CN110292656A - A kind of porous titanium alloy surface biological glass/polycaprolactone/collagenic coating and preparation method thereof - Google Patents
A kind of porous titanium alloy surface biological glass/polycaprolactone/collagenic coating and preparation method thereof Download PDFInfo
- Publication number
- CN110292656A CN110292656A CN201810237720.8A CN201810237720A CN110292656A CN 110292656 A CN110292656 A CN 110292656A CN 201810237720 A CN201810237720 A CN 201810237720A CN 110292656 A CN110292656 A CN 110292656A
- Authority
- CN
- China
- Prior art keywords
- polycaprolactone
- titanium alloy
- bio
- vitric
- porous titanium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/34—Macromolecular materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/56—Porous materials, e.g. foams or sponges
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
Abstract
The invention discloses a kind of porous titanium alloy surface biological glass/polycaprolactone/collagenic coatings and preparation method thereof.Present invention combination Electrostatic Spray Technology, bio-vitric/polycaprolactone/collagenic coating is constructed simultaneously on porous titanium alloy surface, simple process is convenient, spray efficiency is high, bio-vitric/polycaprolactone/collagenic coating is tightly combined with titanium alloy substrate, it is not easily to fall off, it coating and can be coexisted with porous titanium alloy surface by micro-arc oxidation structure;On the other hand, bio-vitric/polycaprolactone/collagenic coating improves biocompatibility and the tissue repairing ability of titanium alloy material, provides more stable chemical bonding and higher bioactivity for titanium alloy implant, is more advantageous to growing into for freshman bone tissue.
Description
Technical field
The present invention relates to bio-medical coating technology fields, and in particular to a kind of porous titanium alloy surface biological glass/poly-
Caprolactone/collagenic coating and preparation method thereof.
Background technique
Titanium alloy lacks good osteoinductive, and surface inertness oxide layer limits while reducing host rejection reaction
The integration of itself and bone tissue.Titanium alloy material implants, and common biological respinse occurs mainly in the table of implant
Face, thus concern of the surface biological functionalization of titanium alloy by extensive researcher.
The surface biological functionalization of titanium alloy can not only keep the mechanical property of titanium alloy, moreover it is possible to significantly improve implant
Osseointegration character, improve the success rate of implant surgery.Titanium alloy surface composite collagen technology is recent bioactivation table
The another hot spot technology in field is modified in face.Collagen is the protein that animal in-vivo content is most, distribution is most wide, is widely present in
The positions such as connective tissue, skin, bone, internal organ and tendon, ligament, sclera are the main constituents of extracellular matrix, wherein
Type I collagen is most widely used.Collagen has low immunogenicity, controlled degradation, catabolite nontoxic, includes to promote
Cell adherence and the RGD of growth (are made of) structural domain arginine, glycine and aspartic acid, can induce cell migration, stimulation
Cell Proliferation is relatively early one of the biomaterial ratified by FDA and SFDA.Active collagen can with fibrin, glycosaminoglycan,
Chitosan, alginate etc. are built into compound rest or growth factor-loaded such as bFGF, BMP or loaded gene, stem cell etc.,
For promoting the reparation of the tissues such as bone, muscle, artificial blood vessel, nerve, cornea, released in wound dressing, artificial skin and drug
Putting equal fields has boundless application prospect.
Bioactivity glass is the biomaterial of a kind of function admirable, has good bioactivity and biocompatibility,
Chemical bonding can be formed between material interface and body bone tissue as Bone Defect Repari implant, induce the reparation of bone with again
It is raw.
Summary of the invention
It is an object of the invention to provide a kind of porous titanium alloy surface biological glass in place of overcome the deficiencies in the prior art
Glass/polycaprolactone/collagenic coating and preparation method thereof enhances the combination of bio-vitric/collagenic coating and titanium alloy substrate, improves
The biocompatibility of titanium alloy material and tissue repairing ability.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method, comprising the following steps:
(1) bio-vitric is mixed with hexafluoroisopropanol, 1~3h of ultrasound;
(2) collagen and polycaprolactone are added in the hexafluoroisopropanol in step (1) after ultrasound, stir 4~8h, is given birth to
Object glass/polycaprolactone/collagen mixed solution;
(3) porous titanium alloy is successively cleaned by ultrasonic each 3 times through acetone, ethyl alcohol, pure water;
(4) bio-vitric/polycaprolactone/collagen mixed solution for obtaining step (2) is through electrostatic spraying in titanium alloy table
On face, after vacuum drying, the porous titanium alloy surface biological glass/polycaprolactone/collagenic coating is obtained.
Electrostatic Spray Technology is combined in above-mentioned technical proposal, constructs bio-vitric/gather oneself simultaneously on porous titanium alloy surface
Lactone/collagen, simple process is convenient, and bio-vitric/polycaprolactone/collagen is tightly combined with titanium alloy substrate, not easily to fall off, applies
Layer and can be coexisted with titanium alloy surface porous structure, titanium alloy surface structure will not be completely covered in coating;On the other hand, biological
Glass/polycaprolactone/collagen improves biocompatibility and the tissue repairing ability of titanium alloy material, mentions for titanium alloy implant
For more stable chemical bonding and higher bioactivity, it is more advantageous to growing into for freshman bone tissue.
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
Preferred embodiment, the bio-vitric are CaO-P2O5-SiO2Bio-vitric, the chemical component SiO of the bio-vitric2:
P2O5: CaO molar ratio is 55~65:2~5:30~40.
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
A kind of preferred embodiment, in the bio-vitric/polycaprolactone/collagen mixed solution, the mass fraction of polycaprolactone is 5%
~15%, the mass fraction of collagen is 0.5%~6%, and the mass fraction of bio-vitric is 1%~20%.
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
Preferred embodiment, in the bio-vitric/polycaprolactone/collagen mixed solution, the mass ratio of collagen and bio-vitric is 1:5
~15.
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
Preferred embodiment, in the bio-vitric/polycaprolactone/collagen mixed solution, the mass ratio of collagen and bio-vitric is 1:
6。
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
Preferred embodiment, in the bio-vitric/polycaprolactone/collagen mixed solution, the mass fraction of polycaprolactone is 10%, glue
Former mass fraction is 2%, and the mass fraction of bio-vitric is 16%.
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
Preferred embodiment, in the step (5), the control parameter of electrostatic spraying are as follows: electrostatic potential 15kV, syringe needle and sample distance are
15cm, sample introduction speed are 1~15mL/min, and the electrostatic spraying time is 5s~5min.
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
Preferred embodiment, in the step (5), the control parameter of electrostatic spraying are as follows: electrostatic potential 15kV, syringe needle and sample distance are
15cm, sample introduction speed are 2~5mL/min, and the electrostatic spraying time is 15~60s.
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
Preferred embodiment, the porous titanium alloy are differential arc oxidation porous titanium alloy.
The present invention also provides the porous titanium alloy surface biological glass/polycaprolactone being prepared according to above-mentioned method/
Collagenic coating.
Compared with prior art, present invention has an advantage that
Present invention combination Electrostatic Spray Technology constructs bio-vitric/polycaprolactone/collagen on porous titanium alloy surface simultaneously
Composite coating, simple process is convenient, and spray efficiency is high, and bio-vitric/polycaprolactone/collagenic coating is tight in conjunction with titanium alloy substrate
It is close, it is not easily to fall off, it coating and can be coexisted with porous titanium alloy surface by micro-arc oxidation structure;On the other hand, bio-vitric/gather oneself
Lactone/collagenic coating improves biocompatibility and the tissue repairing ability of titanium alloy material, provides more for titanium alloy implant
Stable chemical bonding and higher bioactivity, are more advantageous to growing into for freshman bone tissue.
Specific embodiment
Purposes, technical schemes and advantages in order to better illustrate the present invention, below in conjunction with specific embodiment to the present invention
It further illustrates.It will be appreciated by those skilled in the art that described herein, specific examples are only used to explain the present invention, not
For limiting the present invention.
Test method as used in the following examples is conventional method unless otherwise specified;Institute in following embodiments
Material, reagent for using etc., are commercially available unless otherwise specified.
Porous differential arc oxidization surface is formed using the differential arc oxidation method processing titanium alloy of this field routine in the present invention.
Embodiment 1
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
A kind of embodiment, porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method packet described in the present embodiment
Include following steps:
(1) bio-vitric is mixed with hexafluoroisopropanol, ultrasonic 1h, the chemical component SiO of the bio-vitric2: P2O5:
CaO molar ratio is 61:4:35;
(2) collagen and polycaprolactone are added in the hexafluoroisopropanol in step (1) after ultrasound, at room temperature magnetic agitation
6h, obtains bio-vitric/polycaprolactone/collagen mixed solution, in the bio-vitric/polycaprolactone/collagen mixed solution, gathers
The mass fraction of caprolactone is 10%, and the mass fraction of collagen is 2%, and the mass fraction of bio-vitric is 16%;
(3) successively it is cleaned by ultrasonic differential arc oxidation porous titanium alloy using acetone, ethyl alcohol, pure water, every kind of reagent cleans 3 times,
Each 10min is dried in vacuum oven after cleaning;
(4) bio-vitric/collagen blend solution that step (2) obtains is transferred in 20mL syringe, replaces Static Spinning
Silk syringe needle, is fixed on sample injector.High-voltage power voltage is adjusted to 15kV, sample injector speed be adjusted to 2mL/h, syringe needle and sample away from
From being adjusted to 15cm, debugging machine at strong illumination syringe needle, until visible spray sprays, starts to carry out sample preparation, using solid
Determine auxiliary accessories sample one-storey house is fixed on receiver, bottom cylindrical face respectively sprays the corresponding time to sample up and down, then replaces
Fixed auxiliary accessories are fixed to sample is edge-on on receiver, each electrostatic spraying 30s before and after sample cylinder side, after spraying
Titanium alloy is placed in vacuum drying, obtains the porous titanium alloy surface biological glass/polycaprolactone/collagenic coating.
Embodiment 2
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
A kind of embodiment, porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method packet described in the present embodiment
Include following steps:
(1) bio-vitric is mixed with hexafluoroisopropanol, ultrasonic 3h, the chemical component SiO of the bio-vitric2: P2O5:
CaO molar ratio is 55:5:40;
(2) collagen and polycaprolactone are added in the hexafluoroisopropanol in step (1) after ultrasound, at room temperature magnetic agitation
5h, obtains bio-vitric/polycaprolactone/collagen mixed solution, in the bio-vitric/polycaprolactone/collagen mixed solution, gathers
The mass fraction of caprolactone is 5%, and the mass fraction of collagen is 1%, and the mass fraction of bio-vitric is 15%;
(3) successively it is cleaned by ultrasonic differential arc oxidation porous titanium alloy using acetone, ethyl alcohol, pure water, every kind of reagent cleans 3 times,
Each 10min is dried in vacuum oven after cleaning;
(4) bio-vitric/collagen blend solution that step (2) obtains is transferred in 20mL syringe, replaces Static Spinning
Silk syringe needle, is fixed on sample injector.High-voltage power voltage is adjusted to 15kV, sample injector speed be adjusted to 5mL/h, syringe needle and sample away from
From being adjusted to 15cm, debugging machine at strong illumination syringe needle, until visible spray sprays, starts to carry out sample preparation, using solid
Determine auxiliary accessories sample one-storey house is fixed on receiver, bottom cylindrical face respectively sprays the corresponding time to sample up and down, then replaces
Fixed auxiliary accessories are fixed to sample is edge-on on receiver, each electrostatic spraying 60s before and after sample cylinder side, after spraying
Titanium alloy is placed in vacuum drying, obtains the porous titanium alloy surface biological glass/polycaprolactone/collagenic coating.
Embodiment 3
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
A kind of embodiment, porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method packet described in the present embodiment
Include following steps:
(1) bio-vitric is mixed with hexafluoroisopropanol, ultrasonic 2h, the chemical component SiO of the bio-vitric2: P2O5:
CaO molar ratio is 65:2:33;
(2) collagen and polycaprolactone are added in the hexafluoroisopropanol in step (1) after ultrasound, at room temperature magnetic agitation
44h, obtains bio-vitric/polycaprolactone/collagen mixed solution, in the bio-vitric/polycaprolactone/collagen mixed solution,
The mass fraction of polycaprolactone is 15%, and the mass fraction of collagen is 4%, and the mass fraction of bio-vitric is 20%;
(3) successively it is cleaned by ultrasonic differential arc oxidation porous titanium alloy using acetone, ethyl alcohol, pure water, every kind of reagent cleans 3 times,
Each 10min is dried in vacuum oven after cleaning;
(4) bio-vitric/collagen blend solution that step (2) obtains is transferred in 20mL syringe, replaces Static Spinning
Silk syringe needle, is fixed on sample injector.High-voltage power voltage is adjusted to 15kV, sample injector speed be adjusted to 1mL/h, syringe needle and sample away from
From being adjusted to 15cm, debugging machine at strong illumination syringe needle, until visible spray sprays, starts to carry out sample preparation, using solid
Determine auxiliary accessories sample one-storey house is fixed on receiver, bottom cylindrical face respectively sprays the corresponding time to sample up and down, then replaces
Fixed auxiliary accessories are fixed to sample is edge-on on receiver, each electrostatic spraying 5min before and after sample cylinder side, after spraying
Titanium alloy be placed in vacuum drying, obtain the porous titanium alloy surface biological glass/polycaprolactone/collagenic coating.
Embodiment 4
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
A kind of embodiment, porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method packet described in the present embodiment
Include following steps:
(1) bio-vitric is mixed with hexafluoroisopropanol, ultrasonic 2h, the chemical component SiO of the bio-vitric2: P2O5:
CaO molar ratio is 65:5:30;
(2) collagen and polycaprolactone are added in the hexafluoroisopropanol in step (1) after ultrasound, at room temperature magnetic agitation
8h, obtains bio-vitric/polycaprolactone/collagen mixed solution, in the bio-vitric/polycaprolactone/collagen mixed solution, gathers
The mass fraction of caprolactone is 10%, and the mass fraction of collagen is 2%, and the mass fraction of bio-vitric is 12%;
(3) successively it is cleaned by ultrasonic differential arc oxidation porous titanium alloy using acetone, ethyl alcohol, pure water, every kind of reagent cleans 3 times,
Each 10min is dried in vacuum oven after cleaning;
(4) bio-vitric/collagen blend solution that step (2) obtains is transferred in 20mL syringe, replaces Static Spinning
Silk syringe needle, is fixed on sample injector.High-voltage power voltage is adjusted to 15kV, sample injector speed is adjusted to 15mL/h, syringe needle and sample
Distance is adjusted to 15cm, debugging machine, at strong illumination syringe needle, until visible spray sprays, starts to carry out sample preparation, use
Sample one-storey house is fixed on receiver by fixed auxiliary accessories, and bottom cylindrical face respectively sprays the corresponding time to sample up and down, is then set
It changes fixed auxiliary accessories and is fixed to sample is edge-on on receiver, each electrostatic spraying 15s before and after sample cylinder side, after spraying
Titanium alloy be placed in vacuum drying, obtain the porous titanium alloy surface biological glass/polycaprolactone/collagenic coating.
Embodiment 5
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
A kind of embodiment, porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method packet described in the present embodiment
Include following steps:
(1) bio-vitric is mixed with hexafluoroisopropanol, ultrasonic 1h, the chemical component SiO of the bio-vitric2: P2O5:
CaO molar ratio is 65:5:30;
(2) collagen and polycaprolactone are added in the hexafluoroisopropanol in step (1) after ultrasound, at room temperature magnetic agitation
6h, obtains bio-vitric/polycaprolactone/collagen mixed solution, in the bio-vitric/polycaprolactone/collagen mixed solution, gathers
The mass fraction of caprolactone is 9%, and the mass fraction of collagen is 6%, and the mass fraction of bio-vitric is 1%;
(3) successively it is cleaned by ultrasonic differential arc oxidation porous titanium alloy using acetone, ethyl alcohol, pure water, every kind of reagent cleans 3 times,
Each 10min is dried in vacuum oven after cleaning;
(4) bio-vitric/collagen blend solution that step (2) obtains is transferred in 20mL syringe, replaces Static Spinning
Silk syringe needle, is fixed on sample injector.High-voltage power voltage is adjusted to 15kV, sample injector speed is adjusted to 12mL/h, syringe needle and sample
Distance is adjusted to 15cm, debugging machine, at strong illumination syringe needle, until visible spray sprays, starts to carry out sample preparation, use
Sample one-storey house is fixed on receiver by fixed auxiliary accessories, and each electrostatic spraying 5s of bottom cylindrical face above and below sample, then displacement is solid
Determine auxiliary accessories and is fixed to sample is edge-on on receiver, each electrostatic spraying 3min before and after sample cylinder side, after spraying
Titanium alloy is placed in vacuum drying, obtains the porous titanium alloy surface biological glass/polycaprolactone/collagenic coating.
Embodiment 6
As porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method of the present invention
A kind of embodiment, porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method packet described in the present embodiment
Include following steps:
(1) bio-vitric is mixed with hexafluoroisopropanol, ultrasonic 1h, the chemical component SiO of the bio-vitric2: P2O5:
CaO molar ratio is 61:4:35;
(2) collagen and polycaprolactone are added in the hexafluoroisopropanol in step (1) after ultrasound, at room temperature magnetic agitation
6h, obtains bio-vitric/polycaprolactone/collagen mixed solution, in the bio-vitric/polycaprolactone/collagen mixed solution, gathers
The mass fraction of caprolactone is 12%, and the mass fraction of collagen is 0.5%, and the mass fraction of bio-vitric is 18%;
(3) successively it is cleaned by ultrasonic differential arc oxidation porous titanium alloy using acetone, ethyl alcohol, pure water, every kind of reagent cleans 3 times,
Each 10min is dried in vacuum oven after cleaning;
(4) bio-vitric/collagen blend solution that step (2) obtains is transferred in 20mL syringe, replaces Static Spinning
Silk syringe needle, is fixed on sample injector.High-voltage power voltage is adjusted to 15kV, sample injector speed be adjusted to 8mL/h, syringe needle and sample away from
From being adjusted to 15cm, debugging machine at strong illumination syringe needle, until visible spray sprays, starts to carry out sample preparation, using solid
Determine auxiliary accessories sample one-storey house is fixed on receiver, bottom cylindrical face respectively sprays the corresponding time to sample up and down, then replaces
Fixed auxiliary accessories are fixed to sample is edge-on on receiver, each electrostatic spraying 3min before and after sample cylinder side, after spraying
Titanium alloy be placed in vacuum drying, obtain the porous titanium alloy surface biological glass/polycaprolactone/collagenic coating.
Inventor determines the conjunction between collagen solution concentration range, collagen and bio-vitric gel by test repeatedly
Suitable ratio, the ratio of collagen solution concentration, collagen and bio-vitric gel will affect electrostatic spraying effect and bio-vitric/
The bond strength of collagenic coating and matrix.
1, vitro cytotoxicity test
Sample: bio-vitric/collagenic coating titanium alloy artificial bone prepared by embodiment 1.
(1) cell strain
Marrow Mesenchymal Stem Cells (mBMSCs, ATCC CRL-12424).
(2) preparation of test liquid
1) sample leaching liquor: it is filled with extraction medium in the ratio of 0.2g/mL, is extracted for 24 hours at 37 DEG C.
2) it blank control: is placed for 24 hours at same batch culture medium (1 ×) 37 DEG C, as blank control liquid.
3) negative control: taking high density polyethylene (HDPE), is cleaned and is dried with ultrapure water, shreds after ultraviolet light irradiation overnight.By table
Area 3cm2The ratio of/mL is added at same batch culture medium (1 ×) 37 DEG C and extracts for 24 hours, as negative controls.
4) positive control: the pvc material (confirmed reproducible cytotoxicity) containing organotin additive, with super
Pure water, which is cleaned, to be dried, and ultraviolet light irradiation overnight, is filled with extraction medium in the ratio of 0.2mg/mL, is extracted at 37 DEG C for 24 hours, as sun
Property control.
(3) test method
It will cultivate after the eugonic cell of 48~72h is digested with digestive juice and cell culture medium be added, blown with liquid-transfering gun
It beats after mixing and counts under the microscope, cell suspension is configured to density 1.5 × 105Cell/mL is inoculated in diameter 35mm culture
Ware, every ware 2mL, totally 12 ware.Set CO2Incubator (CO2Concentration of volume percent 5%) 37 DEG C of cultures are to closely converging unilateral cell shape
At.
Discard original fluid.It is separately added into each 3 ware of blank control liquid, negative control, positive control solution, sample leaching liquor,
0.2mL calf serum is added in every every ware of ware 1.8mL.Set CO237 DEG C of culture 48h of incubator.
(4) test result
After 48h is cultivated, by culture dish to microscopically observation, 1 the results are shown in Table.
1 cell toxicity test result of table
(5) conclusion:
Test sample group cell-cytotoxic reaction rank is 0 point.Determine by relevant criterion, test sample group cell-cytotoxic reaction journey
Degree is acellular poison.
The bio-vitric that above embodiments are selected is the bio-vitric microballoon that partial size is 300~500nm, and partial size is smaller,
It is matched with electrostatic spinning syringe needle, syringe needle blocking can be avoided in electrostatic spray process.
Present invention combination Electrostatic Spray Technology constructs bio-vitric/collagen composite coating simultaneously on porous titanium alloy surface,
Simple process is convenient, and spray efficiency is high, is easy to industrialization;Bio-vitric/collagenic coating is tightly combined with titanium alloy substrate, is not easy
It falling off, coating and can be coexisted with porous titanium alloy surface by micro-arc oxidation structure, rough surface can promote the adherency of osteocyte,
Be conducive to growing into and integrating for bone;On the other hand, bio-vitric/collagenic coating improve titanium alloy material biocompatibility and
Tissue repairing ability provides more stable chemical bonding and higher bioactivity for titanium alloy implant, is more advantageous to new life
Bone tissue is grown into.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. a kind of porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method, which is characterized in that including
Following steps:
(1) bio-vitric is mixed with hexafluoroisopropanol, 1~3h of ultrasound;
(2) collagen and polycaprolactone are added in the hexafluoroisopropanol in step (1) after ultrasound, stir 4~8h, obtains biological glass
Glass/polycaprolactone/collagen mixed solution;
(3) porous titanium alloy is successively cleaned by ultrasonic each 3 times through acetone, ethyl alcohol, pure water;
(4) bio-vitric/polycaprolactone/collagen mixed solution for obtaining step (2) through electrostatic spraying on titanium alloy surface,
After vacuum drying, the porous titanium alloy surface biological glass/polycaprolactone/collagenic coating is obtained.
2. porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method according to claim 1,
It is characterized in that, the bio-vitric is CaO-P2O5-SiO2Bio-vitric, the chemical component SiO of the bio-vitric2: P2O5:
The molar ratio of CaO is 55~65:2~5:30~40.
3. porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method according to claim 1,
It is characterized in that, in the bio-vitric/polycaprolactone/collagen mixed solution, the mass fraction of polycaprolactone is 5%~
15%, the mass fraction of collagen is 0.5%~6%, and the mass fraction of bio-vitric is 1%~20%.
4. porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method according to claim 1,
It is characterized in that, in the bio-vitric/polycaprolactone/collagen mixed solution, the mass ratio of collagen and bio-vitric be 1:5~
15。
5. porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method according to claim 1,
It is characterized in that, the mass ratio of collagen and bio-vitric is 1:6 in the bio-vitric/polycaprolactone/collagen mixed solution.
6. porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method according to claim 1,
It is characterized in that, the mass fraction of polycaprolactone is 10%, collagen in the bio-vitric/polycaprolactone/collagen mixed solution
Mass fraction be 2%, the mass fraction of bio-vitric is 16%.
7. porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method according to claim 1,
It is characterized in that, in the step (5), the control parameter of electrostatic spraying are as follows: electrostatic potential 15kV, syringe needle and sample distance are
15cm, sample introduction speed are 1~15mL/min, and the electrostatic spraying time is 5s~5min.
8. porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method according to claim 1,
It is characterized in that, in the step (5), the control parameter of electrostatic spraying are as follows: electrostatic potential 15kV, syringe needle and sample distance are
15cm, sample introduction speed are 2~5mL/min, and the electrostatic spraying time is 15~60s.
9. porous titanium alloy surface biological glass/polycaprolactone/collagenic coating preparation method according to claim 1,
It is characterized in that, the porous titanium alloy is differential arc oxidation porous titanium alloy.
10. according to claim 1 ,~the porous titanium alloy surface biological glass that 10 described in any item methods are prepared/gathers oneself
Lactone/collagenic coating.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810237720.8A CN110292656A (en) | 2018-03-21 | 2018-03-21 | A kind of porous titanium alloy surface biological glass/polycaprolactone/collagenic coating and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810237720.8A CN110292656A (en) | 2018-03-21 | 2018-03-21 | A kind of porous titanium alloy surface biological glass/polycaprolactone/collagenic coating and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN110292656A true CN110292656A (en) | 2019-10-01 |
Family
ID=68025562
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810237720.8A Pending CN110292656A (en) | 2018-03-21 | 2018-03-21 | A kind of porous titanium alloy surface biological glass/polycaprolactone/collagenic coating and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110292656A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114732945A (en) * | 2022-04-13 | 2022-07-12 | 广西农业职业技术大学 | Method for improving bioactivity of titanium alloy bone |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20170091447A (en) * | 2016-02-01 | 2017-08-09 | (주)엠티아이지 | Surface treating method of titanium or titanium alloy |
-
2018
- 2018-03-21 CN CN201810237720.8A patent/CN110292656A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20170091447A (en) * | 2016-02-01 | 2017-08-09 | (주)엠티아이지 | Surface treating method of titanium or titanium alloy |
Non-Patent Citations (5)
Title |
---|
ANA CIVANTOS ET AL: "Titanium coatings and surface modifications :toward clinically use ful bioactive implants", 《ACS BIOMATERIALS SCIENCE AND ENGINEERING》 * |
MOSTAFA YAZDIMAMAGHANI ET AL: "surface modification of biodegradable porous Mg bone scaffold using polycaprolactone bioactive glass composite", 《MATERIALS SCIENCE AND ENGINEERING C》 * |
冉丹丹: "纯钛表面微弧氧化结合1型胶原对成骨细胞黏附增殖的影响", 《华西医学》 * |
李理: "《电脑工业设计》", 31 December 2001 * |
轻工业部广州轻工业学校: "《塑料成型工学》", 30 April 1990 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114732945A (en) * | 2022-04-13 | 2022-07-12 | 广西农业职业技术大学 | Method for improving bioactivity of titanium alloy bone |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101302486B (en) | Acetobacter xylinum and method for preparing nano-cellulose skin tissue repair material by using the same | |
CN107213529B (en) | Preparation method of degradable medical high-molecular three-dimensional material for improving adhesion and osteogenic performance of osteoblasts | |
CN1644221A (en) | Composite material for porous material and gel use thereof | |
CN110478528B (en) | Preparation method and application of novel tissue repair promoting material | |
CN101318032A (en) | Small-diameter tissue engineering artificial blood vessel and preparation method thereof | |
CN109224134A (en) | A kind of novel inducting osseous tissue regeneration duplicature and preparation method thereof | |
CN101366977A (en) | Tissue mending material with biological activity and preparation method thereof | |
Olyveira et al. | Human dental pulp stem cell behavior using natural nanotolith/bacterial cellulose scaffolds for regenerative medicine | |
CN107349475A (en) | Artificial organ engineering skin that nano fibrous membrane is layering with stem cell and preparation method thereof | |
CN109157305A (en) | Combined artificial cornea and preparation method thereof | |
CN106806940A (en) | A kind of preparation method of nano hydroxylapatite doped porous Bionics Bone support | |
Nakagawa et al. | Osteoclastogenesis on tissue-engineered bone | |
CN109793934B (en) | Tissue-engineered myocardial patch and preparation and application thereof | |
CN107158465B (en) | Preparation method of bone scaffold composite material | |
CN111298198B (en) | Double-layer absorbable bionic barrier film and preparation method and application thereof | |
CN110292654A (en) | A kind of titanium alloy surface collagenic coating and preparation method thereof loading antibacterial polypeptide | |
CN102294049A (en) | Bioactive glass and chitosan composite bone repair material and preparation method and application thereof | |
CN109453430A (en) | A kind of collagen of hydroxyapatite coating layer-graphene oxide biomimetic material and preparation method thereof | |
CN108853581B (en) | High-molecular polymer hydrogel composite Medpor prosthetic eye holder and preparation method thereof | |
CN112426569B (en) | Inorganic-organic composite living cell scaffold and preparation method and application thereof | |
CN110292656A (en) | A kind of porous titanium alloy surface biological glass/polycaprolactone/collagenic coating and preparation method thereof | |
CN102302807A (en) | Stem cell-loading chitosan biofilm polypropylene mesh and preparation method thereof | |
CN110882416A (en) | Preparation method and application of bionic composite nanofiber scaffold material | |
CN1234429C (en) | Artificial skin, preparing method and application thereof | |
CN111214703B (en) | iPS-derived myocardial cell composite patch and preparation and application thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191001 |
|
RJ01 | Rejection of invention patent application after publication |