CN100594056C - Meltability polytetrafluorethylene tubular film and method for preparing same - Google Patents
Meltability polytetrafluorethylene tubular film and method for preparing same Download PDFInfo
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- CN100594056C CN100594056C CN200710160274A CN200710160274A CN100594056C CN 100594056 C CN100594056 C CN 100594056C CN 200710160274 A CN200710160274 A CN 200710160274A CN 200710160274 A CN200710160274 A CN 200710160274A CN 100594056 C CN100594056 C CN 100594056C
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- coating
- tubular film
- meltability polytetrafluorethyletubular
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- -1 polytetrafluorethylene Polymers 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims description 16
- 229920001343 polytetrafluoroethylene Polymers 0.000 title abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 31
- 238000000576 coating method Methods 0.000 claims abstract description 31
- 239000002344 surface layer Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims description 22
- 239000000839 emulsion Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 11
- 238000005507 spraying Methods 0.000 claims description 11
- 235000013618 yogurt Nutrition 0.000 claims description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 10
- 239000002987 primer (paints) Substances 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 8
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 229920002401 polyacrylamide Polymers 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 238000000280 densification Methods 0.000 claims description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 5
- 239000001103 potassium chloride Substances 0.000 claims description 5
- 235000011164 potassium chloride Nutrition 0.000 claims description 5
- 238000003618 dip coating Methods 0.000 claims description 4
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 claims description 4
- 230000004888 barrier function Effects 0.000 claims description 3
- 238000007590 electrostatic spraying Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 229920002379 silicone rubber Polymers 0.000 abstract description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract description 7
- 239000010410 layer Substances 0.000 abstract description 6
- 150000003839 salts Chemical class 0.000 abstract description 3
- 230000003373 anti-fouling effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 2
- 239000004945 silicone rubber Substances 0.000 abstract 2
- 238000005516 engineering process Methods 0.000 description 10
- 206010013786 Dry skin Diseases 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- 238000003486 chemical etching Methods 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- URXNVXOMQQCBHS-UHFFFAOYSA-N naphthalene;sodium Chemical compound [Na].C1=CC=CC2=CC=CC=C21 URXNVXOMQQCBHS-UHFFFAOYSA-N 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000005421 electrostatic potential Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
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- Laminated Bodies (AREA)
Abstract
The invention discloses a fusible polytetrafluoroethylene tubular film and the manufacturing method thereof. The tubular film is a seamless tubular piece consisting of a bottom layer and a surface layer, wherein the two layers are made mainly from fusible polytetrafluoroethylene, the bottom layer has a coating containing water-soluble inorganic salts that are dissolved out under ultrasonic water washing to form the micropores, and the surface layer is smooth and compact and has anti-sticking effect. The production method includes the following steps: coating the bottom and the surface layers respectively on the surface of an aluminum alloy tube, baking at a high temperature to form film, removing from the surface of the aluminum alloy tube, subjecting to ultrasonic washing to obtain the PFA tubular film with porous inner surface and smooth and compact outer surface. The outer surface of the product is smooth and compact and excellent in anti-fouling function. The inner surface of the product doesn't need subsequent treatment and has good effect of adhersion with silicone rubber after coating. The fusible polytetrafluoroethylene tubular film is particularly suitable for the production of silicone rubber hot rollers used in duplicators and laser printers.
Description
Technical field
The present invention relates to a kind of pressure adjusting rod in laser printer, the digital duplicating machine fixing member (promptly following hot rod) silicon rubber that is mainly used in and cover PFA tubular film and manufacture method thereof outward.
Background technology
Meltability polytetrafluorethyletubular (PFA) has the same high temperature resistant, the low surface property of polytetrafluoroethylene (PTFE) and demonstrates outside the excellent not viscosity, than polytetrafluoroethylene (PTFE) better elevated temperature strength and film clarity are arranged, in recent years, along with fixing device technical development in duplicator and the laser printer, print quality and definition are had higher requirement, hot rod has become main flow under the silicon rubber of outer coating PFA film, does not have the following rod of PFA coating and then is eliminated.
Meltability polytetrafluorethyletubular PFA tubular film, usually adopt blowing or extrusion molding both at home and abroad, because its blowing or extrusion molding require much all complicated than general plastics in technical difficulty and equipment, and, because its material therefor, also must be otherwise coat the back and silicon rubber can not be well bonding through handling such as the inner wall surface porous of chemical etchings such as naphthalene sodium.
Summary of the invention
Technical problem to be solved by this invention is the present situation at prior art, a kind of Meltability polytetrafluorethyletubular tubular film is provided, it is by selecting suitable inside and outside layer material, make not only smooth outer surface densification of tubular film, antifouling property good, and inner surface characteristics good with the silicon rubber cementability after coating.
Another technical problem to be solved by this invention provides a kind of manufacture method of above-mentioned Meltability polytetrafluorethyletubular tubular film, and the prior art difficulty is big to overcome, equipment requirement height and the high deficiency of cost.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: Meltability polytetrafluorethyletubular tubular film of the present invention, and it is the seamless tubular shaped thing that is made of bottom and surface layer, it is characterized in that:
Described bottom is formed by subbing, subbing is based on the Meltability polytetrafluorethyletubular emulsion of solid content 30～50wt%, and wherein blending has the B component that the component A that is equivalent to Meltability polytetrafluorethyletubular weight 3～15% and dry weight are equivalent to Meltability polytetrafluorethyletubular weight 3～15%; Wherein, component A is a water-soluble inorganic salt, and B component is to be selected from least a in polyvinyl alcohol, polyethylene glycol, aqueous polyacrylamide yogurt liquid, the polyvinylpyrrolidone;
Described surface layer is formed by investment precoat, investment precoat is based on the Meltability polytetrafluorethyletubular emulsion of solid content 30～50wt%, and wherein blending has the component D that the component C that is equivalent to Meltability polytetrafluorethyletubular weight 10～50% and dry weight are equivalent to Meltability polytetrafluorethyletubular weight 5～10%; Wherein, component C is perfluoroethylene-propylene or tetrafluoroethylene-ethylene copolymer, and component D is selected from least a in polyvinyl alcohol, polyethylene glycol, aqueous polyacrylamide yogurt liquid, the polyvinylpyrrolidone;
And, described bottom be densely covered with because of described water-soluble inorganic salt be rinsed the back formed micropore.
After the purpose of blending component A is the coating drying in the subbing, inorganic salts become trickle nucleus, these trickle nucleus are dissolved in water and obtain the inner wall surface of porous in the supersonic wave cleaning machine water treatment procedure afterwards, because the blending of inorganic salts in the subbing, very easily cause the instability of emulsion, the purpose of blending B component promptly is to improve the stability of coating emulsion.
The purpose of blending component C is to regulate tubular film shrinkage factor in use in the investment precoat, make it remain on (and not blending C between the 3%-6%, its radial shrinkage ratio has only between the 1.2%-3%), like this can be just right wrap rubber layer, bonding more firm; The purpose of blending component D is to improve the coating character and the levelability of electrostatic spraying.
In addition, all can add conduction, heat conduction and lubriation material as required in subbing and the investment precoat, this has been that prior art is disclosed.Such as, in the end and surface layer, add conductive carbon black or the graphite of 5%-15% respectively, can obtain the conductive coating of sheet resistance 2-200k Ω.The graphite or the boron nitride that add 10%-30% can obtain heat conduction and the lubricant coating of thermal conductivity factor 0.5-1.2w/ (mk).
Consider that from ease of solubility, cost and the material angle that is easy to get described water-soluble inorganic salt is preferably sodium chloride or potassium chloride.
The thickness of described bottom is 10～20 μ m.
The thickness of described surface layer is 15～45 μ m.
The present invention prepares the method for Meltability polytetrafluorethyletubular tubular film, it is characterized in that may further comprise the steps:
A, barrier coating; Adopt spraying or dip-coating method, described subbing is applied on the aluminium-alloy pipe outer surface forms primer coating;
B, coating surface layer; After treating the primer coating drying, adopt spraying or dip-coating method, described investment precoat is applied to forms the surface layer coating in the primer coating;
C, plasticizing film forming; After treating surface layer coating drying, be warming up to 370 ℃～380 ℃ with 3～66 ℃/min speed in the immigration heating furnace and carry out the heating plasticizing film forming;
D, washing; To plastify after film deviates from from the aluminium-alloy pipe surface, and, make the thin nucleus of water-soluble inorganic salt of described bottom inwall be dissolved in water, promptly get the sticking seamless tubular shaped film of inwall porous, the smooth densification of outer wall after drying through the supersonic wave cleaning machine water treatment.
Described spraying method can adopt multiple spraying method, as electrostatic spraying, air-flow spraying or airless spraying etc.
The drying of described primer coating and surface layer coating adopts air dry or is heated to about 100 ℃ dry.
The invention has the advantages that:
The present invention is by selecting suitable coating for use, make the bottom of Meltability polytetrafluorethyletubular tubular film be densely covered with micropore, thereby can with the silicon rubber good bonding, and removed from and follow-up having handled such as chemical etching inner wall surface such as naphthalene sodium, surface layer then has smooth outer surface, densification, characteristics that non-viscosity is good.Thereby the advantage that make that whole film has that bonding with silicon rubber, anti-pickup is effective, transparency and wearability can both be taken into account, and need not follow-up chemical etching inner wall surface and handle.
The inventive method then has simple and reliable, and equipment investment is few, and all kinds of models, specification and quantity are easily controlled, and produces " turning around " soon, and cost is low, and the advantage of constant product quality.
The specific embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
500 gram solid contents are that to add sodium chloride (NaCl) aqueous solution, the 50 gram solid contents that 100 gram concentration are 25wt% in 50wt% Meltability polytetrafluorethyletubular (PFA) emulsion be the aqueous polyacrylamide yogurt liquid of 45wt%, be mixed and made into subbing, insert on the electrostatic sprayer hold-down bars with ￠ 18 * 330mm bright mirror surface aluminium-alloy pipe, rotational velocity 30rpm, electrostatic potential 8KV, spray disk center and workpiece distance are 20～50cm, with the thickness of metering method control primer coating, and air dry.
Adding 150 gram solid contents in the 500 gram solid content 50wt%PFA emulsions is 50wt% perfluoroethylene-propylene yogurt liquid, 50 gram solid contents are 45wt% aqueous polyacrylamide yogurt liquid, be mixed and made into investment precoat, with the same process conditions of barrier coating under, be coated on the primer coating surface of above-mentioned air dry with electrostatic sprayer, with the thickness of metering method chain of command layer coating, and air dry.
After above-mentioned bottom and surface layer are coated, put into heating furnace and be warming up to 375 ℃ of heating plasticizing film forming, obtain the PFA tubular film of the thick 15um of bottom, the thick 30um of surface layer, gross thickness 45um behind the demoulding with 5 ℃/min speed.
The PFA tubular film makes the sodium chloride nucleus in the bottom be dissolved in water through the supersonic wave cleaning machine water treatment, promptly obtains the not sticking seamless tubular shaped finished film of the many micropores of inwall, the smooth densification of outer wall after the drying.
Embodiment 2
500 gram solid contents are potassium chloride (KCl) aqueous solution of 20wt% for the 50wt%PFA emulsion adds 115 gram concentration, and 25 gram polyethylene glycol (PEG) are mixed and made into subbing, adopt the production technology coating identical with embodiment 1, and 100 ℃ of dryings.
500 gram solid contents are 50wt% perfluoroethylene-propylene yogurt liquid for the 50wt%PFA emulsion adds 180 gram solid contents, and 25 gram cetomacrogol 1000s (PEG) are mixed and made into investment precoat, adopt the production technology coating identical with embodiment 1, and 100 ℃ of dryings.
Above-mentioned bottom, surface layer baking plasticizing process is identical with embodiment 1, obtains the PFA tubular film of the thick 20um of bottom, the thick 30um of surface layer, gross thickness 50um behind the demoulding.The PFA tubular film film that after the supersonic wave cleaning machine water treatment, gets product.
Embodiment 3
500 gram solid contents are that the potassium chloride (KCl) of 40wt% is water-soluble for the 30wt%PFA emulsion adds 55 gram concentration, and 22.5 gram polyvinylpyrrolidones (PVP) are mixed and made into subbing, adopt the production technology coating identical with embodiment 1, and 100 ℃ of dryings.
500 gram solid contents are 50wt% tetrafluoroethylene-ethylene copolymer (ETFE) emulsion for the 30wt%PFA emulsion adds 150 gram solid contents, 7.5 gram polyvinylpyrrolidone (PVP) is mixed and made into investment precoat, adopt the production technology coating identical with embodiment 1, and 100 ℃ of dryings.
Above-mentioned bottom, surface layer baking plasticizing process is identical with embodiment 1, obtains the PFA tubular film of the thick 10um of bottom, the thick 30um of surface layer, gross thickness 40um behind the demoulding.The PFA tubular film film that after the supersonic wave cleaning machine water treatment, gets product.
Embodiment 4
500 gram solid contents are that the potassium chloride (KCl) of 30wt% is water-soluble for the 40wt%PFA emulsion adds 20 gram concentration, and 6 gram polyvinyl alcohol (PVA) are mixed and made into subbing, adopt the production technology coating identical with embodiment 1, and 100 ℃ of dryings.
500 gram solid contents are 50wt% perfluoroethylene-propylene yogurt liquid for the 40wt%PFA emulsion adds 40 gram solid contents, and 7.5 gram polyvinyl alcohol (PVA) are mixed and made into investment precoat, adopt the production technology coating identical with embodiment 1, and air dry.
Above-mentioned bottom, surface layer baking plasticizing process is identical with embodiment 1, obtains the PFA tubular film of the thick 20um of bottom, the thick 30um of surface layer, gross thickness 50um behind the demoulding.The PFA tubular film film that after the supersonic wave cleaning machine water treatment, gets product.
Embodiment 5
500 gram solid contents are that the sodium chloride (NaCl) of 30wt% is water-soluble for the 50wt%PFA emulsion adds 30 gram concentration, 50 gram solid contents are that the aqueous polyacrylamide yogurt liquid of 45wt% is mixed and made into subbing, adopt the production technology coating identical with embodiment 1, and 100 ℃ of dryings.
500 gram solid contents are 50wt% perfluoroethylene-propylene yogurt liquid for the 50wt%PFA emulsion adds 100 gram solid contents, and 20 gram polyvinyl alcohol (PVA) are mixed and made into investment precoat, adopt the production technology coating identical with embodiment 1, and 100 ℃ of dryings.
Above-mentioned bottom, surface layer baking plasticizing process is identical with embodiment 1, obtains the PFA tubular film of the thick 20um of bottom, the thick 15um of surface layer, gross thickness 35um behind the demoulding.The PFA tubular film film that after the supersonic wave cleaning machine water treatment, gets product.
Performance test:
Carry out silicon rubber pressure roll parcel (referring to our company's application for a patent for invention number 03116401.3 described method) with the resulting PFA tubular film of above embodiment, the range estimation clad surface is smooth straight, does not see the cracking phenomena that frills.
Bonding fastness detects: with blade shaft to isolating the PFA tubular film that is wrapped in outside the silicon rubber, catch it to isolate the edge with finger, peel off for 180 ° along tangent line, the bonding rubber down of film is torn as a result, film under peeling off has bonding rubbery chip, illustrates that film and rubber are bonding fine.
Last machine is printed and detected: be assembled to respectively with the good pressure dancer rools of parcel and test on the laser printer, print 10000 parts and take off pressure roll, check its no damaged vestige in surface and pickup, clad and silicon rubber do not have delamination and crackle.
Claims (6)
1, a kind of Meltability polytetrafluorethyletubular tubular film, it is the seamless tubular shaped thing that is made of bottom and surface layer, it is characterized in that:
Described bottom is formed by subbing, subbing is based on the Meltability polytetrafluorethyletubular emulsion of solid content 30～50wt%, and wherein blending has the B component that the component A that is equivalent to Meltability polytetrafluorethyletubular weight 3～15% and dry weight are equivalent to Meltability polytetrafluorethyletubular weight 3～15%; Wherein, component A is a water-soluble inorganic salt, and B component is to be selected from least a in polyvinyl alcohol, polyethylene glycol, aqueous polyacrylamide yogurt liquid, the polyvinylpyrrolidone;
Described surface layer is formed by investment precoat, investment precoat is based on the Meltability polytetrafluorethyletubular emulsion of solid content 30～50wt%, and wherein blending has the component D that the component C that is equivalent to Meltability polytetrafluorethyletubular weight 10～50% and dry weight are equivalent to Meltability polytetrafluorethyletubular weight 5～10%; Wherein, component C is perfluoroethylene-propylene or tetrafluoroethylene-ethylene copolymer, and component D is selected from least a in polyvinyl alcohol, polyethylene glycol, aqueous polyacrylamide yogurt liquid, the polyvinylpyrrolidone;
And, described bottom be densely covered with because of described water-soluble inorganic salt be rinsed the back formed micropore.
2, Meltability polytetrafluorethyletubular tubular film according to claim 1 is characterized in that described water-soluble inorganic salt is sodium chloride or potassium chloride.
3, Meltability polytetrafluorethyletubular tubular film according to claim 1 and 2, the thickness that it is characterized in that described bottom are 10～20 μ m.
4, Meltability polytetrafluorethyletubular tubular film according to claim 1 and 2, the thickness that it is characterized in that described surface layer are 15～45 μ m.
5, a kind of method for preparing Meltability polytetrafluorethyletubular tubular film as claimed in claim 1 is characterized in that may further comprise the steps:
A, barrier coating; Adopt spraying or dip-coating method, described subbing is applied on the aluminium-alloy pipe outer surface forms primer coating;
B, coating surface layer; After treating the primer coating drying, adopt spraying or dip-coating method, described investment precoat is applied to forms the surface layer coating in the primer coating;
C, plasticizing film forming; After treating surface layer coating drying, be warming up to 370 ℃～380 ℃ with 3～66 ℃/min speed in the immigration heating furnace and carry out the heating plasticizing film forming;
D, washing; To plastify after film deviates from from the aluminium-alloy pipe surface, and, make the thin nucleus of water-soluble inorganic salt of described bottom inwall be dissolved in water, promptly get the sticking seamless tubular shaped film of inwall porous, the smooth densification of outer wall after drying through the supersonic wave cleaning machine water treatment.
6, preparation method according to claim 5 is characterized in that described spraying method is electrostatic spraying, air-flow spraying or airless spraying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710160274A CN100594056C (en) | 2007-12-17 | 2007-12-17 | Meltability polytetrafluorethylene tubular film and method for preparing same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710160274A CN100594056C (en) | 2007-12-17 | 2007-12-17 | Meltability polytetrafluorethylene tubular film and method for preparing same |
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| Publication Number | Publication Date |
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| CN101254423A CN101254423A (en) | 2008-09-03 |
| CN100594056C true CN100594056C (en) | 2010-03-17 |
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| CN200710160274A Expired - Fee Related CN100594056C (en) | 2007-12-17 | 2007-12-17 | Meltability polytetrafluorethylene tubular film and method for preparing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103007788B (en) * | 2012-12-17 | 2014-11-12 | 浙江理工大学 | Preparation method of wrapped polytetrafluoroethylene ultra-micro filter tube membrane |
| CN103736399A (en) * | 2014-01-20 | 2014-04-23 | 天津工业大学 | Full-fluorine polymer hollow fibrous membrane and preparation method thereof |
| CN107088366B (en) * | 2016-11-17 | 2020-08-21 | 清华大学 | Method for preparing organic-inorganic nano composite film |
| CN107174956B (en) * | 2017-06-09 | 2019-02-01 | 天津工业大学 | The preparation method of perfluoroethylene-propylene hollow-fibre membrane with finishing coat |
| CN108854596B (en) * | 2018-07-03 | 2021-04-16 | 天津工业大学 | A kind of preparation method of continuous oil-water separation hollow fiber membrane |
| CN112742680A (en) * | 2020-12-01 | 2021-05-04 | 江苏金氟隆防腐设备有限公司 | Electrostatic spraying process for meltable polytetrafluoroethylene anticorrosive coating of chemical equipment |
| CN116535786B (en) * | 2023-04-25 | 2024-06-21 | 深圳市华之美科技有限公司 | Fixing film for printer or copier, and preparation method and application thereof |
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Assignee: Ningbo hee hee printer consumables Co., Ltd. Assignor: Chen Xianbin Contract record no.: 2010330001363 Denomination of invention: Meltability polytetrafluorethylene tubular film and method for preparing same Granted publication date: 20100317 License type: Exclusive License Open date: 20080903 Record date: 20100716 |
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