JPH04187542A - Method for preparing glass-ceramic solidified product by hydrothermal hot press - Google Patents
Method for preparing glass-ceramic solidified product by hydrothermal hot pressInfo
- Publication number
- JPH04187542A JPH04187542A JP2314813A JP31481390A JPH04187542A JP H04187542 A JPH04187542 A JP H04187542A JP 2314813 A JP2314813 A JP 2314813A JP 31481390 A JP31481390 A JP 31481390A JP H04187542 A JPH04187542 A JP H04187542A
- Authority
- JP
- Japan
- Prior art keywords
- glass
- hot press
- hydrothermal hot
- solidified product
- hydrothermal
- 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.)
- Granted
Links
- 239000002241 glass-ceramic Substances 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 title description 7
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 239000011521 glass Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000007731 hot pressing Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 11
- 238000010438 heat treatment Methods 0.000 abstract description 5
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract description 4
- 239000007943 implant Substances 0.000 abstract description 4
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 abstract 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 abstract 2
- 230000004071 biological effect Effects 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 230000006835 compression Effects 0.000 abstract 1
- 238000007906 compression Methods 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 101100348017 Drosophila melanogaster Nazo gene Proteins 0.000 description 1
- 241000405961 Scomberomorus regalis Species 0.000 description 1
- 229910020169 SiOa Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 239000005313 bioactive glass Substances 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZTGOUSAYHCYNCG-UHFFFAOYSA-O dicalcium;sodium;dioxido(oxo)silane;hydron Chemical compound [H+].[Na+].[Ca+2].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O ZTGOUSAYHCYNCG-UHFFFAOYSA-O 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052884 pectolite Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002901 radioactive waste Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 102200021395 rs3739168 Human genes 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Glass Compositions (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、水熱ホットプレスによるガラスセラミックス
固化体の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for manufacturing a glass-ceramic solidified body by hydrothermal hot pressing.
「水熱」条件とは、１００°Ｃより高い温度て水か存在
するような条件を言い、水熱ホットプレスとは、第１図
に示すような装置内に「水を混合した試料」を充填し、
これを２つのピストンて挟んで加圧し、同時に１００°
Ｃより高い温度に加熱し、それにより試料を物理的又は
化学的に変質又は変化させて固化させる方法を言う。固
化した塊は固化体と呼ばれ、新たな用途に使用される。"Hydrothermal" conditions refer to conditions in which water is present at a temperature higher than 100°C, and hydrothermal hot press refers to conditions in which a "sample mixed with water" is placed in a device as shown in Figure 1. Fill and
Pressure is applied by sandwiching this between two pistons, and the angle is 100° at the same time.
A method of heating a sample to a temperature higher than C to physically or chemically alter or change the sample and solidify it. The solidified mass is called a solidified material, and is used for new purposes.
ところで、粉末から固化した塊を製造する方法として焼
結法かある。水熱ホットプレスは焼結法に比へ低温で固
化した塊を製造できる利点かある。Incidentally, there is a sintering method as a method for producing a solidified lump from powder. Hydrothermal hot pressing has the advantage of producing a solidified mass at a lower temperature than the sintering method.
本発明者らの一部は、他の発明者と共に、先に、試料と
して、放射性廃棄物をガラス粉体に混合したものを使用
し、これに更に水を混合して水熱ホットプレスにより固
化し、得られた固化体を廃棄物として貯蔵する試みを提
案した。Some of the present inventors, along with other inventors, first used a sample of radioactive waste mixed with glass powder, then mixed this with water and solidified it using a hydrothermal hot press. We then proposed an attempt to store the solidified material as waste.
その後、本発明者らは、試料として、ガラス粉体だけを
使用し、これに水を混合して水熱ホットプレスにより固
化させる方法で１個のガラス状の固化体を製造し、これ
を新規で有用な用途に使用しようとする試験を行なった
。Thereafter, the present inventors used only glass powder as a sample, mixed it with water, and solidified it using a hydrothermal hot press to produce a glass-like solidified body, and created a new glass-like solidified body. We conducted tests to try to use it for useful purposes.
しかしながら、得られたガラス状固化体は、圧縮強度が
満足されないという問題点を有していた。However, the obtained vitrified solidified body had a problem in that the compressive strength was not satisfied.
圧縮強度が不足していると、ガラス状固化体に新規で有
用な用途は見出せない。If the compressive strength is insufficient, new and useful uses cannot be found for the vitrified solidified product.
本発明者らは、鋭意研究の結果、試料として下記に示す
特定の組成を有するガラス粉体を使用すると、得られた
ガラス状固化体は、内部に結晶化した部分を有するガラ
スセラミックスの１種てあり、これが高い圧縮強度を有
することを見出し、本発明を成すに至った。As a result of intensive research, the present inventors found that when a glass powder having the specific composition shown below is used as a sample, the obtained glassy solidified body is a type of glass ceramic having a crystallized part inside. It has been discovered that this has high compressive strength, and the present invention has been completed.
よって、本発明は、 ［次の組成。Therefore, the present invention [The following composition.
Ｓｉ Ｏａ ４０〜７２ ｍｏｌ％（４０〜６０
ｍｏｌ％）ＣａＯＯ〜５０ ｍｏｌ％（１５〜３０ ｍ
ｏｌ％）Ｎａ２０５〜４３ＩＩＩＯ１％（５〜３０ｍｏ
ｌ％）Ｐ２０ｓ １〜６ ｍｏｌ％
（かっこ内の数値は好ましい範囲）を有するガラスの粉
体と水との混合物を、水熱ホットプレスにより固化させ
る、ことを特徴とするガラスセラミックス固化体の製造
方法」を提供する。SiOa 40-72 mol% (40-60
mol%) CaOO~50 mol% (15~30 m
ol%) Na205~43IIIO1% (5~30mo
1%) P20s 1 to 6 mol% (values in parentheses are preferred ranges) A mixture of glass powder and water is solidified by hydrothermal hot pressing. method”.
本発明で使用する上述の特定の組成（場合により、本発
明の目的を損なわない限り、少量の他の成分を含んでい
ても差し支えない）を有するガラスは、生体活性材料と
して公知である。従って、本発明の製法で得られる固化
体は、生体活性を示すのて、骨内インブラントに有用で
ある。Glasses having the above-mentioned specific compositions used in the present invention (optionally containing small amounts of other components as long as they do not defeat the purpose of the present invention) are known as bioactive materials. Therefore, the solidified product obtained by the production method of the present invention exhibits bioactivity and is useful for intraosseous implants.
しかも、既述のように、本発明の固化体は、圧縮強度が
高いのて、骨内インブラントに加工した場合、十分にそ
の役目を果たすことかできる。Furthermore, as described above, the solidified material of the present invention has high compressive strength, and therefore, when processed into an intraosseous implant, it can fully fulfill its role.
本発明を実施するには、特定の組成を有するガラスを入
手した後、１０〜２００μｍ程度の粉体に粉砕する。To carry out the present invention, glass having a specific composition is obtained and then ground into powder of approximately 10 to 200 μm.
この粉体１００重量％を試料とし、これに５〜３０重量
％重量％水を混合し、得られた混合物をホットプレス装
置に充填する。水は中性のものに限らず、ｐＨ４〜ｌＯ
程度の水でも構わない。A sample of 100% by weight of this powder is mixed with 5 to 30% by weight of water, and the resulting mixture is filled into a hot press device. Water is not limited to neutral water, but has a pH of 4 to 10
A small amount of water is fine.
水熱ホットプレスの適当な条件は、次の通りである。圧
力は２０〜１００ ＭＰａ程度で十分である。温度は１
２０〜４００℃程度で十分であり、４００℃より上げて
も無駄であり、好ましくは３００〜３５０℃である。昇
温速度は、１℃／分〜７０℃／分程度で十分であり、好
ましくは１’Ｃ／分〜ｌＯ℃／分である。Suitable conditions for hydrothermal hot pressing are as follows. A pressure of about 20 to 100 MPa is sufficient. temperature is 1
A temperature of about 20 to 400°C is sufficient, and it is wasteful to raise the temperature above 400°C, and the temperature is preferably 300 to 350°C. A temperature increase rate of about 1°C/min to 70°C/min is sufficient, preferably 1'C/min to 10°C/min.
時間はｌＯ分〜５時間程度十分であり、５時間より長く
実行しても無駄である。The time required is approximately 10 minutes to 5 hours, and there is no point in running the process for longer than 5 hours.
これらの条件を選択することによって、析出する結晶の
大きさと形をコントロールすることかできる。例えば、
昇温速度を遅くすると、結晶が太き（なり、針状結晶の
長さか長（なるみそうすると、固化体の機械的強度は向
上する。反対に昇温速度を速くすると、析出する結晶は
小さくなり、形状は多面体又は球状になる。By selecting these conditions, the size and shape of the precipitated crystals can be controlled. for example,
If the heating rate is slowed down, the crystals will become thicker, and the length of the needle-like crystals will be increased.This will improve the mechanical strength of the solidified product.On the other hand, if the heating rate is increased, the precipitated crystals will become smaller. , the shape becomes polyhedral or spherical.
以下、実施例により本発明をより具体的に説明するが、
本発明はこれに限られるものではない。Hereinafter, the present invention will be explained in more detail with reference to Examples.
The present invention is not limited to this.
〔実施例１３
生体活性ガラス（出発原料）として市販されている次の
組成：５ｉＯｔ ４６．１ ｍｏｌ％Ｃａ０
２６．９
Ｎａｚ ｏ’ ２４．４
Ｐ２Ｏ５２，６
を有するガラス（商品名、ニコン５Ｅ５１）を用意し、
これを７５μ（２００メツシユ）以下の粒径になるまで
粉砕した。[Example 13 The following composition commercially available as bioactive glass (starting material): 5iOt 46.1 mol% Ca0
Prepare a glass (trade name, Nikon 5E51) having 26.9 Nazo' 24.4 P2O52,6,
This was ground to a particle size of 75μ (200 mesh) or less.
得られたガラス粉体４．Ｏｇに対し２０重量％の蒸留水
を加えて十分に混合し、これを試料とし、この試料を第
１図に示す水熱ホットプレス装置に充填し、圧力＝５０
ＭＰａ、温度＝ ２００〜３５０°Ｃ１昇温速度＝２°
Ｃ／分、時間２２時間の条件で、水熱ホットプレスを行
ない、固化体を製造した。Obtained glass powder 4. Add 20% by weight of distilled water to Og, mix thoroughly, use this as a sample, fill the hydrothermal hot press device shown in Figure 1, and press at a pressure of 50.
MPa, temperature = 200-350°C1 heating rate = 2°
Hydrothermal hot pressing was performed under the conditions of C/min and 22 hours to produce a solidified product.
尚、第１図の装置は、試料ケース（３）中の試料から放
出された水を空間（４）内に保存できる構造になってい
る。The apparatus shown in FIG. 1 has a structure in which water released from the sample in the sample case (3) can be stored in the space (4).
〔比較例１〕
出発原料として、瓶ガラスなどに使用される最も汎用的
なソーダライムガラス（組成は下記の通り）を用意した
。[Comparative Example 1] As a starting material, soda lime glass (composition is as follows), which is the most commonly used glass bottle, was prepared.
５ｉｎ２７４．Ｏｍｏｌ％
Ｃａ０ １．９
Ｎａ２０ １８．５
Ｐ２０Ｓ ０．０ （セロ）
Ｂｔｕｓ １．２
Ｊ！０ １．３
Ａ１２０，３．１
ニコン５Ｅ５１の代わりにこのガラスを使用する外は実
施例１と全く同様にして、固化体を製造した。5in274. Omol% Ca0 1.9 Na20 18.5 P20S 0.0 (Cero) Btus 1.2 J! 0 1.3 A120, 3.1 A solidified body was produced in exactly the same manner as in Example 1 except that this glass was used instead of Nikon 5E51.
実施例１及び比較例】て製造した固化体について、嵩密
度（単位はｇ−ａｎ−２）の測定、析出相の同定、微構
造の観察を行なった後、マイクロビッカース硬度計によ
り硬度（単位はＧＰａ）を、万能試験機により圧縮強度
（単位はＭ Ｐａ）をそれぞれ測定した。[Example 1 and Comparative Example] After measuring the bulk density (unit: g-an-2), identifying the precipitated phase, and observing the microstructure, the hardness (unit: g-an-2) was measured using a micro-Vickers hardness meter. (GPa) and compressive strength (unit: MPa) were measured using a universal testing machine.
この結果を次の第１表に示す。The results are shown in Table 1 below.
第１表（＊温度はホットプレスの１条件）更に実施例１
の固化体について粉末Ｘ線回折法（ＸＲＤ）で分析した
ところ、固化体はガラスセラミソつてあり、Ｎａ２Ｃａ
２（Ｓｉ（Ｌ）ｓ或いはＮａＣａＪＳ＋＋Ｏ＊（ペクト
ライト）の結晶体を含むことか認められた。また、３５
０ ’Ｃてホットプレスした実施例１の固化体について
、破断面を走査型電子穎微鏡で観察したところ、釣鉤３
×３μｍの針状結晶か認められた。この針状結晶は上記
結晶体と推定される。Table 1 (*Temperature is one condition of hot press) Furthermore, Example 1
When the solidified material was analyzed by powder X-ray diffraction (XRD), it was found that the solidified material was composed of glass ceramics and contained Na2Ca.
It was recognized that it contained crystals of 2(Si(L)s or NaCaJS++O* (pectolite).
When the fracture surface of the solidified material of Example 1 hot-pressed at 0'C was observed with a scanning electronic microscope, it was found that the fishing hook 3
Needle-shaped crystals of ×3 μm were observed. This needle-like crystal is presumed to be the above-mentioned crystal.
それに対して、比較例１の固化体には、そのような結晶
体又は針状結晶は認められなかった。On the other hand, such crystals or needle-like crystals were not observed in the solidified product of Comparative Example 1.
従って、実施例１の固化体の圧縮強度か比較例１に比へ
て高いのは、上記結晶体又は針状結晶の存在によるもの
と推定される。Therefore, it is presumed that the reason why the compressive strength of the solidified material of Example 1 is higher than that of Comparative Example 1 is due to the presence of the crystals or needle-like crystals.
〔実施例２〕
次の組成 ：Ｓ！０２５２．１ ｍｏｌ％ＣａＯ２３
，８
Ｎａ２０ ２１．５
Ｐ２０ｓ ２．６
を有するガラスを用意し、以下、実施例１と同様にして
固化体を製造したところ、はぼ同等の機械的特性を有す
るガラスセラミックス固化体か得られた。[Example 2] The following composition: S! 0252.1 mol%CaO23
, 8 Na20 21.5 P20s 2.6 was prepared and a solidified body was produced in the same manner as in Example 1. A glass ceramic solidified body having almost the same mechanical properties was obtained. .
Ｕ上の通り、本発明に従って、特定の組成を有するガラ
スを試料として使用することにより、圧縮強度の高い同
化体か得られる。As mentioned above, according to the present invention, by using a glass having a specific composition as a sample, an assimilate with high compressive strength can be obtained.
また、水熱ホットプレスの条件を選択することにより、
得られる固化体の物性をコントロールすることかできる
。In addition, by selecting the hydrothermal hot press conditions,
The physical properties of the resulting solidified product can be controlled.
更に、本発明により製造された固化体は、生体活性を示
すことから、骨内インブラント材料として有用である。Furthermore, the solidified material produced according to the present invention exhibits bioactivity and is therefore useful as an intraosseous implant material.
第１図は、代表的な水熱ホットプレス装置の縦断面を示
す概念図である。
〔主要部分の符号の説明〕
１ 試料
２− ピストン
３− 試料ケース
４− 水の逃げ空間
５ ヒーター
６ 測温用熱電対孔
７− ピストン押し棒
８ グランドパソキングFIG. 1 is a conceptual diagram showing a longitudinal section of a typical hydrothermal hot press apparatus. [Explanation of symbols of main parts] 1 Sample 2 - Piston 3 - Sample case 4 - Water escape space 5 Heater 6 Temperature measurement thermocouple hole 7 - Piston push rod 8 Grand Paso King
Claims (1)
ホットプレスにより固化させる、ことを特徴とするガラ
スセラミックス固化体の製造方法。 記 ＳｉＯ＿２４０〜７２ｍｏｌ％ ＣａＯ０〜５０ Ｎａ＿２Ｏ５〜４３ Ｐ＿２Ｏ＿５１〜６[Claims] A method for producing a solidified glass-ceramic body, which comprises solidifying a mixture of glass powder and water having the following composition by hydrothermal hot pressing. SiO_240-72 mol% CaO0-50 Na_2O5-43 P_2O_51-6
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31481390A JP3170593B2 (en) | 1990-11-20 | 1990-11-20 | Method for producing solidified glass ceramics by hydrothermal hot pressing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31481390A JP3170593B2 (en) | 1990-11-20 | 1990-11-20 | Method for producing solidified glass ceramics by hydrothermal hot pressing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04187542A true JPH04187542A (en) | 1992-07-06 |
| JP3170593B2 JP3170593B2 (en) | 2001-05-28 |
Family
ID=18057911
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31481390A Expired - Fee Related JP3170593B2 (en) | 1990-11-20 | 1990-11-20 | Method for producing solidified glass ceramics by hydrothermal hot pressing |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3170593B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001233664A (en) * | 2000-02-22 | 2001-08-28 | Advance Co Ltd | Ceramic having dense texture |
| JP2014083504A (en) * | 2012-10-24 | 2014-05-12 | Ohara Inc | Photocatalyst component and method for manufacturing the same |
| CN106430985A (en) * | 2016-08-09 | 2017-02-22 | 桂林电子科技大学 | Hydrothermal preparation method for microcrystalline glass powder |
| CN111065610A (en) * | 2017-07-14 | 2020-04-24 | 欧文斯-布洛克威玻璃容器有限公司 | Soda-lime-silica glass ceramic |
| JP2020142200A (en) * | 2019-03-07 | 2020-09-10 | 三菱マテリアル株式会社 | Waste glass treatment method and treatment apparatus |
| JP2021509312A (en) * | 2017-12-20 | 2021-03-25 | プガチ， アンドレイＰＵＧＡＣＨ， Ａｎｄｒｅｙ | Bone implant |
-
1990
- 1990-11-20 JP JP31481390A patent/JP3170593B2/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001233664A (en) * | 2000-02-22 | 2001-08-28 | Advance Co Ltd | Ceramic having dense texture |
| JP2014083504A (en) * | 2012-10-24 | 2014-05-12 | Ohara Inc | Photocatalyst component and method for manufacturing the same |
| CN106430985A (en) * | 2016-08-09 | 2017-02-22 | 桂林电子科技大学 | Hydrothermal preparation method for microcrystalline glass powder |
| CN106430985B (en) * | 2016-08-09 | 2019-01-18 | 桂林电子科技大学 | A kind of hydrothermal preparing process of microcrystalline glass powder |
| CN111065610A (en) * | 2017-07-14 | 2020-04-24 | 欧文斯-布洛克威玻璃容器有限公司 | Soda-lime-silica glass ceramic |
| CN111065610B (en) * | 2017-07-14 | 2022-07-05 | 欧文斯-布洛克威玻璃容器有限公司 | Soda-lime-silica glass ceramic |
| JP2021509312A (en) * | 2017-12-20 | 2021-03-25 | プガチ， アンドレイＰＵＧＡＣＨ， Ａｎｄｒｅｙ | Bone implant |
| JP2020142200A (en) * | 2019-03-07 | 2020-09-10 | 三菱マテリアル株式会社 | Waste glass treatment method and treatment apparatus |
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| JP3170593B2 (en) | 2001-05-28 |
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