JPH0448007A - Improved lubricity sheet - Google Patents
Improved lubricity sheetInfo
- Publication number
- JPH0448007A JPH0448007A JP2159243A JP15924390A JPH0448007A JP H0448007 A JPH0448007 A JP H0448007A JP 2159243 A JP2159243 A JP 2159243A JP 15924390 A JP15924390 A JP 15924390A JP H0448007 A JPH0448007 A JP H0448007A
- Authority
- JP
- Japan
- Prior art keywords
- ceramic powder
- sintering
- powder
- improving sheet
- spherical
- 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
- 239000000843 powder Substances 0.000 claims abstract description 54
- 239000000919 ceramic Substances 0.000 claims abstract description 40
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000011148 porous material Substances 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052799 carbon Inorganic materials 0.000 abstract description 13
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract 7
- 239000000956 alloy Substances 0.000 abstract 4
- 229910045601 alloy Inorganic materials 0.000 abstract 4
- 230000016615 flocculation Effects 0.000 abstract 1
- 238000005189 flocculation Methods 0.000 abstract 1
- 238000010304 firing Methods 0.000 description 14
- 238000010586 diagram Methods 0.000 description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920000609 methyl cellulose Polymers 0.000 description 3
- 239000001923 methylcellulose Substances 0.000 description 3
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 238000005255 carburizing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Furnace Charging Or Discharging (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は超硬合金のような被焼成物を真空中又は非酸化
性雰囲気中で焼成する際に被焼成物とセッター間の融着
を防止するために使用される焼成時の滑性向上シートに
関するものである。Detailed Description of the Invention (Industrial Field of Application) The present invention is a method for preventing fusion between the object to be fired and a setter when firing the object, such as cemented carbide, in a vacuum or in a non-oxidizing atmosphere. The present invention relates to a sheet for improving lubricity during firing, which is used to prevent
（従来の技術）
ＷＣ，ＴｉＣ、ＴａＣ、ＮｂＣ等の超硬合金は１０−”
Ｔｏｒｒ程度の真空中あるいは還元性雰囲気中で１３０
０〜１５００°Ｃという高温度で焼成されるものであり
、焼成する際にはセッター本体としてカーボン板を用い
ている。そして、そのカーボンと超硬合金との反応を防
止し、かつ超硬合金とカーボン板との融着を防止するた
めには従来よりカーボン板の表面にＡｌｚＯｓ 、ＡＩ
Ｎなどのセラミック粉末を敷粉として散布、あるいは接
着したり、これらのセラミ・２り粉末を含有させた焼成
用シートを被覆したりする滑性向上の手段を施している
。(Prior art) Cemented carbide such as WC, TiC, TaC, NbC etc. is 10-"
130 in a vacuum or reducing atmosphere of about Torr
It is fired at a high temperature of 0 to 1500°C, and a carbon plate is used as the setter body during firing. In order to prevent the reaction between the carbon and the cemented carbide, and also to prevent the cemented carbide from adhering to the carbon plate, AlzOs, AI, etc. have been conventionally applied to the surface of the carbon plate.
Measures are taken to improve slipperiness, such as scattering or adhering ceramic powder such as N as a bedding powder, or coating a sheet for firing containing these ceramic powders.
（発明が解決しようとするｉ１題）
ところで、被焼成物は焼成によって収縮し、その寸法の
変化は被焼成物が大きい場合に著しい。(I1 Problem to be Solved by the Invention) By the way, the object to be fired shrinks during firing, and the change in size is significant when the object to be fired is large.
また、超硬合金は高温状態において液相状態となるカー
ボン板との接触を避け、スムーズに収縮を進行させる必
要がある。そこでカーボン板上に施す敷粉やシートが、
被焼成物の大きい場合に特に起こりやすい焼成物の反り
や浸炭を防ぐ上で重要な役割を果たすことになる。また
、被焼成物の重量が大きくても被焼成物とカーボン板と
が接触しやすくなるので、敷粉やシートの役割は大きい
といえる。Further, it is necessary for the cemented carbide to shrink smoothly by avoiding contact with the carbon plate, which is in a liquid state at high temperatures. Therefore, the bedding powder and sheet applied on the carbon board,
This plays an important role in preventing warpage and carburization of the fired product, which is particularly likely to occur when the fired product is large. Furthermore, even if the weight of the object to be fired is large, the object to be fired and the carbon plate can easily come into contact with each other, so it can be said that the bed powder or sheet plays a large role.
ところが、人手によって敷粉を散布する方法ではむらが
多く、被焼結体に反りが発生したり、カーボン板と接触
することにより浸炭現象を生じたりして焼結体、即ち超
硬合金の品質低下を招くという問題点があった。また、
焼成時には被焼成体の収縮と連動して敷粉が中央へ移動
しやすく、さらに敷粉のない部分もできやすいので、ま
すます敷粉にむらが生じて超硬合金製造の歩留りが低下
する結果になっていた。However, the method of manually scattering bedding powder is uneven, causing warping of the sintered object, and carburization due to contact with the carbon plate, which deteriorates the quality of the sintered object, that is, the cemented carbide. There was a problem in that it caused a decline. Also,
During firing, the lining powder tends to move to the center as the object to be fired contracts, and there are also areas where there is no lining powder, which makes the lining powder even more uneven and reduces the yield of cemented carbide manufacturing. It had become.
一方、従来の焼成用シートを用いた場合や、敷粉を用い
た場合にはころがり作用がないので、スムーズな収縮が
行えないことがあり、焼結体（超硬合金）に反りが生じ
る可能性があることが問題であった。On the other hand, when conventional firing sheets or bedding powder are used, there is no rolling action, so smooth contraction may not be possible, and the sintered body (cemented carbide) may warp. The problem was gender.
（課題を解決するための手段）
そこで、本発明は上記の点に鑑み、カーボン板上の敷粉
の凝集を防止し、平滑で常に均一な滑性向上シートを提
供することを目的としてなされたもので、不定形状のセ
ラミック粉末と、前記不定形状のセラミック粉末の粒径
と同等あるいはそれ以下の粒径の球状のセラミック粉末
とを有機バインダーで結着したことを特徴とするもので
ある。(Means for Solving the Problems) Therefore, in view of the above points, the present invention was made with the object of preventing the agglomeration of bedding powder on a carbon plate and providing a smooth and always uniform lubricity-improving sheet. It is characterized in that an irregularly shaped ceramic powder and a spherical ceramic powder having a particle size equal to or smaller than that of the irregularly shaped ceramic powder are bound together with an organic binder.
本発明において、有機バインダーとしてはポリビニルア
ルコール（ＰＶＡ）、カルボキシメチルセルロース（Ｃ
ＭＣ） 、メチルセルロース（ＭＣ）などの水溶性樹脂
やポリビニルブチラール、スチレン樹脂、エポキシ樹脂
などの有機溶剤易溶性樹脂、その他、アクリル樹脂や酢
酸ビニル、ブタジェン系樹脂を使用することができる。In the present invention, the organic binder is polyvinyl alcohol (PVA), carboxymethyl cellulose (C
MC), water-soluble resins such as methylcellulose (MC), resins easily soluble in organic solvents such as polyvinyl butyral, styrene resins, and epoxy resins, as well as acrylic resins, vinyl acetate, and butadiene-based resins.
また、セラミック粉末の成分としては＾ｌ、０１、ＡＩ
Ｎ 、 ＣＳＢＮ、 ３Ａ１ｇＯｓ・’１ｓｉｏ！など
が良い。In addition, the components of the ceramic powder are ^l, 01, AI
N, CSBN, 3A1gOs・'1sio! etc. are good.
なお、本発明における不定形状の粉末とは角状、リン片
状、塊状、柱状などの粉末で、適宜それらの形状を混合
して用いてもよいし、同一形状の粉末を用いてもよい。Incidentally, the irregularly shaped powder in the present invention refers to powder having an angular shape, flaky shape, block shape, columnar shape, etc., and these shapes may be appropriately mixed and used, or powders having the same shape may be used.
（実施例） 次に、本発明の実施例を第１図を用いて説明する。(Example) Next, an embodiment of the present invention will be described using FIG.
第１図は本発明の滑性向上シートの模式図で図中の符号
（５）で示される有機バインダーに不定形状（たとえば
塊状）のセラミック粉末（２）と球状のセラミック粉末
（３）とが混合分散されている。球状のセラミック粉末
（３）の粒径は不定形状のセラミック粉末（２）と同等
の粒径あるいはそれ以下が好ましい、この実施例では有
機バインダーであるポリビニルアルコール（ＰＶＡ）を
３０重量％、不定形状（塊状）のアルミナ粉末（１５０
メツシユ、１０５〜４４μｍ）を５０重量％、球状のア
ルミナ粉末（３０μｍ）を１８重量％、さらに可塑剤と
してのポリエチレングリコール２重量％を使用して形成
されている。FIG. 1 is a schematic diagram of the lubricity-improving sheet of the present invention, in which an irregularly shaped (for example, lumpy) ceramic powder (2) and a spherical ceramic powder (3) are added to an organic binder indicated by the reference numeral (5) in the figure. Mixed and dispersed. The particle size of the spherical ceramic powder (3) is preferably equal to or smaller than that of the irregularly shaped ceramic powder (2). In this example, 30% by weight of polyvinyl alcohol (PVA) as an organic binder and irregularly shaped (lump) alumina powder (150
It is formed using 50% by weight of mesh (105 to 44 μm), 18% by weight of spherical alumina powder (30 μm), and 2% by weight of polyethylene glycol as a plasticizer.
なお、図中の符号（１）は気泡、符号（４）は気孔で、
有機バインダー（５）の成分が熱分解して生じた部分で
ある。そして、この滑性向上シートの通気度（ＪＩＳ
Ｐ８１１７に準ず）は平均値１．２ｓｅｃ／１００ｃｃ
、 Ｍａｙ＝ １．８６ｓｅｃ／１００ ｃｃ 、旧
ｎ ＝０．４０ｓｅｃ／’１００ ｃｃ、 Ｒ＝１．４
６ｓｅｃ／１００ ｃｃであった。In addition, the symbol (1) in the figure is a bubble, and the symbol (4) is a pore.
This is a portion generated by thermal decomposition of the components of the organic binder (5). The air permeability (JIS
(according to P8117) has an average value of 1.2sec/100cc
, May=1.86sec/100 cc, old n=0.40sec/'100 cc, R=1.4
It was 6 sec/100 cc.
（作用及び効果）
〔評価試験〕
このように構成された滑性向上シートを用いて超硬合金
（焼成品の大きさφ３２０×φ１００ Ｘ １ｏｔ、重
量１０．９ｋｇ）の焼成を真空中で行い、浸炭、反りの
発生状況を調査し、評価した。なお、比較例として不定
形状のアルミナわ）末のみを散在させた焼成シートを用
いて同様の超硬合金の焼成を行った。サンプルはそれぞ
れ１０枚ずつである。下表にその結果を示す。(Functions and Effects) [Evaluation Test] A cemented carbide (fired product size: φ320 x φ100 x 1 ot, weight 10.9 kg) was fired in a vacuum using the lubricity-improving sheet configured as described above. The occurrence of carburization and warping was investigated and evaluated. As a comparative example, a similar cemented carbide was fired using a fired sheet in which only irregularly shaped alumina powder was scattered. There are 10 samples each. The results are shown in the table below.
Ｎ＝ＩＯ枚
以上の評価試験からも明らかなように本発明の滑性向上
シートを超硬合金の焼成に用いれば浸炭や反りの発生が
低く抑えられ、優れた品質の超硬合金を効率良く得るこ
とができる。As is clear from the evaluation test of N=IO sheets or more, if the lubricity-improving sheet of the present invention is used for firing cemented carbide, carburization and warpage can be suppressed to a low level, and excellent quality cemented carbide can be efficiently produced. Obtainable.
次に本発明の滑性向上シートの超硬合金焼成時の内部状
態を図を用いて考察、説明する。Next, the internal state of the lubricity-improving sheet of the present invention during firing of the cemented carbide will be discussed and explained using figures.
まず、第２図は焼成時の状態図で第１図と同一部材は同
一符号で示されている０図中の符号（６）は被焼成体の
超硬合金、符号（７）はカーボン板であり、焼成時には
超硬合金（６）は図の右方向に向かって収縮している。First of all, Fig. 2 is a state diagram during firing, and the same parts as in Fig. 1 are indicated by the same symbols. In Fig. 0, the code (6) is the cemented carbide of the object to be fired, and the code (7) is the carbon plate. During firing, the cemented carbide (6) contracts toward the right in the figure.
この場合、滑性向上シート中の不定形状のセラミック粉
末（２〕は球状のセラミック粉末（３）が滑らかなため
、バインダー（５）の熱分解後の空隙を比較的自由に転
がることができる。すなわち、本発明のセラミック粉末
は超硬合金（６）の収縮に伴って動くころの役割を果た
すことが示唆される。これに対し、不定形状のセラミン
ク粉末のみを散在させた焼成シートでは球状物による滑
面がないため、自由にセラミック粉末が転がることがで
きず、ころ作用が不充分であり、超硬合金に浸炭や反り
などの発生頻度が高くなるのであろう。In this case, since the spherical ceramic powder (3) is smooth, the irregularly shaped ceramic powder (2) in the lubricity-improving sheet can roll relatively freely in the voids after the binder (5) is thermally decomposed. In other words, it is suggested that the ceramic powder of the present invention plays the role of a roller that moves with the contraction of the cemented carbide (6).On the other hand, in a fired sheet in which only irregularly shaped ceramic powder is scattered, spherical particles Since there is no smooth surface, the ceramic powder cannot roll freely, and the roller action is insufficient, which probably increases the frequency of carburization and warping of the cemented carbide.
次に、第３図（ａ）及び（ｂ）はそれぞれ本発明の滑性
向上シートの平面図及び比較例である焼成シートの平面
図である。Next, FIGS. 3(a) and 3(b) are a plan view of a slipperiness-improving sheet of the present invention and a plan view of a fired sheet as a comparative example, respectively.
平面的にも本発明の滑性向上シートの方が球状セラミッ
ク？５）末の滑面作用でこる効果が生しる可能性が示唆
される。Is the lubricity-improving sheet of the present invention better than spherical ceramic in terms of plane? 5) It is suggested that the stiffening effect may be caused by the smooth surface action at the end.
第４図は球状のセラミック粉末（３）の粒径を不定形状
のセラミック粉末（２）の粒径よりも大きくした場合の
模式図である。FIG. 4 is a schematic diagram when the particle size of the spherical ceramic powder (3) is made larger than the particle size of the irregularly shaped ceramic powder (2).
この場合には球状のセラミック粉末（２）が超硬合金（
６）に部分接触し、不定形状のセラミックＩ５）末（３
）のころ効果が期待できない。また、球状のセラミック
粉末の含有率を大きくすると、焼成後転がりの発生する
危険性があり好ましくない。In this case, the spherical ceramic powder (2) is made of cemented carbide (
6), an irregularly shaped ceramic I5) powder (3)
), the effect cannot be expected. Furthermore, increasing the content of spherical ceramic powder is not preferable since there is a risk of rolling after firing.
したがって、球状のセラミック粉末（２）の粒径は不定
形状のセラミック粉末（３）の粒径と同等、又はそれ以
下にすることが好ましい。Therefore, the particle size of the spherical ceramic powder (2) is preferably equal to or smaller than the particle size of the irregularly shaped ceramic powder (3).
以上に説明したとおり、本発明は超硬合金を反りや浸炭
なく焼成することのできる滑性向上シートとして、従来
の問題点を一掃し、産業の発展に寄与するところは極め
て大きいものである。As explained above, the present invention is a lubricity-improving sheet that can be used to sinter cemented carbide without warping or carburizing, thereby eliminating the conventional problems and greatly contributing to the development of industry.
第１図は本発明の実施例である滑性向上シートの模式図
、第２図は焼成時の状態図、第３図（ａ）及び（ｂ）は
それぞれ本発明の滑性向上シートの平面図及び比較例で
ある焼成シートの平面図、第４図はセラミック粉末の粒
径を検討するための模式（２）：不定形状のセラミック
粉末、（３）：球状のセラミック粉末、（４）：気孔、
（５）：有機バインダー第２図Fig. 1 is a schematic diagram of a lubricity-improving sheet according to an embodiment of the present invention, Fig. 2 is a state diagram during firing, and Figs. 3 (a) and (b) are plane views of the lubricity-improving sheet of the present invention, respectively. Fig. 4 is a schematic diagram for examining the particle size of ceramic powder (2): irregularly shaped ceramic powder, (3): spherical ceramic powder, (4): stomata,
(5): Organic binder Figure 2
Claims (1)
のセラミック粉末（２）の粒径と同等あるいはそれ以下
の粒径の球状のセラミック粉末（３）とを有機バインダ
ー（５）で結着したことを特徴とする滑性向上シート。 ２、球状のセラミック粉末（２）の含有量が不定形状の
セラミック粉末（３）の含有量よりも少ないことを特徴
とする請求項１記載の滑性向上シート。 ３、有機バインダー（５）が気孔（４）を有することを
特徴とする請求項１記載の滑性向上シート。[Claims] 1. An irregularly shaped ceramic powder (2) and a spherical ceramic powder (3) having a particle size equal to or smaller than the irregularly shaped ceramic powder (2) are combined into an organic binder. A lubricity-enhancing sheet characterized by being bound by (5). 2. The lubricity-improving sheet according to claim 1, wherein the content of the spherical ceramic powder (2) is smaller than the content of the irregularly shaped ceramic powder (3). 3. The lubricity-improving sheet according to claim 1, wherein the organic binder (5) has pores (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2159243A JPH0448007A (en) | 1990-06-18 | 1990-06-18 | Improved lubricity sheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2159243A JPH0448007A (en) | 1990-06-18 | 1990-06-18 | Improved lubricity sheet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0448007A true JPH0448007A (en) | 1992-02-18 |
Family
ID=15689477
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2159243A Pending JPH0448007A (en) | 1990-06-18 | 1990-06-18 | Improved lubricity sheet |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0448007A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04131693A (en) * | 1990-09-20 | 1992-05-06 | Ishizuka Glass Co Ltd | Baking sheet |
| WO1999055639A1 (en) * | 1998-04-10 | 1999-11-04 | Nippon Shokubai Co., Ltd. | Ceramic sheet and method of producing ceramic sheet |
| GB2469546A (en) * | 2009-01-21 | 2010-10-20 | Schott Ag | Granulates with smooth particles and binder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63319145A (en) * | 1987-06-24 | 1988-12-27 | Ishizuka Glass Ltd | Sheet for improving lubricity during firing |
| JPH0283242A (en) * | 1988-09-21 | 1990-03-23 | Ishizuka Glass Co Ltd | Baking sheet |
-
1990
- 1990-06-18 JP JP2159243A patent/JPH0448007A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63319145A (en) * | 1987-06-24 | 1988-12-27 | Ishizuka Glass Ltd | Sheet for improving lubricity during firing |
| JPH0283242A (en) * | 1988-09-21 | 1990-03-23 | Ishizuka Glass Co Ltd | Baking sheet |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04131693A (en) * | 1990-09-20 | 1992-05-06 | Ishizuka Glass Co Ltd | Baking sheet |
| WO1999055639A1 (en) * | 1998-04-10 | 1999-11-04 | Nippon Shokubai Co., Ltd. | Ceramic sheet and method of producing ceramic sheet |
| US7108827B1 (en) | 1998-04-10 | 2006-09-19 | Nippon Shokubai Co., Ltd. | Ceramic sheet and method of producing ceramic sheet |
| US7807257B2 (en) | 1998-04-10 | 2010-10-05 | Nippon Shokubai Co., Ltd. | Ceramic sheet and method of producing ceramic sheet |
| GB2469546A (en) * | 2009-01-21 | 2010-10-20 | Schott Ag | Granulates with smooth particles and binder |
| GB2469546B (en) * | 2009-01-21 | 2011-08-03 | Schott Ag | [Granulates with smooth particles and binder |
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