阅读说明：本技术 一种界面改性纤维增强金属基复合材料及其制备方法 (Interface modified fiber reinforced metal matrix composite material and preparation method thereof ) 是由 陈照峰 廖家豪 于 2019-11-06 设计创作，主要内容包括：本发明公开了一种界面改性纤维增强金属基复合材料,体积密度小于3.0g/cm～3,由增强纤维、界面层和金属基体组成。制备方法包括以下步骤：将增强纤维织成纤维预制体,先后制备化学气相渗透涂层和化学镀涂层,然后将铝合金或铜合金熔体压铸到纤维预制体中,冷却得到界面改性纤维增强金属基复合材料。本发明制备复合材料纤维和金属基体结合稳定,材料性能优异,抗弯强度、弹性模量、布氏硬度均大幅度提高,服役温度也分别高出铝合金、铜合金100℃以上,在高温动载领域有重要应用价值。(The invention discloses an interface modified fiber reinforced metal matrix composite material, the volume density of which is less than 3.0g/cm 3 Consists of reinforcing fiber, interface layer and metal matrix. The preparation method comprises the following steps: weaving the reinforced fiber into a fiber preform, preparing a chemical vapor infiltration coating and a chemical plating coating in sequence, then die-casting an aluminum alloy or copper alloy melt into the fiber preform, and cooling to obtain the interface modified fiber reinforced metal matrix composite. The composite material fiber prepared by the invention is stably combined with the metal matrix, and has excellent material performance, bending strength, elastic modulus,The Brinell hardness is greatly improved, the service temperature is also higher than that of aluminum alloy and copper alloy by more than 100 ℃, and the high-temperature dynamic load bearing alloy has important application value in the field of high-temperature dynamic load.)

1. An interface modified fiber reinforced metal matrix composite material with a bulk density less than 3.0g/cm³The fiber reinforced composite material consists of reinforced fiber, interface layer and metal matrix, and features that the reinforced fiber is woven into fiber prefabricated body, the interface layer is coated homogeneously on the fiber surface, and the metal matrix is filled inside the fiber prefabricated body in situ; the reinforced fiber is one of carbon fiber, silicon carbide fiber, alumina fiber and high silica fiber; the fiber preform structure is one of 2D laminated, 2.5D woven, 3D knitted and needled carbon felt, and the volume fraction of the fiber is 15-45%; the interface layer is a chemical vapor infiltration interface and a chemical plating interface composite layer; the metal matrix is one of magnesium alloy and aluminum alloy.

2. The preparation method of the interface modified fiber reinforced metal matrix composite is characterized by comprising the following steps:

(1) weaving the fiber into a required member shape to form a prefabricated body, and then preparing a pyrolytic carbon interface layer, or a silicon oxide interface layer, or a silicon carbide interface layer, or a zirconium oxide interface layer on the surface of the fiber by a chemical vapor infiltration method;

(2) then sequentially carrying out degumming treatment, roughening treatment, sensitizing treatment and activating treatment on the fiber preform;

(3) preparing a chemical plating stock solution, immersing the fiber preform treated in the step (2) into the chemical plating stock solution, ultrasonically vibrating and heating to 70-100 ℃, preserving heat for 1-5 min, slowly adding a reducing agent for reduction, and continuing aging for 30-60 min after the reducing agent is added; the chemical plating solution contains one ion of Ni, Cu and Ag;

(4) adding normal hexane into the surface layer of the chemical plating stock solution reduced in the step (3), taking out the fiber preform, airing at room temperature for 5-15 min, and then drying in a vacuum oven for 2-6 hours to obtain the fiber preform of the chemical plating interface layer;

(5) and (4) placing the fiber preform with the interface layer prepared in the step (4) into a mold for fixing, placing the mold into an infiltration furnace for vacuum environment preheating to 500-700 ℃, then injecting molten metal into the mold, pressurizing to 1.5-5.0 MPa after injection, and cooling along with the furnace after heat preservation and pressure maintaining to obtain the interface modified fiber reinforced metal matrix composite.

Technical Field

The invention relates to a fiber-reinforced metal-based composite material and a preparation method thereof, in particular to an interface modified fiber-reinforced metal-based composite material and a preparation method thereof.

Background

Carbon fibers, silicon carbide fibers, aluminum oxide fibers and high silica fibers are taken as typical high-performance inorganic fibers, have the advantages of light weight, high specific strength, high specific modulus, high temperature resistance, chemical corrosion resistance, low thermal expansion coefficient and the like, and are widely applied to the fields of aerospace, high-speed rail, automobiles, sports goods, nuclear industry and the like.

However, the inorganic fiber has great surface inertness and lacks active functional groups, so that when the inorganic fiber is compounded with a metal material, the inorganic fiber and the metal material have obvious composition difference and interface incompatibility, and the inorganic fiber and the metal material have poor wetting effect, so that the inorganic fiber and the metal material have more problems in compounding. Therefore, surface modification of high performance inorganic fibers is critical.

Chemical plating is a surface metallization modification method which is green, environment-friendly, low in cost and wide in application, a plating layer prepared by using a chemical plating technology is uniform and firm, components are easy to control, and the chemical plating is one of common preparation technologies for surface interface modification of inorganic fibers.

The Chinese patent with application publication number CN107058986A discloses a method for chemically plating nickel on the surface of carbon fiber, which comprises the following steps: (1) pretreatment: the pretreatment of the carbon fiber comprises degreasing treatment, coarsening treatment, sensitizing treatment and activating treatment; (2) preparing a plating solution: deionized water is used as a solution, and the following components are sequentially added: main salt: 30-45 g/L of nickel sulfate hexahydrate, and the compounding agent: 25-30 g/L of ammonium chloride, stabilizer and complexing agent: 15-25 g/L of sodium citrate, and adjusting the pH value to 10-11 by using a sodium hydroxide solution; (3) soaking the pretreated carbon fiber into the plating solution prepared in the second step, and slowly dripping 25ml/L hydrazine hydrate solution into the plating solution for reduction when the temperature of the plating solution is raised to 80-100 ℃; (4) and (3) drying the reduced carbon fiber in a vacuum drying oven at the temperature of 80-100 ℃.

The Chinese patent with application publication number CN108342721A discloses a Ni-Co-Pr-B quaternary alloy plating solution for chemical plating on the surface of glass fiber and a preparation method thereof, which comprises the following operation steps: (1) pretreating glass fibers; (2) dissolving nickel chloride, cobalt chloride, praseodymium sulfate, sodium borohydride, potassium sodium tartrate, sodium metabisulfite and ethylenediamine in distilled water respectively; (3) uniformly mixing the nickel chloride, cobalt chloride, praseodymium sulfate, sodium metabisulfite and the ethylenediamine solution which are completely dissolved in the step (2), adding the mixture into the sodium potassium tartrate solution, and uniformly stirring; (4) slowly adding the sodium borohydride solution into the solution prepared in the step (2), diluting, and adjusting the pH value to 11-14 by using sodium hydroxide; (5) adding the glass fiber pretreated in the step (1) into the plating solution prepared in the step (3) for chemical tin and nickel plating, wherein the plating temperature is 55-90 ℃; (6) and (5) drying the Ni-Co-Pr-B plated glass fiber prepared in the step (5).

The Chinese patent with application publication number CN109161876A discloses a chemical silver plating method on the surface of nylon fiber, which comprises the following steps: (1) oil removal: putting a certain amount of fibers into a clean container, and adding an alkaline degreasing agent for reducing the surface tension of the fibers into the container; (2) sensitizing the sensitizing solution A: completely immersing the fiber obtained in the step (1) in the prepared sensitizing solution A to enable the surface of the fiber to adsorb a layer of metal with catalytic activity; (3) sensitizing the sensitizing solution B: completely immersing the fiber obtained in the step (2) in the sensitizing solution B prepared in situ, so that a carbonyl functional group on the surface of the fiber and a hydroxyl functional group in the sensitizing solution B form a hydrogen bond; (4) and (3) activation: completely immersing the fiber obtained in the step (3) in the prepared silver ammonia solution; (5) adding a quantitative glucose reducing solution into the solution obtained in the step (4).

At present, when inorganic fibers are subjected to surface modification treatment by a chemical plating method, the fibers are directly taken out and put into an oven for drying after reduction treatment, so that plating layers among fiber bundles are easily adhered together, and metal is difficult to fill the fiber bundles in the compounding process of a metal matrix, so that the performance of a composite material is influenced.

Disclosure of Invention

The invention aims to provide an interface modified fiber reinforced metal matrix composite and a preparation method thereof, wherein n-hexane is added when an interface layer is prepared by a chemical plating method, so that the defects of the existing materials and technologies are overcome.

In order to achieve the aim, the invention provides an interface modified fiber reinforced metal matrix composite, the bulk density of which is less than 3.0g/cm3, the composite is composed of reinforced fibers, an interface layer and a metal matrix, and the composite is characterized in that the reinforced fibers are woven into a fiber preform in advance, the interface layer is uniformly wrapped on the surface of the fibers, and the metal matrix is filled in the fiber preform in situ; the reinforced fiber is one of carbon fiber, silicon carbide fiber, alumina fiber and high silica fiber; the fiber preform structure is one of 2D laminated, 2.5D woven, 3D knitted and needled carbon felt, and the volume fraction of the fiber is 15-45%; the interface layer is a chemical vapor infiltration interface and a chemical plating interface composite layer; the metal matrix is one of magnesium alloy and aluminum alloy.

The preparation method of the interface modified fiber reinforced metal matrix composite is characterized by comprising the following steps:

(1) weaving the fiber into a required member shape to form a prefabricated body, and then preparing a pyrolytic carbon interface layer, or a silicon oxide interface layer, or a silicon carbide interface layer, or a zirconium oxide interface layer on the surface of the fiber by a chemical vapor infiltration method;

(2) then sequentially carrying out degumming treatment, roughening treatment, sensitizing treatment and activating treatment on the fiber preform;

(3) preparing a chemical plating stock solution, immersing the fiber preform treated in the step (2) into the chemical plating stock solution, ultrasonically vibrating and heating to 70-100 ℃, preserving heat for 1-5 min, slowly adding a reducing agent for reduction, and continuing aging for 30-60 min after the reducing agent is added; the chemical plating solution contains one ion of Ni, Cu and Ag;

(4) adding normal hexane into the surface layer of the chemical plating stock solution reduced in the step (3), taking out the fiber preform, airing at room temperature for 5-15 min, and then drying in a vacuum oven for 2-6 hours to obtain the fiber preform of the chemical plating interface layer;

(5) and (4) placing the fiber preform with the interface layer prepared in the step (4) into a mold for fixing, placing the mold into an infiltration furnace for vacuum environment preheating to 500-700 ℃, then injecting molten metal into the mold, pressurizing to 1.5-5.0 MPa after injection, and cooling along with the furnace after heat preservation and pressure maintaining to obtain the interface modified fiber reinforced metal matrix composite. Compared with the prior materials and the prior art, the invention has the following beneficial effects: (1) after the fiber is immersed in the chemical plating stock solution and heated to the reduction temperature, the temperature is kept for a period of time, so that the temperature inside and outside the stock solution and the fiber is uniform, and the uniformity and consistency of a plating layer in the reduction process are ensured; (2) normal hexane is added into the surface layer of the reduced chemical plating stock solution, so that a layer of hydrocarbon is wrapped outside a fiber tow coating when the fiber is taken out, and the adhesion of the coating among tows is avoided, thereby ensuring the compactness and uniformity of the fiber tow coating; (3) the reinforced fiber is woven into the fiber prefabricated body, so that the overall structural stability, the impact resistance and the damage tolerance of the composite material are improved.

Detailed Description

The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will occur to those skilled in the art upon reading the present specification and which fall within the limits of the appended claims.

Examples

The fiber reinforced metal matrix composite material takes pyrolytic carbon and metal copper as interfaces and has the volume density of 2.5g/cm³The reinforced silicon carbide fiber reinforced composite material consists of reinforced silicon carbide fiber, an interface layer and an aluminum metal matrix, and is characterized in that the reinforced fiber is pre-woven into a fiber preform, the interface layer is uniformly wrapped on the surface of the fiber, and the metal matrix is filled in the fiber preform in situ; the reinforced fiber is a silicon carbide fiber woven with a 2.5D structure, and the volume fraction of the fiber is 35%; the interface layer is made of pyrolytic carbon and Cu, and the thickness of the interface layer is 0.5 mu m; the metal matrix is aluminum alloy.

The preparation method of the composite material comprises the following steps:

(1) weaving the fiber into a required component shape to form a prefabricated body, taking methane as a precursor, and preparing a pyrolytic carbon interface layer on the surface of the fiber by a chemical vapor infiltration method.

(2) Then sequentially carrying out degumming treatment, roughening treatment, sensitizing treatment and activating treatment on the fiber preform;

(3) preparing a chemical copper plating stock solution, immersing the fiber preform treated in the step (2) into the chemical copper plating stock solution, ultrasonically vibrating and heating to 90 ℃, preserving heat for 3min, slowly adding a reducing agent for reduction, and continuing aging for 50min after the reducing agent is added;

(4) adding normal hexane into the surface layer of the chemical plating stock solution reduced in the step (3), taking out the fiber preform, airing at room temperature for 10min, and then drying in a vacuum oven for 3 hours to obtain the fiber preform of the chemical plating interface layer;

(5) and (4) placing the fiber preform with the interface layer prepared in the step (4) into a mold for fixing, placing the mold into an infiltration furnace for vacuum environment preheating to 550 ℃, then injecting an aluminum alloy body into the mold, pressurizing to 3.0MPa after injection, and cooling along with the furnace after heat preservation and pressure maintaining to obtain the interface modified fiber reinforced metal matrix composite.

The composite material prepared by the embodiment has the bending strength of more than 400MPa and the open porosity of less than 1.5 percent, has the elastic modulus of more than 200 percent, the Brinell hardness of more than 300 percent and the service temperature of more than 100 percent compared with aluminum alloy, and has important application value in the field of high-temperature dynamic load.

The above description is only an embodiment of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modifications made by using the design concept should fall within the scope of infringing the protection of the present invention. However, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the protection scope of the technical solution of the present invention.