CN105967662A - Alumina/strontia biological ceramic and preparation method thereof - Google Patents

Alumina/strontia biological ceramic and preparation method thereof Download PDF

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CN105967662A
CN105967662A CN201610295180.XA CN201610295180A CN105967662A CN 105967662 A CN105967662 A CN 105967662A CN 201610295180 A CN201610295180 A CN 201610295180A CN 105967662 A CN105967662 A CN 105967662A
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oxide
bioceramic
aluminium oxide
strontium oxide
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王泽陆
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Abstract

The invention discloses an alumina/strontia biological ceramic and a preparation method thereof. The alumina/strontia biological ceramic comprises alumina, strontia, tricalcium phosphate, cerium molybdate, calcium citrate, silica, dimolybdenum boride, tin tetrafluoride, zinc oxide, chromium carbide, zirconium phosphate, zeolite powder, niobium pentoxide, ammonium hydroxide and water. The alumina/strontia biological ceramic has good mechanical properties. A test result shows that the alumina/strontia biological ceramic has bending strength of 534.9-588.6MPa and fracture toughness of 13.8-14.6MPa.m<1/2>. The preparation method solves the problems of low strength and toughness of a biological ceramic material. The biological ceramic has good wear resistance and good biocompatibility and has a good application prospect in the field of biomedical materials.

Description

A kind of aluminium oxide/strontium oxide bioceramic and preparation method thereof
Technical field
The invention belongs to bioceramic material field, be specifically related to a kind of aluminium oxide/strontium oxide bioceramic and preparation method thereof.
Background technology
Biomaterial is organism to be treated and replaced the tissue of damage, organ or promotes the material of its function.Along with the development of material science, life sciences and biotechnology, increasing biomaterial is used widely.Wherein it is most widely used with bioceramic material, polymer and composite thereof.
Bioceramic material and composite application thereof, update at biomaterial and account for critical role in hard tissue engineering.Bioceramic refers to the class ceramic material as biology undetermined or physiological function, directly acts on human body or the ceramic material such as the biology directly related with human body, medical, biochemistry.As bioceramic material, need following condition: biocompatibility, mechanical compatibility, antithrombotic, sterilising and good physics, chemical stability.
The kind of bioceramic is many and application wide, but the intensity of existing bioceramic material and toughness are relatively low, accordingly, it would be desirable to the mechanical property of bioceramic material is optimized improvement.
Summary of the invention
The above deficiency of prior art problem to be solved by this invention, it is provided that a kind of aluminium oxide/strontium oxide bioceramic and preparation method thereof.
In order to solve above-mentioned technical problem, the present invention is achieved by the following technical solutions:
The invention discloses a kind of aluminium oxide/strontium oxide bioceramic, be made up of the component of following parts by weight: aluminium oxide 25-60 part, strontium oxide 14-30 part, tricalcium phosphate 10-26 part, cerous molybdate 8-15 part, calcium citrate 8-25 part, silica 1 2-21 part, boronation two molybdenum 6-14 part, tin tetrafluoride 3-7 part, zinc oxide 2-8 part, chromium carbide 5-11 part, zirconium phosphate 8-15 part, zeolite powder 10-20 part, niobium pentaoxide 7-14 part, ammonia 5-13 part, water 80-120 part.
Preferably, described a kind of aluminium oxide/strontium oxide bioceramic, is made up of the component of following parts by weight: aluminium oxide 37-60 part, strontium oxide 18-30 part, tricalcium phosphate 15-26 part, cerous molybdate 10-15 part, calcium citrate 8-18 part, silica 1 4-21 part, boronation two molybdenum 9-14 part, tin tetrafluoride 3-6 part, zinc oxide 4-8 part, chromium carbide 5-9 part, zirconium phosphate 10-15 part, zeolite powder 14-20 part, niobium pentaoxide 9-14 part, ammonia 8-13 part, water 86-120 part.
Described a kind of aluminium oxide/strontium oxide bioceramic, is made up of the component of following parts by weight: aluminium oxide 46 parts, strontium oxide 21 parts, tricalcium phosphate 19 parts, cerous molybdate 12 parts, calcium citrate 9 parts, silica 18 parts, boronation two molybdenum 10 parts, tin tetrafluoride 5 parts, zinc oxide 6 parts, chromium carbide 7 parts, zirconium phosphate 14 parts, zeolite powder 16 parts, niobium pentaoxide 12 parts, ammonia 9 parts, 95 parts of water.
The present invention also provides for the preparation method of described aluminium oxide/strontium oxide bioceramic, including following preparation process:
(1) aluminium oxide, strontium oxide, tricalcium phosphate, calcium citrate and cerous molybdate are added in the there-necked flask filling water, 50-90 DEG C it is warming up to after stirring, then boronation two molybdenum, tin tetrafluoride, zinc oxide, chromium carbide, zirconium phosphate it are sequentially added into, stir 30-60 minute, add silicon dioxide, zeolite powder and niobium pentaoxide, stir 20-40 minute, it is eventually adding ammonia, adjust solution ph to stir 1-3 hour to 8-10, continuation, obtain mixed liquor;
(2) by above-mentioned mixed liquor after filtering, washing, it is placed in blast drier dried overnight rear grinding at 50-80 DEG C and makes powder;
(3) by above-mentioned powder pre-burning 2-5 hour at 300-500 DEG C, then naturally cool to room temperature, compressing after ground one-tenth powder obtain semi-finished product sample;
(4) above-mentioned semi-finished product sample being carried out vacuum-sintering, sintering temperature is 1100-1380 DEG C, cools to room temperature with the furnace after being incubated 1-5 hour, obtains described aluminium oxide/strontium oxide bioceramic.
Preferably, described step (1) is warming up to 65 DEG C, described adjustment pH value of solution to 9-10.
In described step (3), calcined temperature is 380 DEG C, and burn-in time is 3 hours.
In described step (4), sintering temperature is 1260 DEG C, is incubated 2 hours.
Owing to have employed above technical scheme, the present invention compared with prior art has the advantages that
By the present invention based on aluminium oxide, bioceramic material prepared by interpolation strontium oxide, cerous molybdate, zirconium phosphate, boronation two molybdenum and niobium pentaoxide has good mechanical property, test result shows: bending strength reaches 534.9-588.6MPa, and fracture toughness is 13.8-14.6 MPa m1/2, improve the intensity of traditional bioceramic material and toughness is low etc. not enough, additionally, the bioceramic material wearability of preparation is good, biocompatibility is good, has a good application prospect in biomedical materials field.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.Following example are used for illustrating the present invention, but are not limited to the scope of the present invention.
Embodiment 1
Aluminium oxide described in the present embodiment/strontium oxide bioceramic, is made up of the component of following parts by weight: aluminium oxide 25 parts, strontium oxide 14 parts, tricalcium phosphate 10 parts, cerous molybdate 8 parts, calcium citrate 8 parts, silica 12 parts, boronation two molybdenum 6 parts, tin tetrafluoride 3 parts, zinc oxide 2 parts, chromium carbide 5 parts, zirconium phosphate 8 parts, zeolite powder 10 parts, niobium pentaoxide 7 parts, ammonia 5 parts, 80 parts of water.
The preparation method of described aluminium oxide/strontium oxide bioceramic described in the present embodiment, including following preparation process:
(1) aluminium oxide, strontium oxide, tricalcium phosphate, calcium citrate and cerous molybdate are added in the there-necked flask filling water, 50 DEG C it are warming up to after stirring, then boronation two molybdenum, tin tetrafluoride, zinc oxide, chromium carbide, zirconium phosphate it are sequentially added into, stir 30 minutes, add silicon dioxide, zeolite powder and niobium pentaoxide, stir 20 minutes, it is eventually adding ammonia, adjustment solution ph, to 8, continues stirring 1 hour, obtains mixed liquor;
(2) by above-mentioned mixed liquor after filtering, washing, it is placed in blast drier dried overnight rear grinding at 50 DEG C and makes powder;
(3) by above-mentioned powder pre-burning 2 hours at 300 DEG C, then naturally cool to room temperature, compressing after ground one-tenth powder obtain semi-finished product sample;
(4) above-mentioned semi-finished product sample being carried out vacuum-sintering, sintering temperature is 1100 DEG C, cools to room temperature with the furnace, obtain described aluminium oxide/strontium oxide bioceramic after being incubated 1 hour.
Testing the bioceramic of preparation, its test result is: density is 4.37g cm-3, bending strength is 534.9 ± 10MPa, and fracture toughness is 14.4MPa m1/2
Embodiment 2
Aluminium oxide described in the present embodiment/strontium oxide bioceramic, is made up of the component of following parts by weight: aluminium oxide 60 parts, strontium oxide 30 parts, tricalcium phosphate 26 parts, cerous molybdate 15 parts, calcium citrate 25 parts, silicon dioxide 21 parts, boronation two molybdenum 14 parts, tin tetrafluoride 7 parts, zinc oxide 8 parts, chromium carbide 11 parts, zirconium phosphate 15 parts, zeolite powder 20 parts, niobium pentaoxide 14 parts, ammonia 13 parts, 120 parts of water.
The preparation method of described aluminium oxide/strontium oxide bioceramic described in the present embodiment, including following preparation process:
(1) aluminium oxide, strontium oxide, tricalcium phosphate, calcium citrate and cerous molybdate are added in the there-necked flask filling water, 90 DEG C it are warming up to after stirring, then boronation two molybdenum, tin tetrafluoride, zinc oxide, chromium carbide, zirconium phosphate it are sequentially added into, stir 60 minutes, add silicon dioxide, zeolite powder and niobium pentaoxide, stir 40 minutes, it is eventually adding ammonia, adjustment solution ph, to 10, continues stirring 3 hours, obtains mixed liquor;
(2) by above-mentioned mixed liquor after filtering, washing, it is placed in blast drier dried overnight rear grinding at 80 DEG C and makes powder;
(3) by above-mentioned powder pre-burning 5 hours at 500 DEG C, then naturally cool to room temperature, compressing after ground one-tenth powder obtain semi-finished product sample;
(4) above-mentioned semi-finished product sample being carried out vacuum-sintering, sintering temperature is 1380 DEG C, cools to room temperature with the furnace, obtain described aluminium oxide/strontium oxide bioceramic after being incubated 5 hours.
Testing the bioceramic of preparation, its test result is: density is 4.48g cm-3, bending strength is 582.6 ± 13MPa, and fracture toughness is 13.8MPa m1/2
Embodiment 3
Aluminium oxide described in the present embodiment/strontium oxide bioceramic, is made up of the component of following parts by weight: aluminium oxide 42 parts, strontium oxide 22 parts, tricalcium phosphate 18 parts, cerous molybdate 11 parts, calcium citrate 16 parts, silica 16 parts, boronation two molybdenum 10 parts, tin tetrafluoride 5 parts, zinc oxide 5 parts, chromium carbide 8 parts, zirconium phosphate 12 parts, zeolite powder 15 parts, niobium pentaoxide 10 parts, ammonia 9 parts, 100 parts of water.
The preparation method of described aluminium oxide/strontium oxide bioceramic described in the present embodiment, including following preparation process:
(1) aluminium oxide, strontium oxide, tricalcium phosphate, calcium citrate and cerous molybdate are added in the there-necked flask filling water, 70 DEG C it are warming up to after stirring, then boronation two molybdenum, tin tetrafluoride, zinc oxide, chromium carbide, zirconium phosphate it are sequentially added into, stir 45 minutes, add silicon dioxide, zeolite powder and niobium pentaoxide, stir 30 minutes, it is eventually adding ammonia, adjustment solution ph, to 9, continues stirring 2 hours, obtains mixed liquor;
(2) by above-mentioned mixed liquor after filtering, washing, it is placed in blast drier dried overnight rear grinding at 65 DEG C and makes powder;
(3) by above-mentioned powder pre-burning 3.5 hours at 400 DEG C, then naturally cool to room temperature, compressing after ground one-tenth powder obtain semi-finished product sample;
(4) above-mentioned semi-finished product sample being carried out vacuum-sintering, sintering temperature is 1240 DEG C, cools to room temperature with the furnace, obtain described aluminium oxide/strontium oxide bioceramic after being incubated 3 hours.
Testing the bioceramic of preparation, its test result is: density is 4.41g cm-3, bending strength is 563.5 ± 11MPa, and fracture toughness is 14.3MPa m1/2
Embodiment 4
Aluminium oxide described in the present embodiment/strontium oxide bioceramic, is made up of the component of following parts by weight: aluminium oxide 37 parts, strontium oxide 18 parts, tricalcium phosphate 15 parts, cerous molybdate 8-15 part, calcium citrate 18 parts, silica 14 parts, boronation two molybdenum 9 parts, tin tetrafluoride 6 parts, zinc oxide 4 parts, chromium carbide 9 parts, zirconium phosphate 10 parts, zeolite powder 14 parts, niobium pentaoxide 9 parts, ammonia 8 parts, 86 parts of water.
The preparation method of described aluminium oxide/strontium oxide bioceramic described in the present embodiment, including following preparation process:
(1) aluminium oxide, strontium oxide, tricalcium phosphate, calcium citrate and cerous molybdate are added in the there-necked flask filling water, 60 DEG C it are warming up to after stirring, then boronation two molybdenum, tin tetrafluoride, zinc oxide, chromium carbide, zirconium phosphate it are sequentially added into, stir 45 minutes, add silicon dioxide, zeolite powder and niobium pentaoxide, stir 35 minutes, it is eventually adding ammonia, adjustment solution ph, to 9.8, continues stirring 3 hours, obtains mixed liquor;
(2) by above-mentioned mixed liquor after filtering, washing, it is placed in blast drier dried overnight rear grinding at 70 DEG C and makes powder;
(3) by above-mentioned powder pre-burning 3 hours at 400 DEG C, then naturally cool to room temperature, compressing after ground one-tenth powder obtain semi-finished product sample;
(4) above-mentioned semi-finished product sample being carried out vacuum-sintering, sintering temperature is 1200 DEG C, cools to room temperature with the furnace, obtain described aluminium oxide/strontium oxide bioceramic after being incubated 2 hours.
Testing the bioceramic of preparation, its test result is: density is 4.45g cm-3, bending strength is 596.1 ± 10MPa, and fracture toughness is 14.8MPa m1/2
Embodiment 5
Aluminium oxide described in the present embodiment/strontium oxide bioceramic, is made up of the component of following parts by weight: aluminium oxide 46 parts, strontium oxide 21 parts, tricalcium phosphate 19 parts, cerous molybdate 12 parts, calcium citrate 9 parts, silica 18 parts, boronation two molybdenum 10 parts, tin tetrafluoride 5 parts, zinc oxide 6 parts, chromium carbide 7 parts, zirconium phosphate 14 parts, zeolite powder 16 parts, niobium pentaoxide 12 parts, ammonia 9 parts, 95 parts of water.
The preparation method of described aluminium oxide/strontium oxide bioceramic described in the present embodiment, including following preparation process:
(1) aluminium oxide, strontium oxide, tricalcium phosphate, calcium citrate and cerous molybdate are added in the there-necked flask filling water, 60 DEG C it are warming up to after stirring, then boronation two molybdenum, tin tetrafluoride, zinc oxide, chromium carbide, zirconium phosphate it are sequentially added into, stir 50 minutes, add silicon dioxide, zeolite powder and niobium pentaoxide, stir 25 minutes, it is eventually adding ammonia, adjustment solution ph, to 10.4, continues stirring 2 hours, obtains mixed liquor;
(2) by above-mentioned mixed liquor after filtering, washing, it is placed in blast drier dried overnight rear grinding at 65 DEG C and makes powder;
(3) by above-mentioned powder pre-burning 4 hours at 350 DEG C, then naturally cool to room temperature, compressing after ground one-tenth powder obtain semi-finished product sample;
(4) above-mentioned semi-finished product sample being carried out vacuum-sintering, sintering temperature is 1280 DEG C, cools to room temperature with the furnace, obtain described aluminium oxide/strontium oxide bioceramic after being incubated 2 hours.
Testing the bioceramic of preparation, its test result is: density is 4.52g cm-3, bending strength is 588.6 ± 11MPa, and fracture toughness is 14.6MPa m1/2
Comparative example 1
This comparative example is in place of the difference of embodiment 1: without strontium oxide, cerous molybdate and zirconium phosphate, and other components and preparation process reference example 1 prepare bioceramic.
Testing the bioceramic of preparation, its test result is: density is 4.22g cm-3, bending strength is 483.5 ± 11MPa, and fracture toughness is 13.7MPa m1/2
Comparative example 2
This comparative example is in place of the difference of embodiment 1: without boronation two molybdenum and niobium pentaoxide, and other components and preparation process reference example 1 prepare bioceramic.
Testing the bioceramic of preparation, its test result is: density is 4.17g cm-3, bending strength is 496.2 ± 12MPa, and fracture toughness is 14.1MPa m1/2

Claims (7)

1. aluminium oxide/strontium oxide bioceramic, it is characterized in that, be made up of the component of following parts by weight: aluminium oxide 25-60 part, strontium oxide 14-30 part, tricalcium phosphate 10-26 part, cerous molybdate 8-15 part, calcium citrate 8-25 part, silica 1 2-21 part, boronation two molybdenum 6-14 part, tin tetrafluoride 3-7 part, zinc oxide 2-8 part, chromium carbide 5-11 part, zirconium phosphate 8-15 part, zeolite powder 10-20 part, niobium pentaoxide 7-14 part, ammonia 5-13 part, water 80-120 part.
A kind of aluminium oxide/strontium oxide bioceramic the most according to claim 1, it is characterized in that, be made up of the component of following parts by weight: aluminium oxide 37-60 part, strontium oxide 18-30 part, tricalcium phosphate 15-26 part, cerous molybdate 10-15 part, calcium citrate 8-18 part, silica 1 4-21 part, boronation two molybdenum 9-14 part, tin tetrafluoride 3-6 part, zinc oxide 4-8 part, chromium carbide 5-9 part, zirconium phosphate 10-15 part, zeolite powder 14-20 part, niobium pentaoxide 9-14 part, ammonia 8-13 part, water 86-120 part.
A kind of aluminium oxide/strontium oxide bioceramic the most according to claim 1, it is characterized in that, be made up of the component of following parts by weight: aluminium oxide 46 parts, strontium oxide 21 parts, tricalcium phosphate 19 parts, cerous molybdate 12 parts, calcium citrate 9 parts, silica 18 parts, boronation two molybdenum 10 parts, tin tetrafluoride 5 parts, zinc oxide 6 parts, chromium carbide 7 parts, zirconium phosphate 14 parts, zeolite powder 16 parts, niobium pentaoxide 12 parts, ammonia 9 parts, 95 parts of water.
4. the preparation method of a kind of aluminium oxide/strontium oxide bioceramic as described in any one of claim 1-3, it is characterised in that include following preparation process:
(1) aluminium oxide, strontium oxide, tricalcium phosphate, calcium citrate and cerous molybdate are added in the there-necked flask filling water, 50-90 DEG C it is warming up to after stirring, then boronation two molybdenum, tin tetrafluoride, zinc oxide, chromium carbide, zirconium phosphate it are sequentially added into, stir 30-60 minute, add silicon dioxide, zeolite powder and niobium pentaoxide, stir 20-40 minute, it is eventually adding ammonia, adjust solution ph to stir 1-3 hour to 8-10, continuation, obtain mixed liquor;
(2) by above-mentioned mixed liquor after filtering, washing, it is placed in blast drier dried overnight rear grinding at 50-80 DEG C and makes powder;
(3) by above-mentioned powder pre-burning 2-5 hour at 300-500 DEG C, then naturally cool to room temperature, compressing after ground one-tenth powder obtain semi-finished product sample;
(4) above-mentioned semi-finished product sample being carried out vacuum-sintering, sintering temperature is 1100-1380 DEG C, cools to room temperature with the furnace after being incubated 1-5 hour, obtains described aluminium oxide/strontium oxide bioceramic.
The preparation method of a kind of aluminium oxide/strontium oxide bioceramic the most according to claim 4, it is characterised in that be warming up to 65 DEG C in described step (1), described adjustment pH value of solution to 9-10.
The preparation method of a kind of aluminium oxide/strontium oxide bioceramic the most according to claim 4, it is characterised in that in described step (3), calcined temperature is 380 DEG C, burn-in time is 3 hours.
The preparation method of a kind of aluminium oxide/strontium oxide bioceramic the most according to claim 4, it is characterised in that in described step (4), sintering temperature is 1260 DEG C, is incubated 2 hours.
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