CN1112597C - K-type polarization film making process - Google Patents
K-type polarization film making process Download PDFInfo
- Publication number
- CN1112597C CN1112597C CN 00105673 CN00105673A CN1112597C CN 1112597 C CN1112597 C CN 1112597C CN 00105673 CN00105673 CN 00105673 CN 00105673 A CN00105673 A CN 00105673A CN 1112597 C CN1112597 C CN 1112597C
- Authority
- CN
- China
- Prior art keywords
- film
- polarizing coating
- type polarizing
- polyvinyl alcohol
- sandwich
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000000034 method Methods 0.000 title claims abstract description 35
- 230000008569 process Effects 0.000 title description 7
- 230000010287 polarization Effects 0.000 title description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 35
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 239000010408 film Substances 0.000 claims description 79
- 238000000576 coating method Methods 0.000 claims description 33
- 239000011248 coating agent Substances 0.000 claims description 32
- 239000002994 raw material Substances 0.000 claims description 23
- 238000006297 dehydration reaction Methods 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 11
- -1 polyethylene Polymers 0.000 claims description 9
- 230000018044 dehydration Effects 0.000 claims description 8
- 230000002378 acidificating effect Effects 0.000 claims description 7
- 239000004698 Polyethylene Substances 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 6
- 229920005862 polyol Polymers 0.000 claims description 6
- 150000003077 polyols Chemical class 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 230000009477 glass transition Effects 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 229940063013 borate ion Drugs 0.000 claims 1
- 230000033444 hydroxylation Effects 0.000 claims 1
- 238000005805 hydroxylation reaction Methods 0.000 claims 1
- 238000007654 immersion Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 230000003287 optical effect Effects 0.000 abstract description 3
- 239000002253 acid Substances 0.000 description 17
- 239000000243 solution Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 239000003595 mist Substances 0.000 description 4
- 239000003377 acid catalyst Substances 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 229920001197 polyacetylene Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000003287 bathing Methods 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 229920006217 cellulose acetate butyrate Polymers 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Images
Landscapes
- Polarising Elements (AREA)
- Laminated Bodies (AREA)
Abstract
The present invention relates to a method for manufacturing a novel optical material, namely a method for manufacturing a polarizing film in a K shape. The present invention is characterized in that two layers of polyvinyl alcohol films are made into a five-ply board type sandwich film under the protection of three layers of lining films, and then, the sandwich film is stretched. The lining films on both sides of the five-ply board type sandwich film is taken off, and two layers of useful polarizing films in a K shape are simultaneously made.
Description
The present invention relates to a kind of manufacture method of K type polarizing coating.Polarizing coating can be used for " leaching " polarized light in ordinary ray.When making LCD and liquid crystal layer combine the generation image: in photography, polarizing coating is used for reducing dazzle, reduce the direct reflection light intensity, thereby improve shooting quality, in CRT shows, can be used for reducing the lip-deep dazzle of cathode-ray tube display.Covering polarizing coating respectively on the front lamp cover of automobile He on the pilothouse window especially, the light intensity that the other side's headlight is shone in the driver eye weakens greatly, and on the road surface and light intensity all around change less, thereby can avoid the driver because of not seeing the traffic hazard that cause on the road surface.The stronger K type polarization film of tolerance to the temperature and humidity of environment has special using value in above-mentioned field.
Made the method for K type film, be to make the film of polyvinyl alcohol (PVA) pass through the strong acid mist of contact as catalyzer under higher temperature in the past, dehydration takes place, thereby form the polymkeric substance that contains the conjugated double bond section in the molecule.During the light conjugated double bond section that orientation is consistent in the film of making through this polymkeric substance, produced linear polarization.Utilize the result of the acid mist method preparation of this routine, because the unevenness that acid mist distributes causes striped and spot in the product inevitably, thereby reduce the quality of polarizing coating, the polarizing coating of producing like this is not suitable for the occasion that needs high optical accuracy especially.One object of the present invention overcomes this obstacle exactly, makes to avoid adopting acid mist when making K type polarizing coating.
The invention provides the polyvinylene film polarizer, the i.e. method of the K film class polarizer made.The film that this method will contain the linear polymer composition of hydroxyl extends to enough degree to certain direction, makes the superpolymer component molecule of film arrange along the direction of extending.Its method is whenever to press from both sides between any two with layer of polyethylene raw polyol film (the raw material film needs to soak the back in deionized water air-dry) at three layers of flexible lining form, form the board-like sandwich film of pentahapto, each acidic catalyst in addition in the centre of lining form and polyvinyl alcohol film, the raw material film is sticked on the lining form, after then this sandwich film being stretched, in the raw material film, generate the conjugated double bond chromophore after being heated to uniform temperature, promptly make K type polarizing coating.
One of advantage of this method is that material film is under the protection of lining form all the time; avoided wrinkling and give a discount, and the catalyst concentration that film touches in the process of dehydration is uniformly, thereby reduced the possibility that produces striped and spot; therefore produce in this way, yield rate is higher.Acid catalyst is added to can also makes the producer might the lower acid of working concentration on the surface of film, this preparation method may be safer, and manufacture process corrosivity is littler.
According to the above, the purpose of this invention is to provide a method of producing K type polarizing coating, this method relates to polyvinyl alcohol (PVA) raw material film and flexible lining form is built up sandwich film, wherein the acid catalyst that is dewatered on the interface of film and lining form.
Another object of the present invention provides a method of producing K type polarizing coating, will be heated to uniform temperature after the above-mentioned sandwich film stretching that has added acidic dehydration catalyst in this method.
Another object of the present invention provides a method of producing K type polarizing coating, and the raw material film has been avoided the defective that the polarizing coating made is wrinkling and give a discount all the time under the protection of the lining form of flexibility in this method.
Another object of the present invention provides a method of producing K type polarizing coating, and this method is not easy to be subjected to making in the polyvinylene process the striped that the fluctuation owing to environment causes and the problem of spot.
Other details of the present invention and advantage can be illustrated in the best details of implementing for the present invention together with accompanying drawing following.
The invention provides a new method of making the polyvinylene polarizing coating from the linear polymer raw material of hydroxyl.
During beginning, whenever press from both sides between any two with layer of polyethylene raw polyol film at three layers of flexible lining form, form the board-like sandwich film of pentahapto, each acidic catalyst in addition between lining form and polyvinyl alcohol (PVA) raw material film, the raw material film is sticked on the lining form, after then this sandwich film being stretched, be heated to 100 to 200 ℃ to generate the conjugated double bond chromophore, polyvinyl alcohol (PVA) raw material film is converted into K type polarizing coating.
Anyly can down can play the dehydration catalyst effect in higher temperature (or other suitable treatment conditions), in the section of the hydroxyl of said linear polymer molecule, form with end-product nH20 removes 2n H atom and n 0 atom, and the acid (or other reagent) that forms conjugated double bond in these high-polymer moleculars can be considered to use.Preferably use hydrochloric acid.
Some fragility of film itself of having extended, and wrinkling easily and give a discount, in sandwich film, be not easy to be subjected to above-mentioned infringement under the protection of lining form.The more important thing is, be stained with sour film after handling like this and can be transformed into K type polarizing coating.This transformation realizes in the following way: the sandwich film that has stretched, wherein added acidic catalyst is heated to sufficiently high temperature, keep the sufficiently long time, finishing the acid-catalyzed dehydration reaction of said raw material film, thereby in superpolymer, form the conjugated double bond section of extinction.
In order to explain the present invention further, please referring to Fig. 1 and 2.After Fig. 1 represents to constitute sandwich film by flexible lining form and polyvinyl alcohol (PVA) raw material film, in the gap of rete, add acidic catalyst, and then be sent to and go the process that stretches in the drawing machine, that Fig. 2 represents to send from Fig. 1 right-hand member, the sandwich film after stretching is after dewatering heating furnace, separate polarizing coating, be sent to boric acid and go the process handled in bathing.By the represented method of Fig. 1 and 2 is indicative.
As shown in Figure 1, provide 2, two spools 3 of flexible lining form to provide 4, three layers of lining form 2 of polyvinyl alcohol (PVA) raw material film whenever to press from both sides between any two, form the board-like sandwich film 5 of pentahapto with layer of polyethylene raw polyol film 4 by three spools 1.Each acidic catalyst in addition sticks on the raw material film on the lining form between lining form and polyvinyl alcohol film.The typical thickness of polyvinyl alcohol (PVA) raw material film that is adopted is 0.030～0.080mm, is preferably 0.050mm.
Can be with in a variety of materials a kind of as lining form 2.Suitable lining form such as cellulose esters (as cellulose nitrate, cellulose acetate and cellulose acetate-butyrate ester etc.); Polyester; Polycarbonate; Vinyl polymer such as polyvinyl alcohol (PVA) acrylate; Polyvinyl butyral etc., and any material of providing of form that can film.Because use that the present invention is special and needs, polyvinyl butyral and polyester are useful especially materials.The thickness of lining form depends on specific application.Usually, from the viewpoint of the manufacturing process, but used thickness is about the material of 0.020mm to 0.50mm.
As shown in Figure 1, one deck lining form 2 and two layers of polyethylene raw polyol film 4 at first are incorporated into together in nip rolls 6 and 7 clips of forming, and have at this moment formed two turnofves in the middle of them.According to the present invention, from the container 8 of acid solution,, assemble in formed here two ditches of acid to these two turnofves acid solution 9 that drips, be deployed on the interface of 4 of whole lining form 2 and polyvinyl alcohol (PVA) raw material films.Three layers sandwich film 10 has been synthesized in lining form 2 and polyvinyl alcohol (PVA) raw material film 4 and added acid.
Similarly, when other two-layer lining form 2 and above-mentioned sandwich film 10 are incorporated into a time-out in nip rolls 11 and 12 clips of forming, two turnofves have also been formed in the middle of their.According to the present invention, to this turnoff acid solution 9 that drips, acid is here assembled from the container 8 of acid solution, and is deployed on the interface of 4 of whole lining form 2 and polyvinyl alcohol (PVA) raw material films.Three layers of lining form 2 and two layers of polyethylene raw polyol film 4 add that added acid synthesized sandwich film 5 altogether.Wherein added acid provides next conversion procedure needed catalytic action.
Typically,, should in whole manufacturing process, keep the flow velocity and the flow of certain acid solution, enough form and keep the acid solution 9 in four ditches that cover whole nip rolls length continuously in order to guarantee evenly to spread out.The inhomogeneity factor of other influence coatings also should take in.
As shown in Figure 1, stretching is (preferably being heated to more than the glass transition temperature of superpolymer raw material) of carrying out in the heat generator 18 that has heating element 17.Can utilize the difference of rotating speed between nip rolls 15 and 16 to cause that the sandwich film of transmission is subjected to corresponding tension force between them, with its stretching.
Pentahapto plate-type thin film after the stretching is sent to and has heating element 19, nip rolls 20 and fast in the heat generator 22 of nip rolls 21 at a slow speed, and polyvinyl alcohol film through the effect generation dehydration of acid catalyst, generates polarizing coating 23 under heating condition.The optical property of finished product polarizing coating can be used the temperature in the reburner, and the time that film is heated is controlled.The polarizer of the production high grade of transparency if desired, transforming furnace temperature should be lower, and production transparency if desired is relatively low, the polarizer that the blocking rate is higher should adopt higher conversion furnace temperature.
After peeling off, to extend once more polarizing coating 23 and the inside and outside lining form that process transforms.As shown in Figure 2, extending step can (but be not must) carry out in boric acid bath 24.Handle with the aqueous solution of boric acid and borax therein and contain the certain ethenylidene-ethenol copolymer of molecular orientation.Adopt aforesaid being used for that the similar manner that polyvinyl alcohol (PVA) raw material film 4 extends is extended: to adopt at a high speed and nip rolls 25 and 26 low speed.The polarizing coating of Sheng Chenging is rolled on the spool 27 at last, becomes finished product.
Claims (6)
1, a kind of method from polyvinyl alcohol polymer thin film fabrication K type polarizing coating is characterized in that:
(a) immersion of raw material film
Polyvinyl alcohol (PVA) raw material film is soaked back air-dry in deionized water;
(b) the sandwich film of formation lining form and raw material film
Whenever press from both sides between any two with layer of polyethylene raw polyol film at three layers of lining form,, add acidic dehydration catalyst these films are glued together, form the board-like sandwich film of pentahapto at the interface of lining form and polyvinyl alcohol film;
(c) stretching of sandwich film
Sandwich film is stretched more than the glass transition temperature of raw material film;
(d) make K type polarizing coating
Throw off the outermost village film of sandwich film, with molecular orientation polyvinyl alcohol film under the condition that enough causes the hydroxylation linear polymer generation catalytic and dehydration reaction in the film, handle, thereby in said superpolymer, produce light absorbing conjugated double bond section, thereby make K type polarizing coating;
(e) method of described making K type polarizing coating is characterized by two layers of stretch orientation film that will be clipped in three layers of lining form and heats the sufficiently long time under sufficiently high temperature, thereby causes said catalytic and dehydration reaction;
(f) method of described making K type polarizing coating, the heating-up temperature that it is characterized in that dehydration is greatly between 100 ℃ to 200 ℃.
2, by the method for the described making of claim 1 K type polarizing coating, it is characterized by the method that adds dehydration catalyst is the turnoff that the interface constituted that said catalyst drops is added to polyvinyl alcohol film and lining form.
3,, it is characterized by sandwich film and be stretched to about 2.0 times to 5.0 times of former length to certain orientation by the method for the described making of claim 1 K type polarizing coating.
4,, it is characterized by sandwich film and stretched by the different nip rolls of rotating speed or extend by the method for the described making of claim 3 K type polarizing coating.
5, by the described method of making K type polarizing coating of claim 1, it is characterized by by further extension step, stood the said film of said catalytic and dehydration reaction therein, further extended 10% to 160%, so that extend at least 4.8 times of former length altogether to certain orientation.
6, by the method for the described making of claim 1 K type polarizing coating, the polyvinyl alcohol film that it is characterized by stretching further extends in containing the solution of borate ion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00105673 CN1112597C (en) | 2000-04-17 | 2000-04-17 | K-type polarization film making process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00105673 CN1112597C (en) | 2000-04-17 | 2000-04-17 | K-type polarization film making process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1318759A CN1318759A (en) | 2001-10-24 |
| CN1112597C true CN1112597C (en) | 2003-06-25 |
Family
ID=4577867
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00105673 Expired - Fee Related CN1112597C (en) | 2000-04-17 | 2000-04-17 | K-type polarization film making process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1112597C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6949207B2 (en) * | 2002-04-04 | 2005-09-27 | 3M Innovative Properties Company | K-type polarizer and preparation thereof |
| US7087194B2 (en) * | 2002-04-04 | 2006-08-08 | 3M Innovative Properties Company | K-type polarizer and preparation thereof |
| US20050073065A1 (en) * | 2002-04-06 | 2005-04-07 | Mack Jon M. | Process for making an intrinsic polarizer |
| JP4137550B2 (en) * | 2002-08-08 | 2008-08-20 | 日東電工株式会社 | Manufacturing method of polarizer and wet stretching apparatus used therefor |
| JP4861968B2 (en) * | 2007-11-30 | 2012-01-25 | 住友化学株式会社 | Manufacturing method of polarizing plate |
| JP5162695B2 (en) * | 2010-09-09 | 2013-03-13 | 日東電工株式会社 | Manufacturing method of thin polarizing film |
| CN113441017A (en) * | 2021-07-02 | 2021-09-28 | 北京碧水源分离膜科技有限公司 | Process for preparing polyolefin-based reverse osmosis membrane |
-
2000
- 2000-04-17 CN CN 00105673 patent/CN1112597C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1318759A (en) | 2001-10-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5973834A (en) | Method for the manufacture of a light-polarizing polyvinylene sheet | |
| TWI582473B (en) | Polarizing film and its manufacturing method and polarizing plate | |
| TWI344891B (en) | ||
| KR100241971B1 (en) | High-efficiency K-Sheet Polarizers and Manufacturing Method Thereof | |
| KR102400929B1 (en) | Polyvinyl alcohol-based film and manufacturing method thereof, and polarizing film using the polyvinyl alcohol-based film | |
| CN1112597C (en) | K-type polarization film making process | |
| KR20190043624A (en) | Polarizer and liquid crystal display | |
| US20250001713A1 (en) | Method and system for producing a gradient polar film | |
| KR20180074673A (en) | POLYVINYLLLICOHOLE FILM, POLARIZING FILM, POLARIZING PLATE, AND METHOD FOR PRODUCING POLYVINYLLOHOLYE-BASED FILM | |
| KR20190139854A (en) | Polyvinyl alcohol-based film, polarizing film and polarizing plate, and polyvinyl alcohol-based film production method | |
| CN110235031B (en) | Film roll and method for producing same | |
| TW201213864A (en) | Three-dimensional image display device | |
| CN104614791B (en) | Birghtness enhancement film with pyramid structure and manufacture method thereof | |
| CN118732122A (en) | Polarizer and polarizing plate | |
| JP2006072315A (en) | Polarization plate with antireflection function, process for producing the same and image display unit utilizing the same | |
| CN116449599B (en) | A low-side-view haze electrically controlled dimming film and its preparation method | |
| JP2009092974A (en) | Anti-glare film | |
| JP7025166B2 (en) | Polarizing plate, its manufacturing method, and display device | |
| WO2018070131A1 (en) | Polarizing plate and liquid crystal display device | |
| JP2011186287A (en) | Antiglare film and method of manufacturing the same | |
| JP2025006373A (en) | Polarizing plate, manufacturing method thereof, and display device | |
| KR100953945B1 (en) | Composite film manufacturing method for flat panel display device | |
| KR101536087B1 (en) | Rubbing roller and orientation film manufacturing method | |
| KR100705435B1 (en) | Manufacturing method of polarizing plate with protective layer laminated and polarizing plate manufactured by the method | |
| TW202446856A (en) | Polyvinyl alcohol film, polarizing film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20030625 Termination date: 20100417 |