CN101942588B - Magnesium alloy diatomite ferric oxide composite material and preparation method thereof - Google Patents

Abstract

The invention provides a magnesium alloy diatomite iron oxide composite material and a preparation method thereof. The composite material has high wave-absorbing performance and excellent damping performance. The preparation method has simple process, low production cost and is suitable for industrialized production. The composite material uses a magnesium alloy as a matrix, and a diatomite iron oxide compound is distributed on the matrix. The diatomite iron oxide compound accounts for 40-45% by volume of the composite material. The particle size is 0.5-1mm; the weight percentage of the chemical composition of the magnesium alloy matrix: Al is 3%-8%, Th is 0.01%-0.05%, Si is 0.5%-1%, Sb is 0.005%-0.01% , and the rest is Mg; the diatomite iron oxide composite is iron oxide drilled into the pores of diatomite, and forms a thin film on the pore wall.

Description

Magnesium alloy diatomite iron oxide composite material and preparation method thereof

1. Technical field

The invention belongs to the field of metal materials, and relates to a magnesium alloy diatomite iron oxide composite material and a preparation method thereof.

2. Background technology

At present, in the field of materials, the wave-absorbing and vibration-reducing effect of materials has been paid attention to.

CN200410023374.1 relates to an aluminum-based wave-absorbing material and its preparation method, which is characterized in that: the surface layer of an aluminum or aluminum alloy plate is formed by a one-step or two-step anodic oxidation method of direct current or alternating current to form a porous aluminum oxide film to form an aluminum-based porous oxide film Aluminum template, that is, AAO template; use DC or pulse current electrochemical deposition to assemble magnetic nano-metal wire arrays in aluminum-based AAO porous membranes to make aluminum-based absorbing materials for in-situ assembly of magnetic nanowire arrays on the surface. The disadvantage of this method is that it requires high technical difficulty.

CN200910071958.9 proposes a ceramic whisker/ferromagnetic metal composite wave-absorbing material and a preparation method thereof, which relates to a composite material for absorbing electromagnetic waves and a preparation method thereof. Ceramic whiskers coated with ferromagnetic metal coatings are heat-treated for 60 minutes at a temperature of 300-400°C and the heat treatment atmosphere is hydrogen or argon to obtain ceramic whisker/ferromagnetic metal composite wave-absorbing materials. The disadvantage of this method is that the surface of the ceramic whisker is coated with a ferromagnetic metal coating, and the ferromagnetic metal is easy to fall off during processing.

Application No. CN200910191481.8 relates to a preparation method of a short carbon fiber reinforced magnesium-based composite material with excellent damping properties, which includes the following steps: (1) removing the organic glue layer on the surface of the short carbon fiber; (2) depositing metal nickel coating by electroless plating layer, under alkaline conditions by controlling the deposition time to obtain the required thickness of the coating; (3) After the short carbon fiber coated with metal nickel coating is prepared, the powder metallurgy method can be used to prepare the carbon fiber with excellent damping characteristics Short carbon fiber reinforced magnesium matrix composites. The invention adds 3 to 20% by volume of electroless nickel-plated short carbon fibers into the magnesium matrix. Although the matrix is strengthened and the damping performance is endowed with better performance, its damping performance is better than that of pure magnesium, which can reach High damping range of 0.015, but the process is more complicated. The disadvantage of this material is its poor absorbing properties.

3. Contents of the invention

The object of the present invention is to address the above-mentioned technical defects and provide a magnesium alloy diatomite-iron oxide composite material, which has high wave-absorbing performance and excellent damping performance.

Another object of the present invention is to provide a preparation method of magnesium alloy diatomite iron oxide composite material, which has simple process, low production cost and is suitable for industrial production.

The purpose of the present invention is achieved through the following technical solutions:

A magnesium alloy-based diatomite iron oxide composite material, the composite material takes magnesium alloy as a matrix, and diatomite iron oxide composites are distributed on the matrix, and the volume percentage of the diatomite iron oxide composites in the composite material is 40-45%, the particle of diatomite iron oxide composite is 0.5-1mm; the weight percentage of the chemical composition of the magnesium alloy matrix: Al is 3%-8%, Th is 0.01%-0.05%, Si is 0.5%-1%, Sb is 0.005%-0.01%, and the rest is Mg; diatomite iron oxide composite is iron oxide drilled into the pores of diatomite, and forms a film with a thickness of 0.1-10μm on the pore wall .

A method for preparing a magnesium alloy-based diatomite iron oxide composite material, characterized in that it comprises the following steps:

a. Preparation of diatomaceous earth iron oxide compound: put ferric chloride and ammonium ferrous sulfate into a hydrothermal container with Teflon lining, add water to dissolve (add a small amount of water to achieve dissolution), and the container temperature Keep at 80-90°C, then add diatomite, the size of diatomite is 0.5-1mm, stir the above materials for 2-7min, the weight ratio of ferric chloride, ferrous ammonium sulfate and diatomite is 1:1 : (1-2), after the stirring is finished, place the stirred material in an oven at 220° C. for 3 hours and then cool naturally to obtain the diatomite iron oxide compound;

Then dolomite and diatomite iron oxide compound are mixed, the size of dolomite particles is 0.01-0.06mm, the weight ratio of diatomite iron oxide compound and dolomite is 1: (0.05-0.09), and dolomite and silicon The mixture of algae and iron oxide composites is placed in the cavity of a steel mold with a heating device and a vacuum system at the bottom to form a composite prefabricated body, and the composite prefabricated body accounts for 40-45% of the cavity volume of the metal mold; turn on the heating device to control the temperature in the steel mold at 520-540°C;

b. Preparation of magnesium alloy solution: the weight percentage is 3%-8% for Al, 0.01%-0.05% for Th, 0.5%-1% for Si, 0.005%-0.01% for Sb, and the rest is Mg Raw materials are melted into alloy liquid at a temperature of 680-720°C;

c. Turn on the vacuum system, control the relative vacuum in the above-mentioned steel mold to be -30Kpa, pour the above-mentioned magnesium alloy liquid into the composite prefabricated body in the cavity of the steel mold, and fill the mold, the magnesium alloy liquid is in the Infiltrate the gap in the composite preform under the action of vacuum pressure, close the mold heating device, cool and solidify in the steel mold to form the magnesium alloy-based diatomite iron oxide composite material.

The beneficial effects of the present invention compared with prior art are as follows:

In the present invention, the diatomite has large gaps and is easy to accept iron oxide. The iron oxide is in the gaps of the diatomite to form a diatomite iron oxide composite that does not scatter iron oxide, thus becoming a solid material center for the composite material to absorb electromagnetic waves. ;

The diatomite is stirred in the iron oxide raw material solution, and the raw material solution drills into the pores of the diatomite to form a film of iron oxide with a thickness of 0.1-10 μm on the surface of the pores, and the iron oxide is Fe ₃ O ₄ .

The chemical composition of dolomite is CaMg[CO ₃ ] ₂ . The function of dolomite is to separate the diatomite particles during the impregnation preparation of the composite material, so that the magnesium alloy liquid can penetrate into the gap between the diatomite particles. At the same time, the dolomite has a vibration damping effect. .

The iron oxide is in the gap of diatomite and is not in contact with the magnesium alloy liquid, so it will not cause the oxidation of the magnesium alloy;

Si in magnesium alloy can promote the interfacial bonding between magnesium alloy and diatomite. Sb can promote the interfacial bonding between magnesium alloy and dolomite. Th in the magnesium alloy can reduce the particle size of the magnesium alloy and increase the strength of the matrix of the composite material. Robust diatomaceous earth-iron oxide composites enhance compressive properties of magnesium alloy composites. These can improve the mechanical properties of magnesium alloy-based diatomite-iron oxide composites.

In the preparation of the present invention, the diatomite has large voids and is easy to accept iron oxide, so the stirring and heating time in the preparation are short, and the production cycle is short.

The preparation process of the composite material is simple, and the produced composite material has a certain good damping performance and superior wave-absorbing performance, and the production cost is low, which is very convenient for industrial production.

4. Description of drawings See Table 1 for properties of gold.

Fig. 1 is the metallographic structure of the magnesium alloy-based diatomite-iron oxide composite material prepared in Example 1 of the present invention.

It can be seen from Figure 1 that diatomaceous earth iron oxide complexes are distributed on the magnesium alloy matrix.

5. Specific implementation

The following examples are only used to illustrate the present invention, and the weight percentages can be replaced by weight g, kg or other weight units.

Embodiment one:

The preparation process of the magnesium alloy-based diatomite iron oxide composite material of the present invention:

Preparation of diatomaceous earth iron oxide complex: put ferric chloride and ferrous ammonium sulfate into a hydrothermal container with Teflon lining, add water to dissolve (add a small amount of water to achieve dissolution), and keep the container temperature at 80 -90°C, then add diatomite, the size of diatomite particles is 0.5mm, stir the above materials for 2-7min, the weight ratio of ferric chloride, ferrous ammonium sulfate and diatomite is 1:1:1 , after the stirring is completed, place the stirring material in an oven at 220°C for 3 hours and then cool naturally to obtain the diatomite iron oxide compound;

Then dolomite and diatomite iron oxide compound are mixed, the size of dolomite particle is 0.01-0.06mm, the weight ratio of diatomite iron oxide compound and dolomite is 1:0.05, and the size of dolomite particle is 0.01mm ; Put the mixture of dolomite and diatomite iron oxide compound into the cavity of a steel mold with a heating device and a vacuum system at the bottom to form a composite prefabricated body, and the composite prefabricated body accounts for 45% of the cavity volume of the metal mold (40-45% is all right, so the volume percentage of the diatomite iron oxide composite that can be controlled to account for the composite material is 40-45%); turn on the heating device, and control the temperature in the steel mold to 520-540°C;

Preparation of magnesium alloy liquid: Al is 3% by weight, Th is 0.01%, Si is 0.5%, Sb is 0.005%, and the rest is Mg for batching, and is melted into alloy liquid at a temperature of 680-720°C;

Turn on the vacuum system, control the relative vacuum in the above-mentioned steel mold to be -30Kpa, pour the above-mentioned magnesium alloy liquid into the top of the composite prefabricated body in the mold cavity, and fill the mold, the magnesium alloy liquid is under vacuum pressure Infiltrate into the gap in the composite prefabricated body, close the mold heating device, cool and solidify in the steel mold to form the magnesium alloy-based diatomite iron oxide composite material.

Embodiment two:

Preparation of diatomaceous earth iron oxide complex:

When preparing the diatomite iron oxide composite, the weight ratio of ferric chloride, ammonium ferrous sulfate and diatomite is 1:1:2, and the particle size of diatomite is 0.9mm.

When preparing the composite preform, the weight ratio of diatomite iron oxide composite to dolomite is 1:0.09, and the size of dolomite particles is 0.06mm;

Preparation of magnesium alloy liquid: according to weight percentage, Al is 8%, Th is 0.05%, Si is 1%, Sb is 0.01%, and the rest is Mg for batching, and is melted into alloy liquid at a temperature of 680-720°C;

The preparation process is the same as that in Example 1, and the volume percentage of the alginate iron oxide composite in the composite material is controlled to be 40%.

Embodiment three:

Preparation of diatomaceous earth iron oxide complex:

When forming diatomite iron oxide complex, the weight ratio of ferric chloride, ammonium ferrous sulfate and diatomite is 1:1:1.5, and the particle size of diatomite is 0.7mm.

When preparing the composite preform, the weight ratio of diatomite iron oxide composite to dolomite is 1:0.06, and the size of dolomite particles is 0.05mm;

Preparation of magnesium alloy liquid: according to weight percentage, Al is 7%, Th is 0.04%, Si is 0.8%, Sb is 0.008%, and the rest is Mg for batching; it is melted into alloy liquid at a temperature of 680-720°C;

The preparation process is the same as that in Example 1, and the volume percentage of the alginate iron oxide composite in the composite material is controlled to be 45%.

Embodiment four: (raw material proportioning is not the example within the proportioning scope of the present invention)

Preparation of diatomaceous earth iron oxide complex:

When preparing the diatomite iron oxide composite, the weight ratio of ferric chloride, ammonium ferrous sulfate and diatomite is 1:1:0.9, and the particle size of diatomite is 0.4mm;

When preparing the composite prefabricated body, the weight ratio of the diatomite iron oxide composite to dolomite is 1:0.04, and the size of the dolomite particles is 0.005mm; the volume percentage of the diatomite iron oxide composite in the composite material is controlled to be 45 %;

Preparation of magnesium alloy liquid: by weight percentage: Al is 2%, Th is 0.0055%, Si is 0.4%, Sb is 0.004%, and the rest is Mg for batching, melting into alloy liquid at a temperature of 680-720°C;

The preparation process is the same as in Example 1.

Embodiment five: (raw material proportioning is not the example within the proportioning scope of the present invention)

Preparation of diatomaceous earth iron oxide complex:

When forming diatomite iron oxide complex, the weight ratio of ferric chloride, ammonium ferrous sulfate and diatomite is 1:1:2.1, and the particle size of diatomite is 1.2mm;

When preparing the composite prefabricated body, the weight ratio of the diatomite iron oxide composite to dolomite is 1:0.1, and the size of the dolomite particles is 0.7mm; the volume percentage of the diatomite iron oxide composite in the composite material is controlled to be 40 %;

Preparation of magnesium alloy liquid: the weight percentage of the chemical composition of the magnesium alloy matrix: Al is 9%, Th is 0.06%, Si is 1.1%, Sb is 0.02%, and the rest is Mg; at a temperature of 680-720°C Melted into alloy liquid;

The preparation process is the same as in Example 1.

The following table is a comparison table of alloy properties with different components and proportions:

Table 1

Magnesium alloy-based diatomite iron oxide composite material, the particle size of the composite is too small, which reduces the absorbing unit, reduces the absorbing strength and vibration damping strength, and is not conducive to the manufacture of composite materials; If the particle size is too large, the wave-absorbing unit increases, which reduces the number of wave-absorbing units per unit volume of the composite material, and is not conducive to wave absorption and vibration reduction.

When the magnesium alloy-based diatomite iron oxide composite material is prepared, the amount of diatomite is too small, and it is difficult for ferric chloride and ferrous ammonium sulfate to enter the diatomite gap. The total amount of iron oxide in the composite material is small, and the absorbing strength is weak; If the amount of diatomite is too much, it is difficult to form a perfect composite material. The amount of iron oxide contained in the gap of diatomite is small, and the absorbing strength is also weak.

When the magnesium alloy-based diatomite iron oxide composite material is prepared, the amount of dolomite is too small or the dolomite particles are too small to separate the diatomite particles, which is not conducive to the infiltration of magnesium alloy liquid. The amount of dolomite is too large or the dolomite particles are too small. If the particles are too large, the mechanical properties of the magnesium alloy-based diatomite-iron oxide composite will be affected.

Al, Th, Si, and Sb in the magnesium alloy matrix are within the scope of this application, and the composite material has good performance. These elements exceed the ratio range of the present application, the number of brittle compounds is large, the magnesium alloy is difficult to combine with the diatomite interface, the mechanical properties of the titanium alloy itself are reduced, and the wave absorption and vibration damping properties of the composite material are also greatly reduced.

Claims (1)

1. magnesiumalloy based diatomite ferric oxide composite material; This matrix material is matrix with the magnesiumalloy; Zeyssatite red stone mixture and dolomite particles are distributing on matrix; The two volume percent that accounts for matrix material of this zeyssatite red stone mixture and dolomite particles is 40-45%, and the particle of zeyssatite red stone mixture is 0.5-1mm, and wherein red stone is Fe ₃O ₄The following chemical components in percentage by weight of magnesium alloy substrate: Al is 3%～8%, and Th is 0.01%～0.05%, and Si is 0.5%-1%, and Sb is 0.005%-0.01%, and all the other are Mg;

Its preparation process may further comprise the steps:

The preparation of a, zeyssatite red stone mixture: pack iron(ic)chloride and ferrous ammonium sulphate in the hydro-thermal container of being with teflon lined into; Be dissolved in water, vessel temp keeps 80-90 ℃, the zeyssatite of packing into; Diatomite particle is of a size of 0.5-1mm; Stir above material and reach 2-7min, iron(ic)chloride, ferrous ammonium sulphate and diatomaceous weight ratio are 1: 1: (1-2), naturally cooling just obtains zeyssatite red stone mixture after will stirring baking oven that thing places 220 ℃ after stir finishing and being incubated 3h;

Then rhombspar and zeyssatite red stone mixture are mixed; Dolomite particles is of a size of 0.01-0.06mm; The weight ratio of zeyssatite red stone mixture and rhombspar is 1: (0.05-0.09); The cavity of steel die of the mixture of rhombspar and zeyssatite red stone mixture being put into the logical vacuum system in bottom of heating unit forms the mixture precast body, and the mixture precast body accounts for the 40-45% of metal die cavity volume; Opening heating unit, is 520-540 ℃ in the control steel die;

The preparation of b, liquid magnesium alloy: with weight percentage is that Al is 3%～8%, and Th is 0.01%～0.05%, and Si is 0.5%-1%, and Sb is 0.005%-0.01%, and all the other are the raw material of Mg, under 680-720 ℃ of temperature, are fused into alloy liquid;

C, open vacuum system; The relative vacuum degree of controlling in the above-mentioned steel die is-30Kpa; With above-mentioned liquid magnesium alloy pour into mixture precast body in the steel die cavity above, and fill with mould, liquid magnesium alloy infiltrates the gap in the mixture precast body under the vacuum pressure effect; The closing molding heating unit solidifies at the steel die internal cooling and forms magnesiumalloy based diatomite ferric oxide composite material.

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