CN107892561A - A kind of preparation method of high-strength degradable multiporous bioceramic - Google Patents
A kind of preparation method of high-strength degradable multiporous bioceramic Download PDFInfo
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Abstract
The present invention relates to technical field of biological medical material preparation, and in particular to a kind of preparation method of high-strength degradable multiporous bioceramic.Present invention self-control obtains light-burned calcium powder, it is mixed with bio-vitric powder, and mix polystyrene foam microballoon, soak paraffin wax liquation, obtain high solid phase slurry, it is hot-forming to obtain base substrate, base substrate is through dewaxing, pore-forming, sintering obtains descendent map, foam microshell leaves interconnected duct after burning mistake, and controlled by the contact tightness degree between foam microshell, biological substance and bioceramic contact area are bigger, more be advantageous to improve bioceramic intensity, the special construction that porous ceramics has, be advantageous to cell adherence growth, extrtacellular matrix deposition, nutrition and oxygen entrance etc., light-burned calcium powder inherently easily biological-degradable, so that porous bio-ceramic has preferable degradation property, had a extensive future in terms of bone induction and regeneration.
Description
Technical field
The present invention relates to technical field of biological medical material preparation, and in particular to a kind of high-strength degradable multiporous bioceramic
Preparation method.
Background technology
Bioceramic refers to be used as specific biology or a kind of ceramic material of physiological function, that is, be directly used in human body or with
The ceramic material of directly related biological, the medical, biochemistry of human body etc..As bioceramic material, it is necessary to possess following bar
Part：Biocompatibility, mechanical compatibility, there is an excellent compatibility with biological tissue, antithrombotic is sterilising and have good thing
Reason, chemical stability.Bioceramic, can be with biological tissue's table such as cell due to good biocompatibility and osteoconductive
Reveal good compatibility, therefore, be widely used in orthopaedics, dentistry, plastic surgery, department of cardiovascular surgery, oral surgery and general
Logical surgery etc..
Cranial defect caused by fracture, osteopathy and bone cyst etc. is always one of problem of field of orthopaedics.For there occurs disease
The bone tissue for becoming or damaging, can use natural bone, and such as androgynous bone, homogeneous allogenic bone, bone- xenograft or artificial bone is repaired.But
It is that androgynous Bone Defect Repari method can cause secondary insult to patient；The potential danger of transmission be present in homogeneous allogenic bone and bone- xenograft；
And there is potential danger in artificial bone.Important component of the calcium phosphate biological ceramic material as human body hard tissue, has
Good biocompatibility and bioactivity, chemical bond can be formed with bone tissue, be the preferable material of bone tissue engineering scaffold
Material.But the porosity of porous material can have a strong impact on the mechanical property of material when reaching application requirement, and ceramics belong in itself
Fragile material, limit its application in Bone Defect Repari.
The toughness of ceramic material can mutually improve the mechanical property of porous material with intensity by compound or addition toughness reinforcing
Energy and toughness, nano level enhancing grain, whisker or and other materials are mainly added for calcium phosphate bioactive ceramic toughening
It is compound.But there can be a bioactivity of support and the defects of mechanical property is unable to perfect adaptation.
Therefore, developing a kind of bioceramic that can solve the problem that above-mentioned performance issue is highly desirable.
The content of the invention
Present invention mainly solves technical problem, can reduce bioceramic mechanical strength for the hole of porous bio-ceramic
And degradation property it is poor the defects of, there is provided a kind of preparation method of high-strength degradable multiporous bioceramic.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of high-strength degradable multiporous bioceramic, it is characterised in that specifically preparation process is：
（1）Count in parts by weight, take 80~90 parts of Dicalcium Phosphates, 30~40 parts of calcium carbonate to mix, be placed in mortar
Grinding, sieving obtain sieving mixing calcium powder, sieving mixing calcium powder are placed in resistance furnace, power-up procedure heating, insulation reaction, from
After being so cooled to room temperature, phosphoric acid calcium powder is obtained；
（2）Phosphoric acid calcium powder is taken out from resistance furnace, ground, sieving obtains the phosphoric acid calcium powder that sieves, and sieving phosphoric acid calcium powder is placed in
In resistance furnace, power-up procedure heating, high temperature sintering, after naturally cooling to room temperature, light-burned calcium powder is obtained；
（3）Count in parts by weight, by 20~30 parts of calcium carbonate, 50~60 parts of ammonium dihydrogen phosphates, 5~10 parts of light magnesium carbonates, 20
The mixing of~25 parts of sodium carbonate, grind 30~40min, sieving obtains mixed-powder, added into mixed-powder 60~70 parts go from
Sub- water, is placed in high speed dispersor, scattered at a high speed, obtains glass paste；
（4）Glass paste is put into vavuum pump and is vented, glass paste is placed in cucurbit, heat temperature raising, distillation, is steamed
Dry glass gels, glass gels are put into crucible, then crucible is moved into resistance furnace, and be powered heating, after heat preservation sintering, are taken
Go out crucible, with water quenching cold crucible, obtain calcium phosphorus system bio-vitric；
（5）Above-mentioned calcium phosphorus system bio-vitric is ground, sieving obtains bio-vitric powder, counts in parts by weight, by 40~50 parts
Light-burned calcium powder, 30~40 parts of bio-vitric powder are placed in ball milling in ball grinder, and 20~25 parts of palm oils are added into ball grinder, after
Continuous ball milling, discharging, obtain being surface-treated powder, by 20~30 parts of polystyrene foam microballoons, 30~40 parts of surface treatment powders
It is put into paraffin wax liquation, obtains high solid phase slurry；
（6）Above-mentioned high solid phase slurry is poured into the hot die-casting molding machine mould of preheating, it is hot-forming, it is naturally cooling to room temperature
Afterwards, the demoulding obtains base substrate, base substrate is placed in the carbon firing stove with paraffin adsorbent, heat temperature raising, insulation dewaxing, continues to rise
Temperature, pore-forming is incubated, then heated up, sintered, obtain high-strength degradable multiporous bioceramic.
Step（1）The described mixing time is 10~15min, and milling time is 45~55min, and power-up procedure heats up
Temperature is 930~960 DEG C afterwards, and the insulation reaction time is 4~5h.
Step（2）Described milling time is 30~35min, and specification of sieving is 200 mesh, temperature after power-up procedure heating
For 1000~1050 DEG C, heating rate is 100 DEG C/min, and the high temperature sintering time is 3~4h.
Step（3）Described milling time is 30~40min, and specification of sieving is 100 mesh, and high speed dispersor rotating speed is
3000~4000r/min, high speed jitter time are 12~15min.
Step（4）Described to control vacuum be 60~100Pa, and temperature is 100~110 DEG C after cucurbit heat temperature raising,
Distillation time is 3~4h, and temperature is 1200~1300 DEG C after the heating that is powered, and the heat preservation sintering time is 2~3h,
With 45~50min of water quenching cold crucible.
Step（5）Described 30~40min of milling time, Ball-milling Time are 2~3h, and continuation Ball-milling Time is 4~6h, are gathered
The particle diameter of styrenic foams microballoon is 400~600 μm, and the solid masses content of paraffin wax liquation is 50%, paraffin wax liquation
Temperature be 80~90 DEG C.
Step（6）Described preheating temperature is 50~60 DEG C, and the hot-forming time is 2~3h, controls hot press molding pressure
For 0.3~0.5MPa, temperature is 200~250 DEG C after carbon firing stove heat temperature raising, and the dewaxing time is 1~2h,
Temperature is 300~350 DEG C after continuing heating, and the insulation pore-forming time is 1~2h, then temperature is 800~900 DEG C after heating up,
Sintering time is 2~3h.
The beneficial effects of the invention are as follows：
（1）Light-burned calcium powder is made with solid reaction process in the present invention, and light-burned calcium powder mixes with bio-vitric powder, mixes polystyrene
Foam microshell, paraffin wax liquation is soaked, obtains high solid phase slurry, high solid phase slurry obtains base substrate, base substrate through hot die-casting molding
Descendent map is obtained through dewaxing, pore-forming, sintering, polystyrene foam microballoon of the invention leaves after burning mistake in contact position
Interconnected duct, duct can be controlled by the contact compactness degree between organic foam small-sphere, thus can be controlled
Obtain the three-dimensional porous structure that macropore, aperture and micropore are combined, three-dimensional porous structure it is connective good, bioceramic is porous
Middle biological substance filling will be fuller, and biological substance and bioceramic contact area are bigger, so as to be advantageous to improve biological pottery
Porcelain intensity；
（2）The porous ceramics of the present invention has a uniform, controllable three-dimensional communication three-dimensional porous structure, porosity can reach 80% with
On, there is high specific surface area, and be that macropore, aperture and micropore are combined, this structure can provide roomy surface area and
Space, cell adherence growth, extrtacellular matrix deposition, nutrition and oxygen entrance and metabolite discharge are beneficial to, is also had
Grown into beneficial to blood vessel and nerve, osteoclast development secretory activity will be vigorous, and osteoclast passes through secreting acidic material so that
The microcell being in contact with it is in faintly acid feature, and this degraded to calcium microcosmic salt and bio-vitric plays positive role, and of the invention is light
Burn in calcium powder and be rich in bata-tricalcium phosphate, bata-tricalcium phosphate inherently easily biological-degradable, so that porous bio-ceramic has preferably
Degradation property, had a extensive future in terms of bone induction and regeneration.
Embodiment
Count in parts by weight, take 80~90 parts of Dicalcium Phosphates, 30~40 parts of calcium carbonate to mix 10~15min,
45~55min of grinding in mortar is placed in, 200 mesh sieves is crossed and obtains sieving mixing calcium powder, sieving mixing calcium powder is placed in resistance furnace,
It is powered and is warming up to 930~960 DEG C with 100 DEG C/min rate program, 4~5h of insulation reaction, after naturally cooling to room temperature, obtains
To phosphoric acid calcium powder；Phosphoric acid calcium powder is taken out from resistance furnace, grinds 30~35min, 200 mesh sieves is crossed and obtains the phosphoric acid calcium powder that sieves,
Sieving phosphoric acid calcium powder is placed in resistance furnace, power-up procedure is warming up to 1000~1050 DEG C, 3~4h of high temperature sintering, natural cooling
To room temperature, light-burned calcium powder is obtained；Count in parts by weight, by 20~30 parts of calcium carbonate, 50~60 parts of ammonium dihydrogen phosphates, 5~10
Part light magnesium carbonate, 20~25 parts of sodium carbonate mixing, grind 30~40min, sieving obtains 100 mesh mixed-powders, to mixed powder
60~70 parts of deionized waters are added in end, are placed in high speed dispersor with 3000~4000r/min rotating speed, at a high speed scattered 12~
15min, obtain glass paste；Glass paste is put into vavuum pump and is vented, it is 60~100Pa to control vacuum, by glass paste
Material is placed in cucurbit, is heated to 100~110 DEG C, is distilled 3~4h, the glass gels being evaporated, glass gels is put
Enter in crucible, then crucible is moved into resistance furnace, energization is warming up to 1200~1300 DEG C, after 2~3h of heat preservation sintering, takes out earthenware
Crucible, with 0~4 DEG C of water quenching 45~50min of cold crucible, obtain calcium phosphorus system bio-vitric；Above-mentioned calcium phosphorus system bio-vitric is ground 30
~40min, cross 200 mesh sieves and obtain bio-vitric powder, count in parts by weight, by 40~50 parts of light-burned calcium powders, 30~40 parts of lifes
Thing glass powder is placed in 2~3h of ball milling in ball grinder, and 20~25 parts of palm oils are added into ball grinder, continues 4~6h of ball milling, goes out
Material, obtain being surface-treated powder, by polystyrene foam microballoon of 20~30 parts of particle diameters for 400~600 μm, 30~40 parts of surfaces
Processing powder is put into the paraffin wax liquation that the solid masses content that temperature is 80~90 DEG C is 50%, obtains high solid phase slurry；
Above-mentioned high solid phase slurry is poured into the hot die-casting molding machine mould that preheating temperature is 50~60 DEG C, hot-forming 2~3h, control
Hot press molding pressure is 0.3~0.5MPa, and after being naturally cooling to room temperature, the demoulding obtains base substrate, and base substrate is placed in and inhaled with paraffin
In attached dose of carbon firing stove, 200~250 DEG C are heated to, insulation 1~2h of dewaxing, 300~350 DEG C is continuously heating to, is incubated into
1~2h of hole, then 800~900 DEG C are warming up to, 2~3h is sintered, obtains high-strength degradable multiporous bioceramic.
Example 1
Count in parts by weight, take 80 parts of Dicalcium Phosphates, 30 parts of calcium carbonate to mix 10min, be placed in mortar and grind
45min, cross 200 mesh sieves and obtain sieving mixing calcium powder, sieving mixing calcium powder is placed in resistance furnace, is powered and with 100 DEG C/min
Rate program be warming up to 930 DEG C, insulation reaction 4h, after naturally cooling to room temperature, obtain phosphoric acid calcium powder；By phosphoric acid calcium powder from electricity
Taken out in resistance stove, grind 30min, crossed 200 mesh sieves and obtain the phosphoric acid calcium powder that sieves, sieving phosphoric acid calcium powder is placed in resistance furnace, led to
Electric temperature programming after naturally cooling to room temperature, obtains light-burned calcium powder to 1000 DEG C, high temperature sintering 3h；Count in parts by weight, by 20
Part calcium carbonate, 50 parts of ammonium dihydrogen phosphates, 5 parts of light magnesium carbonates, 20 parts of sodium carbonate mixing, grind 30min, sieving obtains 100 mesh
Mixed-powder, 60 parts of deionized waters are added into mixed-powder, be placed in high speed dispersor with 3000r/min rotating speed, high speed
Scattered 12min, obtains glass paste；Glass paste is put into vavuum pump and is vented, it is 60Pa to control vacuum, by glass paste
It is placed in cucurbit, is heated to 100 DEG C, distills 3h, the glass gels being evaporated, glass gels are put into crucible,
Crucible is moved into resistance furnace again, energization is warming up to 1200 DEG C, after heat preservation sintering 2h, crucible is taken out, with 0 DEG C of water quenching cold crucible
45min, obtain calcium phosphorus system bio-vitric；Above-mentioned calcium phosphorus system bio-vitric is ground into 30min, 200 mesh sieves is crossed and obtains bio-vitric
Powder, count in parts by weight, 40 parts of light-burned calcium powders, 30 parts of bio-vitric powder are placed in ball milling 2h in ball grinder, to ball grinder
20 parts of palm oils of middle addition, continue ball milling 4h, discharging, obtain being surface-treated powder, by the polystyrene that 20 parts of particle diameters are 400 μm
Foam microshell, 30 parts of surface treatment powders are put into the paraffin wax liquation that the solid masses content that temperature is 80 DEG C is 50%, are obtained
To high solid phase slurry；Above-mentioned high solid phase slurry is poured into the hot die-casting molding machine mould that preheating temperature is 50 DEG C, it is hot-forming
2h, it is 0.3MPa to control hot press molding pressure, and after being naturally cooling to room temperature, the demoulding obtains base substrate, and base substrate is placed in paraffin
In the carbon firing stove of adsorbent, 200 DEG C are heated to, insulation dewaxing 1h, 300 DEG C is continuously heating to, is incubated pore-forming 1h, then heat up
To 800 DEG C, 2h is sintered, obtains high-strength degradable multiporous bioceramic.
Example 2
Count in parts by weight, take 85 parts of Dicalcium Phosphates, 35 parts of calcium carbonate to mix 13min, be placed in mortar and grind
50min, cross 200 mesh sieves and obtain sieving mixing calcium powder, sieving mixing calcium powder is placed in resistance furnace, is powered and with 100 DEG C/min
Rate program be warming up to 945 DEG C, insulation reaction 4.5h, after naturally cooling to room temperature, obtain phosphoric acid calcium powder；By phosphoric acid calcium powder from
Taken out in resistance furnace, grind 33min, crossed 200 mesh sieves and obtain the phosphoric acid calcium powder that sieves, sieving phosphoric acid calcium powder is placed in resistance furnace,
Power-up procedure is warming up to 1025 DEG C, high temperature sintering 3.5h, after naturally cooling to room temperature, obtains light-burned calcium powder；Count in parts by weight,
25 parts of calcium carbonate, 55 parts of ammonium dihydrogen phosphates, 7 parts of light magnesium carbonates, 23 parts of sodium carbonate are mixed, grind 35min, sieving obtains
100 mesh mixed-powders, 65 parts of deionized waters are added into mixed-powder, are placed in high speed dispersor with 3500r/min rotating speed,
Scattered 13min at a high speed, obtains glass paste；Glass paste is put into vavuum pump and is vented, it is 80Pa to control vacuum, by glass
Slurry is placed in cucurbit, is heated to 105 DEG C, is distilled 3.5h, the glass gels being evaporated, glass gels is put into earthenware
In crucible, then crucible moved into resistance furnace, energization is warming up to 1250 DEG C, after heat preservation sintering 2.5h, crucible is taken out, with 2 DEG C of water quenchings
Cold crucible 47min, obtain calcium phosphorus system bio-vitric；Above-mentioned calcium phosphorus system bio-vitric is ground into 35min, 200 mesh sieves is crossed and is given birth to
Thing glass powder, is counted in parts by weight, and 45 parts of light-burned calcium powders, 35 parts of bio-vitric powder are placed in into ball milling 2.5h in ball grinder,
23 parts of palm oils are added into ball grinder, continues ball milling 5h, discharging, obtains being surface-treated powder, be 500 μm by 25 parts of particle diameters
Polystyrene foam microballoon, 35 parts of surface treatment powders are put into the paraffin wax that the solid masses content that temperature is 85 DEG C is 50%
In liquation, high solid phase slurry is obtained；Above-mentioned high solid phase slurry is poured into the hot die-casting molding machine mould that preheating temperature is 55 DEG C,
Hot-forming 2.5h, it is 0.4MPa to control hot press molding pressure, and after being naturally cooling to room temperature, the demoulding obtains base substrate, and base substrate is put
In the carbon firing stove with paraffin adsorbent, 225 DEG C are heated to, insulation dewaxing 1.5h, is continuously heating to 325 DEG C, insulation
Pore-forming 1.5h, then 850 DEG C are warming up to, 2.5h is sintered, obtains high-strength degradable multiporous bioceramic.
Example 3
Count in parts by weight, take 90 parts of Dicalcium Phosphates, 40 parts of calcium carbonate to mix 15min, be placed in mortar and grind
55min, cross 200 mesh sieves and obtain sieving mixing calcium powder, sieving mixing calcium powder is placed in resistance furnace, is powered and with 100 DEG C/min
Rate program be warming up to 960 DEG C, insulation reaction 5h, after naturally cooling to room temperature, obtain phosphoric acid calcium powder；By phosphoric acid calcium powder from electricity
Taken out in resistance stove, grind 35min, crossed 200 mesh sieves and obtain the phosphoric acid calcium powder that sieves, sieving phosphoric acid calcium powder is placed in resistance furnace, led to
Electric temperature programming after naturally cooling to room temperature, obtains light-burned calcium powder to 1050 DEG C, high temperature sintering 4h；Count in parts by weight, by 30
Part calcium carbonate, 60 parts of ammonium dihydrogen phosphates, 10 parts of light magnesium carbonates, 25 parts of sodium carbonate mixing, grind 40min, sieving obtains 100 mesh
Mixed-powder, 70 parts of deionized waters are added into mixed-powder, be placed in high speed dispersor with 4000r/min rotating speed, high speed
Scattered 15min, obtains glass paste；Glass paste is put into vavuum pump and is vented, it is 100Pa to control vacuum, by glass paste
Material is placed in cucurbit, is heated to 110 DEG C, is distilled 4h, the glass gels being evaporated, glass gels is put into crucible
In, then crucible moved into resistance furnace, energization is warming up to 1300 DEG C, after heat preservation sintering 3h, crucible is taken out, with 4 DEG C of cold earthenwares of water quenching
Crucible 50min, obtain calcium phosphorus system bio-vitric；Above-mentioned calcium phosphorus system bio-vitric is ground into 40min, 200 mesh sieves is crossed and obtains biological glass
Glass powder, is counted in parts by weight, 50 parts of light-burned calcium powders, 40 parts of bio-vitric powder is placed in into ball milling 3h in ball grinder, to ball milling
25 parts of palm oils are added in tank, continues ball milling 6h, discharging, obtains being surface-treated powder, by the polyphenyl second that 30 parts of particle diameters are 600 μm
Alkene foam microshell, 40 parts of surface treatment powders are put into the paraffin wax liquation that the solid masses content that temperature is 90 DEG C is 50%,
Obtain high solid phase slurry；Above-mentioned high solid phase slurry is poured into the hot die-casting molding machine mould that preheating temperature is 60 DEG C, be hot pressed into
Type 3h, it is 0.5MPa to control hot press molding pressure, and after being naturally cooling to room temperature, the demoulding obtains base substrate, and base substrate is placed in stone
In the carbon firing stove of wax adsorbent, 250 DEG C are heated to, insulation dewaxing 2h, 350 DEG C is continuously heating to, is incubated pore-forming 2h, then rise
Temperature sinters 3h, obtains high-strength degradable multiporous bioceramic to 900 DEG C.
The porous bio-ceramic that comparative example is produced with company of Suzhou City is as a comparison case to produced by the present invention high-strength
Porous bio-ceramic in degradable multiporous bioceramic and comparative example is detected, and testing result is as shown in table 1：1st, test
Method
Mechanics Performance Testing is tested using electronic type universal mechanics machine.
Degradation experiment：Precise sample（Example 1 produced by the present invention）Initial weight be designated as W0, by sample and phosphoric acid
Buffer solution（PBS）Ratio according to 1g/30mL is placed in closed polyethylene pipe, is vibrated in 37 DEG C of constant temperature oscillators, vibration
Speed is 50r/min.PBS solution successively is changed weekly.The pH value of PBS solution is measured behind 7,14,21 and 28d and takes out sample
Product, net, weighing example weight W after drying is washed with deionized water1, material degradation weight-loss ratio is calculated by formula.Before sample degradation
With degraded 4 weeks after material drying surface metal spraying, with SEM observe surface topography change.According to identical side
Method, example 2, example 3 and comparative example are tested.
Table 1
| Test event | Example 1 | Example 2 | Example 3 | Comparative example |
| Compression strength（MPa） | 419 | 428 | 435 | 246 |
| Bending strength（MPa） | 434 | 451 | 462 | 242 |
| Modulus of elasticity（GPa） | 25 | 27 | 31 | 14 |
| Biological degradation rate（%） | 85.1 | 85.5 | 86.2 | 65.3 |
It can be seen from data in table 1, high-strength degradable multiporous bioceramic produced by the present invention, excellent in mechanical performance, biology drop
Xie Xingqiang, cost is cheap and environmentally friendly, harmless to the human body, has wide prospect of the application.
Claims (7)
1. a kind of preparation method of high-strength degradable multiporous bioceramic, it is characterised in that specifically preparation process is：
（1）Count in parts by weight, take 80~90 parts of Dicalcium Phosphates, 30~40 parts of calcium carbonate to mix, be placed in mortar
Grinding, sieving obtain sieving mixing calcium powder, sieving mixing calcium powder are placed in resistance furnace, power-up procedure heating, insulation reaction, from
After being so cooled to room temperature, phosphoric acid calcium powder is obtained；
（2）Phosphoric acid calcium powder is taken out from resistance furnace, ground, sieving obtains the phosphoric acid calcium powder that sieves, and sieving phosphoric acid calcium powder is placed in
In resistance furnace, power-up procedure heating, high temperature sintering, after naturally cooling to room temperature, light-burned calcium powder is obtained；
（3）Count in parts by weight, by 20~30 parts of calcium carbonate, 50~60 parts of ammonium dihydrogen phosphates, 5~10 parts of light magnesium carbonates, 20
The mixing of~25 parts of sodium carbonate, grind 30~40min, sieving obtains mixed-powder, added into mixed-powder 60~70 parts go from
Sub- water, is placed in high speed dispersor, scattered at a high speed, obtains glass paste；
（4）Glass paste is put into vavuum pump and is vented, glass paste is placed in cucurbit, heat temperature raising, distillation, is obtained
The glass gels being evaporated, glass gels are put into crucible, then crucible is moved into resistance furnace, and be powered heating, after heat preservation sintering,
Crucible is taken out, with water quenching cold crucible, obtains calcium phosphorus system bio-vitric；
（5）Above-mentioned calcium phosphorus system bio-vitric is ground, sieving obtains bio-vitric powder, counts in parts by weight, by 40~50 parts
Light-burned calcium powder, 30~40 parts of bio-vitric powder are placed in ball milling in ball grinder, and 20~25 parts of palm oils are added into ball grinder, after
Continuous ball milling, discharging, obtain being surface-treated powder, by 20~30 parts of polystyrene foam microballoons, 30~40 parts of surface treatment powders
It is put into paraffin wax liquation, obtains high solid phase slurry；
（6）Above-mentioned high solid phase slurry is poured into the hot die-casting molding machine mould of preheating, it is hot-forming, it is naturally cooling to room temperature
Afterwards, the demoulding obtains base substrate, base substrate is placed in the carbon firing stove with paraffin adsorbent, heat temperature raising, insulation dewaxing, continues to rise
Temperature, pore-forming is incubated, then heated up, sintered, obtain high-strength degradable multiporous bioceramic.
A kind of 2. preparation method of high-strength degradable multiporous bioceramic according to claim 1, it is characterised in that：
Step（1）The described mixing time is 10~15min, and milling time is 45~55min, warm after power-up procedure heating
Spend for 930~960 DEG C, the insulation reaction time is 4~5h.
A kind of 3. preparation method of high-strength degradable multiporous bioceramic according to claim 1, it is characterised in that：
Step（2）Described milling time is 30~35min, and specification of sieving is 200 mesh, and temperature is after power-up procedure heating
1000~1050 DEG C, heating rate is 100 DEG C/min, and the high temperature sintering time is 3~4h.
A kind of 4. preparation method of high-strength degradable multiporous bioceramic according to claim 1, it is characterised in that：
Step（3）Described milling time is 30~40min, and specification of sieving is 100 mesh, high speed dispersor rotating speed is 3000~
4000r/min, high speed jitter time are 12~15min.
A kind of 5. preparation method of high-strength degradable multiporous bioceramic according to claim 1, it is characterised in that：
Step（4）Described to control vacuum be 60~100Pa, and temperature is 100~110 DEG C after cucurbit heat temperature raising, distillation
Time is 3~4h, and temperature is 1200~1300 DEG C after the heating that is powered, and the heat preservation sintering time is 2~3h,
It is 45~50min with the water quenching cold crucible time.
A kind of 6. preparation method of high-strength degradable multiporous bioceramic according to claim 1, it is characterised in that：
Step（5）Described 30~40min of milling time, Ball-milling Time are 2~3h, and continuation Ball-milling Time is 4~6h, polyphenyl second
The particle diameter of alkene foam microshell is 400~600 μm, and the solid masses content of paraffin wax liquation is 50%, the temperature of paraffin wax liquation
Spend for 80~90 DEG C.
A kind of 7. preparation method of high-strength degradable multiporous bioceramic according to claim 1, it is characterised in that：
Step（6）Described preheating temperature is 50~60 DEG C, and the hot-forming time is 2~3h, and it is 0.3 to control hot press molding pressure
~0.5MPa, temperature is 200~250 DEG C after carbon firing stove heat temperature raising, and the dewaxing time is 1~2h,
Temperature is 300~350 DEG C after continuing heating, and the insulation pore-forming time is 1~2h, then temperature is 800~900 DEG C after heating up,
Sintering time is 2~3h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108794059A (en) * | 2018-06-12 | 2018-11-13 | 佛山市华强协兴陶瓷有限公司 | A kind of preparation method of high-strength degradable multiporous bioceramic |
| CN109897984A (en) * | 2018-05-25 | 2019-06-18 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of titanium-based metal porous material |
| CN110029487A (en) * | 2019-04-23 | 2019-07-19 | 宁波江东碧辰环保科技有限公司 | A kind of preparation method of easy cleaning high strength industrial filter cloth |
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| CN1454871A (en) * | 2003-05-30 | 2003-11-12 | 武汉理工大学 | Method of preparing hot pressure casting porous ceramic using organic foam micro ball as perforating agent |
| CN1830907A (en) * | 2006-03-20 | 2006-09-13 | 天津大学 | Method for preparing CaO-P2O5-MgO glass reinforced porous beta-tricalcium phosphate bioceramics |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1454871A (en) * | 2003-05-30 | 2003-11-12 | 武汉理工大学 | Method of preparing hot pressure casting porous ceramic using organic foam micro ball as perforating agent |
| CN1830907A (en) * | 2006-03-20 | 2006-09-13 | 天津大学 | Method for preparing CaO-P2O5-MgO glass reinforced porous beta-tricalcium phosphate bioceramics |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109897984A (en) * | 2018-05-25 | 2019-06-18 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of titanium-based metal porous material |
| CN108794059A (en) * | 2018-06-12 | 2018-11-13 | 佛山市华强协兴陶瓷有限公司 | A kind of preparation method of high-strength degradable multiporous bioceramic |
| CN110029487A (en) * | 2019-04-23 | 2019-07-19 | 宁波江东碧辰环保科技有限公司 | A kind of preparation method of easy cleaning high strength industrial filter cloth |
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