CN102781864A - Process for production of LAS-system crystalline glass - Google Patents
Process for production of LAS-system crystalline glass Download PDFInfo
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- CN102781864A CN102781864A CN2011800107075A CN201180010707A CN102781864A CN 102781864 A CN102781864 A CN 102781864A CN 2011800107075 A CN2011800107075 A CN 2011800107075A CN 201180010707 A CN201180010707 A CN 201180010707A CN 102781864 A CN102781864 A CN 102781864A
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- 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
- C03C10/0018—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 containing SiO2, Al2O3 and monovalent metal oxide as main constituents
- C03C10/0027—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 containing SiO2, Al2O3 and monovalent metal oxide as main constituents containing SiO2, Al2O3, Li2O as main constituents
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- General Chemical & Material Sciences (AREA)
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Abstract
A process for producing an LAS-system crystalline glass by melting a raw material batch, wherein the LAS-system crystalline glass comprises, in mass%, 55 to 75% of SiO2, 17 to 27% of Al2O3, 3 to 6% of Li2O, 0 to 2% of MgO, 0 to 2% of ZnO, 2 to 5.5% of TiO2, 0 to 3% of ZrO2, 0.03 to 1% of a rare earth oxide, and 0.01 to 0.2% of a halogen and does not substantially contain As2O3 or Sb2O3, and wherein the process is characterized in that the raw material batch contains 0.03 to 1% of the rare earth oxide and 0.05 to 1% of the halogen.
Description
Technical field
The present invention relates to be used to make the good LAS (Li of bubble quality
2O-Al
2O
3-SiO
2) bind the method for crystal glass.
Background technology
In the past, as the low bulk crystal glass, known have with β-quartz solid solution be main crystalline transparent crystal glass, be that LAS such as the opaque crystal glass of main crystalline bind crystal glass with β-triphane sosoloid.It is good that these LAS bind the thermotolerance and the resistance to sudden heating of crystal glass, therefore is widely used in cooking top plate, stove window, fire window etc.
Above-mentioned LAS binds crystal glass and makes through following method: at first, with raw material allocate, fusion and shaping, the LAS that makes thus as precursor binds crystal glass, then this LAS is bound crystal glass and implements crystallization treatment.At this,, can access the good glass of bubble quality through when the glass melting or behind the glass melting, melten glass being implemented clarifying treatment.But above-mentioned LAS binds the viscosity height of the glass melt of crystal glass, therefore exists and is difficult to clarifying problem.
In order to promote the clarification of glass, used As in the past
2O
3, Sb
2O
3As finings (for example, referenced patent document 1 and 2).But, As
2O
3And Sb
2O
3Be the big material of carrying capacity of environment, therefore, begin to reduce its usage quantity in recent years as far as possible, perhaps do not use above-mentioned substance.
Therefore, As instead
2O
3, Sb
2O
3Finings, with halogens such as Cl, SnO
2, SO
3Deng using or make up use (for example, the referenced patent document 3) separately.Halogen particularly, because that clarifying effect is good and difficult generation is not expected is painted, thereby very effective as finings.
The prior art document
Patent documentation
Patent documentation 1: japanese kokai publication hei 6-329439 communique
Patent documentation 2: TOHKEMY 2001-48582 communique
Patent documentation 3: japanese kokai publication hei 11-228180 communique
Summary of the invention
Using under the situation of halogen as finings, produce clarifying effect by discharging halogen gas in the glass during glass melting.But halogen remains in the glass easily, thereby has the problem that is difficult to give full play to potential clarification ability.
Therefore, the object of the present invention is to provide that the clarification ability of halogen obtains the method that the good LAS of bubble quality binds crystal glass when the glass melting through improving.
The inventor furthers investigate above-mentioned problem; The result finds, binds in the method for manufacture of crystal glass at LAS, through when using halogen as finings, adding specific composition; Can improve the clarifying effect of halogen, and it is proposed as the present invention.
That is, the present invention relates to the method for manufacture that a kind of LAS binds crystal glass, contain 55～75% SiO by percentage to the quality through the fusion of raw material masterbatch being made as forming
2, 17～27% Al
2O
3, 3～6% Li
2O, 0～2% MgO, 0～2% ZnO, 2～5.5% TiO
2, 0～3% ZrO
2, 0.03～1% rare earth oxide, 0.01～0.2% halogen and do not contain As in fact
2O
3And Sb
2O
3LAS bind crystal glass, said method of manufacture is characterised in that, contains 0.03～1% rare earth oxide in the raw material masterbatch and contains 0.05～1% halogen.
Discoveries such as the inventor are carried out when LAS binds the crystal glass fusion under the clarifying situation of halogen, through adding rare earth oxide, can reduce halogen quantity residual in the glass.That is, rare earth oxide can promote the halogen in the glass in residual bubble, to spread, and the diameter of bubble is increased and easy come-up, thereby can improve clarifying effect.Therefore, even reduce the addition of finings and employed halogen, also can expect with in the past equal or be higher than clarifying effect in the past.
In addition, under the situation of the mf that forms aluminium etc. on the glass surface,, then can there be mf in time passing and the problem that is corroded easily if residual in the glass have a halogen.Manufacturing method according to the invention can reduce halogen residual in the glass, therefore, can also obtain making such mf to be difficult for taking place the corrosive effect.
Need to prove that among the present invention, " LAS binds crystal glass " is meant through the crystallization processing and makes β-quartz solid solution or β-LAS such as triphane sosoloid bind brilliant glass of separating out as main crystallization.
The second, the method for manufacture that LAS of the present invention binds crystal glass is characterised in that rare earth oxide is Nd
2O
3Or Er
2O
3
The 3rd, the present invention relates to a kind of LAS and bind crystal glass, it is characterized in that, be made through above-mentioned any one method of manufacture.
The 4th, the present invention relates to a kind of LAS and bind crystal glass, it is characterized in that, as composition, by percentage to the quality, contain 55～75% SiO
2, 17～27% Al
2O
3, 3～6% Li
2O, 0～2% MgO, 0～2% ZnO, 2～5.5% TiO
2, 0～3% ZrO
2, 0.03～1% rare earth oxide, 0.01～0.2% halogen and do not contain As in fact
2O
3And Sb
2O
3
The 5th, the present invention relates to a kind of LAS and bind crystal glass, it is characterized in that, form through making above-mentioned each described LAS bind the crystal glass crystallization.
The 6th, LAS of the present invention binds crystal glass and is characterised in that, forms through β-quartz solid solution or β-triphane sosoloid is separated out as main crystallization.
Embodiment
The present invention relates to the method for manufacture that a kind of LAS binds crystal glass, it is used to make as forming and contains 55～75% SiO by percentage to the quality
2, 17～27% Al
2O
3, 3～6% Li
2O, 0～2% MgO, 0～2% ZnO, 2～5.5% TiO
2, 0～3% ZrO
2, 0.03～1% rare earth oxide, 0.01～0.2% halogen and do not contain As in fact
2O
3And Sb
2O
3LAS bind crystal glass.Among the present invention, the reason explanation that the composition that LAS is bound crystal glass carries out above-mentioned qualification as follows.Need to prove, if do not specify, " % " expression " quality % " in the then following record.
SiO
2The skeleton and the formation LAS that are formation glass are the crystalline composition.SiO
2Content be preferably 55～75%, 58～70%, be preferably 60～68% especially.SiO
2Content be less than at 55% o'clock, thermal expansivity has the tendency of increase, is difficult to obtain the good crystal glass of resistance to sudden heating.In addition, the weather resistance of chemistry has the tendency of reduction.On the other hand, SiO
2Content more than 75% o'clock, the viscosity of glass melting property variation or glass melt increases and is difficult to clarification, and the tendency that is difficult to carry out forming of glass is arranged.
Al
2O
3The skeleton and the formation LAS that are formation glass are the crystalline composition.Al
2O
3Content be preferably 17～27%, 19～25%, be preferably 20～23% especially.Al
2O
3Content be less than at 17% o'clock, thermal expansivity has the tendency of increase, is difficult to obtain the good crystal glass of resistance to sudden heating.In addition, the weather resistance of chemistry has the tendency of reduction.On the other hand, Al
2O
3Content more than 27% o'clock, the viscosity of glass melting property variation or glass melt increases and is difficult to clarification, and the tendency that is difficult to carry out forming of glass is arranged.In addition, the crystallization of mullite is separated out and is made glass have the tendency of devitrification, and glass is damaged easily.
Li
2O is that formation LAS is the crystalline composition, and crystallinity is had bigger influence, simultaneously, is the composition that the viscosity that makes glass reduces, makes glass melting property and plasticity to improve.Li
2The content of O is preferably 3～6%, 3.3～5.5%, is preferably 3.5～5% especially.Li
2The content of O is less than at 3% o'clock, and the crystallization of mullite is separated out and made glass have the tendency of devitrification.In addition, when making the glass crystallization, LAS binds crystalline substance and becomes and be difficult to separate out, and is difficult to obtain the good crystal glass of resistance to sudden heating.And the viscosity of glass melting property variation or glass melt increases and is difficult to clarification, and the tendency that is difficult to carry out forming of glass is arranged.On the other hand, Li
2The content of O was more than 6% o'clock, and it is strong that crystallinity became, and glass has the tendency of devitrification, and glass is damaged easily.
MgO is that solid solution binds the composition in the crystalline substance in LAS.The content of MgO is preferably 0～2%, 0～1.5%, is preferably 0.1～1.2% especially.The content of MgO was more than 2% o'clock, and crystallinity became strong and had the tendency of devitrification, and glass is damaged easily.
ZnO binds the composition in the crystalline substance with MgO solid solution likewise in LAS.The content of ZnO is preferably 0～2%, 0～1.5%, is preferably 0.1～1.2% especially.The content of ZnO was more than 2% o'clock, and it is strong that crystallinity became, and therefore, when when slowly refrigerative forms simultaneously, glass has the tendency of devitrification.As a result, glass is damaged easily, thereby for example is difficult to utilize that float glass process forms.
TiO
2Be to be used for the one-tenth nuclear composition that crystallization separated out in crystallization step.TiO
2Content be preferably 2～5.5%, 2～5.2%, be preferably 2～5% especially.TiO
2Content more than 5.5% o'clock, glass has the tendency of devitrification, and is easily damaged.On the other hand, TiO
2Content be less than at 2% o'clock, can not fully form nucleus, possibly separate out thick crystallization and cause breakage.
ZrO
2Be and TiO
2Likewise be used for the one-tenth nuclear composition that crystallization separated out in crystallization step.ZrO
2Content be preferably 0～3%, 0.1～2.5%, be preferably 0.5～2.3% especially.ZrO
2Content more than 3% o'clock, have the tendency of devitrification during glass melting, be difficult to carry out the shaping of glass.
Method of manufacture of the present invention is characterised in that, contains 0.03～1% rare earth oxide in the raw material masterbatch and contains 0.05～1% halogen.
As rare earth oxide, can use Nd
2O
3, Er
2O
3, Gd
2O
3, CeO
2Deng lanthanide metal oxide.Nd particularly
2O
3And Er
2O
3, the effect of the clarification ability of promotion halogen is high especially, obtains the good LAS of bubble quality easily and binds crystal glass.The content of the rare earth oxide in the raw material masterbatch is preferably 0.03～1%, is preferably 0.05～0.8% especially.The content of rare earth oxide is less than at 0.03% o'clock, is difficult to obtain to make the effect of the residual halogens amount minimizing in the glass, and the result is difficult to obtain sufficient clarifying effect.On the other hand,, can make overcoloring of glass on the contrary, the tendency that is not suitable for using arranged according to the difference of purposes even the effect that the content of rare earth oxide more than 1%, makes the residual halogens amount in the glass reduce also is difficult to strengthen again.
Need to prove, utilize method of manufacture of the present invention and the LAS that obtains binds the content of the rare earth oxide in the crystal glass and above-mentioned same.
As halogen, can be used singly or in combination Cl, Br, I, F.Wherein, from clarification ability height and easy to handle viewpoint, preferably use Cl.As the halogen raw material, can enumerate alkali metal halide (for example NaCl, KCl, LiCl etc.).The content of the halogen in the raw material masterbatch is preferably 0.05～1%, is preferably 0.1～0.8% especially.The content of the halogen in the raw material masterbatch is less than at 0.05% o'clock, and clarifying effect has inadequate tendency.On the other hand, though content of halogen more than 1%, clarifying effect also no longer strengthens, the halogen residue amount in the glass increases, and is easy to generate the corrosive problem of aforesaid mf.
In addition, utilize method of manufacture of the present invention and the LAS that obtains binds the content of the halogen in the crystal glass is preferably below 0.2%, be preferably below 0.15% especially.LAS bound content of halogen in the crystal glass more than 0.2% o'clock, was easy to generate the corrosive problem of aforesaid mf.On the other hand, do not limit lower limit is special, but say to be more than 0.01% from actual angle.
Need to prove that among the present invention, content of halogen is meant the content in halogen atom.
As
2O
3And Sb
2O
3Also be the finings composition, but carrying capacity of environment is big, it is very important therefore not containing in fact in the present invention.Need to prove that said among the present invention " not containing in fact " is meant and initiatively uses as raw material and with the level that the impurity form is sneaked into, be meant that particularly content is below 0.1%.
Can add SnO as other finings compositions
2, SO
3But, SnO
2Have and make the painted effect that deepens that is contained in Fe in the frit etc. with the impurity form, therefore preferably stay in below 0.2%.SO
3Thereby be with halogen likewise in glass in bubble diffusion promote clarifying composition, but can cause also and heavily boil and have the effect that produces bubble that therefore, the residual quantity in glass preferably stays in below the 200ppm.
Except that mentioned component, in the scope of not damaging desired characteristic, can add various compositions.
For example, in order to suppress thick crystalline growth, can add the B more than 0.1% when making the glass crystallization
2O
3But, B
2O
3Content when too much, the thermotolerance of glass has impaired tendency, so the upper limit is preferably set to below 2%.
P
2O
5Be the phase-splitting that promotes glass, the composition that helps nucleus to form, can in glass, add more than 0.1%.P
2O
5Content when too much, easily phase-splitting takes place in the fusion operation and is difficult to obtain to have the glass that expectation is formed, and the opaque tendency that becomes.Therefore, the upper limit is preferably set to below 3%.
In addition, improve meltbility and plasticity, can add total amount and be 0.1～5% Na for the viscosity that reduces glass
2O, K
2O, CaO, SrO and BaO.Need to prove that CaO, SrO and BaO also are the compositions that when glass melting, makes the glass devitrification, so the total amount of these compositions is preferably set to below 2%.
In addition, can add total amount is NiO, CoO, Cr below 2%
2O
3, Fe
2O
3, V
2O
5Deng tinting material.
The raw material masterbatch that above-mentioned each composition allotment is formed forms, anneals after fusion under 1550～1850 ℃ the temperature, obtains LAS and binds crystal glass.Need to prove,, can use various manufacturing process such as float glass process, pressing, flat (the ロ one Le ア ウ ト) method of roller according to target shape.
Crystal glass by such making is made crystal glass in the following manner.
LAS after being shaped is bound crystal glass after carrying out thermal treatment in 1～5 hour under 600～800 ℃ and making it form nucleus; Further under 800～1100 ℃, carry out thermal treatment in 0.5～3 hour; It is brilliant as main crystallization and separate out that LAS is bound, and can access LAS thus and bind crystal glass.Need to prove, in the time of obtaining transparent crystal glass, form nucleus after, under 800～950 ℃, carry out thermal treatment in 0.5～3 hour and β-quartz solid solution separated out get final product; When obtaining the crystal glass of White-opalescent, after forming nucleus, under 1000～1100 ℃, carry out thermal treatment in 0.5～3 hour and make β-triphane sosoloid separate out and get final product.
In addition, crystal glass of the present invention forms through making LAS bind brilliant separating out as main crystallization, therefore, has pact-10～30 * 10
-7The low thermal coefficient of expansion of/℃ (30～750 ℃ of measurement ranges), excellent heat resistance, and have high mechanical strength.
LAS of the present invention binds crystal glass and LAS and binds crystal glass and be characterised in that, as composition, by percentage to the quality, contains 55～75% SiO
2, 17～27% Al
2O
3, 3～6% Li
2O, 0～2% MgO, 0～2% ZnO, 2～5.5% TiO
2, 0～3% ZrO
2, 0.03～1% rare earth oxide, 0.01～0.2% halogen and do not contain As in fact
2O
3And Sb
2O
3The reason that composition is carried out above-mentioned qualification as previously mentioned.In addition, except that these composition, can suitably contain mentioned component.
Crystal glass of the present invention can be implemented post-treatment such as cutting, grinding, bending machining, perhaps can implement to draw to the surface etc.
Embodiment
Below, utilize embodiment that the present invention at length is described, but the present invention is not limited to these embodiment.
At first, according to the composition allotment raw material powder of record in the table 1, and then the ratio interpolation Nd to put down in writing in table 2～4
2O
3Or Er
2O
3And Cl, thereby obtain the raw material masterbatch.Need to prove,, in masterbatch A, C, use NaCl, in masterbatch B, use LiCl as the Cl raw material.
[table 1]
[table 2]
[table 3]
[table 4]
Each raw material masterbatch is dropped in the crucible, 1600 ℃ of following fusions 20 hours, again 1700 ℃ of following fusions 4 hours.Glass melt is poured on the carbon plate,, and utilizes electric furnace to anneal, obtain glass specimen thus with the thickness of roller stand written treaty 5mm.Annealing is carried out through being cooled to room temperature from 700 ℃ of speed with 100 ℃/hour.For the glass specimen of gained, carry out the evaluation of Cl residual quantity and clarification property.The results are shown in table 2～4.Need to prove that in the glass specimen of gained, the composition beyond the Cl has the content of record in table 1～4.
The Cl residual quantity is measured through following method: each glass specimen is processed into the tabular of 3mm, mirror ultrafinish is carried out on the two sides, utilize x-ray fluorescence analysis (XRF) to carry out total ultimate analysis, and carry out ZAF and proofread and correct.
For clarification property; With the number of bubbles (more than the bubble diameter 0.1mm) of the above-mentioned glass specimen of every 100g is that 0 sample is evaluated as " A "; With above-mentioned number of bubbles is that 1～2 sample is evaluated as " B "; With above-mentioned number of bubbles is that 3～5 sample is evaluated as " C ", is that sample more than 6 is evaluated as " D " with above-mentioned number of bubbles.
Claims (6)
1. a LAS binds the method for manufacture of crystal glass, it is characterized in that, contains 55～75% SiO by percentage to the quality through the fusion of raw material masterbatch being made as forming
2, 17～27% Al
2O
3, 3～6% Li
2O, 0～2% MgO, 0～2% ZnO, 2～5.5% TiO
2, 0～3% ZrO
2, 0.03～1% rare earth oxide, 0.01～0.2% halogen and do not contain As in fact
2O
3And Sb
2O
3LAS bind crystal glass,
In the said method of manufacture, contain 0.03～1% rare earth oxide in the raw material masterbatch and contain 0.05～1% halogen.
2. LAS as claimed in claim 1 binds the method for manufacture of crystal glass, it is characterized in that, rare earth oxide is Nd
2O
3Or Er
2O
3
3. a LAS binds crystal glass, it is characterized in that,
Be made through claim 1 or 2 described method of manufacture.
4. a LAS binds crystal glass, it is characterized in that,
As composition, by percentage to the quality, contain 55～75% SiO
2, 17～27% Al
2O
3, 3～6% Li
2O, 0～2% MgO, 0～2% ZnO, 2～5.5% TiO
2, 0～3% ZrO
2, 0.03～1% rare earth oxide, 0.01～0.2% halogen and do not contain As in fact
2O
3And Sb
2O
3
5. a LAS binds crystal glass, it is characterized in that,
Form through making claim 3 or 4 described LAS bind the crystal glass crystallization.
6. LAS as claimed in claim 5 binds crystal glass, it is characterized in that,
Through being separated out as main crystallization, β-quartz solid solution or β-triphane sosoloid forms.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010038224A JP2011173748A (en) | 2010-02-24 | 2010-02-24 | Method for producing las-based crystalline glass |
| JP2010-038224 | 2010-02-24 | ||
| PCT/JP2011/053089 WO2011105246A1 (en) | 2010-02-24 | 2011-02-15 | Process for production of las-system crystalline glass |
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| Publication Number | Publication Date |
|---|---|
| CN102781864A true CN102781864A (en) | 2012-11-14 |
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|---|---|---|---|
| CN2011800107075A Pending CN102781864A (en) | 2010-02-24 | 2011-02-15 | Process for production of LAS-system crystalline glass |
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|---|---|
| JP (1) | JP2011173748A (en) |
| CN (1) | CN102781864A (en) |
| WO (1) | WO2011105246A1 (en) |
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| CN109015419A (en) * | 2018-08-02 | 2018-12-18 | 大连工业大学 | A kind of LAS microcrystalline glass in series abrasive material combination agent prescription, preparation method and application |
| CN113003939A (en) * | 2019-12-19 | 2021-06-22 | 湖州大享玻璃制品有限公司 | SiO2-CaO-based crystallized glass and method for producing same |
| CN113526865A (en) * | 2020-04-17 | 2021-10-22 | Ａｇｃ株式会社 | Aluminosilicate glass and method for producing same |
| CN115959830A (en) * | 2021-10-08 | 2023-04-14 | 湖州大享玻璃制品有限公司 | SiO (silicon dioxide) 2 Crystallized glass of-CaO system and method for producing same |
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| JP2013087986A (en) * | 2011-10-14 | 2013-05-13 | Nippon Electric Glass Co Ltd | Glass plate for top plate for cooker and method of manufacturing the same |
| DE102012202697A1 (en) * | 2012-02-22 | 2013-08-22 | Schott Ag | Transparent colorless lithium aluminum silicate glass-ceramic and their use |
| FR3002532B1 (en) * | 2013-02-28 | 2015-02-27 | Eurokera | LITHIUM ALUMINOSILICATE TYPE VITROCERAMIC COMPRISING A SOLID BETA-SPODUMENE SOLUTION |
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| ES2306312T3 (en) * | 2006-03-20 | 2008-11-01 | Schott Ag | GLASS BASED SILICATE LITHIUM AND CERAMIZABLE ALUMINUM, CONTAINING ARSENIC AND ANTIMONY, OBTAINED BY FLOATING AND OPTIMALLY DETECTABLE. |
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- 2010-02-24 JP JP2010038224A patent/JP2011173748A/en active Pending
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- 2011-02-15 WO PCT/JP2011/053089 patent/WO2011105246A1/en active Application Filing
- 2011-02-15 CN CN2011800107075A patent/CN102781864A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101213152A (en) * | 2005-06-30 | 2008-07-02 | 欧罗克拉公司 | Preparation of glass-ceramics of beta-quartz and/or of beta-spodumene, of articles made from such glass-ceramics, glass-ceramics, articles made from said glass-ceramics and precursor glasses |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109015419A (en) * | 2018-08-02 | 2018-12-18 | 大连工业大学 | A kind of LAS microcrystalline glass in series abrasive material combination agent prescription, preparation method and application |
| CN113003939A (en) * | 2019-12-19 | 2021-06-22 | 湖州大享玻璃制品有限公司 | SiO2-CaO-based crystallized glass and method for producing same |
| CN113526865A (en) * | 2020-04-17 | 2021-10-22 | Ａｇｃ株式会社 | Aluminosilicate glass and method for producing same |
| CN115959830A (en) * | 2021-10-08 | 2023-04-14 | 湖州大享玻璃制品有限公司 | SiO (silicon dioxide) 2 Crystallized glass of-CaO system and method for producing same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2011173748A (en) | 2011-09-08 |
| WO2011105246A1 (en) | 2011-09-01 |
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