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CN1611623A - Nickel-silicon base intermetallic compound composite material and its preparing method - Google Patents

Nickel-silicon base intermetallic compound composite material and its preparing method Download PDF

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CN1611623A
CN1611623A CN 200310103787 CN200310103787A CN1611623A CN 1611623 A CN1611623 A CN 1611623A CN 200310103787 CN200310103787 CN 200310103787 CN 200310103787 A CN200310103787 A CN 200310103787A CN 1611623 A CN1611623 A CN 1611623A
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reaction
nickel
composite material
silicon
intermetallic compound
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毕秦岭
喇培清
刘维民
薛群基
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

本发明公开了一种镍硅基金属间化合物复合材料及其制备方法。材料的原料由镍23.5~75.6,硅3.7~12.1,三氧化二铬1.9~11.3,三氧化铬6.3~37.3,铝4.1~24.2,活性炭0~1.2(质量百分数)组成。复合材料的制备方法采用燃烧合成熔化法,利用化学反应自身所释放的热量,合成具有高纯度的致密Ni3Si基金属间化合物复合材料。该方法与熔炼法或热压烧结法相比,工艺及所需设备简单,成本明显降低,制备的材料具有良好的微观组织结构及性能。The invention discloses a nickel-silicon-based intermetallic compound composite material and a preparation method thereof. The raw material of the material is composed of 23.5-75.6 nickel, 3.7-12.1 silicon, 1.9-11.3 chromium trioxide, 6.3-37.3 chromium trioxide, 4.1-24.2 aluminum, and 0-1.2 (mass percentage) of activated carbon. The preparation method of the composite material adopts a combustion synthesis melting method, and utilizes the heat released by the chemical reaction itself to synthesize a high-purity dense Ni 3 Si-based intermetallic compound composite material. Compared with the smelting method or the hot pressing sintering method, the method has simple process and required equipment, and the cost is obviously reduced, and the prepared material has good microstructure and performance.

Description

镍硅基金属间化合物复合材料及其制备方法Nickel-silicon-based intermetallic compound composite material and preparation method thereof

技术领域technical field

本发明叙述了一种镍硅基金属间化合物复合材料及其制备方法。The invention describes a nickel-silicon-based intermetallic compound composite material and a preparation method thereof.

背景技术Background technique

Ni3Si基金属间化合物及其复合材料具有高强度、高硬度和优良的耐酸性及高温性能,是具有重要应用前景的高温结构材料。Ni 3 Si-based intermetallic compounds and their composite materials have high strength, high hardness and excellent acid resistance and high temperature performance, and are high-temperature structural materials with important application prospects.

传统的熔炼或粉末冶金方法制备Ni3Si基金属间化合物及其复合材料,需要1200℃以上的高温,粉末冶金法还需要的100MPa的压力。这些方法所需设备复杂、能耗高、生产周期长,成本高。The traditional smelting or powder metallurgy method to prepare Ni 3 Si-based intermetallic compounds and their composite materials requires a high temperature above 1200°C, and the powder metallurgy method also requires a pressure of 100 MPa. These methods require complex equipment, high energy consumption, long production cycle and high cost.

发明内容Contents of the invention

本发明的目的在于克服现有技术中的不足而提供一种镍硅基金属间化合物复合材料及其制备方法。The object of the present invention is to overcome the deficiencies in the prior art and provide a nickel-silicon-based intermetallic compound composite material and a preparation method thereof.

一种镍硅基金属间化合物复合材料,其特征在于材料的原料由镍23.5~75.6,硅3.7~12.1,三氧化二铬1.9~11.3,三氧化铬6.3~37.3,铝4.1~24.2,活性炭0~1.2(质量百分数)组成。A nickel-silicon-based intermetallic compound composite material, characterized in that the raw materials of the material are nickel 23.5-75.6, silicon 3.7-12.1, dichromium trioxide 1.9-11.3, chromium trioxide 6.3-37.3, aluminum 4.1-24.2, activated carbon 0 ~1.2 (mass percent) composition.

复合材料的制备方法采用燃烧合成熔化法,利用化学反应自身所释放的热量,合成具有高纯度的致密Ni3Si基金属间化合物复合材料。由于反应产物存在短时熔融过程且反应产物间存在密度差及互熔特性,可自发进行增强相与基体的均匀混合,并迅速与杂质分离,方便地获得了不同自生相增强的复合材料。通过惰性气体加压,提高了材料的致密度,改善了材料的微观组织结构。The preparation method of the composite material adopts a combustion synthesis melting method, and utilizes the heat released by the chemical reaction itself to synthesize a high-purity dense Ni 3 Si-based intermetallic compound composite material. Due to the short-term melting process of the reaction products and the density difference and mutual melting characteristics between the reaction products, the reinforcement phase can be mixed spontaneously with the matrix and separated from impurities quickly, and composite materials with different self-generated phase reinforcements can be obtained conveniently. Pressurization with inert gas increases the density of the material and improves the microstructure of the material.

本发明的Ni3Si基金属间化合物复合材料制备方法,其特征在于该方法包括:按质量百分数为镍23.5~75.6,硅3.7~12.1,三氧化二铬1.9~11.3,三氧化铬6.3~37.3,铝4.1~24.2,活性炭0~1.2称取粉状反应物料并混合均匀,置于石墨模具中以10~30MPa的压力压制成反应胚体;将装有反应胚体的石墨模具置于反应容器中,用惰性气体吹洗反应容器以排除其中的空气;将胚料加热到150℃~200℃,并在此温度保温1~2小时;再从容器中排除从反应物料表面脱附的气体,通入3~10MPa惰性气体;继续加热到大约250~300℃,通过引燃剂引发反应,引燃剂是由高锰酸盐,镁粉,硫化物组成的混合物,各组分高锰酸盐∶镁粉∶硫化物的质量比为(1.0-2.0)∶(1.5-2.5)∶(1-2.0),引燃剂混合物的重量百分含量占总反应物料的2~10%;反应完成后材料随反应容器冷却至室温。The preparation method of the Ni3Si -based intermetallic compound composite material of the present invention is characterized in that the method comprises: nickel 23.5-75.6, silicon 3.7-12.1, dichromium trioxide 1.9-11.3, chromium trioxide 6.3-37.3 , aluminum 4.1-24.2, activated carbon 0-1.2 Weigh the powdered reaction materials and mix them evenly, place them in a graphite mold and press them into a reaction embryo with a pressure of 10-30MPa; place the graphite mold with the reaction embryo in the reaction vessel In the process, the reaction vessel is purged with an inert gas to remove the air therein; the billet is heated to 150°C-200°C, and kept at this temperature for 1-2 hours; then the gas desorbed from the surface of the reaction material is removed from the vessel, Pass in an inert gas of 3-10MPa; continue heating to about 250-300°C, and initiate the reaction through an igniter. The igniter is a mixture composed of permanganate, magnesium powder, and sulfide. Each component of permanganate : magnesium powder: the mass ratio of sulfide is (1.0-2.0): (1.5-2.5): (1-2.0), and the percentage by weight of igniter mixture accounts for 2~10% of total reaction mass; The material cooled to room temperature with the reaction vessel.

采用以上工艺获得了高纯度,微观组织致密且性能优异的Ni3Si基金属间化合物材料。本发明采用的制备Ni3Si基金属间化合物材料的燃烧合成熔化法与传统的熔炼和热压烧结方法相比,所需外加温度大幅度下降,制备工艺及所需设备简单,制备成本明显降低。该方法制备的材料具有纯度高、组织致密的优点,所得到的材料具有较高强度、较高硬度及良好的抗磨性。本发明制备的材料性能重现性好,所测性能数据离散度不大于10%。The Ni 3 Si-based intermetallic compound material with high purity, compact microstructure and excellent performance was obtained by using the above process. Compared with traditional smelting and hot pressing sintering methods, the combustion synthesis and melting method for preparing Ni 3 Si-based intermetallic compound materials adopted in the present invention requires a large reduction in the required external temperature, simple preparation process and required equipment, and significantly reduced preparation costs . The material prepared by the method has the advantages of high purity and compact structure, and the obtained material has high strength, high hardness and good wear resistance. The performance of the material prepared by the invention has good reproducibility, and the dispersion degree of the measured performance data is not more than 10%.

本发明采用燃烧合成熔化法制备Ni3Si基金属间化合物复合材料,避免了现有技术的不足,设备简便,工艺简单,生产周期短,成本低廉。The invention adopts the combustion synthesis melting method to prepare the Ni3Si -based intermetallic compound composite material, avoids the deficiency of the prior art, has simple equipment, simple process, short production cycle and low cost.

硬度测定条件为,载荷500g,加载持续时间5s。采用三点弯曲试验测定了材料的抗弯强度,试样尺寸为30×3×3mm,跨距为25mm,压头下移速度为0.1mm/min。磨损试验是在球-盘式SRV微动摩擦磨损试验机上进行的,盘为本发明的材料,尺寸为19×19×4mm,对偶为Φ10mm的G Cr15钢球。载荷40N,振幅1mm,频率25Hz,运转时间30分钟。The hardness measurement conditions are as follows: a load of 500 g and a loading duration of 5 s. The flexural strength of the material was measured by a three-point bending test. The sample size was 30×3×3mm, the span was 25mm, and the downward movement speed of the indenter was 0.1mm/min. The wear test is carried out on a ball-disc type SRV fretting friction and wear testing machine. The disc is the material of the present invention, the size is 19×19×4mm, and the pair is a G Cr15 steel ball of Φ10mm. The load is 40N, the amplitude is 1mm, the frequency is 25Hz, and the running time is 30 minutes.

具体实施方式Detailed ways

实施例1:Example 1:

分别称取质量百分数为,镍:62.7,硅:10.0,三氧化二铬:4.3,三氧化铬:14,铝:9.0的粉状反应物料;将反应物料在球磨机中干混10小时;将混合好的物料称取50g在石墨模具中以30MPa压力压制成胚体;同时,称取5g引燃剂,以30MPa压力压制成块;将装有反应胚体及引燃剂块的石墨模具置于反应容器中,用惰性气体吹洗反应容器以排除其中的空气;将胚料加热到200℃,并在此温度保温1小时;然后从容器中排除从反应物料表面脱附的气体,再通入5MPa惰性气体;继续加热到260℃左右,引燃剂在此温度下引发反应;反应完成后材料随反应容器冷却至室温,然后从容器中取出。Weigh the powdered reaction materials with mass percentages of nickel: 62.7, silicon: 10.0, chromium trioxide: 4.3, chromium trioxide: 14, aluminum: 9.0; dry mix the reaction materials in a ball mill for 10 hours; mix the Weigh 50g of a good material and press it into a green body with a pressure of 30MPa in a graphite mold; at the same time, weigh 5g of the igniter and press it into a block with a pressure of 30MPa; place the graphite mold with the reaction green body and igniter block on In the reaction vessel, flush the reaction vessel with an inert gas to remove the air in it; heat the blank to 200°C and keep it at this temperature for 1 hour; then remove the gas desorbed from the surface of the reaction material from the vessel, and then pass it into 5MPa inert gas; continue heating to about 260°C, the igniter initiates the reaction at this temperature; after the reaction is completed, the material is cooled to room temperature with the reaction container, and then taken out from the container.

材料的显微硬度、弯曲强度和磨损率列于表1。The microhardness, flexural strength and wear rate of the materials are listed in Table 1.

表1  Ni3Si-Cr复合材料的硬度、弯曲强度及磨损率 硬度(GPa) 弯曲强度(MPa) 磨损率(10-14m3.N-1.m-1) Ni3Si-Cr复合材料 7.5 897 0.75 Table 1 Hardness, flexural strength and wear rate of Ni 3 Si-Cr composites Hardness (GPa) Bending strength (MPa) Wear rate (10 -14 m 3 .N -1 .m -1 ) Ni 3 Si-Cr composite material 7.5 897 0.75

实施例2:Example 2:

分别称取质量百分数为,镍:62.5,硅:10.0,三氧化二铬:4.3,三氧化铬:14,铝:9.0的粉状反应物料;活性炭:0.2的粉状反应物料;将反应物料在球磨机中干混10小时;将混合好的物料称取50g在石墨模具中以30MPa压力压制成胚体;同时,称取5g引燃剂,以30MPa压力压制成块;将装有反应胚体及引燃剂块的石墨模具置于反应容器中,用惰性气体吹洗反应容器以排除其中的空气;将胚料加热到200℃,并在此温度保温1小时;然后从容器中排除从反应物料表面脱附的气体,再通入5MPa惰性气体;继续加热到260℃左右,引燃剂在此温度下引发反应;反应完成后材料随反应容器冷却至室温,然后从容器中取出。Take by weighing mass percent respectively, nickel: 62.5, silicon: 10.0, dichromium trioxide: 4.3, chromium trioxide: 14, aluminum: the powdery reaction material of 9.0; Activated carbon: the powdery reaction material of 0.2; Dry mix in a ball mill for 10 hours; weigh 50g of the mixed material and press it into a green body in a graphite mold with a pressure of 30MPa; at the same time, weigh 5g of the ignition agent and press it into a block with a pressure of 30MPa; put the reaction green body and The graphite mold of the igniter block is placed in the reaction vessel, and the reaction vessel is purged with an inert gas to remove the air; the billet is heated to 200°C and kept at this temperature for 1 hour; then the reaction material is removed from the vessel The gas desorbed on the surface is then fed with 5MPa inert gas; continue to heat to about 260°C, and the igniter initiates the reaction at this temperature; after the reaction is completed, the material is cooled to room temperature with the reaction container, and then taken out of the container.

材料的显微硬度、弯曲强度和磨损率列于表2。The microhardness, flexural strength and wear rate of the materials are listed in Table 2.

表2  含C的Ni3Si-Cr复合材料的硬度、弯曲强度及磨损率 硬度(GPa) 弯曲强度(MPa) 磨损率(10-14m3.N-1.m-1) 含C的Ni3Si-Cr复合材料 9.8 1010 1.5 Table 2 Hardness, flexural strength and wear rate of Ni 3 Si-Cr composites containing C Hardness (GPa) Bending strength (MPa) Wear rate (10 -14 m 3 .N -1 .m -1 ) Ni 3 Si-Cr Composite Material Containing C 9.8 1010 1.5

Claims (2)

1、一种镍硅基金属间化合物复合材料,其特征在于材料的原料由镍23.5~75.6,硅3.7~12.1,三氧化二铬1.9~11.3,三氧化铬6.3~37.3,铝4.1~24.2,活性炭0~1.2(质量百分数)组成。1. A nickel-silicon-based intermetallic compound composite material, characterized in that the raw materials of the material are nickel 23.5-75.6, silicon 3.7-12.1, dichromium trioxide 1.9-11.3, chromium trioxide 6.3-37.3, aluminum 4.1-24.2, Activated carbon is composed of 0-1.2 (mass percentage). 2、如权利要求1所述材料的制备方法,其特征在于该方法包括:按质量百分数为镍23.5~75.6,硅3.7~12.1,三氧化二铬1.9~11.3,三氧化铬6.3~37.3,铝4.1~24.2,活性炭0~1.2称取粉状反应物料并混合均匀,置于石墨模具中以10~30MPa的压力压制成反应胚体;将装有反应胚体的石墨模具置于反应容器中,用惰性气体吹洗反应容器以排除其中的空气;将胚料加热到150℃~200℃,并在此温度保温1~2小时;再从容器中排除从反应物料表面脱附的气体,通入3~10MPa惰性气体;继续加热到大约250~300℃,通过引燃剂引发反应,引燃剂是由高锰酸盐,镁粉,硫化物组成的混合物,各组分高锰酸盐∶镁粉∶硫化物的质量比为(1.0-2.0)∶(1.5-2.5)∶(1-2.0),引燃剂混合物的重量百分含量占总反应物料的2~10%;反应完成后材料随反应容器冷却至室温。2. The preparation method of the material according to claim 1, characterized in that the method comprises: nickel 23.5-75.6, silicon 3.7-12.1, dichromium trioxide 1.9-11.3, chromium trioxide 6.3-37.3, aluminum 4.1 to 24.2, activated carbon 0 to 1.2 Weigh the powdered reaction materials and mix them evenly, place them in a graphite mold and press them into a reaction embryo with a pressure of 10 to 30 MPa; place the graphite mold with the reaction embryo in the reaction container, Purge the reaction container with an inert gas to remove the air; heat the billet to 150 ° C ~ 200 ° C, and keep it at this temperature for 1 ~ 2 hours; then remove the gas desorbed from the surface of the reaction material from the container, and feed 3 ~ 10MPa inert gas; continue to heat to about 250 ~ 300 ° C, and initiate the reaction through the igniter. The igniter is a mixture composed of permanganate, magnesium powder, and sulfide. The components of permanganate: magnesium Powder: the mass ratio of sulfide is (1.0-2.0): (1.5-2.5): (1-2.0), and the weight percentage composition of igniter mixture accounts for 2~10% of total reaction material; The reaction vessel was cooled to room temperature.
CN 200310103787 2003-10-30 2003-10-30 Nickel-silicon base intermetallic compound composite material and its preparing method Pending CN1611623A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101812622B (en) * 2010-02-08 2011-07-20 吉林大学 Ceramic-intermetallic compound composite material containing binder and preparation method thereof
CN103459019A (en) * 2011-03-14 2013-12-18 公立大学法人大阪府立大学 Hydrogen production catalyst containing Ni3Si-based intermetallic compound, method for activating the catalyst, method and device for hydrogen production using the catalyst
CN103726045A (en) * 2012-10-15 2014-04-16 中国科学院兰州化学物理研究所 Nickel and silicon intermetallic compound based composite coat making method

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101812622B (en) * 2010-02-08 2011-07-20 吉林大学 Ceramic-intermetallic compound composite material containing binder and preparation method thereof
CN103459019A (en) * 2011-03-14 2013-12-18 公立大学法人大阪府立大学 Hydrogen production catalyst containing Ni3Si-based intermetallic compound, method for activating the catalyst, method and device for hydrogen production using the catalyst
CN103459019B (en) * 2011-03-14 2016-04-27 公立大学法人大阪府立大学 Containing Ni 3the catalyst for preparing hydrogen of Si base intermetallic compound, activate the method for this catalyst and the method and apparatus with this catalyst hydrogen manufacturing
CN103726045A (en) * 2012-10-15 2014-04-16 中国科学院兰州化学物理研究所 Nickel and silicon intermetallic compound based composite coat making method

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