Reinforced aluminum alloy material, preparation method therefor and use thereof
By introducing egg-shaped metal-ceramic particles as reinforcing phases into the aluminum alloy matrix, the problem of insufficient strength of aluminum alloy drill pipes at high temperatures was solved, achieving improved strength and structural stability at high temperatures, making it suitable for the preparation of oil pipes.
Patent Information
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- CHINA NAT PETROLEUM CORP
- Filing Date
- 2025-12-22
- Publication Date
- 2026-07-09
Smart Images

Figure PCTCN2025144392-FTAPPB-I100001
Abstract
Description
Reinforced aluminum alloy materials, their preparation methods and applications
[0001] Cross-references to related applications
[0002] This application claims the benefit of Chinese Patent Application No. 202411965194.9, filed on December 30, 2024, the contents of which are incorporated herein by reference. Technical Field
[0003] This invention relates to the field of oil pipe and equipment materials, specifically to a reinforced aluminum alloy material, its preparation method and application, and an aluminum alloy drill pipe body and its preparation method. Background Technology
[0004] With the exploration and development of deep and ultra-deep oil and gas, conventional steel drill pipes are prone to damage and failure due to their high density and insufficient corrosion resistance, seriously affecting drilling efficiency and safety. Aluminum alloy drill pipe materials, characterized by high strength, low density, fatigue resistance, and corrosion resistance, represent a superior technology for solving drill string failure in ultra-deep wells. Existing patents cover aluminum alloy drill pipe materials with pressures of 325MPa (CN201310114425.0), 480MPa (CN201510142849.7), 580MPa (CN201410855573.2), and 620MPa (CN201410853240.6), which can serve for extended periods in downhole conditions with operating temperatures not exceeding 120℃ or 160℃, thus addressing, to some extent, the drilling problems in wells shallower than 6000 meters. However, the maximum drilling depth of ultra-deep wells in my country has reached tens of thousands of meters, with bottom hole temperatures exceeding 180°C. Existing aluminum alloy drill pipe materials can no longer meet the requirements of ultra-deep oil and gas drilling. Therefore, there is an urgent need to develop high-temperature resistant aluminum alloy drill pipe materials to meet the high-temperature drilling requirements of ultra-deep oil and gas formations. Summary of the Invention
[0005] The purpose of this invention is to provide a reinforced aluminum alloy material, its preparation method and application, and an aluminum alloy drill pipe body and its preparation method. The reinforced aluminum alloy material has high strength at room temperature and high temperature, good extrusion molding performance, and is particularly suitable for the preparation of large / long (10m long) oil pipes.
[0006] According to a first aspect of the present invention, the present invention provides a reinforced aluminum alloy material comprising an aluminum alloy matrix phase and an egg-shaped metal-ceramic particle reinforcing phase dispersed in the matrix phase, wherein the content of the reinforcing phase is 0.2-0.5 wt% based on the total weight of the material; the egg-shaped metal-ceramic particle reinforcing phase comprises a ceramic oxide core layer, a cerium-aluminum alloy intermediate layer, and an oxide film layer formed by the cerium-aluminum alloy metal of the intermediate layer.
[0007] According to a second aspect of the present invention, the present invention provides a method for preparing the reinforced aluminum alloy material of the present invention, the method comprising: (1) depositing a cerium-aluminum alloy intermediate layer on the surface of ceramic oxide powder, reacting it with oxygen to generate an oxide film layer, cooling to obtain egg-shaped metal ceramic particles as the reinforcing phase, the egg-shaped metal ceramic particles comprising a ceramic oxide core layer, a cerium-aluminum alloy intermediate layer and an oxide film layer formed by the cerium-aluminum alloy metal of the intermediate layer; preparing an aluminum alloy melt as the matrix phase; (2) adding the metal ceramic particles obtained in step (1) to the aluminum alloy melt, melting and cooling to form an ingot.
[0008] According to a third aspect of the present invention, the present invention provides an application of the reinforced aluminum alloy material described herein in the preparation of oil pipes.
[0009] According to a fourth aspect of the present invention, the present invention provides an aluminum alloy drill pipe body, wherein the material of the aluminum alloy drill pipe body is the material described in the present invention.
[0010] According to a fifth aspect of the present invention, the present invention provides a method for preparing an aluminum alloy drill pipe body, the method comprising: melting, casting, extruding, solution treatment, and aging treatment of the material described in the present invention to obtain an aluminum alloy drill pipe body.
[0011] In the reinforced aluminum alloy material of this invention, the egg-shaped cerium-ceramic reinforcement phase has a dispersion strengthening effect on the aluminum alloy matrix phase, effectively improving the strength of the aluminum alloy material. The cerium-ceramic reinforcement phase has an "egg" structure of "ceramic oxide core layer / cerium-aluminum alloy intermediate layer / oxide thin film layer," which exhibits higher toughness compared to a pure ceramic phase. In subsequent applications, such as tube extrusion molding, the two-dimensional oxide thin film layer deforms within a certain deformation range along with the metal-toughened intermediate layer without cracking. The presence of this special reinforcement phase improves the material strength without affecting the subsequent tube extrusion molding performance. Detailed Implementation
[0012] The endpoints and any values of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoint values of the various ranges, the endpoint values of the various ranges and individual point values, and individual point values can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.
[0013] The present invention provides a reinforced aluminum alloy material comprising an aluminum alloy matrix phase and an egg-shaped metal-ceramic particle reinforcing phase dispersed in the matrix phase, wherein the content of the reinforcing phase is 0.2-0.5 wt% based on the total weight of the material; the egg-shaped metal-ceramic particle reinforcing phase comprises a ceramic oxide core layer, a cerium-aluminum alloy intermediate layer, and an oxide film layer formed by the cerium-aluminum alloy metal of the intermediate layer.
[0014] In this invention, the reinforced aluminum alloy material can be a reinforced aluminum alloy composite material, that is, a composite material containing egg-shaped metal ceramic particles as a reinforcing phase.
[0015] The egg-shaped metal-ceramic particle-reinforced phase of the present invention has an "egg" structure of "ceramic oxide core layer / cerium-aluminum alloy intermediate layer / oxide thin film layer". The ceramic oxide core layer is similar to the yolk of an egg, the cerium-aluminum alloy intermediate layer is similar to the egg white of an egg, and the oxide thin film layer is similar to the eggshell of an egg.
[0016] In this invention, dispersion refers to the presence of the reinforcing phase particles in the aluminum alloy matrix phase in a substantially isolated, discontinuous, and uniformly distributed manner.
[0017] According to a preferred embodiment of the present invention, the diameter of the egg-shaped metal-ceramic particles is 100-145nm, such as 100nm, 105nm, 110nm, 115nm, 120nm, 125nm, 130nm, 135nm, 140nm, 145nm, and any range between any two values.
[0018] In this invention, there is no special limitation on the specific type of ceramic oxide in the egg-shaped metal-ceramic reinforcing phase. In the embodiments of this invention, cerium oxide is used as an example to illustrate the advantages of this invention, but this does not limit the scope of this invention.
[0019] According to a preferred embodiment of the present invention, in the egg-shaped metal-ceramic particles, the particle size of the ceramic oxide is 5-20 nm. This can also be understood as the thickness of the ceramic oxide core layer being 5-20 nm, for example, 5 nm, 8 nm, 11 nm, 14 nm, 17 nm, 20 nm, or any range between any two values. Nanoscale ceramic oxides have a grain boundary fixing effect and dispersion strengthening effect. The material of the present invention, satisfying the aforementioned characteristics, exhibits higher strength and better extrusion molding performance under high-temperature conditions.
[0020] In this invention, the specific type and aluminum content of the cerium-aluminum alloy in the egg-shaped cerium-aluminum particles are not specifically limited. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the cerium-aluminum alloy is a Ce-Al master alloy, and the Al content in the Ce-Al master alloy is 75-85 wt%, such as 75 wt%, 77 wt%, 79 wt%, 81 wt%, 83 wt%, 85 wt%, and any range between any two values, with the remainder being Ce.
[0021] According to a preferred embodiment of the present invention, in the egg-shaped metal ceramic particles, the oxide film layer comprises CeO2 and α-Al2O3, and the content of alumina accounts for 60-85 wt% of the oxide, for example, 60 wt%, 65 wt%, 70 wt%, 75 wt%, 80 wt%, 85 wt%, and any range between any two values.
[0022] In this invention, the oxide film comprises CeO2 and α-Al2O3. The inventors discovered that, since the oxide film corresponding to the Ce-Al master alloy is CeO2 and α-Al2O3, and because the aluminum alloy matrix material lacks O atoms, the CeO2 and α-Al2O3 in the oxide film will not grow. Furthermore, CeO2 and α-Al2O3 are extremely stable at high temperatures, such as 800°C, and will not decompose. This effectively improves the high-temperature thermal stability of reinforcing phases such as CeO2 and α-Al2O3, thereby preventing their growth at high temperatures, which would reduce their strengthening effect and lead to a decrease in material strength. Therefore, reinforcing phases that meet the aforementioned characteristics are more stable at high temperatures, and aluminum alloy drill pipe materials prepared using this material exhibit higher structural stability and high-temperature strength at high temperatures.
[0023] In this invention, there are no special requirements for the thickness of the cerium-aluminum alloy interlayer in the egg-shaped cerium-ceramic particles. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the thickness of the cerium-aluminum alloy interlayer is 40-50 nm. The cerium-ceramic reinforcing phase that meets the aforementioned characteristics has a good dispersion effect in the aluminum alloy matrix phase.
[0024] According to a preferred embodiment of the present invention, in the egg-shaped cerium-aluminum alloy intermediate layer to the oxide film layer in the cerium-aluminum alloy cerium-ceramic particles, the thickness ratio is 4-5:1. The cerium-ceramic particles satisfying the aforementioned characteristics exhibit good dispersion in the aluminum alloy matrix phase.
[0025] In this invention, there are no special requirements regarding the types and contents of metals contained in the aluminum alloy matrix phase. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the aluminum alloy matrix phase contains 4-4.8 wt% Cu, 1.5-2.0 wt% Mg, 0.7-0.9 wt% Mn, 0.5-0.9 wt% Ni, 0.3-0.5 wt% Zn, 0.005-0.008 wt% B, with the balance being Al and unavoidable impurities. The material of the present invention that satisfies the foregoing characteristics has better room temperature and high temperature strength.
[0026] In this invention, the unavoidable impurities refer to trace elements introduced by raw materials or processes during the industrial production of the materials and products, which cannot be completely removed by conventional means. The presence of these elements does not have a substantial adverse effect on the core performance described in this invention.
[0027] In this invention, there is no particular limitation on the preparation method of the material described herein. The following is an illustrative description, but it does not limit the scope of the invention. This invention provides a method for preparing the reinforced aluminum alloy material described herein. The method includes: (1) depositing a cerium-aluminum alloy intermediate layer on the surface of ceramic oxide powder, reacting it with oxygen to generate an oxide film layer, cooling it, and obtaining egg-shaped metal ceramic particles as the reinforcing phase. The egg-shaped metal ceramic particles include a ceramic oxide core layer, a cerium-aluminum alloy intermediate layer, and an oxide film layer formed by the cerium-aluminum alloy metal of the intermediate layer; preparing an aluminum alloy melt as the base phase; (2) adding the metal ceramic particles obtained in step (1) to the aluminum alloy melt, melting and cooling it to form an ingot.
[0028] In this invention, there is no particular limitation on the deposition method described in step (1). According to a preferred embodiment of the present invention, magnetron sputtering is used as an exemplary deposition method to illustrate the advantages of the technical solution of the present invention, but this does not limit the scope of the present invention. Magnetron sputtering can more precisely control the thickness of the cerium-aluminum alloy intermediate layer and the oxide film layer of the reinforcing phase. Before magnetron sputtering deposition, in order to remove contaminants and adsorbates on the surface of the ceramic oxide powder, the ceramic oxide powder was ultrasonically cleaned with acetone, ethanol and deionized water for 10 minutes in sequence, dried and laid flat on the substrate stage.
[0029] In this invention, there are no special requirements for the sputtering power of the magnetron sputtering. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the sputtering power is 310-320W.
[0030] In this invention, there are no special requirements for the sputtering gas pressure of the magnetron sputtering, for example, it is 0.5-0.8 Pa.
[0031] In this invention, there are no special requirements for the substrate temperature of the magnetron sputtering. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the substrate temperature is 250-260°C.
[0032] In this invention, there are no special requirements for the deposition time in step (1), but it is preferable that the thickness of the intermediate layer does not exceed 50 nm. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the deposition time is 120-150 s, such as 120 s, 125 s, 130 s, 135 s, 140 s, 145 s, 150 s, and any range between any two values.
[0033] In this invention, in step (1), the deposition can be carried out in an inert atmosphere. There are no special requirements for the specific type of deposition atmosphere. The following is an illustrative description, but it does not limit the scope of this invention. According to a preferred embodiment of this invention, the deposition atmosphere is an argon atmosphere.
[0034] In this invention, there are no special requirements for the flow rate of the argon atmosphere. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the flow rate of the argon atmosphere is 20-25 mL / min, such as 20 mL / min, 21 mL / min, 22 mL / min, 23 mL / min, 24 mL / min, 25 mL / min, and any range between any two values.
[0035] In this invention, in step (1), after depositing a cerium-aluminum alloy intermediate layer on the surface of ceramic oxide powder, it is reacted with oxygen to generate an oxide film layer. There are no special requirements for the temperature of the contact reaction. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the temperature of the contact reaction is 250-260°C.
[0036] In this invention, there are no special requirements for the contact reaction time in step (1). The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the contact reaction time is 40-50 seconds.
[0037] In this invention, in step (1), argon gas is introduced during the deposition of the cerium-aluminum alloy intermediate layer, and argon gas and oxygen gas are introduced simultaneously during the contact reaction stage.
[0038] According to a preferred embodiment of the present invention, in step (1), the contact reaction is carried out in an argon atmosphere. By employing the aforementioned technical solution, the contact reaction becomes more stable, and the resulting oxide film becomes denser.
[0039] In this invention, during step (1) of the contact reaction process, there are no special requirements for the flow rate of the oxygen gas. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the flow rate of the oxygen is 0.4-0.5 mL / min. In this invention, the introduction of extremely low oxygen content is beneficial to the formation of α-Al2O3 and CeO2 structures in the film layer, thereby improving the high-temperature strength of the aluminum alloy drill rod material. Due to the extremely low oxygen content, due to the selective oxidation characteristics (at 260°C, the Gibbs free energy of α-alumina formation is below -1000 kJ / mol, and that of cerium oxide is above -700 kJ / mol), α-Al2O3 will be preferentially generated on the surface of the cerium-aluminum alloy. For example, when the aluminum alloy is a Ce / Al intermediate alloy, a nano-oxide film mainly composed of α-Al2O3 and containing a small amount of CeO2 will be generated on the alloy surface. Because the diffusion coefficient of elements in heterogeneous oxides is extremely low, CeO2 and α-Al2O3 mutually restrict the transformation of their nanoparticles into macroscopic crystals. This unique structure significantly reduces the impact of size effects on the thermodynamic properties of nano-oxide particles. Specifically, it limits the growth of the CeO2 and α-Al2O3 nanoparticles used for reinforcement, which is beneficial for improving the high-temperature strength of aluminum alloy drill pipe materials.
[0040] In this invention, during step (1) of the contact reaction process, there are no special requirements for the flow rate of the argon atmosphere. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the flow rate of the argon is 20-25 mL / min, such as 20 mL / min, 21 mL / min, 22 mL / min, 23 mL / min, 24 mL / min, 25 mL / min, and any range between any two values.
[0041] In this invention, in step (1), before deposition, the reaction environment needs to be evacuated to 0.001-0.003 Pa, and the sample surface needs to be bombarded with argon gas for 2-5 minutes to remove sample contaminants.
[0042] In this invention, after the contact reaction is completed, the metal-ceramic powder is removed after cooling to room temperature. This is a routine operation and will not be described in detail here.
[0043] In this invention, in step (2), the melting process enables the cerium-ceramic powder to be fully dispersed in the aluminum alloy matrix melt. The melting temperature is preferably such that the cerium-aluminum alloy is fully melted and the low-melting-point metals such as magnesium are oxidized and burned off. The following is an illustrative description, but it does not limit the scope of this invention. According to a preferred embodiment of this invention, the melting temperature is 700-720°C, such as 700°C, 705°C, 710°C, 715°C, 720°C, and any range between any two values.
[0044] In this invention, the melting time in step (2) can be selected from a wide range. The following is an illustrative description, but it does not limit the scope of this invention. According to a preferred embodiment of this invention, the melting time is 10-15 min, such as 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, and any range between any two values.
[0045] The reinforced aluminum alloy material described in this invention has high strength and good extrusion molding performance, making it particularly suitable for use in the manufacture of large / long oil pipes.
[0046] This invention provides an aluminum alloy drill pipe body, the material of which is the material described in this invention. This aluminum alloy drill pipe body exhibits excellent structural stability and high-temperature strength at high temperatures.
[0047] This invention provides a method for preparing an aluminum alloy drill pipe body, the method comprising: melting, casting, homogenizing the cast billet, multi-stage extrusion molding, multi-stage solution treatment, and aging treatment of the material described in this invention to obtain an aluminum alloy drill pipe body.
[0048] In this invention, the smelting, casting, billet homogenization, and extrusion molding are all conventional operations well known to those skilled in the art, and will not be described in detail here. No special requirements are made for their specific conditions.
[0049] In this invention, multi-stage solution treatment refers to one of the heat treatment processes for the aluminum alloy drill pipe body, specifically a solution treatment process comprising at least two stages. The temperature and duration of each subsequent solution treatment stage are higher than the previous stage. The purpose is to allow strengthening elements (such as Cu, Mg, etc.) to dissolve more fully and uniformly into the aluminum matrix through stepped heating and holding, and to optimize the grain boundary state.
[0050] In this invention, as long as the temperature of the secondary solution is higher than that of the primary solution and the time of the secondary solution is longer than that of the primary solution, no special requirements are made for the specific conditions of the primary solution. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the conditions of the primary solution include: a temperature of 480-495℃, such as 480℃, 483℃, 486℃, 489℃, 492℃, 495℃, and any range between any two values; and / or a time of 40-60 min, such as 40 min, 44 min, 48 min, 52 min, 56 min, 60 min, and any range between any two values.
[0051] In this invention, as long as the temperature of the secondary solution is higher than that of the primary solution and the time of the secondary solution is longer than that of the primary solution, no special requirements are made for the specific conditions of the secondary solution. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the conditions of the secondary solution include: a temperature of 495-510℃, such as 495℃, 498℃, 501℃, 504℃, 507℃, 510℃, and any range between any two values; and / or a time of 70-80 min, such as 70 min, 72 min, 74 min, 76 min, 78 min, 80 min, and any range between any two values.
[0052] In this invention, there are no special requirements for the aging process. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the aging process includes a first-stage high-temperature aging and a second-stage air-cooled aging.
[0053] In this invention, there are no special requirements for the conditions of the first-level high-temperature aging. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the conditions of the first-level high-temperature aging are: a temperature of 190-200℃, such as 190℃, 192℃, 194℃, 196℃, 198℃, 200℃, and any range between any two values; and / or a time of 1.5-2h.
[0054] In this invention, there are no special requirements for the conditions of the secondary air-cooled aging process. The following is an illustrative description, but it does not limit the scope of the invention. According to a preferred embodiment of the invention, the conditions of the secondary air-cooled aging process include: a temperature of room temperature, such as 15-35°C; and / or a time of 10-12 days, such as 10 days, 10.5 days, 11 days, 11.5 days, 12 days, and any range between any two values.
[0055] The aluminum alloy drill pipe body prepared by this invention has a yield strength of not less than 380 MPa and a heat resistance temperature of up to 180℃. After being exposed to heat at 180℃ for 500 hours, its yield strength can still maintain 72% of the room temperature value. It can be applied to drilling of deep and ultra-deep oil and gas formations, providing material support for lightweight technology in deep and ultra-deep well drilling.
[0056] The present invention will be described in detail below through embodiments.
[0057] In the following embodiments, the magnetron sputtering equipment is a desktop magnetron sputtering equipment of model MS-400 manufactured by Hefei Zhizhen Precision Equipment Co., Ltd.; the particle size of cerium oxide powder, the diameter of egg-shaped metal ceramic particles, the thickness of the cerium-aluminum alloy intermediate layer, and the thickness of the oxide film layer are obtained by measuring the average value of the embedded particle samples using transmission electron microscopy; the composition of the material can be obtained by calculation of the feed; the room temperature and high temperature yield strength of the aluminum alloy drill pipe are measured by a mechanical testing machine; the argon gas is high-purity argon gas (99.99%), and the oxygen gas is high-purity O2 (99.99%).
[0058]
Preparation Example 1
[0059] (1) Cerium oxide powder (particle size 20 nm), which has been ultrasonically cleaned in sequence with acetone, ethanol and deionized water for 10 min and then dried, is spread evenly on the substrate stage of the magnetron sputtering chamber; the chamber is then evacuated to 2 × 10⁻⁶ ppm. -3 The sample was subjected to a 3-minute argon gas bombardment of the cerium oxide powder surface to remove surface contaminants. Then, the argon gas flow rate was maintained at 25 mL / min, the magnetron sputtering power was set to 320 W, the sputtering pressure to 0.5 Pa, and the substrate temperature to 260 °C. A Ce-Al master alloy (79 wt% Al content) was deposited onto the cerium oxide powder surface via magnetron sputtering. After 150 s, deposition was stopped, and oxygen was introduced to form an oxide film on the sample surface after the Ce-Al master alloy deposition. The oxygen flow rate was 0.5 mL / min. After 50 s, the argon and oxygen supply was stopped, the sample was cooled to room temperature, and removed to obtain egg-shaped cerium ceramic particles. The diameter of these egg-shaped cerium ceramic particles was measured to be 144 nm, the Ce-Al master alloy master layer thickness was 50 nm, the oxide film thickness was 12 nm, and the α-Al₂O₃ content in the oxide film was 80 wt%.
[0060] (2) The cermet powder prepared in step (1) is added to the aluminum alloy matrix melt (the composition by weight is: Cu 4%, Mg 1.5%, Mn 0.7%, Ni 0.5%, Zn 0.3%, B 0.005%, with the balance being Al and unavoidable impurities). The amount of cermet powder added is 0.2% by weight of the total material. The melt is smelted (at a temperature of 700°C for 10 min), cooled to room temperature, and an ingot is formed to obtain the aluminum alloy material.
[0061]
Preparation Example 2
[0062] (1) Cerium oxide powder (particle size 20 nm), which has been ultrasonically cleaned in sequence with acetone, ethanol and deionized water for 10 min and then dried, is spread evenly on the substrate stage of the magnetron sputtering chamber; the chamber is then evacuated to 2 × 10⁻⁶ ppm. -3 The sample was subjected to a 3-minute argon gas bombardment process to remove surface contaminants. Then, the argon gas flow rate was maintained at 20 mL / min, the magnetron sputtering power was set to 310 W, the sputtering pressure to 0.5 Pa, and the substrate temperature to 250 °C. A Ce-Al master alloy (85 wt% Al content) was deposited onto the cerium oxide powder surface via magnetron sputtering. After 120 s, deposition was stopped, and oxygen was introduced at a flow rate of 0.4 mL / min to form an oxide film on the sample surface after Ce-Al master alloy deposition. After 50 s, both argon and oxygen supply were stopped, the sample was cooled to room temperature, and removed to obtain egg-shaped cerium ceramic particles. Analysis showed that the egg-shaped cerium ceramic particles had a diameter of 120 nm, a Ce-Al master alloy master layer thickness of 40 nm, an oxide film thickness of 10 nm, and an α-Al₂O₃ content of 85 wt% in the oxide film.
[0063] (2) The cermet powder prepared in step (1) is added to the aluminum alloy matrix melt (the composition by weight is: Cu 4.5%, Mg 1.7%, Mn 0.8%, Ni 0.6%, Zn 0.4%, B 0.006%, with the balance being Al and unavoidable impurities). The amount of cermet powder added is 0.3% by weight of the total material. The melt is smelted (at a temperature of 700°C for 10 min), cooled to room temperature, and an ingot is formed to obtain the aluminum alloy material.
[0064]
Preparation Example 3
[0065] (1) Prepare metal-ceramic powder according to the method of Preparation Example 1;
[0066] (2) The cermet powder prepared in step (1) is added to the aluminum alloy matrix melt (the composition by weight is: Cu 4.2%, Mg 1.6%, Mn 0.7%, Ni 0.6%, Zn 0.3%, B 0.005%, with the balance being Al and unavoidable impurities). The amount of cermet powder added is 0.3% by weight of the total material. The melt is smelted (at a temperature of 700°C for 10 min), cooled to room temperature, and an ingot is formed to obtain the aluminum alloy material.
[0067]
Preparation Example 4
[0068] (1) Prepare metal-ceramic powder according to the method of Preparation Example 1;
[0069] (2) The cermet powder prepared in step (1) is added to the aluminum alloy matrix melt (the composition by weight is: Cu 4.5%, Mg 1.8%, Mn 0.8%, Ni 0.7%, Zn 0.4%, B 0.007%, with the balance being Al and unavoidable impurities). The amount of cermet powder added is 0.4% by weight of the total material. The melt is smelted (at a temperature of 700°C for 10 min), cooled to room temperature, and an ingot is formed to obtain the aluminum alloy material.
[0070]
Preparation Example 5
[0071] (1) Prepare metal-ceramic powder according to the method of Preparation Example 1;
[0072] (2) The cermet powder prepared in step (1) is added to the aluminum alloy matrix melt (the composition by weight is: Cu 4.8%, Mg 2.0%, Mn 0.9%, Ni 0.9%, Zn 0.5%, B 0.008%, with the balance being Al and unavoidable impurities). The amount of cermet powder added is 0.5% by weight of the total material. The melt is smelted (at a temperature of 700°C for 10 min), cooled to room temperature, and an ingot is formed to obtain the aluminum alloy material.
[0073]
Preparation Example 6
[0074] (1) Prepare metal-ceramic powder according to the method of Preparation Example 1;
[0075] (2) The cermet powder prepared in step (1) is added to the aluminum alloy matrix melt (the composition by weight is: Cu 4%, Mg 1.5%, Mn 0.4%, Ni 0.5%, Zn 0.3%, B 0.005%, with the balance being Al and unavoidable impurities). The amount of cermet powder added is 0.2% by weight of the total material. The melt is smelted (at a temperature of 700℃ for 10 min), cooled to room temperature, and an ingot is formed to obtain the aluminum alloy material.
[0076]
Preparation Example 7
[0077] (1) Cerium oxide powder (20 nm), which has been ultrasonically cleaned in sequence with acetone, ethanol and deionized water for 10 min and then dried, is spread evenly on the substrate stage of the magnetron sputtering chamber; the chamber is then evacuated to a vacuum of 2 × 10⁻⁶. -3 The sample was subjected to a 3-minute argon gas bombardment process to remove surface contaminants. Then, the argon gas flow rate was maintained at 25 mL / min, the magnetron sputtering power was set to 320 W, the sputtering pressure to 0.5 Pa, and the substrate temperature to 260 °C. A Ce-Al master alloy (79 wt% Al content) was then deposited onto the cerium oxide powder surface via magnetron sputtering. After 150 s, deposition was stopped, and oxygen was introduced at a flow rate of 5 mL / min to form an oxide film on the sample surface after Ce-Al master alloy deposition. Argon and oxygen supply was stopped after 50 s, the sample was cooled to room temperature, and then removed to obtain egg-shaped cerium ceramic particles. The diameter of these egg-shaped cerium ceramic particles was measured to be 166 nm, the Ce-Al master alloy master layer thickness was 50 nm, the oxide film thickness was 23 nm, and the α-Al₂O₃ content in the oxide film was 56 wt%.
[0078] (2) The cermet powder prepared in step (1) is added to the aluminum alloy matrix melt (the composition by weight is: Cu 4%, Mg 1.5%, Mn 0.7%, Ni 0.5%, Zn 0.3%, B 0.005%, with the balance being Al and unavoidable impurities). The amount of cermet powder added is 0.2% by weight of the total material. The melt is smelted (at a temperature of 700°C for 10 min), cooled to room temperature, and an ingot is formed to obtain the aluminum alloy material.
[0079]
Preparation Example 8
[0080] (1) Cerium oxide powder (20 nm), which has been ultrasonically cleaned in sequence with acetone, ethanol and deionized water for 10 min and then dried, is spread evenly on the substrate stage of the magnetron sputtering chamber; the chamber is then evacuated to 2 × 10⁻⁶ ppm. -3 Pa, then argon gas was introduced to bombard the surface of cerium oxide powder for 3 min to remove surface contaminants; then, the argon gas flow rate was maintained at 25 mL / min, the magnetron sputtering power was set to 320 W, the sputtering gas pressure was set to 0.5 Pa, and the substrate temperature was maintained at 260 °C, and Ce-Al master alloy (Al content of 79 wt%) was deposited on the surface of cerium oxide powder by magnetron sputtering; after 200 s, the deposition was stopped, cooled to room temperature, and removed, and metal ceramic particles without oxide film were obtained. The thickness of the Ce-Al master alloy intermediate layer of the metal ceramic particles was found to be 50 nm.
[0081] (2) The cermet powder prepared in step (1) is added to the aluminum alloy matrix melt (the composition by weight is: Cu 4%, Mg 1.5%, Mn 0.7%, Ni 0.5%, Zn 0.3%, B 0.005%, with the balance being Al and unavoidable impurities). The amount of cermet powder added is 0.2% by weight of the total material. The melt is smelted (at a temperature of 700°C for 10 min), cooled to room temperature, and an ingot is formed to obtain the aluminum alloy material.
[0082]
Preparation Example 9
[0083] Cerium oxide powder (20 nm) was added to an aluminum alloy matrix melt (components by weight: Cu 4%, Mg 1.5%, Mn 0.7%, Ni 0.5%, Zn 0.3%, B 0.005%, balance Al and unavoidable impurities), wherein the amount of cerium-ceramic powder added was 0.2% by weight of the total material. The melt was smelted (at 700 °C for 10 min), cooled to room temperature, and an ingot was formed to obtain the aluminum alloy material.
[0084]
Example 1
[0085] The aluminum alloy material obtained in Example 1 was processed to obtain an aluminum alloy drill pipe body; the specific processing operations and conditions are as follows:
[0086] (1) Melting: Temperature 720℃, Time 10min;
[0087] (2) Casting: Obtain a casting billet, and homogenize the casting billet (heating temperature 506℃);
[0088] (3) Multi-stage extrusion molding: Two-stage extrusion, both at an extrusion temperature of 440℃, with extrusion ratios of 0.8 and 0.9 respectively;
[0089] (4) Multi-stage solution treatment: The first stage solution treatment temperature is 480℃ and the solution time is 40min; the second stage solution treatment temperature is 495℃ and the solution time is 70min.
[0090] (5) Aging time: Level 1 high temperature aging, 200℃, aging time 2h; Level 2 air cooling aging, temperature 25℃, time 10 days.
[0091]
Example 2
[0092] The method is the same as in Example 1, except that the aluminum alloy material obtained in Preparation Example 2 is used to process the aluminum alloy drill pipe body.
[0093]
Example 3
[0094] The method is the same as in Example 1, except that the aluminum alloy material obtained in Preparation Example 3 is used to process the aluminum alloy drill pipe body.
[0095]
Example 4
[0096] The method is the same as in Example 1, except that the aluminum alloy material obtained in Preparation Example 4 is used to process the aluminum alloy drill pipe body.
[0097]
Example 5
[0098] The method is the same as in Example 1, except that the aluminum alloy material obtained in Preparation Example 5 is used to process the aluminum alloy drill pipe body.
[0099]
Example 6
[0100] The method is the same as in Example 1, except that the aluminum alloy material obtained in Preparation Example 6 is used to process the aluminum alloy drill pipe body.
[0101]
Example 7
[0102] The method is the same as in Example 1, except that the aluminum alloy material obtained in Preparation Example 7 is used to process the aluminum alloy drill pipe body.
[0103] Comparative Example 1
[0104] The method is the same as in Example 1, except that the aluminum alloy material obtained in Preparation Example 8 is used to process the aluminum alloy drill pipe body.
[0105] Comparative Example 2
[0106] The method is the same as in Example 1, except that the aluminum alloy material obtained in Preparation Example 9 is used to process the aluminum alloy drill pipe body.
[0107] The yield strength of the aluminum alloy drill pipe materials prepared in the above embodiments and comparative examples was tested, and the specific data are shown in Table 1.
[0108] Table 1
[0109] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.
Claims
1. A reinforced aluminum alloy material, characterized in that, The material comprises an aluminum alloy matrix phase and an egg-shaped metal-ceramic particle reinforcing phase dispersed in the matrix phase, wherein the content of the reinforcing phase is 0.2-0.5 wt% based on the total weight of the material. The egg-shaped metal-ceramic particle reinforcement phase includes a ceramic oxide core layer, a cerium-aluminum alloy intermediate layer, and an oxide film layer formed by the cerium-aluminum alloy metal of the intermediate layer.
2. The material according to claim 1, characterized in that, The diameter of the egg-shaped metal-ceramic particles is 100-145 nm; and / or In the egg-shaped metal-ceramic particles, the ceramic oxide is cerium oxide; and / or The thickness of the ceramic oxide core layer is 5-20 nm.
3. The material according to claim 1 or 2, characterized in that, In the egg-shaped cerium-aluminum alloy particles, the cerium-aluminum alloy is a Ce-Al master alloy, and the Al content in the Ce-Al master alloy is 75-85 wt%; and / or The oxide film consists of CeO2 and α-Al2O3, with the content of α-Al2O3 being 60-85 wt%.
4. The material according to claim 1 or 2, characterized in that, In the egg-shaped metal-ceramic particles, the thickness of the cerium-aluminum alloy interlayer is 40-50 nm; and / or The thickness ratio of the cerium-aluminum alloy intermediate layer to the oxide film layer is 4-5:
1.
5. The material according to claim 1 or 2, characterized in that, The aluminum alloy matrix contains 4-4.8 wt% Cu, 1.5-2.0 wt% Mg, 0.7-0.9 wt% Mn, 0.5-0.9 wt% Ni, 0.3-0.5 wt% Zn, 0.005-0.008 wt% B, with the balance being Al and unavoidable impurities.
6. A method for preparing the reinforced aluminum alloy material according to any one of claims 1-5, characterized in that, The method includes: (1) After depositing a cerium-aluminum alloy intermediate layer on the surface of ceramic oxide powder, it is reacted with oxygen to generate an oxide film layer. After cooling, egg-shaped metal ceramic particles as the reinforcing phase are obtained. The egg-shaped metal ceramic particles include a ceramic oxide core layer, a cerium-aluminum alloy intermediate layer and an oxide film layer formed by the cerium-aluminum alloy metal of the intermediate layer; an aluminum alloy melt as the matrix phase is prepared. (2) The metal ceramic particles obtained in step (1) are added to the aluminum alloy melt, smelted and cooled to form an ingot.
7. The method according to claim 6, characterized in that, In step (1), the deposition is performed using magnetron sputtering.
8. The method according to claim 7, characterized in that, The conditions for magnetron sputtering include: sputtering power of 310-320W; substrate temperature of 250-260℃.
9. The method according to claim 6 or 7, characterized in that, In step (1), the deposition conditions include: a time of 120-150 s; and an argon atmosphere.
10. The method according to claim 9, characterized in that, In step (1), the flow rate of the argon atmosphere is 20-25 mL / min.
11. The method according to claim 6 or 7, characterized in that, In step (1), the conditions for the contact reaction include: a temperature of 250-260℃; a time of 40-50s; and the reaction is carried out in an argon atmosphere.
12. The method according to claim 11, characterized in that, In step (1), the oxygen flow rate is 0.4-0.5 mL / min; and / or The flow rate of the argon gas is 20-25 mL / min.
13. The method according to claim 6 or 7, characterized in that, In step (2), the melting conditions include: melting temperature of 700-720℃; and holding time of 10-15min.
14. The application of the reinforced aluminum alloy material according to claim 1 or 2 in the preparation of oil pipes.
15. An aluminum alloy drill pipe body, characterized in that, The material of the aluminum alloy drill pipe body is the material described in any one of claims 1-5.
16. A method for preparing an aluminum alloy drill pipe body, characterized in that, The method includes: melting, casting, homogenizing the cast billet, multi-stage extrusion molding, multi-stage solution treatment, and aging treatment of the material described in any one of claims 1-5 to obtain an aluminum alloy drill pipe body.
17. The method according to claim 16, characterized in that, The multi-stage solid solution includes primary solid solution and secondary solid solution. The temperature of the secondary solid solution is higher than that of the primary solid solution, and the time of the secondary solid solution is longer than that of the primary solid solution.
18. The method according to claim 17, characterized in that, The conditions for the first-stage solution treatment include: a temperature of 480-495°C; a time of 40-60 min; and / or The conditions for the secondary solution treatment include: a temperature of 495-510℃ and a time of 70-80 minutes.
19. The method according to claim 16, characterized in that, The aging process includes primary high-temperature aging and secondary air-cooled aging.
20. The method according to claim 19, characterized in that, The conditions for the first-level high-temperature aging include: a temperature of 190-200℃; a time of 1.5-2 hours; and / or The conditions for the secondary air-cooled aging process include: a temperature of 15-35℃ and a time of 10-12 days.