JPH05105463A - Production of crystallized glass - Google Patents
Production of crystallized glassInfo
- Publication number
- JPH05105463A JPH05105463A JP3303944A JP30394491A JPH05105463A JP H05105463 A JPH05105463 A JP H05105463A JP 3303944 A JP3303944 A JP 3303944A JP 30394491 A JP30394491 A JP 30394491A JP H05105463 A JPH05105463 A JP H05105463A
- Authority
- JP
- Japan
- Prior art keywords
- crystallized glass
- mold
- glass
- slip
- binder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Dental Preparations (AREA)
- Glass Compositions (AREA)
- Materials For Medical Uses (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、結晶化ガラスの製造方
法に関し、特に医用材料として有用な結晶化ガラスの製
造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing crystallized glass, and more particularly to a method for producing crystallized glass useful as a medical material.
【０００２】[0002]
【従来の技術】従来、欠損した骨の補填には、患者本人
の正常部位から採取した自家骨が用いられてきたが、こ
の方法では損傷箇所以外の骨組織を切除するため、患者
の苦痛が大きいこと、手術を行うに当たって多大な労力
を要すること、また自家骨の採取量に限界があること等
の問題を有している。2. Description of the Related Art Conventionally, autologous bone collected from a normal site of a patient has been used to replace a defective bone. However, this method excises bone tissue other than the damaged site, resulting in patient's pain. There are problems such as being large, requiring a great deal of labor in performing surgery, and having a limited amount of autogenous bone to be collected.
【０００３】このような事情から、自家骨の代わりに人
工的に作製したインプラント材を使用することが試みら
れている。これらインプラント材の中で近年注目を集め
ているものに、ＳｉＯ2 −ＣａＯ−ＭｇＯ系や、ＳｉＯ
2 −Ｐ2 Ｏ5 −ＣａＯ−ＭｇＯ系等の結晶化ガラスがあ
る。Under these circumstances, it has been attempted to use an artificially produced implant material instead of the autologous bone. Among these implant materials, the ones that have been attracting attention in recent years include SiO 2 —CaO—MgO-based materials and SiO 2 materials.
A crystallization glass such as 2 -P 2 O 5 -CaO-MgO system.
【０００４】ところで上記した結晶化ガラスは、表面か
ら結晶化が起こるため、溶融ガラスを鋳造成形すると、
その後の結晶化の際に体積収縮が起こってクラックが発
生するため好ましくない。それゆえ通常は薄板状に成形
された結晶性ガラスを粉砕して２００メッシュ以下の粉
末とし、これをラバープレス法等によって加圧成形した
後、該成形物を焼成してガラス粉末を焼結、結晶化さ
せ、さらに所望の形状になるように切削加工することに
よって作製される。By the way, since the above-mentioned crystallized glass is crystallized from the surface, when molten glass is cast and molded,
During the subsequent crystallization, volume shrinkage occurs and cracks occur, which is not preferable. Therefore, usually, a crystalline glass formed into a thin plate is pulverized into a powder having a size of 200 mesh or less, which is pressure-molded by a rubber press method or the like, and then the molded product is fired to sinter the glass powder, It is produced by crystallizing and further cutting it into a desired shape.
【０００５】[0005]
【発明が解決しようとする課題】しかしながらこのよう
な方法では、加工に多大な労力と時間を要し、また高度
な加工技術を要するために生産性が低いこと、加工によ
る形状の自由度に制限があり、複雑な形状が得難いこ
と、加工量が多いために、結晶化ガラスにクラックが生
じて機械的強度が低下し易いこと等の問題を有してい
る。However, such a method requires a great deal of labor and time for processing, and requires high processing technology, so that the productivity is low and the degree of freedom of the shape due to processing is limited. However, there are problems that it is difficult to obtain a complicated shape, and that the amount of processing is large, cracks occur in the crystallized glass, and the mechanical strength is likely to decrease.
【０００６】本発明の目的は、生産性が高く、また複雑
な形状であっても容易に成形でき、しかも機械的強度等
の特性を損なわない結晶化ガラスの製造方法を提供する
ことである。An object of the present invention is to provide a method for producing crystallized glass which has high productivity, can be easily molded even in a complicated shape, and does not impair properties such as mechanical strength.
【０００７】[0007]
【課題を解決するための手段】本発明の結晶化ガラスの
製造方法は、アパタイト、ウオラストナイト、及びジオ
プサイドの少なくとも１種を析出する結晶性ガラス粉末
と、有機溶剤、及びバインダーを混練してスリップを作
製し、該スリップを鋳型を用いて鋳込み成形し、脱型、
乾燥後、焼成することによってバインダーを焼失させる
とともに、該結晶性ガラス粉末を焼結、結晶化させるこ
とを特徴とする。The method for producing a crystallized glass of the present invention comprises kneading a crystalline glass powder which precipitates at least one of apatite, wollastonite and diopside, an organic solvent, and a binder. A slip is produced, the slip is cast using a mold, and the mold is removed.
After drying, the binder is burned off by firing, and the crystalline glass powder is sintered and crystallized.
【０００８】[0008]
【作用】本発明の結晶化ガラスの製造方法において使用
する結晶性ガラスは、アパタイト、ウオラストナイト、
及びジオプサイドの少なくとも１種を析出するものであ
り、例えば重量百分率でＳｉＯ2 ４０〜６０％、ＣａＯ
３０〜４５％、ＭｇＯ１〜１７％（ただしＳｉＯ2 ＋
ＣａＯ＋ＭｇＯ≧９０％）の組成を有するガラスや、Ｓ
ｉＯ2 ２２〜５０％、Ｐ2Ｏ5 ８〜３０％、ＣａＯ １
２〜５３％、ＭｇＯ １〜３４％、Ｆ2 ０〜５％の組成
を有するガラスが使用できる。このような結晶性ガラス
は結晶化させることによって、高い機械的強度を有し、
また優れた生体活性及び生体親和性を示す。The crystalline glass used in the method for producing a crystallized glass of the present invention includes apatite, wollastonite,
And at least one of diopside, for example, SiO 2 40 to 60% in weight percentage, CaO
30-45%, MgO 1-17% (however, SiO 2 +
Glass having a composition of CaO + MgO ≧ 90%, S
iO 2 22-50%, P 2 O 5 8-30%, CaO 1
Glass having a composition of 2 to 53%, MgO 1 to 34%, and F 2 0 to 5% can be used. By crystallizing such a crystalline glass, it has high mechanical strength,
It also exhibits excellent bioactivity and biocompatibility.
【０００９】次に、本発明の結晶化ガラスの製造方法を
説明する。Next, a method for producing the crystallized glass of the present invention will be described.
【００１０】まず、上記したような組成を有するガラス
粉末を、有機溶剤、及びバインダーと混練してスリップ
を作製する。有機溶剤及びバインダーの混合量は、ガラ
ス粉末１００重量％に対して、各々１０〜５０％、０．
５〜１０％が好ましい。First, a glass powder having the above composition is kneaded with an organic solvent and a binder to prepare a slip. The mixing amounts of the organic solvent and the binder are 10 to 50% and 0.
5 to 10% is preferable.
【００１１】なお、ガラス粉末は２００メッシュ以下の
ものを使用することが好ましい。また生体活性を有する
ガラス粉末は耐水性が悪く、水と接すると侵食されて焼
結性が低下するため、分散媒として有機溶剤を使用す
る。有機溶剤としてはガラス粉末の分散性が良いもの、
特にメタノール、エタノール、プロパノール、ブタノー
ル等のアルコール類を単独又は混合して使用することが
好ましい。バインダーとしては種々のものが使用できる
が、特に結合力や粉末の分散性に優れたポリビニルブチ
ラール（ＰＶＢ）が好ましい。なお有機溶剤及びバイン
ダーの他にポリエチレングリコール（ＰＥＧ）やフタル
酸エステル等の可塑剤を必要に応じて添加しても良い。The glass powder is preferably 200 mesh or less. Further, since the glass powder having bioactivity is poor in water resistance and corrodes when contacted with water to reduce sinterability, an organic solvent is used as a dispersion medium. Organic solvent with good dispersibility of glass powder,
In particular, alcohols such as methanol, ethanol, propanol and butanol are preferably used alone or in combination. Although various binders can be used, polyvinyl butyral (PVB), which is particularly excellent in binding force and powder dispersibility, is preferable. In addition to the organic solvent and the binder, a plasticizer such as polyethylene glycol (PEG) or phthalic acid ester may be added if necessary.
【００１２】次に作製したスリップを、所望の形状を有
する鋳型に常圧〜１０ｋｇ／ｃｍ2程度の圧力をかけな
がら鋳込み成形した後、脱型する。なお使用する鋳型と
しては吸湿性を有するもの、例えば石膏型、多孔質樹脂
型、素焼き型等が好ましい。Next, the slip thus produced is cast-molded while applying a pressure of about 10 kg / cm 2 to atmospheric pressure in a mold having a desired shape, and then demolded. The mold to be used is preferably one having a hygroscopic property, such as a gypsum mold, a porous resin mold, a unglazed mold and the like.
【００１３】さらに得られた成形体を乾燥させ、焼成す
ることによって、バインダーを焼失させるとともに、結
晶性ガラス粉末を焼結、結晶化させて結晶化ガラスを得
る。By further drying and firing the obtained molded body, the binder is burned off, and the crystalline glass powder is sintered and crystallized to obtain crystallized glass.
【００１４】[0014]
【実施例】以下、実施例及び比較例に基づいて本発明の
結晶化ガラスの製造方法を説明する。EXAMPLES The method for producing crystallized glass of the present invention will be described below based on Examples and Comparative Examples.
【００１５】（実施例）表１及び表２は本発明の実施例
を示すものである。(Examples) Tables 1 and 2 show examples of the present invention.
【００１６】[0016]
【表１】 [Table 1]
【００１７】[0017]
【表２】 [Table 2]
【００１８】試料Ｎｏ．１〜８は次のようにして調製し
た。表中の組成になるようにガラス原料を調合し、白金
坩堝に入れて１４００〜１５００℃で４時間溶融し、ロ
ール成形した後、ボールミルにて粉砕し、２００メッシ
ュの篩で分級して結晶性ガラス粉末を得た。この結晶性
ガラス粉末１００重量％に対して有機溶剤、バインダ
ー、及び可塑剤を表に示す割合で加え、ボールミルにて
２４時間混練し、スリップを作製した。次いでこのスリ
ップを石膏型に常圧〜１０ｋｇ／ｃｍ2 の圧力で鋳込
み、３〜６０分後に脱型し、４．５×３．４×４１ｍｍ
の大きさの成形体を得た。さらにこの成形体を乾燥させ
た後、１時間に３０〜３００℃の速度で昇温し、１００
０〜１２００℃で２〜１０時間焼成して４×３×３６ｍ
ｍの試料を得た。Sample No. 1-8 were prepared as follows. Glass raw materials were mixed so as to have the composition shown in the table, put in a platinum crucible and melted at 1400 to 1500 ° C. for 4 hours, roll-formed, crushed by a ball mill, and classified by a 200-mesh sieve to crystallize. A glass powder was obtained. An organic solvent, a binder, and a plasticizer were added to 100% by weight of this crystalline glass powder in a ratio shown in the table, and kneaded in a ball mill for 24 hours to prepare a slip. Then, this slip is cast into a plaster mold at a normal pressure to a pressure of 10 kg / cm 2 , and after 3 to 60 minutes, it is demolded and 4.5 × 3.4 × 41 mm
A molded body having a size of Further, after drying this molded body, the temperature is raised at a rate of 30 to 300 ° C. for 1 hour to 100
4x3x36m by firing at 0-1200 ° C for 2-10 hours
m samples were obtained.
【００１９】このようにして得られた試料の析出結晶を
Ｘ線回折によって求めたところ、試料Ｎｏ．１〜４はウ
オラストナイト及びジオプサイドを析出しており、また
試料Ｎｏ．５〜８はさらにアパタイトを析出していた。The precipitated crystals of the sample thus obtained were determined by X-ray diffraction. Samples Nos. 1 to 4 had wollastonite and diopside deposited, and Sample No. In Nos. 5 to 8, apatite was further precipitated.
【００２０】また各試料の曲げ強度をオートグラフによ
って測定したところ、２１００〜２６００ｋｇｆ／ｃｍ
2 の値を示した。When the bending strength of each sample was measured by an autograph, it was 2100 to 2600 kgf / cm.
A value of 2 was shown.
【００２１】（比較例）実施例の試料Ｎｏ．１、５、７
と同一の組成を有するガラスを粉砕して、２００メッシ
ュの篩で分級し、ガラス粉末とした。これらのガラス粉
末をそれぞれラバープレス法によって加圧成形し、５０
×５０×１２０ｍｍの大きさの成形体を得た。次いでこ
れらの成形体を１０００〜１２００℃で２〜１０時間焼
成することによって、４３×４３×１０５ｍｍの大きさ
の結晶化ガラスを得た。さらに各結晶化ガラスをダイヤ
モンドカッターによって加工し、４×３×３６ｍｍの大
きさの試料Ｎｏ．Ａ、Ｂ、Ｃを作製した。このようにし
て得られた各試料の析出結晶は、試料Ｎｏ．Ａがウオラ
ストナイト及びジオプサイド、試料Ｎｏ．Ｂ及びＣがさ
らにアパタイトを析出していた。(Comparative Example) Sample No. of the example. 1, 5, 7
A glass having the same composition as the above was crushed and classified with a 200-mesh sieve to obtain a glass powder. Each of these glass powders was press-molded by a rubber press method,
A compact having a size of × 50 × 120 mm was obtained. Then, these molded bodies were fired at 1000 to 1200 ° C. for 2 to 10 hours to obtain crystallized glass having a size of 43 × 43 × 105 mm. Further, each crystallized glass was processed by a diamond cutter, and sample No. 4 having a size of 4 × 3 × 36 mm. A, B, and C were produced. Precipitated crystals of each sample obtained in this manner were sample No. A is wollastonite and diopside, sample No. B and C further precipitated apatite.
【００２２】次に各試料の曲げ強度を測定したところ、
試料Ｎｏ．Ａが２０００ｋｇｆ／ｃｍ2 、試料Ｎｏ．Ｂ
が２２００ｋｇｆ／ｃｍ2、試料Ｎｏ．Ｃが２３００ｋ
ｇｆ／ｃｍ2 であり、本発明の方法で製造した試料Ｎ
ｏ．１、５、７と比較すると、それぞれ３００ｋｇｆ／
ｃｍ2 、２００ｋｇｆ／ｃｍ2 、３００ｋｇｆ／ｃｍ2
も低かった。Next, when the bending strength of each sample was measured,
Sample No. A is 2000 kgf / cm 2 , and sample No. B
Of 2200 kgf / cm 2 , sample No. C is 2300k
gf / cm 2 and sample N produced by the method of the present invention
o. Compared with 1, 5, and 7, 300 kgf /
cm 2 , 200 kgf / cm 2 , 300 kgf / cm 2
Was also low.
【００２３】[0023]
【発明の効果】以上説明したように、本発明の結晶化ガ
ラスの製造方法によれば、適当な鋳型を使用することに
よって、形状が複雑な結晶化ガラスであっても容易に製
造することができる。しかも切削加工を殆ど必要としな
いために、機械的強度等の特性が低下せず、また効率良
く生産することが可能である。As described above, according to the method for producing crystallized glass of the present invention, it is possible to easily produce crystallized glass having a complicated shape by using an appropriate mold. it can. Moreover, since cutting is hardly required, characteristics such as mechanical strength are not deteriorated, and efficient production is possible.
フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｃ０３Ｃ 10/02 6971−4Ｇ 10/04 6971−4Ｇ Continuation of the front page (51) Int.Cl. 5 Identification number Office reference number FI technical display location C03C 10/02 6971-4G 10/04 6971-4G
Claims (3)
オプサイドの少なくとも１種を析出する結晶性ガラス粉
末と、有機溶剤、及びバインダーを混練してスリップを
作製し、該スリップを鋳型を用いて鋳込み成形し、脱
型、乾燥後、焼成することによってバインダーを焼失さ
せるとともに、該結晶性ガラス粉末を焼結、結晶化させ
ることを特徴とする結晶化ガラスの製造方法。1. A slip is prepared by kneading a crystalline glass powder that precipitates at least one of apatite, wollastonite, and diopside, an organic solvent, and a binder, and the slip is cast using a mold. A method for producing crystallized glass, characterized in that the binder is burned off by demolding, drying and firing, and the crystalline glass powder is sintered and crystallized.
プロパノール、若しくはブタノール、又はこれらの混合
物であることを特徴とする請求項１の結晶化ガラスの製
造方法。2. The organic solvent is methanol, ethanol,
The method for producing crystallized glass according to claim 1, which is propanol, butanol, or a mixture thereof.
あることを特徴とする請求項１の結晶化ガラスの製造方
法。3. The method for producing crystallized glass according to claim 1, wherein the binder is polyvinyl butyral.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3303944A JPH05105463A (en) | 1991-10-22 | 1991-10-22 | Production of crystallized glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3303944A JPH05105463A (en) | 1991-10-22 | 1991-10-22 | Production of crystallized glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05105463A true JPH05105463A (en) | 1993-04-27 |
Family
ID=17927172
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3303944A Pending JPH05105463A (en) | 1991-10-22 | 1991-10-22 | Production of crystallized glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05105463A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005118131A (en) * | 2003-10-14 | 2005-05-12 | Pentax Corp | CaO-MgO-SiO2 BASED BIOACTIVE GLASS AND SINTERED CALCIUM PHOSPHATE BODY USING THE SAME |
| US7332452B2 (en) | 2002-07-15 | 2008-02-19 | Pentax Corporation | CaO-SiO2-based bioactive glass and sintered calcium phosphate using same |
| JP2018504361A (en) * | 2014-11-28 | 2018-02-15 | バイオアルファ コーポレーション | High-strength crystallized glass ceramics including wollastonite, hydroxyapatite and akermanite |
| JP2019064907A (en) * | 2017-09-28 | 2019-04-25 | ショット アクチエンゲゼルシャフトＳｃｈｏｔｔ ＡＧ | Method of manufacturing glass ceramic article by slurry casting and usage thereof |
-
1991
- 1991-10-22 JP JP3303944A patent/JPH05105463A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7332452B2 (en) | 2002-07-15 | 2008-02-19 | Pentax Corporation | CaO-SiO2-based bioactive glass and sintered calcium phosphate using same |
| JP2005118131A (en) * | 2003-10-14 | 2005-05-12 | Pentax Corp | CaO-MgO-SiO2 BASED BIOACTIVE GLASS AND SINTERED CALCIUM PHOSPHATE BODY USING THE SAME |
| US7214635B2 (en) | 2003-10-14 | 2007-05-08 | Pentax Corporation | CaO-MgO-SiO2-based bioactive glass and sintered calcium phosphate glass using same |
| JP2018504361A (en) * | 2014-11-28 | 2018-02-15 | バイオアルファ コーポレーション | High-strength crystallized glass ceramics including wollastonite, hydroxyapatite and akermanite |
| JP2019064907A (en) * | 2017-09-28 | 2019-04-25 | ショット アクチエンゲゼルシャフトＳｃｈｏｔｔ ＡＧ | Method of manufacturing glass ceramic article by slurry casting and usage thereof |
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