CN104909788A - Alumina-fiber-enhanced beryllium oxide ceramic-based composite material and preparation method thereof - Google Patents

Abstract

The invention discloses an alumina-fiber-enhanced beryllium oxide ceramic-based composite material and a preparation method thereof. The material is characterized in that the material is prepared from the raw materials of, by weight, 3-5 parts of phosphorus pentoxide, 10-15 parts of modified alumina fiber, 70-80 parts of beryllium oxide, 7-9 parts of hafnium dioxide, 4-6 parts of titanium dioxide, 0.02-0.03 part of t-butyl hydroperoxide, 4-6 parts of butadiene, 1-2 parts of polyvinylpyrrolidone, 1-2 parts of sodium tripolyphosphate, 0.1-0.3 part of diacetone acrylamide, 2-3 parts of polyvinyl alcohol, 20-30 parts of ethanol, and 30-50 parts of deionized water. According to the invention, the alumina fiber processed through an antioxidant treatment is adopted as a ceramic enhancement phase, and has the properties of enhancing the toughness, mechanical properties, wear resistance, hardness and high-temperature resistance of ceramic. With the added titanium dioxide, ceramic acid resistance is enhanced. With the added phosphorus pentoxide, a blank protection effect is provided during a ceramic manufacturing process, air oxidation is reduced, and blank damage is reduced.

Description

A kind of sapphire whisker strengthens beryllium oxide ceramics based composites and preparation method thereof

Technical field

the present invention relates to a kind of sapphire whisker and strengthen beryllium oxide ceramics based composites and preparation method thereof, belong to technical field of ceramic production.

Background technology

The ultimate principle of gel injection molding and forming technology adds low viscous organic monomer and linking agent in the ceramic size of low viscosity, high solid volume fraction, when introducing initiator after injection molding, there is home position polymerization reaction under certain conditions in the organic monomer in slurry and linking agent, form firm interlinkage reticulated structure, make slurry solidify in place immediately, thus make ceramic body formed in situ, then carry out the demoulding, drying, organics removal, sintering, required ceramic component can be obtained.The technique of forming process of ceramics has the methods such as gel injection, injection forming, compression moulding, injection molding and hot die-casting molding, but in molding time gel injection and the injection molding time short, strength gel injection molding after the demoulding is the highest, and its is applied widely, forming defect is few, the advantage that dry body strength is high, compared with traditional dry-forming technique, reduce the quantity of gross blow hole, improve the distribution of pore, improve the homogeneity of base substrate, thus be conducive to the raising of densification and the intensity sintered.

Beryllium oxide ceramics is an important class of electronic ceramics, also be one of leading product of beryllium oxide ceramics substrate, beryllium oxide has the features such as high thermal conductivity, high-melting-point, high insulation, low-k, low dielectric loss and good packaging process, adaptability, is widely used in microwave electrovacuum, microelectronics, the medium field of photoelectric device.Beryllium oxide itself is poisonous, but its sintered compact is nontoxic, beryllium oxide has high thermal conductivity but also has good electricity saving performance and manufacturing process, and be a spotlight in the use of radiating element, power device more at present can not get good solution in the technical problem of heat dissipation.But the toughness of beryllium oxide ceramics is inadequate, easily rupture under external force, current fiber reinforced ceramic the experiment proved that the effect with good raising ceramic fracture toughness, so the present invention adopts the sapphire whisker crossed through modification as the wild phase of beryllium oxide ceramics, improve fracture toughness property, strengthen the Application Areas of beryllium oxide ceramics.

Summary of the invention

The object of this invention is to provide a kind of sapphire whisker and strengthen beryllium oxide ceramics based composites and preparation method thereof.

In order to realize object of the present invention, the present invention is by following scheme implementation:

A kind of sapphire whisker strengthens beryllium oxide ceramics based composites and preparation method thereof, is made up: Vanadium Pentoxide in FLAKES 3-5, modified oxidized aluminum fiber 10-15, beryllium oxide 70-80, hafnium oxide 7-9, titanium dioxide 4-6, tertbutyl peroxide 0.02-0.03, divinyl 4-6, polyvinylpyrrolidone 1-2, tripoly phosphate sodium STPP 1-2, diacetone-acryloamide(DAA) 0.1-0.3, polyvinyl alcohol 2-3, ethanol 20-30, deionized water 30-50 of the raw material of following weight part;

The preparation method of described modified oxidized aluminum fiber is: sapphire whisker is soaked 1-2 hour in acetone, uses distilled water flushing 2-3 time, dry for standby after taking out, the ethanol mixing of the tetrabutyl titanate of 10-15 weight part and 150-180 weight part is added in the flask with magnetic stirring apparatus, by the deionized water of 2-3 weight part, the hydrochloric acid of 0.2-0.4 weight part and the ethanol of 2-5 weight part fully mix, slowly be added drop-wise in flask, add the molybdenum oxide powder of 2-4 weight part again, stir 30-40 minute, sapphire whisker for subsequent use is added in gel under vacuum tightness is 0.09-0.1MPa, floods 1-2 hour, dry under 70-80 ° of C after taking-up, repeatable operation like this 2-3 time, last under the protection of high-purity argon gas under 500-600 ° of C pyroreaction 1-2 hour.

A kind of sapphire whisker of the present invention strengthens beryllium oxide ceramics based composites and preparation method thereof, is made up of following concrete steps:

(1) beryllium oxide, hafnium oxide are added in ball mill, ask as ball-milling medium using aluminum oxide, material ball ratio is 1:2, again divinyl, tertbutyl peroxide are added in the mixing solutions of ethanol and deionized water, adding after dissolving after polyvinylpyrrolidone, tripoly phosphate sodium STPP, polyvinyl alcohol and modified oxidized aluminum fiber stir is added in ball mill, ball milling 20-40 minute;

(2) slurry that ball milling obtains is vacuumized, take out and within 2-5 minute, add diacetone-acryloamide(DAA) in backward slurry and continue to stir, then slurry to be injected into after in laminated glass mould in vacuum drying oven dry 1-2 hour under 60-80 ° of C;

(3) by the wet base demoulding at room temperature seasoning 1-2 days in step (2), then at 95-100 ° of C temperature, humidity is dry 1-2 days under the condition of 60-70%, remaining one-tenth is distributed into plasma spraying powder conveyer in billet surface spraying evenly;

(4) by the base substrate of step (3) at room temperature with the ramp to 200 of 3-5 ° of C/min ° C, again with the ramp to 600 of 1-2 ° of C/min ° C, constant temperature keeps being positioned in vacuum sintering furnace after 1-2 hour, sinters 3-4 hour, can obtain at the temperature of 1400-1600 ° of C.

Advantage of the present invention is: the sapphire whisker through antioxidation treatment that the present invention adds has as the wild phase of pottery and strengthens ceramics toughness, mechanical property, wear resistance, hardness and resistant to elevated temperatures characteristic; the titanium dioxide added adds the acid resistance of pottery; the Vanadium Pentoxide in FLAKES added plays a part to protect base substrate in ceramics manufacturing process; reduce oxidation by air, reduce the characteristic that base substrate damages.

specific embodiments

Below by specific examples, the present invention is described in detail.

A kind of sapphire whisker strengthens beryllium oxide ceramics based composites and preparation method thereof, is made up: Vanadium Pentoxide in FLAKES 4, modified oxidized aluminum fiber 12, beryllium oxide 80, hafnium oxide 8, titanium dioxide 5, tertbutyl peroxide 0.03, divinyl 5, polyvinylpyrrolidone 2, tripoly phosphate sodium STPP 2, diacetone-acryloamide(DAA) 0.3, polyvinyl alcohol 3, ethanol 30, deionized water 50 of the raw material of following weight part (kilogram);

The preparation method of described modified oxidized aluminum fiber is: sapphire whisker is soaked 2 hours in acetone, uses distilled water flushing 3 times, dry for standby after taking out; The ethanol mixing of the tetrabutyl titanate of 12 weight parts and 160 weight parts is added in the flask with magnetic stirring apparatus; the hydrochloric acid of the deionized water of 3 weight parts, 0.3 weight part and the ethanol of 5 weight parts are fully mixed; slowly be added drop-wise in flask; add the molybdenum oxide powder of 4 weight parts again; stir 40 minutes; sapphire whisker for subsequent use is added in gel and floods 1 hour under vacuum tightness is 0.09MPa; dry under 80 ° of C after taking-up; repeatable operation like this 3 times, finally under the protection of high-purity argon gas under 600 ° of C pyroreaction 2 hours.

A kind of sapphire whisker of the present invention strengthens beryllium oxide ceramics based composites and preparation method thereof, is made up of following concrete steps:

(1) beryllium oxide, hafnium oxide are added in ball mill, ask as ball-milling medium using aluminum oxide, material ball ratio is 1:2, again divinyl, tertbutyl peroxide are added in the mixing solutions of ethanol and deionized water, adding after dissolving after polyvinylpyrrolidone, tripoly phosphate sodium STPP, polyvinyl alcohol and modified oxidized aluminum fiber stir is added in ball mill, ball milling 40 minutes;

(2) slurry that ball milling obtains is vacuumized, take out and within 5 minutes, add diacetone-acryloamide(DAA) in backward slurry and continue to stir, then slurry to be injected into after in laminated glass mould in vacuum drying oven under 80 ° of C dry 2 hours;

(3) by the wet base demoulding at room temperature seasoning in step (2) 2 days, then at 100 ° of C temperature, humidity under the condition of 60% dry 2 days, is distributed into plasma spraying powder conveyer in billet surface spraying evenly by remaining one-tenth;

(4) by the base substrate of step (3) at room temperature with the ramp to 200 of 3 ° of C/min ° C, again with the ramp to 600 of 1 ° of C/min ° C, constant temperature is positioned in vacuum sintering furnace after keeping 1 hour, sinters 3 hours, can obtain at the temperature of 1600 ° of C.

In the present embodiment, the performance index result of pottery is as follows:

Ultimate compression strength (MPa): >=680;

Fracture toughness property (Mpa/m ^1/2):>=4.8;

Flexural strength (MPa): >=633;

Thermal expansivity (10 ^-6/ K):>=6.9;

Impelling strength (KJm2): >=4.1.

Claims (2)

1. a sapphire whisker strengthens beryllium oxide ceramics based composites and preparation method thereof, it is characterized in that, be made up of the raw material of following weight part: Vanadium Pentoxide in FLAKES 3-5, modified oxidized aluminum fiber 10-15, beryllium oxide 70-80, hafnium oxide 7-9, titanium dioxide 4-6, tertbutyl peroxide 0.02-0.03, divinyl 4-6, polyvinylpyrrolidone 1-2, tripoly phosphate sodium STPP 1-2, diacetone-acryloamide(DAA) 0.1-0.3, polyvinyl alcohol 2-3, ethanol 20-30, deionized water 30-50;

The preparation method of described modified oxidized aluminum fiber is: sapphire whisker is soaked 1-2 hour in acetone, uses distilled water flushing 2-3 time, dry for standby after taking out, the ethanol mixing of the tetrabutyl titanate of 10-15 weight part and 150-180 weight part is added in the flask with magnetic stirring apparatus, by the deionized water of 2-3 weight part, the hydrochloric acid of 0.2-0.4 weight part and the ethanol of 2-5 weight part fully mix, slowly be added drop-wise in flask, add the molybdenum oxide powder of 2-4 weight part again, stir 30-40 minute, sapphire whisker for subsequent use is added in gel under vacuum tightness is 0.09-0.1MPa, floods 1-2 hour, dry under 70-80 ° of C after taking-up, repeatable operation like this 2-3 time, last under the protection of high-purity argon gas under 500-600 ° of C pyroreaction 1-2 hour.

2. according to claims 1, a kind of sapphire whisker strengthens beryllium oxide ceramics based composites and preparation method thereof, it is characterized in that, is made up of following concrete steps:

(1) beryllium oxide, hafnium oxide are added in ball mill, ask as ball-milling medium using aluminum oxide, material ball ratio is 1:2, again divinyl, tertbutyl peroxide are added in the mixing solutions of ethanol and deionized water, adding after dissolving after polyvinylpyrrolidone, tripoly phosphate sodium STPP, polyvinyl alcohol and modified oxidized aluminum fiber stir is added in ball mill, ball milling 20-40 minute;

(2) slurry that ball milling obtains is vacuumized, take out and within 2-5 minute, add diacetone-acryloamide(DAA) in backward slurry and continue to stir, then slurry to be injected into after in laminated glass mould in vacuum drying oven dry 1-2 hour under 60-80 ° of C;

(3) by the wet base demoulding at room temperature seasoning 1-2 days in step (2), then at 95-100 ° of C temperature, humidity is dry 1-2 days under the condition of 60-70%, remaining one-tenth is distributed into plasma spraying powder conveyer in billet surface spraying evenly;

(4) by the base substrate of step (3) at room temperature with the ramp to 200 of 3-5 ° of C/min ° C, again with the ramp to 600 of 1-2 ° of C/min ° C, constant temperature keeps being positioned in vacuum sintering furnace after 1-2 hour, sinters 3-4 hour, can obtain at the temperature of 1400-1600 ° of C.