阅读说明：本技术 一种TiB2颗粒协同改性碳纤维增强铝基复合材料的制备方法 (TiB2Preparation method of particle-synergistically-modified carbon fiber reinforced aluminum-based composite material ) 是由 高义民 路向前 周璇 于 2021-07-23 设计创作，主要内容包括：本发明公开了一种TiB2颗粒协同改性碳纤维增强铝基复合材料的制备方法,将TiB-(2)颗粒粉末与2024Al进行球磨混粉得到TiB-(2)/Al混合粉末,对T-300SC碳纤维使用化学方法镀镍,然后将TiB-(2)/Al混合粉末与镀镍后的碳纤维通过机械搅拌法进行混粉,最后将所得的烧结预制体粉末通过放电等离子烧结技术来制备得到TiB-(2)颗粒协同改性碳纤维增强铝基复合材料。本发明中引入的TiB-(2)增强相均匀分布在基体中,通过弥散强化提高了材料的强度。碳纤维增强相在拔出和剥离可以有效提高材料的拉伸强度,而且碳纤维表面的镍涂层有效阻止了碳纤维与铝基体的接触与反应,阻止了脆性相Al-(4)C-(3)的形成,显著提高了复合材料的综合力学性能。(The invention discloses a preparation method of a carbon fiber reinforced aluminum matrix composite material synergistically modified by TiB2 particles, which is implemented by mixing TiB and a carrier 2 Ball-milling the particle powder and 2024Al to obtain TiB 2 The mixed powder of/Al is prepared by chemically plating nickel on T-300SC carbon fiber and then plating TiB 2 Mixing Al mixed powder and nickel-plated carbon fiber by a mechanical stirring method, and finally preparing TiB by the obtained sintering preform powder by a spark plasma sintering technology 2 The particles synergistically modify the carbon fiber reinforced aluminum matrix composite. TiB introduced in the invention 2 The reinforcing phase is uniformly distributed in the matrix, and the strength of the material is improved through dispersion strengthening. Carbon (C)The tensile strength of the material can be effectively improved by pulling out and peeling off the fiber reinforced phase, and the nickel coating on the surface of the carbon fiber effectively prevents the carbon fiber from contacting and reacting with the aluminum matrix and prevents brittle phase Al 4 C 3 The comprehensive mechanical property of the composite material is obviously improved.)

1. A preparation method of a TiB2 particle synergistically modified carbon fiber reinforced aluminum matrix composite is characterized by comprising the following steps:

s1, using a ball milling method to mill TiB with the particle purity of 99.9 percent and the average particle size of 5-20 mu m₂Carrying out ball milling on the particles and 2024Al powder with the purity of 99.9% and the average particle size of 30-50 mu m to mix the powder;

s2, carrying out degumming pretreatment on the carbon fibers, soaking the carbon fibers in acetone for 12-36 h, and stirring;

s3, performing roughening pretreatment on the carbon fiber subjected to the photoresist removing pretreatment in the step S2, soaking the carbon fiber in roughening solution for 2-5 hours, and stirring;

s4, carrying out sensitization pretreatment on the carbon fiber subjected to the roughening pretreatment in the step S3, soaking the carbon fiber in a sensitization solution for 10-30 min and stirring;

s5, carrying out activation pretreatment on the carbon fiber subjected to sensitization pretreatment in the step S4, soaking the carbon fiber in an activation solution for activation treatment for 10-30 min, and stirring;

s6, carrying out reduction pretreatment on the carbon fiber subjected to activation pretreatment in the step S5, soaking the carbon fiber in a reduction solution for reduction treatment for 10-30 min, and stirring;

s7, carrying out chemical nickel plating on the carbon fiber subjected to reduction pretreatment in the step S6;

s8, cleaning, filtering and drying the carbon fiber after the chemical nickel plating in the step S7;

s9, drying the nickel-plated carbon fiber obtained in the step S8, and ball-milling the dried nickel-plated carbon fiber with TiB obtained in the step S1₂Performing powder mixing treatment on the 2024Al mixed powder, performing suction filtration, and drying the mixed powder to obtain sintered preform powder;

s10 preparation of TiB by spark plasma sintering method using the sintered preform powder prepared in step S9₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite.

2. The method of claim 1, wherein in step S1, the ball milling time is 4-8 h, the ball milling time is suspended for 10-20 min after 20-50 min, and the protective atmosphere in the ball milling tank is argon.

3. The method according to claim 1, wherein in step S3, the specific component of the roughening solution is 100-300 g/L (NH)₄)₂S₂O₈And 50-150 ml/L of H₂SO₄。

4. The method according to claim 1, wherein in step S4, the sensitizing solution comprises 20-40 g/L SnCl₂·2H₂O and 30-70 ml/L HCl.

5. The method according to claim 1, wherein in step S5, the activating solution comprises PdCl in an amount of 0.2-0.4 g/L₂And 10-20 ml/L of HCl.

6. The method according to claim 1, wherein in step S6, the reducing solution is NaH 10-30 g/L₂PO₂·H₂O。

7. The method of claim 1, wherein in step S7, the electroless nickel plating solution has a NiSO content of 10-30 g/L₄·6H₂O, 10-20 g/L NaH₂PO₂·H₂O, 5-10 g/L of Na₃C₃H₅O₇·2H₂O, 10-20 g/L NH4Cl and 10-16 g/L NaOH, and the solutes of the plating solution are sequentially added into the deionized water according to the sequence and the corresponding concentration, wherein the temperature of the nickel plating reaction is 55-75 ℃, and the reaction time is 5-15 min.

8. The method according to claim 1, wherein in step S9, the mixed powder is prepared by using absolute ethyl alcohol as a solvent, first adding 0.1-4 wt% of nickel-plated carbon fiber, stirring for 1-3 min, and then adding TiB₂(1 wt% -10 wt%)/2024 Al mixed powder and stirring together for 5-10 min.

9. The method according to claim 1, wherein in step S9, the drying temperature is 70-90 ℃ and the drying time is 1-3 h.

10. The method according to claim 1, wherein in step S10, the spark plasma sintering method is specifically:

sintering at 25-35 MPa and 20-50 ℃/min, heating from 0 ℃ to 400 ℃ for 2-5 min, heating to 450-500 ℃ at the same heating rate, and keeping the temperature for 8-15 m at the heat preservation temperaturein to obtain compact TiB₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite.

Technical Field

The invention belongs to the technical field of preparation of aluminum-based composite materials, and particularly relates to TiB₂Particle synergyA preparation method of a modified carbon fiber reinforced aluminum matrix composite.

Background

In recent years, with the increasing demand for lightweight materials in the fields of modern aerospace, war industry, transportation and the like, the research and development of lightweight and high-strength materials become a current hot spot. Pure aluminum has low density and good processing performance, but has low strength and poor wear resistance, and is difficult to meet the requirements of practical application, the improvement of the mechanical property of the pure aluminum is limited by traditional alloy strengthening, 2024Al is high-strength duralumin in aluminum-copper-magnesium alloy, has higher strength, certain heat resistance and better comprehensive performance, can be mainly used for manufacturing various high-load components such as the wing front edge of a framework part on an airplane, a fuselage, a skin, a rivet, an automobile hub and the like, and is widely applied to the aerospace field, the automobile military field and the like. Compared with aluminum alloy, the aluminum-based composite material has the advantages of light weight, high specific strength, high specific stiffness, high wear resistance, low thermal expansion coefficient, stable size and the like, has more excellent performance, and has strong practicability and designability.

The currently commonly used particle reinforced aluminum matrix composite has excellent performances such as high specific strength, high specific modulus, good wear resistance, fatigue resistance and the like, but the elongation after fracture of the nano silicon carbide reinforced 7075Al is slowly reduced when the content is 0.25 wt% -0.50 wt%, and is rapidly reduced when the content exceeds 0.50 wt%.

The pure fiber reinforced aluminum matrix composite material can reduce the plasticity of the material while enhancing the strength of the material.

Disclosure of Invention

The technical problem to be solved by the present invention is to provide a TiB for overcoming the above-mentioned deficiencies in the prior art₂The strength and the toughness of the prepared aluminum-based composite material are improved, the service life is prolonged, the TiB2 particles and the carbon fibers are used as reinforcing phases, the plasticity of the material is maintained or improved while the strength of the material is improved, and the application range of the aluminum-based composite material is further expanded.

The invention adopts the following technical scheme:

a preparation method of a TiB2 particle synergistically modified carbon fiber reinforced aluminum matrix composite material comprises the following steps:

s1, using a ball milling method to mill TiB with the particle purity of 99.9 percent and the average particle size of 5-20 mu m₂Carrying out ball milling on the particles and 2024Al powder with the purity of 99.9% and the average particle size of 30-50 mu m to mix the powder;

s2, carrying out degumming pretreatment on the carbon fibers, soaking the carbon fibers in acetone for 12-36 h, and stirring;

s3, performing roughening pretreatment on the carbon fiber subjected to the photoresist removing pretreatment in the step S2, soaking the carbon fiber in roughening solution for 2-5 hours, and stirring;

s4, carrying out sensitization pretreatment on the carbon fiber subjected to the roughening pretreatment in the step S3, soaking the carbon fiber in a sensitization solution for 10-30 min and stirring;

s5, carrying out activation pretreatment on the carbon fiber subjected to sensitization pretreatment in the step S4, soaking the carbon fiber in an activation solution for activation treatment for 10-30 min, and stirring;

s6, carrying out reduction pretreatment on the carbon fiber subjected to activation pretreatment in the step S5, soaking the carbon fiber in a reduction solution for reduction treatment for 10-30 min, and stirring;

s7, carrying out chemical nickel plating on the carbon fiber subjected to reduction pretreatment in the step S6;

s8, cleaning, filtering and drying the carbon fiber after the chemical nickel plating in the step S7;

s9, drying the nickel-plated carbon fiber obtained in the step S8, and ball-milling the dried nickel-plated carbon fiber with TiB obtained in the step S1₂Performing powder mixing treatment on the 2024Al mixed powder, performing suction filtration, and drying the mixed powder to obtain sintered preform powder;

s10 preparation of TiB by spark plasma sintering method using the sintered preform powder prepared in step S9₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite.

Specifically, in the step S1, the ball milling time is 4-8 hours, the ball milling needs to be suspended for 10-20 min after 20-50 min, and the protective atmosphere in the ball milling tank is argon.

Specifically, in step S3, the roughening solution has a specific composition of (NH) 100 to 300g/L₄)₂S₂O₈And 50-150 ml/L of H₂SO₄。

Specifically, in step S4, the sensitizing solution comprises 20-40 g/L SnCl₂·2H₂O and 30-70 ml/L HCl.

Specifically, in step S5, the activating solution contains PdCl of 0.2-0.4 g/L₂And 10-20 ml/L of HCl.

Specifically, in step S6, the reducing solution is NaH of 10-30 g/L₂PO₂·H₂O。

Specifically, in step S7, the electroless nickel plating solution contains NiSO with a plating solution component of 10-30 g/L₄·6H₂O, 10-20 g/L NaH₂PO₂·H₂O, 5-10 g/L of Na₃C₃H₅O₇·2H₂O, 10-20 g/L NH4Cl and 10-16 g/L NaOH, and the solutes of the plating solution are sequentially added into the deionized water according to the sequence and the corresponding concentration, wherein the temperature of the nickel plating reaction is 55-75 ℃, and the reaction time is 5-15 min.

Specifically, in step S9, the anhydrous ethanol is used as the solvent for the powder mixture, 0.1 wt% -4 wt% of nickel-plated carbon fiber is added and stirred for 1-3 min, and then TiB is added₂(1 wt% -10 wt%)/2024 Al mixed powder and stirring together for 5-10 min.

Specifically, in the step S9, the drying temperature is 70-90 ℃, and the drying time is 1-3 h.

Specifically, in step S10, the spark plasma sintering method specifically includes:

sintering pressure is 25-35 MPa, heating rate is 20-50 ℃/min, heat preservation is carried out for 2-5 min after the temperature is increased from 0 ℃ to 400 ℃, then the temperature is increased to 450-500 ℃ at the same heating rate, and heat preservation is carried out for 8-15 min at the heat preservation temperature, so that compact TiB is obtained₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite.

Compared with the prior art, the invention has at least the following beneficial effects:

the invention relates to a preparation method of a TiB2 particle synergistically modified carbon fiber reinforced aluminum matrix composite, which adopts a ball milling method to carry out TiB₂Granules and 2024Al can ensure the uniform mixing of the powder, and the TiB with micron scale₂On the basis of the obtained TiB, more nano-scale TiB is obtained₂The reinforcing phase enables the mechanical property of the composite material to be more excellent; the sintered preform powder is prepared by adopting a mechanical powder mixing method, so that the problem of easy agglomeration of fibers can be effectively solved, and the mechanical property of the composite material is effectively enhanced. The defect of poor wettability of the carbon fiber and the 2024Al matrix when a casting method is adopted can be overcome by adopting a spark plasma sintering method; the brittle phase Al can be avoided by carrying out chemical nickel plating on the carbon fiber₄C₃The plasticity and toughness of the composite material are effectively enhanced. .

Furthermore, the ball milling time is 4-8 h, so that 2024Al powder and TiB can be ensured₂The powder is mixed fully and uniformly, and TiB with more scale is obtained₂And (3) powder. The ball mill is suspended for 10-20 min after 20-50 min, so that the ball mill cannot continuously work for a long time, and the service life of the ball mill of a preparation instrument is ensured. The protective atmosphere in the ball milling tank is argon, and the argon is used as inert gas to fully protect 2024Al powder from being oxidized in the ball milling process.

Further, the specific component of the roughening liquid is 100-300 g/L (NH)₄)₂S₂O₈And 50-150 ml/L of H₂SO₄The roughness of the surface of the carbon fiber can be effectively enhanced, and the chemical nickel plating reaction is more facilitated.

Further, the specific component of the sensitizing solution is 20-40 g/L SnCl₂·2H₂O and 30-70 ml/L HCl can enable the surface of the fiber to be successfully adsorbed to a layer of gel-like substance for adsorbing palladium ions in the activation process.

Further, the specific component of the activating solution is PdCl of 0.2-0.4 g/L₂And 10-20 ml/L of HCl, so that palladium ions can be successfully adsorbed on the surface of the carbon fiber, and the chemical nickel plating reaction is facilitated.

Further, the reducing solution is NaH with the concentration of 10-30 g/L₂PO₂·H₂O, palladium ions remaining during the activation process can be successfully removed.

Further, the chemical nickel plating solution contains NiSO with the component of 10-30 g/L₄·6H₂O, 10-20 g/L NaH₂PO₂·H₂O, 5-10 g/L of Na₃C₃H₅O₇·2H₂And O, 10-20 g/L of NH4Cl and 10-16 g/L of NaOH, and the solutes of the plating solution are sequentially added into deionized water according to the sequence and the corresponding concentration, the temperature of the nickel plating reaction is 55-75 ℃, the reaction time is 5-15 min, and the carbon fiber with proper thickness and uniformly distributed Ni transition layers can be obtained.

Furthermore, the mixed powder uses absolute ethyl alcohol as a solvent, and is convenient to rapidly dry after being mixed to obtain sintering preform powder; firstly, 0.1-4 wt% of nickel-plated carbon fiber is added and stirred for 1-3 min, so that the carbon fiber which is easy to agglomerate can be fully dispersed in absolute ethyl alcohol; then adding TiB₂(1 wt% -10 wt%)/2024 Al mixed powder is stirred together for 5-10 min, and fully and uniformly mixed sintered preform powder can be obtained.

Further, the drying temperature is 70-90 ℃, the drying time is 1-3 h, ethanol can be quickly evaporated, and the prepared sintering preform powder is quickly dried.

Further, the sintering pressure of the spark plasma sintering is set to be 20-40 MPa, the heating rate is 20-150 ℃/min, the sintering heat preservation temperature is 450-500 ℃, and the heat preservation time is 10-20 min, so that TiB with compact and uniform tissue and excellent performance can be obtained₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite.

In conclusion, the invention can improve the strength of the material, effectively improve the plasticity of the common particle reinforced aluminum matrix composite material, improve the mechanical properties such as tensile strength, hardness and the like, expand the application range and prolong the service life of the material.

The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.

Drawings

FIG. 1 is a view of TiB of the present invention₂A microscopic microstructure macroscopic morphology of the particle synergistic modified carbon fiber reinforced aluminum matrix composite material by a scanning electron microscope;

FIG. 2 is a TiB of the present invention₂And (3) scanning electron microscope microstructure high-power morphology map of the particle synergistic modified carbon fiber reinforced aluminum matrix composite.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

In the description of the present invention, it should be understood that the terms "comprises" and/or "comprising" indicate the presence of the stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.

It is also to be understood that the terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in the specification of the present invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.

It should be further understood that the term "and/or" as used in this specification and the appended claims refers to and includes any and all possible combinations of one or more of the associated listed items.

Various structural schematics according to the disclosed embodiments of the invention are shown in the drawings. The figures are not drawn to scale, wherein certain details are exaggerated and possibly omitted for clarity of presentation. The shapes of various regions, layers and their relative sizes and positional relationships shown in the drawings are merely exemplary, and deviations may occur in practice due to manufacturing tolerances or technical limitations, and a person skilled in the art may additionally design regions/layers having different shapes, sizes, relative positions, according to actual needs.

The invention provides a TiB₂A process for preparing the particle-synergistic modified carbon-fibre reinforced Al-base composite material includes such steps as proportionally mixing TiB with Al₂Ball-milling the particle powder and 2024Al to obtain TiB₂Mixing the mixed powder with carbon fiber modified by chemical nickel plating by mechanical stirring method, and mixing the obtained well-mixed C_f/TiB₂Preparation of TiB from/2024 Al powder by spark plasma sintering₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite.

The invention relates to a TiB₂The preparation method of the particle synergistic modified carbon fiber reinforced aluminum matrix composite material comprises the following steps:

s1, using a ball milling method to mill TiB with the particle purity of 99.9 percent and the average particle size of 5-20 mu m₂Carrying out ball milling on the particles and 2024Al powder with the purity of 99.9% and the average particle size of 30-50 mu m to mix the powder;

the ball milling time is 4-8 h, the ball milling needs to be suspended for 0-20 min after 20-50 min, and the protective atmosphere in the ball milling tank is argon.

S2, carrying out degumming pretreatment on the carbon fibers, and soaking the carbon fibers in acetone for 12-36 h;

the model of the carbon fiber is T-300SC, and a magnetic stirrer is used for stirring the carbon fiber at a constant speed in the soaking process.

S3, carrying out roughening pretreatment on the carbon fiber, and soaking the carbon fiber in roughening solution for 2-5 h;

the roughening liquid comprises the following specific components: (NH)₄)₂S₂O₈100 to 300g/L, H₂SO₄50-150 ml/L, and a magnetic stirrer is used for stirring the mixture at a constant speed in the treatment process.

S4, performing sensitization pretreatment on the carbon fibers, and soaking the carbon fibers in a sensitization solution for 10-30 min;

the sensitizing solution comprises the following specific components: SnCl₂·2H₂O: 20-40 g/L, HCl: 30-70 ml/L, and a magnetic stirrer is used for homogenizing the mixture in the treatment processStirring at a high speed.

S5, performing activation pretreatment on the carbon fibers, and soaking the carbon fibers in an activation solution for activation treatment for 10-30 min;

the specific component of the activating solution is PdCl₂: 0.2-0.4 g/L, HCl: 10-20 ml/L, and stirring the mixture at a constant speed by using a magnetic stirrer in the treatment process.

S6, carrying out reduction pretreatment on the carbon fibers, and soaking the carbon fibers in a reduction solution for reduction treatment for 10-30 min;

the composition of the reducing solution is NaH₂PO₂·H₂O: 10-30 g/L, and uniformly stirring the mixture by using a magnetic stirrer in the treatment process.

S7, carrying out chemical nickel plating on the carbon fiber subjected to the pretreatment process, adding the carbon fiber into plating solution for chemical reaction, wherein the temperature of the nickel plating reaction is 55-75 ℃, the reaction time is 5-15 min, and a magnetic stirrer is used for stirring the carbon fiber at a constant speed and heating the carbon fiber at a constant temperature in the reaction process;

the plating solution for chemical nickel plating comprises the following components: NiSO₄·6H₂O is 10-30 g/L, NaH₂PO₂·H₂O is 10-20 g/L, Na₃C₃H₅O₇·2H₂O is 5-10 g/L, NH4Cl is 10-20 g/L, NaOH is 10-16 g/L, and the solutes of the plating solution need to be added into the deionized water in sequence according to the sequence and the corresponding concentration.

S8, cleaning, filtering and drying the nickel-plated carbon fiber, wherein the drying temperature is 80-120 ℃, and the drying time is set to be 2-4 h;

s9, drying the nickel-plated carbon fiber obtained in the step S8, and ball-milling the dried nickel-plated carbon fiber with TiB obtained in the step S1₂The/2024 Al mixed powder is mixed by using a mechanical stirring method, suction filtration is carried out after stirring is finished, the mixed powder is put into a drying oven to be dried, the drying temperature is 70-90 ℃, and the drying time is 1-3 hours, so that dry sintering preform powder is obtained;

using absolute ethyl alcohol as a solvent, firstly adding 0.1-4 wt% of nickel-plated carbon fiber into the mixed powder, stirring for 1-3 min, and then adding TiB₂(1 wt% -10 wt%)/2024 Al mixed powder adding additiveAnd stirring the mixture by using water and ethanol for 5-10 min.

S10 preparation of TiB by spark plasma sintering method using the sintered preform powder prepared in step S9₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite.

The specific parameters of sintering are as follows: sintering at 25-35 MPa and at a heating rate of 20-50 ℃/min, heating from 0 ℃ to 400 ℃, then preserving heat for 2-5 min, heating to 450-500 ℃ at the same heating rate, and preserving heat for 8-15 min to obtain compact TiB₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite.

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

1) First, 0.3g of TiB is taken₂Mixing the granules with 30g of 2024Al powder, mixing TiB with an average particle size of 5 μm₂The particles were ball-milled with 2024Al powder having an average particle size of 30 μm. The ball milling time is 4h, the ball milling is suspended for 10min after 30min, and the protective atmosphere in the ball milling tank is argon.

2) 1g of short carbon fiber and 500ml of acetone are taken to carry out degumming pretreatment on the carbon fiber, and the carbon fiber is soaked in the acetone. The model of the carbon fiber is T-300SC, the soaking time is 12h, the carbon fiber is stirred at a constant speed by using a magnetic stirrer in the treatment process, and the carbon fiber is cleaned and filtered after the cementation is removed.

3) Roughening pretreatment is carried out on the carbon fiber, and the carbon fiber is soaked in 500ml of roughening solutionIn (1). The roughening liquid comprises the following specific components: (NH)₄)₂S₂O₈Is 100g/L, H₂SO₄50ml/L, soaking time is 2h, a magnetic stirrer is used for stirring the carbon fiber at a constant speed in the treatment process, and the carbon fiber is cleaned and filtered after the coarsening is finished.

4) And (3) carrying out sensitization pretreatment on the carbon fiber, and soaking the carbon fiber in 500ml of sensitization liquid. The sensitizing solution comprises the following specific components: SnCl₂·2H₂O: 20g/L, HCl: 30ml/L, the soaking time is 10min, a magnetic stirrer is used for stirring at a constant speed in the soaking process, and after the coarsening is finished, the carbon fiber is cleaned and filtered.

5) The carbon fiber is subjected to activation pretreatment, and is soaked in an activation solution. The specific component of the activating solution is PdCl₂: 0.2g/L, HCl: 10ml/L, 10min of activation treatment time, uniformly stirring the carbon fiber by using a magnetic stirrer in the treatment process, and cleaning and filtering the carbon fiber after the activation.

6) And (3) carrying out reduction pretreatment on the carbon fibers, and soaking the carbon fibers in a reducing solution. The composition of the reducing solution is NaH₂PO₂·H₂O: 10g/L, the reduction treatment time is 10min, a magnetic stirrer is used for stirring at a constant speed in the treatment process, and the carbon fibers are cleaned and filtered after the reduction is finished.

7) And carrying out chemical nickel plating on the pretreated carbon fiber, and adding the carbon fiber into plating solution for chemical reaction. The plating solution component of the chemical nickel plating is NiSO₄·6H₂O：10g/L，NaH₂PO₂·H₂O：10g/L，Na₃C₃H₅O₇·2H₂5g/L of O, 10g/L of NH4Cl and 10g/L of NaOH, and the solutes of the plating solution are sequentially added into the deionized water according to the sequence and the corresponding concentration. And adding carbon fiber into the plating solution when the temperature of the plating solution reaches 75 ℃, uniformly stirring and heating at constant temperature by using a magnetic stirrer in the whole reaction process, and taking out the carbon fiber after the reaction lasts for 10 min.

8) And (4) cleaning, filtering and drying the nickel-plated carbon fiber. Placing the carbon fiber in a culture dish, putting the culture dish in a drying oven, and drying at the temperature of 80 ℃ for 4 hours.

9) The dried nickel-plated carbon fiber and 1 wt% TiB after ball milling are mixed₂The/2024 Al mixed powder was mixed by a mechanical stirring method. When the powder is mixed, absolute ethyl alcohol is used as a solvent, 0.15g of nickel-plated carbon fiber is firstly added, stirred for 1min, and then TiB is added₂(1 wt%)/2024 Al mixed powder was added to anhydrous ethanol and stirred together for 5 min. And after stirring, carrying out suction filtration, and finally, putting the mixed powder into a drying oven for drying at the drying temperature of 70 ℃ for 3 h.

10) Production of TiB by spark plasma sintering using dry sintered preform powder₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite. The specific parameters of sintering are as follows: sintering at 25MPa and 20 deg.C/min, heating to 400 deg.C, maintaining for 2min, heating to 450 deg.C at the same sintering rate, and maintaining for 5min to obtain 0.5 wt% C_f/1wt％TiB₂/2024Al (0.5 wt% carbon fiber and 1 wt% TiB)₂A composite of 2024Al with synergistic reinforcement).

Example 2

1) Firstly, 0.6g of TiB is taken₂Mixing the granules with 30g of 2024Al powder, mixing TiB with an average particle size of 8 μm₂The particles were ball-milled with 2024Al powder having an average particle size of 35 μm. The ball milling time is 6h, the ball milling is suspended for 10min after 30min, and the protective atmosphere in the ball milling tank is argon.

2) 1.5g of short carbon fiber and 500ml of acetone are taken, the short carbon fiber is subjected to degumming pretreatment, and the carbon fiber is soaked in the acetone. The model of the carbon fiber is T-300SC, the soaking time is 24h, the carbon fiber is stirred at a constant speed by using a magnetic stirrer in the soaking process, and the carbon fiber is cleaned and filtered after the cementation is removed.

3) The carbon fiber is subjected to coarsening pretreatment, and the carbon fiber is soaked in 500ml of coarsening liquid. The roughening liquid comprises the following specific components: (NH)₄)₂S₂O₈Is 200g/L, H₂SO₄100ml/L, soaking for 2h, stirring with a magnetic stirrer at uniform speed during soaking, and cleaning carbon fiber after coarseAnd (5) washing and suction filtering.

4) And (3) carrying out sensitization pretreatment on the carbon fiber, and soaking the carbon fiber in 500ml of sensitization liquid. The sensitizing solution comprises the following specific components: SnCl₂·2H₂O: 30g/L, HCl: 50ml/L, 20min soaking, stirring at constant speed with a magnetic stirrer during soaking, cleaning carbon fiber after sensitization, and vacuum filtering.

5) The carbon fiber is subjected to activation pretreatment, and is soaked in an activation solution. The specific component of the activating solution is PdCl₂: 0.3g/L, HCl: 12ml/L, the activation treatment time is 20min, a magnetic stirrer is used for stirring at a constant speed in the treatment process, and the carbon fibers are cleaned and filtered after the activation.

6) And (3) carrying out reduction pretreatment on the carbon fibers, and soaking the carbon fibers in a reducing solution. The composition of the reducing solution is NaH₂PO₂·H₂O: 20g/L, the reduction treatment time is 20min, a magnetic stirrer is used for stirring at a constant speed in the soaking process, and the carbon fibers are cleaned and filtered after the reduction is finished.

7) And carrying out chemical nickel plating on the pretreated carbon fiber, and adding the carbon fiber into plating solution for chemical reaction. The plating solution component of the chemical nickel plating is NiSO₄·6H₂O：20g/L，NaH₂PO₂·H₂O：15g/L，Na₃C₃H₅O₇·2H₂8g/L of O, 15g/L of NH4Cl and 12g/L of NaOH, and the solutes of the plating solution are sequentially added into the deionized water according to the sequence and the corresponding concentration. And after the temperature of the plating solution is heated to 65 ℃, adding the carbon fiber into the plating solution, uniformly stirring and heating at constant temperature by using a magnetic stirrer in the whole reaction process, and taking out the carbon fiber after the reaction lasts for 10 min.

8) And (4) cleaning, filtering and drying the nickel-plated carbon fiber. Placing the carbon fiber in a culture dish, putting the culture dish in a drying oven for drying, wherein the temperature is set to be 100 ℃, and the drying time is set to be 3 hours.

9) And mixing the dried nickel-plated carbon fibers and the mixed powder after ball milling by using a mechanical stirring method. When mixing the powders, 0.3g of absolute ethanol was added as a solventPlating nickel on carbon fiber, stirring for 2min, and mixing TiB₂Adding the mixed powder with 2024Al into anhydrous ethanol, and stirring for 7 min. And after stirring, carrying out suction filtration, and finally, putting the mixed powder into a drying oven for drying at the drying temperature of 80 ℃ for 2 h.

10) Production of TiB by spark plasma sintering using dry sintered preform powder₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite. The specific parameters of sintering are as follows: sintering at 30MPa and 30 deg.C/min, heating to 400 deg.C, maintaining for 3min, heating to 480 deg.C at the same sintering rate, and maintaining for 10min to obtain 1 wt% C_f/2wt％TiB₂/2024Al (1 wt% carbon fiber and 2 wt% TiB)₂A composite of 2024Al with synergistic reinforcement).

Example 3

1) Firstly, 1.5g of TiB is taken₂Mixing the granules with 30g of 2024Al powder, mixing TiB with an average particle size of 10 μm₂The particles were ball-milled with 2024Al powder having an average particle size of 40 μm. The ball milling time is 8h, the ball milling needs to be suspended for 10min for 30min, and the protective atmosphere in the ball milling tank is argon.

2) Taking 2g of short carbon fiber and 500ml of acetone, carrying out degumming pretreatment on the short carbon fiber, and soaking the carbon fiber in the acetone. The model of the carbon fiber is T-300SC, the soaking time is 36h, the carbon fiber is stirred at a constant speed by using a magnetic stirrer in the soaking process, and the carbon fiber is cleaned and filtered after the cementation is removed.

3) And (3) carrying out roughening pretreatment on all the carbon fibers after photoresist removal, and soaking the carbon fibers in 500ml of roughening solution. The roughening liquid comprises the following specific components: (NH)₄)₂S₂O₈Is 300g/L, H₂SO₄150ml/L, the soaking time is 2h, the soaking process uses a magnetic stirrer to stir the carbon fiber at a constant speed, and the carbon fiber is cleaned and filtered after the coarsening is finished.

4) And (3) carrying out sensitization pretreatment on the carbon fiber, and soaking the carbon fiber in 500ml of sensitization liquid. The sensitizing solution comprises the following specific components: SnCl₂·2H₂O: 40g/L, HCl: 70ml/L, soaking time is 30min, and soaking processThe method comprises the steps of uniformly stirring the carbon fiber by using a magnetic stirrer, and cleaning and filtering the carbon fiber after the sensitization is finished.

5) The carbon fiber is subjected to activation pretreatment, and is soaked in an activation solution. The specific component of the activating solution is PdCl₂: 0.4g/L, HCl: 15ml/L, the activation treatment time is 30min, a magnetic stirrer is used for stirring the carbon fiber at a constant speed in the treatment process, and the carbon fiber is cleaned and filtered after the activation.

6) And (3) carrying out reduction pretreatment on the carbon fibers, and soaking the carbon fibers in a reducing solution. The composition of the reducing solution is NaH₂PO₂·H₂O: 30g/L, the reduction treatment time is 30min, a magnetic stirrer is used for stirring at a constant speed in the soaking process, and the carbon fibers are cleaned and filtered after the reduction is finished.

7) And carrying out chemical nickel plating on the pretreated carbon fiber, and adding the carbon fiber into plating solution for chemical reaction. The plating solution for chemical nickel plating comprises the following components: NiSO₄·6H₂O is 30g/L, NaH₂PO₂·H₂O is 20g/L, Na₃C₃H₅O₇·2H₂10g/L of O, 18g/L of NH4Cl and 16g/L of NaOH, and the solutes of the plating solution are sequentially added into the deionized water according to the sequence and the corresponding concentration. And adding carbon fiber into the plating solution when the temperature of the plating solution reaches 70 ℃, uniformly stirring and heating at constant temperature by using a magnetic stirrer in the whole reaction process, and taking out the carbon fiber after the reaction lasts for 6 min.

8) And (4) cleaning, filtering and drying the nickel-plated carbon fiber. Placing the carbon fiber in a culture dish, putting the culture dish in a drying oven for drying, wherein the temperature is set to be 120 ℃, and the drying time is set to be 2 hours.

9) The dried nickel-plated carbon fiber and the ball-milled TiB are subjected to ball milling₂The mixed powder with 2024Al was mixed by a mechanical stirring method. Using absolute ethanol as a solvent, 0.6g of nickel-plated carbon fiber was added first, and after stirring for 3min, 31.5g of TiB was added₂/2024 adding anhydrous ethanol into the Al mixed powder, and stirring for 10 min. After stirring, carrying out suction filtration, then putting the mixed powder into a drying oven for drying at the drying temperature of 90 ℃,the drying time was 1 h.

10) Production of TiB by spark plasma sintering using dry sintered preform powder₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite. The specific parameters of sintering are as follows: the sintering pressure is 35MPa, the heating rate is 50 ℃/min, the temperature is raised to 400 ℃, then the temperature is preserved for 3.5min, the temperature is raised to 500 ℃ at the same sintering rate, the temperature preservation time is 5-15 min, and the compact 2 wt% C is obtained_f/5wt％TiB₂/2024Al (2 wt% carbon fiber and 5 wt% TiB)₂A composite of 2024Al with synergistic reinforcement).

Example 4

1) Firstly, 2.4g of TiB is taken₂Mixing the granules with 30g of 2024Al powder, mixing TiB with an average particle size of 15 μm₂The particles were ball-milled with 2024Al powder having an average particle size of 45 μm. The ball milling time is 6h, the ball milling needs to be suspended for 10min for 30min, and the protective atmosphere in the ball milling tank is argon.

2) Taking 2g of short carbon fiber and 500ml of acetone, carrying out degumming pretreatment on the short carbon fiber, and soaking the carbon fiber in the acetone. The model of the carbon fiber is T-300SC, the soaking time is 36h, the carbon fiber is stirred at a constant speed by using a magnetic stirrer in the soaking process, and the carbon fiber is cleaned and filtered after the cementation is removed.

3) And (3) carrying out roughening pretreatment on all the carbon fibers after photoresist removal, and soaking the carbon fibers in 500ml of roughening solution. The roughening liquid comprises the following specific components: (NH)₄)₂S₂O₈Is 200g/L, H₂SO₄The soaking time is 5 hours, the soaking process is carried out by using a magnetic stirrer for uniform stirring, and the carbon fiber is cleaned and filtered after the coarsening is finished.

4) And (3) carrying out sensitization pretreatment on the carbon fiber, and soaking the carbon fiber in 500ml of sensitization liquid. The sensitizing solution comprises the following specific components: SnCl₂·2H₂O: 30g/L, HCl: 60ml/L, the soaking time is 30min, a magnetic stirrer is used for stirring at a constant speed in the soaking process, and after sensitization, the carbon fibers are cleaned and filtered.

5) The carbon fiber is subjected to activation pretreatment, and is soaked in an activation solution. Activating liquid utensilThe body composition is PdCl₂: 0.3g/L, HCl: 15ml/L, the activation treatment time is 20min, a magnetic stirrer is used for stirring the carbon fiber at a constant speed in the treatment process, and the carbon fiber is cleaned and filtered after the activation.

6) And (3) carrying out reduction pretreatment on the carbon fibers, and soaking the carbon fibers in a reducing solution. The composition of the reducing solution is NaH₂PO₂·H₂O: 25g/L, the reduction treatment time is 20min, a magnetic stirrer is used for stirring at a constant speed in the soaking process, and the carbon fibers are cleaned and filtered after the reduction is finished.

7) And carrying out chemical nickel plating on the pretreated carbon fiber, and adding the carbon fiber into plating solution for chemical reaction. The plating solution for chemical nickel plating comprises the following components: NiSO₄·6H₂O is 20g/L, NaH₂PO₂·H₂O is 15g/L, Na₃C₃H₅O₇·2H₂8g/L of O, 15g/L of NH4Cl and 12g/L of NaOH, and the solutes of the plating solution need to be added into the deionized water in sequence according to the sequence and the corresponding concentration. And adding carbon fiber into the plating solution when the temperature of the plating solution reaches 70 ℃, uniformly stirring and heating at constant temperature by using a magnetic stirrer in the whole reaction process, and taking out the carbon fiber after the reaction lasts for 6 min.

8) And (4) cleaning, filtering and drying the nickel-plated carbon fiber. Placing the carbon fiber in a culture dish, putting the culture dish in a drying oven, and drying at 100 ℃ for 2.5 hours.

9) The dried nickel-plated carbon fiber and the ball-milled TiB are subjected to ball milling₂The mixed powder with 2024Al was mixed by a mechanical stirring method. Using absolute ethanol as a solvent, 0.6g of nickel-plated carbon fiber was added first, and after stirring for 2min, 32.4g of TiB was added₂/2024Al mixed powder is added into anhydrous ethanol and stirred together for 8 min. And after stirring, carrying out suction filtration, and then putting the mixed powder into a drying oven for drying at the drying temperature of 80 ℃ for 2 h.

10) Production of TiB by spark plasma sintering using dry sintered preform powder₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite. Sintered toolThe body parameters were as follows: sintering at 35MPa and 30 deg.C/min, heating to 400 deg.C, maintaining for 2min, heating to 480 deg.C at the same sintering rate, and maintaining for 10min to obtain compact 2 wt% C_f/8wt％TiB₂/2024Al (2 wt% carbon fiber and 8 wt% TiB)₂A composite of 2024Al with synergistic reinforcement).

Example 5

1) First, 3gTiB is taken₂Mixing the granules with 30g of 2024Al powder, mixing TiB with an average particle size of 20 μm₂The particles were ball-milled with 2024Al powder having an average particle size of 50 μm. The ball milling time is 8h, the ball milling time is 30min and is suspended for 10min, and the protective atmosphere in the ball milling tank is argon.

2) 1.5g of short carbon fiber and 500ml of acetone are taken, the short carbon fiber is subjected to degumming pretreatment, and the carbon fiber is soaked in the acetone. The model of the carbon fiber is T-300SC, the soaking time is 30h, the carbon fiber is stirred at a constant speed by using a magnetic stirrer in the soaking process, and the carbon fiber is cleaned and filtered after the cementation is removed.

3) The carbon fiber is subjected to coarsening pretreatment, and the carbon fiber is soaked in 500ml of coarsening liquid. The roughening liquid comprises the following specific components: (NH)₄)₂S₂O₈Is 200g/L, H₂SO₄The soaking time is 4 hours, the soaking process is carried out by using a magnetic stirrer for uniform stirring, and the carbon fiber is cleaned and filtered after the coarsening is finished.

4) And (3) carrying out sensitization pretreatment on the carbon fiber, and soaking the carbon fiber in 500ml of sensitization liquid. The sensitizing solution comprises the following specific components: SnCl₂·2H₂O: 30g/L, HCl: 50ml/L, the soaking time is 30min, a magnetic stirrer is used for stirring at a constant speed in the soaking process, and the carbon fiber is cleaned and filtered after the sensitization is finished.

5) The carbon fiber is subjected to activation pretreatment, and is soaked in an activation solution. The specific component of the activating solution is PdCl₂: 0.3g/L, HCl: 12ml/L, the activation treatment time is 25min, a magnetic stirrer is used for stirring at a constant speed in the treatment process, and the carbon fibers are cleaned and filtered after the activation.

6) To carbon fibersAnd (4) carrying out reduction pretreatment, namely soaking the carbon fibers in a reduction solution. The composition of the reducing solution is NaH₂PO₂·H₂O: 20g/L, the reduction treatment time is 25min, a magnetic stirrer is used for stirring at a constant speed in the soaking process, and the carbon fibers are cleaned and filtered after the reduction is finished.

7) And carrying out chemical nickel plating on the pretreated carbon fiber, and adding the carbon fiber into plating solution for chemical reaction. The plating solution component of the chemical nickel plating is NiSO₄·6H₂O：20g/L，NaH₂PO₂·H₂O：15g/L，Na₃C₃H₅O₇·2H₂8g/L of O, 15g/L of NH4Cl and 12g/L of NaOH, and the solutes of the plating solution are sequentially added into the deionized water according to the sequence and the corresponding concentration. And after the temperature of the plating solution is heated to 65 ℃, adding the carbon fiber into the plating solution, uniformly stirring and heating at constant temperature by using a magnetic stirrer in the whole reaction process, and taking out the carbon fiber after the reaction lasts for 8 min.

8) And (4) cleaning, filtering and drying the nickel-plated carbon fiber. Placing the carbon fiber in a culture dish, putting the culture dish in a drying oven for drying, wherein the temperature is set to be 100 ℃, and the drying time is set to be 3 hours.

9) And mixing the dried nickel-plated carbon fibers and the mixed powder after ball milling by using a mechanical stirring method. When the powder is mixed, absolute ethyl alcohol is used as a solvent, 0.6g of nickel-plated carbon fiber is firstly added, stirred for 2min, and then TiB is added₂Adding the mixed powder with 2024Al into anhydrous ethanol, and stirring for 7 min. And after stirring, carrying out suction filtration, and finally, putting the mixed powder into a drying oven for drying at the drying temperature of 80 ℃ for 3 h.

10) Production of TiB by spark plasma sintering using dry sintered preform powder₂The particles synergistically modify the carbon fiber reinforced aluminum matrix composite. The specific parameters of sintering are as follows: sintering at 35MPa and 20 deg.C/min, heating to 400 deg.C, maintaining for 2min, heating to 480 deg.C at the same sintering rate, and maintaining for 8min to obtain 2 wt% C_f/10wt％TiB₂/2024Al (2 wt% carbon fiber and 10 wt% carbon fiber)TiB₂A composite of 2024Al with synergistic reinforcement).

TABLE 1 tensile Strength of the samples obtained in the examples

As shown in table 1, the tensile strength and the elongation of the TiB2 particle synergistically modified carbon fiber reinforced aluminum matrix composite material prepared in examples 1 to 5 are far greater than those of the matrix material 2024Al, which indicates that the mechanical property and the plasticity of the 2024Al are greatly improved, and the application range of the 2024Al is expanded.

In conclusion, the invention provides a TiB₂Preparation method of particle synergistically modified carbon fiber reinforced aluminum matrix composite material and introduced TiB₂The reinforcing phase is uniformly distributed in the matrix, and the strength of the material is improved through dispersion strengthening. The tensile strength of the material can be effectively improved by pulling out and peeling off the carbon fiber reinforced phase, and the nickel coating on the surface of the carbon fiber effectively prevents the carbon fiber from contacting and reacting with the aluminum matrix and prevents the brittle phase Al₄C₃The comprehensive mechanical property of the composite material is obviously improved.

The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.