CN115283666A - Aluminum alloy powder spheroidizing process - Google Patents
Aluminum alloy powder spheroidizing process Download PDFInfo
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- CN115283666A CN115283666A CN202210715821.8A CN202210715821A CN115283666A CN 115283666 A CN115283666 A CN 115283666A CN 202210715821 A CN202210715821 A CN 202210715821A CN 115283666 A CN115283666 A CN 115283666A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention provides an aluminum alloy powder spheroidizing process which is characterized by comprising the following steps of: s1, crushing block aluminum alloy into aluminum alloy particles with certain diameters; s2, mixing the aluminum alloy particles and the weakly acidic reaction solution according to a certain proportion, reacting in an ultrasonic magnetic stirring container, and spheroidizing irregular aluminum alloy powder particles to obtain spheroidized aluminum alloy powder particles; and S3, separating the reaction solution from the prepared spherical aluminum alloy powder particles, cleaning the separated spherical aluminum alloy powder particles, and drying the spherical aluminum alloy powder particles in vacuum at a low temperature to obtain the spherical aluminum alloy powder material suitable for additive manufacturing. The method of the invention has the advantages of simplicity, large production batch, small equipment investment, no pollution in the whole process, no waste generation, realization of production automation and suitability for the production of the aluminum alloy spherical powder with most components at present.
Description
Technical Field
The invention relates to the field of preparation of spherical powder materials for additive manufacturing, in particular to a spheroidizing process method for aluminum alloy powder.
Background
With the continuous development of scientific technology, the additive manufacturing technology gradually becomes one of the main research directions of industrial production due to the advantages of simple process, short development period of new products, raw material saving and the like, thereby subverting the idea and concept of traditional manufacturing. In some fields, especially in the aspects of new product development and the like, additive manufacturing technology has irreplaceable technical advantages.
Compared with the traditional powder metallurgy process, the additive manufacturing technology has more strict requirements on the used powder, especially the particle size distribution and the sphericity of the powder. Generally, powder particles with a particle size of less than 1mm may be suitable for additive manufacturing. Repeated research shows that the particles with the particle size of about 50 mu m have better fluidity and can obtain the additive manufacturing component with better internal quality. Currently, methods for preparing alloy powder for additive manufacturing mainly include reduction-chemical methods, vapor deposition methods, electrolytic methods, atomization methods, mechanical pulverization methods, and the like. Although the reduction-combination method and the vapor deposition method can prepare powder particles with higher sphericity, the method is not suitable for preparing all metal alloy powder, especially aluminum alloy spherical powder with more complex components. The electrolysis process is complex and has high cost. The particle size distribution of the powder particles prepared by mechanical pulverization is not uniform, and the sphericity of the powder is poor. The atomization method is a main process for producing the alloy spherical powder at present, but the process is complex, the energy consumption is high, and the equipment investment cost is high. The spherical aluminum alloy powder has higher preparation cost, and limits the wide and large-scale use of the additive manufacturing technology.
Therefore, the preparation process of the spherical aluminum alloy powder with low cost and no pollution has a far-reaching influence on the development and application of the additive manufacturing technology.
Disclosure of Invention
The technical problem to be solved is as follows: the invention aims to provide a spheroidizing process method of aluminum alloy powder, which aims to simplify the spheroidizing process of the aluminum alloy powder, reduce the equipment investment required by production, realize no pollution and no waste generation, can be massively and automatically produced and is suitable for the current production method of the aluminum alloy spherical powder with most components.
The technical scheme is as follows: an aluminum alloy powder spheroidizing process comprises the following steps:
s1, crushing block aluminum alloy into aluminum alloy particles with certain diameters;
s2, mixing the aluminum alloy particles and the weakly acidic reaction solution according to a certain proportion, reacting in an ultrasonic magnetic stirring container, and spheroidizing irregular aluminum alloy powder particles to obtain spheroidized aluminum alloy powder particles;
and S3, separating the reaction solution from the prepared spherical aluminum alloy powder particles, cleaning the separated spherical aluminum alloy powder particles, and drying in vacuum at low temperature to obtain the spherical aluminum alloy powder material suitable for additive manufacturing.
Preferably, the diameter of the aluminum alloy particles in the step S1 is 38 to 75 μm.
Preferably, the weak acid reaction solution in step S2 is any one or a combination of two or more of hydrochloric acid, sulfuric acid and phosphoric acid.
Preferably, in the step S2, the ratio of the amount of the aluminum alloy particles to the amount of the acid in the weakly acidic reaction solution is always maintained between 1.
Preferably, the ultrasonic power of the ultrasonic magnetic stirring reaction in the step S2 is 200 to 800W.
Preferably, the stirring speed of the ultrasonic magnetic stirring reaction in the step S2 is 200 to 500rpm.
Preferably, the temperature of the ultrasonic magnetic stirring reaction in the step S2 is controlled to be 25 to 45 ℃.
Preferably, the diameter of the spherical aluminum alloy powder material in the step S3 is 20 to 55 μm.
Has the advantages that: the aluminum alloy powder spheroidizing process provided by the invention has the following advantages:
(1) The method is simple, large in production batch, small in required equipment investment, free of pollution in the whole process and waste, capable of realizing production automation, and suitable for production of the aluminum alloy spherical powder with most components;
(2) The invention adopts the original powder particles with uneven surface appearance and more edges and sharp corners, adopts weak acid corrosion, and can firstly react the raised parts to ensure that the surface of the powder particles is smooth;
(3) Ultrasonic and stirring are applied in the reaction process, so that the reaction rate is accelerated, the dispersion of particles is facilitated, and irregular powder particles are quickly spheroidized by utilizing the friction and collision action among the particles and between the particles and the solution;
(4) The obtained spherical powder particles have proper granularity, and are not easy to agglomerate in the using process, so that the additive manufacturing effect is influenced;
(5) The by-products of the present invention also include aluminum salts and high purity hydrogen.
Description of the drawings:
FIG. 1 is a flow chart of a spheroidization process for aluminum alloy powder provided by the invention;
FIG. 2 is a schematic diagram of equipment configuration used in the spheroidization process of aluminum alloy powder provided by the invention, wherein 1 is an ultrasonic stirring reaction container, 2 is a reaction solution recovery dispenser, 3 is a hydrogen dehumidifying and drying recoverer, 4 is a spherical powder cleaner, 5 is a residual cleaning solution recovery tower, and 6 is a vacuum drying oven;
FIG. 3 is a diagram showing the morphology of spheroidized aluminum alloy powder prepared by the spheroidizing process of aluminum alloy powder provided by the invention.
Detailed Description
The embodiments of the invention will be described in detail below with reference to the drawings, but the invention can be implemented in many different ways as defined and covered by the claims.
Example 1
A spheroidization process for aluminum alloy powder mainly comprises the following steps:
s1: raw material preparation
(1) Smelting aluminum alloy according to target components to prepare an alloy ingot;
(2) Crushing the aluminum alloy cast ingot into particles by ball milling or other mechanical crushing modes, sieving the particles by a 200-mesh sieve and a 400-mesh sieve, and selecting aluminum alloy particles with the particle size distribution of 38-75 mu m;
(3) Preparing a reaction solution: preparing AlCl according to the pH value of 6 to 7 3 And a HCl solution;
s2: ultrasonic agitation
(1) Weighing aluminum alloy particles and a reaction solution according to a volume ratio of 1;
(2) Vacuumizing the reaction container, turning on an ultrasonic source and a power supply, fully stirring the powder and the reaction solution by using magnetic stirring, and spheroidizing irregular aluminum alloy powder particles to obtain spheroidized aluminum alloy powder particles by using mutual collision and friction among the powder and mutual friction and reaction among the powder and the solution in the stirring process, wherein the ultrasonic power is 200W, and the stirring speed is 500 rpm;
(3) And in the stirring process, a pH detector is used for detecting the pH value of the reaction solution on line, and the supplement of the acid solution is synchronously carried out. In the stirring process, the temperature of the reaction solution is detected at any time by using a temperature agent, and the temperature is controlled within 45 ℃;
(4) In the stirring process, the generated gas is collected by a hydrogen dehumidifying and drying recoverer 3 by using the gas guide tube, and a pure byproduct H is obtained by dehumidifying and drying 2 ；
The third step: standing for separation, cleaning and drying
(1) Closing the ultrasonic source and the power supply, standing and separating the reaction solution and the powder in the container, and collecting the reaction solution by adopting a reaction solution recovery preparation device 2;
(2) Detecting the pH value and components of the separated reaction solution, crystallizing and supplementing a new acidic solution to enable the residual reaction solution to reach the required components and pH values, so that the reaction solution can be used for subsequent production; meanwhile, crystallizing to obtain a byproduct aluminum salt;
(3) Cleaning the separated spherical powder for multiple times by using a spherical powder cleaner 4, placing the spherical powder into a low-temperature vacuum drying box 6 for drying when the solution to be detected has basically no impurity component, and obtaining a spherical aluminum alloy powder material with the diameter of 20 to 55 mu m for additive manufacturing after drying;
(4) And precipitating, removing impurities and distilling the residual cleaning solution to remove impurity components in the cleaning solution, and recovering the cleaning solution obtained after distillation by using a residual cleaning solution recovery tower 5 to be used for subsequent production.
Example 2
A spheroidizing process for aluminum alloy powder mainly comprises the following steps:
s1: raw material preparation
(1) Smelting aluminum alloy according to target components to prepare an alloy ingot;
(2) Crushing the aluminum alloy cast ingot into particles by using a ball milling or other mechanical crushing mode, sieving the particles by using 200-mesh and 400-mesh sieves, and selecting aluminum alloy particles with the particle size distribution of 38-75 mu m;
(3) Preparing a reaction solution: preparing AlCl according to the pH value of 6 to 7 3 And a HCl solution;
s2: ultrasonic agitation
(1) Weighing aluminum alloy particles and a reaction solution according to a volume ratio of 1;
(2) Vacuumizing the reaction container, turning on an ultrasonic source and a power supply, fully stirring the powder and the reaction solution by using magnetic stirring, and spheroidizing irregular aluminum alloy powder particles to obtain spheroidized aluminum alloy powder particles by using mutual collision and friction among the powder and mutual friction and reaction among the powder and the solution in the stirring process, wherein the ultrasonic power is 800W, and the stirring speed is 200 rpm;
(3) And in the stirring process, a pH detector is used for detecting the pH value of the reaction solution on line, and the supplement of the acid solution is synchronously carried out. In the stirring process, the temperature of the reaction solution is detected at any time by using a temperature agent, and the temperature is controlled within 45 ℃;
(4) In the stirring process, the generated gas is collected by a hydrogen dehumidifying and drying recoverer 3 by using the gas guide tube, and a pure byproduct H is obtained by dehumidifying and drying 2 ；
The third step: standing for separation, cleaning and drying
(1) Closing the ultrasonic source and the power supply, standing and separating the reaction solution and the powder in the container, and collecting the reaction solution by adopting a reaction solution recovery preparation device 2;
(2) Detecting the pH value and components of the separated reaction solution, crystallizing and supplementing a new acidic solution to enable the residual reaction solution to reach the required components and pH value, so that the reaction solution can be used for subsequent production; meanwhile, crystallizing to obtain a byproduct aluminum salt;
(3) Cleaning the separated spherical powder for multiple times by using a spherical powder cleaner 4, placing the spherical powder into a low-temperature vacuum drying box 6 for drying when the solution to be cleaned is basically free of impurity components, and drying to obtain a spherical aluminum alloy powder material with the diameter of 20 to 55 microns and suitable for additive manufacturing;
(4) And precipitating, removing impurities and distilling the residual cleaning solution to remove impurity components in the cleaning solution, and recovering the cleaning solution obtained after distillation by using a residual cleaning solution recovery tower 5 to be used for subsequent production.
Example 3
A spheroidization process for aluminum alloy powder mainly comprises the following steps:
s1: raw material preparation
(1) Smelting aluminum alloy according to target components to prepare an alloy ingot;
(2) Crushing the aluminum alloy cast ingot into particles by using a ball milling or other mechanical crushing mode, sieving the particles by using 200-mesh and 400-mesh sieves, and selecting aluminum alloy particles with the particle size distribution of 38-75 mu m;
(3) Preparing a reaction solution: preparing AlCl according to the pH value of 6 to 7 3 And a HCl solution;
s2: ultrasonic agitation
(1) Weighing aluminum alloy particles and a reaction solution according to a volume ratio of 1 to 3 to 1;
(2) Vacuumizing the reaction container, turning on an ultrasonic source and a power supply, fully stirring the powder and the reaction solution by using magnetic stirring, and spheroidizing irregular aluminum alloy powder particles by using mutual collision and friction among the powder and mutual friction and reaction among the powder and the solution in the stirring process, wherein the ultrasonic power is 500W, and the stirring speed is 300rpm to obtain the spheroidized aluminum alloy powder particles;
(3) And in the stirring process, a pH detector is used for detecting the pH value of the reaction solution on line, and the supplement of the acid solution is synchronously carried out. In the stirring process, the temperature of the reaction solution is detected at any time by using a temperature agent, and the temperature is controlled within 35 ℃;
(4) In the stirring process, the generated gas is collected by a hydrogen dehumidifying and drying recoverer 3 by utilizing the gas guide tube, and pure byproduct H is obtained by dehumidifying and drying 2 ；
The third step: standing for separation, cleaning and drying
(1) Closing the ultrasonic source and the power supply, standing and separating the reaction solution and the powder in the container, and collecting the reaction solution by adopting a reaction solution recovery preparation device 2;
(2) Detecting the pH value and components of the separated reaction solution, crystallizing and supplementing a new acidic solution to enable the residual reaction solution to reach the required components and pH value, so that the reaction solution can be used for subsequent production; meanwhile, crystallizing to obtain a byproduct aluminum salt;
(3) Cleaning the separated spherical powder for multiple times by using a spherical powder cleaner 4, placing the spherical powder into a low-temperature vacuum drying box 6 for drying when the solution to be cleaned is basically free of impurity components, and drying to obtain a spherical aluminum alloy powder material with the diameter of 20 to 55 microns and suitable for additive manufacturing;
(4) And precipitating, removing impurities and distilling the residual cleaning solution to remove impurity components in the cleaning solution, and recovering the cleaning solution obtained after distillation by using a residual cleaning solution recovery tower 5 for subsequent production.
Table 1 shows the average diameters of the spherical aluminum alloy powder materials obtained in examples 1 to 3
| Average diameter of spherical aluminum alloy powder material | |
| Example 1 | 45μm |
| Example 2 | 38μm |
| Example 3 | 40μm |
As can be seen from the above table 1, the average diameter of the spherical aluminum alloy powder material is 38-45 μm, and the particle size obtained by acid treatment and ultrasonic magnetic stirring is uniform, so that the standard of additive manufacturing can be reached. Some fine particles are generated because collision between particles occurs during the spheroidization process. In addition, in the byproduct recovery process, the byproducts cannot be completely recovered due to the presence of partial hydrogen dissipation and partial dissolution of aluminum salts in the solution. Specific yields are shown in the following table.
Table 2 shows the yields of the respective products in examples 1 to 3
| Spherical aluminum alloy powder material yield | Hydrogen yield (mass ratio) | Yield of aluminium salt (mass ratio) | |
| Example 1 | 55.6% | 2.3% | 41.3% |
| Example 2 | 53.4% | 2.5% | 42.5% |
| Example 3 | 54.8% | 2.0% | 38.9% |
It should be noted that the above lists only a few specific embodiments of the present invention, and it is obvious that the present invention is not limited to the above embodiments, and other modifications are possible. All modifications directly or indirectly derivable by a person skilled in the art from the present disclosure are to be considered within the scope of the present invention.
Claims (8)
1. The aluminum alloy powder spheroidizing process is characterized by comprising the following steps of:
s1, crushing block aluminum alloy into aluminum alloy particles with certain diameters;
s2, mixing the aluminum alloy particles and the weakly acidic reaction solution according to a certain proportion, reacting in an ultrasonic magnetic stirring container, and spheroidizing the irregular aluminum alloy powder particles to obtain spheroidized aluminum alloy powder particles;
and S3, separating the reaction solution from the prepared spherical aluminum alloy powder particles, cleaning the separated spherical aluminum alloy powder particles, and drying in vacuum at low temperature to obtain the spherical aluminum alloy powder material suitable for additive manufacturing.
2. The aluminum alloy powder spheroidizing process according to claim 1, characterized in that: the diameter of the aluminum alloy particles in the step S1 is 38 to 75 mu m.
3. The spheroidization process of aluminum alloy powder according to claim 1, characterized in that: in the step S2, the weak acidic reaction solution is any one or a combination of two or more of hydrochloric acid, sulfuric acid and phosphoric acid.
4. The spheroidization process of aluminum alloy powder according to claim 1, characterized in that: in the step S2, the ratio of the aluminum alloy particles to the amount of the acid in the weakly acidic reaction solution is maintained between 1 to 1.
5. The aluminum alloy powder spheroidizing process according to claim 1, characterized in that: and the ultrasonic power of the ultrasonic magnetic stirring reaction in the step S2 is 200 to 800W.
6. The spheroidization process of aluminum alloy powder according to claim 1, characterized in that: the stirring speed of the ultrasonic magnetic stirring reaction in the step S2 is 200 to 500rpm.
7. The spheroidization process of aluminum alloy powder according to claim 1, characterized in that: the temperature of the ultrasonic magnetic stirring reaction in the step S2 is controlled to be 25-45 ℃.
8. The spheroidization process of aluminum alloy powder according to claim 1, characterized in that: the diameter of the spherical aluminum alloy powder material in the step S3 is 20 to 55 mu m.
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