CN102643024B - Magnesium oxide (MgO)-silicon dioxide (SiO2)-aluminum oxide (Al2O3)-boron trioxide (B2O3)-potassium fluoride (KF) glass ceramic composite material adopting silicon carbide (SiC) as enhanced-phase and preparation method thereof - Google Patents

Abstract

The invention discloses a magnesium oxide (MgO)-silicon dioxide (SiO2)-aluminum oxide (Al2O3)-boron trioxide (B2O3)-potassium fluoride (KF) glass ceramic composite material adopting silicon carbide (SiC) as an enhanced-phase, which is made of SiO2, Al2O3, MgO, B2O3, KF and SiC, the mass ratio of the SiO2, Al2O3, MgO, B2O3 and KF is 20 to 50: 12 to 35: 10 to 30: 5 to 9: 9 to 18, and the mass of the SiC accounts for 5 to 30 percent of the gross mass of the SiO2, Al2O3, MgO, B2O3 and KF. The preparation method of the composite material comprises the steps of: firstly water quenching the mixed powder of the SiO2, Al2O3, MgO, B2O3 and KF, adding SiC particles after being ground to be further uniformly mixed, completing the crystallization after the shaping, and acquiring the glass ceramic composite material. The tensile strength of the glass ceramic composite material acquired through the method can reach 200 to 400MPa. The composite material and the method are low in cost and applicable to the industrial scale.

Description

A kind ofly using the MgO-SiO of SiC as wild phase 2– Al 2o 3– B 2o 3– KF glass ceramic composite material and preparation method thereof

Technical field

The present invention relates to a kind of novel glass pottery that particle SiC is wild phase of take, improve the technical field of glass-ceramic obdurability.

Background technology

Glass-ceramic, claims again devitrified glass, refers to a class type material simultaneously with crystalline state and amorphous substance feature.Its preparation method is generally, and by thermal treatment, makes the nuclei growth in parent glass, thereby forms equally distributed small crystal.

Traditional metal materials is difficult to meet the high-tech area development service requirementss more and more higher to material such as space flight, aviation, the energy, military affairs, and stupalith provides under without cooling or few cooling conditions the possibility in higher temperature use.But compare with traditional metal materials, the essential fragility that stupalith exists and cause therefrom the low reliability in use, has seriously limited its practical engineering application scope.Current research shows, the fiber (comprising whisker) with high work of rupture is a kind of can enhancing with the compound of ceramic matrix, again can be toughness reinforcing, can keep at comparatively high temps one of effective ways of its highly malleablized effect again simultaneously.Thereby fiber or metal whisker reinforced composite are the another effective ways that improves glass-ceramic mechanical property.Can by having, to be different from fiber or the whisker of glass-ceramic substrate compound with it, also can be compound with it with other materials such as metals, the fiber of glass-ceramic or microsphere can also be compound in other matrix.Find to strengthen MgO-Al with SiC whisker ₂o ₃-SiO ₂the glass-ceramic of base, its folding strength and fracture toughness property are respectively 490MPa and 3.7MPam ^1/2, than increasing powerhouse, do not improve 2 times of left and right.But whisker strengthens and fibre reinforced composites cost is higher.

Because glass-ceramic has glass and ceramic advantage concurrently, aspect calorifics, chemistry, biology, optics and electric property, be often better than metal and organic polymer material.At present, MgO-SiO ₂– Al ₂o ₃– B ₂o ₃– KF glass-ceramic, owing to having good insulative dielectric performance and processability, is widely used in manufacturing heat-resistant part in vacuum insulation parts, high temperature guide rail and corrosive environment etc.Current MgO-SiO ₂– Al ₂o ₃– B ₂o ₃– KF glass-ceramic bending strength is only up to 80MPa, and bending strength performance is not high.

Summary of the invention

The technical problem to be solved in the present invention is to improve to take the MgO-SiO that particle SiC is wild phase ₂– Al ₂o ₃– B ₂o ₃the flexural strength of the glass ceramic composite material of – KF, thus a kind of method that improves its bending strength by add a certain amount of particle SiC in glass-ceramic raw material is provided.Utilize powder method to prepare MgO-SiO ₂– Al ₂o ₃– B ₂o ₃– KF glass-ceramic, is used SiC particle to strengthen, stable components, and technique is simple, and material homogeneity is good, and bending strength stable performance, is applicable to technical scale.

Technical scheme of the present invention is: a kind of SiC of usining is as the MgO-SiO of wild phase ₂– Al ₂o ₃– B ₂o ₃– KF glass ceramic composite material, it is by SiO ₂, Al ₂o ₃, MgO, B ₂o ₃, KF and SiC make, described SiO ₂, Al ₂o ₃, MgO, B ₂o ₃with the mass ratio of KF be 20-50:12-35:10-30:5-9:9-18, the quality of SiC accounts for SiO ₂, Al ₂o ₃, MgO, B ₂o ₃5-30% with the total mass of KF.

Described using the MgO-SiO of SiC as wild phase ₂– Al ₂o ₃– B ₂o ₃the preparation method of – KF glass ceramic composite material, its step is as follows:

(1) by SiO ₂, Al ₂o ₃, MgO, B ₂o ₃after mixing with KF powder, in resistance furnace, in 1400-1600 ℃ of heat fused shrend, obtain frit;

(2) frit is ground, crosses 300-400 mesh sieve, after add SiC powder and mix, obtain compound;

(3) by compound compression moulding, sintering under the condition of 800-1200 ℃ then, and under the condition of 800-1200 ℃, be incubated 2-3 hour crystallization.

The invention has the beneficial effects as follows: the preparation process of this matrix material is for first making MgO, SiO ₂, Al ₂o ₃, B ₂o ₃with the shrend of KF mixed powder, after grinding, add a certain amount of particle SiC further to mix, after moulding, complete crystallization, thereby obtain this glass ceramic composite material.The method can obtain the glass ceramic composite material that bending strength can reach 200-400MPa.Cost is low, is applicable to technical scale.

Embodiment

Embodiment 1

By SiO ₂, Al ₂o ₃, MgO, B ₂o ₃with KF powder respectively in proportion 50.0,15.9,13.8,6.8,13.5wt% mixes, and puts into aluminum oxide porcelain boat.Then in Si-Mo rod resistance furnace, in 1500 ℃ of insulations, within 1.5 hours, melt, and shrend immediately.After drying materials after shrend, put into agate mortar and grind, then cross 300 object mesh screens.After add 30%Wt 2.1 μ m SiC powder and mix.This compound is pressed into 40 * 5 * 5(mm) bar shaped blank, pressing pressure is 1.5MPa.Then at 1100 ℃ of sintering, be incubated 1.5 hours.Furnace cooling.Above-mentioned MgO-SiO ₂– Al ₂o ₃– B ₂o ₃– KF glass ceramic composite material bending strength is 280 ± 20MPa.

Embodiment 2

By SiO ₂, Al ₂o ₃, MgO, B ₂o ₃with KF powder respectively in proportion 40.0,15.9,13.8,10.1,20.2wt% mixes, and puts into aluminum oxide porcelain boat.Then in Si-Mo rod resistance furnace, in 1500 ℃ of insulations, within 1.5 hours, melt, and shrend immediately.After drying materials after shrend, put into agate mortar and grind, then cross 300 object mesh screens.After add 10%Wt 2.0 μ m SiC powder and mix.This compound is pressed into 40 * 5 * 5(mm) bar shaped blank, pressing pressure is 2MPa.Then at 1100 ℃ of sintering, be incubated 2.0 hours.Furnace cooling.Above-mentioned MgO-SiO ₂– Al ₂o ₃– B ₂o ₃– KF glass ceramic composite material bending strength is 290 ± 20MPa.

Embodiment 3

A kind ofly using the MgO-SiO of SiC as wild phase ₂– Al ₂o ₃– B ₂o ₃– KF glass ceramic composite material, it is by SiO ₂, Al ₂o ₃, MgO, B ₂o ₃, KF and SiC make, described SiO ₂, Al ₂o ₃, MgO, B ₂o ₃with the mass ratio of KF be 20:35:30:5:9, the quality of SiC accounts for SiO ₂, Al ₂o ₃, MgO, B ₂o ₃with 5% of the total mass of KF.

Using the MgO-SiO of SiC as wild phase ₂– Al ₂o ₃– B ₂o ₃the preparation method of – KF glass ceramic composite material, its step is as follows:

(1) by SiO ₂, Al ₂o ₃, MgO, B ₂o ₃after mixing with KF powder, in resistance furnace, in 1400 ℃ of heat fused shrend, obtain frit;

(2) frit is ground, crosses 300 mesh sieves, after add SiC powder and mix, obtain compound;

(3) by compound compression moulding, sintering under the condition of 800 ℃ then, and under the condition of 800 ℃, be incubated 2 hours crystallizatioies.Above-mentioned MgO-SiO ₂– Al ₂o ₃– B ₂o ₃– KF glass ceramic composite material bending strength is 350 ± 20MPa.

Embodiment 4

A kind ofly using the MgO-SiO of SiC as wild phase ₂– Al ₂o ₃– B ₂o ₃– KF glass ceramic composite material, it is by SiO ₂, Al ₂o ₃, MgO, B ₂o ₃, KF and SiC make, described SiO ₂, Al ₂o ₃, MgO, B ₂o ₃with the mass ratio of KF be 50:12:10:9:9, the quality of SiC accounts for SiO ₂, Al ₂o ₃, MgO, B ₂o ₃with 30% of the total mass of KF.

Using the MgO-SiO of SiC as wild phase ₂– Al ₂o ₃– B ₂o ₃the preparation method of – KF glass ceramic composite material, its step is as follows:

(1) by SiO ₂, Al ₂o ₃, MgO, B ₂o ₃after mixing with KF powder, in resistance furnace, in 1600 ℃ of heat fused shrend, obtain frit;

(2) frit is ground, crosses 400 mesh sieves, after add SiC powder and mix, obtain compound;

(3) by compound compression moulding, sintering under the condition of 1200 ℃ then, and under the condition of 1200 ℃, be incubated 2 ~ 3 hours crystallizatioies.Above-mentioned MgO-SiO ₂– Al ₂o ₃– B ₂o ₃– KF glass ceramic composite material bending strength is 300 ± 20MPa.

Embodiment 5

A kind ofly using the MgO-SiO of SiC as wild phase ₂– Al ₂o ₃– B ₂o ₃– KF glass ceramic composite material, it is by SiO ₂, Al ₂o ₃, MgO, B ₂o ₃, KF and SiC make, described SiO ₂, Al ₂o ₃, MgO, B ₂o ₃with the mass ratio of KF be 30:20:20:8:15, the quality of SiC accounts for SiO ₂, Al ₂o ₃, MgO, B ₂o ₃with 20% of the total mass of KF.

Using the MgO-SiO of SiC as wild phase ₂– Al ₂o ₃– B ₂o ₃the preparation method of – KF glass ceramic composite material, its step is as follows:

(1) by SiO ₂, Al ₂o ₃, MgO, B ₂o ₃after mixing with KF powder, in resistance furnace, in 1500 ℃ of heat fused shrend, obtain frit;

(2) frit is ground, crosses 350 mesh sieves, after add SiC powder and mix, obtain compound;

(3) by compound compression moulding, sintering under the condition of 1000 ℃ then, and under the condition of 1000 ℃, be incubated 2.5 hours crystallizatioies.Above-mentioned MgO-SiO ₂– Al ₂o ₃– B ₂o ₃– KF glass ceramic composite material bending strength is 380 ± 20MPa.

Claims (1)

1. using the MgO-SiO of SiC as wild phase for one kind ₂– Al ₂o ₃– B ₂o ₃– KF glass ceramic composite material, is characterized in that: it is by SiO ₂, Al ₂o ₃, MgO, B ₂o ₃, KF and SiC make, described SiO ₂, Al ₂o ₃, MgO, B ₂o ₃with the mass ratio of KF be 20-50:12-35:10-30:5-9:9-18, the quality of SiC accounts for SiO ₂, Al ₂o ₃, MgO, B ₂o ₃with the 5-30% of the total mass of KF, its preparation process is as follows:

(1) by SiO ₂, Al ₂o ₃, MgO, B ₂o ₃after mixing with KF powder, in resistance furnace, in 1400-1600 ℃ of heat fused shrend, obtain frit;

(2) frit is ground, crosses 300-400 mesh sieve, after add SiC powder and mix, obtain compound;

(3) by compound compression moulding, sintering under the condition of 800-1200 ℃ then, and under the condition of 800-1200 ℃, be incubated 2-3 hour crystallization.