CN111485160B - High-wear-resistance dual-phase metal compound and preparation method thereof - Google Patents

High-wear-resistance dual-phase metal compound and preparation method thereof Download PDF

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CN111485160B
CN111485160B CN202010555214.0A CN202010555214A CN111485160B CN 111485160 B CN111485160 B CN 111485160B CN 202010555214 A CN202010555214 A CN 202010555214A CN 111485160 B CN111485160 B CN 111485160B
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CN111485160A (en
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刘瑞
李小燕
丁海燕
王志新
马明星
胡领学
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Henan Zhongke Intelligent Equipment Co ltd
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract

一种高耐磨双相金属化合物及其制备方法，属于无机金属化合物制备领域，其分子式为AlxCeyCuFeNiMnpOqZr，其中0.1≤x≤1.3；0.1≤y≤1；0.1≤p≤1.3；0.1≤q≤0.5；0.02≤x/(x+y+p+q+4)<0.25；0.01≤y/(x+y+p+q+4)<0.18；0.02≤p/(x+y+p+q+4)<0.25；0.01≤q/(x+y+p+q+4)<0.10。具体步骤为：按化学式称取所需原料置于球磨罐中，加入不锈钢球，保护气体环境下将球磨罐密封；行星式球磨机上混料；将混料后的粉末装入石墨模具，放电等离子烧结炉中温压成块；将块体置于真空熔炼炉进行熔炼，真空吸铸进水冷铜模中，取出样品，即得目标化合物。本发明金属化合物是由两种简单立方相构成的双相固溶体结构；双相比例可根据性能需求进行调控；所制备合金具有高致密度、高硬度和高耐磨性；成分均匀性好。

Figure 202010555214

A high wear-resistant dual-phase metal compound and a preparation method thereof belong to the field of preparation of inorganic metal compounds, and the molecular formula is AlxCeyCuFeNiMnpOqZr , wherein 0.1≤x≤1.3 ; 0.1≤y≤1 ; 0.1≤p ≤1.3; 0.1≤q≤0.5; 0.02≤x/(x+y+p+q+4)<0.25;0.01≤y/(x+y+p+q+4)<0.18; 0.02≤p/( x+y+p+q+4)<0.25;0.01≤q/(x+y+p+q+4)<0.10. The specific steps are: weighing the required raw materials according to the chemical formula and placing them in a ball mill jar, adding stainless steel balls, and sealing the ball mill jar in a protective gas environment; mixing materials on a planetary ball mill; loading the mixed powder into a graphite mold, discharging plasma The sintering furnace is warmly pressed into blocks; the blocks are placed in a vacuum smelting furnace for smelting, vacuum suction cast into a water-cooled copper mold, and the sample is taken out to obtain the target compound. The metal compound of the invention is a dual-phase solid solution structure composed of two simple cubic phases; the ratio of the dual phases can be adjusted according to performance requirements; the prepared alloy has high density, high hardness and high wear resistance; and the composition uniformity is good.

Figure 202010555214

Description

High-wear-resistance dual-phase metal compound and preparation method thereof
Technical Field
The invention belongs to the field of preparation of inorganic metal compounds, and particularly relates to a high-wear-resistance two-phase metal compound AlxCeyCuFeNiMnpOqZr and a preparation method thereof.
Background
The metal compound (or called inorganic metal compound) is formed by combining a plurality of elements in the compound according to a certain stoichiometric ratio, the crystal structure of the formed metal compound is completely different from the crystal structure types of the constituent elements, the crystal structure of the metal compound is generally complex, the typical characteristic is that the crystal structure type of the metal compound is different from that of any constituent element, and the composition can be represented by a chemical formula rather than a composition. Metal compounds are important constituent phases of many alloys. The presence of metal compounds in conventional alloys generally increases the hardness and wear resistance of the alloy, but decreases the ductility and toughness. At the beginning of the 20 th century, the Ye project group and the Cantor project group in taiwan in the united kingdom each independently reported a novel multi-principal-element high-entropy alloy, which is significantly different from the conventional theory that hard and brittle intermetallic compounds are formed. Although the reported novel multi-principal element high-entropy alloys tend to form simple crystal structures, such as: face Centered Cubic (FCC), Body Centered Cubic (BCC), Hexagonal Close Packed (HCP), Simple Cubic (SC), etc.; but is distinguished from the space group or lattice constant of the Face Centered Cubic (FCC) metals (e.g., aluminum, copper, gold, silver, nickel, etc.), the Body Centered Cubic (BCC) metals (e.g., potassium, molybdenum, tungsten, etc.), the Hexagonal Close Packed (HCP) metals (e.g., magnesium, zinc, beryllium, etc.), the Simple Cubic (SC) metals (e.g., polonium is the only element with a simple cubic structure), and the distinction is made between the types of conventional alloys, i.e., between aluminum and copper belonging to the face centered cubic phase structure, and the distinction is made based on the crystal structure and the lattice constant of the conventional alloys and the high entropy alloy types. Formally based on the design concept of the novel metal compound, a small amount of non-metal elements are introduced to modify the metal compound, and the high-wear-resistance two-phase Al is designed and preparedxCeyCuFeNiMnpOqA Zr metal compound. The invention relates to high-wear-resistance biphase AlxCeyCuFeNiMnpOqThe Zr metal compound belongs to the invention patent of the compound with a typical novel crystal structure, but not the composition invention patent, and improves the hardness and the strength at the same timePlasticity and toughness. Therefore, the novel high-wear-resistance dual-phase metal compound with strong hardness and plasticity and toughness is designed and prepared, and has important practical significance and market prospect.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-wear-resistance two-phase metal compound AlxCeyCuFeNiMnpOqZr and a preparation method thereof.
Al provided by the inventionxCeyCuFeNiMnpOqThe multi-principal-element alloy prepared by the vacuum melting method is a two-phase metal compound structure consisting of two simple cubic phases (SC1 and SC2), and the molecular formula of the multi-principal-element alloy is AlxCeyCuFeNiMnpOqZr; the two-phase proportion can be regulated and controlled according to the performance requirement; the prepared alloy has high density, high hardness and high wear resistance.
The technical scheme for realizing the invention is as follows: al (Al)xCeyCuFeNiMnpOqThe preparation method of the Zr metal compound is characterized by comprising the following specific steps:
(1) according to the chemical formula AlxCeyCuFeNiMnpOqZr, wherein x is more than or equal to 0.1 and less than or equal to 1.3; y is more than or equal to 0.1 and less than or equal to 1; p is more than or equal to 0.1 and less than or equal to 1.3; q is more than or equal to 0.1 and less than or equal to 0.5; 0.02 ≤ x/(x + y + p + q +4)<0.25；0.01≤y/(x+y+p+q+4)<0.18；0.02≤p/(x+y+p+q+4)<0.25；0.01≤q/(x+y+p+q+4)<0.10; respectively weighing the required pure metal powder and adding a proper amount of cerium dioxide according to the proportion of oxygen elements; placing the raw material powder into a ball milling tank, adding a stainless steel ball, and sealing the ball milling tank under a protective gas environment;
(2) placing the ball milling tank sealed in the step (1) on a planetary ball mill for mixing;
(3) putting the fully mixed powder in the step (2) into a graphite die, and pressing the fully mixed powder into a block at 600 ℃ and 35MPa in a discharge plasma sintering furnace;
(4) putting the block in the step (3) into a vacuum smelting furnace, and when the vacuum degree reaches 1 multiplied by 10-3After Pa, argon is filled in, andvacuumizing, repeatedly vacuumizing and filling argon for 3 times, then starting to smelt, repeatedly smelting for 3 times to ensure the uniformity of the material, carrying out vacuum suction casting in a water-cooled copper mold, and taking out a sample to obtain the target compound.
In the step (1), the purity of the metal powder is higher than 99.5%, and the purity of the cerium dioxide is higher than 99.9%.
And (2) the protective gas in the step (1) is argon or nitrogen.
And (3) mixing in the step (2) at the rotating speed of 30-100 rpm for 0.5-6 h.
The smelting process parameters in the step (4) are as follows: the current is 250-400A, and the action time is 30-120 s.
The invention has the beneficial effects that: the metal compound prepared by the method has the same proportioning components with the metal elements of the raw materials, and the phase structure of the metal compound is a two-phase metal compound structure consisting of two simple cubic phases; the two-phase proportion can be regulated and controlled according to the performance requirement; the prepared metal compound has high density, high hardness and high wear resistance; low cost and wide application range.
Drawings
FIG. 1 shows a high wear-resistant two-phase metal compound Al provided by the inventionxCeyCuFeNiMnpOqA process flow diagram of a preparation method of Zr;
FIG. 2 is an X-ray diffraction pattern of the metal compound prepared in example 1.
Detailed Description
The technical solution of the present invention is not limited to the specific embodiments listed below, and includes any combination of the specific embodiments.
Example 1
According to the chemical formula of AlCo0.1CuFeNiMnO0.1Respectively weighing 0.40mol of aluminum powder, copper powder, iron powder, nickel powder, manganese powder and zirconium powder, 0.02mol of cerium powder and 0.02mol of cerium dioxide by using Zr, wherein the purity of each metal powder is higher than 99.5 percent, and the purity of the cerium dioxide is higher than 99.9 percent; placing the raw material powder into a ball milling tank, adding a stainless steel ball, and then sealing the ball milling tank under an argon environment; placing the sealed ball milling tank in a planetary ballMixing materials on a mill at the rotating speed of 30rpm for 6 hours; putting the fully mixed powder into a graphite die, and pressing the fully mixed powder into a block at 600 ℃ and 35MPa in a discharge plasma sintering furnace; placing the block in a vacuum melting furnace, and when the vacuum degree reaches 1 × 10-3And Pa, introducing argon, vacuumizing again, repeatedly vacuumizing and introducing argon for 3 times, then starting smelting, wherein the current is 400A, the action time is 30s, repeatedly smelting for 3 times to ensure the uniformity of the material, performing vacuum suction casting in a water-cooling copper mold, and taking out a sample to obtain the target compound.
Example 2
Is represented by the chemical formula Al1.3Ce0.1CuFeNiMn0.1O0.1Respectively weighing 0.52mol of aluminum powder, 0.40mol of copper powder, iron powder, nickel powder and zirconium powder, 0.02mol of cerium dioxide and 0.04mol of manganese powder by using Zr, wherein the purity of each metal powder is higher than 99.5 percent, and the purity of the cerium dioxide is higher than 99.9 percent; placing the raw material powder into a ball milling tank, adding a stainless steel ball, and then sealing the ball milling tank under an argon environment; placing the sealed ball milling tank on a planetary ball mill for mixing materials, wherein the rotating speed is 50rpm, and the time is 3 hours; putting the fully mixed powder into a graphite die, and pressing the fully mixed powder into a block at 600 ℃ and 35MPa in a discharge plasma sintering furnace; placing the block in a vacuum melting furnace, and when the vacuum degree reaches 1 × 10-3And Pa, introducing argon, vacuumizing again, repeatedly vacuumizing and introducing argon for 3 times, then starting smelting, wherein the current is 350A, the action time is 60s, repeatedly smelting for 3 times to ensure the uniformity of the material, performing vacuum suction casting in a water-cooling copper mold, and taking out a sample to obtain the target compound.
Example 3
Is represented by the chemical formula Al0.1Ce0.1CuFeNiMn1.3O0.1Respectively weighing 0.04mol of aluminum powder, 0.40mol of copper powder, iron powder, nickel powder and zirconium powder, 0.02mol of cerium dioxide and 0.52mol of manganese powder by using Zr, wherein the purity of each metal powder is higher than 99.5 percent, and the purity of the cerium dioxide is higher than 99.9 percent; placing the raw material powder into a ball milling tank, adding a stainless steel ball, and then sealing the ball milling tank under an argon environment; ball milling the sealed ballThe pot is placed on a planetary ball mill for mixing materials, the rotating speed is 100rpm, and the time is 0.5 h; putting the fully mixed powder into a graphite die, and pressing the fully mixed powder into a block at 600 ℃ and 35MPa in a discharge plasma sintering furnace; placing the block in a vacuum melting furnace, and when the vacuum degree reaches 1 × 10-3And Pa, introducing argon, vacuumizing again, repeatedly vacuumizing and introducing argon for 3 times, then starting smelting, wherein the current is 250A, the action time is 120s, repeatedly smelting for 3 times to ensure the uniformity of the material, performing vacuum suction casting in a water-cooling copper mold, and taking out a sample to obtain the target compound.
Example 4
Is represented by the chemical formula Al0.5CeCuFeNiMn0.5O0.1Respectively weighing 0.20mol of aluminum powder and manganese powder, 0.40mol of copper powder, iron powder, nickel powder and zirconium powder, 0.38mol of cerium powder and 0.02mol of cerium dioxide by using Zr, wherein the purity of each metal powder is higher than 99.5 percent, and the purity of the cerium dioxide is higher than 99.9 percent; placing the raw material powder into a ball milling tank, adding a stainless steel ball, and sealing the ball milling tank in a nitrogen environment; placing the sealed ball milling tank on a planetary ball mill for mixing materials, wherein the rotating speed is 100rpm, and the time is 0.5 h; putting the fully mixed powder into a graphite die, and pressing the fully mixed powder into a block at 600 ℃ and 35MPa in a discharge plasma sintering furnace; placing the block in a vacuum melting furnace, and when the vacuum degree reaches 1 × 10-3And Pa, introducing argon, vacuumizing again, repeatedly vacuumizing and introducing argon for 3 times, then starting smelting, wherein the current is 250A, the action time is 120s, repeatedly smelting for 3 times to ensure the uniformity of the material, performing vacuum suction casting in a water-cooling copper mold, and taking out a sample to obtain the target compound.
Example 5
Is represented by the chemical formula Al0.5Ce0.3CuFeNiMn0.5O0.5Respectively weighing 0.20mol of aluminum powder and manganese powder, 0.40mol of copper powder, iron powder, nickel powder and zirconium powder, 0.02mol of cerium powder and 0.10mol of cerium dioxide by using Zr, wherein the purity of each metal powder is higher than 99.5 percent, and the purity of the cerium dioxide is higher than 99.9 percent; placing the raw material powder into a ball milling tank, adding a stainless steel ball, and sealing the ball milling tank in a nitrogen environment; placing the sealed ball milling tankMixing materials on a planetary ball mill at the rotating speed of 50rpm for 3 hours; putting the fully mixed powder into a graphite die, and pressing the fully mixed powder into a block at 600 ℃ and 35MPa in a discharge plasma sintering furnace; placing the block in a vacuum melting furnace, and when the vacuum degree reaches 1 × 10-3And Pa, introducing argon, vacuumizing again, repeatedly vacuumizing and introducing argon for 3 times, then starting smelting, wherein the current is 350A, the action time is 60s, repeatedly smelting for 3 times to ensure the uniformity of the material, performing vacuum suction casting in a water-cooling copper mold, and taking out a sample to obtain the target compound.

Claims (5)

1.一种高耐磨双相金属化合物的制备方法，所述化合物的分子式为AlxCeyCuFeNiMnpOqZr，且其是由两种简单立方相构成的双相金属化合物结构，包括具体步骤如下：1. a preparation method of a high wear-resistant dual-phase metal compound, the molecular formula of the compound is AlxCeyCuFeNiMnpOqZr , and it is a dual-phase metal compound structure composed of two simple cubic phases, including specific Proceed as follows: 步骤(1)：按化学式AlxCeyCuFeNiMnpOqZr，其中0.1≤x≤1.3；0.1≤y≤1；0.1≤p≤1.3；0.1≤q≤0.5；0.02≤x/(x+y+p+q+4)<0.25；0.01≤y/(x+y+p+q+4)<0.18；0.02≤p/(x+y+p+q+4)<0.25；0.01≤q/(x+y+p+q+4)<0.10；分别称取所需的纯金属粉末和按氧元素比例加入适量的二氧化铈；并将原料粉末置于球磨罐中，加入不锈钢球，然后在保护气体环境下将球磨罐密封起来；Step (1): according to the chemical formula Al x Cey CuFeNiMn p O q Zr, wherein 0.1≤x≤1.3; 0.1≤y≤1; 0.1≤p≤1.3; 0.1≤q≤0.5; 0.02≤x/(x+y +p+q+4)<0.25;0.01≤y/(x+y+p+q+4)<0.18;0.02≤p/(x+y+p+q+4)<0.25; 0.01≤q/ (x+y+p+q+4)<0.10; respectively weigh the required pure metal powder and add an appropriate amount of cerium dioxide according to the proportion of oxygen elements; put the raw powder in a ball mill, add stainless steel balls, and then Seal the ball mill tank in a protective gas environment; 步骤(2)：将步骤(1)密封好的球磨罐置于行星式球磨机上进行混料；Step (2): the ball mill jar sealed in step (1) is placed on the planetary ball mill and mixed; 步骤(3)：将步骤(2)充分混料后的粉末装入石墨模具中，在放电等离子烧结炉中600℃、35MPa下温压成块体；Step (3): Load the fully mixed powder in step (2) into a graphite mold, and warmly press it into a block in a spark plasma sintering furnace at 600° C. and 35 MPa; 步骤(4)：将步骤(3)中的块体置于真空熔炼炉中，当真空度达到1×10-3Pa后，充入氩气后，再次抽真空，反复抽真空和充氩气3次后，开始熔炼，为保证材料均匀性，反复熔炼3次，真空吸铸进水冷铜模中，取出样品，即得目标化合物。Step (4): place the block in step (3) in a vacuum melting furnace, when the degree of vacuum reaches 1×10 -3 Pa, fill with argon, then vacuum again, repeat vacuuming and filling with argon After 3 times, the smelting is started. In order to ensure the uniformity of the material, the smelting is repeated 3 times, and the vacuum suction is cast into a water-cooled copper mold, and the sample is taken out to obtain the target compound. 2.如权利要求1所述的高耐磨双相金属化合物的制备方法，其特征在于：所述步骤(1)中金属粉末的纯度高于99.5％，二氧化铈纯度高于99.9％。2 . The method for preparing a high wear-resistant dual-phase metal compound according to claim 1 , wherein in the step (1), the purity of the metal powder is higher than 99.5%, and the purity of ceria is higher than 99.9%. 3 . 3.如权利要求1所述的高耐磨双相金属化合物的制备方法，其特征在于：所述步骤(1)中保护气体为氩气或氮气。3 . The method for preparing a high wear-resistant dual-phase metal compound according to claim 1 , wherein the protective gas in the step (1) is argon or nitrogen. 4 . 4.如权利要求1所述的高耐磨双相金属化合物的制备方法，其特征在于：所述步骤(2)中混料的转速为30～100rpm，时间为0.5-6h。4 . The method for preparing a high wear-resistant dual-phase metal compound according to claim 1 , wherein in the step (2), the mixing speed is 30-100 rpm, and the time is 0.5-6 h. 5 . 5.如权利要求1所述的高耐磨双相金属化合物的制备方法，其特征在于：所述步骤(4)中熔炼工艺参数：电流为250～400A，作用时间30～120s。5 . The method for preparing a high wear-resistant dual-phase metal compound according to claim 1 , wherein the smelting process parameters in the step (4): the current is 250-400A, and the action time is 30-120s. 6 .
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