METHOD FOR PRODUCING UNIFORM BETA-TRICALCIUM PHOSPHATE-BASED BONE CHIP AND BONE CHIP PRODUCED BY METHOD

Hereinafter, the present invention it relates to 2000.

The term used in the present invention all techniques, are not defined or more with, typically encountered in the field of the present invention is generally understand has for the definition of such as sense of one skilled met substrate. In addition the method include a specification or sample are described or, the category of the present invention are also similar or equivalent multiple myelomas are included. The specification described in the present invention are introduced into the contents of the document on the right side of all Publication.

Terms "about" that he was a reference amount, level, value, number, frequency, percentage, dimension, size, amount, weight or length 30, 25, 20, 25, 10, 9, 8, 7, 6, 5, 4, 3, 2 or 1% amount to change degree, level, value, number, frequency, percentage, dimension, size, amount, big weight or length.

The specification through, if context of the race not needed, "comprising" and "including" RM the horse number it became at the time of steps or components, or elements or steps including but group of, any other steps or components, or elements or steps but not to contain a group of the ship number understood to accomplishing.

The present invention according to the sintered body as on chip is beta tricalcium phosphate, beta-tricalcium phosphate (beta-tricalcium phosphate) said hydroxyapatite powder is incident into the bone graft material (hydroxyapatite) powder with one kind of powder biometric ceramic (-decoder a ceramic) are disclosed. Said hydroxyapatite in vivo due to low solubility completely bone grows up into bone joined at longer end which does not destroy the remaining patterned be substituted.

While, beta phase tree calcium phosphate hydroxyapatite bone directly engages the point similar to that of the full-length properties and are ultimately dissolved in vivo but decreasing 2000. In particular bone marrow latency beta phase tricalcium phosphate (wet implantation it boils re- bone defect site; Bone filler) to are located. Beta-tricalcium phosphate dense bone marrow latency bulk form which are disposed, etc. connected pores porous structure and form of the granule. In addition in the form of dense granular bulk (Bulk) porous structure of beta tricalcium phosphate in order to using sufficient strength to have high relative density should receives the sintering.

However, beta tricalcium phosphate is covered and sinter, since α β phase homogeneous on release since it disclosed. I.e., having hexagonal crystals on low temperature on β, β phase temperature of the heat treatment at a temperature of 1100 - 1180 °C on the α phase on the hot temperature having the monoclinal political world onto each other. The temperature of the α phase is water and since write is bio-implant violent reaction-polyisobutylene disclosed. In addition, α β phase such that on low density onto a sintered body of material causing fine cracking to control lowering substrate. Preferably said etc. for reasons of artificial bone materials include beta phase tricalcium phosphate. However beta phase tricalcium phosphate or hydroxyapatite and a beta-tricalcium phosphate composite sintering temperature in order to obtain the phase transition temperature is 1180 °C hereinafter on sintering in one, usually at a temperature state in a relative density of 90% hereinafter the powders to obtain the pin is point number door difficult. The, bioabsorbable excellent biomaterial beta phase tricalcium phosphate in order to obtain high-density sintered body applicable to the inside of the pipe.

According to the manufacturing method of the chip according to the first form of the present invention number 1 embodiment, beta phase tricalcium phosphate (hereinafter, beta-tCP ' also is provided to to by) decodes the calcined powder. The beta phase tricalcium phosphate precursor powder by treating the calcined dispersible, increasing the strength and gamma sterilization can be adjusting a color change. Preferably about 1 - 3 hours the 600 - 800 °C calcining said calcining.

Next, beta phase said tricalcium phosphate powder disintegration substrate.

Said calcined tricalcium phosphate powder treated beta phase mixture number sodium ball mill process using an high pressure liquid coolant therein. Ball mill process adding an acidic solution through the promotion of increased strength.

Said sodium content and size so as to control porosity and pores can be sintered or a quadrature mirror filter.

Next, whether mixed with a binder to said mixture of ethyl cellulose as number the shaped bodies such as high pressure liquid coolant therein. Said molded single or multi-layer can be formed, one not publicly known manufacturing method are specially number enabled by pressure molding of 2000.

Finally said ceramic substrate.

Said cool by the conventional electric furnace atmosphere, at a temperature of 300 °C provided 1230 °C a plurality of hierarchies. Preferably 1 step 100 - 500 °C, more preferably 300 °C holding in 2 - 4 hours, 2 step 600 - 900 °C, more preferably 600 °C maintains in 2 - 4 hours, 3 steps 1000 - 1300 °C, preferably 1230 °C 15 preferably performed maintaining in time. The reason for wanting to about 300 °C moisture in a heat treatment step, a stand-alone number and organic binder, about 600 °C residual organic matter after sodium to volatilize to produce a pore number form a stand-alone, a sintering process at the process 1230 °C beta on phase transition as follows.

In the present invention in the sintered ceramic double shield (shield) to prevent a penetration gas into and through and to keep constant the partial pressure of oxygen content in the sintered by a non-uniform composition on light emitting unit door door number number can be solve.

Specifically, preferably a high purity alumina ceramic boat for using said dual shield. The size of the alumina ceramic boat specially number not meter one proportional to a substrate. In addition composition preferably 99% or more, more preferably 99. 7% or more Al₂ O₃ High purity alumina containing less than 2000.

Benzofuran as in sintering process and cooling shield technique employing constant inflow of external air to be coated. In order to number 15 on pure beta tricalcium phosphate 1230 °C during sintering time of high temperature high pressure liquid coolant to decide, double shield on an end surface forming surface in addition in sintering temperature constant disclosed. In a preferred embodiment, molded body surface oxygen partial pressure comprises an atmospheric reference about 0. 19 - 0. 23 can extent to stay fairly constant.

Of the present invention number 2 embodiment form there is a, the chip comprising the manufacturing method comprises the following steps.

Sodium beta-tCP powder mixing;

Uniaxial pressing said mixture forming step number tank shaped bodies; and

Said shaped bodies at a temperature of 300 °C provided 1230 °C mixed material;

Said aforementioned sodium beta-tCP powder as described, ball mill method preferably cassette is provided.

The embodiment in one form of ethyl cellulose as an organic binder such as uniaxial pressing molding number through the shaped bodies without the use of high pressure liquid coolant therein. The molding is molded using a mold and said uniaxial pressing, can be disks using a magnetic field to mold. Conventional binders such as when molding said number of ethyl cellulose to form high pressure liquid coolant bath gel frame number when the pores of the sintered valve closes in an resulting strength and dispersibility of the prepared by the number chip can be significantly reduced. However, when formed so as to enhance the strength reduces can be uniaxial pressing inside pores.

Said shaped bodies at a temperature of 300 °C provided 1230 °C step number 1 embodiment described efined form prior to sintering.

According of the present invention prepared by the number of the existing method described above the copper chip is the chip before use and is coupled with the constant color changed to gamma sterilization can be spacer. In respect of the grinding/chip number prepared by the pore generating checking, classification/weight measurement, ultrasonic cleaning and sterilizing the dried S. to detect a pH measuring compatibility.

Hereinafter, the present invention in the embodiment experiments e.g. on a detailed the on-sensors other. However the present invention is limited to are not correct.

[In the embodiment 1] number 1 embodiment form according to the number of the chip tank

Average particle diameter (D50) in a range of 1 - 50 μm 600 °C % by weight beta-tCP 500g and calcined mixed through sodium 300g the wheat law and ball % by weight. Sodium pH is 6. 7 - 7. 3 ranges. Mixing said mixture 30g % by weight ethyl cellulose and a number then molding high pressure liquid coolant, said shaped bodies in holding time 300 °C 3, 600 °C maintains in 3 hours, 15 in the present invention according to the sintering time 1230 °C chip number was high pressure liquid coolant. At this time alumina ceramic boat was the use shield. After photographed in fig. 2 shown to sterilizing chip the number produced therewith.

Wherein, alumina ceramic boat also 5 as shown in the variation, about 50 mm height, horizontal and vertical about 100 mm, 200 mm of boat was used. Thickness is about 5 mm are disclosed. Alumina ceramic boat 99. 7% or more purity alumina containing Al2O 3 using substrate.

[Comparison example 1]

Beta-tCP powder is calcined by processing said in the embodiment 1 was not point in the same number for which the chip number under the outside method and high pressure liquid coolant and said in the embodiment 1, gamma sterilization of him. Color change to 3 also shown after sterilization.

[In the embodiment 2] number 2 embodiment form according to the number of the chip tank

Average particle diameter (D50) in the range of 1 - 50 μm sodium 60g and ball the wheat law 100g beta-tCP powder is mixed through. Sodium pH is 6. 7 - 7. 3 ranges. The disc like uniaxial pressing said mixture into a shaped body molded mold are obtained. Shaped bodies in said holding time 300 °C 3, 600 °C maintains in 3 hours, 15 in the present invention according to the sintering time 1230 °C chip number was high pressure liquid coolant. At this time alumina ceramic boat was the use shield. After photographed in fig. 3 shown to chip the number produced therewith for sterilizing.

A feature of the present invention sends more description is provided to exemplify the generally described, the present invention if the properties of the present invention is provided to essentially inputted from deviating from a person with skill in the art in various modifications and deformable will. Thus, the present invention in the embodiment of the present invention are to define the disclosure but rather to explain the feature and, in the embodiment of the present invention by not the limited range of such feature. Under the protection range of the present invention must be interpreted by fee so as to range, and the range of the present invention feature in a range equal to all rights will be interpreted.