CN114101693A - Low-oxygen europium nickel powder for 3D printing and preparation method thereof - Google Patents
Low-oxygen europium nickel powder for 3D printing and preparation method thereof Download PDFInfo
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- CN114101693A CN114101693A CN202010898639.1A CN202010898639A CN114101693A CN 114101693 A CN114101693 A CN 114101693A CN 202010898639 A CN202010898639 A CN 202010898639A CN 114101693 A CN114101693 A CN 114101693A
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- 239000000843 powder Substances 0.000 title claims abstract description 58
- RSTMBJAUVCMABY-UHFFFAOYSA-N europium nickel Chemical compound [Ni][Eu] RSTMBJAUVCMABY-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000001301 oxygen Substances 0.000 title claims abstract description 42
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 42
- 238000010146 3D printing Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 44
- 239000002184 metal Substances 0.000 claims abstract description 44
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 42
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000003723 Smelting Methods 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 229910000990 Ni alloy Inorganic materials 0.000 claims abstract description 27
- 230000008569 process Effects 0.000 claims abstract description 22
- 229910052786 argon Inorganic materials 0.000 claims abstract description 21
- 239000000725 suspension Substances 0.000 claims abstract description 19
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 18
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 17
- 239000000498 cooling water Substances 0.000 claims abstract description 12
- 238000009689 gas atomisation Methods 0.000 claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 8
- 239000000956 alloy Substances 0.000 claims abstract description 8
- 238000005520 cutting process Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 11
- 238000005086 pumping Methods 0.000 claims description 10
- 230000006698 induction Effects 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 4
- 238000004381 surface treatment Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 9
- 238000000889 atomisation Methods 0.000 abstract description 9
- 238000005204 segregation Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 description 9
- 238000002844 melting Methods 0.000 description 8
- 230000008018 melting Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 244000137852 Petrea volubilis Species 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a low-oxygen europium nickel powder for 3D printing and a preparation method thereof, and the method comprises the following steps: s1, weighing equal-mass raw materials of europium and nickel, putting the raw materials into a vacuum suspension smelting furnace, vacuumizing the vacuum suspension smelting furnace and introducing argon; s2, under the cooling water circulation state, increasing current to melt the metal raw material, reducing current to cool the metal melt, repeating the steps for remelting, and obtaining a low-oxygen europium nickel alloy ingot; and S3, cutting the low-oxygen europium nickel alloy cast ingot into small squares, crushing and coarsely grinding the small squares into powder, and then carrying out plasma gas atomization to prepare powder so as to obtain spherical powder. The invention adopts the vacuum suspension smelting process to prepare the low-oxygen europium-nickel powder, can control the oxygen content and the element segregation in the alloy smelting process by keeping the vacuum and argon states in the whole smelting process, and simultaneously adopts the plasma atomization to prepare the europium-nickel powder with excellent physical and mechanical properties and high spheroidization rate, and the europium-nickel powder can be used for 3D printing to obtain high-precision products.
Description
Technical Field
The invention belongs to the technical field of rare earth alloys, and particularly relates to low-oxygen europium nickel powder for 3D printing and a preparation method thereof.
Background
The 3D printing has high requirements on the form and performance of the used material, the material is generally spherical powder, the spheroidization rate is higher than 98%, and the high spheroidization rate can ensure the uniformity of the printed powder and subsequent printing. At present, the preparation technology of domestic high-end spherical metal powder is not mature enough, and the problems of overhigh oxygen content in metal raw materials for preparing powder and the like exist, generally, the oxygen content is controlled to be below 0.15 percent (mass fraction), and the ductility and fracture toughness of a printed product are seriously damaged due to overhigh oxygen content. For example, the vacuum induction melting gas atomization and electrode induction melting gas atomization technologies are generally adopted for preparing spherical metal powder, the vacuum induction melting gas atomization has the problems of low electric energy conversion efficiency, high energy consumption and the like, and carbonization reaction is easy to occur when molten metal flows through a graphite material flow guide pipe at high temperature, so that the carbon content of the powder is increased, and the comprehensive performance of the powder is influenced; the electrode induction melting gas atomization technology has the problems that the liquid flow stability is not easy to control and the like, and meanwhile, the components of the electrode are analyzed due to uneven heating in the melting process, so that the components of the powder are uneven.
Therefore, there is an urgent need for a new method for preparing high spheroidization rate powder for 3D printing.
Disclosure of Invention
The invention aims to provide a low-oxygen europium nickel powder for 3D printing and a preparation method thereof, and the method can control the oxygen content and the element segregation in the whole alloy smelting process.
In order to achieve the above object, according to an aspect of the present invention, there is provided a method for preparing europium nickel powder having low oxygen content for 3D printing, comprising the steps of: s1, weighing equal-mass raw materials of europium and nickel, putting the raw materials into a clean vacuum suspension smelting furnace, vacuumizing a cavity of the vacuum suspension smelting furnace, and introducing argon for cleaning; s2, increasing current to melt the metal raw material under the cooling water circulation state, then reducing the current to cool the metal melt, repeating the steps to re-melt the cast ingot, and obtaining the low-oxygen europium nickel alloy cast ingot with equal mass ratio; and S3, cutting the low-oxygen europium nickel alloy cast ingot into small squares in a multi-line mode, crushing and roughly grinding the small squares to prepare coarse powder, and obtaining spherical powder through plasma gas atomization powder-making equipment.
According to the present invention, step S3 is followed by a step of surface treating the low-oxygen europium nickel alloy. Preferably, the surface treatment step includes sanding the surface of the low-oxygen europium nickel alloy to make the surface bright, and cleaning the surface with absolute ethyl alcohol after sanding.
According to the invention, the method also comprises a step of vacuum drying the low-oxygen europium nickel alloy after surface treatment, and the low-oxygen europium nickel alloy is placed into a vacuum drying oven with the vacuum degree of 3 Pa-5 Mpa and dried for 15-20 minutes at the temperature of 100-120 ℃.
According to the invention, the step of vacuumizing the chamber of the vacuum suspension smelting furnace and introducing argon for cleaning in the step S1 comprises the following steps: s11, opening the mechanical pump, roughing the valve, evacuating the air in the furnace, and reducing the pressure in the furnace to 10-20 Pa; s12, opening the front valve and the molecular pump, and allowing the rotation speed of the molecular pump to reach 25000-; s13, closing the rough pumping valve and opening the main pumping valve to reduce the pressure in the furnace to 5.7-7.7 x 10-3Pa; and S14, closing the main extraction valve, introducing argon gas with half atmospheric pressure, and cleaning the furnace body.
According to the invention, said step S2 comprises: s21, opening a normal temperature water pump and a cooling water pump to ensure that cooling water circulates in the smelting process; s22, opening a power supply box, increasing the current to 15-20A, and starting to increase the current at the rate of 5-10A when the raw materials of europium and nickel turn red to melt the metal raw materials; and S23, after the metal raw materials of europium and nickel are completely melted, reducing the current at the speed of 10-20A, and slowly cooling the metal melt. Preferably, the metal europium and the metal nickel are heated and remelted for 2-3 times. Preferably, the raw materials of europium and nickel are both square blocks, the size is 7 mm-10 mm, and the purity is 99.999%.
Preferably, the electromagnetic stirrer is started to stir in the remelting process so as to ensure the uniformity of the alloy smelting process, and the stirring current of the electromagnetic stirrer is 4-5A.
According to the invention, after the metal melt is cooled, the circulating water is closed, the air release valve is opened to balance the internal pressure and the external pressure, and the furnace door is opened for sampling.
According to the invention, a high-frequency induction plasma generator is adopted to provide plasma of the plasma gas atomization powder making equipment, the working power is 30-80 kw, the argon working flow is 20-50 slpm, the argon protective gas flow is 20-120 splm, and the powder feeding efficiency is 50-90 g/min.
According to another aspect of the present invention, there is also provided a low-oxygen europium nickel powder for 3D printing, prepared by any one of the above methods.
The invention has the beneficial effects that:
the invention adopts the vacuum suspension smelting process to prepare the low-oxygen europium-nickel powder for 3D printing, and controls the oxygen content and the element segregation in the alloy smelting process by keeping the vacuum and argon states in the whole smelting process, so that the elements are uniformly distributed in the alloy, and the conditions that the element content in a certain area is extremely high and the element content in a certain area is extremely low are avoided. Europium-nickel powder with excellent physical and mechanical properties is prepared by adopting a plasma atomization technology subsequently, and the plasma atomization has the following advantages: the atomization efficiency is high, and the metal melting and atomization processes are carried out simultaneously; the whole process is protected by inert atmosphere, which is beneficial to obtaining high-purity powder; the atomizing gas has higher temperature, can delay the solidification of particles and fully spheroidize; the fine powder has high yield and almost no satellite balls; narrow particle size distribution range and the like, advanced preparation process, accurate parameters and capability of being used for 3D printing to obtain products with high precision.
Drawings
Fig. 1 is an ingot diagram of a low-oxygen europium nickel alloy for 3D printing prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and embodiments. It should be emphasized that the specific embodiments described herein are merely illustrative of the invention, are some, not all, and therefore do not limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention provides a preparation method of low-oxygen europium nickel powder for 3D printing, which comprises the following steps:
s1, weighing raw materials of europium (Eu) and nickel (Ni) with equal mass, putting the raw materials into a clean vacuum suspension smelting furnace, vacuumizing a cavity of the vacuum suspension smelting furnace, and introducing argon for cleaning. Preferably, the raw materials of europium and nickel are both square blocks, the size is 7 mm-10 mm, and the purity is 99.999%. The step S1 of vacuumizing the chamber of the vacuum suspension smelting furnace and introducing argon for cleaning comprises the following steps: s11, opening the mechanical pump, roughing the valve, evacuating the air in the furnace, and reducing the pressure in the furnace to 10-20 Pa; s12, opening the front valve and the molecular pump, and allowing the rotation speed of the molecular pump to reach 25000-; s13, closing the rough pumping valve and opening the main pumping valve to reduce the pressure in the furnace to 5.7-7.7 x 10-3Pa; and S14, closing the main extraction valve, introducing argon gas at about half atmospheric pressure, and cleaning the furnace body.
And S2, increasing current to melt the metal raw material in a cooling water circulation state, then reducing the current to cool the metal melt, repeating the steps to remelt the cast ingot, closing the circulating water after the metal melt is cooled, opening a vent valve to balance the internal pressure and the external pressure, and opening a furnace door to sample to obtain the low-oxygen europium nickel alloy cast ingot with equal mass ratio.
Specifically, step S2 includes: s21, opening a normal temperature water pump and a cooling water pump to ensure that cooling water circulates in the smelting process; s22, opening a power supply box, increasing the current to 15-20A, and starting to increase the current at the rate of 5-10A when the raw materials of europium and nickel turn red to melt the metal raw materials; and S23, after the metal raw materials of europium and nickel are completely melted, reducing the current at the speed of 10-20A, and slowly cooling the metal melt. Preferably, the metal europium and the metal nickel are heated and remelted for 2-3 times. And starting the electromagnetic stirrer to stir in the remelting process to ensure the uniformity of the alloy smelting process, wherein the stirring current of the electromagnetic stirrer is 4-5A.
And S3, cutting the low-oxygen europium nickel alloy cast ingot into small squares in a multi-line mode, crushing and roughly grinding the small squares to prepare coarse powder, and obtaining spherical powder through plasma gas atomization powder-making equipment. Preferably, a high-frequency induction plasma generator is adopted to provide plasma of the plasma gas atomization powder making equipment, the working power is 30-80 kw, the argon working flow is 20-50 slpm, the argon protective gas flow is 20-120 splm, and the powder feeding efficiency is 50-90 g/min. High-speed and high-temperature plasma gas emitted by the plasma nozzle is used as an atomizing medium, so that feeding, melting and atomizing of metal raw materials are completed in the same step, the sphericity of powder is guaranteed, and the method can be used for 3D printing.
According to the present invention, step S3 is followed by a step of surface treating the low-oxygen europium nickel alloy. The surface treatment step comprises: and (3) polishing the surface of the low-oxygen europium nickel alloy by using sand paper to ensure that the surface is bright, and cleaning by using absolute ethyl alcohol after polishing. And (3) drying the surface-treated low-oxygen europium nickel alloy in vacuum, putting the dried low-oxygen europium nickel alloy into a vacuum drying oven with the vacuum degree of 3 Pa-5 Mpa, and drying for 15-20 minutes at the temperature of 100-120 ℃.
According to another aspect of the present invention, there is also provided a low-oxygen europium nickel powder for 3D printing, which is prepared by any one of the above methods. Preferably, the low-oxygen europium nickel powder has the characteristics of high spheroidization rate and the like.
The vacuum suspension furnace technology adopted by the invention is based on the vacuum induction melting technology, and utilizes the electromagnetic suspension force to make the metal molten pool in the crucible be in a suspension or quasi-suspension state, thereby eliminating the interaction between the molten pool and the crucible and preparing the material with high purity, uniform components and accuracy. The invention adopts the vacuum suspension furnace technology and has the following advantages: 1) the crucible material does not pollute furnace burden, and strong electromagnetic stirring is realized in the smelting process; 2) the reaction with the crucible can not occur and the furnace charge is hardly burnt; 3) the method can reach higher smelting temperature, has good product quality, less waste products and high yield, and can greatly reduce the preparation cost of the material; 4) the leftover materials can still keep high purity and can be recycled; 5) the crucible burning loss can not occur, the service life of the crucible is long, and the oxygen content of the smelted ingot can be effectively controlled when the smelting is carried out under the high vacuum condition.
Plasma atomization refers to a technology of injecting solid particles into inert gas plasma, completely evaporating the solid particles under the action of high temperature of the plasma, existing in a steam form, and then rapidly cooling the solid particles by using a gas quenching cooling technology to rapidly condense, nucleate and grow saturated steam to form ultrafine powder. The plasma atomization process is a unique process for producing active metal spherical micro powder, and parts produced by the plasma atomization process have excellent physical and mechanical properties due to the fact that the plasma atomization powder is fine.
The technical scheme of the invention is further explained by combining specific examples.
Example 1
Step S1: 400g (7mm) of europium metal square blocks and 400g (7mm) of nickel metal square blocks are weighed as reaction raw materials, and the purity of the square blocks is 99.999 percent.
Step S2: and opening the vacuum suspension smelting furnace, cleaning slag or dust in the furnace body, and then cleaning with absolute ethyl alcohol. Putting the metal square blank into a crucible, closing a furnace door, opening a rough pumping valve of a mechanical pump, evacuating the air in the furnace to reduce the pressure in the furnace to 10Pa, opening a pre-valve and a molecular pump, closing the rough pumping valve after the rotating speed of the molecular pump reaches 27000r/min, and opening a main pumping valve to reduce the pressure in the furnace to 6.7 multiplied by 10-3And Pa, closing the main pumping valve, introducing argon to clean the furnace body, and then opening a normal-temperature water pump and a cooling water pump to ensure the circulation of cooling water in the smelting process.
Step S3: and opening a power supply box, increasing the current to 20A, observing the condition of the metal square in the crucible, waiting for the metal square to turn red, increasing the current according to 10A each time so that the metal raw material starts to melt, and melting all the metal raw material along with the slow increase of the current. The current is reduced by 15A each time so that the metal melt in the crucible is slowly cooled down, during which the circulating water is always in operation. And remelting the ingot by the same method after the ingot is cooled, and repeating the step for 2-3 times. And closing circulating water, opening an air release valve to balance internal pressure and external pressure, opening a furnace door for sampling, and smelting to obtain the europium-nickel alloy with equal mass ratio. And (3) polishing the surface of the europium-nickel alloy by using sand paper to enable the surface of the europium-nickel alloy to be bright, cleaning the polished europium-nickel alloy by using absolute ethyl alcohol, and drying the surface-treated europium-nickel alloy in a vacuum drying oven at the temperature of 120 ℃ and the vacuum degree of 3Pa for 15 min.
Step S4: cutting the europium-nickel alloy ingot into small squares in equal mass ratio, crushing and coarsely grinding the small squares to prepare coarse powder. The method comprises the steps of enabling coarse powder to pass through plasma gas atomization powder making equipment to obtain spherical powder, enabling a high-frequency induction plasma generator to provide plasma, enabling the working power to be 50kw, the argon working flow to be 30slpm, enabling the flow of argon protective gas to be 90splm, enabling the powder feeding efficiency of the equipment to be 60g/min, obtaining metal powder with high spheroidization rate after ball milling treatment, and enabling the metal powder to be used for 3D printing.
Step S5: and (4) sending the spherical powder prepared in the step S4 into a 3D printing device, modeling through computer modeling software, and partitioning the built three-dimensional model into sections layer by layer. And leading the established model into 3D printing equipment, spraying powder onto a workbench, wherein the heating temperature of the workbench is 300 ℃, and gradually accumulating the powder sprayed onto the workbench due to the heating action until the product is printed.
The europium-nickel powder prepared in example 1 was tested for its oxygen content, which was 300ppm, using a glow discharge mass spectrometer.
The foregoing is only a preferred application of the present invention, and it should be noted that, for those skilled in the art, various modifications and improvements can be made without departing from the technical principle of the present invention, and these modifications and improvements should also be considered as the protection scope of the present invention.
Claims (9)
1. A preparation method of low-oxygen europium nickel powder for 3D printing is characterized by comprising the following steps:
s1, weighing equal-mass raw materials of europium and nickel, putting the raw materials into a clean vacuum suspension smelting furnace, vacuumizing a cavity of the vacuum suspension smelting furnace, and introducing argon for cleaning;
s2, increasing current to melt the metal raw material under the cooling water circulation state, then reducing the current to cool the metal melt, repeating the steps to re-melt the cast ingot, and obtaining the low-oxygen europium nickel alloy cast ingot with equal mass ratio;
and S3, cutting the low-oxygen europium nickel alloy cast ingot into small squares in a multi-line mode, crushing and roughly grinding the small squares to prepare coarse powder, and obtaining spherical powder through plasma gas atomization powder-making equipment.
2. The method of claim 1, further comprising a step of surface treating the europium-reduced nickel alloy after step S3.
Preferably, the surface treatment step includes sanding the surface of the low-oxygen europium nickel alloy to make the surface bright, and cleaning the surface with absolute ethyl alcohol after sanding.
3. The preparation method according to claim 2, further comprising a step of vacuum drying the surface-treated low-oxygen europium-nickel alloy, wherein the surface-treated low-oxygen europium-nickel alloy is placed in a vacuum drying oven with a vacuum degree of 3Pa to 5MPa, and dried at 100 ℃ to 120 ℃ for 15 to 20 minutes.
4. The preparation method according to claim 1, wherein the step of vacuumizing and introducing argon gas to clean the chamber of the vacuum suspension smelting furnace in the step S1 comprises the following steps:
s11, opening the mechanical pump, roughing the valve, evacuating the air in the furnace, and reducing the pressure in the furnace to 10-20 Pa;
s12, opening the front valve and the molecular pump, and allowing the rotation speed of the molecular pump to reach 25000-;
s13, closing the rough pumping valve and opening the main pumping valve to reduce the pressure in the furnace to 5.7-7.7 x 10-3Pa；
And S14, closing the main extraction valve, introducing argon gas with half atmospheric pressure, and cleaning the furnace body.
5. The production method according to claim 1 or 2, wherein the step S2 includes:
s21, opening a normal temperature water pump and a cooling water pump to ensure that cooling water circulates in the smelting process;
s22, opening a power supply box, increasing the current to 15-20A, and starting to increase the current at the rate of 5-10A when the raw materials of europium and nickel turn red to melt the metal raw materials;
and S23, after the metal raw materials of europium and nickel are completely melted, reducing the current at the speed of 10-20A, and slowly cooling the metal melt.
Preferably, the metal europium and the metal nickel are heated and remelted for 2-3 times.
Preferably, the raw materials of europium and nickel are both square blocks, the size is 7 mm-10 mm, and the purity is 99.999%.
6. The preparation method according to claim 1, wherein stirring of the electromagnetic stirrer is started during remelting so as to ensure uniformity of an alloy smelting process, and the stirring current of the electromagnetic stirrer is 4A-5A.
7. The preparation method according to claim 1, wherein after the metal melt is cooled, the circulating water is closed, the air release valve is opened to balance the internal pressure and the external pressure, and the furnace door is opened for sampling.
8. The preparation method of claim 1, wherein a high-frequency induction plasma generator is adopted to provide plasma of the plasma gas atomization powder preparation device, the working power is 30-80 kw, the argon working flow is 20-50 slpm, the argon protective gas flow is 20-120 splm, and the powder feeding efficiency is 50-90 g/min.
9. A low-oxygen europium nickel powder for 3D printing, prepared by the method of any one of claims 1 to 8.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011082595A1 (en) * | 2010-01-05 | 2011-07-14 | 北京科技大学 | Method for preparing superfine spherical neodymium-iron-boron powder |
| CN105057689A (en) * | 2015-08-19 | 2015-11-18 | 山西卓锋钛业有限公司 | Device and method for preparing superfine micro-spherical titanium powder for 3D printing |
| CN106334791A (en) * | 2016-10-24 | 2017-01-18 | 贵州省钛材料研发中心有限公司 | Production method for spherical titanium powder for 3D printing |
| CN106334799A (en) * | 2016-11-21 | 2017-01-18 | 张森 | Method for producing metal powder |
| WO2018121688A1 (en) * | 2016-12-29 | 2018-07-05 | 江民德 | 3d printing spherical powder preparation method utilizing plasma |
| CN110396613A (en) * | 2019-08-13 | 2019-11-01 | 南京理工大学 | A kind of preparation method of the titanium-zirconium alloy applied to tooth root planting body |
-
2020
- 2020-08-31 CN CN202010898639.1A patent/CN114101693A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011082595A1 (en) * | 2010-01-05 | 2011-07-14 | 北京科技大学 | Method for preparing superfine spherical neodymium-iron-boron powder |
| CN105057689A (en) * | 2015-08-19 | 2015-11-18 | 山西卓锋钛业有限公司 | Device and method for preparing superfine micro-spherical titanium powder for 3D printing |
| CN106334791A (en) * | 2016-10-24 | 2017-01-18 | 贵州省钛材料研发中心有限公司 | Production method for spherical titanium powder for 3D printing |
| CN106334799A (en) * | 2016-11-21 | 2017-01-18 | 张森 | Method for producing metal powder |
| WO2018121688A1 (en) * | 2016-12-29 | 2018-07-05 | 江民德 | 3d printing spherical powder preparation method utilizing plasma |
| CN110396613A (en) * | 2019-08-13 | 2019-11-01 | 南京理工大学 | A kind of preparation method of the titanium-zirconium alloy applied to tooth root planting body |
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