CN115041683A - Titanium alloy product with compact layer and production method thereof - Google Patents
Titanium alloy product with compact layer and production method thereof Download PDFInfo
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
-
- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
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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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/108—Mixtures obtained by warm mixing
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
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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
- B33Y10/00—Processes of additive manufacturing
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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
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
Abstract
The invention discloses a titanium alloy product with a compact layer and a production method thereof, and the production method comprises the following steps: s1, preparing a feed material by using titanium alloy powder and a binder, and preparing a titanium alloy substrate by using a metal injection molding process; and S2, forming a compact layer on the surface of the titanium alloy substrate by using the titanium alloy powder as a compact layer raw material through a metal 3D printing process, thereby preparing the titanium alloy product with the compact layer. The compactness of the compact layer printed and formed by the metal 3D printing process in the titanium alloy product can almost reach 100 percent, so that the compact layer can form a high-brightness polished surface after mirror polishing treatment, and the problem that the existing titanium alloy product is difficult to apply to the production of high-brightness polished products is effectively solved.
Description
Technical Field
The invention relates to the technical field of metal products, in particular to a titanium alloy product with a compact layer and a production method thereof.
Background
In recent years, intelligent devices are rapidly developed and updated, and particularly, electronic devices are increasingly popular among people when the 5G era is started. Titanium and titanium alloys are favored by the smart industry for their light weight, high strength, corrosion resistance, allergy resistance, etc. Titanium and titanium alloys are chemically reactive and easily combine with interstitial elements (C, O, N) to produce compounds that induce cold hardness. Meanwhile, the titanium has large specific heat capacity during cutting, is easy to accumulate heat and is difficult to conduct heat, and the accumulated heat during cutting enables the cutting edge to be softened. Therefore, titanium is more difficult to cut than stainless steel, next to liquid metal, and thus CNC machining is used, which makes the machining process difficult due to the properties of the titanium alloy itself. Meanwhile, due to the existence of the R angle on the surface of the product and the threaded column, the product is difficult to form at one time, and meanwhile, the material waste is caused, and the time and the raw material cost are increased.
The metal injection molding process can well solve the problem of difficult titanium processing. Metal Injection Molding (MIM) is a new near-net-shape forming technique that has been rapidly developed internationally in recent years, and has advantages in that it is possible to form small metal parts of complicated shapes, and the density of parts of the product is uniform, and the mechanical properties are excellent. Although the density of the product prepared by Metal Injection Molding (MIM) is quite high, the product still has 1-5 vol% of pores, and the application of the product in the aspect of high-brightness polishing products is restricted.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a production method of a titanium alloy product with a compact layer, which mainly solves the technical problem that the metal product prepared by the existing metal injection molding process is difficult to form a compact surface. The surface porosity of the titanium alloy product obtained by the method is lower than 1-5 vol%, and a high-brightness polished product can be formed after polishing treatment.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method of producing a titanium alloy product having a dense layer, comprising the steps of:
s1, preparing a feed material by using titanium alloy powder and a binder, and preparing a titanium alloy substrate by using a metal injection molding process;
and S2, forming a compact layer on the surface of the titanium alloy substrate by using the titanium alloy powder as a compact layer raw material through a metal 3D printing process, thereby preparing the titanium alloy product with the compact layer.
In the invention, the density of the titanium alloy substrate prepared by the metal injection molding process in the step S1 is quite high, but the density of the titanium alloy substrate still has 1-5 vol% of pores, so that in the step S2, a titanium alloy dense layer with high compactness, good dimensional accuracy and surface roughness is grafted on the titanium alloy substrate prepared by the step S1 through a metal 3D printing process, and the compactness of the titanium alloy dense layer almost reaches 100% compared with the titanium alloy substrate prepared by the existing metal injection molding process. And the titanium alloy dense layer grafted on the titanium alloy substrate can be applied to the aspect of manufacturing high-brightness polishing products.
Further, after S2, S3 is included, and the mirror polishing process is performed on the dense layer formed on the titanium alloy substrate to obtain a titanium alloy product having a highly polished surface.
Further, in S1, the method for preparing the titanium alloy substrate specifically includes the following steps:
s11, feed preparation: preheating titanium alloy powder to a preset temperature, then mixing a binder and the titanium alloy powder reaching the preset temperature, and then sending the mixture into a mixing roll for mixing, so that the titanium alloy powder and the binder are pre-formed into a mud-shaped material, then sending the mud-shaped material into an extruder, plasticizing, extruding and granulating to prepare a feed to be injection molded;
s12, injection molding: injecting and forming the feed at the temperature of 120-150 ℃ to obtain a green blank;
s13, degreasing and sintering: putting the green blank obtained by injection molding into an oxalic acid degreasing furnace for degreasing treatment, and then carrying out vacuum sintering treatment in a vacuum metal furnace to obtain a titanium alloy substrate;
preferably, in S11, preheating the titanium alloy powder and mixing the binder and the preheated titanium alloy powder are performed under vacuum condition;
preferably, in S11, preheating the titanium alloy powder and mixing the binder and the preheated titanium alloy powder are both performed under a vacuum condition with a vacuum degree of 10-500 Pa;
preferably, the working conditions of the mixer are: the rotation speed of the mixing roll is 15-35 r/min, and the stirring time is 40-70 min.
Further, in S11, preheating the titanium alloy powder to 120 +/-10 ℃ under the vacuum condition;
preferably, the titanium alloy powder is TC4 titanium alloy powder;
preferably, the particle size of the titanium alloy powder is 18-24 um.
Further, in S13, the acid inlet amount in the degreasing treatment process is 0.010-0.050 mL/min, the degreasing temperature is 120-125 ℃, and the degreasing time is 8-24 hours;
preferably, in S13, the sintering temperature in the vacuum sintering treatment process is 1230-1250 ℃, the heat preservation time is 90-120 min, and the pressure is kept at 0.5-4 Mpa;
preferably, in S13, in the vacuum sintering process, a zirconia setter plate is used to place the titanium alloy substrate semi-finished product to be sintered;
preferably, in order to reduce the oxygen content better, a double-layer molybdenum box made of molybdenum metal is used as a sintering protection, titanium sponge is filled in an interlayer of the double-layer molybdenum box, an yttrium oxide coating is brushed on the inside of the molybdenum box, and protection is performed in a protection mode of the double-molybdenum box, the titanium sponge and the yttrium oxide coating.
Further, in the step S1, the binder comprises the following components in parts by weight: 1-2.5 parts of stearic acid, 3-6 parts of a photo-thermal stabilizer, 3-7 parts of a high-molecular polymer wax, 5-10 parts of high-density polyethylene, 1.5-3 parts of polyethylene-acetate, 2-4 parts of carnauba wax and 70-85 parts of polyformaldehyde.
In the invention, the titanium alloy substrate prepared by combining the specific feeding with the specific metal injection molding process can well overcome the influence of the gap elements on the material performance in the sintering process of the titanium alloy substrate, and effectively solve the problems of difficult processing, cold hardness, brittleness and the like of the titanium alloy product.
Further, in step S2, the method for preparing a dense layer specifically includes the steps of:
s21, uniformly paving a layer of titanium alloy powder layer with a preset thickness on the titanium alloy substrate;
s22, selectively scanning the titanium alloy powder layer by using a metal 3D printer to enable the titanium alloy powder to be heated, melted and solidified to form a titanium alloy compact thin layer integrated with the titanium alloy substrate;
s23, laying a layer of titanium alloy powder layer with a preset thickness on the titanium alloy compact thin layer again, and selectively scanning the titanium alloy powder layer by using the metal 3D printer again to form a new titanium alloy compact thin layer on the previous titanium alloy compact thin layer;
and S24, repeating the step S23, and forming a compact layer for mirror polishing treatment by a plurality of layers of the titanium alloy compact thin layers which are overlapped together.
Further, in S21 or S23 or S24, the single layer thickness of the laid titanium alloy powder layer is 30 um;
preferably, the overall thickness of the dense layer is 0.94 ± 0.03 mm.
Further, the output power of the metal 3D printer was 135W, the scanning speed was 800mm/s, and the exposure time was 0.4 s.
In the invention, the selected 3D printer is a metal 3D printer of the Technology Co, Lezifeng materials, Suzhou, the laser scanning trace on the surface of the finished product printed by the printer is shallow, and the finished product can obtain smaller surface roughness more easily through post-processing. When the laser scanning device works, laser with the spot diameter of 52um is used as an energy source, the laser is focused on a forming platform after being modulated by a group of precise optical lenses and the direction of a high-precision scanning galvanometer is controlled, the exposure time is 0.4s, and single-layer titanium alloy powder with the thickness of 30um uniformly paved on a titanium alloy substrate is selectively scanned under the conditions that the scanning speed is 800mm/s and the output power is 135W. The titanium alloy powder is heated and melted and then quickly solidified, and the titanium alloy powder in the scanned area is melted and sintered into a whole; and then uniformly spreading the titanium alloy powder on the scanned titanium alloy powder layer again, scanning, melting and solidifying again, and combining the titanium alloy powder layer with the previous layer. And continuously repeating the process until the thickness of the compact layer formed by the 3D printing reaches a preset thickness value. A titanium alloy dense layer having a polished surface capable of being mirror-polished to form a high brightness is produced and integrally grafted on the titanium alloy substrate.
Based on the same inventive concept, the invention also provides a titanium alloy product with a compact layer, which is prepared by any one of the production methods.
The technical scheme has the following advantages or beneficial effects:
in the titanium alloy product with the compact layer and the production method thereof, the surface texture of the compact layer after mirror polishing is fine and uniform, and the density of the compact layer printed and formed by a metal 3D printing process can almost reach 100%, so that the compact layer can form a high-brightness polished surface after mirror polishing treatment, and the problem that the existing titanium alloy product is difficult to apply to the production of the high-brightness polished product is effectively solved.
Drawings
FIG. 1 is a graph showing the polishing effect of the titanium alloy product having a dense layer according to example 1 of the present invention after the dense layer is mirror-polished.
FIG. 2 is a graph showing the polishing effect of the mirror-polished surface of the titanium alloy substrate according to the comparative example of the present invention, which was manufactured by the metal injection molding process.
Detailed Description
In the present invention, preferably, in S1, the binder is composed of the following components in parts by weight: 1-2.5 parts of stearic acid, 3-6 parts of a photo-thermal stabilizer, 3-7 parts of a high-molecular polymer wax, 5-10 parts of high-density polyethylene, 1.5-3 parts of polyethylene-acetate, 2-4 parts of carnauba wax and 70-85 parts of polyformaldehyde.
In the present invention, preferably, in S11, the preheating of the titanium alloy powder and the mixing of the binder and the preheated titanium alloy powder are both performed under a vacuum condition of a vacuum degree of 10 to 500Pa, and when the titanium alloy powder is preheated to 120 ± 10 ℃, the preformed binder is further added to the titanium alloy powder which has reached the preheating temperature under the vacuum condition; the working conditions of the mixing mill are as follows: the rotation speed of the mixing roll is 15-35 r/min, and the stirring time is 40-70 min.
In the invention, in S13, preferably, the acid inlet amount in the degreasing treatment process is 0.010-0.050 mL/min, the degreasing temperature is 120-125 ℃, and the degreasing time is 8-24 h; and in S13, the sintering temperature in the vacuum sintering treatment process is 1230-1250 ℃, the heat preservation time is 90-120 min, and the pressure is kept at 0.5-4 Mpa.
According to the invention, the titanium alloy substrate prepared by the special binder formula and the specific metal injection molding process is protected by sintering by using the double-layer molybdenum box made of metal molybdenum, titanium sponge is filled in the interlayer of the double-layer molybdenum box, and the inside of the molybdenum box is brushed with an yttrium oxide coating. The protection is carried out in a protection mode of a double molybdenum box, titanium sponge and yttrium oxide coating, so that the influence of poor mechanical properties of materials caused by the fact that interstitial elements such as oxygen and nitrogen permeate into the materials in the sintering process of titanium alloy products can be overcome, and the defect that the titanium alloy products are cold, hard and brittle is effectively overcome.
In the present invention, preferably, in step S2, the single-layer thickness of the laid titanium alloy powder layer is 30 um; the output power of the metal 3D printer is 135W, the scanning speed is 800mm/s, and the exposure time is 0.4 s; in step S2, the overall thickness of the dense layer formed by printing with the metal 3D printer is set to 0.94 ± 0.03mm, preferably 0.942 mm.
The invention is further described with reference to the following figures and examples.
Example 1
The embodiment provides a production method of a titanium alloy product with a compact layer, which comprises the following steps:
s1, preparing a feed material by using titanium alloy powder and a binder, and preparing a titanium alloy substrate by using a metal injection molding process;
and S2, forming a compact layer on the surface of the titanium alloy substrate by using the titanium alloy powder as a compact layer raw material through a metal 3D printing process, thereby preparing the titanium alloy product with the compact layer.
Specifically, in S1, the method for preparing the titanium alloy substrate specifically includes the following steps:
s11, feed preparation: in this embodiment, the titanium alloy powder is TC4 titanium alloy powder with a particle size of 20um, and the binder is composed of the following components in parts by weight: 2 parts of stearic acid, 3 parts of light-heat stabilizer, 3 parts of high-molecular polymer wax, 5 parts of high-density polyethylene, 3 parts of polyethylene-acetate, 4 parts of carnauba wax and 85 parts of polyformaldehyde. Preheating titanium alloy powder to a preset temperature of 120 +/-10 ℃ under a vacuum condition with the vacuum degree of 200Pa, mixing a binder and the titanium alloy powder reaching the preset temperature, feeding the mixture into a mixing roll for mixing, pre-forming the titanium alloy powder and the binder into a mud-shaped material, feeding the mud-shaped material into an extruder, plasticizing, extruding, and granulating to prepare a feed to be injection molded;
s12, injection molding: injecting and forming the feed at the temperature of 130 ℃ to obtain a green blank;
s13, degreasing and sintering: and (3) putting the green blank obtained by injection molding into an oxalic acid degreasing furnace for degreasing, and then carrying out vacuum sintering treatment in a vacuum metal furnace to obtain the titanium alloy substrate.
In step S2, the method for preparing a dense layer specifically includes the steps of:
s21, uniformly paving a layer of titanium alloy powder layer with a preset thickness on the titanium alloy substrate;
s22, selectively scanning the titanium alloy powder layer by using a metal 3D printer, heating and melting the titanium alloy powder, and then quickly solidifying the titanium alloy powder to form a titanium alloy compact thin layer integrated with the titanium alloy substrate;
s23, laying a layer of titanium alloy powder layer with a preset thickness on the titanium alloy compact thin layer again, and selectively scanning the titanium alloy powder layer by using the metal 3D printer again to form a new titanium alloy compact thin layer on the previous titanium alloy compact thin layer;
and S24, repeating the step S23, and forming a dense layer for mirror polishing treatment by a plurality of stacked dense thin titanium alloy layers.
And after S2, S3 is further included, and the titanium alloy product with the highlight polished surface is obtained by carrying out mirror polishing treatment on the dense layer formed on the titanium alloy substrate. As shown in the attached drawing 1, the polishing effect graph is formed after the compact layer grafted on the titanium alloy substrate is subjected to mirror polishing treatment, and as can be seen from the attached drawing 1, the surface texture of the compact layer subjected to mirror polishing is fine and uniform, and the density of the compact layer printed and formed by a metal 3D printing process can almost reach 100%, so that the compact layer can form a high-brightness polishing surface after being subjected to mirror polishing treatment, and the problem that the existing titanium alloy product is difficult to apply to the production of high-brightness polishing products is effectively solved.
Example 2
The embodiment provides a production method of a titanium alloy product with a compact layer, which comprises the following steps:
s1, preparing a feed material by using titanium alloy powder and a binder, and preparing a titanium alloy substrate by using a metal injection molding process;
and S2, taking the titanium alloy powder as a raw material of the compact layer, and forming a compact layer on the surface of the titanium alloy substrate through a metal 3D printing process to obtain the titanium alloy product with the compact layer.
Specifically, in S1, the method for preparing the titanium alloy substrate specifically includes the following steps:
s11, feed preparation: in this embodiment, the titanium alloy powder is TC4 titanium alloy powder with a particle size of 18um, and the binder is composed of the following components in parts by weight: 1 part of stearic acid, 4 parts of light-heat stabilizer, 4 parts of high-molecular polymer wax, 10 parts of high-density polyethylene, 1.5 parts of polyethylene-acetate, 3 parts of carnauba wax and 80 parts of polyformaldehyde. Preheating titanium alloy powder to a preset temperature of 120 +/-10 ℃ under a vacuum condition with the vacuum degree of 200Pa, mixing a binder and the titanium alloy powder reaching the preset temperature, feeding the mixture into a mixing roll for mixing, pre-forming the titanium alloy powder and the binder into a mud-shaped material, feeding the mud-shaped material into an extruder, plasticizing, extruding, and granulating to prepare a feed to be injection molded;
s12, injection molding: injecting the feed at 120 deg.c to form green blank;
s13, degreasing and sintering: and (3) putting the green blank obtained by injection molding into an oxalic acid degreasing furnace for degreasing, and then carrying out vacuum sintering treatment in a vacuum metal furnace to obtain the titanium alloy substrate.
In step S2, the method for preparing a dense layer specifically includes the steps of:
s21, uniformly paving a layer of titanium alloy powder layer with a preset thickness on the titanium alloy substrate;
s22, selectively scanning the titanium alloy powder layer by using a metal 3D printer, heating and melting the titanium alloy powder, and then quickly solidifying the titanium alloy powder to form a titanium alloy compact thin layer integrated with the titanium alloy substrate;
s23, laying a layer of titanium alloy powder layer with a preset thickness on the titanium alloy compact thin layer again, and selectively scanning the titanium alloy powder layer by using the metal 3D printer again to form a new titanium alloy compact thin layer on the previous titanium alloy compact thin layer;
and S24, repeating the step S23, and forming a dense layer for mirror polishing treatment by a plurality of stacked dense thin titanium alloy layers.
And after S2, S3 is further included, and the titanium alloy product with the highlight polished surface is obtained by carrying out mirror polishing treatment on the dense layer formed on the titanium alloy substrate.
Example 3
The embodiment provides a production method of a titanium alloy product with a compact layer, which comprises the following steps:
s1, preparing a feed material by using titanium alloy powder and a binder, and preparing a titanium alloy substrate by using a metal injection molding process;
and S2, forming a compact layer on the surface of the titanium alloy substrate by using the titanium alloy powder as a compact layer raw material through a metal 3D printing process, thereby preparing the titanium alloy product with the compact layer.
Specifically, in S1, the method for preparing the titanium alloy substrate specifically includes the following steps:
s11, feed preparation: in this embodiment, the titanium alloy powder is TC4 titanium alloy powder with a particle size of 22um, and the binder is composed of the following components in parts by weight: 1.5 parts of stearic acid, 5 parts of light and heat stabilizer, 5 parts of high-molecular polymer wax, 7 parts of high-density polyethylene, 2 parts of polyethylene-acetate, 2 parts of carnauba wax and 70 parts of polyformaldehyde. Preheating titanium alloy powder to a preset temperature of 120 +/-10 ℃ under a vacuum condition with the vacuum degree of 200Pa, mixing a binder and the titanium alloy powder reaching the preset temperature, feeding the mixture into a mixing roll for mixing, pre-forming the titanium alloy powder and the binder into a mud-shaped material, feeding the mud-shaped material into an extruder, plasticizing, extruding, and granulating to obtain feed to be injection-molded;
s12, injection molding: injecting the feed at 140 deg.C to obtain a blank;
s13, degreasing and sintering: and (3) putting the green blank obtained by injection molding into an oxalic acid degreasing furnace for degreasing, and then performing vacuum sintering treatment in a vacuum metal furnace to obtain the titanium alloy substrate.
In step S2, the method for preparing a dense layer specifically includes the steps of:
s21, uniformly paving a layer of titanium alloy powder layer with a preset thickness on the titanium alloy substrate;
s22, selectively scanning the titanium alloy powder layer by using a metal 3D printer, heating and melting the titanium alloy powder, and then quickly solidifying the titanium alloy powder to form a titanium alloy compact thin layer integrated with the titanium alloy substrate;
s23, laying a layer of titanium alloy powder layer with a preset thickness on the titanium alloy compact thin layer again, and selectively scanning the titanium alloy powder layer by using the metal 3D printer again to form a new titanium alloy compact thin layer on the previous titanium alloy compact thin layer;
and S24, repeating the step S23, and forming a dense layer for mirror polishing treatment by a plurality of stacked dense thin titanium alloy layers.
And after S2, S3 is further included, and the titanium alloy product with the highlight polished surface is obtained by carrying out mirror polishing treatment on the dense layer formed on the titanium alloy substrate.
Example 4
The embodiment provides a production method of a titanium alloy product with a compact layer, which comprises the following steps:
s1, preparing a feed material by using titanium alloy powder and a binder, and preparing a titanium alloy substrate by using a metal injection molding process;
and S2, taking the titanium alloy powder as a raw material of the compact layer, and forming a compact layer on the surface of the titanium alloy substrate through a metal 3D printing process to obtain the titanium alloy product with the compact layer.
Specifically, in S1, the method for preparing the titanium alloy substrate specifically includes the following steps:
s11, feed preparation: in this embodiment, the titanium alloy powder is TC4 titanium alloy powder with a particle size of 24um, and the binder is composed of the following components in parts by weight: 2.5 parts of stearic acid, 6 parts of light and heat stabilizer, 7 parts of high-molecular polymer wax, 6 parts of high-density polyethylene, 2.5 parts of polyethylene-acetate, 4 parts of carnauba wax and 75 parts of polyformaldehyde. Preheating titanium alloy powder to a preset temperature of 120 +/-10 ℃ under a vacuum condition with the vacuum degree of 200Pa, mixing a binder and the titanium alloy powder reaching the preset temperature, feeding the mixture into a mixing roll for mixing, pre-forming the titanium alloy powder and the binder into a mud-shaped material, feeding the mud-shaped material into an extruder, plasticizing, extruding, and granulating to prepare a feed to be injection molded;
s12, injection molding: injecting and forming the feed at the temperature of 150 ℃ to obtain a green blank;
s13, degreasing and sintering: and (3) putting the green blank obtained by injection molding into an oxalic acid degreasing furnace for degreasing, and then carrying out vacuum sintering treatment in a vacuum metal furnace to obtain the titanium alloy substrate.
In step S2, the method for preparing a dense layer specifically includes the steps of:
s21, uniformly paving a layer of titanium alloy powder layer with a preset thickness on the titanium alloy substrate;
s22, selectively scanning the titanium alloy powder layer by using a metal 3D printer, heating and melting the titanium alloy powder, and then quickly solidifying the titanium alloy powder to form a titanium alloy compact thin layer integrated with the titanium alloy substrate;
s23, laying a layer of titanium alloy powder layer with a preset thickness on the titanium alloy compact thin layer again, and selectively scanning the titanium alloy powder layer by using the metal 3D printer again to form a new titanium alloy compact thin layer on the previous titanium alloy compact thin layer;
and S24, repeating the step S23, and forming a dense layer for mirror polishing treatment by a plurality of stacked dense thin titanium alloy layers.
And after S2, S3 is further included, and the titanium alloy product with the highlight polished surface is obtained by carrying out mirror polishing treatment on the dense layer formed on the titanium alloy substrate.
Comparative example 1
The difference between the comparative example 1 and the example 1 is that after the step of S1, the mirror polishing treatment of the step S3 is directly performed on the titanium alloy substrate prepared by the metal injection molding process in S1 without the step S2, and although the density of the titanium alloy substrate prepared by the metal injection molding process is quite high, the titanium alloy substrate still has 1 to 5 vol% of pores, as shown in fig. 2, when the mirror polishing treatment is directly performed on the surface of the titanium alloy substrate, the polished surface is relatively rough, uneven and fine, and the uniformity is obviously inferior to the polished surface formed on the dense layer in the example, and the polishing effect requirement of the high-brightness polished product cannot be well satisfied.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and these modifications or substitutions do not make the corresponding technical solutions depart from the spirit and scope of the technical solutions of the embodiments of the present invention, so that all other embodiments obtained by those skilled in the art without making creative efforts belong to the protection scope of the present invention.
Claims (10)
1. A method of producing a titanium alloy product having a dense layer, characterized by: the method comprises the following steps:
s1, preparing a feed material by using titanium alloy powder and a binder, and preparing a titanium alloy substrate by using a metal injection molding process;
and S2, forming a compact layer on the surface of the titanium alloy substrate by using the titanium alloy powder as a compact layer raw material through a metal 3D printing process, thereby preparing the titanium alloy product with the compact layer.
2. A method for producing a titanium alloy product with a dense layer according to claim 1, characterized in that: and after S2, S3 is further included, and the compact layer formed on the titanium alloy substrate is subjected to mirror polishing treatment to obtain a titanium alloy product with a polished surface.
3. A method for producing a titanium alloy product with a dense layer according to claim 1, characterized in that: in S1, the method for preparing the titanium alloy substrate specifically includes the following steps:
s11, feed preparation: preheating titanium alloy powder to a preset temperature, then mixing a binder and the titanium alloy powder reaching the preset temperature, and then sending the mixture into a mixing roll for mixing, so that the titanium alloy powder and the binder are pre-formed into a mud-shaped material, then sending the mud-shaped material into an extruder, plasticizing, extruding and granulating to prepare a feed to be injection molded;
s12, injection molding: injecting and forming the feed at the temperature of 120-150 ℃ to obtain a green blank;
s13, degreasing and sintering: putting the green blank obtained by injection molding into a degreasing furnace for degreasing, and then carrying out vacuum sintering treatment in a vacuum metal furnace to obtain a titanium alloy substrate;
preferably, in S11, the preheating of the titanium alloy powder and the mixing of the binder and the preheated titanium alloy powder are both performed under vacuum conditions;
preferably, in S11, preheating the titanium alloy powder and mixing the binder and the preheated titanium alloy powder are both performed under a vacuum condition with a vacuum degree of 10-500 Pa;
preferably, the working conditions of the mixer are: the rotation speed of the mixing roll is 15-35 r/min, and the stirring time is 40-70 min.
4. A method for producing a titanium alloy product with a dense layer according to claim 3, characterized in that: in S11, preheating titanium alloy powder to 120 +/-10 ℃ under the vacuum condition;
preferably, the titanium alloy powder is TC4 titanium alloy powder;
preferably, the particle size of the titanium alloy powder is 18-24 um.
5. A method for producing a titanium alloy product with a dense layer according to claim 3, characterized in that: in S13, the acid inlet amount in the degreasing treatment process is 0.010-0.050 mL/min, the degreasing temperature is 120-125 ℃, and the degreasing time is 8-24 hours;
preferably, in S13, the sintering temperature in the vacuum sintering process is 1230-1250 ℃, the heat preservation time is 90-120 min, and the pressure is kept at 0.5-4 Mpa.
6. A method for producing a titanium alloy product with a dense layer according to claim 1, characterized in that: in S1, the binder comprises the following components in parts by weight: 1-2.5 parts of stearic acid, 3-6 parts of a photo-thermal stabilizer, 3-7 parts of a high-molecular polymer wax, 5-10 parts of high-density polyethylene, 1.5-3 parts of polyethylene-acetate, 2-4 parts of carnauba wax and 70-85 parts of polyformaldehyde.
7. A method for producing a titanium alloy product with a dense layer according to any one of claims 1 to 6, characterized in that: in step S2, the method for preparing a dense layer specifically includes the steps of:
s21, uniformly paving a layer of titanium alloy powder layer with a preset thickness on the titanium alloy substrate;
s22, selectively scanning the titanium alloy powder layer by using a metal 3D printer to enable the titanium alloy powder to be heated, melted and solidified to form a titanium alloy compact thin layer integrated with the titanium alloy substrate;
s23, laying a layer of titanium alloy powder layer with a preset thickness on the titanium alloy compact thin layer again, and selectively scanning the titanium alloy powder layer by using the metal 3D printer again to form a new titanium alloy compact thin layer on the previous titanium alloy compact thin layer;
and S24, repeating the step S23, and forming a dense layer for mirror polishing treatment by a plurality of stacked dense thin titanium alloy layers.
8. A method for producing a titanium alloy product with a dense layer according to claim 7, characterized in that: in S21 or S23 or S24, the single-layer thickness of the laid titanium alloy powder layer is 25-35 um;
preferably, the overall thickness of the dense layer is 0.94 ± 0.03 mm.
9. A method for producing a titanium alloy product with a dense layer according to claim 7, characterized in that: the output power of the metal 3D printer is 100-200W, the scanning speed is 500-1000mm/s, and the exposure time is 0.1-3s, preferably, the output power of the metal 3D printer is 135W, the scanning speed is 800mm/s, and the exposure time is 0.4 s.
10. A titanium alloy product having a densified layer, characterized by: produced by the production method according to any one of claims 1 to 9.
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