CN103643075B - Cu-base composites of nano-particle reinforcement and preparation method thereof - Google Patents
Cu-base composites of nano-particle reinforcement and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000002787 reinforcement Effects 0.000 title claims abstract 14
- 239000000758 substrate Substances 0.000 claims abstract description 34
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000010949 copper Substances 0.000 claims abstract description 31
- 229910052802 copper Inorganic materials 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011733 molybdenum Substances 0.000 claims abstract description 12
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 10
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical group [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910039444 MoC Inorganic materials 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 23
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 6
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 4
- 238000005137 deposition process Methods 0.000 claims description 2
- 238000000050 ionisation spectroscopy Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 239000000428 dust Substances 0.000 claims 1
- 238000000151 deposition Methods 0.000 abstract description 10
- 238000000034 method Methods 0.000 description 26
- 238000010438 heat treatment Methods 0.000 description 6
- 238000002955 isolation Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- ZLVDRPIZTVABIW-UHFFFAOYSA-N [Cu].[C].[Mo] Chemical compound [Cu].[C].[Mo] ZLVDRPIZTVABIW-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229910000881 Cu alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 229910017767 Cu—Al Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- XACAZEWCMFHVBX-UHFFFAOYSA-N [C].[Mo] Chemical compound [C].[Mo] XACAZEWCMFHVBX-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 borides Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005328 electron beam physical vapour deposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 230000000754 repressing effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及一种纳米颗粒增强的铜基复合材料及其制备方法，具体涉及一种纳米颗粒增强的铜-钼-碳复合材料及制备方法。The invention relates to a copper-based composite material reinforced by nanoparticles and a preparation method thereof, in particular to a copper-molybdenum-carbon composite material reinforced by nanoparticles and a preparation method thereof.
背景技术Background technique
铜及铜合金材料是一种重要的有色金属材料，由于具有优异的物理和力学性能，在电子工业等领域获得了广泛的应用。但随着科学技术（尤其是微电子工业的快速发展）的快速发展，传统的铜及其合金由于电性能和强度不能兼顾，已经不能满足要求。纳米弥散强化铜合是以纳米粒子为第二相的新型复合材料，由于纳米粒子可以有效地阻碍位错运动和晶界滑移使材料的力学性能提高，同时不会明显降低电导率，从而较好地解决了电性能和强度不能兼顾的问题。目前，此材料中的增强粒子有氧化物、碳化物、硼化物、氮化物和难熔金属等。制备此材料的方法主要由内氧化法、粉末冶金方法和机械合金化方法等。内氧化法是利用低氧条件下Cu-Al合金中Al发生选择性氧化形成Al2O3的工艺。该工艺是目前用于制备Cu-Al2O3弥散强化复合材料的主要工艺，制备的材料性能好，但此工艺还存在着工序复杂、周期长、成本高的缺点。粉末冶金法是利用铜粉与增强粒子按一定配比在干混或湿混条件下，经过机械混合可得到增强粒子混合均匀的混合粉末，成型、真空或保护气氛条件下烧结，复压、复烧来制备材料的工艺。该工艺虽然可制备各种尺寸增强粒子分布的复合材料，但还存在着制备的复合材料的力学性能差、工序多、成本高的缺点。机械合金化方法是采用高能球磨机将铜粉与增强粒子混合均匀后，成型、真空或保护气氛条件下烧结，复压、复烧来制备材料的工艺。同样，该工艺也存在力学性能差、工序多、成本高的缺点。总之，目前关于制备纳米弥散强化的铜基复合材料都存在工序多、周期长、成本高的问题。因此，在此背景下发明一种高强高导电性能的复合材料及工序简单、成本低的制备工艺具有重要的意义。Copper and copper alloy materials are important non-ferrous metal materials, which have been widely used in the electronics industry and other fields due to their excellent physical and mechanical properties. However, with the rapid development of science and technology (especially the rapid development of the microelectronics industry), traditional copper and its alloys cannot meet the requirements due to the inability to balance electrical properties and strength. Nano-dispersion strengthened copper alloy is a new type of composite material with nanoparticles as the second phase. Because nanoparticles can effectively hinder dislocation movement and grain boundary slippage, the mechanical properties of the material can be improved, and the electrical conductivity will not be significantly reduced. It solves the problem that the electrical performance and the strength cannot be balanced. At present, the reinforcing particles in this material include oxides, carbides, borides, nitrides and refractory metals. The methods of preparing this material mainly include internal oxidation method, powder metallurgy method and mechanical alloying method. The internal oxidation method is a process in which Al in Cu-Al alloy is selectively oxidized to form Al 2 O 3 under low oxygen conditions. This process is currently the main process used to prepare Cu-Al 2 O 3 dispersion-strengthened composite materials, and the prepared materials have good properties, but this process still has the disadvantages of complicated procedures, long cycle time, and high cost. The powder metallurgy method is to use copper powder and reinforcing particles according to a certain ratio under dry or wet mixing conditions, and mechanically mix to obtain a mixed powder with reinforced particles mixed uniformly, forming, sintering under vacuum or protective atmosphere conditions, and repressing and recombining. The process of firing to prepare materials. Although this process can prepare composite materials with enhanced particle distribution in various sizes, it still has the disadvantages of poor mechanical properties, many procedures and high cost. The mechanical alloying method is to use a high-energy ball mill to mix copper powder and reinforcing particles evenly, then shape, sinter under vacuum or protective atmosphere conditions, and repress and refire to prepare materials. Similarly, this process also has the disadvantages of poor mechanical properties, many processes, and high cost. In a word, the current preparation of nano-dispersion-strengthened copper matrix composites has the problems of many processes, long cycle time and high cost. Therefore, in this context, it is of great significance to invent a composite material with high strength and high conductivity and a preparation process with simple process and low cost.
发明内容Contents of the invention
本发明的目的是提供一种具有优异力学性能、电性能的纳米颗粒增强的铜基复合材料及其制备方法。The object of the present invention is to provide a copper-based composite material reinforced by nanoparticles with excellent mechanical properties and electrical properties and a preparation method thereof.
为实现上述发明目的，本发明采用如下技术方案：In order to realize the above-mentioned purpose of the invention, the present invention adopts following technical scheme:
本发明提供了一种纳米颗粒增强的铜基复合材料，所述的铜基复合材料中，铜基体晶粒尺寸小于20μm，纳米颗粒增强相为碳化钼、或碳化钼与钼、或碳化钼与碳，纳米颗粒增强相的颗粒尺寸在200nm以下；所述铜基复合材料中，Mo的质量百分含量为0.1-15%，C的质量百分含量为在1%以下。The invention provides a nanoparticle-reinforced copper-based composite material. In the copper-based composite material, the grain size of the copper matrix is less than 20 μm, and the nanoparticle-reinforced phase is molybdenum carbide, or molybdenum carbide and molybdenum, or molybdenum carbide and molybdenum Carbon, the particle size of the nano-particle reinforced phase is below 200nm; in the copper matrix composite material, the mass percentage of Mo is 0.1-15%, and the mass percentage of C is below 1%.
所述的铜基复合材料的性能指标如下：屈服强度Rp0.2≥420MPa，抗拉强度Rm≥480MPa，电导率≥70%ICAS。The performance indexes of the copper-based composite material are as follows: yield strength R p0.2 ≥ 420MPa, tensile strength Rm ≥ 480MPa, electrical conductivity ≥ 70% ICAS.
本发明还提供了一种所述纳米颗粒增强的铜基复合材料的制备方法，包括如下步骤：The present invention also provides a method for preparing the nanoparticle-reinforced copper-based composite material, comprising the following steps:
（1）将铜锭料与钼源、碳源中的一种的或两种分别放于坩埚内，并在铜锭料上面放隔离层原料；(1) Put the copper ingot, one or both of the molybdenum source and the carbon source in the crucible, and place the isolation layer raw material on the copper ingot;
（2）抽真空，加热基板；(2) Vacuumize and heat the substrate;
（3）当真空度达到9×10-2Pa以下、基板温度达到500-800℃，打开基板旋转装置，使基板旋转，沉积隔离层；(3) When the vacuum degree reaches below 9×10 -2 Pa and the substrate temperature reaches 500-800°C, turn on the substrate rotation device to rotate the substrate and deposit the isolation layer;
（4）打开挡板，开始沉积材料；(4) Open the baffle and start to deposit materials;
（5）沉积完成，待基板冷却后，取下基板，分离获得沉积层材料，即为纳米颗粒增强的铜基复合材料。(5) After the deposition is completed, after the substrate is cooled, the substrate is removed, and the deposition layer material is obtained by separation, that is, the nanoparticle-reinforced copper-based composite material.
所述步骤（1）中，钼源或者碳源可制成相应的锭料分别置于坩埚中，或者将碳制成锭料，在该锭料上面放上钼原料置于同一个坩埚中。In the step (1), the molybdenum source or the carbon source can be made into corresponding ingots and placed in crucibles respectively, or carbon can be made into ingots, and molybdenum raw materials are placed on the ingots and placed in the same crucible.
进一步，所述的碳源是碳靶，或碳粉，或蒽粉。Further, the carbon source is carbon target, or carbon powder, or anthracene powder.
进一步，隔离层原料选自CaF2或ZrO2。Further, the raw material of the isolation layer is selected from CaF 2 or ZrO 2 .
进一步，沉积过程中，基板转速控制在3-20rev/min。Further, during the deposition process, the rotational speed of the substrate is controlled at 3-20 rev/min.
所述步骤（4）中，本领域技术人员可根据实际需要通过控制电子枪的束流大小和沉积时间控制沉积材料的组成和厚度。In the step (4), those skilled in the art can control the composition and thickness of the deposited material by controlling the beam current size and deposition time of the electron gun according to actual needs.
与现有技术相比，本发明的有益效果是：Compared with prior art, the beneficial effect of the present invention is:
（1）本发明制得的纳米颗粒增强的铜-钼-碳复合材料具有优异的力学性能和电性能，其屈服强度Rp0.2≥420MPa，抗拉强度Rm≥480MPa，电导率≥70%IACS，而纯铜的室温屈服强度为33MPa，抗拉强度为209MPa；(1) The nanoparticle-reinforced copper-molybdenum-carbon composite material prepared in the present invention has excellent mechanical properties and electrical properties, and its yield strength R p0.2 ≥ 420MPa, tensile strength Rm ≥ 480MPa, and electrical conductivity ≥ 70% IACS, while the room temperature yield strength of pure copper is 33MPa, and the tensile strength is 209MPa;
（2）本发明采用的电子束物理气相沉积工艺简单，成本低，易于控制。具体地，目前铜的沉积速率可以达到20μm/min，即沉积直径1m，厚度为2mm的板材只需沉积100min。而同样的内氧化法制备纳米弥散强化铜基复合材料，光内氧化过程就需4-60h，而且在还原气氛条件进行热压烧结，所需工序多，时间长。(2) The electron beam physical vapor deposition process adopted in the present invention is simple, low in cost and easy to control. Specifically, the current copper deposition rate can reach 20 μm/min, that is, a plate with a deposition diameter of 1 m and a thickness of 2 mm only needs to be deposited for 100 min. However, the preparation of nano-dispersion strengthened copper-based composite materials by the same internal oxidation method requires 4-60 hours for the light internal oxidation process, and hot-pressing sintering under reducing atmosphere conditions requires many processes and takes a long time.
附图说明Description of drawings
图1为实施例1制备的铜-钼-碳材料表面SEM照片。FIG. 1 is an SEM photo of the surface of the copper-molybdenum-carbon material prepared in Example 1.
图2为实施例1制备的铜-钼-碳材料TEM照片。FIG. 2 is a TEM photo of the copper-molybdenum-carbon material prepared in Example 1.
具体实施方式detailed description
下面通过优选实施例对本发明的技术方案做进一步说明，但不应将其理解为对本发明保护范围的限制。The technical solutions of the present invention will be further described through preferred embodiments below, but they should not be construed as limiting the protection scope of the present invention.
实施例1：Example 1:
将铜锭料和石墨锭料放入坩埚中，并在石墨锭料上面放上200g钼，在铜锭料上面放上5gCaF2;关上真空室，开始抽真空；启动转动装置使基板以6rpm的速度转动，并打开基板加热装置，加热基板温度使之稳定在650℃；当真空度达到3×10-2Pa时，打开挡板、电子枪，沉积隔离层CaF2；以束流大小1.5A加热铜锭料，以束流大小1.5A加热石墨锭料，开始沉积材料，沉积50min后，关闭电子枪，拉上挡板，关闭加热装置，关闭基板旋转装置；当基板温度降到200℃以下时，关闭真空系统，取下基板，分离获得厚度0.26mm，直径520mm的板材。制备的板材成分为Cu-Mo1.3wt%-C0.086wt%，根据国家标准GB/T228.1-2010对对最终产品进行力学性能测试，其屈服强度Rp0.2=426MPa，抗拉强度Rm=480MPa。以四探针法对材料的电导率进行检测，其电导率为82%IACS。制备的铜-钼碳复合材料铜基体晶粒尺寸为5-10μm（见图1），第二相为Mo2C,平均尺寸约为5nm（见图2）。Copper ingot and graphite ingot are put into the crucible, and 200g molybdenum is put on the graphite ingot, and 5gCaF is put on the copper ingot; Close the vacuum chamber and start vacuuming; Start the rotating device to make the substrate at 6rpm Rotate at high speed and turn on the substrate heating device to heat the substrate temperature to stabilize it at 650°C; when the vacuum reaches 3×10 -2 Pa, turn on the baffle and electron gun to deposit the isolation layer CaF 2 ; heat with a beam size of 1.5A For the copper ingot, heat the graphite ingot with a beam size of 1.5A, and start to deposit materials. After 50 minutes of deposition, turn off the electron gun, pull up the baffle, turn off the heating device, and turn off the substrate rotation device; when the substrate temperature drops below 200°C, Turn off the vacuum system, remove the substrate, and separate to obtain a plate with a thickness of 0.26 mm and a diameter of 520 mm. The composition of the prepared plate is Cu-Mo1.3wt%-C0.086wt%, and the mechanical properties of the final product are tested according to the national standard GB/T228.1-2010. The yield strength R p0.2 =426MPa, the tensile strength Rm =480MPa. The electrical conductivity of the material was detected by the four-probe method, and the electrical conductivity was 82% IACS. The copper matrix grain size of the prepared copper-molybdenum carbon composite material is 5-10μm (see Figure 1), the second phase is Mo 2 C, and the average size is about 5nm (see Figure 2).
实施例2：Example 2:
将铜锭料、钼锭料和蒽粉分别放入坩埚中，并在铜锭料上面放上5gCaF2;关上真空室，开始抽真空；启动转动装置使基板以15rpm的速度转动，并打开基板加热装置，加热基板温度使之稳定在750℃；当真空度达到3×10-2Pa时，打开挡板、电子枪，沉积隔离层CaF2；以束流大小2.2A加热铜锭料，以束流大小2.6A加热钼锭料，以束流大小0.6A加热蒽粉，开始沉积材料，当沉积30min后，关闭电子枪，拉上挡板，关闭加热装置，关闭基板旋转装置；当基板温度降到200℃以下时，关闭真空系统，取下基板，分离获得厚度0.3mm，直径520mm的板材。制备的板材成分为Cu-Mo15wt%-C0.2wt%，根据国家标准GB/T228.1-2010对对最终产品进行力学性能测试，其屈服强度Rp0.2=540MPa，抗拉强度Rm=600MPa。以四探针法对材料的电导率进行检测，其电导率为70%IACS。制备态材料基体晶粒尺寸为1-5μm，第二相颗粒为Mo（平均尺寸为180nm），Mo2C（平均尺寸为20nm）。Put the copper ingot, molybdenum ingot and anthracene powder into the crucible respectively, and put 5gCaF2 on the copper ingot; close the vacuum chamber and start vacuuming; start the rotating device to rotate the substrate at a speed of 15rpm, and open the substrate Heating device to heat the substrate temperature to stabilize it at 750°C; when the vacuum reaches 3×10 -2 Pa, open the baffle and electron gun to deposit the isolation layer CaF 2 ; heat the copper ingot with a beam size of 2.2A, and Heat the molybdenum ingot with a current size of 2.6A, heat the anthracene powder with a beam size of 0.6A, and start to deposit materials. After 30 minutes of deposition, turn off the electron gun, pull up the baffle, turn off the heating device, and turn off the substrate rotation device; when the temperature of the substrate drops to When the temperature is below 200°C, turn off the vacuum system, remove the substrate, and separate to obtain a plate with a thickness of 0.3mm and a diameter of 520mm. The composition of the prepared plate is Cu-Mo15wt%-C0.2wt%, and the mechanical properties of the final product are tested according to the national standard GB/T228.1-2010. The yield strength R p0.2 =540MPa, and the tensile strength Rm=600MPa . The electrical conductivity of the material was detected by the four-probe method, and the electrical conductivity was 70% IACS. The matrix grain size of the prepared material is 1-5μm, and the second phase particles are Mo (average size 180nm) and Mo 2 C (average size 20nm).
实施例3：Example 3:
将铜锭料、钼锭料和蒽粉分别放入坩埚中，并在铜锭料上面放上5gZrO2;关上真空室，开始抽真空；启动转动装置使基板以8rpm的速度转动，并打开基板加热装置，加热基板温度使之稳定在650℃；当真空度达到3×10-2Pa时，打开挡板、电子枪，沉积隔离层ZrO2；以束流大小2.2A加热铜锭料，以束流大小2.0A加热钼锭料，以束流大小1A加热蒽粉，开始沉积材料，当沉积40min后，关闭电子枪，拉上挡板，关闭加热装置，关闭基板旋转装置；当基板温度降到200℃以下时，关闭真空系统，取下基板，分离获得厚度0.38mm，直径520mm的板材。制备的板材成分为Cu-Mo0.2wt%-C1wt%,根据国家标准GB/T228.1-2010对最终产品进行力学性能测试，其屈服强度Rp0.2=440MPa，抗拉强度Rm=500MPa。以四探针法对材料的电导率进行检测，其电导率为80%IACS。制备态材料基体晶粒尺寸为1-5μm，第二相颗粒为C（平均尺寸为16nm），Mo2C（平均尺寸为20nm）。Put the copper ingot, molybdenum ingot and anthracene powder into the crucible respectively, and put 5gZrO2 on the copper ingot; close the vacuum chamber and start vacuuming; start the rotating device to rotate the substrate at a speed of 8rpm, and open the substrate Heating device to heat the substrate temperature to stabilize it at 650°C; when the vacuum reaches 3×10 -2 Pa, open the baffle and electron gun to deposit the isolation layer ZrO 2 ; heat the copper ingot with a beam size of 2.2A, and Heat the molybdenum ingot with a current size of 2.0A, heat the anthracene powder with a beam size of 1A, and start to deposit materials. After 40 minutes of deposition, turn off the electron gun, pull up the baffle, turn off the heating device, and turn off the substrate rotation device; when the temperature of the substrate drops to 200 When the temperature is below ℃, turn off the vacuum system, remove the substrate, and separate to obtain a plate with a thickness of 0.38mm and a diameter of 520mm. The composition of the prepared plate is Cu-Mo0.2wt%-C1wt%, and the mechanical properties of the final product are tested according to the national standard GB/T228.1-2010. The yield strength R p0.2 = 440MPa, and the tensile strength Rm = 500MPa. The electrical conductivity of the material was detected by the four-probe method, and the electrical conductivity was 80% IACS. The matrix grain size of the prepared material is 1-5 μm, and the second phase particles are C (average size 16nm) and Mo 2 C (average size 20nm).
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