃、900℃等還原溫度，持溫1小時至12小時後，再自然冷卻到室溫後取出，即形成該鎢銅合金粉末。本發明實施例之還原程序，如第五圖所示，係以3℃/min到500℃，持溫1小時，再以3℃/min升溫至750℃，持溫1小時至12小時後，再自然冷卻到室溫後取出。 C. Adjust the reduction parameters to reduce the tungsten copper-plated powder into a tungsten-copper alloy powder. Put an appropriate amount of the tungsten copper-plated powder (10 g to 50 g) into a reduction space of an alumina crucible, and add hydrogen into the reduction space for heating and reduction. The hydrogen flow rate in the reduction space is 1 liter/min. Raise the temperature at 3°C/min to 500°C, hold the temperature for 1 hour, and then raise the temperature at 3°C/min to 700°C, 750°C, 800°C, 850°C, 900°C and other reduction temperatures, hold the temperature for 1 hour to 12 hours , And then take it out after natural cooling to room temperature to form the tungsten copper alloy powder. The reduction procedure of the embodiment of the present invention, as shown in the fifth figure, is from 3°C/min to 500°C, holding the temperature for 1 hour, and then raising the temperature to 750°C at 3°C/min. After holding the temperature for 1 hour to 12 hours, Then take it out after cooling to room temperature.
D.對於該鎢銅合金粉末進行球磨分散。將該鎢銅合金粉末置入於一塑膠桶(聚丙烯材質)的一研磨空間內，依照該鎢銅合金粉末是否團聚嚴重，如果團聚不嚴重則直接進行無磨球乾磨；如果團聚嚴重，則加入少量氧化鉛球進行乾磨，藉以能打散粉團，但是又不會破壞鎢鍍銅的粉末結構。 D. Ball milling and dispersing the tungsten copper alloy powder. Put the tungsten-copper alloy powder into a grinding space of a plastic bucket (polypropylene material). According to whether the tungsten-copper alloy powder is severely agglomerated, if the agglomeration is not severe, proceed directly to dry grinding without grinding balls; if the agglomeration is severe, A small amount of lead oxide ball is added for dry grinding, which can break up the powder mass, but will not damage the tungsten copper-plated powder structure.
E.對於該鎢銅合金粉末進行性質分析。該性質分析包含： E. Perform property analysis on the tungsten copper alloy powder. This property analysis includes:
E1.粒徑分析，透過雷射粒徑分析儀量測該鎢銅合金粉末的平均粒徑，藉以確認該鎢銅合金粉末全部的平均粒徑有90%≦6um，有50%≦2um，有10%≦0.8um。 E1. Particle size analysis: Measure the average particle size of the tungsten copper alloy powder through a laser particle size analyzer to confirm that the average particle size of the tungsten copper alloy powder is 90%≦6um, 50%≦2um, yes 10%≦0.8um.
E2.振實密度，透過粉體振實密度儀之測量，確認該振實密度需高於30%理論密度(理論密度是15.68g/cm3)。 E2. Tap density. Through the measurement of a powder tap density meter, confirm that the tap density must be higher than 30% of the theoretical density (theoretical density is 15.68g/cm 3 ).
E3.含氧(O2)量分析，透過能量散射光譜儀(EDS)量測該鎢銅合金粉末的含氧量需要<3000ppm(0.3wt%)，或是透過X-射線繞射(XRD)分析，只有鎢與銅的繞射峰。 E3. Oxygen (O 2 ) analysis, measuring the oxygen content of the tungsten copper alloy powder by energy scattering spectrometer (EDS) requires <3000ppm (0.3wt%), or by X-ray diffraction (XRD) analysis , Only the diffraction peaks of tungsten and copper.
E4.外觀觀察，透過掃描式電子顯微鏡(SEM)進行該鎢銅合金粉末的外觀觀察，需要在放大5000倍與10000倍的放大倍率範圍下可看到獨立的顆粒〔如第六圖及第七圖所示〕。 E4. Appearance observation. Observe the appearance of the tungsten-copper alloy powder through a scanning electron microscope (SEM). Separate particles need to be seen under the magnification range of 5000 times and 10000 times (as shown in Figure 6 and Figure 7). As shown in the picture].
F.對於該鎢銅合金粉末進行燒結程序，以形成一鎢銅複合材料。該燒結程序包含：模壓成型與氣氛燒結，燒結密度對鎢銅合金的導熱性質影很大，製備完成的鎢銅合金粉末需要適當的燒結程序方能得到最佳的緻密度，除了粉末本身的特性外，還有許多影響參數需要最佳化，其中影響鎢銅合金性質的重要變數包括：模壓壓力、燒結溫度、持溫時間及升溫速率等。經由本發明實施例還原後的該鎢銅合金粉末，透過前導實驗設計選擇以200MPa模壓成型，最終燒結溫度分別設定為1220℃、1250℃、1280℃。本發明實施例之燒結程序，如第八圖所示，模壓壓力設定為200MPa，以3℃/min升溫到500℃後，持溫1小時，再以2℃/min升溫至950℃後，持溫2小時，再以2℃/min升溫至1150℃後，持溫1小時，再以3℃/min升溫至1250℃後，持溫1小時至2小時，再自然冷卻到室溫後取出，即形成該鎢銅複合材料。 F. Perform a sintering process on the tungsten-copper alloy powder to form a tungsten-copper composite material. The sintering process includes: compression molding and atmosphere sintering. The sintering density has a great influence on the thermal conductivity of the tungsten copper alloy. The prepared tungsten copper alloy powder requires a proper sintering process to obtain the best density, except for the characteristics of the powder itself. In addition, there are many influencing parameters that need to be optimized. Among them, the important variables that affect the properties of tungsten copper alloys include: molding pressure, sintering temperature, temperature holding time, and heating rate. The tungsten-copper alloy powder reduced by the embodiment of the present invention was selected to be molded at 200 MPa through pilot experiment design, and the final sintering temperature was set to 1220° C., 1250° C., and 1280° C., respectively. For the sintering procedure of the embodiment of the present invention, as shown in the eighth figure, the molding pressure is set to 200MPa, the temperature is raised to 500°C at 3°C/min, and the temperature is held for 1 hour, and then the temperature is raised to 950°C at 2°C/min. Warm for 2 hours, then heat up to 1150°C at 2°C/min, hold the temperature for 1 hour, then heat up to 1250°C at 3°C/min, hold the temperature for 1 hour to 2 hours, then cool to room temperature and take it out. That is, the tungsten copper composite material is formed.
G.對於該鎢銅複合材料進行燒結性質分析。燒結性質分析包含： G. Analyze the sintering properties of the tungsten copper composite material. The analysis of sintering properties includes:
G1.密度量測：密度是衡量燒結體最終緻密程度的快速量測指標，根據ASTMB311、B328；MPIF42、57；JISZ2505、Z2506、GB/T5163等規範，通過浮力與密度計算公式的推導與變換形成等式，首先利用高精密固體分析天平分別計算出該鎢銅複合材料之待測樣品在空氣中的重量(W1)和在水中之重量(W2)，並計算出W1-W2值，水(D水)的密度為1g/cm3，通過V樣品=V排水建立等式，即可計算出該樣品的密度值(D)。 G1. Density measurement: Density is a quick measurement index to measure the final compactness of sintered body. It is formed according to ASTM B311, B328; MPIF42, 57; JISZ2505, Z2506, GB/T5163 and other specifications, through the derivation and transformation of buoyancy and density calculation formulas Equation, first use a high-precision solid analytical balance to calculate the weight of the sample to be tested in the air (W 1 ) and the weight in water (W 2 ) of the tungsten-copper composite material, and calculate the W 1 -W 2 value , The density of water (D water) is 1g/cm 3 , and the density value (D) of the sample can be calculated by establishing the equation of V sample=V drainage.
D=W1/(W1-W2)×D水。 D=W 1 /(W 1 -W 2 )×D water.
依據本發明實施例所製成之鎢銅複合材料之緻密度係能夠大於>98%或密度至少大於15g/cm3。 The density of the tungsten copper composite material made according to the embodiment of the present invention can be greater than >98% or the density can be at least greater than 15 g/cm 3 .
G2.導電率量測：以微歐姆計量測燒結試片之電阻。 G2. Conductivity measurement: measure the resistance of the sintered test piece by micro-ohm measurement.
R：材料的電阻，ρ：材料的電阻係數，A：試片截面積，L：試片長度。 R: electrical resistance of the material, ρ: electrical resistivity of the material, A: cross-sectional area of the test piece, L: length of the test piece.
導電率σ(electrical conductivity)為電阻係數的倒數，該鎢銅複合材料的導電率係能大於46%IACS(IACS：體積導電率百分值)。 The electrical conductivity σ (electrical conductivity) is the reciprocal of the electrical resistivity, and the electrical conductivity of the tungsten copper composite material can be greater than 46% IACS (IACS: Percent Volume Conductivity).
G3.微觀結構觀察：燒結參數的控制與製程所製備的鎢銅合金粉末是否均勻，將會影響最終燒結品的金相組織，因此需要透過掃描式電子顯微鏡(SEM)進行微結構觀察。 G3. Microstructure observation: The control of sintering parameters and the uniformity of the tungsten copper alloy powder prepared by the process will affect the metallographic structure of the final sintered product. Therefore, it is necessary to observe the microstructure through a scanning electron microscope (SEM).
G4.硬度量測：硬度是衡量燒結品機械性質的重要指標，使用微克氏硬度試驗機量測該鎢銅複合材料之硬度值，每一個鎢銅複合材料之試片測量3個不同位置，最後將所有硬度值再予以平均即可。其硬度值係為Hv175至325之間。 G4. Hardness measurement: Hardness is an important index to measure the mechanical properties of sintered products. The hardness value of the tungsten-copper composite material is measured using a micro-Kr's hardness tester. Each test piece of the tungsten-copper composite material is measured at 3 different positions, and finally All the hardness values can be averaged again. Its hardness value is between Hv175 and 325.
本發明上述實施例之製造方法，係經過實驗測試，經過處理完成後的鎢鍍銅粉末，分別升溫至700℃、750℃、800℃、850℃、900℃，再持溫12小時後進行還原，下列表一係為還原後該鎢鍍銅粉末的相關特性。 The manufacturing method of the above-mentioned embodiment of the present invention is experimentally tested. After the treatment, the tungsten copper-plated powder is heated to 700°C, 750°C, 800°C, 850°C, and 900°C respectively, and the temperature is maintained for 12 hours before reduction , The following table lists the relevant characteristics of the tungsten copper-plated powder after reduction.
由上述表一中的實驗結果，可以看出還原後的該鎢銅合金粉末，已經過處理後的團塊狀變成鬆散，且容易打散的粉末顆粒，振實密度大於29%理論密度(理論密度是15.68g/cm3)以上，已達設定標準。最終氧含量會隨著還原溫度而有很大的差異，如第十四圖所示，係為該鎢銅合金粉末的氧含量隨著還原溫度增加而減少的變化曲線。從第十四圖中可以明顯看出在700℃進行還原，氧含量高達10.09wt%，而隨著還原溫度增加，殘留氧含量也明顯持續下降，在900℃進行還原時，氧含量已剩0.17wt%，也就是說明了鎢、銅氧化物的還原，不但需要時間而且溫度也很重要。為了確認氧化物的種類，也進行了該鎢銅合金粉末的X-射線繞射分析，如第十五圖所示，係為該鎢銅合金粉末在不同溫度還原下的X-射線繞射分析比對結果。由圖中結果顯示，在700℃進行還原時，幾乎已經觀察不到氧化銅的峰值，也就是說明了氧化銅應該已經大部分被還原完成為銅，但鎢的氧化物二氧化鎢(WO2)卻依舊存在，一直到850℃才被還原完成為鎢，這個現象 將對後續燒結結果產生重大影響。而在850℃時也嘗試降低持溫時間，即時將持溫時間縮短至3小時也依舊可將二氧化鎢還原完成，如第十六圖所示。 From the experimental results in Table 1 above, it can be seen that the reduced tungsten-copper alloy powder has become loose and easily broken powder particles in the form of agglomerates after reduction. The tap density is greater than 29% of the theoretical density (theoretical density). The density is above 15.68g/cm 3 ), which has reached the set standard. The final oxygen content will vary greatly with the reduction temperature. As shown in Figure 14, it is a curve where the oxygen content of the tungsten copper alloy powder decreases as the reduction temperature increases. From the fourteenth figure, it can be clearly seen that the oxygen content is as high as 10.09wt% when the reduction is performed at 700℃, and as the reduction temperature increases, the residual oxygen content also obviously continues to decrease. When the reduction is performed at 900℃, the oxygen content is already 0.17. wt%, which means that the reduction of tungsten and copper oxides not only requires time but also temperature. In order to confirm the type of oxide, the X-ray diffraction analysis of the tungsten-copper alloy powder was also performed. As shown in Figure 15, it is the X-ray diffraction analysis of the tungsten-copper alloy powder at different temperatures Compare the results. The results in the figure show that when the reduction is carried out at 700°C, the peak of copper oxide is almost no longer observed, which means that most of the copper oxide should have been reduced to copper, but tungsten oxide tungsten dioxide (WO 2 ) Still exists, and it is not reduced to tungsten until 850°C. This phenomenon will have a significant impact on the subsequent sintering results. At 850℃, try to reduce the holding time. Even if the holding time is shortened to 3 hours, the tungsten dioxide can still be reduced, as shown in Figure 16.
如第十七圖及第十八圖所示，係為該鎢銅合金粉末透過掃描式電子顯微鏡(SEM)，在放大5000倍與10000倍的放大倍率範圍下所觀察到的外觀，由圖中可看出粉末呈現的是一種多角型態。 As shown in Figures 17 and 18, this is the appearance of the tungsten-copper alloy powder observed through a scanning electron microscope (SEM) under a magnification range of 5000 times and 10000 times. It can be seen that the powder presents a polygonal shape.
為了暸解該鎢銅合金粉末的燒結性質，同時比較不同還原條件的性質差異，將各還原條件下所獲得的粉末依照實驗規劃進行燒結實驗，如第十九圖所示，係為不同還原溫度所獲得的該鎢銅合金粉末，其密度隨著燒結溫度增加的變化曲線，從圖中結果可以看出，密度隨著燒結溫度增加而增加是共同的成長趨勢，其中以800℃、850℃的結果最好，尤其是850℃進行還原的該鎢銅合金粉末在1280℃燒結下，可得到最高密度15.62g/cm3，其緻密度已達100%。如第二十圖所示，係為不同還原溫度所獲得的該鎢銅合金粉末，其硬度隨燒結溫度增加的變化曲線。從其結果可以看出和密度變化趨勢一致，隨著燒結溫度增加，越來越緻密，因此硬度也隨之增加，其中以850℃還原、1280℃燒結並持溫2小時具有最佳的硬度值Hv323.5。另外，鎢銅複合材料之應用最重要的性質之一是導電能力，如第二十一圖所示，係為不同還原溫度所獲得的該鎢銅合金粉末，其導電率(%IACS)隨燒結溫度增加的變化曲線。一般而言，鎢銅複合材料能夠燒得越均勻緻密，其導電能力也就越好，由圖中可明顯看出此趨勢；850℃還原、1280℃燒結並持溫2小時具有最佳的導電能力，高達47.3%IACS。 In order to understand the sintering properties of the tungsten-copper alloy powder and compare the differences in properties under different reduction conditions, the powders obtained under each reduction condition were subjected to sintering experiments according to the experimental plan. The density curve of the obtained tungsten copper alloy powder increases with the increase of sintering temperature. From the results in the figure, it can be seen that the increase in density with the increase of sintering temperature is a common growth trend. Among them, the results of 800 ℃ and 850 ℃ Preferably, the tungsten-copper alloy powder reduced at 850°C can be sintered at 1280°C to obtain the highest density of 15.62g/cm 3 , and its density has reached 100%. As shown in Figure 20, the hardness of the tungsten-copper alloy powder obtained at different reduction temperatures varies with the increase in sintering temperature. It can be seen from the results that it is consistent with the density change trend. As the sintering temperature increases, it becomes more and more dense, so the hardness also increases. Among them, reduction at 850°C, sintering at 1280°C and holding the temperature for 2 hours have the best hardness value. Hv323.5. In addition, one of the most important properties for the application of tungsten-copper composite materials is electrical conductivity. As shown in Figure 21, the tungsten-copper alloy powders obtained at different reduction temperatures. The electrical conductivity (%IACS) varies with sintering. The change curve of temperature increase. Generally speaking, the more uniform and dense the tungsten-copper composite material can be burned, the better its conductivity. This trend can be clearly seen from the figure; reduction at 850°C, sintering at 1280°C and holding the temperature for 2 hours have the best conductivity Ability, up to 47.3% IACS.
如第二十二圖至第二十六圖所示，係為不同還原溫度(700℃、750℃、800℃、850℃、900℃)的該鎢銅合金粉末經最終燒結溫度1220℃、持溫2小時燒結後所獲得的斷面微結構，從該等圖式中可以明顯看出1220℃的燒結溫度不夠高，整體緻密度偏低，因此連續式網狀銅結構並不明顯。如第二十七圖至第三十一圖所示，係為不同還原溫度(700℃、750℃、800℃、850℃、900℃)的該鎢 銅合金粉末經最終燒結溫度1250℃、持溫2小時燒結後所獲得的斷面微結構。如第三十二圖至第三十六圖所示，係為不同還原溫度(700℃、750℃、800℃、850℃、900℃)的該鎢銅合金粉末經最終燒結溫度1280℃、持溫2小時燒結後所獲得的斷面微結構。隨著燒結溫度增加，燒結微結構看起來越來越緻密，特別是第三十五圖之850℃還原溫度的斷面微結構已經出現很均勻且明顯的連續式銅網包覆鎢晶粒結構，這是最希望得到的理想微結構。 As shown in Figure 22 to Figure 26, the tungsten copper alloy powders with different reduction temperatures (700°C, 750°C, 800°C, 850°C, 900°C) have been sintered at a final sintering temperature of 1220°C, The cross-sectional microstructure obtained after sintering at a temperature of 2 hours, it can be clearly seen from the diagram that the sintering temperature of 1220°C is not high enough, and the overall density is low, so the continuous network copper structure is not obvious. As shown in Figure 27 to Figure 31, the tungsten has different reduction temperatures (700°C, 750°C, 800°C, 850°C, 900°C) The cross-sectional microstructure of copper alloy powder is obtained after sintering at a final sintering temperature of 1250°C and holding the temperature for 2 hours. As shown in Figure 32 to Figure 36, the tungsten copper alloy powders with different reduction temperatures (700°C, 750°C, 800°C, 850°C, 900°C) have been sintered at a final sintering temperature of 1280°C. The microstructure of the cross-section obtained after sintering at a temperature of 2 hours. As the sintering temperature increases, the sintered microstructure looks denser and denser, especially the cross-sectional microstructure at the reduction temperature of 850℃ in Figure 35 has a very uniform and obvious continuous copper mesh-coated tungsten grain structure. , This is the most desired ideal microstructure.
本發明所製成之鎢銅複合材料，經由850℃的氫氣還原後，再以1280℃燒結後，並持溫2小時可以得到最佳之性質，如第三十七圖所示，可以清楚看到銅在高溫熔解成為液相後，因為毛細作用快速形成連續式的網狀結構，並且包覆著平均粒徑小於1μm的鎢晶粒，最佳之性質組合包括：密度15.62g/cm3(緻密度達100%)、硬度Hv323.5、47.3%IACS。 The tungsten-copper composite material made by the present invention is reduced by hydrogen at 850°C, then sintered at 1280°C and held at the temperature for 2 hours to obtain the best properties. As shown in Figure 37, it can be clearly seen After the copper melts into a liquid phase at high temperature, it quickly forms a continuous network structure due to capillary action, and it is covered with tungsten grains with an average particle size of less than 1μm. The best combination of properties includes: density 15.62g/cm 3 ( Density reaches 100%), hardness Hv323.5, 47.3%IACS.
綜合上述實施例之說明，當可充分瞭解本發明之操作、使用及本發明產生之功效，惟以上所述實施例僅係為本發明之較佳實施例，當不能以此限定本發明實施之範圍，即依本發明申請專利範圍及發明說明內容所作簡單的等效變化與修飾，皆屬本發明涵蓋之範圍內。 Based on the description of the above-mentioned embodiments, when one can fully understand the operation and use of the present invention and the effects of the present invention, the above-mentioned embodiments are only the preferred embodiments of the present invention, and the implementation of the present invention cannot be limited by this. The scope, that is, simple equivalent changes and modifications made according to the scope of the patent application of the present invention and the content of the description of the invention, are all within the scope of the present invention.
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| CN101214553A (en) * | 2008-01-02 | 2008-07-09 | 中南大学 | Method for preparing ultra-fine/nano tungsten molybdenum copper composite powder |
| CN106756376A (en) * | 2016-11-24 | 2017-05-31 | 深圳市圆梦精密技术研究院 | tungsten-copper alloy and its processing method and application |
| CN109014232A (en) * | 2018-08-29 | 2018-12-18 | 北京科技大学 | A method of preparing ultra-fine tungsten-copper composite powder |
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| CN101214553A (en) * | 2008-01-02 | 2008-07-09 | 中南大学 | Method for preparing ultra-fine/nano tungsten molybdenum copper composite powder |
| CN106756376A (en) * | 2016-11-24 | 2017-05-31 | 深圳市圆梦精密技术研究院 | tungsten-copper alloy and its processing method and application |
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