CN101757687B - Surface modification method of bio-absorbable material implanted in polyester - Google Patents

Surface modification method of bio-absorbable material implanted in polyester Download PDF

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Publication number
CN101757687B
CN101757687B CN200910260219.4A CN200910260219A CN101757687B CN 101757687 B CN101757687 B CN 101757687B CN 200910260219 A CN200910260219 A CN 200910260219A CN 101757687 B CN101757687 B CN 101757687B
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reactor
bio
polyester
supercritical fluid
absorbable
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CN101757687A (en
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章培标
崔立国
陈学思
崔毅
高战团
王宇
王宗良
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CHANGCHUN SINOBIOMATERIALS Co Ltd
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Changchun Institute of Applied Chemistry of CAS
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Abstract

The invention discloses a surface modification method of a bio-absorbable material implanted in a polyester, and the bio-absorbable material implanted in the polyester is treated by supercritical fluid. The invention utilizes the supercritical carbon dioxide technology to modify the surface of various existing internally absorbable implanted materials, so as to form holes with nanometer size or micron size on the surface of the material, the invention solves the problem that the interface of existing internally absorbable implanted material is not suitable for cell adhesion and proliferation, thereby facilitating protein adsorption and deposition of extracellular matrix, and integration with the surrounding tissues; moreover, the invention can form tiny blood vessels timely, and can achieve good synchronization of material degradation and replacement of bone cells.

Description

The surface modifying method of bio-absorbable material implanted in polyester
Technical field
The present invention relates to a kind of surface modifying method, especially the surface modifying method to bio-absorbable material implanted in polyester.
Background technology
Biological absorbable material implanted, be class strand under physiological environment can automatically rupture, from macromole become micromolecule, from insoluble matter become solubilized, finally can be gradually by the material of organism metabolism or absorption.At present, in more common body, absorbable material comprises resorbable polymeric materials in polyesters body, as polylactic acid, PGA, polymeric polyglycolide-polylactide copolymer etc., and natural polymer, as collagen, chitosan, alginate etc.
Biological absorbable material implanted, can be used to make various medical apparatus and instruments, as degradable in vivo artificial teeth, skin, joint, kidney, pancreas, heart, cardiac valve, blood vessel, trachea, trunnion, esophagus, bladder, bone repairing support, and orthopaedics internal fixation material, as nail, hone lamella, cervical vertebral fusion cage, lumbar fusion cages, thoracic vertebra fusion cage etc., also have intravascular stent etc., in modern medicine treatment, progressively applied widely.
Use at present all kinds of medical apparatus and instruments of material implanted making of biological absorbable, there is the shortcomings such as poor mechanical property and degradation property be slow, be mainly because the material implanted surface that exists itself is very fine and close smooth, be unfavorable for adhesion and the propagation of cell.Although also have by osteoinductive inorganic particulates such as doped hydroxyapatites wherein, improve adhesion and the propagation of cell, common practices is by spraying hydroxyapatite particle on the outer surface to medical apparatus and instruments at present, thereby reaches shaggy object.But can not well improve like this cell adhesion, also be difficult to realize transport and the exchange of tissue fluid, nutrient substance.
Also have by improve the propagation that adheres to of cell at the surperficial drilling method of medical apparatus and instruments in addition, but because porosity is too low, pore quantity is less, the restriction such as mutually directly do not connect, cell is not easy the growth inside to medical apparatus and instruments uniformly, is difficult to realize degraded and the osteoblastic alternative synchronicity of accomplishing of material.
Summary of the invention
The present invention is directed to deficiency, propose a kind of surface modifying method of bio-absorbable material implanted in polyester, can make the surface of this material produce micropore, be suitable for cell adhesion and propagation.
In order to realize foregoing invention object, the invention provides following technical scheme: a kind of surface modifying method of bio-absorbable material implanted in polyester, this surface modifying method is through treatment with supercritical fluid by bio-absorbable material implanted in polyester.
Preferably, described supercritical fluid is supercritical carbon dioxide fluid.
Preferably, described treatment with supercritical fluid bio-absorbable material implanted in polyester, comprises following process:
(1), bio-absorbable material implanted in polyester is put into reactor;
(2), in reactor, pass into supercritical carbon dioxide fluid, 30 DEG C～120 DEG C, 7.5MPa～30MPa, 1 hour～48 hours;
(3), be slowly down to normal pressure.
Preferably, in step (3), blood pressure lowering process is 1 minute～60 minutes.
Preferably, this surface modifying method was also included in bio-absorbable material implanted in polyester before treatment with supercritical fluid, and bio-absorbable material implanted in polyester is soaked in polyesters solution.
Preferably, described soak time is 10 seconds～1 hour.
Preferably, described polyesters solution is dimethyl sulfoxide or dioxane solution.
The action principle of supercritical fluid (SCF) is: under sufficiently high pressure, polymer can absorb certain gas and cause the increase of volume own, occur swelling, if be first dissolved with alloy in SCF, as inorganic matter molecule or bioactive molecule, medicine etc., because SCF can make polymers swell, improve the diffusion coefficient of the alloy that molecular weight is larger, sometimes even strengthen several orders of magnitude, thereby the adulterant that can within the suitable time, these hope be counted joins among the skeleton of polymer.Once after blood pressure lowering, SCF removes from interface, the speed that alloy will diffuse out from polymer is much smaller while entering than originally, thereby sneaks into the inside of material.The time that control polymer contacts with supercritical liq can change the mechanical property of support, and the gas that blood pressure lowering produces can produce three-dimensional porous structure at material internal.Concentration and venting speed between pressure, polymer and the carbon dioxide of change gas, inner pore structure can be controlled.
Compared with prior art, the present invention can be to absorbing the modifying surface of medical apparatus and instruments by super critical CO 2 technology in multiple body, make its surface form micron, submicron and nanoscale hole, and form certain roughness on its surface, this bore hole size and roughness are applicable to cell adhesion and growing multiplication, be conducive to protein adsorption and extrtacellular matrix deposition, be conducive to merge with surrounding tissue, be conducive to transmission and the exchange of tissue fluid and various nutrient substance, in such structure, be more suitable for the formation of capillary vessel, and be conducive in osteoblastic proliferation process the support medical apparatus and instruments of alternative corresponding biological absorbable progressively.
Brief description of the drawings
Fig. 1 is the testing result photo of embodiment 1;
Fig. 2 is the testing result photo of embodiment 2;
Fig. 3 is the testing result photo of embodiment 3;
Fig. 4 is the testing result photo of embodiment 4;
Fig. 5 is the testing result photo of embodiment 5;
Fig. 6 is the testing result photo of embodiment 6;
Fig. 7 is the testing result photo of embodiment 7;
Fig. 8 is the testing result photo of embodiment 8;
Fig. 9 is the testing result photo of embodiment 9;
Figure 10 is the testing result photo of embodiment 10;
Figure 11 is the testing result photo of embodiment 11;
Figure 12 is the testing result photo of embodiment 12;
Figure 13 is the testing result photo of embodiment 13;
Figure 14 is the testing result photo of embodiment 14;
Figure 15 is the testing result photo of embodiment 15;
Figure 16 is the testing result photo of embodiment 16;
Figure 17 is the surperficial testing result photo of the bio-absorbable material implanted in polyester of existing non-modified processing.
Detailed description of the invention
Understand better the present invention for ease of those skilled in the art, below in conjunction with embodiment, further set forth the present invention:
Embodiment 1
1. put into autoclave by absorbing threaded fusion cage in polylactic acid (PLA) body;
2. reactor is put into oil bath pan, regulate temperature constant temperature to 55 DEG C;
3. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
4. regulate supercritical fluid pump output CO 2pressure constant voltage is to 20MPa;
5. keep 55 DEG C of reactor constant temperatures, constant voltage 20MPa, 1 hour;
6. reaction finishes rear decompression eliminating CO 2, 10 minutes control times.
7. take out the absorbed threaded fusion cage after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in Figure 1.
Embodiment 2
1. put into autoclave by absorbing thoracic vertebra fusion cage in the polylactic acid of grafting 10% hydroxyapatite (10%HA/PLA) body;
2. reactor is put into oil bath pan, regulate temperature constant temperature to 55 DEG C;
3. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
4. regulate supercritical fluid pump output CO 2pressure constant voltage is to 20MPa;
5. keep 55 DEG C of reactor constant temperatures, constant voltage 20MPa, 1 hour;
6. reaction finishes rear decompression eliminating CO 2, 10 minutes control times.
7. take out the absorbed thoracic vertebra fusion cage after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in Figure 2.
Embodiment 3
1. absorbable stent in polylactide Acetic acid, hydroxy-, bimol. cyclic ester (PLGA) body is put into autoclave;
2. reactor is put into oil bath pan, regulate temperature constant temperature to 45 DEG C;
3. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
4. regulate supercritical fluid pump output CO 2pressure constant voltage is to 20MPa;
5. keep 45 DEG C of reactor constant temperatures, constant voltage 20MPa, 3 hours;
6. reaction finishes rear decompression eliminating CO 2, 10 minutes control times.
7. take out the absorbable stent after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in Figure 3.
Embodiment 4
1 soaks absorbable bone peg in polylactide Acetic acid, hydroxy-, bimol. cyclic ester (PLGA) body 12 hours in dimethyl sulfoxide (DMSO);
2. absorbable bone peg in the body soaking is put into autoclave;
3. reactor is put into oil bath pan, regulate temperature constant temperature to 50 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 15MPa;
6. keep 50 DEG C of reactor constant temperatures, constant voltage 15MPa, 1 hour;
7. reaction finishes rear decompression eliminating CO 2, 5 minutes control times.
8. take out the absorbable bone peg after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in Figure 4.
Embodiment 5
1 soaked for 10 seconds by absorbing artificial root of the tooth in polylactic acid (PLA) body in dioxane;
2. put into autoclave by absorbing artificial teeth in the body soaking;
3. reactor is put into oil bath pan, regulate temperature constant temperature to 35 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 20MPa;
6. keep 35 DEG C of reactor constant temperatures, constant voltage 15MPa, 1 hour;
7. reaction finishes rear decompression eliminating CO 2, 15 minutes control times.
8. take out the absorbed artificial teeth after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in Figure 5.
Embodiment 6
1. adsorbable bone recovery support in the polylactic acid of grafting 10% hydroxyapatite (10%HA/PLA) body is soaked to 10 seconds in dioxane;
2. adsorbable bone recovery support in the body soaking is put into autoclave;
3. reactor is put into oil bath pan, regulate temperature constant temperature to 50 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 20MPa;
6. keep 50 DEG C of reactor constant temperatures, constant voltage 15MPa, 1 hour;
7. reaction finishes rear decompression eliminating CO 2, 1 minute control time.
8. take out the adsorbable bone recovery support after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in Figure 6.
Embodiment 7
1. in dioxane, soaked for 10 seconds by absorbing threaded fusion cage in the polylactic acid of 40% hydroxyapatite blend (40%HA/PLA blend) body;
2. put into autoclave by absorbing threaded fusion cage in the body soaking;
3. reactor is put into oil bath pan, regulate temperature constant temperature to 55 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 20MPa;
6. keep 55 DEG C of reactor constant temperatures, constant voltage 20MPa, 1 hour;
7. reaction finishes rear decompression eliminating CO 2, 1 minute control time.
8. take out the absorbed threaded fusion cage after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in Figure 7.
Embodiment 8
1. in dioxane, soaked for 10 seconds by absorbing cervical vertebral fusion cage in polylactide Acetic acid, hydroxy-, bimol. cyclic ester (PLGA) body;
2. put into autoclave by absorbing cervical vertebral fusion cage in the body soaking;
3. reactor is put into oil bath pan, regulate temperature constant temperature to 55 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 20MPa;
6. keep 55 DEG C of reactor constant temperatures, constant voltage 20MPa, 1 hour;
7. reaction finishes rear decompression eliminating CO 2, 10 minutes control times.
8. take out the absorbed cervical vertebral fusion cage after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in Figure 8.
Embodiment 9
1. absorbable-bone plate in polylactic acid (PLA) body is soaked to 10 seconds in dioxane;
2. absorbable-bone plate in the body soaking is put into autoclave;
3. reactor is put into oil bath pan, regulate temperature constant temperature to 45 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 10MPa;
6. keep 45 DEG C of reactor constant temperatures, constant voltage 10MPa, 1 hour;
7. reaction finishes rear decompression eliminating CO 2, 10 minutes control times.
8. take out the absorbable-bone plate after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in Figure 9.
Embodiment 10
1. in dioxane, soaked for 10 seconds by absorbing threaded fusion cage in polylactic acid (PLA) body;
2. put into autoclave by absorbing threaded fusion cage in the body soaking;
3. reactor C is put into oil bath pan, regulate temperature constant temperature to 55 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 20MPa;
6. keep 55 DEG C of reactor constant temperatures, constant voltage 10MPa, 1 hour;
7. reaction finishes rear decompression eliminating CO 2, 1 minute control time.
8. take out the absorbed threaded fusion cage after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in figure 10.
Embodiment 11
1. in dioxane, soaked for 10 seconds by absorbing thoracic vertebra fusion cage in the polylactic acid of 10% hydroxyapatite blend (10%HA/PLA blend) body;
2. put into autoclave by absorbing thoracic vertebra fusion cage in the body soaking;
3. reactor is put into oil bath pan, regulate temperature constant temperature to 55 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 20MPa;
6. keep 55 DEG C of reactor constant temperatures, constant voltage 10MPa, 1 hour;
7. reaction finishes rear decompression eliminating CO 2, 1 minute control time.
8. take out the absorbed thoracic vertebra fusion cage after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in figure 11.
Embodiment 12
1. absorbable stent in the polylactic acid of 10% hydroxyapatite blend (10%HA/PLA blend) body is soaked to 10 seconds in dioxane;
2. absorbable stent in the body soaking is put into autoclave;
3. reactor is put into oil bath pan, regulate temperature constant temperature to 55 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 20MPa;
6. keep 55 DEG C of reactor constant temperatures, constant voltage 10MPa, 1 hour;
7. reaction finishes rear decompression eliminating CO 2, 20 minutes control times.
8. take out the absorbable stent after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in figure 12.
Embodiment 13
1. in dioxane, soaked for 10 seconds by absorbing joint in the polylactic acid of 10% hydroxyapatite blend (10%HA/PLA blend) body;
2. put into autoclave by absorbing joint in the body soaking;
3. reactor is put into oil bath pan, regulate temperature constant temperature to 65 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 20MPa;
6. keep 55 DEG C of reactor constant temperatures, constant voltage 10MPa, 4 hours;
7. reaction finishes rear decompression eliminating CO 2, 10 minutes control times.
8. take out the absorbed joint after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in figure 13.
Embodiment 14
1. in dioxane, soaked for 10 seconds by absorbing cervical vertebral fusion cage in the polylactic acid of grafting 10% hydroxyapatite (10%HA/PLA grafting) body;
2. put into autoclave by absorbing cervical vertebral fusion cage in the body soaking;
3. reactor is put into oil bath pan, regulate temperature constant temperature to 50 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 15MPa;
6. keep 50 DEG C of reactor constant temperatures, constant voltage 10MPa, 3 hours;
7. reaction finishes rear decompression eliminating CO 2, 15 minutes control times.
8. take out the absorbed cervical vertebral fusion cage after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in figure 14.
Embodiment 15
1. in dioxane, soaked for 10 seconds by absorbing skin in the polylactic acid of grafting 10% hydroxyapatite (10%HA/PLA grafting) body;
2. put into autoclave by absorbing skin in the body soaking;
3. reactor is put into oil bath pan, regulate temperature constant temperature to 55 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 10MPa;
6. keep 55 DEG C of reactor constant temperatures, constant voltage 10MPa, 2 hours;
7. reaction finishes rear decompression eliminating CO 2, 10 minutes control times.
8. take out the absorbed skin after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in figure 15.
Embodiment 16
1. in dioxane, soaked for 10 seconds by absorbing threaded fusion cage in the polylactic acid of 40% hydroxyapatite blend (10%HA/PLA blend) body;
2. put into autoclave by absorbing threaded fusion cage in the body soaking;
3. reactor is put into oil bath pan, regulate temperature constant temperature to 65 DEG C;
4. open CO 2steel cylinder gas valve, opens supercritical fluid pump, and reactor intake valve, off-response still vent valve; In reactor, pass into CO 2, and repeatedly take a breath for several times;
5. regulate supercritical fluid pump output CO 2pressure constant voltage is to 30MPa;
6. keep 65 DEG C of reactor constant temperatures, constant voltage 30MPa, 1 hour;
7. reaction finishes rear decompression eliminating CO 2, 10 minutes control times.
8. take out the absorbed threaded fusion cage after surface modification, vacuum drying, field emission scanning electron microscope (ESEM) detects surface to be changed.As shown in figure 16.
Product comparison from accompanying drawing 1～16 and modification, before modification, the surface of product is detected as shown in figure 17, can find out, embedded material after surface modification treatment of the present invention, there are a large amount of holes in its surface, and there is uneven phenomenon in surface, more be conducive to cell adhesion and growing multiplication, be conducive to protein adsorption and extrtacellular matrix deposition, be conducive to merge with surrounding tissue, be conducive to transmission and the exchange of tissue fluid and various nutrient substance, in such structure, be more suitable for the formation of capillary vessel, and be conducive in osteoblastic proliferation process the support medical apparatus and instruments of alternative corresponding biological absorbable progressively.
Need to further illustrate, for those skilled in the art, under the premise without departing from the principles of the invention, can also make some improvements and modifications as described below, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (5)

1. a surface modifying method for bio-absorbable material implanted in polyester, is characterized in that: this surface modifying method is through treatment with supercritical fluid by bio-absorbable material implanted in polyester;
This surface modifying method was also included in bio-absorbable material implanted in polyester before treatment with supercritical fluid, and bio-absorbable material implanted in polyester is soaked in dimethyl sulfoxide or dioxane solution;
Described bio-absorbable material implanted in polyester is can absorb medical apparatus and instruments in body.
2. surface modifying method according to claim 1, is characterized in that: described supercritical fluid is supercritical carbon dioxide fluid.
3. surface modifying method according to claim 2, is characterized in that: described treatment with supercritical fluid bio-absorbable material implanted in polyester, comprises following process:
(1), bio-absorbable material implanted in polyester is put into reactor;
(2), in reactor, pass into supercritical carbon dioxide fluid, 30 DEG C～120 DEG C, 7.5MPa～30MPa, 1 hour～48 hours;
(3), be slowly down to normal pressure.
4. surface modifying method according to claim 3, is characterized in that: step (3) in, blood pressure lowering process is 1 minute～60 minutes.
5. surface modifying method according to claim 1, is characterized in that: described soak time is 10 seconds～1 hour.
CN200910260219.4A 2009-12-25 2009-12-25 Surface modification method of bio-absorbable material implanted in polyester Active CN101757687B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1476907A (en) * 2003-06-30 2004-02-25 暨南大学 Bio-active 3-D porous tissue engineering support material and its preparation method

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JP2001158827A (en) * 1999-09-21 2001-06-12 Daicel Chem Ind Ltd Method for modifying surface of plastic molding product and surface-modified plastic molding product
CN1313191C (en) * 2004-09-24 2007-05-02 浙江大学 Method for preparing polymer microporous membrane by supercritical or nearcritical CO2 technology
KR20060113463A (en) * 2005-04-27 2006-11-02 히다치 막셀 가부시키가이샤 Surface reforming method of polymeric substrate, method for forming plated film on polymeric substrate, method for manufacturing polymer member, and coating member

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1476907A (en) * 2003-06-30 2004-02-25 暨南大学 Bio-active 3-D porous tissue engineering support material and its preparation method

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