CN107693848A - A kind of biomedical metallic material and preparation method thereof - Google Patents
A kind of biomedical metallic material and preparation method thereof Download PDFInfo
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- CN107693848A CN107693848A CN201710988994.6A CN201710988994A CN107693848A CN 107693848 A CN107693848 A CN 107693848A CN 201710988994 A CN201710988994 A CN 201710988994A CN 107693848 A CN107693848 A CN 107693848A
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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Abstract
The invention provides a kind of biomedical metallic material, it is related to biology medical material technical field, in order to solve the problems, such as existing bone renovating material anti-microbial property it is poor, intolerant to the bad technology of the biomechanical compatibility of burn into and bone, the invention provides a kind of biomedical metallic material.The present invention is by the characteristic of extracellular matrix protein come the bionical biomedical metal material that designs, pass through the microenvironment being connected with each other between analog cell, induction bone tissue is attached on titanium alloy surface, a large amount of Porcine HGFs are secreted, promote clearing up and discharging for inflammatory cell (such as neutrophil leucocyte, macrophage);Migrated, bred and broken up by bone and its cells, ultimately form new functional tissue, with with the biomechanical compatibility of bone it is preferable the characteristics of, and the biomedical metallic material for preparing of the present invention also has the characteristics of hardness is high, corrosion resistance is strong, strong antibacterial.
Description
Technical field
The present invention relates to biology medical material technical field, especially, is related to a kind of biomedical metallic material and its system
Preparation Method.
Background technology
Biomedical metallic material refers to a kind of metal or alloy for being used as biomaterial, also known as surgery metal material.
It is a kind of bio-inert material.Most common purposes be as the load materials applications such as artificial prosthesis, orthopedic thing in oral cavity, rectify
The sclerous tissues such as shape surgery system.The medical metal material of clinical practice at present mainly has stainless steel, cobalt-base alloys, titanium and titanium alloy
Etc. several major classes.In addition with marmem, noble metal and simple metal tantalum, niobium, zirconium etc..With bioceramic and biological high score
Sub- material is compared.
Applied in bone renovating material is exactly earliest metal material.Metal and alloy are with high intensity, endurance and easy processing
Deng premium properties, clinically occupy critical role.At present, be subjected to the bone of high load, tooth portion is still regarded as first choice
Implantation material.Most important application has:Solid plate, screw, joint prosthesis and tooth root planting body etc. in fracture.Conventional Bone Defect Repari
Material mainly has stainless steel (ferrous alloy), cobalt-base alloys and titanium-base alloy.But the structure of medical metal material and property with
Bone tissue is differed greatly, and chemical key, which occurs, with bone tissue generally unlike bioactive materials is combined.And metal material
Under physiological fluid effect, energy dissolution metal ion, these releasers do not have compatibility in itself under various corrosion, wears,
The eubolism of biological tissue can not be participated in, biological tissue can produce rejection to it, and fiber bag is formed in surrounding materials
Thing is wrapped up in, with the extension of time, the ion or monomer of release increase, fiber integument also progressive additive, and gradually densification, calcium
Change, even result in fiber-like neoplasia, it is same with rejection phenomenons such as hydrops, inflammation and necrosis etc.;It is and most medical
Elastic Modulus for Metals is too high compared with bone, bad with the biomechanical compatibility of bone, easily causes bone stress absorption, causes planting body loose
Dynamic, therefore, research and development performance is more excellent, the more preferable new bio medical metal material of biocompatibility be material worker and
The problem of medical personnel's common concern.
The content of the invention
Present invention aims at a kind of biomedical metallic material and preparation method thereof is provided, to solve existing Bone Defect Repari material
Expect anti-microbial property it is poor, intolerant to burn into and bone biomechanical compatibility bad technology the problem of.
To achieve the above object, the invention provides a kind of biomedical metallic material and preparation method thereof.
A kind of biomedical metallic material of the present invention, by base material, active layer, antibiotic layer, bioactivity egg
White is formed, and active layer is formed in substrate material surface coating activator, in the activation layer surface coating antibacterial dosage form
Into antibiotic layer, biological activity protein dosage form is coated into biological activity protein layer in the antibacterial layer surface.
Further, described base material is porous titanium alloy, and the porous titanium alloy is by pore former and parent metal powder
Compare 1-3 according to weight:9-12, which is mixed with, to be formed.
Further, described pore former is the stearic acid particles that particle diameter is 400 μm.
Further, described parent metal powder is by percentage to the quality 6-8% zirconium powders, 0.5-0.9% niobiums powder,
0.4-0.7% tantalum powders, 0.1-0.3% boron powder, surplus is titanium valve.
Further, described activator, it is made up of the raw material of following parts by weight:5-8 parts hydroxyapatite, 1.5-2.7
Part dicalcium silicate, 4-7 parts chitin, 2.1-3.6 parts polyamide, 1.2-2.8 parts polyaminoacid, 2.3-2.7 parts calcium sulfate, 2-3
Part poly- (2- oxazolines), 15-30 part polyethylene glycol 1.5-3.5 part modified starches.
Further, described biological activity protein agent, is made up of the raw material of following parts by weight:0.5-1.5 part chitins gather
Sugar, 2-4 parts calcium alginate, 5-9 parts silk fibroin, 1-3 parts gelatin, 1.5-2.5 parts phosphoserine, 2-4 part fiber eggs
In vain, appropriate distilled water.
Further, described antiseptic, it is made up of the raw material of following parts by weight:1-3.5 parts nano zine oxide, 1-3 parts
Polyurethane, 2.5-4.5 parts chitosan, 1.2-2.4 parts poly butyric ester, 0.5-1.6 parts Nano Silver, 2.5-3.8 parts PLA,
2-6 part hydroxyacetic acids.
Further, described a kind of biomedical metallic material preparation method, specifically includes following steps:
1. prepared by base material:
A, take zirconium powder, niobium powder, tantalum powder, boron powder and titanium valve to be blended in high vacuum arc heating furnace by mass percentage to melt
Refining, 15min is stirred, pore former is added, is sufficiently stirred 30min, is finally pressed into blank;
B, blank is placed in 1000-1400 DEG C of environment and sintered, be incubated 1-4h, base material is obtained after furnace cooling;
2. prepared by activator:
A, in parts by weight, hydroxyapatite, calcium sulfate, dicalcium silicate mixing are taken, it is 200um to be crushed to particle diameter, then
Mixed powder is placed in 400-500 DEG C of environment and calcines 1-2h, is then to be protected in the environment that 300 DEG C of vacuums are 0.08 as temperature
Warm 40min, take out, room temperature is cooled in 60s, then be placed in 60-70 DEG C of environment and dry to constant weight;
B, will dry to constant weight mixed powder, then with modified starch, chitin, polyamide, polyaminoacid, poly- (2- oxazoles
Quinoline), polyethylene glycol mixing, be placed in ball mill, grind 30-40min, take out as in reactor, after stirring, heating is anti-
Kettle is answered to 120-160 DEG C, 50-70min is reacted, temperature of charge is then down to 50-60 DEG C, it is standby to obtain activator;
3. prepared by antiseptic:
In parts by weight, nano zine oxide, chitosan, Nano Silver, PLA, hydroxyacetic acid mixing is taken to be placed in high-speed stirred
In machine, rotating speed 2000r/min is controlled, stirs 10min, then is well mixed to be placed in polyurethane, poly butyric ester and disperses at a high speed
Machine disperses 30-40min in 1500r/min, then is placed in constant temperature 40-50min in 70-80 DEG C of water bath with thermostatic control, and it is small to stand 24 at room temperature
When, centrifugation, supernatant is antiseptic;
4. prepared by bioprotein agent:
A, in parts by weight, silk fibroin, fibrin are placed at -20 DEG C respectively and freeze 15h;
B, the distilled water that chitosan, calcium alginate, phosphoserine and gelatin are mixed to 1 times of mixture weight of addition is ground
1-1.5h is ground, is then well mixed with silk fibroin, fibrin, is placed in oscillator and handles 20min, filtering precipitation,
Supernatant is bioprotein agent;
5. prepared by biomedical metallic material:
The base material of preparation is placed in electric furnace and preheated, then 2. activator is coated uniformly on base material by step
Surface, 15-20min is handled the base material coated with activator in 30-40 DEG C of environment afterwards, form active layer;Again
With 3. antiseptic is coated uniformly on active layer the step of preparation, the base material coated with active layer and antibiotic layer is existed afterwards
15-20min is handled in 35-40 DEG C of environment, forms antibiotic layer;Finally 4. bioprotein agent that step is prepared is coated uniformly on anti-
Bacterium layer surface, the base material coated with active layer, antibiotic layer and bioprotein layer is handled in 37-40 DEG C of environment afterwards
15-20min, produce biomedical metallic material.
The invention has the advantages that:
1st, the present invention passes through analog cell by the characteristic of extracellular matrix protein come the bionical biomedical metal material designed
Between the microenvironment that is connected with each other, induction bone tissue is attached on titanium alloy surface, secretes a large amount of Porcine HGFs, promotes inflammatory thin
Born of the same parents (such as neutrophil leucocyte, macrophage) clears up and discharges;Migrated, bred and broken up by bone and its cells, ultimately formed new
Functional tissue, have with the biomechanical compatibility of bone it is preferable the characteristics of, and the bio-medical metal for preparing of the present invention
Material also has the characteristics of hardness is high, corrosion resistance is strong, strong antibacterial.
2nd, titanium alloy has good mechanical property and nontoxicity.But the biology of growth in the inorganizable progress of its dense body
Environment, so poor with the compatibility of bone, in order to preferably improve the compatibility of bone tissue and titanium alloy, thus prior art compared with
More uses porous titanium alloy, and not only its mechanical performance matches porous titanium alloy very much with human body bone, and greatly reduces
The generation of stress, compression performance and the hole of artificial bone are advantageous to the growth of green bone, therefore can reach more natural fixation
Purpose, therefore be largely used for medical and health industry.In conventional porous titanium alloy preparation process, the more use of pore creating material
Ammonium hydrogen carbonate, and ammonium hydrogen carbonate pore creating material is easily decomposed, and causes the quality of each metal-powder and ammonium hydrogen carbonate in titanium alloy
Proportioning deviates larger, and is formed in the porous material after the gill shape ammonium bicarbonate breaks down of commercialization in sintering process sharp
Corner apertures gap is more, and easily producing stress concentration in sharp corner under external force triggers fracture, greatly influences the intensity of titanium alloy,
Therefore, the present invention using new stearic acid as pore creating material, due to stearic acid particles shape spherical in shape, and density ratio ammonium hydrogen carbonate
It is low, therefore under identical mass fraction, the volume shared by stearic acid particles is larger, when suppressing titanium alloy to the hole of titanium alloy
Rate influence is smaller, can effectively improve the mechanical property of titanium alloy, show through overtesting, is prepared compared with using ammonium hydrogen carbonate
Porous titanium alloy mechanical property it is more excellent, apparent porosity improves 7.98%, and incompressible intensity improves 8.45MPa.With hard
The increase of resin acid content, then titanium alloy porosity is higher, but porosity is higher, then alloy strength declines, and it is internal effective
Loaded area can also greatly reduce, therefore, test proves that, when parent metal powder and stearic acid weight ratio are 2:When 11,
Alloy mechanical property is also more excellent while alloy porosity is high, and porosity reaches 69.49%, and compression strength reaches 69.26MPa.
3rd, in order that porous titanium alloy and bone tissue prepared by the present invention have more preferable biocompatibility, the present invention utilizes
Bionics, active layer, antibiotic layer and biological activity protein layer are sequentially coated with porous titanium alloy surface.The present invention will be prepared into
Activator is coated on porous titanium alloy surface first, and porous titanium alloy surface is activated, further enhances porous titanium alloy
With the compatibility of bone tissue, and the activator for preparing of the present invention have it is nontoxic, non-stimulated, will not allergic reaction, not mutagenesis,
Will not haemolysis, do not destroy the characteristic of biological tissue, in the preparation process of activator, be not only commonly used to modified titanium alloy surface
The hydroxyapatite of biocompatibility, promote adhesion, the propagation of Gegenbaur's cell, promote New born formation, and also added poly- ammonia
Base acid, calcium sulfate, can further guide new Bone Ingrowth and with the firm bony union of host's ostosis, while also contain silicon
Sour dicalcium, on the one hand not only coating is promoted preferably to be combined with porous titanium alloy so that coating is not susceptible to come off, the opposing party
Face, can also be by electrostatic attraction, by the Ca in bone tissue on dicalcium silicate particle2+、PO4 3-、HPO4 2-It is attracted to surface deposition
Also adsorbed into calcium phosphate, and by external hydroxyapatite, progressively deposition forms class bone podolite layer and not only carried
The high utilization ratio of hydroxyapatite, also further enhances the biocompatibility with bone tissue.
4th, one layer of antiseptic is coated with again in activation layer surface, form one layer of antibiotic layer again on the surface of active layer, this
Not only with the addition of the nano zine oxide with good bacteriostasis when invention prepares antiseptic, Nano Silver also added PLA,
The compound that hydroxyacetic acid is formed with the hydroxyapatite in activator, not only increases the antimicrobial of biomedical metal material
Performance, and metal material embedded postoperative complications are reduced, rejection phenomenon is reduced, enhances biomedical metal material and bone tissue
Biocompatibility.
5th, be coated with one layer of bioprotein agent again in antibacterial layer surface, the bioprotein agent by chitosan, calcium alginate,
Phosphoserine, fibroin, fibrin etc. form, and fibrin is one of albumen common in body bone tissue, addition
Fibrin can further mitigate the rejection of body, promote bone tissue preferably to be merged with biomedical metal material, together
Shi Tianjia fibroin, phosphoserine, with the chitosan of addition polymer is formed, not only play good antibacterial of chitosan
Effect, and the chitosan-fibroin-phosphoserine polymer formed can significantly improve early stage of Gegenbaur's cell and stick
It is attached, there is the effect that remarkably promotes, and the chitosan and calcium alginate added to the growing multiplication of Gegenbaur's cell, not only improve
Biomedical metallic material microbial resistance and corrosion resistance, and the adhesiveness of medical metal material and bone tissue is improved, promote
Enter body chondrocyte growth, and then promote the growth of cartilaginous tissue, moreover it is possible to accelerate the healing of wound.
In addition to objects, features and advantages described above, the present invention also has other objects, features and advantages.
The present invention is further detailed explanation below.
Embodiment
Embodiments of the invention are described in detail below, but the present invention can be limited and covered according to claim
Multitude of different ways implement.
Embodiment 1
A kind of biomedical metallic material, it is made up of base material, active layer, antibiotic layer, biological activity protein layer, in institute
State substrate material surface coating activator and form active layer, antibiotic layer is formed in the activation layer surface coating antiseptic, in institute
State antibacterial layer surface and coat biological activity protein dosage form into biological activity protein layer.
Described base material is porous titanium alloy, and the porous titanium alloy is by pore former and parent metal powder according to weight
Than 1:9 are mixed with and form;Described pore former is the stearic acid particles that particle diameter is 400 μm;Described parent metal powder, with
Mass percent is calculated as 6% zirconium powder, 0.5% niobium powder, 0.4% tantalum powder, 0.1% boron powder, 93% titanium valve;Described activator, by
The raw material composition of following parts by weight:5 parts of hydroxyapatites, 1.5 parts of dicalcium silicates, 4 parts of chitins, 2.1 parts of polyamide, 1.2
Part polyaminoacid, 2.3 parts of calcium sulfate, 2 parts poly- (2- oxazolines), 15 parts of polyethylene glycol, 1.5 portions of modified starches;Described biology is living
Property protein agent, is made up of the raw material of following parts by weight:0.5 part of chitosan, 2 parts of calcium alginates, 5 parts of silk fibroins, 1
Part gelatin, 1.5 parts of phosphoserines, 2 parts of fibrins, appropriate distilled water;Described antiseptic, by the original of following parts by weight
Material composition:1 part of nano zine oxide, 1 part of polyurethane, 2.5 parts of chitosans, 1.2 parts of poly butyric esters, 0.5 part of Nano Silver, 2.5
Part PLA, 2 parts of hydroxyacetic acids.
A kind of described biomedical metallic material preparation method, specifically includes following steps:
1. prepared by base material:
A, take zirconium powder, niobium powder, tantalum powder, boron powder and titanium valve to be blended in high vacuum arc heating furnace by mass percentage to melt
Refining, 15min is stirred, pore former is added, is sufficiently stirred 30min, is finally pressed into blank;
B, blank is placed in 1000 DEG C of environment and sintered, be incubated 1h, base material is obtained after furnace cooling;
2. prepared by activator:
A, in parts by weight, hydroxyapatite, calcium sulfate, dicalcium silicate mixing are taken, it is 200um to be crushed to particle diameter, then
Mixed powder is placed in 400 DEG C of environment and calcines 1h, is then to be incubated in the environment that 300 DEG C of vacuums are 0.08 as temperature
40min, take out, room temperature is cooled in 60s, then be placed in 60 DEG C of environment and dry to constant weight;
B, will dry to constant weight mixed powder, then with modified starch, chitin, polyamide, polyaminoacid, poly- (2- oxazoles
Quinoline), polyethylene glycol mixing, be placed in ball mill, grind 30min, take out as in reactor, after stirring, heating response
Kettle reacts 50min, temperature of charge then is down into 50 DEG C, it is standby to obtain activator to 120 DEG C;
3. prepared by antiseptic:
In parts by weight, nano zine oxide, chitosan, Nano Silver, PLA, hydroxyacetic acid mixing is taken to be placed in high-speed stirred
In machine, rotating speed 2000r/min is controlled, stirs 10min, then is well mixed to be placed in polyurethane, poly butyric ester and disperses at a high speed
Machine disperses 30min in 1500r/min, then is placed in constant temperature 40min in 70 DEG C of waters bath with thermostatic control, stands 24 hours at room temperature, centrifugation, on
Clear liquid is antiseptic;
4. prepared by bioprotein agent:
A, in parts by weight, silk fibroin, fibrin are placed at -20 DEG C respectively and freeze 15h;
B, the distilled water that chitosan, calcium alginate, phosphoserine and gelatin are mixed to 1 times of mixture weight of addition is ground
1h is ground, is then well mixed with silk fibroin, fibrin, is placed in oscillator and handles 20min, filtering precipitation, supernatant
Liquid is bioprotein agent;
5. prepared by biomedical metallic material:
The base material of preparation is placed in electric furnace and preheated, then 2. activator is coated uniformly on base material by step
Surface, 15min is handled the base material coated with activator in 30 DEG C of environment afterwards, form active layer;Again with preparation
The step of 3. antiseptic be coated uniformly on active layer, afterwards to the base material coated with active layer and antibiotic layer in 35 DEG C of rings
15min is handled in border, forms antibiotic layer;4. bioprotein agent that step is prepared finally is coated uniformly on antibacterial layer surface, it
15min is handled in 37 DEG C of environment to the base material coated with active layer, antibiotic layer and bioprotein layer afterwards, produces biological doctor
Use metal material.
Embodiment 2
A kind of biomedical metallic material, it is made up of base material, active layer, antibiotic layer, biological activity protein layer, in institute
State substrate material surface coating activator and form active layer, antibiotic layer is formed in the activation layer surface coating antiseptic, in institute
State antibacterial layer surface and coat biological activity protein dosage form into biological activity protein layer.
Described base material is porous titanium alloy, and the porous titanium alloy is by pore former and parent metal powder according to weight
Than 3:12 are mixed with and form;Described pore former is the stearic acid particles that particle diameter is 400 μm;Described parent metal powder,
It is by percentage to the quality 8% zirconium powder, 0.9% niobium powder, 0.7% tantalum powder, 0.3% boron powder, 90.1% titanium valve;Described activation
Agent, it is made up of the raw material of following parts by weight:8 parts of hydroxyapatites, 2.7 parts of dicalcium silicates, 7 parts of chitins, 3.6 parts of polyamides
Amine, 2.8 parts of polyaminoacid, 2.7 parts of calcium sulfate, 3 portions of poly- (2- oxazolines), 30 parts of polyethylene glycol, 3.5 portions of modified starches;It is described
Biological activity protein agent, be made up of the raw material of following parts by weight:1.5 parts of chitosans, 4 parts of calcium alginates, 9 parts of silk silks
Fibroin, 3 parts of gelatin, 2.5 parts of phosphoserines, 4 parts of fibrins, appropriate distilled water;Described antiseptic, by following weight
The raw material composition of number:3.5 parts of nano zine oxides, 3 parts of polyurethane, 4.5 parts of chitosans, 2.4 parts of poly butyric esters, 1.6 parts
Nano Silver, 3.8 parts of PLAs, 6 parts of hydroxyacetic acids.
A kind of described biomedical metallic material preparation method, specifically includes following steps:
1. prepared by base material:
A, take zirconium powder, niobium powder, tantalum powder, boron powder and titanium valve to be blended in high vacuum arc heating furnace by mass percentage to melt
Refining, 15min is stirred, pore former is added, is sufficiently stirred 30min, is finally pressed into blank;
B, blank is placed in 1400 DEG C of environment and sintered, be incubated 4h, base material is obtained after furnace cooling;
2. prepared by activator:
A, in parts by weight, hydroxyapatite, calcium sulfate, dicalcium silicate mixing are taken, it is 200um to be crushed to particle diameter, then
Mixed powder is placed in 500 DEG C of environment and calcines 2h, is then to be incubated in the environment that 300 DEG C of vacuums are 0.08 as temperature
40min, take out, room temperature is cooled in 60s, then be placed in 70 DEG C of environment and dry to constant weight;
B, will dry to constant weight mixed powder, then with modified starch, chitin, polyamide, polyaminoacid, poly- (2- oxazoles
Quinoline), polyethylene glycol mixing, be placed in ball mill, grind 40min, take out as in reactor, after stirring, heating response
Kettle reacts 70min, temperature of charge then is down into 60 DEG C, it is standby to obtain activator to 160 DEG C;
3. prepared by antiseptic:
In parts by weight, nano zine oxide, chitosan, Nano Silver, PLA, hydroxyacetic acid mixing is taken to be placed in high-speed stirred
In machine, rotating speed 2000r/min is controlled, stirs 10min, then is well mixed to be placed in polyurethane, poly butyric ester and disperses at a high speed
Machine disperses 40min in 1500r/min, then is placed in constant temperature 50min in 80 DEG C of waters bath with thermostatic control, stands 24 hours at room temperature, centrifugation, on
Clear liquid is antiseptic;
4. prepared by bioprotein agent:
A, in parts by weight, silk fibroin, fibrin are placed at -20 DEG C respectively and freeze 15h;
B, the distilled water that chitosan, calcium alginate, phosphoserine and gelatin are mixed to 1 times of mixture weight of addition is ground
1.5h is ground, is then well mixed with silk fibroin, fibrin, is placed in oscillator and handles 20min, filtering precipitation, on
Clear liquid is bioprotein agent;
5. prepared by biomedical metallic material:
The base material of preparation is placed in electric furnace and preheated, then 2. activator is coated uniformly on base material by step
Surface, 20min is handled the base material coated with activator in 40 DEG C of environment afterwards, form active layer;Again with preparation
The step of 3. antiseptic be coated uniformly on active layer, afterwards to the base material coated with active layer and antibiotic layer in 40 DEG C of rings
20min is handled in border, forms antibiotic layer;4. bioprotein agent that step is prepared finally is coated uniformly on antibacterial layer surface, it
20min is handled in 40 DEG C of environment to the base material coated with active layer, antibiotic layer and bioprotein layer afterwards, produces biological doctor
Use metal material.
Embodiment 3
A kind of biomedical metallic material, it is made up of base material, active layer, antibiotic layer, biological activity protein layer, in institute
State substrate material surface coating activator and form active layer, antibiotic layer is formed in the activation layer surface coating antiseptic, in institute
State antibacterial layer surface and coat biological activity protein dosage form into biological activity protein layer;Described base material is porous titanium alloy,
The porous titanium alloy is by pore former and parent metal powder according to weight ratio 2:11 are mixed with and form;Described pore former is grain
Footpath is 400 μm of stearic acid particles;Described parent metal powder is by percentage to the quality 7% zirconium powder, 0.7% niobium powder,
0.55% tantalum powder, 0.2% boron powder, 91.55% titanium valve;Described activator, it is made up of the raw material of following parts by weight:7 parts of hydroxyls
Base apatite, 2.2 parts of dicalcium silicates, 5.5 parts of chitins, 2.8 parts of polyamide, 2.4 parts of polyaminoacid, 2.5 parts of calcium sulfate, 2.5
Part poly- (2- oxazolines), 20 parts of polyethylene glycol, 2 portions of modified starches;Described biological activity protein agent, by following parts by weight
Raw material forms:1 part of chitosan, 3 parts of calcium alginates, 7 parts of silk fibroins, 2 parts of gelatin, 2 parts of phosphoserines, 3 parts of fibres
Fibrillarin, appropriate distilled water;Described antiseptic, it is made up of the raw material of following parts by weight:2.5 parts of nano zine oxides, 2 parts it is poly-
Urethane, 3.5 parts of chitosans, 1.8 parts of poly butyric esters, 1.2 parts of Nano Silvers, 3.2 parts of PLAs, 4 parts of hydroxyacetic acids.
Further, described a kind of biomedical metallic material preparation method, specifically includes following steps:
1. prepared by base material:
A, take zirconium powder, niobium powder, tantalum powder, boron powder and titanium valve to be blended in high vacuum arc heating furnace by mass percentage to melt
Refining, 15min is stirred, pore former is added, is sufficiently stirred 30min, is finally pressed into blank;
B, blank is placed in 1200 DEG C of environment and sintered, be incubated 3h, base material is obtained after furnace cooling;
2. prepared by activator:
A, in parts by weight, hydroxyapatite, calcium sulfate, dicalcium silicate mixing are taken, it is 200um to be crushed to particle diameter, then
Mixed powder is placed in 450 DEG C of environment and calcines 1.5h, is then to be incubated in the environment that 300 DEG C of vacuums are 0.08 as temperature
40min, take out, room temperature is cooled in 60s, then be placed in 65 DEG C of environment and dry to constant weight;
B, will dry to constant weight mixed powder, then with modified starch, chitin, polyamide, polyaminoacid, poly- (2- oxazoles
Quinoline), polyethylene glycol mixing, be placed in ball mill, grind 35min, take out as in reactor, after stirring, heating response
Kettle reacts 60min, temperature of charge then is down into 55 DEG C, it is standby to obtain activator to 140 DEG C;
3. prepared by antiseptic:
In parts by weight, nano zine oxide, chitosan, Nano Silver, PLA, hydroxyacetic acid mixing is taken to be placed in high-speed stirred
In machine, rotating speed 2000r/min is controlled, stirs 10min, then is well mixed to be placed in polyurethane, poly butyric ester and disperses at a high speed
Machine disperses 35min in 1500r/min, then is placed in constant temperature 45min in 75 DEG C of waters bath with thermostatic control, stands 24 hours at room temperature, centrifugation, on
Clear liquid is antiseptic;
4. prepared by bioprotein agent:
A, in parts by weight, silk fibroin, fibrin are placed at -20 DEG C respectively and freeze 15h;
B, the distilled water that chitosan, calcium alginate, phosphoserine and gelatin are mixed to 1 times of mixture weight of addition is ground
1.2h is ground, is then well mixed with silk fibroin, fibrin, is placed in oscillator and handles 20min, filtering precipitation, on
Clear liquid is bioprotein agent;
5. prepared by biomedical metallic material:
The base material of preparation is placed in electric furnace and preheated, then 2. activator is coated uniformly on base material by step
Surface, 17min is handled the base material coated with activator in 35 DEG C of environment afterwards, form active layer;Again with preparation
The step of 3. antiseptic be coated uniformly on active layer, afterwards to the base material coated with active layer and antibiotic layer at 37.5 DEG C
17min is handled in environment, forms antibiotic layer;4. bioprotein agent that step is prepared finally is coated uniformly on antibacterial layer surface,
17min is handled in 38.5 DEG C of environment to the base material coated with active layer, antibiotic layer and bioprotein layer afterwards, produces life
Thing medical metal material.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Test example 1
Porous titanium alloy performance test
It is by porous titanium alloy (numbering 1-3) and number of patent application prepared by 1-3 of the embodiment of the present invention
The 2013105188953 bio-medical porous titanium alloys (numbering 4) prepared carry out the test of apparent porosity and incompressible intensity.
Described apparent porosity assay method, according to Archimedes's theorem, POROUS TITANIUM is carried out using scales/electronic balance weighing method
The measure of apparent porosity, the determination techniques method are the technology that those skilled in the art should know.
Described incompressible strength detection method, according to porous ceramics compressive strength test method in GB/T1964-1996
Carry out, the determination techniques method is the technology that those skilled in the art should know.
Measurement result is shown in Table 1
Table 1
Numbering | Apparent porosity | Incompressible intensity |
1 | 61.25% | 72.96MPa |
2 | 60.34% | 75.67MPa |
3 | 63.28% | 78.96MPa |
4 | 56.72% | 67.86MPa |
By table 1 it will be apparent that, 1-3 of the embodiment of the present invention prepare porous titanium alloy and number of patent application
The usability of medical porous titanium alloy is satisfied by for the 2013105188953 bio-medical porous titanium alloys prepared
Can, but compared with number of patent application is the 2013105188953 bio-medical porous titanium alloys prepared, the present invention prepares more
Hole titanium alloy performance is more more excellent, and apparent porosity improves 6.56%, and incompressible intensity improves 11.1MPa.
Test example 2
Influence of the different pore creating materials to porous alloy performance
Base material preparation method described in the embodiment of the present invention 3, by parent metal powder respectively at stearic acid, bicarbonate
Ammonium is according to weight than 11:2 are prepared by mixing into porous titanium alloy, then determine apparent porosity and the resistance to compression of its porous titanium alloy respectively
Contracting intensity.
Measurement result is as shown in table 2
Table 2
Pore creating material type | Apparent porosity | Incompressible intensity |
Stearic acid | 58.21% | 71.24MPa |
Ammonium hydrogen carbonate | 50.23% | 62.79MPa |
By table 2, it will be apparent that, compared with the porous titanium alloy prepared by the use of the strong hydrogen ammonium of carbonic acid as pore creating material, the present invention uses
Stearic acid is more excellent as porous titanium alloy performance prepared by pore creating material, and apparent porosity improves 7.98%, and incompressible intensity improves
8.45MPa.
Test example 3
Influence of the pore former and parent metal powder of different ratio to porous titanium alloy performance
Measurement result is shown in Table 3
Table 3
Numbering | Pore creating material | Parent metal powder | Apparent porosity | Incompressible intensity |
1 | 1 | 9 | 61.21% | 63.26MPa |
2 | 3 | 12 | 61.33% | 61.38MPa |
3 | 2 | 11 | 69.49% | 69.26MPa |
4 | 1.5 | 9.5 | 53.29% | 55.18MPa |
5 | 2.5 | 11.5 | 51.37% | 53.49MPa |
By table 3 it will be apparent that, when pore creating material and parent metal powder according to weight than 2:11 ratios are prepared by mixing into more
It is more excellent that hole titanium alloy performance compares the porous titanium alloy completed with the preparation of other ratios.
Test example 3
The comparative test of biomedical metallic material anti-microbial property prepared by the present invention
By disclosed in the biomedical metallic material obtained by embodiment 1 to 3 and number of patent application 2016107246302
" a kind of preferable biomedical metallic material of antibacterial ability " carries out antibacterial experiment:All samples are in 121 DEG C of autoclavings
40min, the bacterium solution that concentration is 107CFU/mL is dropped in the sample surfaces (0.06mL/cm2) to sterilize, drop is then had into bacterium solution
Sample be put into 37 DEG C of constant incubator culture 24h.Take out 24h culture sample, will be seeded in after bacterium solution doubling dilution containing
On the agar plate of culture medium.Agar plate after inoculation is put into 37 DEG C of constant incubator culture 24h, is taken out after 24h culture
Agar plate calculates bacterial population living (with reference to standard GB/T/T4789.2).
Measurement result shows, " a kind of preferable bio-medical of antibacterial ability disclosed in number of patent application 2016107246302
To Escherichia coli, its antibiotic rate reaches 99.5% to metal material ";98.45% is reached to staphylococcus aureus antibiotic rate, this hair
Biomedical metallic material prepared by bright embodiment 1-3, is respectively reached to Escherichia coli antibiotic rate:99.5%th, 99.7% and
99.8%, staphylococcus aureus antibiotic rate is respectively reached:98.5%th, 98.7% and 99.1%.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (4)
1. a kind of biomedical metallic material, it is made up of base material, active layer, antibiotic layer, biological activity protein layer, described
Substrate material surface coating activator forms active layer, antibiotic layer is formed in the activation layer surface coating antiseptic, described
Antibacterial layer surface coats biological activity protein dosage form into biological activity protein layer, it is characterised in that:
Described base material is porous titanium alloy, the porous titanium alloy be mixed with by pore former and parent metal powder and
Into;
Described pore former is the stearic acid particles that particle diameter is 400 μm;
Described parent metal powder is by percentage to the quality 6-8% zirconium powders, 0.5-0.9% niobiums powder, 0.4-0.7% tantalum powders,
0.1-0.3% boron powder, surplus are titanium valve;
Described activator, it is made up of the raw material of following parts by weight:5-8 parts hydroxyapatite, 1.5-2.7 parts dicalcium silicate,
4-7 parts chitin, 2.1-3.6 parts polyamide, 1.2-2.8 parts polyaminoacid, 2.3-2.7 parts calcium sulfate, poly- (the 2- oxazoles of 2-3 parts
Quinoline), 15-30 part polyethylene glycol 1.5-3.5 part modified starches;
Described biological activity protein agent, is made up of the raw material of following parts by weight:0.5-1.5 parts chitosan, 2-4 part marine algas
Sour calcium, 5-9 parts silk fibroin, 1-3 parts gelatin, 1.5-2.5 parts phosphoserine, 2-4 parts fibrin, appropriate distillation
Water;
Described antiseptic, it is made up of the raw material of following parts by weight:1-3.5 parts nano zine oxide, 1-3 parts polyurethane, 2.5-
4.5 parts of chitosans, 1.2-2.4 parts poly butyric ester, 0.5-1.6 parts Nano Silver, 2.5-3.8 parts PLA, 2-6 part hydroxyl second
Acid.
A kind of 2. biomedical metallic material preparation method according to claim 1, it is characterised in that:Specifically include following
Step:
1. prepared by base material:
A, take zirconium powder, niobium powder, tantalum powder, boron powder and titanium valve to be blended in melting in high vacuum arc heating furnace by mass percentage, stir
15min is mixed, adds pore former, 30min is sufficiently stirred, is finally pressed into blank;
B, blank is placed in 1000-1400 DEG C of environment and sintered, be incubated 1-4h, base material is obtained after furnace cooling;
2. prepared by activator:
A, in parts by weight, hydroxyapatite, calcium sulfate, dicalcium silicate mixing are taken, it is 200um to be crushed to particle diameter, then will be mixed
Conjunction powder, which is placed in 400-500 DEG C of environment, calcines 1-2h, is then to be incubated in the environment that 300 DEG C of vacuums are 0.08 as temperature
40min, take out, room temperature is cooled in 60s, then be placed in 60-70 DEG C of environment and dry to constant weight;
B, will dry to constant weight mixed powder, then with modified starch, chitin, polyamide, polyaminoacid, poly- (2- oxazolines),
Polyethylene glycol mixes, and is placed in ball mill, grinds 30-40min, takes out as in reactor, after stirring, heating response kettle
To 120-160 DEG C, 50-70min is reacted, temperature of charge is then down to 50-60 DEG C, it is standby to obtain activator;
3. prepared by antiseptic:
In parts by weight, nano zine oxide, chitosan, Nano Silver, PLA, hydroxyacetic acid mixing is taken to be placed in homogenizer
In, rotating speed 2000r/min is controlled, stirs 10min, then be well mixed with polyurethane, poly butyric ester and be placed in high speed dispersor
Disperse 30-40min in 1500r/min, then be placed in constant temperature 40-50min in 70-80 DEG C of water bath with thermostatic control, stand 24 hours at room temperature,
Centrifugation, supernatant is antiseptic;
4. prepared by bioprotein agent:
A, in parts by weight, silk fibroin, fibrin are placed at -20 DEG C respectively and freeze 15h;
Chitosan, calcium alginate, phosphoserine and gelatin are mixed to the distilled water grinding 1- for adding 1 times of mixture weight b,
1.5h, then it is well mixed with silk fibroin, fibrin, is placed in oscillator and handles 20min, filtering precipitation, supernatant
Liquid is bioprotein agent;
5. prepared by biomedical metallic material:
The base material of preparation is placed in electric furnace and preheated, then 2. activator is coated uniformly on the table of base material by step
Face, 15-20min is handled the base material coated with activator in 30-40 DEG C of environment afterwards, form active layer;Use again
The step of preparation, 3. antiseptic was coated uniformly on active layer, and the base material coated with active layer and antibiotic layer is existed afterwards
15-20min is handled in 35-40 DEG C of environment, forms antibiotic layer;Finally 4. bioprotein agent that step is prepared is coated uniformly on anti-
Bacterium layer surface, the base material coated with active layer, antibiotic layer and bioprotein layer is handled in 37-40 DEG C of environment afterwards
15-20min, produce biomedical metallic material.
A kind of 3. biomedical metallic material according to claim 1, it is characterised in that:Porous titanium alloy is by pore former and base
Body metal dust compares 1-3 according to weight:9-12, which is mixed with, to be formed.
A kind of 4. biomedical metallic material according to claim 3, it is characterised in that:Porous titanium alloy is by pore former and base
Body metal dust is according to weight than 2:11 are mixed with and form.
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CN108939159A (en) * | 2018-07-27 | 2018-12-07 | 吉林大学 | Small intestine acellular matrix film combination metal mesh wall of the chest sticking patch preparation method |
CN109432507A (en) * | 2018-11-08 | 2019-03-08 | 中南大学 | The antibacterial hydroxylapatite composite material and preparation method of containing metal oxide |
CN109851371A (en) * | 2019-04-10 | 2019-06-07 | 肇庆市盛浩新材料科技有限公司 | A kind of high-efficiency antimicrobial new material and preparation method thereof for ceramics and quartz plate |
CN110012912A (en) * | 2019-04-10 | 2019-07-16 | 肇庆市盛浩新材料科技有限公司 | A kind of ceramic efficacious anti-microbial material and the preparation method and application thereof |
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CN108939159A (en) * | 2018-07-27 | 2018-12-07 | 吉林大学 | Small intestine acellular matrix film combination metal mesh wall of the chest sticking patch preparation method |
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CN109432507B (en) * | 2018-11-08 | 2020-08-04 | 中南大学 | Antibacterial hydroxyapatite composite material containing metal oxide and preparation method thereof |
CN109851371A (en) * | 2019-04-10 | 2019-06-07 | 肇庆市盛浩新材料科技有限公司 | A kind of high-efficiency antimicrobial new material and preparation method thereof for ceramics and quartz plate |
CN110012912A (en) * | 2019-04-10 | 2019-07-16 | 肇庆市盛浩新材料科技有限公司 | A kind of ceramic efficacious anti-microbial material and the preparation method and application thereof |
CN109851371B (en) * | 2019-04-10 | 2019-12-27 | 肇庆市盛浩新材料科技有限公司 | Novel efficient antibacterial material for ceramic and quartz plates and preparation method thereof |
CN115418021A (en) * | 2022-10-11 | 2022-12-02 | 中国科学技术大学 | Cellulose aerogel, preparation method and application thereof |
CN115418021B (en) * | 2022-10-11 | 2024-02-09 | 中国科学技术大学 | Cellulose aerogel, preparation method and application thereof |
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