CN109261977B - Metal powder for 3D printing of ultrasonic refined grains and preparation method thereof - Google Patents
Metal powder for 3D printing of ultrasonic refined grains and preparation method thereof Download PDFInfo
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- CN109261977B CN109261977B CN201811445981.5A CN201811445981A CN109261977B CN 109261977 B CN109261977 B CN 109261977B CN 201811445981 A CN201811445981 A CN 201811445981A CN 109261977 B CN109261977 B CN 109261977B
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 177
- 239000002184 metal Substances 0.000 title claims abstract description 177
- 239000000843 powder Substances 0.000 title claims abstract description 72
- 238000010146 3D printing Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 69
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000007711 solidification Methods 0.000 claims abstract description 21
- 230000008023 solidification Effects 0.000 claims abstract description 21
- 239000011159 matrix material Substances 0.000 claims abstract description 9
- 238000005266 casting Methods 0.000 claims abstract description 5
- 229910000838 Al alloy Inorganic materials 0.000 claims description 81
- 239000000523 sample Substances 0.000 claims description 69
- 239000000956 alloy Substances 0.000 claims description 48
- 229910045601 alloy Inorganic materials 0.000 claims description 47
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 45
- 229910052782 aluminium Inorganic materials 0.000 claims description 41
- 238000007670 refining Methods 0.000 claims description 25
- 239000002893 slag Substances 0.000 claims description 24
- 239000010953 base metal Substances 0.000 claims description 19
- 238000002844 melting Methods 0.000 claims description 15
- 230000008018 melting Effects 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 12
- 239000011362 coarse particle Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000003723 Smelting Methods 0.000 abstract description 13
- 239000013078 crystal Substances 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 5
- 229910001338 liquidmetal Inorganic materials 0.000 abstract description 2
- 238000005058 metal casting Methods 0.000 abstract 2
- 239000003795 chemical substances by application Substances 0.000 description 17
- 238000004512 die casting Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 239000000155 melt Substances 0.000 description 10
- 238000003801 milling Methods 0.000 description 10
- 238000010907 mechanical stirring Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B22F1/0003—
-
- 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
- C22C1/026—Alloys based on aluminium
-
- 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
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- 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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
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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)
- Powder Metallurgy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses metal powder for 3D printing of ultrasonic refined crystal grains and a preparation method thereof; the preparation method uses one-time ultrasonic treatment in the metal smelting process to promote the grain refiner to be more uniformly melted in the liquid of the matrix metal, and uses the ultrasonic treatment again in the solidification process to refine grains in the ingot casting solidification process; through two times of ultrasonic treatment, the solidification structure of the cast ingot is changed from thick columnar crystal into uniform and fine isometric crystal, the cavitation effect generated by the ultrasonic wave can promote the generation of liquid metal mesonucleus, and the macrosegregation and the microsegregation of the cast ingot can be improved; the prepared metal powder has small microscopic grains, and the prepared metal casting has high mechanical property, so that the mechanical property of the prepared metal casting is fundamentally improved.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of 3D printing, and relates to metal powder for 3D printing of ultrasonic refined grains and a preparation method thereof.
[ background of the invention ]
The mechanical properties of the metal material mainly depend on the internal structure and structure, and an important characteristic parameter in the structure is the grain size, so that grain size refinement and grain size control are particularly important. At present, two methods for refining grains are mainly used, one is to add a grain refiner into a metal melt, and the other is to adopt a physical vibration method. The kinds of grain refiner are limited, and like commercial Al-Ti-B master alloy commonly used in aluminum and aluminum alloy, the grain refiner cannot be used for grain refinement of high-purity aluminum, and can not effectively inhibit solidification segregation of some alloys. For magnesium and magnesium alloy, the grain refining effect and various limitations are particularly outstanding, and some of the magnesium and magnesium alloy even have no grain refiner, so when the variety of the grain refiner can not relate to all metals and alloys, the applicability of the physical vibration method is the widest, and the ultrasonic vibration is the most advanced technology and has great application prospect and research value.
[ summary of the invention ]
The invention aims to overcome the defects of the prior art and provides the metal powder for the ultrasonic thinning 3D printing and the preparation method thereof; according to the invention, ultrasonic vibration is applied in the preparation process of the metal powder, so that the crystal grains of the metal powder for 3D printing are refined, and the mechanical properties of the metal material for 3D printing are fundamentally optimized.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a preparation method of metal powder for 3D printing of ultrasonic refined grains comprises the following steps:
(1) melting aluminum or aluminum alloy to obtain molten aluminum or aluminum alloy liquid serving as matrix molten metal A;
(2) adding any one of Al-Ti-C series intermediate alloys into the base metal melt A obtained in the step (1); stirring the mixture after adding the intermediate alloy until the intermediate alloy is completely melted to obtain a base metal melt added with the intermediate alloy, namely a metal melt B;
(3) carrying out ultrasonic treatment on the molten metal B to obtain molten metal C;
(4) removing dross on the surface in the molten metal C obtained in the step (3) by using a slag remover to obtain molten metal D;
(5) casting the molten metal D into a metal mold, and cooling to obtain a cast ingot;
(6) and crushing and fine grinding the cast ingot to obtain aluminum or aluminum alloy powder containing Al-Ti-C series intermediate alloy with a particle size of-200 to +500 meshes, wherein the aluminum or aluminum alloy powder is ultrasonically refined metal powder for 3D printing.
The invention is further improved in that:
preferably, in the step (1), the melting temperature of the aluminum or the aluminum alloy is 750 ℃, and after the aluminum or the aluminum alloy is melted, the temperature is kept for 30min, so that the matrix metal melt A is obtained.
Preferably, in the step (2), the equivalent of Ti in the Al-Ti-C series master alloy accounts for 20-200 ppm of the aluminum or the aluminum alloy in the step (1).
Preferably, in the step (2), the master alloy is added into the base metal melt A and then stirred for 5-10 min.
Preferably, in the step (3), the specific process of the ultrasonic treatment is as follows: lowering an ultrasonic probe of an ultrasonic device to a position above the molten metal B, contacting the molten metal B with the liquid level of the molten metal B, and preheating the molten metal B until the temperature of the ultrasonic probe reaches 750 ℃; and continuously descending the probe to 10-15 mm below the liquid level of the molten metal, and carrying out ultrasonic treatment on the molten metal.
Preferably, in the step (3), the probe is lowered to 10-15 mm below the liquid level of the molten liquid, heat preservation is carried out for 5min, and ultrasonic treatment is carried out for 5-10 min.
Preferably, in the step (4), the slag remover is added, and dross on the surface of the molten metal is removed after refining for 10min, so as to obtain the molten metal D.
Preferably, in the step (5), after the molten metal D is cast into the metal mold, the ultrasonic probe of the ultrasonic device is lowered into the molten metal of the mold; and (3) gradually moving the ultrasonic probe upwards along with the solidification of the metal liquid D, continuously applying ultrasonic waves in the upward moving process until the metal is completely solidified, and lifting the ultrasonic probe out of the cast ingot before the metal is completely solidified.
Preferably, in the step (6), after the ingot casting is crushed, coarse particles with a size of more than 100 meshes are removed by a sieve; the aluminum or aluminum alloy powder containing Al-Ti-C intermediate alloy is obtained in a size of-200 to +500 mesh by fine grinding.
The metal powder for 3D printing of the ultrasonic refined grains prepared by any one of the preparation methods.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of metal powder for 3D printing of ultrasonic refined crystal grains; the preparation method uses one-time ultrasonic treatment in the metal smelting process to promote the grain refiner to be more uniformly melted in the melt of the matrix metal, and uses the ultrasonic treatment again in the solidification process to refine grains in the ingot casting solidification process; through two times of ultrasonic treatment, the solidification structure of the cast ingot is changed from thick columnar crystal into uniform and fine isometric crystal, the cavitation effect generated by the ultrasonic wave can promote the generation of liquid metal mesonucleus, and the macrosegregation and the microsegregation of the cast ingot can be improved; the method simultaneously avoids the problem of adding the refiner into the softer matrix powder of aluminum and aluminum alloy by adopting mechanical ball milling, and provides an idea for adding the refiner into the softer matrix metal powder; the method can prepare the base powder containing the refiner in a large batch, has obvious effect on refining the crystal grains of the aluminum and the aluminum alloy, can refine the crystal grains of the aluminum and the aluminum alloy to a large extent by adding a small amount of the intermediate alloy, reduces the manufacturing cost, and has great significance and application value on the grain refinement of the aluminum and the aluminum alloy and the family metal.
The invention also discloses the ultrasonically refined metal powder for 3D printing, the refiner is added into the matrix metal powder, and the ultrasonic treatment is carried out twice, so that the prepared metal powder has fine microscopic grains, the mechanical property of the prepared metal part is high, and the mechanical property of the prepared metal part is fundamentally improved.
[ description of the drawings ]
FIG. 1 is a macroscopic view of an ultrasonic pure Al ingot of a comparative example of the present invention;
FIG. 2 is a macroscopic view of an ingot containing 25ppm pure Al in terms of equivalent weight of Ti, which is obtained by ultrasonic processing in example 1 of the present invention;
[ detailed description ] embodiments
The invention is further described in detail with reference to specific steps, and discloses metal powder for 3D printing of ultrasonic refined grains and a preparation method thereof, wherein the preparation method specifically comprises the following steps:
(1) melting the base metal: placing aluminum or aluminum alloy materials into a crucible, wherein the aluminum alloy can be any aluminum alloy, such as 7050 and 7075; and putting the crucible into a crucible type resistance smelting furnace, heating to 750 ℃, and preserving heat for 30min after the aluminum material is completely melted to obtain molten aluminum or aluminum alloy liquid, namely molten base metal liquid A.
(2) Adding an intermediate alloy: adding any one of grain refiner Al-Ti-C series intermediate alloys such as Al-5Ti-1C, Al-3Ti-1C and Al-3Ti-0.15C into molten matrix metal liquid; the addition amount of the refiner is calculated according to the equivalent of Ti in the master alloy, namely the equivalent of Ti in the master alloy accounts for 25-200 ppm of the weight of the aluminum or the aluminum alloy in the step (1); and (3) after the intermediate alloy is added, mechanically stirring for 5-10 min by using a stirring rod to fully melt the grain refiner, so as to obtain a base metal melt added with the intermediate alloy, namely a metal melt B.
(3) Ultrasonic treatment: and (3) lowering an ultrasonic probe of the ultrasonic device to be in contact with the liquid level of the molten liquid, preheating the ultrasonic probe (preventing splashing of the molten liquid), continuing to lower the probe to 10-15 mm below the liquid level of the molten liquid after the temperature of the probe is 750 ℃, keeping the temperature for 5min again, and then carrying out ultrasonic treatment at the temperature of 750 ℃ for 5-10 min to obtain the molten metal C after the ultrasonic treatment.
(4) Refining and deslagging: and adding a slag remover into the molten metal C, wherein the adding amount of the slag remover is 1g of the slag remover added into every 500g of the molten metal C, and removing dross on the surface of the molten metal after refining for 10min to obtain the molten metal D.
(5) Die casting: pouring the melt subjected to ultrasonic treatment into a prepared metal mold, and simultaneously: the ultrasonic probe of the ultrasonic device is lowered to be below the liquid level of the molten metal, and the lowest part of the cast ingot is firstly solidified due to the fact that metal solidification is from outside to inside, so that the ultrasonic probe gradually moves upwards along with the solidification of the metal, ultrasonic waves are continuously applied in the process of moving upwards until the metal is completely solidified, and the ultrasonic probe is also lifted out of the metal before the metal is completely solidified; while forming an ingot. Because a certain amount of Al-Ti-C intermediate alloy is added into the molten aluminum and aluminum alloy and ultrasonic waves are applied in the solidification process, the crystal grains of the molten aluminum and aluminum alloy can obtain the effect of in-situ/synchronous double refinement in the solidification process of the molten aluminum and aluminum alloy.
(6) Milling: crushing the cast ingot by a press machine, removing coarse powder particles with a size of more than 100 meshes by a sieve, and then finely grinding to obtain aluminum or aluminum alloy powder containing Al-Ti-C series intermediate alloy with a size of-200 to +500 meshes, wherein the aluminum or aluminum alloy powder is metal powder for ultrasonic thinning 3D printing.
The prepared powder is printed on a 3D printer, and because the laid powder is refined by Al-Ti-C intermediate alloy and ultrasonic vibration treatment, the printed parts can obtain finer aluminum alloy grains on the basis of the refined powder under the melting action of laser beams, so that the mechanical property of printed parts is greatly improved.
FIG. 1 is a macroscopic view of a comparative example ultrasonic pure Al ingot in accordance with the present invention; FIG. 2 is a macroscopic view of an ingot containing 25ppm pure Al in equivalent of Ti in the ultrasound of example 1 of the present invention; comparing fig. 1 and fig. 2, it can be seen that the crystal grains of the whole ingot in fig. 2 are uniformly distributed under the same condition of the whole smelting process, and particularly, the crystal grains in the central part of the ultrasonically treated ingot are obviously finer and more uniform compared with the crystal grains of the ingot which are not ultrasonically treated.
Comparative example:
(1) melting the base metal: and putting the aluminum into a crucible, putting the crucible into a crucible type resistance smelting furnace, heating to 750 ℃, and preserving heat for 30min after the aluminum is completely melted to obtain molten aluminum liquid.
(2) Adding an intermediate alloy: adding Al-5Ti-1C into the aluminum liquid, wherein the equivalent weight of Ti in the Al-5Ti-1C accounts for 25ppm of the mass of the aluminum in the step (1); after addition, mechanical stirring was carried out for 8min by a stir bar.
(2) Refining and deslagging: adding a certain amount of slag removing agent into the molten liquid, refining for 10min, and removing the dross on the surface of the molten liquid.
(5) Die casting: pouring the refined molten liquid into a prepared metal mold, and solidifying the metal to form an ingot; the ingot in this example was cut, and the grain pattern thereof is shown in fig. 1.
(6) Milling: crushing the cast ingot by a press machine, removing coarse powder particles with a size of more than 100 meshes by using a screen, and then finely grinding to obtain aluminum powder containing Al-Ti-C intermediate alloy with a size of-200 to +500 meshes, wherein the aluminum powder is metal powder for 3D printing;
example 1
(1) Melting the base metal: and putting the aluminum into a crucible, putting the crucible into a crucible type resistance smelting furnace, heating to 750 ℃, and preserving heat for 30min after the aluminum is completely melted to obtain molten aluminum liquid.
(2) Adding an intermediate alloy: adding Al-5Ti-1C into the aluminum liquid, wherein the equivalent weight of Ti in the Al-5Ti-1C accounts for 25ppm of the mass of aluminum in the step (1); after addition, mechanical stirring was carried out for 8min by a stir bar.
(3) Ultrasonic treatment: and (3) lowering an ultrasonic probe of the ultrasonic device to be in contact with the liquid level of the molten liquid, preheating until the temperature of the probe is 750 ℃, continuing to lower the probe to be 10mm below the liquid level of the molten liquid, preserving heat for 5min again, and carrying out ultrasonic treatment for 10 min.
(4) Refining and deslagging: adding slag removing agent into the molten metal, adding 1g of slag removing agent into every 500g of molten metal C, refining for 10min, and removing the dross on the surface of the molten metal.
(5) Die casting: pouring the melt subjected to ultrasonic treatment into a prepared metal mold, and simultaneously: and (3) lowering an ultrasonic probe of the ultrasonic device below the liquid level of the molten metal, gradually moving the ultrasonic probe upwards along with the solidification of the metal, continuously applying ultrasonic waves in the process of moving upwards until the metal is completely solidified, and before the metal is completely solidified, taking the ultrasonic probe out of the metal to form an ingot. The ingot in this example was cut, and the grain pattern thereof is shown in fig. 2.
(6) Milling: crushing the cast ingot by a press machine, removing coarse powder particles with a size of more than 100 meshes by a sieve, and then finely grinding to obtain aluminum powder containing Al-Ti-C intermediate alloy with a size of-200 to +500 meshes, wherein the aluminum powder is ultrasonically refined metal powder for 3D printing.
Example 2
(1) Melting the base metal: and (3) putting the aluminum alloy 7075 into a crucible, putting the crucible into a crucible type resistance smelting furnace, heating to 750 ℃, and preserving heat for 30min after the aluminum alloy 7075 is completely melted to obtain molten aluminum alloy solution.
(2) Adding an intermediate alloy: adding Al-5Ti-1C into the aluminum alloy melt, wherein the equivalent weight of Ti in the Al-5Ti-1C accounts for 50ppm of the mass of the aluminum alloy in the step (1); after the addition, mechanical stirring was carried out for 10min by a stirring rod.
(3) Ultrasonic treatment: and (3) lowering an ultrasonic probe of the ultrasonic device to be in contact with the liquid level of the molten liquid, preheating until the temperature of the probe is 750 ℃, continuing to lower the probe to 15mm below the liquid level of the molten liquid, preserving heat for 5min again, and carrying out ultrasonic treatment for 5 min.
(4) Refining and deslagging: adding slag removing agent into the molten metal, adding 1g of slag removing agent into every 500g of molten metal, refining for 10min, and removing the dross on the surface of the molten metal.
(5) Die casting: pouring the melt subjected to ultrasonic treatment into a prepared metal mold, and simultaneously: and (3) lowering an ultrasonic probe of the ultrasonic device below the liquid level of the molten metal, gradually moving the ultrasonic probe upwards along with the solidification of the metal, continuously applying ultrasonic waves in the process of moving upwards until the metal is completely solidified, and before the metal is completely solidified, taking the ultrasonic probe out of the metal to form an ingot.
(6) Milling: and crushing the cast ingot by a press machine, removing coarse powder particles with a size of more than 100 meshes by using a screen, and then finely grinding to obtain aluminum alloy powder containing Al-Ti-C intermediate alloy with a size of-200 to +500 meshes, wherein the aluminum alloy powder is ultrasonically refined metal powder for 3D printing.
Example 3
(1) Melting the base metal: and (3) putting the aluminum alloy 7050 into a crucible, putting the crucible into a crucible type resistance smelting furnace, heating to 750 ℃, and preserving heat for 30min after the aluminum alloy 7050 is completely melted to obtain molten aluminum alloy solution.
(2) Adding an intermediate alloy: adding Al-3Ti-1C into the aluminum alloy melt, wherein the Ti equivalent of the Al-3Ti-1C accounts for 70ppm of the mass of the aluminum alloy in the step (1); after the addition, mechanical stirring was carried out for 5min by a stirring rod.
(3) Ultrasonic treatment: and (3) lowering an ultrasonic probe of the ultrasonic device to be in contact with the liquid level of the molten liquid, preheating until the temperature of the probe is 750 ℃, continuing to lower the probe to 12mm below the liquid level of the molten liquid, preserving heat for 5min again, and carrying out ultrasonic treatment for 8 min.
(4) Refining and deslagging: adding slag removing agent into the molten metal, adding 1g of slag removing agent into every 500g of molten metal, refining for 10min, and removing the dross on the surface of the molten metal.
(5) Die casting: pouring the melt subjected to ultrasonic treatment into a prepared metal mold, and simultaneously: and (3) lowering an ultrasonic probe of the ultrasonic device below the liquid level of the molten metal, gradually moving the ultrasonic probe upwards along with the solidification of the metal, continuously applying ultrasonic waves in the process of moving upwards until the metal is completely solidified, and before the metal is completely solidified, taking the ultrasonic probe out of the metal to form an ingot.
(6) Milling: and crushing the cast ingot by a press machine, removing coarse powder particles with a size of more than 100 meshes by using a screen, and then finely grinding to obtain aluminum alloy powder containing Al-Ti-C intermediate alloy with a size of-200 to +500 meshes, wherein the aluminum alloy powder is ultrasonically refined metal powder for 3D printing.
Example 4
(1) Melting the base metal: and (3) putting the aluminum alloy 7075 into a crucible, putting the crucible into a crucible type resistance smelting furnace, heating to 750 ℃, and preserving heat for 30min after the aluminum alloy 7075 is completely melted to obtain molten aluminum alloy solution.
(2) Adding an intermediate alloy: adding Al-3Ti-0.15C into the aluminum alloy melt, wherein the equivalent weight of Ti in the Al-3Ti-0.15C accounts for 100ppm of the mass of the aluminum alloy in the step (1); after the addition, mechanical stirring was carried out for 5min by a stirring rod.
(3) Ultrasonic treatment: and (3) lowering an ultrasonic probe of the ultrasonic device to be in contact with the liquid level of the molten liquid, preheating until the temperature of the probe is 750 ℃, continuing to lower the probe to 13mm below the liquid level of the molten liquid, preserving heat for 5min again, and carrying out ultrasonic treatment for 9 min.
(4) Refining and deslagging: adding slag removing agent into the molten metal, adding 1g of slag removing agent into every 500g of molten metal, refining for 10min, and removing the dross on the surface of the molten metal.
(5) Die casting: pouring the melt subjected to ultrasonic treatment into a prepared metal mold, and simultaneously: and (3) lowering an ultrasonic probe of the ultrasonic device below the liquid level of the molten metal, gradually moving the ultrasonic probe upwards along with the solidification of the metal, continuously applying ultrasonic waves in the process of moving upwards until the metal is completely solidified, and before the metal is completely solidified, taking the ultrasonic probe out of the metal to form an ingot.
(6) Milling: and crushing the cast ingot by a press machine, removing coarse powder particles with a size of more than 100 meshes by using a screen, and then finely grinding to obtain aluminum alloy powder containing Al-Ti-C intermediate alloy with a size of-200 to +500 meshes, wherein the aluminum alloy powder is ultrasonically refined metal powder for 3D printing.
Example 5
(1) Melting the base metal: and (3) putting the aluminum alloy 7050 into a crucible, putting the crucible into a crucible type resistance smelting furnace, heating to 750 ℃, and preserving heat for 30min after the aluminum alloy 7050 is completely melted to obtain molten aluminum alloy solution.
(2) Adding an intermediate alloy: adding Al-3Ti-0.15C into the aluminum alloy melt, wherein the equivalent weight of Ti in the Al-3Ti-0.15C accounts for 150ppm of the mass of the aluminum alloy in the step (1); after the addition, mechanical stirring was carried out for 10min by a stirring rod.
(3) Ultrasonic treatment: and (3) lowering an ultrasonic probe of the ultrasonic device to be in contact with the liquid level of the molten liquid, preheating until the temperature of the probe is 750 ℃, continuing to lower the probe to be 10mm below the liquid level of the molten liquid, preserving heat for 5min again, and carrying out ultrasonic treatment for 7 min.
(4) Refining and deslagging: adding slag removing agent into the molten metal, adding 1g of slag removing agent into every 500g of molten metal, refining for 10min, and removing the dross on the surface of the molten metal.
(5) Die casting: pouring the melt subjected to ultrasonic treatment into a prepared metal mold, and simultaneously: and (3) lowering an ultrasonic probe of the ultrasonic device below the liquid level of the molten metal, gradually moving the ultrasonic probe upwards along with the solidification of the metal, continuously applying ultrasonic waves in the process of moving upwards until the metal is completely solidified, and before the metal is completely solidified, taking the ultrasonic probe out of the metal to form an ingot.
(6) Milling: and crushing the cast ingot by a press machine, removing coarse powder particles with a size of more than 100 meshes by using a screen, and then finely grinding to obtain aluminum alloy powder containing Al-Ti-C intermediate alloy with a size of-200 to +500 meshes, wherein the aluminum alloy powder is ultrasonically refined metal powder for 3D printing.
Example 6
(1) Melting the base metal: and (3) putting the aluminum alloy 7075 into a crucible, putting the crucible into a crucible type resistance smelting furnace, heating to 750 ℃, and preserving heat for 30min after the aluminum alloy 7075 is completely melted to obtain molten aluminum alloy solution.
(2) Adding an intermediate alloy: adding Al-3Ti-1C into the aluminum alloy melt, wherein the equivalent weight of Ti in the Al-3Ti-1C accounts for 200ppm of the mass of the aluminum alloy in the step (1); after addition, mechanical stirring was carried out for 8min by a stir bar.
(3) Ultrasonic treatment: and (3) lowering an ultrasonic probe of the ultrasonic device to be in contact with the liquid level of the molten liquid, preheating until the temperature of the probe is 750 ℃, continuing to lower the probe to 15mm below the liquid level of the molten liquid, preserving heat for 5min again, and carrying out ultrasonic treatment for 7 min.
(4) Refining and deslagging: adding slag removing agent into the molten metal, adding 1g of slag removing agent into every 500g of molten metal, refining for 10min, and removing the dross on the surface of the molten metal.
(5) Die casting: pouring the melt subjected to ultrasonic treatment into a prepared metal mold, and simultaneously: and (3) lowering an ultrasonic probe of the ultrasonic device below the liquid level of the molten metal, gradually moving the ultrasonic probe upwards along with the solidification of the metal, continuously applying ultrasonic waves in the process of moving upwards until the metal is completely solidified, and before the metal is completely solidified, taking the ultrasonic probe out of the metal to form an ingot.
(6) Milling: and crushing the cast ingot by a press machine, removing coarse powder particles with a size of more than 100 meshes by using a screen, and then finely grinding to obtain aluminum alloy powder containing Al-Ti-C intermediate alloy with a size of-200 to +500 meshes, wherein the aluminum alloy powder is ultrasonically refined metal powder for 3D printing.
Example 7
(1) Melting the base metal: and (3) putting the aluminum alloy 7050 into a crucible, putting the crucible into a crucible type resistance smelting furnace, heating to 750 ℃, and preserving heat for 30min after the aluminum alloy 7050 is completely melted to obtain molten aluminum alloy solution.
(2) Adding an intermediate alloy: adding Al-3Ti-1C into the aluminum alloy melt, wherein the equivalent weight of Ti in the Al-3Ti-1C accounts for 20ppm of the mass of the aluminum alloy in the step (1); after the addition, mechanical stirring was carried out for 5min by a stirring rod.
(3) Ultrasonic treatment: and (3) lowering an ultrasonic probe of the ultrasonic device to be in contact with the liquid level of the molten liquid, preheating until the temperature of the probe is 750 ℃, continuing to lower the probe to 13mm below the liquid level of the molten liquid, preserving heat for 5min again, and carrying out ultrasonic treatment for 5 min.
(4) Refining and deslagging: adding slag removing agent into the molten metal, adding 1g of slag removing agent into every 500g of molten metal, refining for 10min, and removing the dross on the surface of the molten metal.
(5) Die casting: pouring the melt subjected to ultrasonic treatment into a prepared metal mold, and simultaneously: and (3) lowering an ultrasonic probe of the ultrasonic device below the liquid level of the molten metal, gradually moving the ultrasonic probe upwards along with the solidification of the metal, continuously applying ultrasonic waves in the process of moving upwards until the metal is completely solidified, and before the metal is completely solidified, taking the ultrasonic probe out of the metal to form an ingot.
(6) Milling: and crushing the cast ingot by a press machine, removing coarse powder particles with a size of more than 100 meshes by using a screen, and then finely grinding to obtain aluminum alloy powder containing Al-Ti-C intermediate alloy with a size of-200 to +500 meshes, wherein the aluminum alloy powder is ultrasonically refined metal powder for 3D printing.
Example 8
(1) Melting the base metal: and (3) putting the aluminum alloy 7075 into a crucible, putting the crucible into a crucible type resistance smelting furnace, heating to 750 ℃, and preserving heat for 30min after the aluminum alloy 7075 is completely melted to obtain molten aluminum alloy solution.
(2) Adding an intermediate alloy: adding Al-5Ti-1C into the aluminum alloy melt, wherein the equivalent weight of Ti in the Al-5Ti-1C accounts for 200ppm of the mass of the aluminum alloy in the step (1); after the addition, mechanical stirring was carried out for 10min by a stirring rod.
(3) Ultrasonic treatment: and (3) lowering an ultrasonic probe of the ultrasonic device to be in contact with the liquid level of the molten liquid, preheating until the temperature of the probe is 750 ℃, continuing to lower the probe to 12mm below the liquid level of the molten liquid, preserving heat for 5min again, and carrying out ultrasonic treatment for 10 min.
(4) Refining and deslagging: adding slag removing agent into the molten metal, adding 1g of slag removing agent into every 500g of molten metal, refining for 10min, and removing the dross on the surface of the molten metal.
(5) Die casting: pouring the melt subjected to ultrasonic treatment into a prepared metal mold, and simultaneously: and (3) lowering an ultrasonic probe of the ultrasonic device below the liquid level of the molten metal, gradually moving the ultrasonic probe upwards along with the solidification of the metal, continuously applying ultrasonic waves in the process of moving upwards until the metal is completely solidified, and before the metal is completely solidified, taking the ultrasonic probe out of the metal to form an ingot.
(6) Milling: and crushing the cast ingot by a press machine, removing coarse powder particles with a size of more than 100 meshes by using a screen, and then finely grinding to obtain aluminum alloy powder containing Al-Ti-C intermediate alloy with a size of-200 to +500 meshes, wherein the aluminum alloy powder is ultrasonically refined metal powder for 3D printing.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A preparation method of metal powder for 3D printing of ultrasonic refined grains is characterized by comprising the following steps:
(1) melting aluminum or aluminum alloy to obtain molten aluminum or aluminum alloy liquid serving as matrix molten metal A;
(2) adding any one of Al-Ti-C series intermediate alloys into the base metal melt A obtained in the step (1); stirring the mixture after adding the intermediate alloy until the intermediate alloy is completely melted to obtain a base metal melt added with the intermediate alloy, namely a metal melt B;
(3) carrying out ultrasonic treatment on the molten metal B to obtain molten metal C;
in the step (3), the specific process of ultrasonic treatment is as follows: lowering an ultrasonic probe of an ultrasonic device to a position above the molten metal B, contacting the molten metal B with the liquid level of the molten metal B, and preheating the molten metal B until the temperature of the ultrasonic probe reaches 750 ℃; continuously descending the probe to 10-15 mm below the liquid level of the molten metal, and carrying out ultrasonic treatment on the molten metal;
(4) removing dross on the surface in the molten metal C obtained in the step (3) by using a slag remover to obtain molten metal D;
(5) casting the molten metal D into a metal mold, and cooling to obtain a cast ingot;
in the step (5), after the molten metal D is cast into a metal mold, an ultrasonic probe of an ultrasonic device is lowered into the molten metal of the mold; gradually moving the ultrasonic probe upwards along with the solidification of the metal liquid D, continuously applying ultrasonic waves in the process of moving upwards until the metal is completely solidified, and lifting the ultrasonic probe out of the cast ingot before the metal is completely solidified;
(6) and crushing and fine grinding the cast ingot to obtain aluminum or aluminum alloy powder containing Al-Ti-C series intermediate alloy with a particle size of-200 to +500 meshes, wherein the aluminum or aluminum alloy powder is ultrasonically refined metal powder for 3D printing.
2. The method for preparing metal powder for 3D printing of ultrasonically refined grains according to claim 1, wherein in the step (1), the melting temperature of aluminum or aluminum alloy is 750 ℃, and after the aluminum or aluminum alloy is melted, the temperature is kept for 30min to obtain the base metal melt A.
3. The method for preparing metal powder for 3D printing of ultrasonically refined grains according to claim 1, wherein in the step (2), the equivalent amount of Ti in the added Al-Ti-C based master alloy accounts for 20 to 200ppm of the aluminum or aluminum alloy in the step (1).
4. The method for preparing metal powder for 3D printing of ultrasonically refined grains according to claim 1, wherein in the step (2), the master alloy is added into the base metal melt A and then stirred for 5-10 min.
5. The method for preparing the metal powder for 3D printing of the ultrasonically refined grains according to claim 1, wherein in the step (3), the probe is lowered to 10-15 mm below the liquid level of the molten liquid, then the temperature is kept for 5min, and ultrasonic treatment is carried out for 5-10 min.
6. The method according to claim 1, wherein in the step (4), a slag remover is added, and dross on the surface of the molten metal is removed after refining for 10min to obtain the molten metal D.
7. The method for preparing metal powder for 3D printing of ultrasonically refined grains according to claim 1, wherein in the step (6), after the ingot is crushed, coarse particles of more than 100 meshes are removed by a sieve; the aluminum or aluminum alloy powder containing Al-Ti-C intermediate alloy is obtained in a size of-200 to +500 mesh by fine grinding.
8. A metal powder for 3D printing of ultrasonically refined grains prepared by the preparation method of any one of claims 1 to 7.
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| CN111636008B (en) * | 2020-05-22 | 2022-01-07 | 广州致远新材料科技有限公司 | Ultrasonic treatment method suitable for aluminum-silicon alloy melt |
| CN112570706A (en) * | 2020-12-03 | 2021-03-30 | 山东大学 | Aluminum alloy powder, preparation method and application of aluminum alloy powder in laser additive manufacturing |
| CN113523184A (en) * | 2021-06-08 | 2021-10-22 | 上海航天精密机械研究所 | Magnesium alloy sand mold casting method |
| CN114734035A (en) * | 2022-03-14 | 2022-07-12 | 嘉兴数字三维智能制造研究院有限公司 | Metal powder for 3D printing and preparation method thereof |
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