CN108165898A - A kind of preparation method of copper carbon nano-tube composite powder end enhancing magnesium cu-base amorphous alloy composite material - Google Patents
A kind of preparation method of copper carbon nano-tube composite powder end enhancing magnesium cu-base amorphous alloy composite material Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 155
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 150
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 146
- 239000002131 composite material Substances 0.000 title claims abstract description 146
- AHADSRNLHOHMQK-UHFFFAOYSA-N methylidenecopper Chemical compound [Cu].[C] AHADSRNLHOHMQK-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052749 magnesium Inorganic materials 0.000 title claims description 9
- 229910000808 amorphous metal alloy Inorganic materials 0.000 title abstract description 8
- 239000011777 magnesium Substances 0.000 title description 44
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title 1
- 230000002708 enhancing effect Effects 0.000 title 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 106
- 239000010949 copper Substances 0.000 claims abstract description 105
- OWXLRKWPEIAGAT-UHFFFAOYSA-N [Mg].[Cu] Chemical compound [Mg].[Cu] OWXLRKWPEIAGAT-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052802 copper Inorganic materials 0.000 claims abstract description 32
- 239000002243 precursor Substances 0.000 claims abstract description 27
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims abstract description 23
- 239000000126 substance Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 239000006185 dispersion Substances 0.000 claims abstract description 15
- 238000005118 spray pyrolysis Methods 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 14
- 238000004512 die casting Methods 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 230000006698 induction Effects 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 27
- 239000007789 gas Substances 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- 238000000227 grinding Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 229910052727 yttrium Inorganic materials 0.000 claims description 8
- 239000002048 multi walled nanotube Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000007496 glass forming Methods 0.000 abstract description 8
- 229910001092 metal group alloy Inorganic materials 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000000889 atomisation Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000011056 performance test Methods 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 6
- 239000002071 nanotube Substances 0.000 description 5
- 239000013526 supercooled liquid Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- ATTFYOXEMHAYAX-UHFFFAOYSA-N magnesium nickel Chemical compound [Mg].[Ni] ATTFYOXEMHAYAX-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000009689 gas atomisation Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/005—Amorphous alloys with Mg as the major constituent
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- C22C1/1005—Pretreatment of the non-metallic additives
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- C22C1/00—Making non-ferrous alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
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- C22C1/00—Making non-ferrous alloys
- C22C1/11—Making amorphous alloys
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Abstract
本发明涉及一种铜碳纳米管复合粉末增强镁铜基非晶复合材料的制备方法,属于金属合金复合材料技术领域。本发明将乙酸铜溶解于去离子水得到乙酸铜水溶液,加入碳纳米管分散液并混合均匀得到前驱液;前驱液经喷雾热解法得到Cu单质/碳纳米管复合粉末;将Mg粉、Cu粉、Y粉、Cu单质/碳纳米管复合粉末进行低能球磨混合,得到铜碳纳米管复合粉末‑镁铜基非晶复合粉,再压制成块体,将块体置于温度为600~1000℃的感应压铸炉中熔炼15~25s,再在压力为1~10Mpa的条件下压铸成型,即得铜碳纳米管复合粉末增强的镁铜基非晶复合材料。本发明方法制备的镁铜基非晶复合材料,相比较于纯Mg基非晶合金具有较高的玻璃形成能力。The invention relates to a preparation method of a copper-carbon nanotube composite powder reinforced magnesium-copper-based amorphous composite material, which belongs to the technical field of metal alloy composite materials. In the present invention, copper acetate is dissolved in deionized water to obtain an aqueous solution of copper acetate, and a carbon nanotube dispersion is added and mixed uniformly to obtain a precursor solution; the precursor solution is subjected to a spray pyrolysis method to obtain Cu simple substance/carbon nanotube composite powder; Mg powder, Cu Powder, Y powder, Cu simple substance/carbon nanotube composite powder are mixed by low-energy ball milling to obtain copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder, which is then pressed into a block, and the block is placed at a temperature of 600~1000 ℃ induction die-casting furnace for 15-25s, and then die-casting under the condition of 1-10Mpa to obtain copper-carbon nanotube composite powder-reinforced magnesium-copper-based amorphous composite material. Compared with the pure Mg-based amorphous alloy, the magnesium-copper-based amorphous composite material prepared by the method of the invention has higher glass-forming ability.
Description
技术领域technical field
本发明涉及一种铜碳纳米管复合粉末增强镁铜基非晶复合材料的制备方法,属于金属合金复合材料技术领域。The invention relates to a preparation method of a copper-carbon nanotube composite powder reinforced magnesium-copper-based amorphous composite material, which belongs to the technical field of metal alloy composite materials.
背景技术Background technique
自1991年碳纳米管 (CNTs)被日本的电子显微镜专家饭岛发现以来,CNTs就以其优异的性能迅速成为科学研究领域的热点。在973K以下温度,基本不发生变化,高的弹性模量,可达1.8 TPa;强度是钢强度的100倍,同时具有很好的变形性能,其弹性应变可达5%,约为钢的60倍,而其密度只有1.35g/cm3,为钢的六分之一,而且碳纳米管有优于其他纤维的韧性。很高的长径比,一般为100~1000,最高可达l000-10000。正因为以上的特性,使得CNTs被寄予厚望作为复合材料的增强相,而且CNTs还具有半径小、表面积大、不易与金属基体反应形成脆性界面、耐高温和耐腐蚀性等优点。因此CNTs有望成为最具前景的复合材料增强相。Since carbon nanotubes (CNTs) were discovered by Japanese electron microscope expert Iijima in 1991, CNTs have rapidly become a hot spot in the field of scientific research due to their excellent performance. At a temperature below 973K, there is basically no change, and the high elastic modulus can reach 1.8 TPa; the strength is 100 times that of steel, and it has good deformation properties. Its elastic strain can reach 5%, which is about 60 times that of steel. times, and its density is only 1.35g/cm3, which is one-sixth of steel, and carbon nanotubes have better toughness than other fibers. Very high aspect ratio, generally 100-1000, up to 1000-10000. Because of the above characteristics, CNTs are expected to be used as the reinforcing phase of composite materials, and CNTs also have the advantages of small radius, large surface area, not easy to react with the metal matrix to form a brittle interface, high temperature resistance and corrosion resistance. Therefore, CNTs are expected to become the most promising reinforcement phase for composite materials.
中国专利CN102650027A公开了一种制备碳纳米管增强的铁基非晶合金热喷涂层及方法,其方法是采用气体雾化法制备Fe基非晶粉末,再与碳纳米管混合,经机械球磨进行粒子重构,得到铁基非晶—碳纳米管复合粉,然后对喷涂基底表明预处理,进行热喷涂加工。该涂层,碳纳米管与铁基非晶结合良好,但是气体雾化法制备Fe基非晶粉末,合金粉末的粒径随着雾化气压的增加、导流管直径的减小和过热度的增加而逐渐降低.随着粉末粒径的减少,合金粉末的组织结构发生了转变,最终得到特定粒径粉末的完全非晶态。雾化过程中适当的细粉率控制较难,合适的粒径调控较复杂,组织结构转变不易控制。Chinese patent CN102650027A discloses a thermal spray coating and method for preparing carbon nanotube-reinforced iron-based amorphous alloys. The method is to prepare Fe-based amorphous powder by gas atomization method, then mix it with carbon nanotubes, and carry out mechanical ball milling. Particles are reconstructed to obtain iron-based amorphous-carbon nanotube composite powder, and then the sprayed substrate is pretreated for thermal spraying. In this coating, carbon nanotubes are well combined with Fe-based amorphous powder, but Fe-based amorphous powder is prepared by gas atomization method. The increase gradually decreases. With the decrease of the powder particle size, the microstructure of the alloy powder changes, and finally a completely amorphous state of a specific particle size powder is obtained. It is difficult to control the appropriate fine powder rate in the atomization process, the control of the appropriate particle size is more complicated, and the transformation of the organizational structure is not easy to control.
中国专利CN104630662A公开了一种碳纳米管增强镁镍基非晶复合材料及其制备方法,其方法是用电弧炉制备镁镍基非晶,再与碳纳米管混合,经机械球磨进行粒子重构,得到镁镍基非晶—碳纳米管复合粉,再经压铸得到碳纳米管增强的镁镍基块体非晶复合材料。该复合材料,非晶形成能力得到提高,强韧性也得到改善,但是该方法需要先制备中间合金,再添加金属Mg制备母合金,敲碎后球磨,工艺复杂,工程繁琐,耗时耗力。Chinese patent CN104630662A discloses a carbon nanotube-reinforced magnesium-nickel-based amorphous composite material and its preparation method. The method is to prepare magnesium-nickel-based amorphous with an electric arc furnace, then mix it with carbon nanotubes, and perform particle reconstruction by mechanical ball milling , to obtain magnesium-nickel-based amorphous-carbon nanotube composite powder, and then die-cast to obtain magnesium-nickel-based bulk amorphous composite material reinforced by carbon nanotubes. The composite material has improved amorphous forming ability and improved strength and toughness. However, this method needs to prepare a master alloy first, then add metal Mg to prepare a master alloy, crush it and then ball mill it. The process is complex, tedious, time-consuming and labor-intensive.
发明内容Contents of the invention
本发明针对现有技术的不足,提供一种铜碳纳米管复合粉末增强镁铜基非晶复合材料的制备方法,通过向镁铜基非晶合金中添加单质Cu和碳纳米管复合粉末,来提高镁铜基非晶合金的玻璃形成能力,从而获得强度和韧性较高的非晶复合材料。Aiming at the deficiencies in the prior art, the present invention provides a method for preparing a copper-carbon nanotube composite powder reinforced magnesium-copper-based amorphous composite material, by adding elemental Cu and carbon nanotube composite powder to the magnesium-copper-based amorphous alloy. Improve the glass-forming ability of magnesium-copper-based amorphous alloys to obtain amorphous composites with higher strength and toughness.
一种铜碳纳米管复合粉末增强镁铜基非晶复合材料的制备方法,具体步骤为:A method for preparing a copper-carbon nanotube composite powder reinforced magnesium-copper-based amorphous composite material, the specific steps are:
(1)在搅拌条件下,将乙酸铜溶解于去离子水得到乙酸铜水溶液,然后加入碳纳米管分散液并混合均匀得到前驱液;在温度为400~500℃、还原气体氛围条件下,前驱液经喷雾热解法得到Cu单质/碳纳米管复合粉末;(1) Under stirring conditions, dissolve copper acetate in deionized water to obtain copper acetate aqueous solution, then add carbon nanotube dispersion liquid and mix uniformly to obtain precursor liquid; Cu simple substance/carbon nanotube composite powder was obtained by liquid spray pyrolysis;
(2)分别将金属Mg、Cu、Y打磨、超声清洗、真空干燥、研磨得到Mg粉、Cu粉、Y粉,将Mg粉、Cu粉、Y粉、步骤(1)所得Cu单质/碳纳米管复合粉末进行低能球磨混合,得到铜碳纳米管复合粉末-镁铜基非晶复合粉;(2) Grinding, ultrasonic cleaning, vacuum drying, and grinding metal Mg, Cu, and Y respectively to obtain Mg powder, Cu powder, and Y powder, and Mg powder, Cu powder, Y powder, Cu elemental/carbon nano Tube composite powder is mixed by low-energy ball milling to obtain copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder;
(3)在压力为0.5~1Mpa的条件下,将步骤(2)所得铜碳纳米管复合粉末-镁铜基非晶复合粉压制成块体,将块体置于温度为600~1000℃的感应压铸炉中熔炼15~25s,再在压力为1~10 Mpa的条件下压铸成型,即得铜碳纳米管复合粉末增强的镁铜基非晶复合材料;(3) Under the condition of a pressure of 0.5-1Mpa, press the copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder obtained in step (2) into a block, and place the block at a temperature of 600-1000°C Melting in an induction die-casting furnace for 15-25 seconds, and then die-casting under a pressure of 1-10 Mpa to obtain a magnesium-copper-based amorphous composite material reinforced with copper-carbon nanotube composite powder;
所述步骤(1)中乙酸铜水溶液的浓度为4.938 g/L,碳纳米管分散液中碳纳米管的质量百分数浓度为10 %,前驱液中碳纳米管的质量百分数浓度为0.013 ~0.068%。The concentration of copper acetate aqueous solution in the step (1) is 4.938 g/L, the mass percent concentration of carbon nanotubes in the carbon nanotube dispersion is 10%, and the mass percent concentration of carbon nanotubes in the precursor solution is 0.013 ~ 0.068% .
所述步骤(1)还原气体为氢气、一氧化碳、分解氨气、氢气-惰性气体、一氧化碳-惰性气体或分解氨气-惰性气体中的一种或几种;In the step (1), the reducing gas is one or more of hydrogen, carbon monoxide, decomposed ammonia, hydrogen-inert gas, carbon monoxide-inert gas or decomposed ammonia-inert gas;
所述步骤(1)中碳纳米管为多壁碳纳米管,纯度≥95%,外径20~60 nm,长度为0.5~15μm;The carbon nanotubes in the step (1) are multi-walled carbon nanotubes with a purity ≥ 95%, an outer diameter of 20-60 nm, and a length of 0.5-15 μm;
所述步骤(2)中Mg、Cu、Y原材料纯度>99.9(wt.%);The purity of Mg, Cu and Y raw materials in the step (2) is >99.9 (wt.%);
铜碳纳米管复合粉末增强镁铜基非晶复合材料为(CNTs)x (Mg65Cu25Y10)100-x,其中x为碳纳米管的体积百分比,x=1~5。Copper-carbon nanotube composite powder reinforced magnesium-copper-based amorphous composite material is (CNTs) x (Mg 65 Cu 25 Y 10 ) 100-x , where x is the volume percentage of carbon nanotubes, and x=1~5.
所述喷雾热解法为将炉腔抽真空,再通入还原气体至炉腔内不含氧气,开始加热直至温度达到反应温度且为恒温,将前驱液通过雾化器进行雾化,再将雾化后的微米级液滴在还原气氛的带动下进入加热炉腔,进行干燥、分解反应、还原反应,开启粉末收集系统收集反应产物即Cu单质/碳纳米管复合粉末。The spray pyrolysis method is to evacuate the furnace cavity, and then introduce a reducing gas until the furnace cavity does not contain oxygen, start heating until the temperature reaches the reaction temperature and is constant temperature, atomize the precursor solution through the atomizer, and then The atomized micron-sized droplets are driven by the reducing atmosphere into the heating chamber for drying, decomposition, and reduction reactions, and the powder collection system is opened to collect the reaction product, that is, the Cu element/carbon nanotube composite powder.
本发明的有益效果:Beneficial effects of the present invention:
(1)本发明方法采用喷雾热解法合成Cu单质/碳纳米管的复合粉末可改善碳纳米管与铜的界面结合性,可避免直接球磨过程中碳纳米管与铜不润湿的现象,提高碳纳米管与基体结合界面的强度;由于粉末颗粒在高温腔体里面停留的时间非常短,可有效避免发生二次团聚,解决碳纳米管在球磨过程中分散性差的问题;(1) The method of the present invention adopts the spray pyrolysis method to synthesize Cu simple substance/carbon nanotube composite powder, which can improve the interfacial bonding between carbon nanotubes and copper, and can avoid the non-wetting phenomenon of carbon nanotubes and copper in the direct ball milling process, Improve the strength of the bonding interface between carbon nanotubes and the matrix; because the powder particles stay in the high-temperature cavity for a very short time, it can effectively avoid secondary agglomeration and solve the problem of poor dispersion of carbon nanotubes during ball milling;
(2)本发明方法制备的铜碳纳米管复合粉末增强镁铜基非晶复合材料较纯Mg基非晶合金具有较高的玻璃形成能力。(2) The copper-carbon nanotube composite powder reinforced magnesium-copper-based amorphous composite material prepared by the method of the present invention has higher glass-forming ability than the pure Mg-based amorphous alloy.
附图说明Description of drawings
图1为实施例2制备的Cu单质/碳纳米管复合粉末的SEM图;Fig. 1 is the SEM picture of the Cu simple substance/carbon nanotube composite powder prepared in embodiment 2;
图2为实施例2制备的铜碳纳米管复合粉末增强的镁铜基非晶复合材料在60000倍下的组织形貌图;Fig. 2 is the microstructure figure of the magnesium-copper-based amorphous composite material reinforced by the copper-carbon nanotube composite powder prepared in Example 2 at 60,000 times;
图3为实施例2制备的铜碳纳米管复合粉末增强的镁铜基非晶复合材料在240000倍下的组织形貌图。Fig. 3 is a microstructure diagram of the copper-carbon nanotube composite powder reinforced magnesium-copper-based amorphous composite material prepared in Example 2 at 240,000 times.
具体实施方式Detailed ways
下面结合具体实施方式对本发明作进一步详细说明,但本发明的保护范围并不限于所述内容。The present invention will be described in further detail below in conjunction with specific embodiments, but the protection scope of the present invention is not limited to the content described.
实施例1:一种铜碳纳米管复合粉末增强镁铜基非晶复合材料的制备方法,具体步骤为:Embodiment 1: A kind of preparation method of copper-carbon nanotube composite powder reinforced magnesium-copper-based amorphous composite material, the specific steps are:
(1)在搅拌条件下,将乙酸铜溶解于去离子水得到乙酸铜水溶液,然后加入碳纳米管分散液并混合均匀得到前驱液;在温度为400℃、还原气体(氢气)氛围条件下,前驱液经喷雾热解法得到Cu单质/碳纳米管复合粉末;其中乙酸铜水溶液的浓度为4.938g/L,碳纳米管分散液中碳纳米管的质量百分数浓度为10%,前驱液中碳纳米管的质量百分数浓度为0.013%;碳纳米管为多壁碳纳米管,纯度为95%,外径20~60 nm,长度为0.5~15μm;还原气体(氢气)的流速为100 mL/min;本实施例制备的Cu单质/碳纳米管复合粉末的SEM图如图1所示,从图1中可知,碳纳米管表面均匀包覆一层单质铜,并且碳纳米管与铜之间界面结合良好,而且没有发现碳纳米管有明显的团聚产生;(1) Under stirring conditions, dissolve copper acetate in deionized water to obtain a copper acetate aqueous solution, then add carbon nanotube dispersion liquid and mix uniformly to obtain a precursor liquid; at a temperature of 400°C and a reducing gas (hydrogen) atmosphere, The precursor liquid was obtained Cu simple substance/carbon nanotube composite powder by spray pyrolysis; wherein the concentration of copper acetate aqueous solution was 4.938g/L, the mass percentage concentration of carbon nanotubes in the carbon nanotube dispersion liquid was 10%, and the carbon nanotubes in the precursor liquid The mass percent concentration of nanotubes is 0.013%; carbon nanotubes are multi-walled carbon nanotubes with a purity of 95%, an outer diameter of 20-60 nm, and a length of 0.5-15 μm; the flow rate of reducing gas (hydrogen) is 100 mL/min The SEM figure of the Cu simple substance/carbon nanotube composite powder prepared by the present embodiment is as shown in Figure 1, as can be seen from Figure 1, the carbon nanotube surface is uniformly coated with one layer of simple substance copper, and the interface between the carbon nanotube and copper The combination is good, and no obvious agglomeration of carbon nanotubes is found;
(2)分别将金属Mg、Cu、Y打磨、超声清洗、真空干燥、研磨得到Mg粉、Cu粉、Y粉,将Mg粉、Cu粉、Y粉、步骤(1)所得Cu单质/碳纳米管复合粉末进行低能球磨混合得到铜碳纳米管复合粉末-镁铜基非晶复合粉;其中Mg粉、Cu粉、Y粉摩尔比为65:20:10,Cu粉与Cu单质/碳纳米管复合粉末中Cu单质的摩尔比为20:5;以质量百分数计,铜碳纳米管复合粉末-镁铜基非晶复合粉中碳纳米管占1%;(2) Grinding, ultrasonic cleaning, vacuum drying, and grinding metal Mg, Cu, and Y respectively to obtain Mg powder, Cu powder, and Y powder, and Mg powder, Cu powder, Y powder, Cu elemental/carbon nano The tube composite powder is mixed by low-energy ball milling to obtain copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder; the molar ratio of Mg powder, Cu powder, and Y powder is 65:20:10, and Cu powder and Cu simple substance/carbon nanotube The molar ratio of Cu in the composite powder is 20:5; in terms of mass percentage, the carbon nanotubes in the copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder account for 1%;
(3)在压力为0.5Mpa的条件下,将步骤(2)所得铜碳纳米管复合粉末-镁铜基非晶复合粉压制成块体,将块体置于温度为600℃的感应压铸炉中熔炼25s,再在压力为1Mpa的条件下压铸成型,可获得铜碳纳米管复合粉末增强的Mg65Cu25Y10镁铜基非晶复合材料,即成分表示为(CNTs)1 (Mg65Cu25Y10)99,其中x为碳纳米管的体积百分比;(3) Under the condition of a pressure of 0.5Mpa, the copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder obtained in step (2) is pressed into a block, and the block is placed in an induction die-casting furnace with a temperature of 600°C Melting in medium temperature for 25s, and then die-casting under the condition of 1Mpa, the Mg 65 Cu 25 Y 10 magnesium copper-based amorphous composite material reinforced by copper-carbon nanotube composite powder can be obtained, that is, the composition is expressed as (CNTs) 1 (Mg 65 Cu 25 Y 10 ) 99 , where x is the volume percentage of carbon nanotubes;
本实施例中喷雾热解法为将炉腔抽真空,再通入还原气体(氢气)至炉腔内不含氧气,开始加热直至温度达到反应温度且为恒温,将前驱液通过雾化器进行雾化,再将雾化后的微米级液滴在还原气氛的带动下进入加热炉腔,进行干燥、分解反应、还原反应,开启粉末收集系统收集反应产物即Cu单质/碳纳米管复合粉末;In this embodiment, the spray pyrolysis method is to evacuate the furnace chamber, and then introduce reducing gas (hydrogen) until the furnace chamber does not contain oxygen, start heating until the temperature reaches the reaction temperature and is constant temperature, and the precursor solution is carried out through the atomizer. Atomization, and then the atomized micron-sized droplets are driven by the reducing atmosphere into the heating furnace chamber for drying, decomposition reaction, and reduction reaction, and the powder collection system is opened to collect the reaction product, namely Cu elemental substance/carbon nanotube composite powder;
本实施例的热性能测试结果如表1所示,从表1中可知,在相同的加热速率下,相比较于纯Mg基非晶合金,复合材料具有49.89K的过冷液相区间,即较高的玻璃形成能力。The thermal performance test results of this embodiment are shown in Table 1. It can be seen from Table 1 that at the same heating rate, compared with the pure Mg-based amorphous alloy, the composite material has a supercooled liquid phase interval of 49.89K, that is High glass forming ability.
实施例2:一种铜碳纳米管复合粉末增强镁铜基非晶复合材料的制备方法,具体步骤为:Embodiment 2: A kind of preparation method of copper-carbon nanotube composite powder reinforced magnesium-copper-based amorphous composite material, the specific steps are:
(1)在搅拌条件下,将乙酸铜溶解于去离子水得到乙酸铜水溶液,然后加入碳纳米管分散液并混合均匀得到前驱液;在温度为420 ℃、还原气体(氢气)氛围条件下,前驱液经喷雾热解法得到Cu单质/碳纳米管复合粉末;其中乙酸铜水溶液的浓度为4.938g/L,碳纳米管分散液中碳纳米管的质量百分数浓度为10%,前驱液中碳纳米管的质量百分数浓度为0.027%;碳纳米管为多壁碳纳米管,纯度为95%,外径20~60 nm,长度为0.5~15μm;还原气体(氢气)的流速为100 mL/min;(1) Under stirring conditions, dissolve copper acetate in deionized water to obtain a copper acetate aqueous solution, then add carbon nanotube dispersion liquid and mix uniformly to obtain a precursor liquid; at a temperature of 420 °C and a reducing gas (hydrogen) atmosphere, The precursor liquid was obtained Cu simple substance/carbon nanotube composite powder by spray pyrolysis; wherein the concentration of copper acetate aqueous solution was 4.938g/L, the mass percentage concentration of carbon nanotubes in the carbon nanotube dispersion liquid was 10%, and the carbon nanotubes in the precursor liquid The mass percent concentration of nanotubes is 0.027%; the carbon nanotubes are multi-walled carbon nanotubes with a purity of 95%, an outer diameter of 20-60 nm, and a length of 0.5-15 μm; the flow rate of reducing gas (hydrogen) is 100 mL/min ;
(2)分别将金属Mg、Cu、Y打磨、超声清洗、真空干燥、研磨得到Mg粉、Cu粉、Y粉,将Mg粉、Cu粉、Y粉、步骤(1)所得Cu单质/碳纳米管复合粉末进行低能球磨混合得到铜碳纳米管复合粉末-镁铜基非晶复合粉;其中Mg粉、Cu粉、Y粉摩尔比为65:20:10,Cu粉与Cu单质/碳纳米管复合粉末中Cu单质的摩尔比为20:5;以质量百分数计,铜碳纳米管复合粉末-镁铜基非晶复合粉中碳纳米管占2%;(2) Grinding, ultrasonic cleaning, vacuum drying, and grinding metal Mg, Cu, and Y respectively to obtain Mg powder, Cu powder, and Y powder, and Mg powder, Cu powder, Y powder, Cu elemental/carbon nano The tube composite powder is mixed by low-energy ball milling to obtain copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder; the molar ratio of Mg powder, Cu powder, and Y powder is 65:20:10, and Cu powder and Cu simple substance/carbon nanotube The molar ratio of Cu in the composite powder is 20:5; in terms of mass percentage, carbon nanotubes account for 2% in the copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder;
(3)在压力为0.6Mpa的条件下,将步骤(2)所得铜碳纳米管复合粉末-镁铜基非晶复合粉压制成块体,将块体置于温度为700℃的感应压铸炉中熔炼21s,再在压力为3Mpa的条件下压铸成型,即得铜碳纳米管复合粉末增强的Mg65Cu25Y10镁铜基非晶复合材料,即成分表示为(CNTs)2(Mg65Cu25Y10)98,其中x为碳纳米管的体积百分比;(3) Under the condition of a pressure of 0.6Mpa, the copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder obtained in step (2) is pressed into a block, and the block is placed in an induction die-casting furnace with a temperature of 700°C smelted for 21s, and then die-casted under the condition of 3Mpa to obtain the copper-carbon nanotube composite powder reinforced Mg 65 Cu 25 Y 10 magnesium copper-based amorphous composite material, that is, the composition is expressed as (CNTs) 2 (Mg 65 Cu 25 Y 10 ) 98 , wherein x is the volume percentage of carbon nanotubes;
本实施例中喷雾热解法为将炉腔抽真空,再通入还原气体(氢气)至炉腔内不含氧气,开始加热直至温度达到反应温度且为恒温,将前驱液通过雾化器进行雾化,再将雾化后的微米级液滴在还原气氛的带动下进入加热炉腔,进行干燥、分解反应、还原反应,开启粉末收集系统收集反应产物即Cu单质/碳纳米管复合粉末;In this embodiment, the spray pyrolysis method is to evacuate the furnace chamber, and then introduce reducing gas (hydrogen) until the furnace chamber does not contain oxygen, start heating until the temperature reaches the reaction temperature and is constant temperature, and the precursor solution is carried out through the atomizer. Atomization, and then the atomized micron-sized droplets are driven by the reducing atmosphere into the heating furnace chamber for drying, decomposition reaction, and reduction reaction, and the powder collection system is opened to collect the reaction product, namely Cu elemental substance/carbon nanotube composite powder;
本实施例制备的铜碳纳米管复合粉末增强的Mg65Cu25Y10镁铜基非晶复合材料60000倍下的组织形貌图如图2所示,240000倍下组织形貌图如图3所示,从图2和图3中可知,碳纳米管与镁铜基非晶结合良好,且在基体中分布均匀,增强效果明显;The microstructure of the copper-carbon nanotube composite powder reinforced Mg 65 Cu 25 Y 10 magnesium copper-based amorphous composite material prepared in this example at 60,000 times is shown in Figure 2, and the microstructure at 240,000 times is shown in Figure 3 It can be seen from Figure 2 and Figure 3 that the carbon nanotubes are well combined with the magnesium-copper-based amorphous, and they are evenly distributed in the matrix, and the strengthening effect is obvious;
本实施例的热性能测试结果如表1所示,从表1中可知,在相同的加热速率下,相比较于纯Mg基非晶合金,复合材料具有53.86K的过冷液相区间,即较高的玻璃形成能力。The thermal performance test results of this embodiment are shown in Table 1. It can be seen from Table 1 that at the same heating rate, compared with the pure Mg-based amorphous alloy, the composite material has a supercooled liquid phase interval of 53.86K, that is High glass forming ability.
实施例3:一种铜碳纳米管复合粉末增强镁铜基非晶复合材料的制备方法,具体步骤为:Embodiment 3: A kind of preparation method of copper-carbon nanotube composite powder reinforced magnesium-copper-based amorphous composite material, the specific steps are:
(1)在搅拌条件下,将乙酸铜溶解于去离子水得到乙酸铜水溶液,然后加入碳纳米管分散液并混合均匀得到前驱液;在温度为450℃、还原气体(氢气)氛围条件下,前驱液经喷雾热解法得到Cu单质/碳纳米管复合粉末;其中乙酸铜水溶液的浓度为4.938g/L,碳纳米管分散液中碳纳米管的质量百分数浓度为10%,前驱液中碳纳米管的质量百分数浓度为0.040%;碳纳米管为多壁碳纳米管,纯度为95%,外径20~60 nm,长度为0.5~15μm;还原气体(氢气)的流速为100 mL/min;(1) Under stirring conditions, dissolve copper acetate in deionized water to obtain copper acetate aqueous solution, then add carbon nanotube dispersion and mix uniformly to obtain a precursor solution; at a temperature of 450°C and a reducing gas (hydrogen) atmosphere, The precursor liquid was obtained Cu simple substance/carbon nanotube composite powder by spray pyrolysis; wherein the concentration of copper acetate aqueous solution was 4.938g/L, the mass percentage concentration of carbon nanotubes in the carbon nanotube dispersion liquid was 10%, and the carbon nanotubes in the precursor liquid The mass percent concentration of nanotubes is 0.040%; carbon nanotubes are multi-walled carbon nanotubes with a purity of 95%, an outer diameter of 20-60 nm, and a length of 0.5-15 μm; the flow rate of reducing gas (hydrogen) is 100 mL/min ;
(2)分别将金属Mg、Cu、Y打磨、超声清洗、真空干燥、研磨得到Mg粉、Cu粉、Y粉,将Mg粉、Cu粉、Y粉、步骤(1)所得Cu单质/碳纳米管复合粉末进行低能球磨混合得到铜碳纳米管复合粉末-镁铜基非晶复合粉;其中Mg粉、Cu粉、Y粉摩尔比为65:20:10,Cu粉与Cu单质/碳纳米管复合粉末中Cu单质的摩尔比为20:5;以质量百分数计,铜碳纳米管复合粉末-镁铜基非晶复合粉中碳纳米管占3%;(2) Grinding, ultrasonic cleaning, vacuum drying, and grinding metal Mg, Cu, and Y respectively to obtain Mg powder, Cu powder, and Y powder, and Mg powder, Cu powder, Y powder, Cu elemental/carbon nano The tube composite powder is mixed by low-energy ball milling to obtain copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder; the molar ratio of Mg powder, Cu powder, and Y powder is 65:20:10, and Cu powder and Cu simple substance/carbon nanotube The molar ratio of Cu in the composite powder is 20:5; in terms of mass percentage, carbon nanotubes account for 3% in the copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder;
(3)在压力为0.7Mpa的条件下,将步骤(2)所得铜碳纳米管复合粉末-镁铜基非晶复合粉压制成块体,将块体置于温度为800℃的感应压铸炉中熔炼20s,再在压力为5Mpa的条件下压铸成型,即得铜碳纳米管复合粉末增强的Mg65Cu25Y10镁铜基非晶复合材料,即成分表示为(CNTs)3(Mg65Cu25Y10)97,其中x为碳纳米管的体积百分比;(3) Under the condition of a pressure of 0.7Mpa, the copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder obtained in step (2) is pressed into a block, and the block is placed in an induction die-casting furnace with a temperature of 800°C smelted for 20s, and then die-casted under the condition of 5Mpa to obtain the copper-carbon nanotube composite powder reinforced Mg 65 Cu 25 Y 10 magnesium-copper-based amorphous composite material, that is, the composition is expressed as (CNTs) 3 (Mg 65 Cu 25 Y 10 ) 97 , wherein x is the volume percentage of carbon nanotubes;
本实施例中喷雾热解法为将炉腔抽真空,再通入还原气体(氢气)至炉腔内不含氧气,开始加热直至温度达到反应温度且为恒温,将前驱液通过雾化器进行雾化,再将雾化后的微米级液滴在还原气氛的带动下进入加热炉腔,进行干燥、分解反应、还原反应,开启粉末收集系统收集反应产物即Cu单质/碳纳米管复合粉末;In this embodiment, the spray pyrolysis method is to evacuate the furnace chamber, and then introduce reducing gas (hydrogen) until the furnace chamber does not contain oxygen, start heating until the temperature reaches the reaction temperature and is constant temperature, and the precursor solution is carried out through the atomizer. Atomization, and then the atomized micron-sized droplets are driven by the reducing atmosphere into the heating furnace chamber for drying, decomposition reaction, and reduction reaction, and the powder collection system is opened to collect the reaction product, namely Cu elemental substance/carbon nanotube composite powder;
本实施例的热性能测试结果如表1所示,从表1中可知,在相同的加热速率下,相比较于纯Mg基非晶合金,复合材料具有52.53K的过冷液相区间,即较高的玻璃形成能力。The thermal performance test results of this embodiment are shown in Table 1. It can be seen from Table 1 that at the same heating rate, compared with the pure Mg-based amorphous alloy, the composite material has a supercooled liquid phase interval of 52.53K, that is High glass forming ability.
实施例4:一种铜碳纳米管复合粉末增强镁铜基非晶复合材料的制备方法,具体步骤为:Embodiment 4: A kind of preparation method of copper-carbon nanotube composite powder reinforced magnesium-copper-based amorphous composite material, the specific steps are:
(1)在搅拌条件下,将乙酸铜溶解于去离子水得到乙酸铜水溶液,然后加入碳纳米管分散液并混合均匀得到前驱液;在温度为480℃、还原气体(氢气)氛围条件下,前驱液经喷雾热解法得到Cu单质/碳纳米管复合粉末;其中乙酸铜水溶液的浓度为4.938g/L,碳纳米管分散液中碳纳米管的质量百分数浓度为10%,前驱液中碳纳米管的质量百分数浓度为0.054%;碳纳米管为多壁碳纳米管,纯度为95%,外径20~60 nm,长度为0.5~15μm;还原气体(氢气)的流速为100 mL/min;(1) Under stirring conditions, dissolve copper acetate in deionized water to obtain a copper acetate aqueous solution, then add carbon nanotube dispersion liquid and mix uniformly to obtain a precursor liquid; at a temperature of 480°C and a reducing gas (hydrogen) atmosphere, The precursor liquid was obtained Cu simple substance/carbon nanotube composite powder by spray pyrolysis; wherein the concentration of copper acetate aqueous solution was 4.938g/L, the mass percentage concentration of carbon nanotubes in the carbon nanotube dispersion liquid was 10%, and the carbon nanotubes in the precursor liquid The mass percent concentration of nanotubes is 0.054%; carbon nanotubes are multi-walled carbon nanotubes with a purity of 95%, an outer diameter of 20-60 nm, and a length of 0.5-15 μm; the flow rate of reducing gas (hydrogen) is 100 mL/min ;
(2)分别将金属Mg、Cu、Y打磨、超声清洗、真空干燥、研磨得到Mg粉、Cu粉、Y粉,将Mg粉、Cu粉、Y粉、步骤(1)所得Cu单质/碳纳米管复合粉末进行低能球磨混合得到铜碳纳米管复合粉末-镁铜基非晶复合粉;其中Mg粉、Cu粉、Y粉摩尔比为65:20:10,Cu粉与Cu单质/碳纳米管复合粉末中Cu单质的摩尔比为20:5;以质量百分数计,铜碳纳米管复合粉末-镁铜基非晶复合粉中碳纳米管占4%;(2) Grinding, ultrasonic cleaning, vacuum drying, and grinding metal Mg, Cu, and Y respectively to obtain Mg powder, Cu powder, and Y powder, and Mg powder, Cu powder, Y powder, Cu elemental/carbon nano The tube composite powder is mixed by low-energy ball milling to obtain copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder; the molar ratio of Mg powder, Cu powder, and Y powder is 65:20:10, and Cu powder and Cu simple substance/carbon nanotube The molar ratio of Cu in the composite powder is 20:5; in terms of mass percentage, carbon nanotubes account for 4% in the copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder;
(3)在压力为0.8Mpa的条件下,将步骤(2)所得铜碳纳米管复合粉末-镁铜基非晶复合粉压制成块体,将块体置于温度为900℃的感应压铸炉中熔炼18s,再在压力为8Mpa的条件下压铸成型,即得铜碳纳米管复合粉末增强的Mg65Cu25Y10镁铜基非晶复合材料,即成分表示为(CNTs)4(Mg65Cu25Y10)96,其中x为碳纳米管的体积百分比;(3) Under the condition of a pressure of 0.8Mpa, the copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder obtained in step (2) is pressed into a block, and the block is placed in an induction die-casting furnace with a temperature of 900°C Melted in medium for 18s, and then die-casted under the condition of 8Mpa to obtain copper-carbon nanotube composite powder-reinforced Mg 65 Cu 25 Y 10 magnesium-copper-based amorphous composite material, that is, the composition is expressed as (CNTs) 4 (Mg 65 Cu 25 Y 10 ) 96 , where x is the volume percentage of carbon nanotubes;
本实施例中喷雾热解法为将炉腔抽真空,再通入还原气体(氢气)至炉腔内不含氧气,开始加热直至温度达到反应温度且为恒温,将前驱液通过雾化器进行雾化,再将雾化后的微米级液滴在还原气氛的带动下进入加热炉腔,进行干燥、分解反应、还原反应,开启粉末收集系统收集反应产物即Cu单质/碳纳米管复合粉末;In this embodiment, the spray pyrolysis method is to evacuate the furnace chamber, and then introduce reducing gas (hydrogen) until the furnace chamber does not contain oxygen, start heating until the temperature reaches the reaction temperature and is constant temperature, and the precursor solution is carried out through the atomizer. Atomization, and then the atomized micron-sized droplets are driven by the reducing atmosphere into the heating furnace chamber for drying, decomposition reaction, and reduction reaction, and the powder collection system is opened to collect the reaction product, namely Cu elemental substance/carbon nanotube composite powder;
本实施例的热性能测试结果如表1所示,从表1中可知,在相同的加热速率下,相比较于纯Mg基非晶合金,复合材料具有48.51K的过冷液相区间,即较高的玻璃形成能力。The thermal performance test results of this embodiment are shown in Table 1. It can be seen from Table 1 that at the same heating rate, compared with the pure Mg-based amorphous alloy, the composite material has a supercooled liquid phase interval of 48.51K, that is High glass forming ability.
实施例5:一种铜碳纳米管复合粉末增强镁铜基非晶复合材料的制备方法,具体步骤为:Example 5: A method for preparing a copper-carbon nanotube composite powder reinforced magnesium-copper-based amorphous composite material, the specific steps are:
(1)在搅拌条件下,将乙酸铜溶解于去离子水得到乙酸铜水溶液,然后加入碳纳米管分散液并混合均匀得到前驱液;在温度为500℃、还原气体(氢气)氛围条件下,前驱液经喷雾热解法得到Cu单质/碳纳米管复合粉末;其中乙酸铜水溶液的浓度为4.938g/L,碳纳米管分散液中碳纳米管的质量百分数浓度为10 %,前驱液中碳纳米管的质量百分数浓度为0.068%;碳纳米管为多壁碳纳米管,纯度为95%,外径20~60 nm,长度为0.5~15μm;还原气体(氢气)的流速为100 mL/min;(1) Under stirring conditions, dissolve copper acetate in deionized water to obtain a copper acetate aqueous solution, then add carbon nanotube dispersion liquid and mix uniformly to obtain a precursor liquid; at a temperature of 500°C and a reducing gas (hydrogen) atmosphere, Precursor solution obtains Cu simple substance/carbon nanotube composite powder through spray pyrolysis; Wherein the concentration of copper acetate aqueous solution is 4.938g/L, the mass percentage concentration of carbon nanotube in the carbon nanotube dispersion liquid is 10%, the carbon nanotube in the precursor solution The mass percent concentration of nanotubes is 0.068%; the carbon nanotubes are multi-walled carbon nanotubes with a purity of 95%, an outer diameter of 20-60 nm, and a length of 0.5-15 μm; the flow rate of reducing gas (hydrogen) is 100 mL/min ;
(2)分别将金属Mg、Cu、Y打磨、超声清洗、真空干燥、研磨得到Mg粉、Cu粉、Y粉,将Mg粉、Cu粉、Y粉、步骤(1)所得Cu单质/碳纳米管复合粉末进行低能球磨混合得到铜碳纳米管复合粉末-镁铜基非晶复合粉;其中Mg粉、Cu粉、Y粉摩尔比为65:20:10,Cu粉与Cu单质/碳纳米管复合粉末中Cu单质的摩尔比为20:5;以质量百分数计,铜碳纳米管复合粉末-镁铜基非晶复合粉中碳纳米管占5%;(2) Grinding, ultrasonic cleaning, vacuum drying, and grinding metal Mg, Cu, and Y respectively to obtain Mg powder, Cu powder, and Y powder, and Mg powder, Cu powder, Y powder, Cu elemental/carbon nano The tube composite powder is mixed by low-energy ball milling to obtain copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder; the molar ratio of Mg powder, Cu powder, and Y powder is 65:20:10, and Cu powder and Cu simple substance/carbon nanotube The molar ratio of Cu in the composite powder is 20:5; in terms of mass percentage, carbon nanotubes account for 5% in the copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder;
(3)在压力为1Mpa的条件下,将步骤(2)所得铜碳纳米管复合粉末-镁铜基非晶复合粉压制成块体,将块体置于温度为1000℃的感应压铸炉中熔炼15s,再在压力为10Mpa的条件下压铸成型,即得铜碳纳米管复合粉末增强的Mg65Cu25Y10镁铜基非晶复合材料,即成分表示为(CNTs)5 (Mg65Cu25Y10)95,其中x为碳纳米管的体积百分比;(3) Under the condition of a pressure of 1Mpa, press the copper-carbon nanotube composite powder-magnesium-copper-based amorphous composite powder obtained in step (2) into a block, and place the block in an induction die-casting furnace with a temperature of 1000°C Melting for 15s, and then die-casting under the condition of 10Mpa, the copper-carbon nanotube composite powder reinforced Mg 65 Cu 25 Y 10 magnesium copper-based amorphous composite material, that is, the composition is expressed as (CNTs) 5 (Mg 65 Cu 25 Y 10 ) 95 , wherein x is the volume percentage of carbon nanotubes;
本实施例中喷雾热解法为将炉腔抽真空,再通入还原气体(氢气)至炉腔内不含氧气,开始加热直至温度达到反应温度且为恒温,将前驱液通过雾化器进行雾化,再将雾化后的微米级液滴在还原气氛的带动下进入加热炉腔,进行干燥、分解反应、还原反应,开启粉末收集系统收集反应产物即Cu单质/碳纳米管复合粉末;In this embodiment, the spray pyrolysis method is to evacuate the furnace chamber, and then introduce reducing gas (hydrogen) until the furnace chamber does not contain oxygen, start heating until the temperature reaches the reaction temperature and is constant temperature, and the precursor solution is carried out through the atomizer. Atomization, and then the atomized micron-sized droplets are driven by the reducing atmosphere into the heating furnace chamber for drying, decomposition reaction, and reduction reaction, and the powder collection system is opened to collect the reaction product, namely Cu elemental substance/carbon nanotube composite powder;
本实施例的热性能测试结果如表1所示,The thermal performance test result of the present embodiment is as shown in table 1,
表 1 复合材料性能测试结果Table 1 Performance test results of composite materials
从表1中可知,在相同的加热速率下,相比较于纯Mg基非晶合金,复合材料具有46.32K的过冷液相区间,即较高的玻璃形成能力。It can be seen from Table 1 that at the same heating rate, compared with pure Mg-based amorphous alloys, the composite material has a supercooled liquid phase interval of 46.32K, that is, a higher glass-forming ability.
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CN113098163A (en) * | 2021-04-19 | 2021-07-09 | 云南铜业压铸科技有限公司 | Cast copper rotor for high-rotation-speed motor and preparation method thereof |
CN118385597A (en) * | 2024-04-26 | 2024-07-26 | 北京科技大学 | Preparation method of network interface design of copper-based carbon nanotube composite material |
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CN111647766A (en) * | 2020-06-11 | 2020-09-11 | 昆明理工大学 | Preparation method of copper-based composite material |
CN113098163A (en) * | 2021-04-19 | 2021-07-09 | 云南铜业压铸科技有限公司 | Cast copper rotor for high-rotation-speed motor and preparation method thereof |
CN113098163B (en) * | 2021-04-19 | 2023-03-24 | 云南铜业压铸科技有限公司 | Preparation method of cast copper rotor for high-rotation-speed motor |
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