CN114351001A - Preparation method of adjustable TiB2 in-situ reinforced aluminum-based composite material - Google Patents
Preparation method of adjustable TiB2 in-situ reinforced aluminum-based composite material Download PDFInfo
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Abstract
The invention discloses a method for preparing an adjustable TiB2 in-situ reinforced aluminum-based composite material, which comprises the steps of mixing and melting an aluminum-boron alloy and an aluminum-titanium alloy or pure titanium to prepare TiB2Compounding the preform melt and adding TiB2And adding the composite preform melt into the aluminum alloy matrix melt, mechanically stirring uniformly, and pouring to obtain the adjustable TiB2 in-situ reinforced aluminum matrix composite. The invention can independently design TiB2Preparing different TiB by proportioning the composite prefabricated body and the high-element-content matrix2The aluminum-based composite material with high content has high automatic regulation and control performance, and TiB in the invention2The adding processes of the alloy elements of the composite preform and the aluminum-based composite material are respectively and independently completed,TiB2the generation process of the aluminum-based composite material does not produce burning loss or interactive reaction on alloy elements in the matrix of the aluminum-based composite material, and the element content is accurate and controllable.
Description
Technical Field
The invention belongs to the technical field of aluminum-based composite materials, and relates to an adjustable TiB2A method for preparing an in-situ reinforced aluminum-based composite material.
Background
The in-situ particle reinforced aluminum-based composite material has a series of excellent characteristics of light weight, high specific strength, tight combination of reinforced particles and a matrix and the like, and has very wide application prospect in the field of national defense such as aviation, aerospace, ships, electronics and the like. Currently, in situ autogenous TiB2The reinforced aluminum-based composite material is an aluminum-based composite material which is widely developed and applied and can generate TiB in situ at present2The main preparation method of the reinforced aluminum-based composite material is a fluoride salt method, wherein an aluminum alloy matrix is firstly melted in the production process of the material, then fluoride salt is introduced into the matrix, and TiB is synthesized in situ2And preparing the aluminum matrix composite.
Patent CN201610757301.8 reports a method for preparing a melt-controlled autogenous aluminum-based composite material, which patent uses NaBF4And Na2TiF6As a reaction mix salt, supplemented with Na3AlF6、LiF3、LiCl3As a reaction auxiliary agent, directly reacts in a matrix of aluminum or aluminum alloy to prepare TiB2A reinforced aluminum matrix composite.
Patent CN201711477083.3 reports a high-performance TiB2The preparation process of the/A356 composite material plate comprises the steps of uniformly mixing potassium fluotitanate and potassium fluoborate, adding the mixture into a melted A356 alloy, and obtaining a composite material plate blank after casting and extruding.
Because a large amount of salt reactants are introduced in the preparation process of the material, molten salt residue exists in a reaction system, generated slag is not easy to remove, and the molten salt residue is mixed in the aluminum matrix composite material, so that the performance of the material is greatly influenced. On the other hand, because the reaction of the villiaumite in the system belongs to exothermic reaction, the mixed villiaumite directly reacts in the matrix melt, the melt temperature is extremely high, the elements in the matrix are easily burnt and damaged, and great difficulty is brought to the accurate control of the chemical components of the aluminum matrix composite.
Disclosure of Invention
The invention aims to provide an adjustable TiB2The preparation method of the in-situ reinforced aluminum-based composite material solves the problem that the chemical components in the aluminum-based composite material are difficult to accurately control by the existing method.
The invention adopts the technical scheme that the preparation method of the adjustable TiB2 in-situ reinforced aluminum-based composite material is characterized in that an aluminum-boron alloy and an aluminum-titanium alloy or pure titanium are mixed and melted to prepare TiB2Compounding the preform melt and adding TiB2And adding the composite preform melt into the aluminum alloy matrix melt, mechanically stirring uniformly, and pouring to obtain the adjustable TiB2 in-situ reinforced aluminum matrix composite.
The method specifically comprises the following steps:
step 1, mixing and melting aluminum-boron alloy and aluminum-titanium alloy or pure titanium to prepare TiB2Compounding the preform melt;
step 2, preparing an aluminum alloy matrix melt with high element content, wherein the melt temperature is 720-760 ℃;
step 3, the TiB prepared in the step 1 is used2Pouring the composite preform melt into the high-element-content aluminum alloy matrix melt prepared in the step 2, and mechanically stirring to fully and uniformly mix the two melts;
and 4, degassing and refining the uniformly mixed melt, slagging off and pouring to obtain the adjustable TiB2 in-situ reinforced aluminum matrix composite.
The specific steps of step 1 are as follows:
step 1.1, according to Ti: b atomic ratio is 1: 2, weighing m1Of an aluminum-boron alloy of weight m2Of an aluminum-titanium alloy or pure titanium particles having a particle diameter of 3mm to 5mm, TiB2Designing the generation amount to be m';
step 1.2, smelting an aluminum-boron alloy in a crucible I, controlling the temperature of a melt to be 800-850 ℃, and scattering a covering agent on the surface for later use;
step 1.3, smelting an aluminum-titanium alloy in a crucible II, controlling the temperature of a melt to be 800-850 ℃, or preheating pure titanium particles to be 300-500 ℃;
step 1.4, adding the aluminum-titanium alloy melt or preheated pure titanium particles into the aluminum-boron alloy melt in the crucible I for TiB2The in-situ autogenous reaction of the phases is carried out for 30 to 90min, and the temperature is controlled to be between 800 and 850 ℃;
step 1.5, refining the melt by argon gas and degassing for 10-20min to obtain TiB2The content is m'/(m)1+m2) X 100% of TiB2And compounding the preform melt.
The specific steps of step 2 are as follows:
step 2.1, preparing high-content matrix alloy containing element A and element B … … N, wherein the weight of the matrix alloy is m3Wherein the content of the element A is ma/m3X 100%, the content of B element is mb/m3X 100%, the content of N element is mn/m3×100％；
Step 2.2, according to the smelting process, sequentially adding the alloy of the element A and the alloy of the element B … … N into a crucible III, and melting and heating to 720-760 ℃;
step 2.3, degassing and refining for 10-20min by adopting argon;
and 2.4, after refining is finished, slagging off to obtain the high-element-content aluminum alloy matrix melt.
The specific steps of step 3 are as follows:
step 3.1, mixing TiB in the crucible I2Pouring the composite preform melt into the high-element-content aluminum alloy matrix melt in the crucible III;
and 3.2, mechanically stirring for 5-10min to fully and uniformly mix the melt, and preserving the temperature of the melt at 720-760 ℃.
In the step 4, argon gas is adopted to degas and refine the evenly mixed melt for 10-20 min.
TiB in the adjustable TiB2 in-situ reinforced aluminum-based composite material prepared in the step 42The content is m'/(m)1+m2+m3)×100% and the content of the element A is ma/(m1+m2+m3) X 100%, the content of B element is mb/(m1+m2+m3) X 100%, the content of N element is mn/(m1+m2+m3)×100％。
The invention has the beneficial effects that:
(1) the aluminum-titanium alloy, the pure titanium and the aluminum-boron alloy are adopted as raw materials, the purity is high, salt residues and byproducts generated by a villiaumite method are avoided, and in addition, TiB2The pre-generation process is completed in a pure aluminum medium environment, the problem of burning loss of alloy elements does not exist, and TiB2After the preparation of the composite preform is finished, through thorough refining, degassing and slag removal, the defects of slag inclusion and the like in the subsequent preparation process of the aluminum matrix composite are greatly improved;
(2) when TiB2After the composite prefabricated body and the high-element-content matrix are respectively prepared, the two melts are directly and uniformly mixed, and the TiB is reserved2The preparation of the aluminum-based composite material is efficiently finished under the original generation state of the phase, and the sedimentation and aggregation growth of different components and elements of the aluminum-based composite material due to density difference are avoided;
(3) can design TiB independently2TiB in composite preform2The phase content, the system capable of independently selecting high element content matrix, such as Al-Si series aluminum alloy, Al-Cu series aluminum alloy, etc., and the TiB capable of being independently designed2Preparing different TiB by proportioning the composite prefabricated body and the high-element-content matrix2The aluminum-based composite material with high content has high automatic regulation and control performance, and TiB in the invention2The adding process of the alloy elements of the composite preform and the aluminum-based composite material is respectively and independently completed, and TiB2The generation process of the aluminum-based composite material does not produce burning loss or interactive reaction on alloy elements in the matrix of the aluminum-based composite material, and the element content is accurate and controllable.
Drawings
FIG. 1 is a TiB prepared in example 1 of the present invention2A golden phase diagram of the composite preform;
FIG. 2 is a gold phase diagram of the tunable TiB2 in-situ reinforced aluminum matrix composite prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
A preparation method of a controllable TiB2 in-situ reinforced aluminum matrix composite material comprises the following steps:
step 1, preparing TiB2The composite preform melt comprises the following specific steps:
step 1.1, according to Ti: b atomic ratio is 1: 2, weighing the weight m11kg of an aluminum-boron alloy (AlB8) with a weight m23.55kg of an aluminum titanium alloy (AlTi5), i.e. TiB2The design yield m' is 0.26 kg;
step 1.2, smelting an aluminum-boron alloy in a crucible I, controlling the temperature of a melt to be 800 ℃, and scattering a covering agent on the surface for later use;
step 1.3, smelting an aluminum-titanium alloy in a crucible II, and controlling the melt temperature to be 800 ℃;
step 1.4, adding the aluminum-titanium alloy melt into the aluminum-boron alloy melt in the crucible I to perform TiB2Carrying out in-situ self-generated reaction for 30min at 800 ℃;
step 1.5, refining the melt by argon gas and degassing for 10min to obtain TiB2TiB content of 5.66%2And compounding the preform melt. Preparing another part of TiB by adopting the step 12TiB content of 5.66%2Casting the composite preform melt to obtain TiB2And (3) observing the micro-topography of the composite preform, as shown in FIG. 1.
TiB2In the process of preparing the composite preform, Ti atoms and B atoms TiB released by the raw materials are molten at high temperature2The thermodynamic equation of the reaction is shown in the following formula 1:
Ti+B→TiB2(s) (1)
according to thermodynamic calculation, the gibbs free energy of the reaction formula becomes:
ΔG＝－73381+38.996T
it can be seen that Δ G is still a large negative value at 780 ℃, i.e. 1053K, and the tendency of spontaneous progression is large, during the melting process, the B atom of the Ti nucleus is preferentially bonded, the bonding energy is large, and the Ti nucleus can stably exist in the melt for a long time.
Step 2, preparing the high-element-content aluminum alloy matrix melt, which comprises the following specific steps:
step 2.1, taking pure aluminum, an Al-Si intermediate alloy, an Al-Ti intermediate alloy and pure magnesium as raw materials, and preparing a high-element-content matrix alloy containing 14 wt.% of Si element, 0.7 wt.% of Mg element, 0.3 wt.% of Ti element and the balance of Al, wherein the weight m is34.55 kg;
step 2.2, according to the smelting process, adding pure aluminum, Al-Si intermediate alloy, Al-Ti intermediate alloy and pure magnesium into a crucible III in sequence, and melting and heating to 720 ℃;
step 2.3, degassing and refining for 10min by adopting argon;
and 2.4, after refining is finished, slagging off to obtain the high-element-content aluminum alloy matrix melt.
Step 3, mixing TiB2The method comprises the following steps of uniformly mixing a composite preform melt and a high-element-content aluminum alloy matrix melt:
step 3.1, mixing TiB in the crucible I2Pouring the composite preform melt into the high-element-content aluminum alloy matrix melt in the crucible III;
and 3.2, mechanically stirring for 5min to fully and uniformly mix the melt, and preserving the temperature of the melt at 720 ℃.
And 4, degassing and refining the uniformly mixed melt for 10min by adopting argon, slagging off and pouring to obtain the adjustable TiB2 in-situ reinforced aluminum-based composite material, wherein TiB in the prepared adjustable TiB2 in-situ reinforced aluminum-based composite material2The content was 2.83%, the content of Si element was 7 wt.%, the content of Mg element was 3.5 wt.%, and the content of Ti element was 0.15 wt.%.
Metallographic structure observation is carried out on the adjustable TiB2 in-situ reinforced aluminum-based composite material prepared in the embodiment 1, a metallographic phase diagram of the metallographic phase diagram is shown in figure 2, and as can be seen from figure 2, the adjustable TiB2 in-situ reinforced aluminum-based composite material prepared by the method disclosed by the invention is uniform in component and low in impurity content.
Example 2
Step 1, preparing TiB2The composite preform melt comprises the following specific steps:
step 1.1, according to Ti: b atomic ratio is 1: 2, weighing the weight m11kg of an aluminum-boron alloy (AlB8) with a weight m21.64kg of an aluminum titanium alloy (AlTi10), i.e. TiB2The design yield m' is 0.26 kg;
step 1.2, smelting an aluminum-boron alloy in a crucible I, controlling the temperature of a melt to be 820 ℃, and scattering a covering agent on the surface for later use;
step 1.3, smelting an aluminum-titanium alloy in a crucible II, and controlling the melt temperature to be 820 ℃;
step 1.4, adding the aluminum-titanium alloy melt into the aluminum-boron alloy melt in the crucible I to perform TiB2Carrying out in-situ self-generated reaction for 50min at 820 ℃;
step 1.5, refining the melt by argon gas and degassing for 15min to obtain TiB2TiB content of 9.8%2And compounding the preform melt.
Step 2, preparing the high-element-content aluminum alloy matrix melt, which comprises the following specific steps:
step 2.1, taking pure aluminum, an Al-Si intermediate alloy, an Al-Ti intermediate alloy and pure magnesium as raw materials, and preparing a high-element-content matrix alloy containing 14 wt.% of Si element, 0.7 wt.% of Mg element, 0.3 wt.% of Ti element and the balance of Al, wherein the weight m is32.64 kg;
step 2.2, according to the smelting process, adding pure aluminum, Al-Si intermediate alloy, Al-Ti intermediate alloy and pure magnesium into a crucible III in sequence, and melting and heating to 740 ℃;
step 2.3, degassing and refining for 15min by adopting argon;
and 2.4, after refining is finished, slagging off to obtain the high-element-content aluminum alloy matrix melt.
Step 3, mixing TiB2The method comprises the following steps of uniformly mixing a composite preform melt and a high-element-content aluminum alloy matrix melt:
step 3.1, mixing TiB in the crucible I2Pouring the composite preform melt into the high-element-content aluminum alloy matrix melt in the crucible III;
and 3.2, mechanically stirring for 7min to fully and uniformly mix the melt, and keeping the temperature of the melt at 740 ℃.
And 4, degassing and refining the uniformly mixed melt for 15min by adopting argon, slagging off and pouring to obtain the adjustable TiB2 in-situ reinforced aluminum-based composite material, wherein TiB in the prepared adjustable TiB2 in-situ reinforced aluminum-based composite material2The content was 4.9%, the content of Si element was 7 wt.%, the content of Mg element was 3.5 wt.%, and the content of Ti element was 0.15 wt.%.
Example 3
Step 1, preparing TiB2The composite preform melt comprises the following specific steps:
step 1.1, according to Ti: b atomic ratio is 1: 2, weighing the weight m110kg of an aluminium boron alloy (AlB3), weight m20.67kg of pure titanium particles, i.e. TiB2The design yield m' is 0.97 kg;
step 1.2, smelting an aluminum-boron alloy in a crucible I, controlling the temperature of a melt to be 850 ℃, and scattering a covering agent on the surface for later use;
step 1.3, preheating pure titanium particles, controlling the temperature to be 400 ℃, and the preheating time to be 2 hours;
step 1.4, adding the preheated pure titanium particles into an aluminum boron alloy melt in a crucible I to perform TiB2Carrying out in-situ self-generated reaction for 90min at 850 ℃;
step 1.5, refining the melt by argon gas and degassing for 20min to obtain TiB2TiB content of 9.0%2And compounding the preform melt.
Step 2, preparing the high-element-content aluminum alloy matrix melt, which comprises the following specific steps:
step 2.1, taking pure aluminum, an Al-Si intermediate alloy, an Al-Ti intermediate alloy and pure magnesium as raw materials, and preparing a high-element-content matrix alloy containing 14 wt.% of Si element, 0.7 wt.% of Mg element, 0.3 wt.% of Ti element and the balance of Al, wherein the weight m is310.67 kg;
step 2.2, according to the smelting process, sequentially adding pure aluminum, Al-Si intermediate alloy, Al-Ti intermediate alloy and pure magnesium into a crucible III, and melting and heating to 760 ℃;
step 2.3, degassing and refining for 20min by adopting argon;
and 2.4, after refining is finished, slagging off to obtain the high-element-content aluminum alloy matrix melt.
Step 3, mixing TiB2The method comprises the following steps of uniformly mixing a composite preform melt and a high-element-content aluminum alloy matrix melt:
step 3.1, mixing TiB in the crucible I2Pouring the composite preform melt into the high-element-content aluminum alloy matrix melt in the crucible III;
and 3.2, mechanically stirring for 10min to fully and uniformly mix the melt, and keeping the temperature of the melt at 760 ℃.
And 4, degassing and refining the uniformly mixed melt for 20min by adopting argon, slagging off and pouring to obtain the adjustable TiB2 in-situ reinforced aluminum-based composite material, wherein TiB in the prepared adjustable TiB2 in-situ reinforced aluminum-based composite material2The content was 4.5%, the content of Si element was 7 wt.%, the content of Mg element was 3.5 wt.%, and the content of Ti element was 0.15 wt.%.
Claims (7)
1. The preparation method of the adjustable TiB2 in-situ reinforced aluminum-based composite material is characterized in that an aluminum-boron alloy and an aluminum-titanium alloy or pure titanium are mixed and melted to prepare the TiB2Compounding the preform melt and adding TiB2And adding the composite preform melt into the aluminum alloy matrix melt, mechanically stirring uniformly, and pouring to obtain the adjustable TiB2 in-situ reinforced aluminum matrix composite.
2. The method for preparing the controllable TiB2 in-situ reinforced aluminum-based composite material according to claim 1, comprising the following steps:
step 1, mixing and melting aluminum-boron alloy and aluminum-titanium alloy or pure titanium to prepare TiB2Compounding the preform melt;
step 2, preparing an aluminum alloy matrix melt with high element content, wherein the melt temperature is 720-760 ℃;
step 3, the TiB prepared in the step 1 is used2Pouring the composite preform melt into the mold prepared in step 2Mechanically stirring the element-content aluminum alloy matrix melt to fully and uniformly mix the two melts;
and 4, degassing and refining the uniformly mixed melt, slagging off and pouring to obtain the adjustable TiB2 in-situ reinforced aluminum matrix composite.
3. The method for preparing the controllable TiB2 in-situ reinforced aluminum-based composite material according to claim 2, wherein the specific steps of step 1 are as follows:
step 1.1, according to Ti: b atomic ratio is 1: 2, weighing m1Of an aluminum-boron alloy of weight m2Of an aluminum-titanium alloy or pure titanium particles having a particle diameter of 3mm to 5mm, TiB2Designing the generation amount to be m';
step 1.2, smelting an aluminum-boron alloy in a crucible I, controlling the temperature of a melt to be 800-850 ℃, and scattering a covering agent on the surface for later use;
step 1.3, smelting an aluminum-titanium alloy in a crucible II, controlling the temperature of a melt to be 800-850 ℃, or preheating pure titanium particles to be 300-500 ℃;
step 1.4, adding the aluminum-titanium alloy melt or preheated pure titanium particles into the aluminum-boron alloy melt in the crucible I for TiB2The in-situ autogenous reaction of the phases is carried out for 30 to 90min, and the temperature is controlled to be between 800 and 850 ℃;
step 1.5, refining the melt by argon gas and degassing for 10-20min to obtain TiB2The content is m'/(m)1+m2) X 100% of TiB2And compounding the preform melt.
4. The method for preparing the controllable TiB2 in-situ reinforced aluminum-based composite material according to claim 3, wherein the specific steps of step 2 are as follows:
step 2.1, preparing high-content matrix alloy containing element A and element B … … N, wherein the weight of the matrix alloy is m3Wherein the content of the element A is ma/m3X 100%, the content of B element is mb/m3X 100%, the content of N element is mn/m3×100％；
Step 2.2, according to the smelting process, sequentially adding the alloy of the element A and the alloy of the element B … … N into a crucible III, and melting and heating to 720-760 ℃;
step 2.3, degassing and refining for 10-20min by adopting argon;
and 2.4, after refining is finished, slagging off to obtain the high-element-content aluminum alloy matrix melt.
5. The method for preparing the controllable TiB2 in-situ reinforced aluminum-based composite material according to claim 4, wherein the specific steps of step 3 are as follows:
step 3.1, mixing TiB in the crucible I2Pouring the composite preform melt into the high-element-content aluminum alloy matrix melt in the crucible III;
and 3.2, mechanically stirring for 5-10min to fully and uniformly mix the melt, and preserving the temperature of the melt at 720-760 ℃.
6. The method for preparing the controllable TiB2 in-situ reinforced aluminum-based composite material according to claim 5, wherein in the step 4, argon degassing refining is performed on the uniformly mixed melt for 10-20 min.
7. The method for preparing the adjustable TiB2 in-situ reinforced Al-based composite material of claim 6, wherein the adjustable TiB2 in-situ reinforced Al-based composite material prepared in the step 4 comprises TiB2The content is m'/(m)1+m2+m3) X 100%, the content of A element is ma/(m1+m2+m3) X 100%, the content of B element is mb/(m1+m2+m3) X 100%, the content of N element is mn/(m1+m2+m3)×100％。
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| CN112831680A (en) * | 2020-12-31 | 2021-05-25 | 南京理工大学 | Superhard multi-component boride particle reinforced aluminum matrix composite material and preparation method thereof |
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| CN105441701A (en) * | 2014-09-29 | 2016-03-30 | 邬青 | TiB2/Al-Si-Mg alloy |
| CN107377903A (en) * | 2017-06-26 | 2017-11-24 | 永杰新材料股份有限公司 | A kind of casting and rolling molding method and system of in-situ endogenic particle enhanced aluminum-based composite material |
| CN109957685A (en) * | 2019-04-19 | 2019-07-02 | 大连科天新材料有限公司 | A kind of high dispersive TiB2/ A356 composite material and preparation method thereof |
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