JPH0761880B2 - Mold for molding calcium phosphate-based crystallized glass - Google Patents
Mold for molding calcium phosphate-based crystallized glassInfo
- Publication number
- JPH0761880B2 JPH0761880B2 JP12726786A JP12726786A JPH0761880B2 JP H0761880 B2 JPH0761880 B2 JP H0761880B2 JP 12726786 A JP12726786 A JP 12726786A JP 12726786 A JP12726786 A JP 12726786A JP H0761880 B2 JPH0761880 B2 JP H0761880B2
- Authority
- JP
- Japan
- Prior art keywords
- mold
- molding
- calcium phosphate
- crystallized glass
- glass
- 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.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Dental Prosthetics (AREA)
- Glass Compositions (AREA)
Description
【発明の詳細な説明】 (産業上の利用分野) 本発明はリン酸カルシウム系結晶化ガラスの成形用型、
特にリン酸カルシウム系結晶化ガラスの表面や内部に泡
を生ぜしめないことの出来る成形用型に係るものであ
る。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a mold for molding calcium phosphate-based crystallized glass,
In particular, the present invention relates to a molding die capable of preventing bubbles from being generated on the surface or inside of the calcium phosphate crystallized glass.
(従来の技術) リン酸カルシウム系結晶化ガラスは生体との親和性がよ
く、天然歯に近い物性を有しており、又リン酸カルシウ
ム系ガラスを溶融して型を用いて鋳造した後、結晶化を
行なう方法により金属と同の成形が可能であることから
歯科用材料としての応用が提案されている。(Prior Art) Calcium phosphate-based crystallized glass has good affinity with living organisms and has physical properties similar to those of natural teeth. Also, calcium phosphate-based glass is melted and cast using a mold, and then crystallized. Since it can be formed in the same manner as metal by the method, its application as a dental material has been proposed.
処で、一般に歯科用金属の鋳造用型としては、鋳造成形
部に至る湯道は成形部に溶融金属(湯)が入りさえすれ
ばよい為、特に形状を考慮する必要もなく、通常単に円
筒状の空隙として設けられていた。In general, as a casting mold for dental metal, since the molten metal (hot water) needs only to enter the casting part of the casting metal part, it is not necessary to consider the shape, and it is usually just a cylinder. It was provided as a void.
しかしながら、この様な鋳造型をリン酸カルシウム系ガ
ラスに用いる場合には、その後の結晶化処理に際し、成
形物表面や内部に一部泡の生成が見られ、その為形状が
損われたり破折する等の欠点がある。However, when such a casting mold is used for calcium phosphate-based glass, during the subsequent crystallization treatment, some bubbles are observed on the surface and inside of the molded product, which causes the shape to be damaged or broken. There is a drawback of.
本発明者はかかる欠点を排除し、泡の発生しないリン酸
カルシウム系結晶化ガラスを得るべく種々研究、検討し
た結果、結晶化ガラスの結晶化は表面から起り、内側に
向つてかなり均一な速度で進行するが、結晶化ガラスは
通常のガラスより高密度の為、結晶化が最後に起る部分
に結晶化による収縮分だけ空隙が生じ、これが泡となつ
て残ることが知見された。The present inventor eliminates such drawbacks, and as a result of various studies and studies to obtain a calcium phosphate-based crystallized glass that does not generate bubbles, as a result, crystallization of the crystallized glass occurs from the surface and proceeds toward the inside at a fairly uniform speed. However, since crystallized glass has a higher density than ordinary glass, it has been found that voids are generated in the portion where crystallization last occurs due to shrinkage due to crystallization, and these remain as bubbles.
そしてかかる知見に基づき、空洞を成形体以外の部分に
生ぜしめる手段として既に鋳造法によりリン酸カルシウ
ム系結晶化ガラス成形体を得る際、鋳型のスプルー線
(湯道)の径をガラス成形体の肉厚より大きくしてここ
に最後の結晶化を起させることを特開昭61-71044号とし
て提案した。Based on this knowledge, when a calcium phosphate-based crystallized glass molded body is already obtained by the casting method as a means of creating a cavity in a portion other than the molded body, the diameter of the sprue wire (runner) of the mold is set to the thickness of the glass molded body. It was proposed in JP-A-61-71044 to make it larger to cause the final crystallization.
(発明の解決しようとする問題点) 上記提案の方法は、確かに有効な手段であり、通常のこ
の種結晶化ガラスの製法として問題はない。(Problems to be Solved by the Invention) The method proposed above is certainly an effective means, and there is no problem as an ordinary method for producing this seed crystallized glass.
しかしながら、リン酸カルシウム系結晶化ガラスの場合
には、主要な結晶相はメタリン酸カルシウム結晶であ
り、その結晶形態としてβ晶とδ晶があり、通常はこれ
らが共存した形で結晶化が行なわれる。However, in the case of calcium phosphate-based crystallized glass, the main crystal phase is calcium metaphosphate crystal, and the crystal forms thereof are β crystal and δ crystal, and crystallization is usually performed in the coexistence of these.
又、かかる結晶化ガラスの場合、耐水性及び透明観のあ
るガラスを得るには、より多くβ晶にすることが望まし
い。そしてこれを達成せしめる手段としてガラスと接す
る鋳型表面にメタリン酸カルシウムの微細結晶を存在せ
しめることが有効であり、これと共に前記提案の鋳型の
湯道の径をガラス成形体の肉厚より大にすることを併用
した処、意外にも成形体に空洞が生じる場合があり、単
にスプルー線径を大にするだけでは、空洞防止の効果が
十分でないことを知見した。Further, in the case of such crystallized glass, it is desirable to make more β crystal in order to obtain glass having water resistance and a transparent appearance. And it is effective to allow the presence of fine crystals of calcium metaphosphate on the surface of the mold in contact with the glass as a means for achieving this, and to make the diameter of the runner of the proposed mold larger than the wall thickness of the glass molding together with this. It was found that, when used in combination, a cavity may unexpectedly occur in the molded body, and merely increasing the sprue wire diameter is not sufficient to prevent the cavity.
(問題点を解決するための手段) 本発明はかかる知見に基づきなされたもので、鋳型の湯
道の特定箇所に湯溜りを設けることにより、メタリン酸
カルシウムを表面に有する鋳型を用いても成形体中に空
洞を生ぜしめないことが見出された。(Means for Solving Problems) The present invention has been made based on such findings, and by forming a basin at a specific location of the runner of the mold, a molded product can be obtained even if a mold having calcium metaphosphate on its surface is used. It was found that it did not create a cavity in it.
かくして本発明は、リン酸カルシウム系の溶融ガラスを
鋳造成形し、かつ脱型前に結晶化させてリン酸カルシウ
ム系結晶化ガラス歯冠材料を得るための型の形状におい
て、型の鋳造成形部に至る湯道の該成形部より20mm以内
の位置に内径5mm以上の球状の湯溜りを設けたことを特
徴とするリン酸カルシウム系結晶化ガラスの成形用型を
提供するにある。Thus, the present invention is a mold for casting and molding a calcium phosphate-based molten glass and crystallizing it before demolding to obtain a calcium phosphate-based crystallized glass dental crown material, and a runner leading to a cast molding part of the mold. Another object of the present invention is to provide a mold for molding calcium phosphate-based crystallized glass, characterized in that a spherical pool having an inner diameter of 5 mm or more is provided within 20 mm from the molding part.
以下本発明を添付図面により具体的に説明する。The present invention will be specifically described below with reference to the accompanying drawings.
第1図は本発明の一例によるリン酸カルシウム系結晶化
ガラスの成形用型の基本的構成を説明する断面図であ
る。第1図において1は歯等の鋳造成形物を成形する成
形部であり、2及び3はリン酸カルシウム系ガラス溶融
物(湯)が成形部1に鋳込まれる湯道である。4は湯道
2及び3の間に設けられた湯溜りであり、該湯溜りは成
形部1の下部、即ちこれと湯道2の接点から測定して下
方に向けて20mm以内に湯溜りの頂部が来る様に、即ち第
1図中aで示された部分が最大20mmとなる様に設けられ
る。FIG. 1 is a sectional view for explaining the basic structure of a mold for molding calcium phosphate-based crystallized glass according to an example of the present invention. In FIG. 1, 1 is a forming part for forming a cast formed product such as a tooth, and 2 and 3 are runners into which a calcium phosphate-based glass melt (melt) is cast into the forming part 1. Reference numeral 4 denotes a basin provided between the runners 2 and 3, and the basin of the basin is measured at a lower portion of the forming part 1, that is, a contact point between the runner 2 and the basin 2 and is directed downward within 20 mm. It is provided so that the top comes, that is, the portion indicated by a in FIG. 1 has a maximum of 20 mm.
aで示される部分は、最大20mmであり、好ましくは10mm
以下、特に5mm以下であり、成形部1の下部に面接設け
ることも出来る。The part indicated by a has a maximum of 20 mm, preferably 10 mm
Hereafter, it is especially 5 mm or less, and it is also possible to provide a face-to-face contact with the lower part of the molding part 1.
湯溜りを設ける位置が20mmを超える場合には、成形物中
に空洞が生ずるのが避けられず、不適当である。湯溜り
は、内径5mm以上の球状であることが必要である。湯溜
りの体積は、成形体の体積の10倍未満が好ましい。If the position where the basin is provided exceeds 20 mm, it is unavoidable that cavities occur in the molded product, which is unsuitable. The basin should be spherical with an inner diameter of 5 mm or more. The volume of the basin is preferably less than 10 times the volume of the molded body.
湯道3、注湯口5の形状は、溶融ガラスが成形部1中に
流入し成形が出来れば特に制限はないが、溶融ガラスの
流入を容易にする為その内径は0.5mm以上、好ましくは1
mm以上が適当である。The shapes of the runner 3 and the pouring port 5 are not particularly limited as long as the molten glass can flow into the molding portion 1 and molding can be performed, but in order to facilitate the inflow of the molten glass, the inner diameter thereof is 0.5 mm or more, preferably 1
mm or more is suitable.
一方、湯道2は成形部1の最大肉厚部と直結しているの
が好ましく、湯道2の内径は成形部1の最大肉厚部の肉
厚と少なくとも同じか大であることが好ましく、かくす
ることにより成形体中への空洞の発生を十分抑制するこ
とが可能となる。成形体が歯冠材料である場合、湯道2
の内径は2mm以上、好ましくは3mm以上が適当である。On the other hand, it is preferable that the runner 2 is directly connected to the maximum thickness part of the forming part 1, and the inner diameter of the runner 2 is preferably at least the same as or larger than the maximum thickness part of the forming part 1. By doing so, it becomes possible to sufficiently suppress the generation of voids in the molded body. If the compact is a crown material, runner 2
The inner diameter of is 2 mm or more, preferably 3 mm or more.
この様な鋳造を構成する材料として例えばリン酸塩系埋
没材、エチルシリケート系埋没材、石膏系埋没材等を適
宜採用出来、特に成形部1の表面は、窒化ホウ素とメタ
リン酸カルシウムの微細結晶(通常100μ以下)が存在
していることが好ましく、かくすることにより成形体の
結晶化、特にβ晶の成長が顕著であり、又型離れを容易
にすることが可能となる。As a material constituting such casting, for example, a phosphate-based investment material, an ethylsilicate-based investment material, a gypsum-based investment material, or the like can be appropriately adopted, and in particular, the surface of the molding part 1 has fine crystals of boron nitride and calcium metaphosphate ( (Usually 100 μm or less) is preferable. By doing so, crystallization of the molded body, particularly growth of β crystal, is remarkable, and mold release can be facilitated.
窒化ホウ素は型の表面から10μ〜1mm程度迄に1〜80重
量%が、又メタリン酸カルシウムの微細結晶は、やはり
型の表面から10μ〜1mm程度迄に1〜50重量%程度存在
せしめておくのが効果的である。Boron nitride should be present in an amount of 1 to 80% by weight from the surface of the mold to approximately 10 μ to 1 mm, and fine crystals of calcium metaphosphate should be present in an amount of approximately 1 to 50% by weight by approximately 10 μ to 1 mm from the surface of the mold. Is effective.
鋳型は通常ロストワツクス法の様な埋没系であるが、割
り型等他の形式の型であつても差し支えない。The mold is usually a buried system such as the Lost Wax method, but other types such as a split mold may be used.
本発明に用いられるリン酸カルシウム系ガラスとして
は、主要な析出結晶相としてメタリン酸カルシウム結晶
が析出するものが好ましい。例えば、リンに対するカル
シウムの原子比Ca/Pが0.35〜0.7のリン酸カルシウム質
を80重量%以上含有するものが好ましい。The calcium phosphate-based glass used in the present invention is preferably one in which calcium metaphosphate crystals are precipitated as a main precipitation crystal phase. For example, those containing 80% by weight or more of calcium phosphate having an atomic ratio Ca / P of calcium to phosphorus of 0.35 to 0.7 are preferable.
本発明において実際リン酸カルシウム系結晶化ガラスを
鋳造するには、例えば1000℃以上で溶融したガラスを鋳
型中に遠心力や雰囲気の圧力差等を利用して鋳込み、所
定の形状に成形後、鋳型中で冷却し、次いで700℃に4
時間保持することにより結晶化を行ない、その後脱型す
る手段が採用される。In the present invention, in order to cast a calcium phosphate-based crystallized glass, for example, glass melted at 1000 ° C. or higher is cast into a mold by utilizing centrifugal force or a pressure difference of atmosphere, and after molding into a predetermined shape, in a mold. And then to 700 ° C 4
A method is employed in which crystallization is carried out by holding for a period of time, and then demolding is performed.
本発明による成形型は、成形部表面に結晶化を制御促進
する為にメタリン酸カルシウムの結晶を存在せしめたと
きに有効なものであるが、この様な制御促進剤の存在し
ない型に対しても成形体中に空洞を生ぜしめない効果を
有していることは言う迄もない。The mold according to the present invention is effective when calcium metaphosphate crystals are allowed to exist on the surface of the molded part to control and promote crystallization, but it is also effective for molds in which such a control accelerator does not exist. It goes without saying that it has the effect of not causing voids in the molded body.
(実施例) 実施例1 第1図に示した形状の鋳型を次の様にして作成した。(Example) Example 1 A mold having the shape shown in FIG. 1 was prepared as follows.
外径30mm、高さ10mmの円錐形のゴム製台上に、直径2mm
のワツクス棒(而至歯科工業社製レデイ−キヤステイン
グワツクス)を5mmの長さに切つたもの3を立て、その
上部に直径8mmの球形に成形したワツクス球4(而至歯
科工業社製レデイ−キヤステイングワツクス)をつけ、
更にその上部に直径3mmのワツクス棒2(同上社製同ワ
ツクス)を5mmの長さに切つて立て、その上部に最大肉
厚1.8mmの歯冠形状のワツクスパターンをその最大肉厚
部で取り付けた。そしてその周囲に内径30mm、高さ50mm
のステンレス製リングを配置した。一方、窒化ホウ素粉
末30重量%、平均粒径5μのメタリン酸カルシウム結晶
20重量%、残部がリン酸塩系埋没材(徳山曹達社製ブル
ーベスト)を十分混合し、常法に従つてスラリー状とし
て前記リング内に流入し、硬化する迄放置した。2 mm diameter on a conical rubber stand with an outer diameter of 30 mm and a height of 10 mm
Wax stick (Lady-Casting Wax manufactured by Meta Dental Industry Co., Ltd.) cut into a length of 5 mm, 3 is set up, and a wax ball 4 formed in a spherical shape with a diameter of 8 mm on the upper side (manufactured by Meta Dental Industry Co., Ltd.) Ready-casting wax)
In addition, a wax rod 2 with a diameter of 3 mm (same wax produced by Dojo Co., Ltd.) is cut up to a length of 5 mm on the upper portion thereof, and a crown-shaped wax pattern with a maximum wall thickness of 1.8 mm is formed on the upper portion thereof at the maximum wall portion. I installed it. And around it, the inner diameter is 30 mm and the height is 50 mm.
A stainless steel ring was placed. On the other hand, 30% by weight boron nitride powder, calcium metaphosphate crystals with an average particle size of 5μ
20% by weight, and the balance was a phosphate-based investment material (Blue vest manufactured by Tokuyama Soda Co., Ltd.) was sufficiently mixed, and it was made to flow into the ring in the form of slurry according to a conventional method, and was left until it was cured.
その後ゴム製台を取り除き、800℃で30分間加熱してワ
ツクスを焼却して鋳型を得た。After that, the rubber base was removed, and the wax was incinerated by heating at 800 ° C. for 30 minutes to obtain a mold.
次にCaO 24.5重量%、P2O5 74.5重量%、Al2O
3 1.0重量%の組成物を1250℃で溶融してリン酸カル
シウム系ガラスを得、該ガラスを前記鋳型に常法に従つ
て遠心鋳造せしめた。次いで鋳型ごと700℃に2時間保
持せしめて鋳型中のガラスを結晶化せしめた。Next, CaO 24.5% by weight, P 2 O 5 74.5% by weight, Al 2 O
3 1.0% by weight of the composition was melted at 1250 ° C. to obtain a calcium phosphate glass, and the glass was centrifugally cast into the mold according to a conventional method. Then, the mold was kept at 700 ° C. for 2 hours to crystallize the glass in the mold.
常温迄冷却後、鋳型をこわして結晶化ガラスを取り出
し、歯冠成形物を湯道との界面で切断した。After cooling to room temperature, the mold was broken and the crystallized glass was taken out, and the crown molding was cut at the interface with the runner.
同様にして計10個の歯冠を作成し、夫々X線探傷法によ
り検査を行なつた処、何れにも全く空洞は存在しなかつ
た。In the same manner, a total of 10 crowns were created and inspected by the X-ray flaw detection method, respectively, and no cavity was found in any of them.
尚、湯溜り部を同様に観察した処、そこの結晶化ガラス
に大小の空洞が認められた。When the pool of water was observed in the same manner, large and small cavities were observed in the crystallized glass.
比較例1 実施例1と同様な円錐形のゴム製台上に直径3mmのワツ
クス棒を10mmの長さに切つたものを立て、その上部に実
施例1と同様な歯冠形状をしたワツクスパターンを取り
付けた。以下実施例1と同様に埋没、鋳造、結晶化を行
ない、計10個の結晶化ガラス歯冠を得、夫々X線探傷法
により検査を行なつた。その結果、2個は表面迄貫通し
ている空洞が存在し、残りは0.3〜1.8mmの空洞が存在し
ていた。Comparative Example 1 A wax stick having a diameter of 3 mm cut into a length of 10 mm was erected on a conical rubber stand similar to that of Example 1, and a crown having the same crown shape as that of Example 1 was placed above the wax stick. Attached the pattern. Thereafter, burying, casting and crystallization were performed in the same manner as in Example 1 to obtain a total of 10 crystallized glass crowns, which were inspected by the X-ray flaw detection method. As a result, two had cavities that penetrated to the surface and the rest had cavities of 0.3 to 1.8 mm.
実施例2〜6及び比較例2〜6 厚さ1.5mm、直径15mmの円板形状(体積265mm3)をした
結晶化ガラス成形体を得る為に同形状のワツクス板を作
成し、これを第2図及び表1に夫々示した形状の湯道の
上部に角度が30度となるように取り付け、夫々につき実
施例1と同様に埋没、鋳造、結晶化を行ない、結晶化ガ
ラス板を夫々について10枚づつ得た。Examples 2 to 6 and Comparative Examples 2 to 6 In order to obtain a crystallized glass molded body having a disk shape (volume 265 mm 3 ) having a thickness of 1.5 mm and a diameter of 15 mm, a wax plate having the same shape was prepared, As shown in Fig. 2 and Table 1, the runners each having the shape shown in Fig. 2 were attached so that the angle was 30 degrees, and each of them was buried, cast, and crystallized in the same manner as in Example 1, and the crystallized glass plate was attached to each of them. I got 10 each.
実施例1と同様に検査を行なつた結果を表1に示した。Table 1 shows the result of the inspection conducted in the same manner as in Example 1.
第1図は本発明の一例によるリン酸カルシウム系結晶化
ガラスの成形用型の基本的構成を説明する為の断面図、 第2図は本発明の実施例及び比較例を示す為のリン酸カ
ルシウム系結晶化ガラスの成形用型を説明する為の断面
図である。 1,21:成形部、2,3,22,24:湯道、4,23:湯溜り FIG. 1 is a cross-sectional view for explaining the basic structure of a mold for molding calcium phosphate-based crystallized glass according to an example of the present invention, and FIG. 2 is a calcium phosphate-based crystallization for showing examples and comparative examples of the present invention. It is sectional drawing for demonstrating the shaping | molding die of glass. 1,21: forming part, 2,3,22,24: runner, 4,23: hot water pool
Claims (3)
形し、かつ脱型前に結晶化させてリン酸カルシウム系結
晶化ガラス歯冠材料を得るための型の形状において、型
の鋳造成形部に至る湯道の該成形部より20mm以内の位置
に内径5mm以上の球状の湯溜りを設けたことを特徴とす
るリン酸カルシウム系結晶化ガラスの成形用型。1. In a mold shape for obtaining a calcium phosphate crystallized glass crown material by casting and molding calcium phosphate-based molten glass and crystallizing it before demolding, a runner leading to a casting molding part of the mold. 1. A mold for molding calcium phosphate-based crystallized glass, characterized in that a spherical basin having an inner diameter of 5 mm or more is provided at a position within 20 mm from the molding part.
が15mm以下である特許請求の範囲第1項に記載の成形用
型。2. The molding die according to claim 1, wherein the length of the runner connecting the casting molding portion of the mold and the molten metal pool is 15 mm or less.
ルシウムの結晶を有している特許請求の範囲第1項に記
載の成形用型。3. The molding die according to claim 1, wherein the cast molding portion of the mold has crystals of calcium metaphosphate on its surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12726786A JPH0761880B2 (en) | 1986-06-03 | 1986-06-03 | Mold for molding calcium phosphate-based crystallized glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12726786A JPH0761880B2 (en) | 1986-06-03 | 1986-06-03 | Mold for molding calcium phosphate-based crystallized glass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62288121A JPS62288121A (en) | 1987-12-15 |
| JPH0761880B2 true JPH0761880B2 (en) | 1995-07-05 |
Family
ID=14955784
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12726786A Expired - Fee Related JPH0761880B2 (en) | 1986-06-03 | 1986-06-03 | Mold for molding calcium phosphate-based crystallized glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0761880B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0613221Y2 (en) * | 1988-07-30 | 1994-04-06 | 九州耐火煉瓦株式会社 | Sprue structure for lost wax casting |
| AU2017212882B2 (en) * | 2016-01-26 | 2019-05-16 | Gc Corporation | Dental investment material |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60158856A (en) * | 1984-01-28 | 1985-08-20 | 九州耐火煉瓦株式会社 | Sprueing method of ceramics casting dental repairing material |
| JPS6171044A (en) * | 1984-09-14 | 1986-04-11 | 旭硝子株式会社 | Production of calcium phosphate type crystallized glass dental molded body |
-
1986
- 1986-06-03 JP JP12726786A patent/JPH0761880B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62288121A (en) | 1987-12-15 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |