CN111014683B - Heat treatment process for 3D printing of scandium-containing zirconium-aluminum alloy - Google Patents
Heat treatment process for 3D printing of scandium-containing zirconium-aluminum alloy Download PDFInfo
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- CN111014683B CN111014683B CN201911234602.2A CN201911234602A CN111014683B CN 111014683 B CN111014683 B CN 111014683B CN 201911234602 A CN201911234602 A CN 201911234602A CN 111014683 B CN111014683 B CN 111014683B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F3/24—After-treatment of workpieces or articles
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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
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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
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Abstract
The invention discloses a heat treatment method for 3D printing of scandium-containing zirconium-aluminum alloy, which comprises the following steps of heating 3D printing parts and then rapidly cooling; electrifying, heating and preserving heat; wherein: the heatingRapidly cooling after 3D printing of the parts, namely raising the temperature to 300-500 ℃ within 10-50 s, and then reducing the temperature of the parts to-50-100 ℃ within 1-240 s; the electrified heating and heat preservation is carried out when the pulse current density is 250A/cm2Heating to 200-300 ℃, heating at a speed of 30-70 ℃/min, and keeping the temperature for 20-60 min. In the heat treatment process for 3D printing of scandium-containing zirconium-aluminum alloy, Al can be ensured after the heat treatment process is carried out on the printed parts3The nano-size dispersion distribution of the (Sc, Zr) precipitated phase can improve the hardness of parts by 52HV to the maximum0.2。
Description
Technical Field
The invention belongs to the field of additive manufacturing aluminum alloy heat treatment, and particularly relates to a heat treatment process for 3D printing of scandium-containing zirconium-aluminum alloy, which can ensure precipitation of a nano-sized precipitated phase and stabilize the grain size of parts in the heat treatment process.
Background
At present, additive manufacturing technology is widely applied to manufacturing alloy parts, printed mechanical parts have high strength and fine grain structures, and mature printed mechanical parts comprise iron-based, aluminum alloy, copper alloy, nickel-based superalloy and the like. In the following studies, in order to obtain a printed part having a higher strength, the printed product is often subjected to a heat treatment, particularly an aluminum alloy, which can improve the strength by about 80MPa after a heat treatment such as aging and solution treatment, and a heat treatment method is generally adopted in which a solution treatment is performed at 100 ℃, 200 ℃ or higher to obtain a precipitated phase to strengthen the printed part. In particular, Al is precipitated from an aluminum alloy containing scandium and zirconium by keeping the temperature at 300 ℃ for 5 hours3The (Sc, Zr) phase forms precipitates and enhances the solid solution of rare elements, and improves both the tensile strength and the plasticity. However, the heat treatment mode can not avoid the grain group of the parts due to long heat preservation timeThe growth of the weaving and precipitation phase limits the upper limit of the improvement of the strength of the printing aluminum alloy to a certain extent, and in addition, the hardness of the parts after heat treatment is reduced due to the growth of crystal grains and precipitation phase.
Therefore, in order to solve the above problems, the method includes: (1) the traditional heat treatment process causes precipitated phases and crystal grains to grow; (2) precipitated phases in the aluminum alloy can not be uniformly precipitated in a grain boundary; (3) the traditional heat treatment mode has large energy consumption and long time, and the invention is provided. The invention provides an innovative heat treatment process for 3D printing of scandium-containing zirconium-aluminum alloy, and the mechanical property of the 3D printed aluminum alloy after heat treatment is improved to the maximum extent by microwave heating, rapid cooling and pulse current introduction.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above-mentioned technical drawbacks.
Therefore, as one aspect of the present invention, the present invention overcomes the disadvantages in the prior art, and provides a heat treatment method for 3D printing of scandium-containing zirconium-aluminum alloy.
In order to solve the technical problems, the invention provides the following technical scheme: a heat treatment method for 3D printing of scandium-containing zirconium-aluminum alloy comprises the steps of heating 3D printed parts and then rapidly cooling; and (5) electrifying, heating and preserving heat.
The preferable scheme of the heat treatment method for 3D printing of the scandium-containing zirconium-aluminum alloy is as follows: after the 3D printed parts are heated, the temperature is rapidly reduced, namely the temperature is increased to 300-500 ℃ within 10-50 s, and then the temperature of the parts is 1-EReducing the temperature to-50-200 ℃ within 240 s; the electrified heating and heat preservation is carried out when the pulse current density is 250A/cm2Heating to 200-300 ℃, heating at a speed of 30-70 ℃/min, and keeping the temperature for 20-60 min.
The preferable scheme of the heat treatment method for 3D printing of the scandium-containing zirconium-aluminum alloy is as follows: rapidly cooling after heating 3D printing parts by adopting microwave heating and liquid nitrogen rapid cooling mode, and aiming at achieving Al3Optimum temperature for nucleation of (Sc, Zr), increased supercooling degree, improved nucleation driving force, promoted nucleation rate, and ensured Al3A large amount of precipitated phases (Sc and Zr) are nucleated without growing, and simultaneously, the crystal grains of the parts do not grow because the time is extremely short; the heat preservation adopts a pulse current heating mode and mainly aims at controlling Al3And (Sc, Zr) phase nucleation and growth are carried out, the (Sc, Zr) phase nucleation and growth slowly grows to about 5-15 nm, and meanwhile, the growth of crystal grains of parts is inhibited.
The preferable scheme of the heat treatment method for 3D printing of the scandium-containing zirconium-aluminum alloy is as follows: the 3D printing part is obtained by printing an aluminum alloy containing scandium and zirconium, and the part is subjected to the heat treatment process to obtain Al3The precipitated phases (Sc, Zr) are dispersed in the matrix, the size is nano-scale, and the hardness can be improved by 52HV at the maximum0.2。
The preferable scheme of the heat treatment method for 3D printing of the scandium-containing zirconium-aluminum alloy is as follows: in the aluminum alloy, scandium and zirconium are main elements for strengthening the aluminum alloy.
The preferable scheme of the heat treatment method for 3D printing of the scandium-containing zirconium-aluminum alloy is as follows: the liquid nitrogen rapid cooling is to rapidly reduce the temperature of the 3D printing part by using the low temperature of the liquid nitrogen.
The preferable scheme of the heat treatment method for 3D printing of the scandium-containing zirconium-aluminum alloy is as follows: the liquid nitrogen rapid cooling is carried out in a special rapid cooling device, and the rapid cooling device is carried out in a cooling furnace with an air duct on the inner wall.
As another aspect of the invention, the invention provides a heat treatment for 3D printing of scandium-containing zirconium-aluminum alloysThe 3D printing part processed by the method is characterized in that: al (Al)3The (Sc, Zr) precipitated phase is dispersed in the matrix, the size is 5-15 nm, and the hardness can be improved by 52HV0.2。
The invention has the beneficial effects that:
in the heat treatment process for 3D printing of scandium-containing zirconium-aluminum alloy, Al can be ensured after the heat treatment process is carried out on the printed parts3The nano-size of the (Sc, Zr) precipitated phase is dispersed and distributed, the rigid nucleus of the nano precipitated phase is frozen, the grain growth is very small, and the maximum hardness of the part can be improved by 52HV0.2。
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a heat treatment curve and a process flow, wherein (i) is a microwave heating stage; ② a rapid cooling stage; thirdly, a heat preservation stage;
FIG. 2 is a rapid cooling device;
FIG. 3 is a schematic diagram of the power-on of the sintering furnace in the heat preservation stage.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1:
firstly, carrying out selective laser melting printing on a scandium-containing zirconium-aluminum-magnesium alloy, wherein the microhardness value of the scandium-containing zirconium-aluminum-magnesium alloy is 110 HV; in the components of the aluminum alloy, in percentage by mass, Sc: 0.7 percent; zr: 0.5 percent; mg: 5.5 percent; si: 0.2 percent; mn: 0.3 percent and the balance of Al.
The components are used for selective laser melting printing of aluminum alloy parts, and preferably, the process parameters are that the laser power is 400W; the scanning speed is 800 mm/s; the scanning distance is 0.05 mm; the scanning layer is 0.05mm thick, and the preheating temperature of the substrate is 150 ℃ during printing.
The 3D printing aluminum alloy is subjected to heat treatment through the following heat treatment process, and the scheme is as follows:
(1) placing the cooled 3D printed small parts into a microwave sintering furnace, controlling the temperature by adopting a thermocouple, and raising the temperature in the furnace to 400 ℃ within 30 s;
(2) after the temperature reaches 400 ℃, quickly placing the parts into a special quick cooling device, wherein the section of the quick cooling device is shown in figure 3, introducing liquid nitrogen into a pipeline, and reducing the temperature of the parts to 100 ℃ within 30 s;
(3) to control Al3The growth speed of the precipitated phase (Sc, Zr) is ensured, the nano-size strengthening effect is ensured, the parts are placed in a spark plasma sintering furnace for heat preservation, and the pulse current density is 250A/cm2The temperature is 200 ℃, the heating speed is 50 ℃/min, and the heat preservation time is 30 min;
(4) and after the heat treatment is finished, opening the furnace, taking out the aluminum alloy parts, and naturally cooling the aluminum alloy parts to room temperature in the air.
After heat treatment, the mechanical properties are shown in table 1; the size of the precipitated phase is basically maintained at about 5nm, and the precipitated phase is uniformly dispersed in the matrix, so that the strengthening effect is obvious; heating is considered at the speed of 50 ℃/min to enable the alloy to be heated more uniformly, the temperature can be quickly reduced to below 200 ℃ in the temperature reduction process, but if the temperature is reduced too low, energy-saving factors need to be considered, the temperature is increased to 200 ℃ subsequently, but the temperature is directly maintained at 200 ℃, the temperature reduction effect cannot be guaranteed due to too short intermediate time, so that the temperature is continuously reduced to 200 ℃, and a buffer interval is reserved when the temperature is reduced to 150 ℃.
Example 2:
firstly, carrying out selective laser melting printing on scandium-containing zirconium-aluminum alloy, wherein the microhardness value of the scandium-containing zirconium-aluminum alloy is 117 HV; the aluminum alloy comprises the following components in percentage by mass, wherein Sc: 0.8 percent; zr: 0.6 percent; mg: 5.8 percent; si: 0.2 percent; mn: 0.3 percent and the balance of Al. The printing parameters are preferably the same as those in embodiment 1.
The 3D printing aluminum alloy is subjected to heat treatment through the following heat treatment process, and the scheme is as follows:
(1) placing the cooled 3D printed small parts into a microwave sintering furnace, controlling the temperature by adopting a thermocouple, and raising the temperature in the furnace to 400 ℃ within 30 s;
(2) after the temperature reaches 400 ℃, quickly placing the parts into a special quick cooling device, wherein the section of the quick cooling device is shown in figure 3, introducing liquid nitrogen into a pipeline, and reducing the temperature of the parts to 80 ℃ within 10 s;
(3) to control Al3The growth speed of the precipitated phase (Sc, Zr) is ensured, the nano-size strengthening effect is ensured, the parts are placed in a spark plasma sintering furnace for heat preservation, and the pulse current density is 250A/cm2The temperature is 200 ℃, the heating speed is 50 ℃/min, and the heat preservation time is 30 min;
(4) and after the heat treatment is finished, opening the furnace, taking out the aluminum alloy parts, and naturally cooling the aluminum alloy parts to room temperature in the air.
After heat treatment, the mechanical properties are shown in table 1; in microscopic structure observation, the size of precipitated phase is basically maintained at about 5nm, and the precipitated phase is dispersed in the matrix, so that the strengthening effect is obvious.
Example 3:
firstly, carrying out selective laser melting printing on a scandium-containing zirconium-aluminum alloy, wherein the microhardness value of the scandium-containing zirconium-aluminum alloy is 121 HV; (ii) a The aluminum alloy comprises the following components in percentage by mass, wherein Sc: 0.9 percent; zr: 0.7 percent; mg: 4.6 percent; si: 0.9 percent; mn: 0.3 percent and the balance of Al. The printing parameters are preferably the same as those in embodiment 1.
The 3D printing aluminum alloy is subjected to heat treatment through the following heat treatment process, and the scheme is as follows:
(1) placing the cooled 3D printed small parts into a microwave sintering furnace, controlling the temperature by adopting a thermocouple, and raising the temperature in the furnace to 400 ℃ within 30 s;
(2) after the temperature reaches 400 ℃, quickly placing the parts into a special quick cooling device, wherein the section of the quick cooling device is shown in figure 3, introducing liquid nitrogen into a pipeline, and reducing the temperature of the parts to 50 ℃ within 15 s;
(3) to control Al3The growth speed of the precipitated phase (Sc, Zr) is ensured, the nano-size strengthening effect is ensured, the parts are placed in a spark plasma sintering furnace for heat preservation, and the pulse current density is 250A/cm2The temperature is 200 ℃, the heating speed is 50 ℃/min, and the heat preservation time is 30 min;
(4) after the heat treatment is finished, opening the furnace and taking out the aluminum alloy parts, and naturally cooling the aluminum alloy parts to room temperature in the air
After heat treatment, the mechanical properties are shown in table 1; in microscopic structure observation, the size of a precipitated phase is basically kept at about 6nm, and the precipitated phase is dispersed in a distribution matrix, so that the average hardness value is obviously increased.
Comparative example 1:
the raw material proportion in the example 1 is selected, the microwave heating time and the rapid cooling time are expanded to 6min, the other heat treatment conditions are the same as the example 1, the performances before and after the heat treatment are shown in the table 1, and Al3The size of the (Sc, Zr) precipitated phase exceeds 15nm, and in addition, as the microwave heating time is long, the dispersion distribution effect is good, the grain size is also increased to a certain extent, and the mechanical property improvement effect is obviously reduced.
Comparative example 2:
the raw material proportion in the example 1 is selected, the microwave heating temperature is raised to 520 ℃, the other heat treatment conditions are the same as those in the example 1, the performances before and after the heat treatment are shown in the table 1, the precipitated phase grows obviously due to overhigh temperature, and the grain size of the part is increased by 7 microns before and after the heat treatment, so that the mechanical property is not obviously increased.
Comparative example 3:
the raw material proportion in the example 1 is selected, the microwave heating temperature is reduced to 300 ℃, the other heat treatment conditions are the same as those in the example 1, the performances before and after the heat treatment are shown in the table 1, the maximum temperature reduction causes the reduction of the temperature reduction difference and the supercooling degree, thereby causing the reduction of the nucleation rate and the Al under the actual condition3The nucleation rate of (Sc, Zr) is reduced, the particle size is increased, and the crystal grains are also grown, so that the mechanical property is not obviously increased.
Comparative example 4:
the raw material proportion in the example 1 is selected, the electrifying heat preservation temperature is raised to 400 ℃, the other heat treatment conditions are the same as those in the example 1, the performances before and after the heat treatment are shown in the table 1, the heat preservation temperature is too high, the grain size is enlarged, the grains are also enlarged, the size before and after the heat treatment is increased by 12 microns, and the mechanical property increasing effect is reduced.
TABLE 1
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (3)
1. A heat treatment method for 3D printing of scandium-containing zirconium-aluminum alloy is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
rapidly cooling the 3D printing part after heating;
electrifying, heating and preserving heat;
the heating 3D prints rapid cooling behind the spare part, it is in 30sRaising the temperature to 400 ℃, and then reducing the temperature of the parts to 100 ℃ within 30 s; the electrified heating and heat preservation is carried out when the pulse current density is 250A/cm2Heating to 200 deg.C, heating at 50 deg.C/min, and maintaining for 30min to obtain Al3(Sc，Zr)；
The heating 3D printing part is an aluminum alloy, and the aluminum alloy comprises the following components in percentage by weight: 0.7 percent; zr: 0.5 percent; mg: 5.5 percent; si: 0.2 percent; mn: 0.3 percent of Al;
the Al is3The precipitated phases (Sc, Zr) are dispersed in the matrix, and the size is 5nm, the hardness increase value is delta HV0.2Is 52.
2. The thermal processing method for 3D printing of scandium-containing zirconium-aluminum alloy according to claim 1, wherein: rapidly cooling after heating 3D printing parts by adopting microwave heating and liquid nitrogen rapid cooling mode, and aiming at achieving Al3Optimum temperature for nucleation of (Sc, Zr), increased supercooling degree, improved nucleation driving force, promoted nucleation rate, and ensured Al3A large amount of precipitated phases (Sc and Zr) are nucleated without growing, and simultaneously, the crystal grains of the parts do not grow because the time is extremely short; the heat preservation adopts a pulse electric current heating mode.
3. The thermal processing method for 3D printing of scandium-containing zirconium-aluminum alloy according to claim 2, wherein: the liquid nitrogen rapid cooling is carried out in a special rapid cooling device which is a cooling furnace with an air duct on the inner wall.
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| JP3945455B2 (en) * | 2002-07-17 | 2007-07-18 | 株式会社豊田中央研究所 | Powder molded body, powder molding method, sintered metal body and method for producing the same |
| US7811395B2 (en) * | 2008-04-18 | 2010-10-12 | United Technologies Corporation | High strength L12 aluminum alloys |
| EP2546373A1 (en) * | 2011-07-13 | 2013-01-16 | Aleris Aluminum Koblenz GmbH | Method of manufacturing an Al-Mg alloy sheet product |
| US9551050B2 (en) * | 2012-02-29 | 2017-01-24 | The Boeing Company | Aluminum alloy with additions of scandium, zirconium and erbium |
| CN103422037B (en) * | 2012-05-23 | 2015-05-20 | 中国科学院金属研究所 | Technology for separation of recrystallization and precipitated phase precipitation of low scandium Al-Mg alloy |
| CN103866216A (en) * | 2012-12-12 | 2014-06-18 | 北京有色金属研究总院 | Heat treatment process for scandium-containing Al-Zn-Mg-Cu base squeeze casting aluminum alloy |
| CN103233147B (en) * | 2013-05-06 | 2015-10-28 | 北京工业大学 | A kind of Al-Er-Zr-Si aluminium alloy and thermal treatment process |
| CN104674142A (en) * | 2015-02-12 | 2015-06-03 | 东北大学 | Aging heat treatment method for high-zinc aluminum alloy containing scandium |
| CN104651764A (en) * | 2015-02-12 | 2015-05-27 | 东北大学 | Solid solution thermal treatment method for high-zinc scandium-containing aluminum alloy |
| CN105603237A (en) * | 2016-02-04 | 2016-05-25 | 东南大学 | Scandium-containing casting conductive aluminum alloy and preparation process thereof |
| CN106167884B (en) * | 2016-04-22 | 2018-06-22 | 昆山捷安特轻合金科技有限公司 | A kind of multistage heat treatment process of Al-Mg-Si-Cu-Zr-Sc aluminium alloys |
| CN107604222B (en) * | 2017-09-22 | 2019-04-05 | 东北大学 | It is a kind of can ageing strengthening Al-Mg alloy and preparation method thereof |
| CN108456812B (en) * | 2018-06-29 | 2020-02-18 | 中南大学 | Low-Sc high-strength high-toughness high-hardenability aluminum-zinc-magnesium alloy and preparation method thereof |
| CN109487126B (en) * | 2018-12-19 | 2020-06-02 | 中车工业研究院有限公司 | Aluminum alloy powder for 3D printing and preparation method and application thereof |
| CN109666812A (en) * | 2019-02-19 | 2019-04-23 | 中南大学 | A kind of high thermal stability ultra-high-strength aluminum alloy and preparation method thereof |
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