CN106747400A - A kind of high-performance bioceramic material - Google Patents

A kind of high-performance bioceramic material Download PDF

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CN106747400A
CN106747400A CN201611029218.5A CN201611029218A CN106747400A CN 106747400 A CN106747400 A CN 106747400A CN 201611029218 A CN201611029218 A CN 201611029218A CN 106747400 A CN106747400 A CN 106747400A
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parts
reaction
performance
bioceramic material
temperature
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CN106747400B (en
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俞潮军
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Shaoxing Xinhui Biotechnology Co ltd
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Abstract

The invention discloses a kind of high-performance bioceramic material, its formula is as follows:30 50 parts of ammonium phosphate, 25 35 parts of calcium chloride, 8 14 parts of nano-calcium carbonate, 4 10 parts of silicon nitride, 10 16 parts of waterglass, 10 15 parts of aluminium chloride, 11 15 parts of tetrabutyl titanate, 34 parts of dispersant, 20 40 parts of deionized water, and there is provided preparation method.Preferably, bioactivity is higher for ceramic biocompatibility of the invention, with certain anti-inflammatory bactericidal property, meanwhile, possess good mechanical performance, biomaterial can be substituted as bone repair.

Description

A kind of high-performance bioceramic material
Technical field
The invention belongs to bone repair technical field, and in particular to a kind of high-performance bioceramic material.
Background technology
With the development of material science and technology, the particularity that biomaterial is repaired to body tissue, substituted and regenerated by it Can, have become one of important research direction of current biomedical sector.Biological hard tissue substitute material is earliest to use body Bone, Animal Bone, are developed into using stainless steel and plastics later, and because stainless steel has dissolved, corrosion and fatigue problem, plastics are deposited In stability difference and the problem of low intensity.The bottleneck of biomaterial development is thus resulted in, the appearance of bioceramic is improved existing The deficiency of alternative materials, because of its many advantages, therefore, bioceramic is provided with vast potential for future development.
Calcium phosphate ceramic (CPC) is the important species in biological active ceramic material, studies at present and is using most Hydroxyapatite (HA) and tricalcium phosphate (TCP).Calcium phosphate ceramic contains CaO and P2O5Two kinds of compositions, are to constitute human body hard tissue Important inorganic substances, implantation human body after, its surface with tissue can by the combination of key, reach completely it is affine.HA is biological Active ceramic is typical bioactive ceramics, can form chemical key and be combined with being organized on interface after implanting, with compared with Mechanical property high, resolvability is relatively low in human physiological environment.
The content of the invention
It is an object of the invention to provide a kind of high-performance bioceramic material, ceramic biocompatibility of the invention is preferable, Bioactivity is higher, with certain anti-inflammatory bactericidal property, meanwhile, possessing good mechanical performance, can be replaced as bone repair For biomaterial.
A kind of high-performance bioceramic material, its formula is as follows:
Ammonium phosphate 30-50 parts, calcium chloride 25-35 parts, nano-calcium carbonate 8-14 parts, silicon nitride 4-10 parts, waterglass 10-16 parts, Aluminium chloride 10-15 parts, tetrabutyl titanate 11-15 parts, dispersant 3-4 parts, deionized water 20-40 parts.
The dispersant uses polyvinylpyrrolidone.
Preferably, each group is divided into ammonium phosphate 35-45 parts, calcium chloride 28-33 parts, nano-calcium carbonate 9-11 parts, silicon nitride 6-8 parts, waterglass 13-15 parts, aluminium chloride 11-14 parts, tetrabutyl titanate 13-14 parts, dispersant 3-4 parts, deionized water 30-35 Part.
Preferably, each group is divided into 38 parts of ammonium phosphate, 31 parts of calcium chloride, 10 parts of nano-calcium carbonate, 7 parts of silicon nitride, water glass 14 parts of glass, 13 parts of aluminium chloride, 14 parts of tetrabutyl titanate, 4 parts of dispersant, 33 parts of deionized water.
The preparation method of the bioceramic material, its step is as follows:
Step 1, ammonium phosphate and calcium chloride are added into deionized water, are stirred, and form suspension;
Step 2, nano-calcium carbonate, silicon nitride, waterglass, aluminium chloride are sequentially added into deionized water, are stirred, and are formed Mixed serum,
Step 3, dispersant is added into slurries simultaneously with tetrabutyl titanate and is stirred, and forms forerunner's slurries;
Forerunner's slurries are carried out aerated reaction 3-5h by step 4;
Step 5, after aerated reaction terminates, be put into revolving instrument in carry out rotary evaporation formed thick slurry;
Step 6, secondary aerated reaction 2-4h is carried out by thick slurry, and then cold moudling carry out pressurized high-temperature reaction;
Step 7, after reaction terminates, natural cooling, you can obtain bioceramic material.
Mixing speed in the preparation method is 300-1000r/min.
Aerated reaction in the step 4 uses ammonia gas, and the gas flow rate of the aerated reaction is 15-30mL/ Min, the aerated reaction reacts for cyclic aeration, and the pressure of the aerated reaction is 0.5-1.2MPa, and the reaction temperature is Room temperature.
The temperature of the rotary evaporation reaction in the step 5 is 80-100 DEG C, and the pressure of the revolving evaporation is 0.2- 0.5MPa
The gas of the secondary aerated reaction in the step 6 is nitrogen, and the temperature of the secondary aerated reaction is 60-70 DEG C, institute The pressure for stating pressurized high-temperature reaction is 10-20MPa, and the temperature is 800-1000 DEG C.
Compared with prior art, the invention has the advantages that:
1st, preferably, bioactivity is higher for ceramic biocompatibility of the invention, with certain anti-inflammatory bactericidal property, meanwhile, tool Standby good mechanical performance, can substitute biomaterial as bone repair.
2nd, the present invention is using suspension and slurries as precursor liquid, is aerated, secondary aerated reaction, is possible to phosphoric acid DFP, carborundum, titanium source material tight are combined, with good combination effect, while biological living through the material after high temperature sintering Property is steadily improved, and mechanical strength is further improved.
3rd, the present invention to environment without particular/special requirement;Material purity is high, and strong mechanical property, it is easy to carry out industrial metaplasia Produce.
Specific embodiment
The present invention is described further with reference to embodiment:
Embodiment 1
A kind of high-performance bioceramic material, its formula is as follows:
30 parts of ammonium phosphate, 25 parts of calcium chloride, 8 parts of nano-calcium carbonate, 4 parts of silicon nitride, 10 parts of waterglass, 10 parts of aluminium chloride, metatitanic acid 11 parts of N-butyl, 3 parts of dispersant, 20 parts of deionized water.
The dispersant uses polyvinylpyrrolidone.
The preparation method of the bioceramic material, its step is as follows:
Step 1, ammonium phosphate and calcium chloride are added into deionized water, are stirred, and form suspension;
Step 2, nano-calcium carbonate, silicon nitride, waterglass, aluminium chloride are sequentially added into deionized water, are stirred, and are formed Mixed serum,
Step 3, dispersant is added into slurries simultaneously with tetrabutyl titanate and is stirred, and forms forerunner's slurries;
Forerunner's slurries are carried out aerated reaction 3h by step 4;
Step 5, after aerated reaction terminates, be put into revolving instrument in carry out rotary evaporation formed thick slurry;
Step 6, secondary aerated reaction 2h is carried out by thick slurry, and then cold moudling carry out pressurized high-temperature reaction;
Step 7, after reaction terminates, natural cooling, you can obtain bioceramic material.
Mixing speed in the preparation method is 300r/min.
Aerated reaction in the step 4 uses ammonia gas, and the gas flow rate of the aerated reaction is 15mL/min, institute Aerated reaction is stated for cyclic aeration reacts, the pressure of the aerated reaction is 0.5MPa, and the reaction temperature is room temperature.
The temperature of the rotary evaporation reaction in the step 5 is 80 DEG C, and the pressure of the revolving evaporation is 0.2MPa
The gas of the secondary aerated reaction in the step 6 is nitrogen, and the temperature of the secondary aerated reaction is 60 DEG C, described to add The pressure of super pressure-high temperature reaction is 10MPa, and the temperature is 800 DEG C.
Embodiment 2
A kind of high-performance bioceramic material, its formula is as follows:
50 parts of ammonium phosphate, 35 parts of calcium chloride, 14 parts of nano-calcium carbonate, 10 parts of silicon nitride, 16 parts of waterglass, 15 parts of aluminium chloride, titanium 15 parts of sour N-butyl, 4 parts of dispersant, 40 parts of deionized water.
The dispersant uses polyvinylpyrrolidone.
The preparation method of the bioceramic material, its step is as follows:
Step 1, ammonium phosphate and calcium chloride are added into deionized water, are stirred, and form suspension;
Step 2, nano-calcium carbonate, silicon nitride, waterglass, aluminium chloride are sequentially added into deionized water, are stirred, and are formed Mixed serum,
Step 3, dispersant is added into slurries simultaneously with tetrabutyl titanate and is stirred, and forms forerunner's slurries;
Forerunner's slurries are carried out aerated reaction 5h by step 4;
Step 5, after aerated reaction terminates, be put into revolving instrument in carry out rotary evaporation formed thick slurry;
Step 6, secondary aerated reaction 4h is carried out by thick slurry, and then cold moudling carry out pressurized high-temperature reaction;
Step 7, after reaction terminates, natural cooling, you can obtain bioceramic material.
Mixing speed in the preparation method is 1000r/min.
Aerated reaction in the step 4 uses ammonia gas, and the gas flow rate of the aerated reaction is 30mL/min, institute Aerated reaction is stated for cyclic aeration reacts, the pressure of the aerated reaction is 1.2MPa, and the reaction temperature is room temperature.
The temperature of the rotary evaporation reaction in the step 5 is 100 DEG C, and the pressure of the revolving evaporation is 0.5MPa
The gas of the secondary aerated reaction in the step 6 is nitrogen, and the temperature of the secondary aerated reaction is 70 DEG C, described to add The pressure of super pressure-high temperature reaction is 10-20MPa, and the temperature is 1000 DEG C.
Embodiment 3
A kind of high-performance bioceramic material, its formula is as follows:
35 parts of ammonium phosphate, 28 parts of calcium chloride, 9 parts of nano-calcium carbonate, 6 parts of silicon nitride, 13 parts of waterglass, 11 parts of aluminium chloride, metatitanic acid 13 parts of N-butyl, 3 parts of dispersant, 30 parts of deionized water.
The dispersant uses polyvinylpyrrolidone.
The preparation method of the bioceramic material, its step is as follows:
Step 1, ammonium phosphate and calcium chloride are added into deionized water, are stirred, and form suspension;
Step 2, nano-calcium carbonate, silicon nitride, waterglass, aluminium chloride are sequentially added into deionized water, are stirred, and are formed Mixed serum,
Step 3, dispersant is added into slurries simultaneously with tetrabutyl titanate and is stirred, and forms forerunner's slurries;
Forerunner's slurries are carried out aerated reaction 4h by step 4;
Step 5, after aerated reaction terminates, be put into revolving instrument in carry out rotary evaporation formed thick slurry;
Step 6, secondary aerated reaction 3h is carried out by thick slurry, and then cold moudling carry out pressurized high-temperature reaction;
Step 7, after reaction terminates, natural cooling, you can obtain bioceramic material.
Mixing speed in the preparation method is 500r/min.
Aerated reaction in the step 4 uses ammonia gas, and the gas flow rate of the aerated reaction is 18mL/min, institute Aerated reaction is stated for cyclic aeration reacts, the pressure of the aerated reaction is 0.7MPa, and the reaction temperature is room temperature.
The temperature of the rotary evaporation reaction in the step 5 is 90 DEG C, and the pressure of the revolving evaporation is 0.3MPa
The gas of the secondary aerated reaction in the step 6 is nitrogen, and the temperature of the secondary aerated reaction is 65 DEG C, described to add The pressure of super pressure-high temperature reaction is 13MPa, and the temperature is 900 DEG C.
Embodiment 4
A kind of high-performance bioceramic material, its formula is as follows:
45 parts of ammonium phosphate, 33 parts of calcium chloride, 11 parts of nano-calcium carbonate, 8 parts of silicon nitride, 15 parts of waterglass, 14 parts of aluminium chloride, metatitanic acid 14 parts of N-butyl, 4 parts of dispersant, 35 parts of deionized water.
The dispersant uses polyvinylpyrrolidone.
The preparation method of the bioceramic material, its step is as follows:
Step 1, ammonium phosphate and calcium chloride are added into deionized water, are stirred, and form suspension;
Step 2, nano-calcium carbonate, silicon nitride, waterglass, aluminium chloride are sequentially added into deionized water, are stirred, and are formed Mixed serum,
Step 3, dispersant is added into slurries simultaneously with tetrabutyl titanate and is stirred, and forms forerunner's slurries;
Forerunner's slurries are carried out aerated reaction 4h by step 4;
Step 5, after aerated reaction terminates, be put into revolving instrument in carry out rotary evaporation formed thick slurry;
Step 6, secondary aerated reaction 3h is carried out by thick slurry, and then cold moudling carry out pressurized high-temperature reaction;
Step 7, after reaction terminates, natural cooling, you can obtain bioceramic material.
Mixing speed in the preparation method is 700r/min.
Aerated reaction in the step 4 uses ammonia gas, and the gas flow rate of the aerated reaction is 20mL/min, institute Aerated reaction is stated for cyclic aeration reacts, the pressure of the aerated reaction is 0.7MPa, and the reaction temperature is room temperature.
The temperature of the rotary evaporation reaction in the step 5 is 85 DEG C, and the pressure of the revolving evaporation is 0.4MPa
The gas of the secondary aerated reaction in the step 6 is nitrogen, and the temperature of the secondary aerated reaction is 65 DEG C, described to add The pressure of super pressure-high temperature reaction is 15MPa, and the temperature is 850 DEG C.
Embodiment 5
A kind of high-performance bioceramic material, its formula is as follows:
38 parts of ammonium phosphate, 31 parts of calcium chloride, 10 parts of nano-calcium carbonate, 7 parts of silicon nitride, 14 parts of waterglass, 13 parts of aluminium chloride, metatitanic acid 14 parts of N-butyl, 4 parts of dispersant, 33 parts of deionized water.
The preparation method of the bioceramic material, its step is as follows:
Step 1, ammonium phosphate and calcium chloride are added into deionized water, are stirred, and form suspension;
Step 2, nano-calcium carbonate, silicon nitride, waterglass, aluminium chloride are sequentially added into deionized water, are stirred, and are formed Mixed serum,
Step 3, dispersant is added into slurries simultaneously with tetrabutyl titanate and is stirred, and forms forerunner's slurries;
Forerunner's slurries are carried out aerated reaction 3h by step 4;
Step 5, after aerated reaction terminates, be put into revolving instrument in carry out rotary evaporation formed thick slurry;
Step 6, secondary aerated reaction 3h is carried out by thick slurry, and then cold moudling carry out pressurized high-temperature reaction;
Step 7, after reaction terminates, natural cooling, you can obtain bioceramic material.
Mixing speed in the preparation method is 800r/min.
Aerated reaction in the step 4 uses ammonia gas, and the gas flow rate of the aerated reaction is 25mL/min, institute Aerated reaction is stated for cyclic aeration reacts, the pressure of the aerated reaction is 1.0 MPa, and the reaction temperature is room temperature.
The temperature of the rotary evaporation reaction in the step 5 is 95 DEG C, and the pressure of the revolving evaporation is 0.4MPa
The gas of the secondary aerated reaction in the step 6 is nitrogen, and the temperature of the secondary aerated reaction is 65 DEG C, described to add The pressure of super pressure-high temperature reaction is 18MPa, and the temperature is 850 DEG C.
The bioceramic material of embodiment 1-5 is tested
Embodiment Hardness(HV) Compressive strength MPa Bending strength MPa Toughness MPam0.5
Embodiment 1 840 1100 420 16
Embodiment 2 870 1300 430 15
Embodiment 3 850 1429 437 14
Embodiment 4 867 1234 459 15
Embodiment 5 890 1500 480 16
One embodiment of the invention is the foregoing is only, the side of the present invention, all use equivalents or equivalent transformation is not intended to limit The technical scheme that formula is obtained, all falls within protection scope of the present invention.

Claims (9)

1. a kind of high-performance bioceramic material, it is characterised in that its formula is as follows:
Ammonium phosphate 30-50 parts, calcium chloride 25-35 parts, nano-calcium carbonate 8-14 parts, silicon nitride 4-10 parts, waterglass 10-16 parts, Aluminium chloride 10-15 parts, tetrabutyl titanate 11-15 parts, dispersant 3-4 parts, deionized water 20-40 parts.
2. a kind of high-performance bioceramic material according to claim 1, it is characterised in that the dispersant uses poly- second Alkene pyrrolidone.
3. a kind of high-performance bioceramic material according to claim 1, it is characterised in that each group is divided into ammonium phosphate 35- 45 parts, calcium chloride 28-33 parts, nano-calcium carbonate 9-11 parts, silicon nitride 6-8 parts, waterglass 13-15 parts, aluminium chloride 11-14 parts, Tetrabutyl titanate 13-14 parts, dispersant 3-4 parts, deionized water 30-35 parts.
4. a kind of high-performance bioceramic material according to claim 3, it is characterised in that each group is divided into ammonium phosphate 38 Part, 31 parts of calcium chloride, 10 parts of nano-calcium carbonate, 7 parts of silicon nitride, 14 parts of waterglass, 13 parts of aluminium chloride, 14 parts of tetrabutyl titanate, 4 parts of dispersant, 33 parts of deionized water.
5. a kind of high-performance bioceramic material according to claim 1, it is characterised in that the bioceramic material Preparation method, its step is as follows:
Step 1, ammonium phosphate and calcium chloride are added into deionized water, are stirred, and form suspension;
Step 2, nano-calcium carbonate, silicon nitride, waterglass, aluminium chloride are sequentially added into deionized water, are stirred, and are formed Mixed serum,
Step 3, dispersant is added into slurries simultaneously with tetrabutyl titanate and is stirred, and forms forerunner's slurries;
Forerunner's slurries are carried out aerated reaction 3-5h by step 4;
Step 5, after aerated reaction terminates, be put into revolving instrument in carry out rotary evaporation formed thick slurry;
Step 6, secondary aerated reaction 2-4h is carried out by thick slurry, and then cold moudling carry out pressurized high-temperature reaction;
Step 7, after reaction terminates, natural cooling, you can obtain bioceramic material.
6. a kind of high-performance bioceramic material according to claim 5, it is characterised in that stirring in the preparation method Speed is mixed for 300-1000r/min.
7. a kind of high-performance bioceramic material according to claim 5, it is characterised in that the aeration in the step 4 Reaction uses ammonia gas, and the gas flow rate of the aerated reaction is 15-30mL/min, and the aerated reaction is that cyclic aeration is anti- Should, the pressure of the aerated reaction is 0.5-1.2MPa, and the reaction temperature is room temperature.
8. a kind of high-performance bioceramic material according to claim 5, it is characterised in that the rotation in the step 5 The temperature for evaporating reaction is 80-100 DEG C, and the pressure of the revolving evaporation is 0.2-0.5MPa.
9. a kind of high-performance bioceramic material according to claim 5, it is characterised in that secondary in the step 6 The gas of aerated reaction is nitrogen, and the temperature of the secondary aerated reaction is 60-70 DEG C, and the pressure of the pressurized high-temperature reaction is 10-20MPa, the temperature is 800-1000 DEG C.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101156964A (en) * 2007-11-08 2008-04-09 浙江大学 Similar bone biology medical material for slow releasing bioactivity factor as well as its preparing method
CN101880033A (en) * 2010-03-04 2010-11-10 上海纳米技术及应用国家工程研究中心有限公司 Method for preparing calcium phosphate for biological ceramics
CN104446432A (en) * 2014-11-10 2015-03-25 苏州维泰生物技术有限公司 Magnetic hydroxyapatite bioceramic and preparation method thereof
CN104744028A (en) * 2015-03-31 2015-07-01 苏州维泰生物技术有限公司 Tricalcium phosphate/silicon carbide composite biological ceramic and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101156964A (en) * 2007-11-08 2008-04-09 浙江大学 Similar bone biology medical material for slow releasing bioactivity factor as well as its preparing method
CN101880033A (en) * 2010-03-04 2010-11-10 上海纳米技术及应用国家工程研究中心有限公司 Method for preparing calcium phosphate for biological ceramics
CN104446432A (en) * 2014-11-10 2015-03-25 苏州维泰生物技术有限公司 Magnetic hydroxyapatite bioceramic and preparation method thereof
CN104744028A (en) * 2015-03-31 2015-07-01 苏州维泰生物技术有限公司 Tricalcium phosphate/silicon carbide composite biological ceramic and preparation method thereof

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