Al-Cu-Fe-La quaternary quasicrystal alloy powder and preparation method thereof

Abstract

The invention relates to a preparation method of Al-Cu-Fe-La quaternary quasicrystal alloy powder. The expression of the quaternary quasicrystal alloy powder is (Al63Cu25Fe12) 100-xLax (x is equal to 0-1.0 at%). Pure aluminum (99.9 wt%), pure copper (99.9 wt%), an Al-60% Fe intermediate alloy and an Al-80% La intermediate alloy are adopted as raw materials for burdening, an Al-Cu-Fe-La quaternary quasicrystal as-cast alloy is prepared through a vacuum arc melting furnace, the prepared as-cast alloy is subjected to mechanical crushing, grinding and ball milling treatment, and quaternary quasicrystal alloy powder is obtained. The Al-Cu-Fe-La quaternary quasicrystal powder prepared through the method is high in quasicrystal phase forming amount, small in powder granularity and high in hardness. When the composite material is added into a base material as reinforcing particles, the strength and ductility of the composite material can be remarkably improved.

Description

Technical Field

[0001] The invention relates to the field of new alloy materials, in particular to an Al-Cu-Fe-La quasi-crystal alloy powder and a preparation method thereof. Background Art

[0002] Al-Cu-Fe ternary alloy quasicrystal material has the characteristics of high hardness, high strength, low surface energy, high elastic modulus and good thermodynamic stability. Its hardness is 600-900HV and its compressive strength can reach more than 700MPa. In view of these excellent properties, quasicrystal alloys are widely used as the reinforcement phase of metal matrix composites.

[0003] However, the Al-Cu-Fe ternary alloy quasicrystal material itself has the problem of high brittleness and difficulty in processing and forming. More importantly, at high temperatures, the quasicrystal phase of the ternary alloy undergoes a phase transition due to poor thermal stability, which in turn affects the performance of the quasicrystal alloy under high temperature conditions, which seriously restricts the basic research and industrial application of quasicrystal alloy materials.

[0004] At present, the methods for preparing Al-Cu-Fe quasicrystal powder mainly include plasma method, mechanical alloying method and vacuum gas atomization method. However, these methods have the disadvantages of complicated preparation process, huge energy consumption and high cost, and are not suitable for small batch production, which also seriously restricts the research and application of quasicrystal alloy materials in particle reinforced composite materials. Summary of the invention

[0005] In order to overcome the shortcomings of the above-mentioned prior art, the purpose of the present invention is to provide an Al-Cu-Fe-La quasi-crystalline alloy powder and a preparation method thereof, so as to solve the technical problems of poor thermal stability of existing quasi-crystalline alloys and complex powder preparation process.

[0006] The technical solution adopted by the present invention is as follows:

[0007] An Al-Cu-Fe-La quaternary quasi-crystal alloy powder,

[0008] The expression of the quaternary quasi-crystal alloy powder is (Al 63 Cu 25 Fe 12 ) 100-X La × ; Wherein, x = 0 ~ 1.0at%.

[0009] In another aspect, the present invention provides a method for preparing Al-Cu-Fe-La quasi-crystalline alloy powder.

[0010] The method comprises the following steps:

[0011] Step 1: Ingredients

[0012] According to the expression (Al 63 Cu 25 Fe 12 ) 100-X La × (x=0~1.0at%), 80g of each material is prepared, and pure aluminum (99.9wt%), pure copper (99.9wt%), Al-60%Fe and Al-80%La intermediate alloys are used as raw materials for preparation.

[0013] Step 2: Smelting

[0014] The Al-Cu-Fe-La quaternary quasi-crystalline alloy was prepared by vacuum arc melting furnace. The vacuum arc melting process parameters were as follows: melting current 500A, stirring current and voltage 30A and 5V respectively to prepare the cast quasi-crystalline alloy, and then the obtained sample was turned over and remelted four times to improve the uniformity of the alloy composition. After the melting was completed, air cooling was carried out to obtain the cast quasi-crystalline alloy.

[0015] Step 3: Crushing and Grinding

[0016] The obtained cast quasicrystalline alloy was mechanically crushed and ground. The grinding was performed using a planetary ball mill, the grinding ball particle size ratio was 3mm:5mm:8mm=5:3:2, and the ball-to-material ratio was 1:1. The ball mill was paused for 15 minutes after every 30 minutes of operation, and the forward and reverse directions were alternately operated. The total ball milling time was 3 hours, and the ball milling speed was 650r / min.

[0017] Step 4: Sieving

[0018] After the above grinding and screening, the cast quasicrystalline alloy powder with a particle size of 38-75 μm can be obtained.

[0019] Furthermore, the ball milling is performed under argon protection.

[0020] The cast quasi-crystalline alloy powder of the present invention is proved by X-ray diffraction technology that the alloy composition is composed of monoclinic structure λ-Al 13 Fe4 phase, τ-AlCu phase and quasicrystal I-Al 65 Cu 20 Fe 15 Phase composition, when adding 0, 0.25, 0.5, 0.75 and 1.0at% lanthanum quasicrystal alloy, the formation amount of quasicrystal phase is 34.98%, 24.79%, 45.68%, 26.72% and 35.8% respectively. Transmission electron microscopy observation found that the prepared powder has five-fold, three-fold and two-fold rotational symmetry diffraction rotation patterns; the Vickers hardness of the bulk quasicrystal is 650-900HV 0.3 .

[0021] Compared with the prior art, the present invention has the following significant beneficial effects:

[0022] 1. Improving the quasi-crystalline phase forming ability and thermal stability: The Al-Cu-Fe-La quasi-crystalline alloy powder provided in this application has a reasonable composition design, which can effectively improve the quasi-crystalline phase forming ability and thermal stability. It is not easy to transform from the quasi-crystalline phase to the quasi-crystalline-like phase at high temperature, and is particularly suitable for rapid solidification surface strengthening application fields such as laser cladding and plasma spraying.

[0023] 2. Refine the alloy structure: By adding an appropriate amount of rare earth lanthanum, the addition of lanthanum causes the components to be supercooled, making the alloy structure fine and evenly distributed.

[0024] 3. Improve the hardness and elastic modulus of the alloy: Due to the rapid cooling rate of the melt under the action of water cooling during the vacuum melting process, the nucleation of the quasicrystal phase is further accelerated, the alloy grain size is further reduced, the grain boundary area is significantly increased, the dislocation movement is hindered, the hardness and elastic modulus of the alloy are improved, and the mechanical strength of the prepared quasicrystal coating is enhanced. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 : XRD diffraction patterns of the Al-Cu-Fe-La quasi-crystalline alloy powders prepared in Examples 1-5.

[0026] Figure 2 : Microhardness distribution diagram of the Al-Cu-Fe-La quasicrystalline cast alloy prepared in Examples 1-5.

[0027] Figure 3 : Volume fraction diagram of quasicrystalline phase formation amount of Al-Cu-Fe-La quasicrystalline cast alloy prepared in Examples 1-5.

[0028] Figure 4 : SEM image of Al-Cu-Fe ternary quasi-crystal alloy powder prepared in Example 1. Wherein: a-overall morphology; b-cross-sectional morphology;

[0029] Figure 5 : SEM image of Al-Cu-Fe-La quasi-crystalline alloy powder prepared in Example 5. Wherein: a-overall morphology; b-cross-sectional morphology. DETAILED DESCRIPTION

[0030] The present invention will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall within the scope limited by the appended claims of the application equally.

[0031] The following examples use conventional instruments and equipment in the art. The experimental methods in the following examples without specifying specific conditions are usually carried out under conventional conditions or under conditions recommended by the manufacturer. The various raw materials used in the following examples, unless otherwise specified, are conventional commercial products, and their specifications are conventional specifications in the art.

[0032] Example 1

[0033] An Al-Cu-Fe-La quaternary quasi-crystal alloy powder and a preparation method thereof, comprising the following steps:

[0034] S1. Determine the alloy powder expression: The expression of the quaternary quasi-crystal alloy powder is (Al 63 Cu 25 Fe 12 ) 100- X La × ; Wherein, x = 0at%.

[0035] S2. Ingredients and smelting: According to the expression Al 63 Cu 25 Fe 12 80g of ingredients were used to prepare Al-Cu-Fe ternary quasi-crystalline alloy in a vacuum arc melting furnace to obtain a cast quasi-crystalline alloy. The vacuum arc melting process parameters were: melting current 500A, stirring current and voltage 30A and 5V respectively, the obtained sample was turned over and remelted four times, and air-cooled after melting.

[0036] S3. Crushing and grinding: The obtained ternary quasicrystal alloy is crushed and ground. In order to make the shape of the quasicrystal alloy particles roughly the same, the quasicrystal powder is further ground using a planetary ball mill. The grinding ball particle size ratio is 3mm:5mm:8mm=5:3:2, the ball-to-material ratio is 1:1, and the ball mill is paused for 15 minutes after every 30 minutes of operation, and the forward and reverse directions are alternately operated. The total ball milling time is 3 hours, and the ball milling speed is 650r / min.

[0037] S4. Screening: After screening, the ternary quasi-crystalline alloy powder with a particle size of 38-75 μm can be obtained.

[0038] Example 2

[0039] An Al-Cu-Fe-La quaternary quasi-crystal alloy powder and a preparation method thereof, comprising the following steps:

[0040] S1. Determine the alloy powder expression: The expression of the quaternary quasi-crystal alloy powder is (Al 63 Cu 25 Fe 12 ) 100- X La ×; wherein x = 0.25 at%.

[0041] S2. Ingredients and smelting: According to the expression (Al 63 Cu 25 Fe 12 ) 99.75 La 0.25 80g of ingredients were used to prepare Al-Cu-Fe-La quaternary quasi-crystalline alloy in a vacuum arc melting furnace to obtain a cast quasi-crystalline alloy. The vacuum arc melting process parameters were: melting current 500A, stirring current and voltage 30A and 5V respectively, the obtained sample was turned over and remelted four times, and air-cooled after melting.

[0042] S3. Crushing and grinding: The obtained quaternary quasi-crystal alloy is crushed and ground. In order to make the shape of the quasi-crystal alloy particles roughly the same, the quasi-crystal powder is further ground using a planetary ball mill. The grinding ball particle size ratio is 3mm:5mm:8mm=5:3:2, the ball-to-material ratio is 1:1, and the ball mill is paused for 15 minutes after every 30 minutes of operation, and the forward and reverse directions are alternately operated. The total ball milling time is 3 hours, and the ball milling speed is 650r / min.

[0043] S4. Screening: After screening, quaternary quasi-crystalline alloy powder with a particle size of 38-75 μm can be obtained.

[0044] Example 3

[0045] An Al-Cu-Fe-La quaternary quasi-crystal alloy powder and a preparation method thereof, comprising the following steps:

[0046] S1. Determine the alloy powder expression: The expression of the quaternary quasi-crystal alloy powder is (Al 63 Cu 25 Fe 12 ) 100- X La × ; wherein x = 0.5 at%.

[0047] S2. Ingredients and smelting: According to the expression (Al 63 Cu 25 Fe 12 ) 99.5 La 0.5 80g of ingredients were used to prepare Al-Cu-Fe-La quaternary quasi-crystalline alloy in a vacuum arc melting furnace to obtain a cast quasi-crystalline alloy. The vacuum arc melting process parameters were: melting current 500A, stirring current and voltage 30A and 5V respectively, the obtained sample was turned over and remelted four times, and air-cooled after melting.

[0048] S3. Crushing and grinding: The obtained quaternary quasi-crystal alloy is crushed and ground. In order to make the shape of the quasi-crystal alloy particles roughly the same, the quasi-crystal powder is further ground using a planetary ball mill. The grinding ball particle size ratio is 3mm:5mm:8mm=5:3:2, the ball-to-material ratio is 1:1, and the ball mill is paused for 15 minutes after every 30 minutes of operation, and the forward and reverse directions are alternately operated. The total ball milling time is 3 hours, and the ball milling speed is 650r / min.

[0049] S4. Screening: After screening, quaternary quasi-crystalline alloy powder with a particle size of 38-75 μm can be obtained.

[0050] Depend on Figure 2 It can be seen that the microhardness value of the Al-Cu-Fe-La quasi-crystalline cast alloy prepared in this embodiment is the highest, reaching 814.16±65.69 HV 0.3 Depend on Figure 3 It can be seen that the quasi-crystal phase formation amount of the Al-Cu-Fe-La quasi-crystal cast alloy prepared in this embodiment reaches 45.68%.

[0051] Example 4

[0052] An Al-Cu-Fe-La quaternary quasi-crystal alloy powder and a preparation method thereof, comprising the following steps:

[0053] S1. Determine the alloy powder expression: The expression of the quaternary quasi-crystal alloy powder is (Al 63 Cu 25 Fe 12 ) 100- X La × ; wherein x = 0.75 at%.

[0054] S2. Ingredients and smelting: According to the expression (Al 63 Cu 25 Fe 12 ) 99.25 La 0.75 80g of ingredients were used to prepare Al-Cu-Fe-La quaternary quasi-crystalline alloy in a vacuum arc melting furnace to obtain a cast quasi-crystalline alloy. The vacuum arc melting process parameters were: melting current 500A, stirring current and voltage 30A and 5V respectively, the obtained sample was turned over and remelted four times, and air-cooled after melting.

[0055] S3. Crushing and grinding: The obtained quaternary quasi-crystal alloy is crushed and ground. In order to make the shape of the quasi-crystal alloy particles roughly the same, the quasi-crystal powder is further ground using a planetary ball mill. The grinding ball particle size ratio is 3mm:5mm:8mm=5:3:2, the ball-to-material ratio is 1:1, and the ball mill is paused for 15 minutes after every 30 minutes of operation, and the forward and reverse directions are alternately operated. The total ball milling time is 3 hours, and the ball milling speed is 650r / min.

[0056] S4. Screening: After screening, quaternary quasi-crystalline alloy powder with a particle size of 38-75 μm can be obtained.

[0057] Example 5

[0058] An Al-Cu-Fe-La quaternary quasi-crystal alloy powder and a preparation method thereof, comprising the following steps:

[0059] S1. Determine the alloy powder expression: The expression of the quaternary quasi-crystal alloy powder is (Al 63 Cu 25 Fe 12 ) 100- X La × ; Wherein, x = 1at%.

[0060] S2. Ingredients and smelting: According to the expression (Al 63 Cu 25 Fe 12 ) 99 La1 was prepared with 80g of ingredients, and Al-Cu-Fe-La quaternary quasi-crystalline alloy was prepared in a vacuum arc melting furnace to obtain a cast quasi-crystalline alloy. The vacuum arc melting process parameters were: melting current 500A, stirring current and voltage 30A and 5V respectively, and the obtained sample was turned over and remelted four times, and air-cooled after melting.

[0061] S3. Crushing and grinding: The obtained quaternary quasi-crystal alloy is crushed and ground. In order to make the shape of the quasi-crystal alloy particles roughly the same, the quasi-crystal powder is further ground using a planetary ball mill. The grinding ball particle size ratio is 3mm:5mm:8mm=5:3:2, the ball-to-material ratio is 1:1, and the ball mill is paused for 15 minutes after every 30 minutes of operation, and the forward and reverse directions are alternately operated. The total ball milling time is 3 hours, and the ball milling speed is 650r / min.

[0062] S4. Screening: After screening, quaternary quasi-crystalline alloy powder with a particle size of 38-75 μm can be obtained.

[0063] like Figure 1As shown, the Al-Cu-Fe-La quaternary quasicrystalline alloy powders prepared in Examples 1-5 all have quasicrystalline phases generated. The present invention significantly improves the quasicrystalline-forming ability and thermal stability of the Al-Cu-Fe ternary alloy by adding the rare earth element lanthanum, making the alloy less likely to undergo phase change at high temperatures, thereby maintaining excellent performance.

[0064] The preparation method of the present invention has simple process, low energy consumption and low cost, is particularly suitable for small batch production, and is conducive to promoting the research and application of quasicrystal alloy materials in particle-reinforced composite materials and surface strengthening technology.

[0065] The prepared Al-Cu-Fe-La quaternary quasicrystalline alloy powder has a high quasicrystalline phase formation amount, fine powder particle size and excellent hardness. Adding it to the matrix as a reinforcing particle can significantly improve the strength and ductility of the composite material.

[0066] In summary, the present invention successfully prepares Al-Cu-Fe-La quasi-crystalline alloy powder with high quasi-crystalline phase formation, fine particle size, high hardness and good thermal conductivity through reasonable component design and unique preparation method, which effectively solves the problems existing in existing quasi-crystalline alloys and has broad application prospects.

Claims

1. An Al-Cu-Fe-La quaternary quasi-crystal alloy powder, characterized in that: The expression of the quaternary quasi-crystal alloy powder is (Al 63 Cu 25 Fe 12 ) 100-X La×; wherein the value of x ranges from 0 to 1.0 at%.

2. A method for preparing the Al-Cu-Fe-La quasi-crystalline alloy powder according to claim 1, characterized in that: The following steps are involved: Step 1, ingredients: according to the expression (Al 63 Cu 25 Fe 12 ) 100-X La×(x=0-1.0at%) is prepared by 80g each, and 99.9wt% pure aluminum, 99.9wt% pure copper, Al-60% Fe and Al-80% La master alloy are used as raw materials for preparation; Step 2, melting: a vacuum arc melting furnace is used to prepare an Al-Cu-Fe-La quaternary quasi-crystalline alloy. The vacuum arc melting process parameters are: a melting current of 500A, a stirring current of 30A, and a voltage of 5V to prepare a cast quasi-crystalline alloy. The obtained sample is then turned over and remelted four times to improve the uniformity of the alloy composition. After the melting is completed, air cooling is performed to obtain a cast quasi-crystalline alloy. Step 3, crushing and grinding: the obtained cast quasicrystalline alloy is mechanically crushed and ground, the grinding is performed using a planetary ball mill, the grinding ball particle size ratio is 3mm:5mm:8mm=5:3:2, the ball-to-material ratio is 1:1, the ball mill is paused for 15min after every 30min of operation, and the forward and reverse directions are alternately operated. The total ball milling time is 3h, and the ball milling speed is 650r / min; Step 4, screening: After the above grinding, screening is performed to obtain a cast quasicrystalline alloy powder with a particle size of 38-75 μm.

3. The preparation method according to claim 2, characterized in that: The ball milling was carried out under argon protection.

4. The Al-Cu-Fe-La quaternary quasicrystalline alloy powder according to claim 1, characterized in that: The cast quasicrystalline alloy powder is proved to have an alloy composition of monoclinic λ-Al 13 Fe4 phase, τ-AlCu phase and quasicrystal I-Al 65 Cu 20 Fe 15 Phase composition.

5. The Al-Cu-Fe-La quaternary quasicrystalline alloy powder according to claim 1, characterized in that: When 0, 0.25, 0.5, 0.75 and 1.0 at% lanthanum is added, the formation amount of quasicrystalline phase of the quasicrystalline alloy is 34.98%, 24.79%, 45.68%, 26.72% and 35.8%, respectively.

6. The Al-Cu-Fe-La quaternary quasicrystalline alloy powder according to claim 1, characterized in that: The as-cast quasicrystalline alloy powder has diffraction rotation patterns with quintic, cubic and quadratic rotational symmetry.

7. The Al-Cu-Fe-La quaternary quasicrystalline alloy powder according to claim 1, characterized in that: The Vickers hardness of the bulk quasicrystal is 650-900 HV. 0.3 .

Images