CN104254349A - Method for producing biological implant material - Google Patents

Method for producing biological implant material Download PDF

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Publication number
CN104254349A
CN104254349A CN201380021544.XA CN201380021544A CN104254349A CN 104254349 A CN104254349 A CN 104254349A CN 201380021544 A CN201380021544 A CN 201380021544A CN 104254349 A CN104254349 A CN 104254349A
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China
Prior art keywords
matrix
warm water
embedded material
liquid temperature
tunicle
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CN201380021544.XA
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Chinese (zh)
Inventor
加茂道正
北野宏幸
喜多将喜
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Kyocera Medical Corp
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Kyocera Medical Corp
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    • 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
    • A61L27/32—Phosphorus-containing materials, e.g. apatite
    • 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
    • A61L2400/00—Materials characterised by their function or physical properties
    • A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
    • 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

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Transplantation (AREA)
  • Dermatology (AREA)
  • Medicinal Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Inorganic Chemistry (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Materials For Medical Uses (AREA)
  • Dental Prosthetics (AREA)

Abstract

Provided is a production method for producing a biological implant material having excellent bindability to a hard tissue. The method for producing a biological implant material according to the present invention comprises an alkali treatment step and a warm water treatment step, wherein the alkali treatment step comprises immersing a base formed from titanium or a titanium alloy in an aqueous alkaline solution and the warm water treatment step comprises immersing the base that has been immersed in the aqueous alkaline solution in warm water having a liquid temperature of 30 DEG C or higher and lower than 40 DEG C for 3 to 36 hours inclusive.

Description

The manufacture method of organism embedded material
Technical field
The present invention relates to the manufacture method of the organism embedded material of heeling-in in vivo.
Background technology
Known: as in vivo in order to replace the organism embedded material of the sclerous tissues such as bone, root of the tooth and heeling-in, use the metal material such as titanium, titanium alloy as matrix, be formed with the organism embedded material of the tunicle of the affinity had sclerous tissues on the surface of this matrix.
Such as, in patent documentation 1, disclose: the base material be made up of titanium or its alloy be impregnated in alkaline aqueous solution, then flood more than 1 hour in the water more than 40 DEG C or flood more than 1 minute in water more than 80 DEG C, the surface being formed in base material is thus contained anatase and is not contained amorphous titanate in fact and the manufacture method of the organism implant of tunicle that internally uprises of titanium concentration.Expect that the organism implant short time in organism obtained by this manufacture method forms apatite layer.
Prior art document
Patent documentation
Patent documentation 1: Japan Patent No. 3877505 publication
Summary of the invention
The problem that invention will solve
Because the apatite Forming ability of anatase is excellent, therefore excellent by the Forming ability of the apatite of the organism implant of the manufacture of manufacture method disclosed in patent documentation 1.
In patent documentation 1, describe: for having separated out the organism implant of anatase and not separated out the organism implant of anatase, compare the adhesion with the tibia of rabbit, the adhesion having separated out the embedded material of anatase is higher than the embedded material of not separating out anatase.Because the Forming ability of the apatite of not separating out the embedded material of anatase is significantly deteriorated, therefore relatively diminish with the adhesion of bone, because the Forming ability of the apatite of the embedded material of separating out anatase is high, therefore relatively become large with the adhesion of bone.
Present inventor finds, in the manufacture method of organism embedded material, not only relevant with apatite Forming ability with the adhesion of bone, and also relevant by film-strength with organism embedded material top layer, thus completes the present application.
The object of the present invention is to provide a kind of manufacture method of the organism embedded material for the manufacture of the adhesion excellence with sclerous tissues.
Solve the means of problem
The present invention is a kind of manufacture method of organism embedded material, it is characterized in that, it is the manufacture method of the organism embedded material of heeling-in in vivo,
It comprises: by the matrix impregnates that formed by titanium or titanium alloy in the alkali treatment operation of aqueous alkali and
Impregnated in the matrix after aqueous alkali liquid temperature more than 30 DEG C and flood more than 3 hours and the warm water treatment process of less than 36 hours by described lower than in the warm water of 40 DEG C.
Further, in the present invention, described liquid temperature is preferably more than 30 DEG C and less than 35 DEG C.
In addition in the present invention, preferably obtain following organism embedded material: by utilize that the shear load additional testing of universal testing machine measures, represent and the fracture strength of adhesion of bone for more than 1.60MPa and below 2.20MPa.
Invention effect
According to the present invention, in alkali treatment operation by the matrix impregnates that formed by titanium or titanium alloy in aqueous alkali, and the matrix that impregnated in aqueous alkali to be flooded more than 3 hours and less than 36 hours lower than in the warm water of 40 DEG C liquid temperature more than 30 DEG C in warm water treatment process.
Thus, obtain by heeling-in high with the affinity of Gu Deng sclerous tissues, with the organism embedded material of the adhesion excellence of sclerous tissues.
According to the present invention, the described liquid temperature in warm water treatment process is particularly preferably more than 30 DEG C and less than 35 DEG C.
According to the present invention, following organism embedded material can be obtained: by utilize that the shear load additional testing of universal testing machine measures, represent and the fracture strength of adhesion of bone for more than 1.60MPa and below 2.20MPa.
Accompanying drawing explanation
Object of the present invention, characteristic and advantage comprise following detailed description and accompanying drawing, thus become clear and definite.
Fig. 1 is the process chart of the manufacturing process of the manufacture method of the organism embedded material represented as the 1st embodiment of the present invention.
Fig. 2 is the process chart of the manufacturing process of the manufacture method of the organism embedded material represented as the 2nd embodiment of the present invention.
Fig. 3 represents in warm water treatment process with the SEM photo on the surface after the simulated solution dipping of the test film after liquid temperature 35 DEG C, dip time process in 24 hours.
Fig. 4 represents in warm water treatment process with the SEM photo on the surface after the simulated solution dipping of the test film after liquid temperature 80 DEG C, dip time process in 24 hours.
Detailed description of the invention
Preferred embodiment be described in detail to of the present invention below with reference to accompanying drawing.
Fig. 1 is the process chart of the manufacturing process of the manufacture method of the organism embedded material represented as the 1st embodiment of the present invention.The manufacture method of present embodiment comprises matrix formation process s1, degreasing process s2, alkali treatment operation s3, warm water treatment process s4 and heating treatment step s5.
In matrix formation process s1, with titanium or titanium alloy for material, be formed into the matrix of organism embedded material.As the titanium alloy forming matrix, Ti-6Al-4V, Ti-5Al-2.5Sn, Ti-3Al-13V-11Cr, Ti-15Mo-5Nb-3Ta, Ti-15Zr-4Nb-4Ta, Ti-6Al-2Mo-Ta, Ti-6Al-2Nb-Ta, Ti-15Mo-5Zr-3Al, Ti-6Al-7Nb etc. can be enumerated.
In degreasing process s2, the defats such as the oil content on the surface of the matrix formed in matrix formation process s1 will be attached to.In this degreasing process s2, such as, first carry out cleaning by degreasing with acetone, then clean with distilled water, ungrease treatment terminates.
In alkali treatment operation s3, the matrix impregnates after defat will be carried out by degreasing process s2 in aqueous alkali.Aqueous alkali is as containing sodium ion (Na +), potassium ion (K +) etc. alkali metal ion and calcium ion (Ca 2+) etc. the solution that is made of the aqueous solution of at least any one metal ion in alkaline-earth metal ions, such as, be the solution be made as sodium hydroxide (NaOH) aqueous solution or potassium hydroxide (KOH) aqueous solution.
The concentration of at least any one metal ion in the alkali metal ion in aqueous alkali and alkaline-earth metal ions is preferably more than 0.1M (molar concentration) and below 20M, is particularly preferably more than 3M and below 10M.In addition, in alkali treatment operation s3, the liquid temperature of aqueous alkali is set as more than 40 DEG C and less than 90 DEG C, and the dip time of matrix in aqueous alkali is preferably 12 times more than and less than 96 hours.
By aforementioned bases process, formed on the surface of matrix and contain titanium or titanium alloy, alkali metal or alkaline-earth metal and oxygen and with the sclerous tissues such as bone, root of the tooth, there is the tunicle of affinity.Specifically, formed on the surface of the matrix after alkali treatment containing alkaline titanate, the tunicle with sclerous tissues's affinity.It should be noted that originally there is the thin film formed by oxide on the surface of titanium or titanium alloy, the composition of this oxide all carries out the titanium oxide (TiO of the amphiprotic substance reacted with as with any one in strong acid and highly basic 2) close.Therefore, if impregnated in aqueous alkali by the matrix formed by titanium or titanium alloy in alkali treatment operation s3, then the Concentraton gradient increased gradually from the inside that response magnitude is few towards the outside that response magnitude is many with the concentration of titanium oxide and alkaline titanate is at the Surface Creation alkalescence titanate of matrix.
In warm water treatment process s4, the matrix (hereinafter referred to as " tunicle formation matrix ") that defines the tunicle with sclerous tissues's affinity in alkali treatment operation s3 is flooded more than 3 hours and less than 36 hours lower than in the warm water of 40 DEG C liquid temperature more than 30 DEG C.
In warm water treatment process s4, the water forming matrix for flooding tunicle can use such as distilled water, deionized water, pure water and ultra-pure water etc.In warm water treatment process s4, the water retained is adjusted to the liquid temperature of regulation in treatment trough, the mode of mass-impregnation in warm water forming matrix with tunicle is flooded, and takes out matrix at the time point of dip time through the stipulated time from treatment trough.
In the operation of such impregnation process in warm water, the amount of warm water when being set in impregnation matrix in warm water according to the summation of the surface area of matrix.Specifically, the amount of warm water is set in the mode meeting following formula (1).
1(mL/cm 2)≤V 1/S 1≤100(mL/cm 2)…(1)
[in formula, V 1represent the volume (mL) of warm water, S 1represent the surface area (cm that impregnated in the matrix of warm water 2) summation.]
In addition, the amount of warm water is more preferably set in the mode meeting following formula (2).
3(mL/cm 2)≤V 1/S 1≤50(mL/cm 2)…(2)
[in formula, V 1represent the volume (mL) of warm water, S 1represent the surface area (cm that impregnated in the matrix of warm water 2) summation.]
Although relate the circumstances later, by carrying out warm water treatment process s4 in the scope of dip time in the scope of liquid temperature as above, as above, the organism embedded material with the adhesion excellence of sclerous tissues can be obtained thus.In addition, liquid temperature and the above-mentioned scope of dip time are the scopes different from the scope of the apatite Forming ability excellence in organism implantation material surface.Even if the apatite Forming ability on the surface of organism embedded material is excellent, the adhesion that also may not be certain this organism embedded material and sclerous tissues is large.Shown in embodiment described later, even the organism embedded material of the Forming ability same degree excellence of apatite, for the adhesion with sclerous tissues, also can observe significant difference significantly.
Due to the main constituent that apatite is the Gu Deng sclerous tissues generated in vivo, therefore think as the surface characteristic of organism embedded material, more easily form apatite then higher with the affinity of sclerous tissues, also higher with the adhesion of sclerous tissues.But present inventor finds, even the organism embedded material that the apatite Forming ability in surface is identical, if the treatment conditions in warm water treatment process s4 are different, then different from the adhesion of sclerous tissues.The liquid temperature condition of the warm water of matrix is particularly formed about dipping tunicle, when being set to the situation of 20 DEG C and being set to 40 DEG C, the adhesion of organism embedded material and sclerous tissues is same degree, when liquid temperature being set to more than 30 DEG C and lower than 40 DEG C, with situation liquid temperature being set to 20 DEG C and be set to 40 DEG C situation compared with, adhesion becomes large.
Only from apatite Forming ability, liquid temperature is set to more than 30 DEG C and is same degree lower than the situation of 40 DEG C with the situation being set to 40 DEG C, thus the adhesion of the apatite Forming ability of organism embedded material and sclerous tissues is uncorrelated.Therefore, with regard to the treatment conditions in warm water treatment process s4, the situation being conceived to the apatite Forming ability in the surface of organism embedded material is different from being conceived to the situation of the adhesion of sclerous tissues.
From such a viewpoint, tunicle is formed matrix liquid temperature more than 30 DEG C and lower than flooding more than 3 hours and less than 36 hours in the warm water of 40 DEG C as the treatment conditions in warm water treatment process s4 by present inventor as mentioned above.When treatment conditions are not within the scope of these, such as, liquid temperature is lower than 30 DEG C or dip time lower than 3 hours, and because the Forming ability of apatite reduces, therefore the adhesion of organism embedded material and sclerous tissues reduces, not preferably.In addition, if liquid temperature be more than 40 DEG C or dip time more than 36 hours, although then the Forming ability of apatite is high, can reduce with the adhesion of sclerous tissues, therefore not preferred.
If only from by film-strength, then liquid temperature is more than 20 DEG C and is not being observed difference lower than the words of 40 DEG C by film-strength, but with the adhesion of sclerous tissues in observe difference.In addition, when not carrying out warm water treatment process, although high by film strength, low with the adhesion of sclerous tissues.Depend on apatite Forming ability with the adhesion of sclerous tissues and by film-strength, in warm water treatment process s4, preferably impregnated in liquid temperature more than 30 DEG C and lower than the warm water of 40 DEG C.
In addition, about liquid temperature, be preferably more than 30 DEG C and less than 38 DEG C, be more preferably more than 30 DEG C and less than 35 DEG C.About dip time, be preferably more than 6 hours and less than 24 hours, be more preferably 12 times more than and less than 24 hours.
In heating treatment step s5, carry out the heat treated that the tunicle after terminating warm water treatment process s4 forms matrix heating.In this heating treatment step s5, more than 300 DEG C of the temperature below the transition temperature as titanium or titanium alloy and heat more than 30 minutes and time in the scope of less than 24 hours at the temperature of less than 800 DEG C.By carrying out heat treated like this, oxygen forms the diffusion into the surface of matrix at tunicle, has and increases with the thickness of the tunicle of the affinity of sclerous tissues, also increased by the stability of membrane structure.It should be noted that, if the temperature of heat treated is lower than 300 DEG C, then the surface that oxygen can not form matrix at tunicle is fully spread, is supplied, and is difficult to the thickness fully guaranteeing tunicle.On the other hand, if the temperature of heat treated is more than 800 DEG C, then can reach the transition temperature of titanium or titanium alloy, tunicle can be caused to form the reduction of the mechanical strength of matrix, thus not preferred.
Terminated by such heating treatment step s5, the manufacture of organism embedded material completes.What the surface part about organism embedded material was formed has and the tunicle of the affinity of sclerous tissues (anatase tunicle), reduces gradually, mode that on the other hand concentration of titanium oxide and alkaline titanate increases gradually towards outside formed with the concentration of Titanium towards outside.
What formed in the surface part of organism embedded material has with the tunicle of the affinity of sclerous tissues, containing concentration with the titanium oxide of the change of Concentraton gradient slowly and alkaline titanate, and the therefore interface firm engagement of matrix and the tunicle formed.Thus, at organism embedded material by heeling-in in vivo and with under the state of bioresorbable, this tunicle Surface Creation easily and calcium, phosphorus reaction hydroxide titanio.The hydroxide titanio generated is rich reactive, reacts and generate apatite core with the bone formation composition in body fluid.
Fig. 2 is the process chart of the manufacturing process of the manufacture method of the organism embedded material represented as the 2nd embodiment of the present invention.The manufacture method of present embodiment comprises matrix formation process a1, degreasing process a2, alkali treatment operation a3, warm water treatment process a4, heating treatment step a5 and steam winding-up treatment process a6.
In matrix formation process a1, in the same manner as the matrix formation process s1 in aforementioned 1st embodiment, form the matrix formed by titanium or titanium alloy.Now, also tunicle is not formed on the surface of matrix.
In degreasing process a2, in the same manner as the degreasing process s2 in aforementioned 1st embodiment, defat is carried out to the oil content etc. of the surface attachment of the matrix formed in matrix formation process a1.
In alkali treatment operation a3, in the same manner as the alkali treatment operation s3 in aforementioned 1st embodiment, the matrix impregnates after defat will be carried out in aqueous alkali in degreasing process a2, form the tunicle containing alkaline titanate thus on the surface of matrix, obtain tunicle and form matrix.
In warm water treatment process a4, in the same manner as the warm water treatment process s4 in aforementioned 1st embodiment, tunicle is formed matrix liquid temperature more than 30 DEG C and flood more than 3 hours and less than 36 hours lower than in the warm water of 40 DEG C.
In heating treatment step a5, in the same manner as the heating treatment step s5 in aforementioned 1st embodiment, the tunicle after terminating warm water process forms matrix heating.Heat treated condition (temperature, time etc.) is identical with heating treatment step s5.By carrying out heat treated, oxygen forms the diffusion into the surface of matrix at tunicle, has and increases with the thickness of the tunicle of the affinity of sclerous tissues, also increased by the stability of membrane structure.By such heating treatment step a5, form on the surface that tunicle forms matrix that the concentration of Titanium reduces gradually towards outside, the anatase tunicle that increases gradually towards outside of the concentration of titanium oxide and alkaline titanate on the other hand.
In steam winding-up treatment process a6, the tunicle after heating in heating treatment step a5 is formed to the surface winding-up steam of matrix.In steam winding-up treatment process a6, use the aqueous vapor injection apparatus with the nozzle of injection water steam, the steam sprayed the leading section from this nozzle forms the surface winding-up of matrix to the tunicle after heat treated.As aqueous vapor injection apparatus, such as, the steam washing machine (model: ST-II) of GC Corp. can be enumerated.During steam winding-up, tunicle formation matrix limit winding-up can be moved by limit Xuan Zhuan Huo Oscillating.
As the injection conditions of the steam in aqueous vapor injection apparatus, such as, pressure setting is more than 0.40MPa and below 0.45MPa, water-vapour spray amount is set as 30 (mL/30 seconds) more than and 55 (mL/30 seconds) below.
In steam winding-up treatment process a6, form the surface winding-up steam of matrix to the tunicle after heat treated, the part forming the easy stripping existed in the tunicle of the surface formation of matrix at tunicle can be removed thus.
In addition, from steam, tunicle is formed to the spacing distance of winding-up position to the surface of tunicle formation matrix of matrix winding-up, the spacing distance namely forming the surface of matrix from the spray nozzle front end portion of aqueous vapor injection apparatus to tunicle is preferably more than 30mm and below 100mm.Further, the winding-up time forming the surface winding-up steam of matrix at tunicle is selected according in the scope of described spacing distance preferably more than 5 seconds and below 120 seconds.
Terminated by steam winding-up treatment process a6 as above, the manufacture of organism embedded material completes.
Embodiment
By manufacturing organism embedded material based on the manufacture method of the 1st embodiment (anhydrous steam winding-up treatment process) and the 2nd embodiment (having steam winding-up treatment process) respectively, carry out each evaluation.
< matrix formation process >
Simulation reconstruction forms the matrix of organism embedded material, has prepared columned base sheet.This base sheet is formed by titanium alloy (Ti-6Al-4V), is the straight cylinder type of diameter 4mm, length 10mm.
< degreasing process >
With acetone, cleaning by degreasing is carried out to described base sheet, then clean with distilled water.
< alkali treatment operation >
Base sheet after ungrease treatment be impregnated of 48 hours in the 5M sodium hydrate aqueous solution remaining 80 DEG C.
< warm water treatment process >
In warm water treatment process, the liquid temperature of distilled water is set to 20 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 80 DEG C, in each liquid temperature, dip time is set to 3 hours, 6 hours, 12 hours, 24 hours respectively.
< heating treatment step >
Tunicle after warm water process under above-mentioned each condition is formed base sheet 600 DEG C of heating 1 hour.
< steam winding-up treatment process >
From above-mentioned matrix formation process to heating treatment step, the treatment conditions of the 1st embodiment and the 2nd embodiment are identical.In the 2nd embodiment, under following condition, carry out steam winding-up process further.
As aqueous vapor injection apparatus, the steam cleaner (model: ST-II) of GC Corp. is used to set steam winding-up condition as follows.
The expulsion pressure of steam: 0.4MPa
Water-vapour spray amount: 55mL/30 second
The spacing distance on the surface of spray nozzle front end portion and base sheet: 55mm
The steam winding-up time: 10 seconds
Terminated by heating treatment step, the organism embedded material based on the 1st embodiment simulation reconstruction, obtains test film.Terminate additionally by steam winding-up treatment process, the organism embedded material based on the 2nd embodiment simulation reconstruction, obtains test film.
The evaluation > of the adhesion of < and sclerous tissues
Each test film based on the diameter 4mm of the 1st embodiment manufacture, the straight cylinder type of length 10mm is imbedded at the tibia peri position portion of white rabbits, after raising 8 weeks, have rated the adhesion of test film and tibia.
About adhesion, for the test film being imbedded at tibia, shear load is given at the axis direction of test film, the fracture strength calculated (MPa), divided by the lateral area (4mm × π × 10mm) of straight cylinder type test film, is evaluated as adhesion by the shear load during boundary fault of the surrounding bone combined with test film and test film.Determinator uses universal testing machine (Instron Japan system, model 1123), and by heeling-in, the tibia of test film is fixed with pedestal shape resin, crosshead speed is set to 0.5mm/min and gives shear load to test film.The results are shown in table 1.
[table 1]
Unit (MPa)
Owing to being the evaluation based on assay method as above, therefore fracture strength is larger then represents that the adhesion of test film and tibia is larger.
Be aware of according to table 1, liquid temperature is that compared with the situation of 20 DEG C and 40 DEG C and the situation of 30 DEG C and 35 DEG C, adhesion is little, and when 80 DEG C, adhesion diminishes further, and tendency such under arbitrary dip time is identical.
The evaluation > of < apatite Forming ability
Each test film be impregnated in the simulated body fluid 4 days with the inorganic ion concentration roughly the same with the body fluid of people, have rated the presence or absence of the formation of apatite.As simulated body fluid, employ that to have each ion concentration be K +: 5.0 [mM], Na +: 142 [mM], Mg 2+: 1.5 [mM], Ca 2+: 2.5 [mM], Cl -: 148 [mM], HCO 3-: 4.2 [mM], HPO 2-: 1.0 [mM], SO 4 2-: the composition of 0.5 [mM], to be prepared as the solution of the pH=7.4 of 37 DEG C with Tris and hydrochloric acid.
Fig. 3 is the SEM photo on the surface after the simulated body fluid dipping of the test film represented in warm water treatment process after liquid temperature 35 DEG C, dip time process in 24 hours, and Fig. 4 represents the SEM photo on the surface after the simulated solution dipping of the test film in warm water treatment process after liquid temperature 80 DEG C, dip time process in 24 hours.Although not shown, but in addition to these, test film in warm water treatment process after liquid temperature 20 DEG C, dip time process in 24 hours, the test film in warm water treatment process after liquid temperature 30 DEG C, dip time process in 24 hours, the test film in warm water treatment process after liquid temperature 40 DEG C, dip time process in 24 hours be impregnated in simulated body fluid 4 days similarly, have rated the presence or absence of the formation of apatite.
By evaluating based on the surface observation of SEM photo, as metewand, "×" is evaluated as by what almost do not observe the formation of apatite completely at material surface, being evaluated as " △ " of the formation of apatite is observed in a part for material surface, to a part of material surface be observed but observe the formation of apatite in major part be evaluated as "○", being evaluated as " ◎ " of the formation of apatite will be observed at whole material surface.
< is by the evaluation > of film-strength
Peel off after Scotch (registered trade mark) adhesive tape is sticked on the surface of each test film, observe whether adhere to the tunicate sheet that comes off on the adhesive tape peeled off with SEM (scanning electron microscope).Adhesive tape does not adhere to tunicle come off sheet, due to high by film-strength, therefore evaluation result is evaluated as "○", when the matrix as substrate is observed in whole tape stripping face, because the bond strength of tunicle and matrix is weak, therefore evaluation result is evaluated as "×".In addition, on adhesive tape the tunicate sheet that comes off attachment and when the part in tape stripping face observes the matrix as substrate, due to somewhat weak by film-strength, therefore evaluation result is evaluated as " △ ".
The results are shown in table 2.In order to compare adhesion and apatite Forming ability and by film-strength, in table 2, record the result of the adhesion (fracture strength) of table 1 in the lump.In addition, in the same manner as other test films, the test film of comparative example has been made except not carry out except warm water treatment process.The evaluation result of comparative example is recorded in table 2 with the form that liquid temperature is " * ".
[table 2]
Liquid temperature (DEG C) Fracture strength (MPa) Apatite Forming ability By film-strength
20 1.77 ○ ○
30 1.91 ◎ ○
35 2.20 ◎ ○
40 1.74 ◎ ○
80 1.57 ◎ △
* 0.95 △ ○
As known from Table 2, think that apatite Forming ability is slightly poor, and consequently, adhesion diminishes when liquid temperature lower 20 DEG C.On the other hand, be aware of: when liquid temperature higher 40 DEG C and 80 DEG C, the situation same degree of apatite Forming ability and liquid temperature 30 DEG C and 35 DEG C is excellent, but for adhesion, although apatite Forming ability is excellent, but when liquid temperature 40 DEG C and 80 DEG C, obvious variation compared with the situation of liquid temperature 30 DEG C and 35 DEG C.
When liquid temperature is below 40 DEG C, is not being observed difference, but observe difference by film-strength in adhesion, when liquid temperature is 35 DEG C, adhesion is high.In addition, be aware of and do not carrying out in the comparative example of warm water process, although high by film-strength, in adhesion compared with the embodiment after warm water process obvious variation.
Depend on apatite Forming ability with the adhesion of bone and by film-strength, preferably impregnated in liquid temperature more than 30 DEG C and lower than the warm water of 40 DEG C.By such warm water process, fracture strength can be obtained and be more than 1.60MPa and the organism embedded material of below 2.20MPa.
It should be noted that, the test film based on the 2nd embodiment manufacture is evaluated similarly, obtain identically with the 1st embodiment and preferably impregnated in liquid temperature more than 30 DEG C and the result of warm water lower than 40 DEG C.
If be conceived to apatite Forming ability like this and judged from the adhesion with bone by film-strength, then can say the treatment conditions as warm water treatment process in any one in the 1st embodiment and the 2nd embodiment, all preferably liquid temperature is set to more than 30 DEG C and lower than 40 DEG C, is particularly preferably set to more than 30 DEG C and less than 35 DEG C.
The present invention, when not departing from its spirit or principal character, can implement in other various modes.Therefore, aforesaid embodiment is all only illustrate in all respects, and scope of the present invention is the scope shown in claim, and not by any restriction of description text.Further, belong to the distortion of claim, change all within the scope of the invention.

Claims (3)

1. a manufacture method for organism embedded material, is characterized in that,
It is the manufacture method of the organism embedded material of heeling-in in vivo, and it comprises:
Alkali treatment operation, by the matrix impregnates that formed by titanium or titanium alloy in aqueous alkali, and
Warm water treatment process, impregnated in the matrix after aqueous alkali liquid temperature more than 30 DEG C and floods more than 3 hours and less than 36 hours by described lower than in the warm water of 40 DEG C.
2. the manufacture method of organism embedded material according to claim 1, is characterized in that,
Described liquid temperature is more than 30 DEG C and less than 35 DEG C.
3. the manufacture method of organism embedded material according to claim 1 and 2, is characterized in that,
Obtain following organism embedded material: by utilize that the shear load additional testing of universal testing machine measures, represent and the fracture strength of adhesion of bone for more than 1.60MPa and below 2.20MPa.
CN201380021544.XA 2012-04-27 2013-04-25 Method for producing biological implant material Pending CN104254349A (en)

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JP2012-103028 2012-04-27
PCT/JP2013/062288 WO2013161963A1 (en) 2012-04-27 2013-04-25 Method for producing biological implant material

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JP2002345948A (en) * 2001-05-23 2002-12-03 Kobe Steel Ltd Bone substitute material
CN1442120A (en) * 2003-04-11 2003-09-17 四川大学 Surface active strong internal fixed titanium bone connection plate and its making method
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Application publication date: 20141231