CN108560057A - A kind of preparation method of modified hydroxylapatite whisker - Google Patents
A kind of preparation method of modified hydroxylapatite whisker Download PDFInfo
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- CN108560057A CN108560057A CN201810292803.7A CN201810292803A CN108560057A CN 108560057 A CN108560057 A CN 108560057A CN 201810292803 A CN201810292803 A CN 201810292803A CN 108560057 A CN108560057 A CN 108560057A
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- ethyl alcohol
- absolute ethyl
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- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical class [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000013078 crystal Substances 0.000 claims abstract description 26
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 18
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 60
- 238000003756 stirring Methods 0.000 claims description 13
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 4
- 229910052586 apatite Inorganic materials 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 20
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000012620 biological material Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 9
- 210000000988 bone and bone Anatomy 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- -1 silica modified hydroxyapatite Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- FRIKWZARTBPWBN-UHFFFAOYSA-N [Si].O=[Si]=O Chemical compound [Si].O=[Si]=O FRIKWZARTBPWBN-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical class CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000011856 silicon-based particle Substances 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 238000000844 transformation Methods 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000035 biogenic effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- CUXQLKLUPGTTKL-UHFFFAOYSA-M microcosmic salt Chemical compound [NH4+].[Na+].OP([O-])([O-])=O CUXQLKLUPGTTKL-UHFFFAOYSA-M 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 241000251539 Vertebrata <Metazoa> Species 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Inorganic materials [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 1
- MWKXCSMICWVRGW-UHFFFAOYSA-N calcium;phosphane Chemical compound P.[Ca] MWKXCSMICWVRGW-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011005 laboratory method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000012783 reinforcing fiber Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/54—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
Abstract
The present invention discloses a kind of preparation method of modified hydroxylapatite whisker, uses ethyl orthosilicate, ammonium hydroxide, hydroxyapatite crystal whisker for raw material, and the hydroxyapatite crystal whisker of surface modification of silica is made in hydrolyzing tetraethoxy orthosilane in ethanol solution.Present invention process is simple, easy to operation, stable yield, can be applied to biomaterial and other engineering material activeness and quietness fields.
Description
Technical field
The present invention relates to a kind of preparation methods of modified hydroxylapatite whisker, belong to biological engineering material and engineering enhancing
The fields such as toughening material.
Background technology
Calcium microcosmic salt（CaP）It is the main inorganic composition of vertebrate skeletal and tooth, has been obtained extensively in biomedical aspect
General application.Bone and other calcified tissues are by biogenic mineral（One or more calcium microcosmic salts）, protein matrix, other inorganic materials
What material and water formed.Biogenic mineral mutually accounts for the 70% of bone composition, and water accounts for 5-8%, and other organic phases such as collagen account for 22-25%.According to calcium
The different physical property of microcosmic salt, chemical property, bioactivity, degradation absorbability are applied to different biological fields.In calcium phosphorus
In salt, hydroxyapatite（HAP）With the mineral composition most like with bone, good thermal stability obtain most widely study with
Using.In the 1970's, American scholar Jarcho, Japanese scholars Aoki, Europe scholar Groot have almost been started simultaneously to biology
Material hydroxyapatite is in synthesis and in the research of Bone Defect Repari application aspect.So far it after, has started to hydroxyapatite material
The upsurge of experiment basis studies and clinical application.
Research shows that HAP material fragilities are larger and longer the time required to bioactivity reaction occurs after implanting, significantly
Its extensive use clinically is limited, still, HAP whiskers can be lured with demineralized bone composite material as a kind of existing bone
Effect is led, and has the graft of enhancing volume and mechanism supports effect and is used for craniofacial orthopedics.Accordingly, with respect to other inorganic materials
For material, HAP whiskers not only have good biocompatibility and bioactivity, also have stronger mechanical property, chemistry steady
Qualitative and wearability is one of ideal bone renovating bracket material.
Hydroxyapatite crystal whisker is under manual control condition with the short fibre of micro/nano level made of high-purity crystal growth
Dimension.Its diameter is very small（The micron order of magnitude）, there is very high draw ratio and bulk density, without containing scarce present in usual material
It falls into（Crystal boundary, dislocation, hole etc.）, atomic arrangement high-sequential, thus its intensity is close to the theoretical value of perfect crystal.Whisker
Height-oriented structure make it have high intensity, high-modulus and high elongation rate.The intensity of whisker is far above other chopped strands, main
To be used as the reinforcement of composite material, for manufacturing high strength composite.It will be appreciated, however, that with regard to the reinforcement of structural material
For phase, pure ha whisker surface is smooth, is used as reinforcing fiber, when by larger shearing or drawing stress, is easy to
Relative sliding in the base, and keep its toughening effect less apparent.
Invention content
The present invention adopts in view of the deficienciess of the prior art, provide a kind of preparation method of modified hydroxylapatite whisker
It is raw material with ethyl orthosilicate, ammonium hydroxide, hydroxyapatite crystal whisker, nano-silica is made in hydrolyzing tetraethoxy orthosilane in ethanol solution
The hydroxyapatite crystal whisker that SiClx surface is modified, the surface that similar " screw-thread steel " is carried out to hydroxyapatite crystal whisker is modified, from work
Its toughening benefit can be relatively significantly improved known to Cheng Xue angles, prepared modified hydroxylapatite whisker can be used for biological work
Journey material or biological engineering material activeness and quietness mutually use.The specific steps are：
（1）It measures a certain amount of ethyl orthosilicate stirring and dissolving and A liquid is made in absolute ethyl alcohol；It is molten to measure a certain amount of ammonium hydroxide stirring
B liquid is made in solution in absolute ethyl alcohol；
（2）B liquid is stirred under certain condition, and A liquid is added dropwise to certain rate of addition in B liquid, after being added dropwise to complete, continues to stir
Reaction certain time length is mixed, silicon dioxide gel is obtained, is denoted as C liquid；
（3）It weighs a certain amount of hydroxyapatite crystal whisker ultrasonic disperse and D liquid is made in absolute ethyl alcohol.D liquid is added in C liquid,
Be aged certain time length, take out hydroxyapatite crystal whisker it is dry and be sintered to get.
Step（1）The volume ratio of ethyl orthosilicate and absolute ethyl alcohol is 1 in A liquid:4~1:10；Ammonium hydroxide and anhydrous second in B liquid
The volume ratio of alcohol is 1:3~1:5；The volume ratio of A liquid and B liquid is 1:1.0~1:2.5.
Step（2）B liquid is stirred under the certain condition is under 40 ~ 60 DEG C of water baths, stir speed (S.S.) is 60 ~ 300 turns/
min。
Step（2）Certain rate of addition is 0.5 ~ 1.5mL/min.
Step（2）It is described to continue to be stirred to react certain time length, this when a length of 24 ~ 48h.
Step（3）The ratio of hydroxyapatite crystal whisker and absolute ethyl alcohol is 0.1 ~ 0.5g/mL in the D liquid.
Step（3）The volume ratio of the D liquid and C liquid is 1:5~1:10.
Step（3）A length of 24 ~ 72h when the described ageing.
Step（3）The drying is vacuum or forced air drying, and drying temperature is 30 ~ 60 DEG C.
Step（3）The sintering is sintered using vacuum-sintering or air atmosphere, and sintering temperature is 650 ~ 800 DEG C, the time
For 4 ~ 12h.
Used hydroxyapatite crystal whisker is made by oneself for laboratory, and preparation method is using under hydro-thermal process alkaline environment
Ca(NO3)2With (NH4)2HPO4, and carry out related ageing and be dried, finally obtain hydroxyapatite crystal whisker finished product.
The present invention has the following advantages：
1, reaction process is simple, of low cost, easy to operate, and material property is stablized；
2, the mechanical property of modified hydroxylapatite whisker obtained and biology performance are excellent, and yield is high；
3, modified hydroxylapatite whisker obtained deposits in hydroxyapatite crystal whisker material surface and prepares one layer of spherical nanometer two
Silicon oxide particle can more show the enhancement effect of similar " screw-thread steel ", be more advantageous to hydroxyapatite crystal whisker and be applied to biology
The related fields such as the activeness and quietness of engineering material and other engineering material.
Description of the drawings
Fig. 1 is preparation technology flow chart of the present invention；
Fig. 2 is that silica modified hydroxyapatite crystal whisker SEM schemes；
Fig. 3 is the XRD diagram of silica modified hydroxyapatite crystal whisker.
Specific implementation mode
Following embodiment preparation process flow is as shown in Fig. 1.
Embodiment 1
（1）It measures 25mL ethyl orthosilicates stirring and dissolving and A liquid is made in 100mL absolute ethyl alcohols, measure 30mL ammonium hydroxide stirring and dissolvings
B liquid is made in 150mL absolute ethyl alcohols；
（2）Under 40 DEG C of water bath conditions, B liquid is stirred with the rate of 60 turns/min, by constant flow pump by A liquid with the drop of 1mL/min
Acceleration is added dropwise in B liquid, after being added dropwise to complete, is continued to be stirred to react for 24 hours, is obtained silicon dioxide gel, is denoted as C liquid；
（3）D liquid is made in the hydroxyapatite crystal whisker ultrasonic disperse for weighing 5g in 50mL absolute ethyl alcohols.D liquid is added in C liquid,
It is aged 72h, takes out 60 DEG C of dryings of hydroxyapatite crystal whisker for 24 hours, 800 DEG C of sintering 4h obtain silica modified hydroxyapatite whisker
Palpus.Gained whisker length is about 200 μm, and width is about 3 μm, and superficial silicon dioxide silicon particle is about 600nm, and SEM schemes such as Fig. 2 institutes
Show, it can be seen that silica homogeneity is fine；Its XRD diagram is fig. 3, it is shown that material composition is HAP and SiO2,
Other phase transformations do not occur, therefore do not influence its bioactivity.
Embodiment 2
（1）It measures 18mL ethyl orthosilicates stirring and dissolving and A liquid is made in 100mL absolute ethyl alcohols, measure 40mL ammonium hydroxide stirring and dissolvings
B liquid is made in 150mL absolute ethyl alcohols；
（2）Under 50 DEG C of water bath conditions, B liquid is stirred with the rate of 200 turns/min, by constant flow pump by A liquid with 0.5mL/min's
Rate of addition is added dropwise in B liquid, after being added dropwise to complete, is continued to be stirred to react 36h, is obtained silicon dioxide gel, is denoted as C liquid；
（3）D liquid is made in the hydroxyapatite crystal whisker ultrasonic disperse for weighing 10g in 35mL absolute ethyl alcohols.D liquid is added in C liquid,
It is aged 48h, takes out 40 DEG C of dryings of hydroxyapatite crystal whisker for 24 hours, 700 DEG C of sintering 8h obtain silica modified hydroxyapatite whisker
Must, wherein whisker length is about 200 μm, and width is about 3 μm, and superficial silicon dioxide silicon particle is about 550nm, silica homogeneity
Very well, and material composition is HAP and SiO2, other phase transformations do not occur, therefore do not influence its bioactivity.
Embodiment 3
（1）It measures 10mL ethyl orthosilicates stirring and dissolving and A liquid is made in 100mL absolute ethyl alcohols, measure 50mL ammonium hydroxide stirring and dissolvings
B liquid is made in 150mL absolute ethyl alcohols；
（2）Under 60 DEG C of water bath conditions, B liquid is stirred with the rate of 300 turns/min, by constant flow pump by A liquid with 1.5mL/min's
Rate of addition is added dropwise in B liquid, after being added dropwise to complete, is continued to be stirred to react 48h, is obtained silicon dioxide gel, is denoted as C liquid；
（3）D liquid is made in the hydroxyapatite crystal whisker ultrasonic disperse for weighing 30g in 60mL absolute ethyl alcohols.D liquid is added in C liquid,
Ageing for 24 hours, takes out 30 DEG C of hydroxyapatite crystal whisker dry 36h, 650 DEG C of sintering 12h and obtains silica modified hydroxyapatite
Whisker, wherein whisker length are about 150 μm, and width is about 2 μm, and superficial silicon dioxide silicon particle is about 500nm, and silica is uniform
Property it is fine, and material composition be HAP and SiO2, other phase transformations do not occur, therefore do not influence its bioactivity.
Claims (10)
1. a kind of preparation method of modified hydroxylapatite whisker, includes the following steps：
（1）A liquid is made in absolute ethyl alcohol in ethyl orthosilicate stirring and dissolving, B liquid is made in absolute ethyl alcohol in ammonium hydroxide stirring and dissolving；
（2）B liquid is stirred under 40 ~ 60 DEG C of water baths, and A drops are added in B liquid, after being added dropwise to complete, continue to be stirred to react
Silicon dioxide gel is denoted as C liquid；
（3）D liquid is made in hydroxyapatite crystal whisker ultrasonic disperse in absolute ethyl alcohol, D liquid is added in C liquid, hydroxyl is taken out in ageing
Base apatite whiskers it is dry and be sintered to get.
2. preparation method according to claim 1, it is characterised in that：Step（1）Ethyl orthosilicate and absolute ethyl alcohol in A liquid
Volume ratio be 1:4~1:The volume ratio of ammonium hydroxide and absolute ethyl alcohol is 1 in 10, B liquid:3~1:The volume ratio of 5, A liquid and B liquid is 1:
1.0~1:2.5。
3. preparation method according to claim 1, it is characterised in that：Step（2）Stir speed (S.S.) is 60 ~ 300 turns/min.
4. preparation method according to claim 1, it is characterised in that：Step（2）A drops are added to the dropwise addition speed in B liquid
Degree is 0.5 ~ 1.5mL/min.
5. preparation method according to claim 1, it is characterised in that：Step（2）After being added dropwise to complete, continue to be stirred to react 24
~48h。
6. preparation method according to claim 1, it is characterised in that：Step（3）In D liquid hydroxyapatite crystal whisker with it is anhydrous
The ratio of ethyl alcohol is 0.1 ~ 0.5g/mL.
7. restructuring Preparation Method according to claim 1, it is characterised in that：Step（3）The volume ratio of D liquid and C liquid is 1:5~
1:10。
8. preparation method according to claim 1, it is characterised in that：Step（3）It is aged 24 ~ 72h.
9. preparation method according to claim 1, it is characterised in that：Step（3）The drying is that vacuum or air blast are dry
Dry, drying temperature is 30 ~ 60 DEG C.
10. preparation method according to claim 1, it is characterised in that：Step（3）The sintering using vacuum-sintering or
Air atmosphere is sintered, and sintering temperature is 650 ~ 800 DEG C, and the time is 4 ~ 12h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111139594A (en) * | 2020-03-11 | 2020-05-12 | 昆明理工大学 | Preparation method of composite porous material for bone repair |
| CN113024119A (en) * | 2021-03-26 | 2021-06-25 | 昆明理工大学 | Glass ceramic material and preparation method thereof |
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|---|---|---|---|---|
| CN101327167A (en) * | 2008-07-14 | 2008-12-24 | 昆明理工大学 | Hydroxylapatite crystal whisker with modified surface and preparation and use thereof |
| CN101401965A (en) * | 2008-11-17 | 2009-04-08 | 昆明理工大学 | Synthesis of composite bone restoration bioactive material |
| CN104524638A (en) * | 2014-11-19 | 2015-04-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Silicon oxide-calcium phosphate class composite nano-filler and preparation method thereof |
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2018
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| CN101327167A (en) * | 2008-07-14 | 2008-12-24 | 昆明理工大学 | Hydroxylapatite crystal whisker with modified surface and preparation and use thereof |
| CN101401965A (en) * | 2008-11-17 | 2009-04-08 | 昆明理工大学 | Synthesis of composite bone restoration bioactive material |
| CN104524638A (en) * | 2014-11-19 | 2015-04-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Silicon oxide-calcium phosphate class composite nano-filler and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| YIN YANTING ET AL.: ""Synthesis of Silica Modified Large-sized Hydroxyapatite Whiskers By a Hydrothermal Co-precipitation Method"", 《KEY ENGINEERING MATERIALS》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111139594A (en) * | 2020-03-11 | 2020-05-12 | 昆明理工大学 | Preparation method of composite porous material for bone repair |
| CN113024119A (en) * | 2021-03-26 | 2021-06-25 | 昆明理工大学 | Glass ceramic material and preparation method thereof |
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