CN114351001B - Method for preparing adjustable TiB2 in-situ reinforced aluminum-based composite material - Google Patents
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Abstract
The invention discloses a method for preparing an adjustable TiB2 in-situ reinforced aluminum-based composite material, which mixes and melts an aluminum-boron alloy and an aluminum-titanium alloy or pure titanium to prepare TiB 2 Compounding the preform melt and adding TiB 2 And 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 TiB 2 Preparing different TiB by proportioning the composite prefabricated body and the high-element-content matrix 2 The aluminum-based composite material with high content has high automatic regulation and control performance, and TiB in the invention 2 The adding processes of the alloy elements of the composite preform and the aluminum-based composite material are respectively and independently operated and finished, and TiB 2 The 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 TiB 2 A 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 TiB 2 The reinforced aluminum-based composite material is an aluminum-based composite material which is widely developed and applied and can generate TiB in situ at the present stage 2 The main preparation method of the reinforced aluminum-based composite material is a fluoride salt method, and the production process of the material is firstly to prepare the reinforced aluminum-based composite materialMelting the aluminum alloy matrix, introducing villiaumite into the matrix, and synthesizing TiB in situ 2 And preparing the aluminum matrix composite.
CN201610757301.8 reports a preparation method of melt-controlled autogenous aluminum matrix composite, which adopts NaBF 4 And Na 2 TiF 6 As a reaction mix salt, supplemented with Na 3 AlF 6 、LiF 3 、LiCl 3 As a reaction auxiliary agent, directly reacts in a matrix of aluminum or aluminum alloy to prepare TiB 2 A reinforced aluminum matrix composite.
Patent CN201711477083.3 reports a high-performance TiB 2 The 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 residues exist in a reaction system, and generated slag is not easy to remove and is mixed in the aluminum-based 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 TiB 2 The 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 technical scheme adopted by the invention is that the adjustable TiB2 in-situ reinforced aluminum-based composite material preparation method comprises the steps of mixing and melting an aluminum-boron alloy and an aluminum-titanium alloy or pure titanium to prepare TiB 2 Compounding the preform melt, and adding TiB 2 And 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 TiB 2 Compounding 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 used 2 Pouring 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 m 1 Of an aluminum-boron alloy of weight m 2 Of an aluminum-titanium alloy or pure titanium particles having a particle diameter of 3mm to 5mm, tiB 2 Designing 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 the preheated pure titanium particles into the aluminum-boron alloy melt in the crucible I for TiB 2 Carrying out in-situ autogenous reaction for 30-90min at 800-850 ℃;
step 1.5, refining the melt by argon gas and degassing for 10-20min to obtain TiB 2 The content is m'/(m) 1 +m 2 ) X 100% of TiB 2 And compounding the preform melt.
The specific steps of step 2 are as follows:
step 2.1, preparing matrix alloy with high content of A element, B element (8230) \8230and N element (m weight) 3 Wherein the content of the element A is m a /m 3 X 100%, the content of B element is m b /m 3 X 100%, the content of N element is m n /m 3 ×100％；
2.2, according to a smelting process, sequentially adding the alloy of the element A and the element B \8230, the alloy of the element B8230and the element 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 I 2 Pouring 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 10-20min.
TiB in the adjustable TiB2 in-situ reinforced aluminum-based composite material prepared in the step 4 2 The content is m'/(m) 1 +m 2 +m 3 ) X 100%, the content of A element is m a /(m 1 +m 2 +m 3 ) X 100%, and the content of B element is m b /(m 1 +m 2 +m 3 ) X 100%, the content of N element is m n /(m 1 +m 2 +m 3 )×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, tiB 2 The pre-generation process is completed in a pure aluminum medium environment, the problem of burning loss of alloy elements does not exist, and TiB 2 After 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 TiB 2 After 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 reserved 2 The original generation state of the phase, and the aluminum-based composite is efficiently completedThe material preparation avoids the sedimentation, aggregation and growth of different components and elements of the aluminum matrix composite material due to density difference;
(3) Can design TiB independently 2 TiB in composite preform 2 The phase content, a system capable of independently selecting a high-element-content matrix, such as Al-Si aluminum alloy, al-Cu aluminum alloy and the like, and independently designed TiB 2 Preparing different TiB by proportioning the composite prefabricated body and the high-element-content matrix 2 The aluminum-based composite material with high content has high automatic regulation and control performance, and TiB in the invention 2 The adding process of the alloy elements of the composite preform and the aluminum-based composite material is respectively and independently completed, and TiB 2 The 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 invention 2 A golden phase diagram of the composite preform;
FIG. 2 is a metallographic graph of the controllable TiB2 in-situ reinforced Al-based composite material 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 an adjustable TiB2 in-situ reinforced aluminum matrix composite material comprises the following steps:
step 1, preparation of TiB 2 The composite preform melt comprises the following specific steps:
step 1.1, according to Ti: b atomic ratio is 1:2, weighing the weight m 1 1kg of an aluminum-boron alloy (AlB 8) with a weight m 2 3.55kg of an aluminum titanium alloy (AlTi 5), i.e., tiB 2 The design yield m' is 0.26kg;
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, aluminum-titanium alloyAdding the gold melt into the aluminum boron alloy melt in the crucible I to carry out TiB 2 Carrying 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 TiB 2 TiB content of 5.66% 2 And compounding the preform melt. Preparing another part of TiB by adopting the step 1 2 TiB content of 5.66% 2 Casting the composite preform melt to obtain TiB 2 And (3) observing the micro-topography of the composite preform, as shown in FIG. 1.
TiB 2 In the process of preparing the composite preform, ti atoms and B atoms TiB released by the raw materials are molten at high temperature 2 The 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 14wt.% of Si element, 0.7wt.% of Mg element, 0.3wt.% of Ti element and the balance of Al, wherein the weight m is 3 4.55kg;
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 TiB 2 Mixing the composite preform melt with the high-element-content aluminum alloy matrix meltAnd (3) homogenizing, which comprises the following specific steps:
step 3.1, mixing TiB in the crucible I 2 Pouring 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 material 2 The content was 2.83%, the content of Si element was 7wt.%, the content of Mg element was 3.5wt.%, and the content of Ti element was 0.15wt.%.
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 TiB 2 The composite preform melt comprises the following specific steps:
step 1.1, according to Ti: b atomic ratio is 1:2, weighing the weight m 1 1kg of an aluminium boron alloy (AlB 8), weight m 2 1.64kg of an aluminum titanium alloy (AlTi 10), i.e. TiB 2 The design yield m' is 0.26kg;
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;
1.3, smelting an aluminum-titanium alloy in a crucible II, and controlling the temperature of a melt to be 820 ℃;
step 1.4, adding the aluminum-titanium alloy melt into the aluminum-boron alloy melt in the crucible I to perform TiB 2 Carrying out in-situ self-generated reaction for 50min at 820 ℃;
step 1.5, refining and degassing the melt for 15min by argon to obtain TiB 2 TiB content of 9.8% 2 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 14wt.% of Si element, 0.7wt.% of Mg element, 0.3wt.% of Ti element and the balance of Al, wherein the weight m is 3 2.64kg;
2.2, according to a smelting process, sequentially adding pure aluminum, an Al-Si intermediate alloy, an Al-Ti intermediate alloy and pure magnesium into a crucible III, 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 TiB 2 The 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 I 2 Pouring 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 material 2 The content was 4.9%, the content of Si element was 7wt.%, the content of Mg element was 3.5wt.%, and the content of Ti element was 0.15wt.%.
Example 3
Step 1, preparing TiB 2 The composite preform melt comprises the following specific steps:
step 1.1, according to Ti: b atomic ratio is 1:2, weighing the weight m 1 10kg of an aluminum boron alloy (AlB 3) with a weight m 2 0.67kg of pure titanium particles, i.e. TiB 2 The design yield m' is 0.97kg;
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 h;
step 1.4, adding the preheated pure titanium particles into an aluminum boron alloy melt in a crucible I to perform TiB 2 Carrying out in-situ spontaneous reaction for 90min at the temperature of 850 ℃;
step 1.5, refining the melt by argon gas and degassing for 20min to obtain TiB 2 TiB content of 9.0% 2 And 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 14wt.% of Si element, 0.7wt.% of Mg element, 0.3wt.% of Ti element and the balance of Al, wherein the weight m is 3 10.67kg;
2.2, according to a smelting process, sequentially adding pure aluminum, an Al-Si intermediate alloy, an 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 TiB 2 The 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 I 2 Pouring 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 material 2 The content was 4.5%, the content of Si element was 7wt.%, the content of Mg element was 3.5wt.%, and the content of Ti element was 0.15wt.%.
Claims (6)
1. Adjustable TiB 2 The preparation method of the in-situ reinforced aluminum-based composite material is characterized by comprising the following steps:
step 1, mixing and melting aluminum-boron alloy and aluminum-titanium alloy or pure titanium to prepare TiB 2 Compounding 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 processed 2 Pouring 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;
step 4, degassing and refining the uniformly mixed melt, slagging off and pouring to obtain the adjustable TiB 2 And (3) in-situ reinforcing the aluminum matrix composite.
2. The tunable TiB of claim 1 2 The preparation method of the in-situ reinforced aluminum-based composite material is characterized in that the specific steps of the step 1 are as follows:
step 1.1, according to Ti: b atomic ratio is 1:2, weighing m 1 Of an aluminum-boron alloy of weight m 2 Of an aluminum-titanium alloy or pure titanium particles having a particle diameter of 3mm to 5mm, tiB 2 Designing 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 TiB 2 The 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 TiB 2 The content is m'/(m) 1 +m 2 ) X 100% of TiB 2 Composite prefabricated partA bulk melt.
3. The tunable TiB of claim 2 2 The preparation method of the in-situ reinforced aluminum-based composite material is characterized in that the step 2 comprises the following specific steps:
step 2.1, preparing matrix alloy with high content of A element, B element (8230) \8230and N element (m weight) 3 Wherein the content of the element A is ma/m 3 X is 100 percent, and the content of the B element is mb/m 3 X 100%, the content of N element is mn/m 3 ×100％；
Step 2.2, according to the smelting process, sequentially adding the alloy of the element A and the element B for 8230, 8230and the alloy of the element 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.
4. The tunable TiB of claim 3 2 The preparation method of the in-situ reinforced aluminum-based composite material is characterized in that the step 3 comprises the following specific steps:
step 3.1, mixing TiB in the crucible I 2 Pouring 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 ℃.
5. The regulatable TiB of claim 4 2 The preparation method of the in-situ reinforced aluminum-based composite material is characterized in that in the step 4, argon is adopted to degas and refine the uniformly mixed melt for 10-20min.
6. The tunable TiB of claim 5 2 The preparation method of the in-situ reinforced aluminum-based composite material is characterized in that the adjustable TiB prepared in the step 4 2 TiB in-situ reinforced aluminum-based composite material 2 The content is m'/(m) 1 +m 2 +m 3 ) X 100%, the content of A element is ma/(m) 1 +m 2 +m 3 ) X is 100 percent, and the content of the B element is mb/(m) 1 +m 2 +m 3 ) X 100 percent, and the content of N element is mn/(m) 1 +m 2 +m 3 )×100％。
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| CN110129641B (en) * | 2019-05-13 | 2021-05-25 | 贵州航天风华精密设备有限公司 | High-performance in-situ TiB2Particle reinforced aluminum-based composite material and preparation method thereof |
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