CN111318656B - RbCl/BaCl2Mixed aerosol and method for preparing magnesium-based metal semisolid slurry by using same - Google Patents

RbCl/BaCl2Mixed aerosol and method for preparing magnesium-based metal semisolid slurry by using same Download PDF

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CN111318656B
CN111318656B CN202010200483.5A CN202010200483A CN111318656B CN 111318656 B CN111318656 B CN 111318656B CN 202010200483 A CN202010200483 A CN 202010200483A CN 111318656 B CN111318656 B CN 111318656B
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rbcl
bacl
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CN111318656A (en
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铁镝
刘海峰
陈民芳
张博彧
付莹
李卫荣
金刚
马立新
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Liaoning Ruiou New Material Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D1/00—Treatment of fused masses in the ladle or the supply runners before casting
    • B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract

RbCl/BaCl2A mixed aerosol and a method for preparing magnesium-based metal semisolid slurry by using the same belong to the field of metal material preparation. The RbCl/BaCl2Mixed aerosol comprising aerosol solute and aerosol solvent, the aerosol solute comprising total RbCl/BaCl2The mass percentage of the mixed aerosol is 80-85%; the aerosol solutes are RbCl and BaCl2Mixed powder with the mass ratio of 2: 3; the aerosol solvent is a single or mixed gas that does not react with the magnesium alloy melt, including but not limited to inert gases and/or shielding gases commonly used in magnesium melting. Mixing RbCl/BaCl2The mixed aerosol is introduced into the magnesium alloy melt in the semi-solid temperature range and is fully contacted with the magnesium alloy melt, so that magnesium-based metal semi-solid slurry is formed. Compared with the traditional preparation method of magnesium alloy semi-solid slurry, the method has the advantages of simple and reliable equipment, stable process, high product quality and the like, and can achieve the effects of energy conservation and emission reduction while reducing the cost.

Description

RbCl/BaCl2Mixed aerosol and method for preparing magnesium-based metal semisolid slurry by using same
Technical Field
The invention discloses an RbCl/BaCl2A mixed aerosol and a method for preparing magnesium-based metal semisolid slurry by using the same relate to the field of metal material preparation, and can be used for quickly and efficiently preparing magnesium-based alloy metal semisolid slurry.
Background
The semi-solid metal forming process has short technological process, high product performance and other features, and is one of the metal forming technologies with wide application foreground in the 21 st century. After decades of research and development, the semi-solid metal forming technology is rapidly developed and is currently in the industrial application stage. The basic principle of metal semi-solid forming is to form and process alloy in a solid-liquid two-phase region, and the alloy has the characteristics and advantages of liquid and solid forming. The metal semi-solid forming product has strong technological adaptability, is suitable for producing alloy products with complex structures, and has excellent mechanical properties. Compared with the traditional liquid and solid forming, the method has the following advantages: the die has small thermal shock and long service life; the product has small shrinkage and low gas content; the machining allowance is small, and the yield is high; low energy consumption, environmental protection and the like. Not only broadens the application range of alloy products, but also has important significance for the preparation of new materials such as metal matrix composite materials and the like.
The technical core of the metal semi-solid forming process is to prepare metal semi-solid slurry, obtain spheroidized and refined solidification structures and effectively avoid coarse dendrites influencing mechanical properties in alloy structures solidified in a conventional liquid state. The method for quickly and efficiently obtaining the metal semi-solid slurry with good structure is the basis and the key of metal semi-solid forming, but the problems of high energy consumption, long flow, unstable process, low structure nodularity and the like generally exist in the existing pulping means.
An aerosol is a colloidal dispersion of small particles of a solid or liquid dispersed and suspended in a gaseous medium, also known as a gas dispersion. The dispersion phase is solid or liquid small particles with a size of 0.001-100 μm, and the dispersion medium is gas. Because the solute particles have small diameters, the diffusion speed in a liquid phase is high, and the traditional mechanical stirring is not relied on to promote the particle diffusion. In actual production, aerosols are mainly used in the field of fire protection; can also be used for spraying pesticides to improve the pesticide effect and reduce the consumption of the drugs; the meteorological department also uses aerosol to make artificial rainfall so as to improve the drought. But their use in the metallurgical and material processing fields has been rarely reported.
Disclosure of Invention
In order to overcome the defects of the preparation of metal semi-solid slurry in the prior art, the invention provides RbCl/BaCl2Mixed gas solutionGlue and a method for preparing magnesium-based metal semi-solid slurry. The method comprises the steps of introducing RbCl/BaCl into a melt2Mixing the aerosols as RbCl/BaCl2As active solute particles, the characteristics of small diameter and high dispersion degree of the active solute particles are utilized, when RbCl/BaCl2The mixed aerosol dispersed fine active solute particle phase is adsorbed to the surface when it encounters the larger volume of the primary solid phase. The active solute particles form a coating effect on the primary solid phase, so that the heat exchange of the primary solid phase is prevented, the surface tension of the contact surface of the crystal nucleus and the melt is greatly improved, and the primary solid phase is promoted to be converted to be nearly spherical. Compared with the traditional preparation method of magnesium alloy semi-solid slurry, the method has the advantages of simple and reliable equipment, stable process, high product quality and the like, and can obviously shorten the process flow and reduce the production cost.
RbCl/BaCl2A mixed aerosol comprising an aerosol solute and an aerosol solvent, said aerosol solute comprising total RbCl/BaCl2The mass percentage of the mixed aerosol is 80-85%;
the aerosol solute is RbCl and BaCl2The mixed powder comprises the following components in percentage by mass, RbCl: BaCl22:3, the purity of solute raw materials is chemical purity; the equivalent diameter of RbCl powder is less than or equal to 200nm, and BaCl2The equivalent diameter of the powder is less than or equal to 200 nm;
the aerosol solvent is a single or mixed gas which does not react with the magnesium alloy melt, and includes but is not limited to inert gas and/or protective gas commonly used for magnesium smelting.
In the aerosol solvent, the purity of the used gas is chemical purity or more.
RbCl/BaCl2Mixed aerosols, dispersed phase RbCl/BaCl2The equivalent diameter is less than or equal to 200nm, and the diffusion speed in the melt is high due to the small equivalent diameter, so that a compact film layer can be formed on the surface of the primary solid phase by virtue of the adsorption of the primary solid phase and the surface tension effect, the heat and mass transfer isolation effect is realized, the growth of the primary solid phase is inhibited, and the nucleation mass point is used as a nucleation mass point, and the nucleation rate is enhanced. Meanwhile, the aerosol solvent has a refining effect on the melt, so that the quality of the melt can be improved.
RbCl/BaCl2The preparation method of the mixed aerosol comprises the following steps:
step 1:
according to the preparation requirements of the aerosol solvent, if a single gas can be directly used as the aerosol solvent; if the gas mixture is a plurality of mixed gases, the gas mixture is mixed under the same temperature and pressure to obtain an aerosol solvent;
step 2:
RbCl and BaCl are weighed according to the mass ratio of each powder in aerosol solute2Uniformly mixing to obtain aerosol solute;
and step 3:
mixing aerosol solute and aerosol solvent according to mass percent to obtain RbCl/BaCl2The aerosols are mixed.
The invention relates to RbCl/BaCl2The method for preparing the magnesium-based metal semi-solid slurry by the mixed aerosol comprises the following steps:
mixing RbCl/BaCl2The mixed aerosol is introduced into the magnesium alloy melt in the semi-solid temperature range and is fully contacted with the magnesium alloy melt, so that magnesium-based metal semi-solid slurry is formed.
The semi-solid temperature range is determined according to the components of the magnesium alloy melt and the mass percentage of each component, and is preferably 600-650 ℃.
The leading-in flow is 100-300 mL/min, the leading-in time of the tundish type pulping device is 28-35 min, and the temperature needs to be heated to 575-585 ℃ before leading-in.
Wherein, under the condition of using the tundish device for pulping, the quality of the magnesium alloy melt and RbCl/BaCl2The volume consumption proportion of the mixed aerosol is preferably that RbCl/BaCl is correspondingly added into each kilogram of magnesium alloy melt2The volume of the mixed aerosol is 1-2L.
The invention relates to RbCl/BaCl2Compared with the prior preparation of metal semi-solid slurry, the mixed aerosol and the method for preparing the magnesium-based metal semi-solid slurry have the beneficial effects that:
in the method for preparing the metal semi-solid slurry of the invention, the advantages areThe active component RbCl/BaCl is used under the action of aerosol dispersion distribution2Attached to the surface of the primary solid phase of the alloy melt, the surface tension of the contact surface of the crystal nucleus and the melt can be greatly improved, and the nodularity of the metal semi-solid slurry is improved, wherein the schematic diagram of the pulping mechanism of the metal semi-solid slurry is shown in figure 1. The powder can prevent the solid phase from continuously growing after being uniformly attached to the primary solid phase, or can be used as nucleation particles of heterogeneous nucleation, so that the microstructure of a product cast or die-cast by adopting semi-solid slurry is obviously refined, and the average grain size of the product after casting or die-casting is 20-35 microns. Compared with the traditional preparation method of magnesium alloy semi-solid slurry, the method has the advantages of simple and reliable equipment, stable process, high product quality and the like, and can achieve the effects of energy conservation and emission reduction while reducing the cost.
Drawings
FIG. 1 shows RbCl/BaCl of the present invention2And (3) a mixed aerosol pulping mechanism schematic diagram.
Fig. 2 is a schematic structural diagram of a device in a manufacturing process according to embodiment 1 of the present invention.
Fig. 3 is a schematic structural diagram of a device in a manufacturing process according to embodiment 2 of the present invention.
Fig. 4 is a schematic structural diagram of a device in a manufacturing process according to embodiment 3 of the present invention.
In the above figures, 1 is a crucible tundish, 2 is an introduction tube, and 3 is RbCl/BaCl2And (3) mixing aerosol, wherein 4 is alloy melt, 5 is a launder, and 6 is a mould.
Detailed Description
The following three examples illustrate specific embodiments of the present invention, but are not intended to limit the scope of the present invention. Any changes and modifications to the following real-time modes according to the technical essence of the present invention are within the scope of the technical solution of the present invention, unless the contents of the technical solution of the present invention are departed.
In the following examples, unless otherwise specified, the starting materials and equipment used are commercially available, wherein the starting materials are chemically pure or more.
Example 1
In this example, 3Kg-AZ91 magnesium alloy semi-solid slurry was prepared using the present method.
RbCl/BaCl2The preparation method of the mixed aerosol comprises the following steps:
firstly, chemically pure RbCl (rubidium chloride) and BaCl2The mass ratio of (barium chloride) powder RbCl: BaCl22:3, mixing to obtain aerosol solute;
adding the prepared aerosol solute into a 50L high-pressure resistant gas tank, wherein the mass of the added aerosol solute is RbCl/BaCl2The mass ratio of the mixed aerosol is 80%;
then the chemical pure argon gas is compressed into a high pressure resistant gas tank under the conditions of room temperature and 14.5MPa to be mixed to form RbCl/BaCl2And storing the mixed aerosol for later use.
Using the above RbCl/BaCl2The preparation process schematic diagram of the method for preparing magnesium-based metal semi-solid slurry by mixed aerosol is shown in figure 2, and the method specifically comprises the following steps:
pouring the well smelted AZ91 magnesium alloy melt 4 at 645 ℃ into a crucible tundish 1 preheated to 600 ℃, and heating under a protective atmosphere. AZ91 magnesium alloy melt 4 in the crucible tundish 1 is heated to 645 ℃ and kept at a constant temperature, and RbCl/BaCl preheated to 575 ℃ is prepared through an introducing pipe 2 at a flow rate of 100mL/min2And introducing the mixed aerosol 3 into the AZ91 magnesium alloy melt 4 for 40min, and after the time is up to closing an aerosol pipeline valve, keeping the temperature at the constant temperature for 4 min, finishing pulping to obtain the AZ91 magnesium alloy semi-solid slurry.
The prepared AZ91 magnesium alloy semi-solid slurry can prove that the surface tension difference is formed in the melt due to the solid phase volume difference, so that the adsorption effect exists. The equivalent diameter of primary grains and the shape factor of the slurry prepared in this example are shown in Table 1.
Example 2
In this example, 3Kg-AZ91 magnesium alloy semi-solid slurry was prepared using the present method.
Firstly, chemically pure RbCl (rubidium chloride) and BaCl2The mass ratio of (barium chloride) powder RbCl: BaCl2Mixing as aerosol solute 2: 3;
adding the prepared aerosol solute into 50L of the resistantIn the high-pressure gas tank, the mass of the added aerosol solute is RbCl/BaCl282% of the mass ratio of the mixed aerosol;
then the chemically pure helium gas under the conditions of room temperature and 14.5MPa is compressed into a high pressure resistant gas tank for mixing to form RbCl/BaCl2And storing the mixed aerosol for later use.
Using the above RbCl/BaCl2The preparation method of the magnesium-based metal semi-solid slurry by the mixed aerosol is shown in figure 3, and comprises the following steps:
heating the AZ91 alloy to 650 ℃, and placing the obtained AZ91 alloy melt 4 into a mould 6; the AZ91 alloy melt 4 was poured into a launder 5 preheated to 620 ℃ at an angle of 35 ℃ to the horizontal and 420mm long. RbCl/BaCl prepared and preheated to 580 ℃ is introduced into the reactor through the introduction pipe 22The mixed aerosol 3 and the AZ91 alloy melt 4 flow in the same direction, and RbCl/BaCl2The introduction flow rate of the mixed aerosol 3 was 250mL/min, and RbCl/BaCl was adjusted to2The mixed aerosol 3 is in full contact with the alloy melt 4. Refining the melt with an aerosol solvent, and obtaining active RbCl/BaCl2And (3) enabling the particles to enter the melt and be adsorbed on the surface of the primary solid phase to finish the preparation of the semi-solid slurry, thus obtaining the AZ91 magnesium alloy semi-solid slurry.
The equivalent diameter of primary grains and the shape factor of the slurry prepared in this example are shown in Table 1.
Example 3
In this example, 3Kg-AM60 magnesium alloy semi-solid slurry was prepared using the present method.
Firstly, chemically pure RbCl (rubidium chloride) and BaCl2The mass ratio of (barium chloride) powder RbCl: BaCl2Mixing as aerosol solute 2: 3;
adding the prepared aerosol solute into a 50L high-pressure-resistant gas tank, wherein the added aerosol solute accounts for 85% of the mass of the aerosol;
then argon and helium with equal volume ratio under the conditions of room temperature and 14.5MPa are compressed into the high pressure resistant gas tank for mixing to form RbCl/BaCl2And storing the mixed aerosol for later use.
Using the above RbCl/BaCl2MixingThe preparation process schematic diagram of the method for preparing magnesium-based metal semisolid slurry by using aerosol is shown in figure 4, and the method comprises the following steps:
weighing 3Kg of AM60 magnesium alloy with an oxide layer removed, heating to 630 ℃, and placing the obtained AM60 magnesium alloy melt 4 in a die 6; the AM60 magnesium alloy melt 4 is poured into a launder 5 which is preheated to 620 ℃, forms an inclination angle of 30 degrees with the horizontal plane and has a length of 420 mm. The prepared RbCl/BaCl preheated to 585 ℃ was introduced into the reactor through the introduction tube 22The mixed aerosol 3 and the AM60 magnesium alloy melt 4 flow in the opposite directions, and RbCl/BaCl2The introduction flow rate of the mixed aerosol 3 is 200mL/min, so that RbCl/BaCl2The mixed aerosol 3 is fully contacted with the alloy melt 4 from bottom to top. Refining the melt with an aerosol solvent, and obtaining active RbCl/BaCl2And (3) enabling the particles to enter the melt and be adsorbed on the surface of the primary solid phase to finish the preparation of the semi-solid slurry, thus obtaining the AZ91 magnesium alloy semi-solid slurry.
The equivalent diameter of primary grains and the shape factor of the slurry prepared in this example are shown in Table 1.
TABLE 1 Primary grain equivalent diameter and shape factor for slurries prepared in three examples
Figure BDA0002419188650000051

Claims (6)

1. RbCl/BaCl2Mixed aerosol, characterized in that the RbCl/BaCl2The mixed aerosol comprises aerosol solute and aerosol solvent, wherein the aerosol solute accounts for total RbCl/BaCl2The mass percentage of the mixed aerosol is 80-85%;
the aerosol solute is RbCl and BaCl2The mixed powder comprises the following components in percentage by mass, RbCl: BaCl2=2:3, the purity of solute raw materials is chemical purity; the equivalent diameter of RbCl powder is less than or equal to 200nm, and BaCl2The equivalent diameter of the powder is less than or equal to 200 nm;
the aerosol solvent is a single or mixed gas which does not react with the magnesium alloy melt, and the purity of the gas raw material for preparing the aerosol solvent is chemical purity or more.
2. The RbCl/BaCl of claim 12The preparation method of the mixed aerosol is characterized by comprising the following steps:
step 1:
according to the preparation requirements of the aerosol solvent, if a single gas can be directly used as the aerosol solvent; if the gas mixture is a plurality of mixed gases, the gas mixture is mixed under the same temperature and pressure to obtain an aerosol solvent;
step 2:
RbCl and BaCl are weighed according to the mass ratio of each powder in aerosol solute2Uniformly mixing to obtain aerosol solute;
and step 3:
mixing aerosol solute and aerosol solvent according to mass percent to obtain RbCl/BaCl2The aerosols are mixed.
3. The RbCl/BaCl of claim 12The method for preparing the magnesium-based metal semi-solid slurry by the mixed aerosol is characterized by comprising the following steps of:
mixing RbCl/BaCl2The mixed aerosol is introduced into the magnesium alloy melt in the semi-solid temperature range and is fully contacted with the magnesium alloy melt, so that magnesium-based metal semi-solid slurry is formed.
4. The RbCl/BaCl of claim 32The method for preparing magnesium-based metal semi-solid slurry by mixed aerosol is characterized in that the semi-solid temperature range is determined according to the components of a magnesium alloy melt and the mass percentage content of each component, and is specifically 600-650 ℃.
5. The RbCl/BaCl of claim 32The method for preparing magnesium-based metal semi-solid slurry by mixed aerosol is characterized in that the introducing flow is 100-300 mL/min, the introducing time of a tundish type pulping device is 28-35 min, and the magnesium-based metal semi-solid slurry needs to be heated to 575-585 ℃ before introduction.
6. Root of herbaceous plantRbCl/BaCl of claim 32The method for preparing magnesium-based metal semi-solid slurry by using mixed aerosol is characterized in that the mass of magnesium alloy melt and RbCl/BaCl are mixed under the condition of using a tundish device for pulping2The volume consumption proportion of the mixed aerosol is as follows: RbCl/BaCl is correspondingly added into each kilogram of magnesium alloy melt2The volume of the mixed aerosol is 1-2L.
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1119460A (en) * 1994-01-21 1996-03-27 勃勒许·威尔曼股份有限公司 Semi-solid processed magnesium-beryllium alloys
CN101367124A (en) * 2008-07-31 2009-02-18 镁联科技（芜湖）有限公司 Method of manufacturing magnesium alloy semi-solid state blank
CN101437967A (en) * 2005-04-19 2009-05-20 斯特恩利奇公司 Method for adding boron to metal alloys
CN103170603A (en) * 2013-03-27 2013-06-26 福建省瑞奥麦特轻金属有限责任公司 Preparation method for aluminum alloy or magnesium alloy semi-solid sizing agents
CN103789590A (en) * 2014-03-04 2014-05-14 哈尔滨工业大学 Preparation method of particle-reinforced magnesium-based composite material
CN103820661A (en) * 2014-02-27 2014-05-28 上海交通大学 Preparation method of semisolid slurry of rare earth magnesium alloy
CN104313371A (en) * 2014-09-29 2015-01-28 南昌大学 Method for preparing magnesium matrix composite semisolid slurry by adopting ultrasonic in situ synthesis
CN104668500A (en) * 2013-12-02 2015-06-03 北京有色金属研究总院 Device and method for preparing aluminum/magnesium alloy semi-solid slurry

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1119460A (en) * 1994-01-21 1996-03-27 勃勒许·威尔曼股份有限公司 Semi-solid processed magnesium-beryllium alloys
CN101437967A (en) * 2005-04-19 2009-05-20 斯特恩利奇公司 Method for adding boron to metal alloys
CN101367124A (en) * 2008-07-31 2009-02-18 镁联科技（芜湖）有限公司 Method of manufacturing magnesium alloy semi-solid state blank
CN103170603A (en) * 2013-03-27 2013-06-26 福建省瑞奥麦特轻金属有限责任公司 Preparation method for aluminum alloy or magnesium alloy semi-solid sizing agents
CN104668500A (en) * 2013-12-02 2015-06-03 北京有色金属研究总院 Device and method for preparing aluminum/magnesium alloy semi-solid slurry
CN103820661A (en) * 2014-02-27 2014-05-28 上海交通大学 Preparation method of semisolid slurry of rare earth magnesium alloy
CN103789590A (en) * 2014-03-04 2014-05-14 哈尔滨工业大学 Preparation method of particle-reinforced magnesium-based composite material
CN104313371A (en) * 2014-09-29 2015-01-28 南昌大学 Method for preparing magnesium matrix composite semisolid slurry by adopting ultrasonic in situ synthesis

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