CN1315745C - Multilayer film mould core for molding glass - Google Patents
Multilayer film mould core for molding glass Download PDFInfo
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- CN1315745C CN1315745C CNB2004100304183A CN200410030418A CN1315745C CN 1315745 C CN1315745 C CN 1315745C CN B2004100304183 A CNB2004100304183 A CN B2004100304183A CN 200410030418 A CN200410030418 A CN 200410030418A CN 1315745 C CN1315745 C CN 1315745C
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Abstract
The present invention relates to a multilayer film mold core for molding glass, which comprises a base material and a first protecting film connected with the base material, wherein the first protecting film is orderly provided with a ceramic layer, a first buffer layer and a metal layer from the base material to the direction far away from the base material; the metal layer is made from a component containing precious metal elements; the first buffer layer is provided with a ceramic material and a precious metal material; the first buffer layer has a ceramic side with rich ceramics, and a precious metal side with rich precious metals, which is opposite to the ceramic side with rich ceramics; and the ceramic side with rich ceramics is connected with the ceramic layer. The multilayer film mold core increases the homogeneity between the interface of the ceramic material and the interface of the metal material so as to enhance the adhesiveness between every two layers.
Description
[technical field]
The present invention relates to the die (molding core) that a kind of glass moulding is used, particularly relate to multilayer film (multi layer) die that a kind of glass moulding is used.
[background technology]
Be applied to the problem that often runs on the die that glass moulding uses in recent years, normally be to obtain suitable die Coating Materials.Be formed on precious metal (noblemetal) alloy film on the die base material owing to have unreactiveness, therefore, be difficult for glass and model atmosphere in reactive gas react.But under high temperature model long-time continuous is used, but, make glass behind model, can't meet the requirement of optical quality easily because of crystal grain-growth (grain growth) produces surface roughening (roughen).In addition, though be formed at the high thermal resistance of the ceramic membrane (as chromium nitride (CrN), tantalum nitride (TaN) etc.) on the die base material good and with wolfram varbide (tungstencarbide; Hereinafter to be referred as WC) tack of base material is good, but when the high temperature model is used, but easily with glass and model atmosphere in reactive gas react, cause ceramic membrane surface produce variable color or and glass between produce and adhere.
As shown in Figure 1, Japanese 05-294642 patent is exposed the multilayer film die 1 that a kind of glass moulding is used.This multilayer film die 1 can suppress precious metal alloys and produce crystal grain-growth under high temperature model long-time continuous is used, and also can solve problems such as ceramic membrane surface variable color or glass adhesion.This multilayer film die 1 comprises: one is formed on the multilayer film 12 on a surface of this base material 11 by the made base material 11 and of WC.
This multilayer film 12 be have ceramic layer that several materials is titanium nitride (TiN), and several materials be the metal level of platinoiridita (Pt-Ir) alloy, and these ceramic layers and metal level are to be the interlaced shape that piles up, and the material that wherein is connected in these base material 11 places is a ceramic layer.
Above the multilayer film die 1 used of mentioned glass moulding, though under high temperature model long-time continuous is used, can suppress precious metal alloys and produce crystal grain-growth, also can solve problems such as ceramic membrane surface variable color or glass adhesion, but because the surface property difference of this ceramic layer and two kinds of storerooms of metal level is very big, therefore how improving the tack between this ceramic layer and the metal level, is the relevant required a great problem that overcomes of dealer of multilayer film die that current exploitation glass moulding is used.
[summary of the invention]
The objective of the invention is to be the multilayer film die that provides a kind of glass moulding to use, utilizing increases homogeneous principle between stupalith and metallic substance interface, can improve the tack between each layer, and avoid the surperficial roughening of multilayer film die, to meet the requirement of the optical quality of glass behind model.
In order to achieve the above object, the invention provides the multilayer film die that a kind of glass moulding is used, it is characterized in that: it comprises:
One base material; And
One is connected in first protective membrane of this base material, this first protective membrane has a ceramic layer, one first buffer layer and a metal level by this base material in regular turn to the direction away from this base material, and this metal level is that to contain the component (noble metal-containing component) of precious metal element by one made;
Wherein, this first buffer layer (buffer layer) is to have a stupalith and a precious metal material, and this first buffer layer has one and is rich in ceramic side and and is rich in the precious metal side in contrast to what this was rich in ceramic side, and this is rich in ceramic side is to be connected in this ceramic layer.
The multilayer film die that described glass moulding is used; it is characterized in that: also comprise at least one second protective membrane that is connected in this first protective membrane; this second protective membrane has one second buffer layer by this first protective membrane in regular turn to the direction away from this first protective membrane; one ceramic layer; one first buffer layer and a metal level; this metal level is made by the component that contains above-mentioned precious metal element; each buffer layer of this second protective membrane is to have above-mentioned stupalith and precious metal material; and each buffer layer has one and is rich in ceramic side and and is rich in precious metal side, above-mentioned first in contrast to what this was rich in ceramic side; the ceramic side that is rich in of two buffer layers all is to be connected in this ceramic layer.
The multilayer film die that described glass moulding is used is characterized in that: each ceramic layer is made by in the following compounds any one: nitride, carbide or boride; This component that contains precious metal element is to comprise in the following precious metal element any one or a few: iridium, rhenium, ruthenium, rhodium, platinum, osmium.
The multilayer film die that described glass moulding is used is characterized in that: this compound is a mononitride, and this nitride is made by in the following nitride any one: titanium nitride chromium, TiAlN, chromium nitride, tantalum nitride, titanium nitride or aluminium nitride.
The multilayer film die that described glass moulding is used is characterized in that: this compound is a monocarbide, and this carbide is made by in the following carbide any one: titanium carbide, chromium carbide, zirconium carbide, niobium carbide or tantalum carbide.
The multilayer film die that described glass moulding is used is characterized in that: this component that contains precious metal element comprises iridium and rhenium.
The multilayer film die that described glass moulding is used is characterized in that: this component that contains precious metal element comprises iridium and ruthenium.
The multilayer film die that described glass moulding is used is characterized in that: this component that contains precious metal element also comprises any one in the following high-melting-point element: tantalum, carbon, titanium, chromium, tungsten or manganese.
The multilayer film die that described glass moulding is used is characterized in that: this high-melting-point element is a tantalum.
The multilayer film die that described glass moulding is used is characterized in that: this stupalith is that in the following compounds any one is made: nitride, carbide or boride; This precious metal material comprises any one or a few in the following precious metal element: iridium, rhenium, ruthenium, rhodium, platinum, osmium.
The multilayer film die that described glass moulding is used, it is characterized in that: this compound is a mononitride, this nitride is made by in the following nitride any one: titanium nitride chromium, TiAlN, chromium nitride, tantalum nitride, titanium nitride or aluminium nitride, this component that contains precious metal element comprises iridium and rhenium.
The multilayer film die that described glass moulding is used, it is characterized in that: this compound is a monocarbide, this carbide is made by in the following carbide any one: titanium carbide, chromium carbide, zirconium carbide, niobium carbide or tantalum carbide, this component that contains precious metal element comprises iridium and ruthenium.
The multilayer film die that described glass moulding is used, it is characterized in that: this compound is a monocarbide, this carbide is made by in the following carbide any one: titanium carbide, chromium carbide, zirconium carbide, niobium carbide or tantalum carbide, this component that contains precious metal element comprises iridium and rhenium.
The multilayer film die that described glass moulding is used is characterized in that: comprise six to 20 layers second protective membrane, and the thickness of each ceramic layer, first buffer layer, metal level and second buffer layer is between 10nm to 30nm.
According to described, each specific embodiment of the multilayer film die that glass moulding of the present invention is used has following several advantages:
One, utilize to increase homogeneous principle between stupalith and metallic substance interface, improving the tack between each layer, and prolong the work-ing life of this die.
Two, be lower than the principle of 30nm by each metal bed thickness, make the inner grain-size of precious metal be lower than a predetermined nucleation size, and then the inhibition crystal grain-growth, and avoid the surface of this multilayer film die to produce roughening, to meet the requirement of the optical quality of glass behind model.
Three, be positioned at the metal level (precious metal) of these die the superiors owing to have an inactivity, be difficult for glass and model atmosphere in reactive gas react, therefore, do not have problems such as layer on surface of metal variable color or glass adhesion.
Four, ceramic layer provides enough hardness, the damage that produces because of friction so as to opposing, and excellent heat-resisting shake (thermal shock) character is to improve the hurried number of film of die.
[description of drawings]
The present invention is described in detail below in conjunction with drawings and Examples:
Fig. 1 is a schematic side view, and the multilayer film die that a kind of existing glass moulding is used is described.
Fig. 2 is a schematic side view, and one of multilayer film die that glass moulding of the present invention is used is described
Specific embodiment one.
Fig. 3 is the local enlarged diagram of this Fig. 2, and the thin bilge construction of one second protective membrane in this specific embodiment one is described.
Fig. 4 is a component proportions synoptic diagram, one first buffer layer is described in a plating process, the variation of the concentration gradient of a stupalith and a precious metal material.
Fig. 5 is a component proportions synoptic diagram, one second buffer layer is described in a plating process, the variation of the concentration gradient of a stupalith and a precious metal material.
Fig. 6 is a schematic side view, and one of multilayer film die that glass moulding of the present invention is used is described
Specific embodiment two.
Fig. 7 is the local enlarged diagram of this Fig. 6, and the thin bilge construction of second protective membrane in this specific embodiment two is described.
Fig. 8 is a schematic side view, and one of multilayer film die that glass moulding of the present invention is used is described
Specific embodiment three.
Fig. 9 is the local enlarged diagram of this Fig. 8, and the thin bilge construction of second protective membrane in this specific embodiment three is described.
[embodiment]
The multilayer film die that glass moulding of the present invention is used comprises: a base material and one first protective membrane.
This first protective membrane is to be connected in this base material, and this first protective membrane has a ceramic layer, one first buffer layer and a metal level by this base material in regular turn to the direction away from this base material, and this metal level is that to contain the component of precious metal element by one made.
Wherein, this first buffer layer is to have a stupalith and a precious metal material, and this first buffer layer has one and be rich in ceramic side and and be rich in the precious metal side in contrast to what this was rich in ceramic side, and this is rich in ceramic side is to be connected in this ceramic layer.
Preferably, the multilayer film die used of glass moulding of the present invention more comprises at least one second protective membrane that is connected in this first protective membrane.This second protective membrane has one second buffer layer, a ceramic layer, one first buffer layer and a metal level by this first protective membrane in regular turn to the direction away from this first protective membrane.This metal level is made by the mentioned component that contains precious metal element in front.Each buffer layer of this second protective membrane is to have mentioned stupalith in front and precious metal material; and each buffer layer has one and is rich in ceramic side and and is rich in the precious metal side in contrast to what this was rich in ceramic side, and the ceramic side that is rich in of each buffer layer of this second protective membrane is to be connected to these ceramic layers.
Be applicable to that each ceramic layer of the present invention is that to be selected from the compound of the following group that constitutes by one made: nitride (nitride), carbide (carbide) and boride (boride).
In a preferred embodiment, this compound is a mononitride, and this nitride is that to be selected from the nitride of the following group that constitutes by one made: titanium nitride chromium (TiCrN), TiAlN (TiAlN), chromium nitride (CrN), tantalum nitride (TaN), titanium nitride (TiN) and aluminium nitride (AlN).In one embodiment, this nitride is made by titanium nitride chromium.
In another preferred embodiment, this compound is a monocarbide, and this carbide is that to be selected from the carbide of the following group that constitutes by one made: titanium carbide (TiC), chromium carbide (Cr
2C
3), zirconium carbide (ZrC), niobium carbide (NbC) and tantalum carbide (TaC).In one embodiment, this carbide is made by titanium carbide.
Be applicable to that the component that contains precious metal element of the present invention is to include the precious metal element that is selected from the following group that constitutes: iridium, rhenium (Re), ruthenium (Ru), rhodium (Rh), platinum, osmium (Os) and these a combination.In one embodiment, this component that contains precious metal element comprises iridium and rhenium.In another specific embodiment, this component that contains precious metal element comprises iridium and ruthenium.
Preferably, this component that contains precious metal element more comprises high-melting-point (melting point) element that is selected from the following group that constitutes: tantalum, carbon, titanium, chromium, tungsten and manganese (Mn).In one embodiment, this high-melting-point element is tantalum (hereinafter to be referred as Ta).
The stupalith that is applicable to these buffer layers of the present invention is that to be selected from the compound of the following group that constitutes by one made: nitride, carbide and boride.The precious metal material that is applicable to these buffer layers of the present invention is made by a component that contains precious metal element that is selected from the following group that constitutes: iridium, rhenium, ruthenium, rhodium, platinum, osmium and these a combination.
Preferably, the compound that is used for these buffer layers is a mononitride, and this nitride is that to be selected from the nitride of the following group that constitutes by one made: titanium nitride chromium, TiAlN, chromium nitride, tantalum nitride, titanium nitride and aluminium nitride.In one embodiment, the nitride that is used for these buffer layers is made by titanium nitride chromium (hereinafter to be referred as TiCrN), and this component that contains precious metal element comprises iridium and rhenium.
Preferably, the compound that is used for these buffer layers is a monocarbide, and this carbide is that to be selected from the carbide of the following group that constitutes by one made: titanium carbide (TiC), chromium carbide (Cr
2C
3), zirconium carbide (ZrC), niobium carbide (NbC) and tantalum carbide (TaC).In one embodiment, the carbide that is used for these buffer layers is made by titanium carbide, and this component that contains precious metal element comprises iridium and ruthenium (hereinafter to be referred as Ir-Ru).In another specific embodiment, the carbide that is used for these buffer layers is made by titanium carbide (hereinafter to be referred as TiC), and this component that contains precious metal element comprises iridium and rhenium (hereinafter to be referred as Ir-Re).
Preferably, the multilayer film die that this glass moulding is used is to comprise six to 20 layers second protective membrane, and the thickness of each ceramic layer, first buffer layer, metal level and second buffer layer is between 10nm to 30nm.
＜specific embodiment one 〉
Consult Fig. 2 and Fig. 3, a specific embodiment one of the multilayer film die that glass moulding of the present invention is used comprises: a WC base material 2, is connected in first protective membrane 3 and several second protective membranes 4 of this base material 2.
It is that ceramic layer 311, the material of TiCrN is first buffer layer 312 of TiCrN-Ir-Re that this first protective membrane 3 has a material by this base material 2 in regular turn to the direction away from this base material 2, and a material is the metal level 313 of Ir-Re.
Each second protective membrane 4 by near the position of this first protective membrane 3 to the direction away from this first protective membrane 3 have second buffer layer 411 that a material is Ir-Re-TiCrN in regular turn, ceramic layer 412, the material that a material is TiCrN is first buffer layer 413 of TiCrN-Ir-Re, and a material is the metal level 414 of Ir-Re.
What deserves to be mentioned is, each buffer layer the 312,411, the 413rd of the present invention utilizes sputter (co-sputtering) method altogether, in the plating process, regulate the ceramic target be arranged on the negative electrode and the power of a metal targets, so that the relative plating rate of this metallic substance (precious metal) of this stupalith, on plating time, be the variation (as Fig. 4 and shown in Figure 5) of a gradual concentration gradient (gradient).Making each buffer layer 312,411,413 have one is rich in ceramic side and and is rich in the precious metal side in contrast to what this was rich in ceramic side, and the ceramic side that is rich in of this first buffer layer 312 is to be connected in this ceramic layer 311, and the ceramic side that is rich in of each first and second buffer layer 413,411 is to be connected in each ceramic layer 412.Thus, utilize the principle that increases the homogeneity (coherence) between differing materials interface (interface), improve two kinds of tacks between the material.
In this specific embodiment one, the bed thickness of each layer is between 10～30nm, and the total thickness of this first protective membrane 3 and these second protective membranes 4 is to be lower than 1 μ m.Utilize each metal level 313,414 bed thickness to be lower than the principle of 30nm, make the inner grain-size of Ir-Re precious metal be lower than predetermined nucleation (nucleation) size, and then inhibition crystal grain-growth, and avoid the surface of this multilayer film die to produce roughening, to meet the requirement of the optical quality of glass behind model.
＜specific embodiment two 〉
Consult Fig. 6 and Fig. 7, a specific embodiment two of the multilayer film die that glass moulding of the present invention is used is identical with this specific embodiment one haply, and its difference is in this first and second protective membrane 3,4.
It is that ceramic layer 321, the material of TiC is first buffer layer 322 of TiC-Ir-Ru that this first protective membrane 3 has a material by this base material 2 in regular turn to the direction away from this base material 2, and a material is the metal level 323 of Ir-Ru.
Each second protective membrane 4 by near the position of this first protective membrane 3 to the direction away from this first protective membrane 3 have second buffer layer 421 that a material is Ir-Ru-TiC in regular turn, ceramic layer 422, the material that a material is TiC is first buffer layer 423 of TiC-Ir-Ru, and a material is the metal level 424 of Ir-Ru.
＜specific embodiment three 〉
Consult Fig. 8 and Fig. 9, a specific embodiment three of the multilayer film die that glass moulding of the present invention is used is identical with this specific embodiment one haply, and its difference is in this first and second protective membrane 3,4.
It is that ceramic layer 331, the material of TiC is first buffer layer 332 of TiC-Ir-Re that this first protective membrane 3 has a material by this base material 2 in regular turn to the direction away from this base material 2, and a material is the metal level 333 of Ir-Re-Ta.
Each second protective membrane 4 by near the position of this first protective membrane 3 to the direction away from this first protective membrane 3 have second buffer layer 431 that a material is Ir-Re-TiC in regular turn, ceramic layer 432, the material that a material is TiC is first buffer layer 433 of TiC-Ir-Re, and a material is the metal level 434 of Ir-Re-Ta.
What deserves to be mentioned is, each metal level 333,434 in this specific embodiment three adds the purpose of high-melting-point element T a, be to utilize the Ta atom to locate to pin down crystal boundary and merge, produce crystal grain-growth so as to avoiding crystal grain to merge via crystal boundary at crystal boundary (grain boundary).
From the above mentioned, each specific embodiment of the multilayer film die used of glass moulding of the present invention has following several characteristics:
One, utilize to increase homogeneous principle between stupalith and metallic substance interface, improving the tack between each layer, and prolong the work-ing life of this die.
Two, be lower than the principle of 30nm by each metal level 313,323,333,414,424,434 bed thickness, make the inner grain-size of precious metal be lower than a predetermined nucleation size, and then inhibition crystal grain-growth, and avoid the surface of this multilayer film die to produce roughening, to meet the requirement of the optical quality of glass behind model.
Three, be positioned at the metal level (precious metal) of these die the superiors owing to have an inactivity, be difficult for glass and model atmosphere in reactive gas react, therefore, do not have problems such as layer on surface of metal variable color or glass adhesion.
Four, ceramic layer provides enough hardness, the damage that produces because of friction so as to opposing, and excellent heat-resisting shake (thermal shock) character is to improve the hurried number of film of die.
Conclude above-mentioned, the multilayer film die that glass moulding of the present invention is used have between each layer tack good, meet the requirement of the optical quality of glass behind model, the characteristics such as long service life of die, so can reach purpose of the present invention really.
Claims (14)
1, the multilayer film die used of a kind of glass moulding, it is characterized in that: it comprises:
One base material; And
One is connected in first protective membrane of this base material, and this first protective membrane has a ceramic layer, one first buffer layer and a metal level by this base material in regular turn to the direction away from this base material, and this metal level is that to contain the component of precious metal element by one made;
Wherein, this first buffer layer is to have a stupalith and a precious metal material, and this first buffer layer has one and be rich in ceramic side and and be rich in the precious metal side in contrast to what this was rich in ceramic side, and this is rich in ceramic side is to be connected in this ceramic layer.
2; the multilayer film die that glass moulding as claimed in claim 1 is used; it is characterized in that: also comprise at least one second protective membrane that is connected in this first protective membrane; this second protective membrane has one second buffer layer by this first protective membrane in regular turn to the direction away from this first protective membrane; one ceramic layer; one first buffer layer and a metal level; this metal level is made by the component that contains above-mentioned precious metal element; each buffer layer of this second protective membrane is to have above-mentioned stupalith and precious metal material; and each buffer layer has one and is rich in ceramic side and and is rich in precious metal side, above-mentioned first in contrast to what this was rich in ceramic side; the ceramic side that is rich in of two buffer layers all is to be connected in this ceramic layer.
3, the multilayer film die used of glass moulding as claimed in claim 2 is characterized in that: each ceramic layer is made by in the following compounds any one: nitride, carbide or boride; This component that contains precious metal element is to comprise in the following precious metal element any one or a few: iridium, rhenium, ruthenium, rhodium, platinum, osmium.
4, the multilayer film die used of glass moulding as claimed in claim 3, it is characterized in that: this compound is a mononitride, and this nitride is made by in the following nitride any one: titanium nitride chromium, TiAlN, chromium nitride, tantalum nitride, titanium nitride or aluminium nitride.
5, the multilayer film die used of glass moulding as claimed in claim 3, it is characterized in that: this compound is a monocarbide, this carbide is made by in the following carbide any one: titanium carbide, chromium carbide, zirconium carbide, niobium carbide or tantalum carbide.
6, the multilayer film die used of glass moulding as claimed in claim 3, it is characterized in that: this component that contains precious metal element comprises iridium and rhenium.
7, the multilayer film die used of glass moulding as claimed in claim 3, it is characterized in that: this component that contains precious metal element comprises iridium and ruthenium.
8, the multilayer film die used of glass moulding as claimed in claim 6, it is characterized in that: this component that contains precious metal element also comprises any one in the following high-melting-point element: tantalum, carbon, titanium, chromium, tungsten or manganese.
9, the multilayer film die used of glass moulding as claimed in claim 8, it is characterized in that: this high-melting-point element is a tantalum.
10, the multilayer film die used of glass moulding as claimed in claim 2 is characterized in that: this stupalith is made by in the following compounds any one: nitride, carbide or boride; This precious metal material comprises any one or a few in the following precious metal element: iridium, rhenium, ruthenium, rhodium, platinum, osmium.
11, the multilayer film die used of glass moulding as claimed in claim 10, it is characterized in that: this compound is a mononitride, this nitride is made by in the following nitride any one: titanium nitride chromium, TiAlN, chromium nitride, tantalum nitride, titanium nitride or aluminium nitride, this component that contains precious metal element comprises iridium and rhenium.
12, the multilayer film die used of glass moulding as claimed in claim 10, it is characterized in that: this compound is a monocarbide, this carbide is made by in the following carbide any one: titanium carbide, chromium carbide, zirconium carbide, niobium carbide or tantalum carbide, this component that contains precious metal element comprises iridium and ruthenium.
13, the multilayer film die used of glass moulding as claimed in claim 10, it is characterized in that: this compound is a monocarbide, this carbide is made by in the following carbide any one: titanium carbide, chromium carbide, zirconium carbide, niobium carbide or tantalum carbide, this component that contains precious metal element comprises iridium and rhenium.
14, the multilayer film die used of glass moulding as claimed in claim 2 is characterized in that: comprise six to 20 layers second protective membrane, and the thickness of each ceramic layer, first buffer layer, metal level and second buffer layer is between 10nm to 30nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100304183A CN1315745C (en) | 2004-03-15 | 2004-03-15 | Multilayer film mould core for molding glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100304183A CN1315745C (en) | 2004-03-15 | 2004-03-15 | Multilayer film mould core for molding glass |
Publications (2)
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| CN1669963A CN1669963A (en) | 2005-09-21 |
| CN1315745C true CN1315745C (en) | 2007-05-16 |
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| CNB2004100304183A Expired - Fee Related CN1315745C (en) | 2004-03-15 | 2004-03-15 | Multilayer film mould core for molding glass |
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| CN (1) | CN1315745C (en) |
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| CN103182806B (en) * | 2011-12-30 | 2016-01-20 | 财团法人金属工业研究发展中心 | Work mould and film plating layer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002348131A (en) * | 2001-05-28 | 2002-12-04 | Asahi Glass Co Ltd | Die for molding glass and its manufacturing method |
| JP2003165730A (en) * | 2001-11-26 | 2003-06-10 | Nippon Electric Glass Co Ltd | Glass block and method for producing the same |
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2004
- 2004-03-15 CN CNB2004100304183A patent/CN1315745C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002348131A (en) * | 2001-05-28 | 2002-12-04 | Asahi Glass Co Ltd | Die for molding glass and its manufacturing method |
| JP2003165730A (en) * | 2001-11-26 | 2003-06-10 | Nippon Electric Glass Co Ltd | Glass block and method for producing the same |
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| CN1669963A (en) | 2005-09-21 |
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Granted publication date: 20070516 Termination date: 20140315 |