CN115415528A - Preparation method of aluminum-silicon-titanium alloy powder - Google Patents

Preparation method of aluminum-silicon-titanium alloy powder Download PDF

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CN115415528A
CN115415528A CN202210979007.7A CN202210979007A CN115415528A CN 115415528 A CN115415528 A CN 115415528A CN 202210979007 A CN202210979007 A CN 202210979007A CN 115415528 A CN115415528 A CN 115415528A
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aluminum
powder
silicon
alloy powder
titanium alloy
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CN115415528B (en
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苟海鹏
祁永峰
王云
裴忠冶
陈学刚
姚亮
陈宋璇
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China ENFI Engineering Corp
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention provides a preparation method of aluminum silicon titanium alloy powder, which comprises the following steps: adding aluminum-silicon alloy powder and sodium fluotitanate powder into a ball milling device according to a preset mixing proportion, uniformly mixing, and introducing inert protective gas for ball milling treatment to obtain mixed powder; pressing the mixed powder into a mixed powder block by adopting a mould; adding the mixed powder block into a vacuum smelting furnace, heating the mixed powder block to a preset temperature under a vacuum condition, and preserving heat for a preset time to obtain a reacted material; and cooling the reacted materials to room temperature to obtain the aluminum-silicon-titanium alloy powder. The method can solve the problem that the quality of the aluminum-silicon-titanium alloy is influenced by higher content of impurity element oxygen in the aluminum-silicon-titanium alloy prepared by taking titanium oxide, titanium-containing blast furnace slag or high titanium slag as raw materials in the prior art.

Description

Preparation method of aluminum-silicon-titanium alloy powder
Technical Field
The invention relates to the technical field of alloy preparation, in particular to a preparation method of aluminum-silicon-titanium alloy powder.
Background
The Al-Si-Ti alloy has the characteristics of light weight, high hardness and strong toughness, and is widely applied to the manufacturing of high-speed trains, high-grade cars and motorcycles and the industrial fields of aerospace, traffic, building and the like.
Currently, the method for preparing the aluminum-silicon-titanium alloy generally takes titanium-containing slag and silicon-containing aluminum slag as raw materials to synthesize and prepare the aluminum-silicon-titanium alloy, for example, patent CN113122728A uses the titanium slag and the silicon-aluminum alloy as raw materials to prepare the silicon-titanium alloy through aluminothermic reduction reaction at 1600-1700 ℃; patent CN112719275B uses silicon-titanium alloy as raw material, and obtains silicon-titanium alloy particles by grinding the alloy with magnetic grinding particles; patent 109457114B evenly mixes titanium-containing slag, silicon material and additive to obtain smelting material and carries out smelting; completely melting the smelting material at a temperature of more than 1673K, and then smelting at a constant temperature for more than 15min to separate slag and gold to obtain a Ti-Si alloy; the Ti-Si alloy is separated and purified to simultaneously obtain high-purity silicon, high-purity titanium and Ti 5 Si 3 、Ti 5 Si 4 、TiSi、TiSi 2 High-purity Ti-Si alloys such as eutectic Ti-Si alloys; and patent CN109402420B, mixing the titanium-containing blast furnace slag, aluminum materials and additives uniformly to obtain a total material, preserving heat for 0.5-10 h at a smelting temperature of 1573K-1973K, and then separating slag and gold to obtain Ti-Si-Al alloy; separating and primarily purifying the obtained Ti-Si-Al alloy by adopting an electromagnetic or resistance heating directional solidification method at a directional solidification speed of 10-4000 mu m/min, and mechanically cutting and separating to obtain Ti-Si alloy and Al-Si alloy; grinding the obtained Ti-Si alloy, and then carrying out acid washing, vacuum melting or vacuum directional solidificationRemoving impurities and purifying again to obtain high-purity Ti-Si alloy and the like.
However, the content of impurity element oxygen in the aluminum silicon titanium alloy prepared by taking titanium oxide, titanium-containing blast furnace slag or high titanium slag as raw materials is higher, thereby influencing the quality of the aluminum silicon titanium alloy.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for preparing an aluminum-silicon-titanium alloy powder, so as to solve the problem that the quality of the aluminum-silicon-titanium alloy is affected by the high content of impurity element oxygen in the aluminum-silicon-titanium alloy prepared by using titanium oxide, titanium-containing blast furnace slag or high titanium slag as raw materials.
The invention provides a preparation method of aluminum silicon titanium alloy powder, which comprises the following steps:
adding aluminum-silicon alloy powder and sodium fluotitanate powder into a ball-milling device according to a preset mixing proportion, uniformly mixing, and introducing inert protective gas for ball-milling treatment to obtain mixed powder;
pressing the mixed powder into a mixed powder block by adopting a mould;
adding the mixed powder block into a vacuum smelting furnace, heating the mixed powder block to a preset temperature under a vacuum condition, and keeping the temperature for a preset time to obtain a reacted material;
and cooling the reacted materials to room temperature to obtain the aluminum-silicon-titanium alloy powder.
Further, it is preferable that the aluminum-silicon alloy powder and the sodium fluorotitanate powder are each a powder having a particle size of less than 100 μm; and/or the purities of the aluminum-silicon alloy powder and the sodium fluotitanate powder are both more than 99%.
In addition, it is preferable that the preset mixing ratio is: a ratio of the number of moles of aluminum-silicon alloy in the aluminum-silicon alloy powder to the number of moles of sodium fluorotitanate in the sodium fluorotitanate powder is greater than 7.
In addition, the preferred scheme is that the ball milling device is a ball mill; the rotating speed of the ball mill is 300-800 rpm.
In addition, according to a preferable scheme, in the process of adding the aluminum-silicon alloy powder and the sodium fluotitanate powder into a ball milling device according to a preset mixing ratio, uniformly mixing, and then introducing inert protective gas for ball milling treatment to obtain mixed powder, the ball milling time of the aluminum-silicon alloy powder and the sodium fluotitanate powder in the ball milling device is 5-10 h.
In addition, it is preferable that the inert shielding gas includes one of nitrogen, argon, helium, neon, or at least two mixed in any ratio.
In addition, it is preferable that, in the process of pressing the mixed powder into the mixed powder block by using the mold, the pressure of the mold on the mixed powder is greater than 40Mpa.
In addition, the pressure in the vacuum smelting furnace is preferably less than 10Pa.
In addition, the preferable scheme is that the preset temperature is 1100-1300 ℃; the preset time is 2-4 h.
In addition, the particle size of the aluminum-silicon-titanium alloy powder is micron-sized; the content of impurity element oxygen in the aluminum-silicon-titanium alloy powder is lower than 150ppm.
According to the technical scheme, the aluminum-silicon-titanium alloy powder and the sodium fluotitanate powder are used as raw materials, and the aluminum-silicon-titanium alloy powder prepared by ball milling, briquetting and vacuum smelting is low in impurity element content and high in purity, so that the quality of the aluminum-silicon-titanium alloy is effectively improved.
To the accomplishment of the foregoing and related ends, one or more aspects of the invention comprise the features hereinafter fully described. The following description and the annexed drawings set forth in detail certain illustrative aspects of the invention. These aspects are indicative, however, of but a few of the various ways in which the principles of the invention may be employed. Further, the present invention is intended to include all such aspects and their equivalents.
Drawings
Other objects and results of the present invention will become more apparent and readily appreciated by reference to the following description taken in conjunction with the accompanying drawings, and as the invention becomes more fully understood. In the drawings:
FIG. 1 is a schematic flow chart of a method for preparing an AlSiTi alloy powder according to an embodiment of the invention.
In the drawings, the same reference numerals indicate similar or corresponding features or functions.
Detailed Description
In the following description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of one or more embodiments. It may be evident, however, that such embodiment(s) may be practiced without these specific details.
Aiming at the problem that the quality of the aluminum-silicon-titanium alloy is influenced by the high content of the impurity element oxygen in the aluminum-silicon-titanium alloy prepared by taking titanium oxide, titanium-containing blast furnace slag or high titanium slag as raw materials at present, the invention provides the method and the device for preparing the aluminum-silicon-titanium alloy powder.
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
In order to illustrate the preparation method of the aluminum-silicon-titanium alloy powder provided by the invention, fig. 1 shows the flow of the preparation method of the aluminum-silicon-titanium alloy powder according to the embodiment of the invention.
As shown in FIG. 1, the preparation method of the aluminum silicon titanium alloy powder provided by the invention comprises the following steps:
s1, adding aluminum-silicon alloy powder and sodium fluotitanate powder into a ball milling device according to a preset mixing proportion, uniformly mixing, and introducing inert protective gas for ball milling treatment to obtain mixed powder;
s2, pressing the mixed powder into a mixed powder block by adopting a mold;
s3, adding the mixed powder block into a vacuum smelting furnace, heating the mixed powder block to a preset temperature under a vacuum condition, and keeping the temperature for a preset time to obtain a reacted material;
and S4, cooling the reacted materials to room temperature to obtain the aluminum-silicon-titanium alloy powder.
The mechanism of the preparation method of the aluminum-silicon-titanium alloy powder provided by the invention is as follows:
the reaction equation of the aluminum-silicon alloy and the sodium fluotitanate is as follows: 7Al x Si 1-x +3Na 2 TiF 6 =Ti 3 Al 7x-4 Si 7-7x +6NaF+4AlF 3 Generating NaF and AlF after heat preservation for preset time at preset temperature 3 . By incubation under vacuum, naF and AlF 3 And separating the aluminum silicon titanium alloy powder by distillation to obtain pure aluminum silicon titanium alloy powder.
Therefore, the aluminum-silicon-titanium alloy powder prepared by adopting the aluminum-silicon alloy powder and the sodium fluotitanate powder as raw materials and matching with ball milling, briquetting and vacuum smelting has low impurity element content and high purity, thereby effectively improving the quality of the aluminum-silicon-titanium alloy.
In a preferred embodiment of the present invention, the aluminum-silicon alloy powder and the sodium fluorotitanate powder are each a powder having a particle size of less than 100 μm; and/or the purities of the aluminum-silicon alloy powder and the sodium fluotitanate powder are both more than 99 percent.
As a preferable embodiment of the present invention, the preset mixing ratio is: the ratio of the number of moles of aluminum-silicon alloy in the aluminum-silicon alloy powder to the number of moles of sodium fluorotitanate in the sodium fluorotitanate powder is greater than 7.
As a preferred scheme of the invention, the ball milling device is a ball mill; the rotating speed of the ball mill is 300-800 rpm.
As a preferable scheme of the invention, in the process of adding the aluminum-silicon alloy powder and the sodium fluotitanate powder into a ball milling device according to a preset mixing proportion, uniformly mixing, and introducing inert protective gas for ball milling treatment to obtain mixed powder, the ball milling time of the aluminum-silicon alloy powder and the sodium fluotitanate powder in the ball milling device is 5-10 h.
As a preferable embodiment of the present invention, the inert shielding gas includes one of nitrogen, argon, helium, neon or at least two mixed in any ratio.
In a preferred embodiment of the present invention, the pressure of the mold against the mixed powder is greater than 40Mpa during the process of pressing the mixed powder into the mixed powder mass using the mold.
As a preferable scheme of the invention, the pressure in the vacuum smelting furnace is less than 10Pa.
As a preferred scheme of the invention, the preset temperature is 1100-1300 ℃; the preset time is 2-4 h.
As a preferable scheme of the invention, the particle size of the aluminum-silicon-titanium alloy powder is micron-sized; the content of impurity element oxygen in the aluminum-silicon-titanium alloy powder is less than 150ppm.
The following examples are presented to further illustrate the present invention so that those skilled in the art may better understand the advantages and features of the present invention.
Example 1:
adding the aluminum-silicon alloy powder and the sodium fluotitanate powder into a ball mill under the condition of nitrogen for ball milling and uniformly mixing, wherein the rotating speed of the ball mill is 300rmp in the ball milling process, and the ball milling time is 10 hours; the molar ratio of aluminum to silicon to titanium in the mixture obtained after ball milling is 5; pressing the mixed material into blocks under the pressure of 40Mpa, putting the blocks into a vacuum tube furnace, reducing the pressure in the vacuum tube furnace to 10Pa, raising the temperature to 1100 ℃ at the heating rate of 5 ℃/min, and preserving the temperature for 2 hours to finally obtain the Al-Si-Ti alloy powder with the particle size of 90 mu m and the oxygen content of 160ppm as shown in Table 1.
TABLE 1
Composition (A) Al Si Ti Fe O
Content/%) 14.14 49.19 63.33 0.001 160ppm
Example 2
Adding the aluminum-silicon alloy powder and the sodium fluotitanate powder into a ball mill under the condition of nitrogen for ball milling and uniformly mixing, wherein the rotating speed of the ball mill is 800rmp in the ball milling process, and the ball milling time is 5 hours; the molar ratio of aluminum to silicon to titanium in the mixture obtained after ball milling is respectively 7; pressing the mixed material into blocks under the pressure of 60Mpa, putting the blocks into a vacuum tube furnace, reducing the pressure in the vacuum tube furnace to 1Pa, raising the temperature to 1300 ℃ at the heating rate of 5 ℃/min, and preserving the temperature for 4h to finally obtain the Al-Si-Ti alloy powder with the particle size of 55 mu m and the oxygen content of 70ppm as shown in Table 2.
TABLE 2
Composition (I) Al Si Ti Fe O
Content/% 45.15 18.59 63.75 0.0005 70ppm
According to the preparation method of the aluminum-silicon-titanium alloy powder, the aluminum-silicon-titanium alloy powder and the sodium fluotitanate powder are used as raw materials, and the aluminum-silicon-titanium alloy powder prepared by ball milling, briquetting and vacuum smelting is matched to be low in impurity element content and high in purity, so that the quality of the aluminum-silicon-titanium alloy is effectively improved.
The proposed method for producing an aluminum silicon titanium alloy powder according to the present invention is described above by way of example with reference to the accompanying drawings. However, it will be appreciated by those skilled in the art that various modifications may be made to the method for preparing the Al-Si-Ti alloy powder set forth in the foregoing without departing from the scope of the invention. Therefore, the scope of the present invention should be determined by the contents of the appended claims.

Claims (10)

1. The preparation method of the aluminum-silicon-titanium alloy powder is characterized by comprising the following steps of:
adding aluminum-silicon alloy powder and sodium fluotitanate powder into a ball-milling device according to a preset mixing proportion, uniformly mixing, and introducing inert protective gas for ball-milling treatment to obtain mixed powder;
pressing the mixed powder into a mixed powder block by adopting a mould;
adding the mixed powder block into a vacuum smelting furnace, heating the mixed powder block to a preset temperature under a vacuum condition, and keeping the temperature for a preset time to obtain a reacted material;
and cooling the reacted materials to room temperature to obtain the aluminum-silicon-titanium alloy powder.
2. The method of producing an AlSiTi alloy powder according to claim 1,
the aluminum-silicon alloy powder and the sodium fluotitanate powder are both powder with the particle size less than 100 mu m; and/or the presence of a gas in the gas,
the purities of the aluminum-silicon alloy powder and the sodium fluotitanate powder are both more than 99%.
3. The method of producing an AlSiTi alloy powder according to claim 1,
the preset mixing proportion is as follows: the ratio of the number of moles of aluminum-silicon alloy in the aluminum-silicon alloy powder to the number of moles of sodium fluorotitanate in the sodium fluorotitanate powder is greater than 7.
4. The method of producing an AlSiTi alloy powder according to claim 1,
the ball milling device is a ball mill;
the rotating speed of the ball mill is 300-800 rpm.
5. The method for preparing the aluminum-silicon-titanium alloy powder according to claim 1, wherein in the process of adding the aluminum-silicon alloy powder and the sodium fluotitanate powder into a ball milling device according to a preset mixing ratio, uniformly mixing, introducing inert protective gas for ball milling treatment to obtain mixed powder,
the ball milling time of the aluminum-silicon alloy powder and the sodium fluotitanate powder in the ball milling device is 5-10 h.
6. The method of producing an AlSiTi alloy powder according to claim 1,
the inert protective gas comprises one of nitrogen, argon, helium and neon or at least two of nitrogen, argon, helium and neon which are mixed according to any proportion.
7. The method for preparing the Al-Si-Ti alloy powder according to claim 1, wherein in the step of pressing the mixed powder into the mixed powder block by using the die,
the pressure of the die on the mixed powder is more than 40Mpa.
8. The method of producing an AlSiTi alloy powder according to claim 1,
the pressure in the vacuum smelting furnace is less than 10Pa.
9. The method of producing an AlSiTi alloy powder according to claim 1,
the preset temperature is 1100-1300 ℃;
the preset time is 2-4 h.
10. The method of producing an AlSiTi alloy powder of claim 1,
the granularity of the aluminum-silicon-titanium alloy powder is micron;
the content of impurity element oxygen in the aluminum-silicon-titanium alloy powder is lower than 150ppm.
CN202210979007.7A 2022-08-16 2022-08-16 Preparation method of aluminum-silicon-titanium alloy powder Active CN115415528B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103243228A (en) * 2013-06-03 2013-08-14 攀钢集团攀枝花钢铁研究院有限公司 Method for producing aluminum silicon titanium alloy with high-titanium blast furnace slag and fly ash as raw materials
CN103266232A (en) * 2013-06-03 2013-08-28 攀钢集团攀枝花钢铁研究院有限公司 Production method of aluminum-silicon-titanium alloy
CN103276241A (en) * 2013-05-13 2013-09-04 攀枝花学院 Titanium aluminum silicon alloy material and preparation method thereof
CN104911376A (en) * 2015-07-17 2015-09-16 东北大学 Method of preparing titanium or titanium-aluminum alloy and additionally producing titanium-free cryolite through two-stage aluminothermic reduction
CN108220601A (en) * 2018-02-11 2018-06-29 沈阳北冶冶金科技有限公司 A kind of preparation method of titanium alloy
CN109402420A (en) * 2018-10-29 2019-03-01 昆明理工大学 A method of titanium silicon and alusil alloy are prepared using titanium-containing blast furnace slag
CN113337745A (en) * 2021-06-04 2021-09-03 中国恩菲工程技术有限公司 Device and method for preparing titanium-based alloy by melting titanium-containing slag

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103276241A (en) * 2013-05-13 2013-09-04 攀枝花学院 Titanium aluminum silicon alloy material and preparation method thereof
CN103243228A (en) * 2013-06-03 2013-08-14 攀钢集团攀枝花钢铁研究院有限公司 Method for producing aluminum silicon titanium alloy with high-titanium blast furnace slag and fly ash as raw materials
CN103266232A (en) * 2013-06-03 2013-08-28 攀钢集团攀枝花钢铁研究院有限公司 Production method of aluminum-silicon-titanium alloy
CN104911376A (en) * 2015-07-17 2015-09-16 东北大学 Method of preparing titanium or titanium-aluminum alloy and additionally producing titanium-free cryolite through two-stage aluminothermic reduction
WO2017012185A1 (en) * 2015-07-17 2017-01-26 东北大学 Method for preparing titanium or titanium aluminum alloy and byproduct- titanium-free cryolite through two-stage aluminothermic reduction
CN108220601A (en) * 2018-02-11 2018-06-29 沈阳北冶冶金科技有限公司 A kind of preparation method of titanium alloy
CN109402420A (en) * 2018-10-29 2019-03-01 昆明理工大学 A method of titanium silicon and alusil alloy are prepared using titanium-containing blast furnace slag
CN113337745A (en) * 2021-06-04 2021-09-03 中国恩菲工程技术有限公司 Device and method for preparing titanium-based alloy by melting titanium-containing slag

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