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WO2009142296A1 - Procédé permettant la polarisation de céramique et biomatériau contenant une céramique polarisée - Google Patents

Procédé permettant la polarisation de céramique et biomatériau contenant une céramique polarisée Download PDF

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Publication number
WO2009142296A1
WO2009142296A1 PCT/JP2009/059433 JP2009059433W WO2009142296A1 WO 2009142296 A1 WO2009142296 A1 WO 2009142296A1 JP 2009059433 W JP2009059433 W JP 2009059433W WO 2009142296 A1 WO2009142296 A1 WO 2009142296A1
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electrode
ceramic
biomaterial
fine particles
ceramics
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English (en)
Japanese (ja)
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仁大 山下
聰一郎 伊藤
亜希子 永井
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Tokyo Medical and Dental University NUC
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Tokyo Medical and Dental University NUC
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/32—Phosphates of magnesium, calcium, strontium, or barium

Definitions

  • the present invention relates to a polarization treatment method for ceramics and a biomaterial containing ceramics subjected to polarization treatment by the method.
  • polarized biocompatible ceramics As biomaterials such as artificial tooth roots (implant bodies) and artificial bones, it is known to use polarized biocompatible ceramics. For example, a biocompatible substance such as hydroxyapatite is subjected to polarization treatment. It is known that the obtained ceramic can be used as a material for proliferating living cells and a dental bone material (for example, Patent Documents 1, 2, and 3). Also, a method of controlling the temperature during polarization treatment has been devised to adjust the amount of charge stored in such polarized ceramics (Patent Document 4).
  • Patent Document 5 a fluid bone prosthetic composition containing calcium phosphate, a hydrophilic binder material and an aqueous liquid medium is known.
  • Patent Document 6 a medical material composed of an inorganic compound complex in which a bioactive inorganic compound such as calcium phosphate is chemically bonded to a substrate such as fibroin.
  • Patent Document 7 a bone prosthetic material made of a composite of bioceramic particles and a biodegradable polymer is known (Patent Document 7).
  • a conventional polarized ceramic is manufactured by attaching an electrode to the ceramic before the polarization and applying a voltage.
  • it is difficult to perform sufficient polarization treatment with a simple planar electrode. For this reason, it was necessary to perform polarization treatment using an electrode having a shape that fits the surface shape of the member.
  • such an electrode is difficult to manufacture because it requires a very high shape accuracy, is expensive, and cannot be used for polarization treatment of members having different shapes, and therefore lacks versatility.
  • contamination of the contact surface with the electrode becomes a problem, and there is a restriction that a biomaterial that has been packaged after sterilization cannot be polarized.
  • both the positive electrode and the negative electrode are attached to the ceramic, it is difficult to apply to the ceramic in a fine particle state.
  • pressure may be applied to the ceramic by the electrode.
  • adhesion or the like may occur between particles due to pressure during the treatment.
  • fine ceramics particularly fine ceramics such as nanoparticles.
  • the present invention has been made in view of the above circumstances, and can easily polarize a member including ceramics having any shape and prevent surface contamination caused by electrodes used for the polarization treatment.
  • An object of the present invention is to provide a ceramic polarization treatment method that can be used.
  • Another object of the present invention is to provide a method for performing polarization treatment on ceramics in a fine particle state, and a biomaterial using ceramic fine particles polarized by the method.
  • the present invention relates to the following.
  • a member containing ceramics is provided between the first electrode that acts as the positive electrode and the second electrode that acts as the negative electrode disposed to face the first electrode, and the second electrode and the second electrode.
  • An electric field gradient of 0.5 kV / cm or more is formed between the first electrode and the second electrode in a state where the first electrode and the second electrode are arranged in a non-contact state with at least one electrode selected from the above electrodes
  • the ceramic polarization treatment method according to 1 above, wherein the ceramic-containing member is ceramic fine particles. 5).
  • the calcium phosphate compound is selected from the group consisting of ⁇ -type tricalcium phosphate, ⁇ -type tricalcium phosphate, hydroxyapatite, carbonate apatite, and combinations thereof, 11. 10.
  • the present invention it is possible to easily polarize a member including ceramics having any shape, and to prevent surface contamination caused by electrodes used for the polarization treatment.
  • a processing method can be provided.
  • a polarization treatment method capable of performing polarization treatment on ceramics in a fine particle state, and a biomaterial using the polarized ceramic fine particles can be provided.
  • the biomaterial of the present invention contains polarized ceramic fine particles, it has a high cell activation effect. Therefore, according to the present invention, it is possible to provide a biomaterial including the ceramic fine particles subjected to the polarization treatment and the biocompatible polymer compound, in particular, a biomaterial suitable for treatment of tissue damage or defect.
  • FIG. 1 is a schematic diagram showing an example of a ceramic polarization treatment method of the present invention.
  • FIG. 2 is a schematic diagram showing another example of the ceramic polarization treatment method of the present invention.
  • FIG. 3 is a schematic diagram illustrating the polarization treatment method of Example A1.
  • FIG. 4 is a graph showing the TSDC measurement results of Example A1.
  • FIG. 5 is a graph showing the TSDC measurement results of Comparative Example A1.
  • FIG. 6 is a graph showing TSDC measurement results of Examples B1 and B2.
  • FIG. 7 is a graph showing the TSDC measurement results of Comparative Example B1.
  • a member containing ceramics is provided between a first electrode that acts as a positive electrode and a second electrode that acts as a negative electrode disposed to face the first electrode. , 0.5 kV between the first electrode and the second electrode in a state where the first electrode and the second electrode are arranged in a non-contact state with at least one electrode selected from the first electrode and the second electrode.
  • the ceramic is subjected to polarization treatment by applying a voltage to the first electrode and the second electrode so that an electric field gradient of at least / cm is formed.
  • the polarization treatment is performed in a state where at least one of the first electrode and the second electrode is disposed in a non-contact position with a member containing ceramics. Therefore, it is possible to easily polarize a member including ceramics having any shape.
  • the electrode is disposed so as not to contact the surface of the member. Can be polarized.
  • the polarization treatment can be performed without damaging the shape by applying pressure to the ceramic.
  • non-contact means that the electrode is not in electrical contact with a member containing ceramics. If the electrode is not in contact with the member containing ceramics, there is no particular limitation on the distance between them, but the distance between the electrode and the member containing ceramics is, for example, in the range of 0.1 mm to 5 cm, or 0.5 mm to The range is 1 cm, or 1 mm to 5 mm.
  • the electric field gradient formed between the first electrode and the second electrode needs to be 0.5 kV / cm or more.
  • the electric field gradient is less than 0.5 kV / cm, the ceramic cannot be polarized.
  • the electric field gradient is preferably 1 kV / cm or more, and more preferably 5 kV / cm or more.
  • the upper limit of the electric field gradient is not particularly limited, but is preferably 20 kV / cm or less from a practical viewpoint such as a power source that can be used to apply a voltage.
  • the treatment temperature during the polarization treatment is not particularly limited, and can be arbitrarily selected according to the purpose, for example, in the range of room temperature (20 ° C.) to about 1000 ° C.
  • room temperature 20 ° C.
  • the treatment temperature is preferably higher.
  • the treatment temperature is preferably 200 ° C. or higher, and more preferably 300 ° C. or higher.
  • the upper limit of the treatment temperature may be in a range in which the member containing ceramics used for the polarization treatment is not decomposed, damaged, or oxidized and deteriorated by heating.
  • the temperature is generally preferably 500 ° C. or lower, and more preferably 400 ° C. or lower.
  • the member containing ceramics used for the polarization treatment may be a member composed only of ceramics (hereinafter sometimes referred to as a “bulk member”), but a solid member other than ceramics such as a metal member (hereinafter referred to as “a bulk member”). And a member composed of a ceramic film covering at least a part of the surface of the solid member (hereinafter, sometimes referred to as “ceramic film coating member”).
  • Examples of the material constituting the solid member other than ceramics include glass and resin other than the above-described metals.
  • the metal material constituting the metal member is not particularly limited, and can be appropriately selected according to the application of the ceramic film coating member.
  • a known metal material such as stainless steel, titanium, or a titanium alloy can be used.
  • the ceramic film coating member is used as a biomaterial used in a living body such as an artificial bone, an artificial tooth root, or a fracture fixing material
  • a biomaterial used in a living body such as an artificial bone, an artificial tooth root, or a fracture fixing material
  • stainless steel such as SUS316L, Co -Cr alloy, COP alloy (Fe-20Cr-20Ni-20Co-4Mo-0.2P [unit: mass%]), titanium, and titanium alloys such as Ti-Al-V alloy and Ti-Al-Nb alloy, Can be used.
  • the film thickness of the ceramic film provided on the ceramic film coating member is not particularly limited and can be appropriately selected depending on the application, but when used as a biomaterial, it may be in the range of 1 ⁇ m to 100 ⁇ m. Preferably, it is in the range of 5 ⁇ m to 50 ⁇ m.
  • the ceramic film can be formed so as to cover an arbitrary region on the surface of the support member, and may be formed so as to cover only a part of the surface of the support member depending on the application. It may be formed so as to cover the entire surface.
  • the shape of the bulk member and the support member is not particularly limited, and may be a simple shape such as a flat plate shape, a disk shape, or a column shape. Moreover, it may have a complicated shape such as an artificial bone or an artificial tooth root that can be used as a substitute member for a bone forming a human or animal skeleton, such as a femur.
  • the supporting member is a ceramic film coating member made of a metal member
  • the ceramic film may be formed so as to cover the surface of the screw portion.
  • an artificial tooth root using titanium as a metal member and using hydroxyapatite as a ceramic film coated on the surface of a screw part can be cited.
  • the polarization treatment can be performed even using an electrode having a simple shape such as a flat plate shape.
  • the distance between the member having a complicated shape and the electrode varies depending on the position of the member surface, when the member having the complicated shape is a ceramic film coating member, the ceramic film coated on the surface of the support member is uniform and A uniform polarization process may be difficult. Therefore, in such a case, it is preferable to use an electrode (hereinafter sometimes referred to as a “similar electrode”) having a shape that is substantially similar to and slightly larger than the surface shape of a member having a complicated shape. .
  • “larger shape” means the distance between the surface of a member having a complicated shape and the surface of a similar electrode positioned in a direction perpendicular to the surface (the surface facing the member having a complicated shape).
  • the distance (margin distance) between the member having the complicated shape and the similar electrode is 1 mm to 5 mm. It is within the range.
  • the ceramic film coated on the surface of the support member can be uniformly and uniformly polarized.
  • a similar electrode is not required to have a very high shape accuracy like a close contact electrode, so that it is very easy to manufacture and low cost.
  • the surface of the bulk member or the ceramic film may be smooth or uneven.
  • the degree of unevenness is not particularly limited and can be appropriately selected depending on the application.
  • the bulk member surface or the support surface on which the ceramic film is formed may be porous.
  • the surface of the bulk member or the ceramic film is rough enough to have roughened surface by sandblasting (center average roughness Ra is about 1 ⁇ m) to unevenness with a height difference of about 5 mm. It is preferable to have a thickness. From the same viewpoint, the surface of the bulk member or the support surface on which the ceramic film is formed may be porous.
  • the member containing ceramics used for the polarization treatment may be ceramic fine particles.
  • ceramic fine particles having an average particle size of 0.1 to 1000 ⁇ m, or 1 to 500 ⁇ m, or 10 to 300 ⁇ m can be used.
  • the member containing ceramics is ceramic fine particles
  • the member may be composed of only ceramic fine particles, or may be mixed with fine particles of a solid member other than ceramics.
  • the average particle diameter can be measured by, for example, a microscope method, an optical scanning method, a laser diffraction scattering method, or the like.
  • the ceramic fine particles may be porous fine particles.
  • the ceramic constituting the ceramic-containing member is not particularly limited as long as it is a ceramic material that can be polarized.
  • ⁇ -type tricalcium phosphate, ⁇ -type tricalcium phosphate, hydroxyapatite, carbonate apatite, and fluorapatite Calcium phosphate compounds such as barium titanate, strontium hydroxide apatite, calcium and strontium solid solution hydroxyapatite, lithium niobate, sodium niobate, potassium niobate, zirconia, ⁇ -alumina, and inorganic materials thereof
  • examples include materials containing at least two types of inorganic materials.
  • hydroxyapatite, ⁇ -type tricalcium phosphate, ⁇ -type tricalcium phosphate, and inorganic materials obtained by mixing these are particularly preferable because they exhibit excellent affinity as a biomaterial.
  • FIG. 1 is a schematic diagram showing an example of a ceramic polarization treatment method of the present invention.
  • 10 and 20 are flat electrodes
  • 30 is a disk-shaped sample (a member containing ceramics)
  • 40 is a DC power source
  • 50 is a non-conductive member.
  • the two flat electrodes 10 and 20 connected to the DC power supply 40 are arranged to face each other so that the electrode surfaces are parallel to each other, and the disk-shaped sample 30 is interposed between the pair of electrodes 10 and 20. Is installed. In this state, a voltage is applied between the electrodes 10 and 20, and the disk-shaped sample 30 is polarized.
  • the disk-shaped sample 30 may be arranged so as to be in contact with one electrode 10 and not in contact with the other electrode 20, as shown in FIG.
  • the electrodes 10 and 20 may be arranged without contacting each other.
  • a resin is placed in the gap between the electrode 20 and the disk-shaped sample 30 in a state where the electrode 20 is in contact with the other electrode 20 and is not in contact with the other electrode 20.
  • An insulating member 50 such as a film can also be disposed.
  • the distance X between the electrode 20 and the disk-shaped sample 30 is usually 0.1 mm although it depends on the polarization treatment such as the strength of the electric field gradient formed between the electrodes 10 and 20. It is preferably in the range of ⁇ 5 cm, and more preferably in the range of 0.5 mm to 1 cm, or 1 mm to 5 mm.
  • the distance X is less than 0.1 mm, the electrodes 20 and the disk-shaped sample 30 are likely to come into contact with each other. Therefore, it is not preferable particularly when contamination of the surface of the disk-shaped sample 30 or generation of scratches becomes a problem.
  • the distance X exceeds 5 cm, it may be necessary to apply a very large voltage between the electrodes 10 and 20 in order to obtain an electric field gradient necessary for the polarization treatment.
  • the electrodes 10, 20, the disk-shaped sample 30, and the insulating member 250 can be placed in a heating furnace to perform polarization treatment.
  • the member containing ceramics to be polarized is ceramic fine particles
  • a layer containing ceramic fine particles is provided on the electrode 10 with a uniform thickness instead of the disk-shaped sample 30 in FIG.
  • the polarization process can be performed.
  • the ceramic fine particles in the container can be polarized by placing the ceramic fine particles in a suitable container and placing it in place of the disk-shaped sample 30 in FIGS. 1 (A) and 1 (B). .
  • FIG. 2 is a schematic diagram (cross-sectional view) showing another example of the ceramic polarization treatment method of the present invention, in which 100 and 110 are electrodes, 120 is a sample (a member containing ceramics), and 120A is a screw. , 120B is a base, and 400 is a DC power source.
  • the sample 120 used for the polarization treatment includes a disk-shaped base 120B and a screw portion 120A provided on the upper surface of the base 120B, and the base 120B and the screw portion 120A are made of metal.
  • a ceramic film (not shown) is coated only on the surface of the screw portion 120A.
  • titanium can be used as the metal constituting the base portion 120B and the screw portion 120A, and hydroxyapatite can be used as the ceramic film.
  • polarized ceramics can be used as a material for proliferating living cells.
  • ceramic fine particles can be polarized.
  • the polarized ceramic is in a fine particle state, various materials can be easily prepared by combining with other components as compared with the case where the ceramic is in a lump state.
  • the present invention provides, as one aspect, a biomaterial containing ceramic fine particles polarized by the method of the present invention, a biocompatible polymer compound, and a liquid medium. Moreover, as one aspect, a biomaterial comprising a biocompatible polymer compound in which ceramic fine particles polarized by the method of the present invention are uniformly dispersed and a liquid medium is provided.
  • the ceramic that can be used for the biomaterial of the present invention is not particularly limited as long as it is a ceramic that can be polarized and applied to a living body.
  • a calcium phosphate compound can be used in that it exhibits excellent affinity as a biomaterial.
  • Examples of calcium phosphate compounds include ⁇ -type tricalcium phosphate ( ⁇ -TCP), ⁇ -type tricalcium phosphate ( ⁇ -TCP), calcium hydrogen phosphate, calcium hydrogen phosphate dihydrate, and tetracalcium phosphate. , Octacalcium phosphate, hydroxyapatite, carbonate apatite, and fluorinated apatite. These calcium phosphate compounds can be used in combination of two or more.
  • the ceramic fine particle used in the biomaterial of the present invention is not particularly limited as long as it is polarized.
  • the biomaterial of the present invention contains polarized ceramic fine particles, a biocompatible polymer compound and a liquid medium, and, if necessary, inorganic salts such as sodium chloride, calcium chloride, sodium phosphate and sodium carbonate Other components such as fine particles of ceramics (for example, calcium phosphate compound) that have not been polarized can be included.
  • the biomaterial of the present invention is obtained by dissolving or dispersing polarized ceramic fine particles and the other components used as necessary in a biocompatible polymer compound or the liquid medium.
  • the ratio of the ceramic fine particles subjected to the polarization treatment and the biocompatible polymer compound in the biomaterial of the present invention is, for example, 1 to 500 masses of the ceramic fine particles subjected to the polarization treatment per 100 parts by mass of the biocompatible polymer compound. Part, or 5 to 100 parts by mass, or 10 to 50 parts by mass.
  • the liquid medium is used in an amount of 1 to 5000 parts by mass, 10 to 1000 parts by mass, or 100 to 500 parts by mass with respect to 100 parts by mass of the total mass of the ceramic fine particles subjected to polarization treatment and the biocompatible polymer compound. Can do.
  • the other components used as necessary can be used in an amount of 1 to 100 parts by mass with respect to 100 parts by mass of the total mass of the polarized ceramic fine particles and the biocompatible polymer compound.
  • the total mass is suitably 1 to 100 parts by mass with respect to the total mass of 100 parts by mass of the ceramic fine particles and the biocompatible polymer compound. Can be used in combination.
  • the biocompatible polymer compound refers to a polymer compound that does not adversely affect the living body such as a strong inflammatory reaction in the surface of the living body or in vivo when applied to a living body.
  • polymer compound examples include natural high compounds such as fibroin, agarose, collagen, chitosan, glycosaminoglycan, hyaluronic acid, chondroitin sulfate, alginic acid, starch, pectin and pectinic acid. Mention may be made of molecular compounds. Examples thereof include synthetic polymer compounds exhibiting bioabsorbability such as polyvinyl alcohol, polyethylene glycol, polymethyl methacrylate, methacrylate ester polymer, silicone resin, polylactic acid, polyglycolic acid and poly- ⁇ -caprolactone. . Such a high molecular compound can be used individually or in combination of 2 or more types. The molecular weight of such a polymer compound is, for example, 5000 to 1000000, or 10,000 to 500000, or 20000 to 100,000 as a weight average molecular weight.
  • liquid medium examples include water, ethanol, artificial body fluid, physiological saline, and a mixture thereof.
  • the biomaterial of the present invention containing fine ceramic particles after polarization treatment is, for example, an optimal mixing ratio of the liquid ceramic medium to the biocompatible polymer compound, and other components used as necessary. Can be prepared by mixing.
  • the biomaterial of the present invention can be prepared in the form of a suspension, gel, paste, etc., depending on the amount of the liquid medium used, the type and amount of the biocompatible polymer compound, and the like.
  • the biomaterial of the present invention comprising a biocompatible polymer compound in which polarized ceramic fine particles are dispersed exhibits excellent biocompatibility, and since it contains polarized ceramic fine particles, Has an activating effect. Therefore, the biomaterial of the present invention can be applied to a living body surface and in vivo damage or a tissue defect site for the purpose of treatment or the like.
  • the biomaterial of the present invention can be applied by an appropriate method such as applying the biomaterial of the present invention to a wound portion on the surface of a living body or injecting it into a tissue defect site. Then, by activating the applied site and surrounding cells, the cells can be differentiated and proliferated to promote tissue regeneration.
  • the biomaterial of the present invention in which the ceramic is a calcium phosphate compound can be applied to a bone defect and used as a material for bone replacement and regeneration.
  • a gel-like material composed of a biocompatible polymer compound and a liquid medium in which fine particles of a calcium phosphate compound subjected to polarization treatment are uniformly dispersed or dissolved, and inject the material into a bone defect.
  • the biomaterial of the present invention containing polarized carbonate apatite or ⁇ -TCP is less susceptible to ectopic calcification because carbonate apatite and ⁇ -TCP are bioabsorbable. Therefore, a biomaterial containing carbonate apatite or ⁇ -TCP subjected to polarization treatment can be suitably used not only for regeneration of hard tissue but also for regeneration of soft tissue.
  • the biomaterial of the present invention can stimulate and activate cells, application to the skin activates skin keratinocytes and subcutaneous fibroblasts to remove fine lines, etc. Preventive effect can be expected (anti-aging effect). In addition, if melanocytes are activated, the same effect as a tanning salon can be expected safely without receiving ultraviolet rays (beauty effect).
  • the action of the biomaterial of the present invention on a living body can be evaluated by, for example, any one of the following methods (i) to (v):
  • the biomaterial of the present invention is applied or transplanted (treatment of skin ulcers and burns) to the rat dorsal skin defect, or the biomaterial of the present invention is injected subcutaneously (soft tissue formation). This histologically quantifies absorption rate, biocompatibility, neovascular invasion and soft tissue replacement;
  • IIi) Using a rat sciatic nerve constriction model the biomaterial of the present invention is injected around the nerve constriction portion, and histological observation and functional evaluation of nerve regeneration are performed over time (promotion of damaged nerve regeneration).
  • a sciatic nerve defect model is prepared, and the biomaterial of the present invention is immobilized on an artificial nerve and crosslinked and transplanted to evaluate nerve regeneration inducing ability beyond the nerve defect part (crosslinking of the nerve defect part).
  • the biomaterial of the present invention is injected around the sciatic nerve of a spontaneously diabetic rat and the same evaluation is performed (treatment of multiple neuropathy);
  • a bone marrow abrasion model (bone marrow wear model) is prepared by hollowing out the femur bone marrow of the rat, and the biomaterial of the present invention is injected to observe the bone regeneration process and measure the bone mass histologically with ⁇ CT.
  • the biomaterial of the present invention is injected around the carotid artery of a spontaneously developing rat with arteriosclerosis, and cerebral blood flow is measured using functional MRI or MRI angio (vascular endothelium, damaged vascular regeneration promotion); and (v ) Various cells are cultured on a petri dish coated with the biomaterial of the present invention, and cell differentiation / proliferation and gene expression levels of various cytokines are measured (effect on cells at the gene level).
  • the prepared HA precursor was aged at room temperature and separated into a supernatant and a precipitate, and the precipitate was filtered.
  • the filtrated product was dried at 60 ° C. and coarsely pulverized in a mortar, and calcined at 850 ° C. for 2 hours to obtain HA powder. After calcination, the HA powder was pulverized in a mortar and classified to a particle size of 74 to 149 ⁇ m using a sieve.
  • Target material 60CaO-40P 2 O 5 glass • Power density: 8.5 W / cm 2 Sputtering gas: Ar 80% by volume + CO 2 20% by volume ⁇ Sputtering gas pressure: 0.67 Pa ⁇ Target distance: 50mm Sputtering device: Multifunctional PVD device manufactured by Vacuum Metallurgical Co., Ltd. Next, a ceramic film coating sample was obtained by firing the disk on which this inorganic film was formed at 700 ° C. in a steam stream.
  • Example A1 The bulk sample was placed in an alumina tube (height 2 mm, inner diameter 20 mm, outer diameter 25 mm), and the upper and lower sides thereof were sandwiched by platinum electrodes (vertical 20 mm, width 20 mm, thickness 0.2 mm) to perform polarization treatment.
  • FIG. 3 is a schematic diagram showing a cross section of an embodiment of the present polarization treatment.
  • 10 'and 20' are platinum electrodes, 30 'is a sample, 40' is a DC power source, 50 'is an alumina plate, and 60' is an alumina tube.
  • the bulk sample (30 ′) is in contact with only one platinum electrode (10 ′), and the other platinum electrode (20 ′) is disposed by an alumina tube (60 ′) arranged so as to surround the bulk sample.
  • the sample is not in contact (the distance X between the sample 30 ′ and the electrode 20 ′ is 1 mm, and the distance Y between the platinum electrodes is 2 mm).
  • Example A1 the polarization treatment was performed in the same manner as in Example A1 except that the polarization treatment was performed with the distance X between the sample 30 ′ and the electrode 20 ′ set to 0 mm (that is, the contact method).
  • TSDC measurement is a method in which a sample in a polarized state is heated at a constant speed, and a relaxation phenomenon at the time when a frozen charge in a quasi-equilibrium state shifts to a thermal equilibrium state is measured as a depolarization current.
  • TSDC measurement is performed when the bulk sample is heated from room temperature to 700 ° C. at a heating rate of 5 ° C./min with the electrodes attached to both surfaces of the polarized bulk sample. This was done by measuring the current generated in the process of relaxation.
  • the results of TSDC measurement are shown in FIG. 4 (Example A1) and FIG. 5 (Comparative Example A1). 4 and 5, the horizontal axis represents temperature (° C.), and the vertical axis represents the amount of current per unit area (nA / cm 2 ).
  • FIG. 5 also shows the measurement results of a sample that has not been polarized.
  • Example A1 As is clear from FIGS. 4 and 5, although the amount of current detected was smaller in Example A1 than in Comparative Example A1, a current associated with the heat treatment was observed. From this, it was found that the ceramic could be polarized even if the ceramic and the electrode were arranged in a non-contact manner.
  • thermo stimulation relaxation current shown on the vertical axis of FIGS.
  • the coated sample is placed in an alumina tube (height 5.1 mm, inner diameter 20 mm, outer diameter 25 mm), and the upper and lower sides of the coated sample are on the upper side (side on which the electrode 20 'is placed).
  • the sample was heated to 300 ° C.
  • Example B2 Polarization treatment was performed in the same manner as in Example B1 except that an alumina tube having a height of 7.1 mm was used and the distance X was set to 4 mm.
  • Example B1 The polarization treatment was performed in the same manner as in Example B1, except that the polarization treatment was performed at a distance X of 0 mm (that is, the contact method) in Example B1.
  • Evaluation The presence or degree of the polarization state was evaluated by performing TSDC measurement on the polarization-treated ceramic film coating sample.
  • TSDC measurement is performed when a ceramic film coating sample is heated from room temperature to 700 ° C. at a temperature rising rate of 5 ° C./min in a state where electrodes are adhered to both surfaces of the polarization-treated ceramic film coating sample. This was carried out by measuring the current generated in the process in which the polarization state of the coating sample was relaxed.
  • the results of TSDC measurement are shown in FIG. 6 (Examples B1 and B2) and FIG. 7 (Comparative Example B1). 6 and 7, the horizontal axis represents temperature (° C.), and the vertical axis represents the amount of current per unit area (nA / cm 2 ).
  • the accumulated charge amount Q ( ⁇ C / cm 2 ) obtained by time integration of the current value (thermal stimulation relaxation current) shown on the vertical axis in FIGS. 6 and 7 according to Equation 1 is as follows.
  • Example B2: Q 2.1 Comparative
  • Example B1: Q 1.8

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Abstract

La présente invention concerne un procédé permettant la polarisation de céramique, caractérisé en ce qu'il comprend la disposition d'un élément contenant de la céramique entre une première électrode, qui fonctionne comme une électrode positive, et une seconde électrode, qui fonctionne comme une électrode négative disposée à l'opposé de la première électrode, de sorte que l'élément contenant de la céramique ne soit pas en contact avec au moins une électrode parmi la première électrode et la seconde électrode, et l'application d'une tension à la première électrode et à la seconde électrode pour former un gradient de champ électrique égal ou inférieur à 0,5 kV/cm entre la première électrode et la seconde électrode, entraînant la polarisation de la céramique. L'invention concerne également un biomatériau contenant de fines particules de céramique soumises à une polarisation par le procédé selon l'invention.
PCT/JP2009/059433 2008-05-23 2009-05-22 Procédé permettant la polarisation de céramique et biomatériau contenant une céramique polarisée Ceased WO2009142296A1 (fr)

Applications Claiming Priority (2)

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JP2008135751A JP5414021B2 (ja) 2008-05-23 2008-05-23 セラミックスの分極処理方法及び分極処理したセラミックスを含む生体材料
JP2008-135751 2008-05-23

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WO2009142296A1 true WO2009142296A1 (fr) 2009-11-26

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