CN104909742A - Alumina-fiber-enhanced hydroxyapatite ceramic-based composite material and preparation method thereof - Google Patents

Abstract

The invention discloses an alumina-fiber-enhanced hydroxyapatite 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, 70-80 parts of hydroxyapatite, 4-8 parts of acrylamide, 0.2-0.4 parts of N,N'-methylene bisacrylamide, 0.04-0.08 parts of ammonium persulfate, 2-3 parts of polyvinyl alcohol, 3-5 parts of aluminum alloy powder, 1-2 parts of sodium lignosulfonate, 10-15 parts of modified alumina fiber, 7-9 parts of niobium nitride, 20-30 parts of ethanol, and 40-60 parts of deionized water. According to the invention, the alumina fiber with an antioxidant treatment is added as an enhancement phase of ceramic, and has the characteristics of enhancing the toughness, mechanical performances, wear resistance, hardness and high-temperature resistance of ceramic. With the added aluminum alloy powder, a three-dimensional network structure can be formed with a blank under high temperature, such that ceramic toughness and fracture resistance can be enhanced. According to the invention, the application range of the hydroxyapatite ceramic-based composite material is expanded.

Description

A kind of sapphire whisker strengthens hydroxylapatite ceramic based composites and preparation method thereof

Technical field

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

Background technology

The deadly defect of stupalith is fragility, under external force, produce stress concentration at material surface or internal tiny crack tip, crack propagation forms surface energy with consumed energy, thus the propagation rate of crackle is extremely rapid, often just makes stupalith suffer catastrophic destruction in moment.When crack propagation runs into fiber, absorb energy by the disengaging of fiber and basal body interface, relax stress concentration; When few fibers fracture occurs under tension stress effect and extracts from matrix, also larger energy will be absorbed.Therefore, FRCMC is a kind of approach of effective solution stupalith fragility.FRCMC has the advantages such as high temperature resistant, wear-resisting, high temperature creep-resisting, thermal conductivity are low, thermal expansivity is low, chemerosiveness resistent is good, is widely used under resin base and metal matrix and even some ceramic matric composites can not meet the working condition of performance requriements.Hydroxyapatite chemical constitution is to the inorganic composition of human bone is closely similar and crystalline structure is also similar, there is after implant into body good biological activity and biocompatibility, to human non-toxic's side effect, thus hydroxyapatite porous ceramics is considered to the Surface active biological pottery most with application prospect, is subject to the close attention of people always.But hydroxyapatite at high temperature very easily decomposes, its sintering character also therefore non-constant, causes Mechanical Property of Ceramics very low, the breaking tenacity of cyano group Apatite Ceramic material prepared by single component and fracture toughness property very low, be difficult to meet clinical demand.

Summary of the invention

The object of this invention is to provide a kind of sapphire whisker and strengthen hydroxylapatite ceramic based composites and preparation method thereof, there is the breaking tenacity and fracture toughness property of improving hydroxylapatite ceramic material.

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

A kind of sapphire whisker strengthens hydroxylapatite ceramic based composites and preparation method thereof, be made up of the raw material of following weight part: hydroxyapatite 70-80, acrylamide 4-8, N, N '-methylene-bisacrylamide 0.2-0.4, ammonium persulphate 0.04-0.08, polyvinyl alcohol 2-3, Al alloy powder 3-5, sodium lignosulfonate 1-2, modified oxidized aluminum fiber 10-15, niobium nitride 7-9, ethanol 20-30, deionized water 40-60;

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 hydroxylapatite ceramic based composites and preparation method thereof, is made up of following concrete steps:

(1) hydroxyapatite, niobium nitride are added in ball mill, ask as ball-milling medium using aluminum oxide, material ball ratio is 1:2, again acrylamide, ammonium persulphate are added in the mixing solutions of ethanol and deionized water, adding after dissolving after polyvinyl alcohol, sodium lignosulfonate and modified oxidized aluminum fiber stir is added in ball mill, ball milling 20-40 minute;

(2) vacuumized by the slurry that ball milling obtains, take out and add N in backward slurry in 2-5 minute, N '-methylene-bisacrylamide continues 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 1000-1200 ° 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 Al alloy powder added at high temperature can form tridimensional network with base substrate, strengthen the toughness of pottery, improve breaking property, increase the use range of hydroxylapatite ceramic based composites.

specific embodiments

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

A kind of sapphire whisker strengthens hydroxylapatite ceramic based composites and preparation method thereof, be made up of the raw material of following weight part (kilogram): hydroxyapatite 75, acrylamide 7, N, N '-methylene-bisacrylamide 0.3, ammonium persulphate 0.05, polyvinyl alcohol 3, Al alloy powder 4, sodium lignosulfonate 2, modified oxidized aluminum fiber 13, niobium nitride 7, ethanol 30, deionized water 60;

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 hydroxylapatite ceramic based composites and preparation method thereof, is made up of following concrete steps:

(1) hydroxyapatite, niobium nitride are added in ball mill, ask as ball-milling medium using aluminum oxide, material ball ratio is 1:2, again acrylamide, ammonium persulphate are added in the mixing solutions of ethanol and deionized water, adding after dissolving after polyvinyl alcohol, sodium lignosulfonate and modified oxidized aluminum fiber stir is added in ball mill, ball milling 40 minutes;

(2) vacuumized by the slurry that ball milling obtains, take out and add N in backward slurry in 3 minutes, N '-methylene-bisacrylamide continues 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 65% 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 4 ° of C/min ° C, again with the ramp to 600 of 2 ° of C/min ° C, constant temperature is positioned in vacuum sintering furnace after keeping 2 hours, sinters 3 hours, can obtain at the temperature of 1200 ° of C.

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

Ultimate compression strength (MPa): >=850;

Fracture toughness property (Mpa/m ^1/2):>=6.8;

Flexural strength (MPa): >=442;

Thermal expansivity (10 ^-6/ K):>=5.8;

Impelling strength (KJm2): >=4.6.

Claims (2)

1. a sapphire whisker strengthens hydroxylapatite ceramic based composites and preparation method thereof, it is characterized in that, be made up of the raw material of following weight part: hydroxyapatite 70-80, acrylamide 4-8, N, N '-methylene-bisacrylamide 0.2-0.4, ammonium persulphate 0.04-0.08, polyvinyl alcohol 2-3, Al alloy powder 3-5, sodium lignosulfonate 1-2, modified oxidized aluminum fiber 10-15, niobium nitride 7-9, ethanol 20-30, deionized water 40-60;

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 hydroxylapatite ceramic based composites and preparation method thereof, it is characterized in that, is made up of following concrete steps:

(1) hydroxyapatite, niobium nitride are added in ball mill, ask as ball-milling medium using aluminum oxide, material ball ratio is 1:2, again acrylamide, ammonium persulphate are added in the mixing solutions of ethanol and deionized water, adding after dissolving after polyvinyl alcohol, sodium lignosulfonate and modified oxidized aluminum fiber stir is added in ball mill, ball milling 20-40 minute;

(2) vacuumized by the slurry that ball milling obtains, take out and add N in backward slurry in 2-5 minute, N '-methylene-bisacrylamide continues 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 1000-1200 ° of C.