CN1844206A - Day/night light conversion agricultural film and preparation method thereof - Google Patents
Day/night light conversion agricultural film and preparation method thereof Download PDFInfo
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- CN1844206A CN1844206A CN 200610075947 CN200610075947A CN1844206A CN 1844206 A CN1844206 A CN 1844206A CN 200610075947 CN200610075947 CN 200610075947 CN 200610075947 A CN200610075947 A CN 200610075947A CN 1844206 A CN1844206 A CN 1844206A
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Abstract
The invention relates to an agricultural thin film composition and method for preparation, which comprises 0.05-1% of inorganic fluorescent powder, 0.1-0.3% of organic light stabilizing agent, and 98.7-99.85% of organic polymer, wherein the ratio of the blue light fluorescent powder and red light fluorescent powder in the inorganic fluorescent powder can be 1:3-2:1.
Description
Technical field
The present invention relates to a kind of polymer thin film field, refer to that especially a kind of be used in hotbed, greenhouse and the greenhouse covers rice shoot and seedling to avoid by the day/night light conversion agricultural film composition and method of making the same of weather effect.
Background technology
In the general thin-film material of a large amount of uses, also use heat-light sensation thin-film material in a large number now, wherein part can promote to revise the infrared long-wave radiation of warm light of the sun and the reflection of hotbed soil.Known agricultural film, on its polymeric matrix such as, those light conversion additives that distribute on polyethylene or the polyvinyl chloride, such as LaOCl:Eu, Y
2O
2S:Eu, GaOF:Eu etc. are by Eu
+ 3Catalytic oxy-compound.The solar ultraviolet optical radiation can change orange-red light into after to the film, wavelength is that such agricultural film of 595-640nm (please refer to No. 98121668.04 case of Russ P application) has numerous advantages, but two major defects are arranged simultaneously: 1. lack according to K.A Temiriazev find necessary second time of spectrum peak (=470nm) do not have for 2. nights luminously fully, and sun plant needs long sunshine.
At first shortcoming of above-mentioned prior art agricultural film, No. 96212779.04 case of Russ P application attempts to solve this shortcoming, and it recommends to adopt the blueness and the red fluorescence powder of two kinds of standards.But this patent does not solve above-mentioned second deficiency that known agricultural film exists equally, because need prolong the sunshine duration for the agricultural crops seedling, such as being longer than 20 hours.
Preparation sees through and add steady persistence sulfenyl fluorescent material trial (please refer to Russ P No. 2127511) in polymeric film.This optical conversion film scheme is used as the prototype of this case.Confirm that in this patent adding ZnS:Cu or CaS:Bi type fluorescent material can be found quite long twilight sunset in film, can continue 10 minutes at night.Indication covering material-prototype hardware severally can prolong the plant illumination time although have, but also has serial major defect simultaneously: 1. the phosphor persistence brightness of the employing in the prototype is not enough; 2. the sulfenyl fluorescent material environmental stability that adds film is not enough, and can fade fast; 3. because the difficulty of the extremely low thermostability production covering material extrusion molding of sulfenyl fluorescent material is very big.
Certainly, this invention scheme is only used for patent application, because visible time of persistence of the length of this fluorescent material is less than 10 minutes, is not enough to reach apparent agro-ecology effect.Really, still exist a fly in the ointment less than 1% this time of persistence for 1200 minutes required sunshine durations (20 hours).
Summary of the invention
For solving the shortcoming of above-mentioned prior art, main purpose of the present invention is that a kind of luminous round the clock light conversion agricultural film and preparation method thereof is provided, and fixed illumination is promptly arranged between photoperiod and very high optical storage level is arranged, can be luminous during night.
For reaching above-mentioned purpose, the invention provides a kind of day/night light conversion agricultural film composition, said composition comprises the 0.05-1wt% inorganic fluorescent powder; The organic photostabilizer of 0.1-0.3wt%, the 98.7%-99.85wt% organic polymer, wherein inorganic fluorescent powder comprises that the two ratio of blue light fluorescent powder and red light fluorescent powder can be 1: 3-2: 1.
Composition of the present invention can be chosen wantonly in addition and comprise 0.01-5wt%, and the oxidation inhibitor of preferred 0.1-1wt% and ultraviolet lower agent, 1-15wt%, preferred 5-10wt% thermal resistance decomposed substance.
The present invention provides a kind of preparation method of day/night light conversion agricultural film in addition, and it comprises the following step: see through material inlet adds blue light fluorescent powder and red light fluorescent powder in the high pressure polyethylene particle material additive; The material that randomly in the polyethylene material inlet, adds the thermal resistance decomposition in addition; Add organic photostabilizer; All components are mixed, obtain the super enriched material of polyethylene particle homogeneous, evenly soak and boil with liquid state; And said composition sent in the extrusion machine, be heated to proper temperature, with the agricultural film product of preparation homogeneous.
For reaching above-mentioned purpose, the invention provides a kind of day/night light conversion agricultural film, wherein two kinds of inorganic oxygen-containing fluorescent material in the polymeric film component, have been added in addition (promptly, blue light and red light fluorescent powder), this fluorescent material has the steady persistence of the 10-50% in daytime, and two not cross one another spectrum luminous zones are arranged, and be retained in reservation indication spectral signature under the steady persistence state.
Embodiment
Therefore, the present invention relates to a kind of day/night light conversion agricultural film composition, said composition comprises the 0.05-1wt% inorganic fluorescent powder; The organic photostabilizer of 0.1-0.3wt%, the 98.7%-99.85wt% organic polymer, wherein inorganic fluorescent powder comprises that the two ratio of blue light fluorescent powder and red light fluorescent powder can be 1: 3-2: 1.
Composition of the present invention can further preferably include 0.01-5wt% in addition, and the oxidation inhibitor of preferred 0.1-1wt% and ultraviolet lower agent, 1-15wt%, preferred 5-10wt% thermal resistance decomposed substance.
Light conversion agricultural film of the present invention adds two kinds of inorganic fluorescent powders in its component, their spectrum luminous positions are had any different Just because of this, and be maximum sunlight time 10%-50% (north latitude 50 on June 22 ") time of persistence that also has them.In the invention working process, the contriver determines that traditional CaS:Bi or ZnS:Ag.Ga base long persistence blue light fluorescent powder are receiving to have very low radiation stability under the situation that solar ultraviolet periodically acts on.In addition, these material require wavelength excite at the long wave of 340-400nm, and promptly this interval excites the needed of red light fluorescent powder just.So the inventor proposes to adopt simultaneously blue light and red light fluorescent powder in film composite.
Blue light of the present invention and red light fluorescent powder can adopt those that sell on the market.
As the basic fluorescence composition of the present invention, preferably adopt two kinds to contain oxygen fluorescent material, blue light fluorescent powder (SrOX)
2.5Al
2O
3: Eu
+ 2Nd (wherein X is that Cl is or/and F) and red light fluorescent powder Y
2-x-yEu
xSr
yMe
+ 4O
4S (Me is Zn for x=0.01～0.1 wherein, y=0.01～0.05, Si, among the Ti one or more).Eu with accordingly+2 ionic speciess exist, send the regional sky blue coloured light of spectrum, and+the interval red light of 3 ion fluorescence powder luminous spectrums, second kind of activator adopts+4 Nd, Ce, Tb, Pr, Zr, Hf, Ge, recommending the characteristics that showing of fluorescent material is that be the 10-50% of hours of darkness in one day the time of persistence of the fluorescent material of every kind of recommendation.
Organic polymer of the present invention is preferably high-pressure polyethylene, and more preferably density is 0.92-0.94, the high-pressure polyethylene of molecular chain 2400-3200 carbosilane unit.
Organic stabilizer of the present invention can be commonly used those in this area, and for example nitrogenous or phosphorated photostabilizer for example can be the photostabilizer of quaternary amine (quaternary ammonium) form.
It can be commonly used those in this area that oxidation inhibitor of the present invention and ultraviolet lower agent.
Thermal resistance decomposed substance of the present invention can be a high-pressure polyethylene 1020.
The present invention relates to the preparation method of day/night light conversion agricultural film in addition, comprises the following steps: to see through material inlet adds blue light fluorescent powder and red light fluorescent powder in the high pressure polyethylene particle material additive (step 1); Randomly in the polyethylene material inlet, add thermal resistance decomposed substance (step 2) in addition; Photostabilizer (the step 3) that adds the quaternary amine form; Optional input oxidation inhibitor and ultraviolet lower agent, and all components are mixed, and obtain the super enriched material of polyethylene particle homogeneous, evenly soak and boil (step 4) with liquid state; And said composition sent in the extrusion machine, be heated to proper temperature, with the agricultural film product (step 5) of preparation homogeneous.
Embodiment
The preparation of blue-fluorescence powder
1, at first weighing the fully mixed back of following former material puts in the crucible.
SrCO
3：73.8g，NH
4Cl：26.2g，Al
2O
3：20.4g，Eu
2O
3：1.8g，Nd
2O
3：0.9g
2, mixed former material crucible will be housed fully and put into the high temperature baking box and heat, temperature rise rate is 5 ℃/min, and temperature rises to 1200 ℃.
3, keep temperature in the high temperature baking box, to charge into nitrogen after 1200 ℃ of two each hour, kept again one hour.
4, charge into nitrogen hydrogen mixed air afterwards again in the high temperature baking box, mixing ratio is N
2: H
2=95: 5, kept again three hours.
5, charge in the high temperature baking box and begin cooling under the situation of nitrogen hydrogen mixed air, rate of temperature fall is 5 ℃/min, and temperature is reduced to 800 ℃.
6, change after the high temperature oven temperature is reduced to 800 ℃ and charge into nitrogen, rate of temperature fall is constant, and temperature is reduced to 150 ℃.
7, opening chamber door after the high temperature oven temperature is reduced to 150 ℃ takes out crucible.
8, the finished product in the sweet pot is taken out, be the finished product of blue-fluorescence powder after careful the grinding.
The preparation of red fluorescent powder
1, at first weighing the fully mixed back of following former material puts in the crucible.
Y
2O
3：54.5g，SrCO
3：0.37g，Eu
2O
3：2.2g，TiO
2：20g，S：8g
2, mixed former material crucible will be housed fully and put into the high temperature baking box and heat, temperature rise rate is 5 ℃/min, and temperature rises to 1200 ℃.
3, keep temperature in the high temperature baking box, to charge into nitrogen after 1200 ℃ of two each hour, kept again one hour.
4, charge into nitrogen hydrogen mixed air afterwards again in the high temperature baking box, mixing ratio is N
2: H
2=95: 5, kept again three hours.
5, charge in the high temperature baking box and begin cooling under the situation of nitrogen hydrogen mixed air, rate of temperature fall is 5 ℃/min, and temperature is reduced to 800 ℃.
6, change after the high temperature oven temperature is reduced to 800 ℃ and charge into nitrogen, rate of temperature fall is constant, and temperature is reduced to 150 ℃.
7, opening chamber door after the high temperature oven temperature is reduced to 150 ℃ takes out crucible.
8, the finished product in the sweet pot is taken out, be the finished product of red fluorescent powder after careful the grinding.
The preparation of film
In step 1, see through material inlet adds blue light fluorescent powder and red light fluorescent powder in the high pressure polyethylene particle material additive; Wherein, the quantity of high pressure polyethylene particle is that 1000kg and its model are the 158-03 model, and this blue light fluorescent powder is (SrOX)
2.5Al
2O
3: Eu
+ 2Nd and its quantity are 1kg; And this red light fluorescent powder is Y
2-x-yEu
xSr
yMe
+ 4O
4S and its quantity are 2kg.
In step 2, in the polyethylene material inlet, add the thermal resistance decomposed substance in addition; Wherein, the material label of this thermal resistance decomposition is a high-pressure polyethylene 1020, and the throwing ratio of putting of itself and polyethylene quality is 1: 10.
In step 3, add the photostabilizer of 2kg quaternary amine form; Wherein, this photostabilizer is the photostabilizer of quaternary amine form, and its industry name is called tinuvin-622, and its molecular weight is at the 1000-2000 carbosilane unit.
In step 4, add 2kg oxidation inhibitor and ultraviolet and lower agent, and obtain the super enriched material of polyethylene particle homogeneous and evenly soak and boil with liquid state; Wherein, this super enriched material evenly soaks with liquid state and boils being higher than under 220 ℃ the temperature; This proper temperature is 185-195 ℃.
In step 5, the mixture of high-pressure polyethylene, irganox photostabilizer is sent in the extrusion machine, be heated to proper temperature, with the agricultural film product of preparation homogeneous; Wherein, this proper temperature is 185-195 ℃; And this agricultural film is 1.5 in the intensity of red light district and blue light region: 2-1: 2, and its after-glow brightness is 20 milli candle light/m after exposing in the sun 1 hour
2, then drop to 2 milli candle light/m after 4 hours
2
It lies in and has added two kinds of inorganic oxygen-containing fluorescent material in the polymeric film component in addition according to the prepared agricultural film of aforesaid method, this fluorescent material has the steady persistence of the 10-50% in daytime, and two not cross one another spectrum luminous zones are arranged, and be retained in reservation indication spectral signature under the steady persistence state.
Wherein, these two kinds of inorganic oxygen-containing fluorescent material are respectively blue light fluorescent powder and red light fluorescent powder, and wherein this blue light fluorescent powder is (SrOX)
2.5Al
2O
3: Eu
+ 2Nd; And this red light fluorescent powder is Y
2-x-yEu
xSr
yMe
+ 4O
4S.
This spectrum luminous zone is that this sky blue spectrum luminous zone is 450-470nm between sky blue and orange red color area, and this orange red spectrum luminous zone is 588-626nm, and these two districts are intermittently cut apart by the spectrum of 510-560nm.
Its principle of work of the present invention's agricultural film is as follows: the content with fluorescent material in the polymeric components is the 0.05-1% of quality.The film that is deployed under the sunlight is subjected to irradiation of sunlight, and short wave ultraviolet light, visible light and heavy dose of ir radiation are arranged in the sunlight.The fluorescence response of spontaneous generation blue light conversion factor and ruddiness conversion factor under the ultraviolet radiation effect, and form sun visible light.Along with the luminous naturally carrier that takes place to exist with electronics and fine porosity form in fluorescent material is accumulated, accumulated value is up to 10 simultaneously
20～10
21/ cm
3
Cumulative electronics and fine porosity form big light storage unit, can not interrupt during 1-10 hour, promptly can reach circadian 10-50%.This luminous intensity is very strong, and the luminosity of the brightness convergence circle moon is enough for vegetative organ and the morphological system of strengthening sun plant promptly.In the greenhouse, test to have confirmed the present invention's hypothesis with two kinds of polymkeric substance coating films that contain oxygen optical storage fluorescent material that the present invention added.
Wherein, the best base material of preparation polymeric film is: high-pressure polyethylene, density are 0.92-0.94, molecular chain 2400-3200 carbosilane unit.This material is according to Russian national standard production, and merchant's label is: Russian high-pressure polyethylene 153-03-20 or 158-03-20.
This red light district and blue light region intensity are 1.5: 2-1: 2.The 1 hour after-glow brightness that exposes in the sun is 20 milli candle light/m
2, drop to 2 milli candle light/m after 4 hours
2
The prepared agricultural film mass parameter of preparation method according to the present invention is as follows:
Table-1: the physics of agricultural film and optical tech parameter
| Project | Plastic sheeting for farm use component % | Buckling strength kg/cm 2 | Relative brightness, % | The storage luminance brightness (candle light/Mi Pingfang) | ||
| High-pressure polyethylene | Blue light fluorescent powder+red fluorescence powder content | Photostabilizer content | ||||
| 1 | 99.4 | 0.1+0.1 | 0.4 | 16.0~15.2 | 100 | 10 |
| 2 | 99.3 | 0.2+0.1 | 0.4 | 15.0~14.4 | 120 | 28 |
| 3 | 99.0 | 0.25+0.25 | 0.5 | 15.2~14.8 | 180 | 45 |
| 4 | 99.5 | 0.13+0.12 | 0.25 | 17.0~15.6 | 110 | 18 |
| 5 | 99.5 | 0,2+0.1 | 0.2 | 17.2~16.2 | 128 | 35 |
| 6 | 99.75 | 0 | 0.25 | 16.7~14.2 | 78 | 0 |
Describe the result that the agricultural film coverture is tested in advance that is prepared in detail.At first, the agricultural film of preparation has the luminous energy storage effect of not mentioning in the former document under the sunlight effect.Really, Standard Thin membrane sample (6) sees through the interpolation red light fluorescent powder and makes, and has the luminance brightness of 78 unit levels, but can not obtain luminous energy.Sample strength physical mechanical pointer is good.The second, promote the content of two kinds of fluorescent material in film, the luminous energy store content can promote.
The mass unit of optical storage fluorescent material reaches the 0.5 storage luminous energy value with maximum and reaches 45 units in the sample (3).The characteristics of this sample are that initial light emitting indicator is very high, reach 180 units.Sample (1) is in the original intensity value during up to 100 units, storage luminous energy value is not high, this general with contain a large amount of photostabilizers and not only absorb solar ultraviolet light, simultaneously also absorb purplish blue light, cause taken in excess (at the very effective effect optical storage of the light of hyacinthine sub-band fluorescent material) sunlight.Must be pointed out that a bit that is exactly an optical storage fluorescent powder grain diameter d 15=15-20 micron, can't reduce the physical mechanical parameter of film, this is the conclusion that draws from its strength property, with (6) sample comparison in characteristic do not have any reduction.
The agricultural film sample of listing in all tables-1 has all prepared a great deal of nature test that is used to carry out.Naturally test to have in the private little hotbed of villa and carry out, also have in the Moscow State University Botanical gardens and carry out.Test hotbed area covers 20m
2, the non-light conversion agricultural film of hotbed one skew back face coverage criteria, opposite side covers the optical storage film.Article two, the solar azimuth of diaphragm is identical (from the southeast to the northeastward).Plantation 6 row sun plants in the hotbed (the loose De Depressive gold of 2 row is fragrant, 2 row radish, 2 row wild cabbages).
Onion, seed and seedling were sowed in year on February 28th, 2003.Weekly hotbed is once checked.Radish under the optical storage film was harvested for the first time on May 9th, 2003, and use the standard film the first time harvest the date on May 15th, 2003.Depressive gold is fragrant to have sent bright-coloured seedling after week, and the gold of the Depressive under standard film perfume just occurred on May 15th, 2003, and the quantitative proportion of the flower under two kinds of different films is 1.32: 1.Wild cabbage under the optical storage film began to harvest at July 28, and the wild cabbage under general thin postpones 12 days than the phase of harvesting of the wild cabbage under the optical storage film, yields poorly 23%.
Test naturally to the optical storage film has been carried out 2 years.Test-results sees Table-2.
The optical tech parameter of table-2 optical storage films in Natural Environmental Test changes
| Date | Sample 3 brightness, % storage, % | Sample 4 brightness, % storage, % |
| 28.02.2001 | 100 100 | 100 100 |
| 28.03.2001 | 98 91 | 96 95 |
| 28.04.2002 | 99 98 | 95 93 |
| 28.05.2002 | 97 97 | 95 94 |
| 28.08.2002 | 94 95 | 92 93 |
| 28.09.2002 | 93 94 | 92 92 |
| 23.02.2003 | 93 91 | 90 90 |
| 23.03.2003 | 93 92 | 91 91 |
| 24.04.2003 | 92 91 | 90 88 |
| 25.05.2003 | 92 90 | 88 87 |
| 15.09.2003 | 91 90 | 89 85 |
Reach a conclusion from the natural testing data that carry out two seasons, two kinds of film samples have not only kept original intensity but also kept the optical storage value.The very fast reduction of sample (4) brightness needs further research, can point out here, and adds photostabilizer concentration in the thin-film material component and has very significantly and get in touch.Sample (4) and sample (3) brightness Comparatively speaking reduce fast and are to be closely related with the concentration that adds the optical stabilization agent that exists with quaternary amido form in the agricultural film.
Can clearly learn like this, in hotbed, use the optical storage film can play obvious effects: the output that promotes farm crop.The agricultural film of recommending has satisfactory stability to solar radiation, and its characteristic is basic in two agriculture seasons not to be changed.
In sum, luminous round the clock light conversion agricultural film of the present invention, it has fixed illumination and very high optical storage level is arranged between photoperiod, advantage such as can be during night luminous, therefore, can improve the shortcoming of prior art agricultural film and preparation method thereof really.
Though for example understand the present invention according to preferred embodiment; right its is not in order to limit the present invention; those of ordinary skills can make many variations and retouching without departing from the spirit and scope of the invention, so protection scope of the present invention should limit according to claims.
Claims (12)
1, a kind of day/night light conversion agricultural film composition, said composition comprises the 0.05-1wt% inorganic fluorescent powder; The organic photostabilizer of 0.1-0.3wt%, the 98.7%-99.85wt% organic polymer, wherein inorganic fluorescent powder comprises that the two ratio of blue light fluorescent powder and red light fluorescent powder is 1: 3-2: 1.
2, composition according to claim 1 further comprises 0.01-5wt%, and the oxidation inhibitor of preferred 0.1-1wt% and ultraviolet lower agent, 1-15wt%, preferred 5-10wt% thermal resistance decomposed substance.
3, composition according to claim 1 and 2, wherein organic polymer is a high-pressure polyethylene.
4, according to each described composition of claim 1-3, wherein this blue light fluorescent powder is (SrOX)
2.5Al
2O
3: Eu
+ 2Nd, wherein X is that Cl is or/and F; And this red light fluorescent powder is Y
2-x-yEu
xSr
yMe
+ 4O
4S, x=0.01～0.1 wherein, y=0.01～0.05, Me is Zn, Si, one or more among the Ti.
5, according to each described composition of claim 1-4, wherein organic photostabilizer is the photostabilizer of quaternary amine form.
6, according to each described composition of claim 1-5, wherein organic polymer is that density is 0.92-0.94, the high-pressure polyethylene of molecular chain 2400-3200 carbosilane unit.
7, by the agricultural film of the preparation of compositions of above each claim, it is characterized in that the intensity at red light district and blue light region is 1.5: 2-1: 2, and its after-glow brightness is 20 milli candle light/m after exposing in the sun 1 hour
2, then drop to 2 milli candle light/m after 4 hours
2
8, agricultural film according to claim 7 is characterized in that wherein this spectrum luminous zone is between sky blue and orange red color area.
9, agricultural film according to claim 7 is characterized in that this sky blue spectrum luminous zone is 450-470nm, and this orange red spectrum luminous zone is 588-626nm, and these two districts are intermittently cut apart by the spectrum of 510-560nm.
10, by the method for each described preparation of compositions day/night light conversion agricultural film of claim 1-7, it comprises the following step:
See through material inlet adds blue light fluorescent powder and red light fluorescent powder in the high pressure polyethylene particle material additive;
The material that randomly in the polyethylene material inlet, adds the thermal resistance decomposition in addition;
The photostabilizer that adds the quaternary amine form;
Optional adding oxidation inhibitor and ultraviolet lower agent, and all components is mixed, and obtain the super enriched material of polyethylene particle homogeneous, evenly soak and boil with liquid state; And
Said composition is sent in the extrusion machine, be heated to proper temperature, with the agricultural film product of preparation homogeneous.
11, blue light fluorescent powder, its chemical formula are (SrOX)
2.5Al
2O
3: Eu
+ 2Nd, wherein X is that Cl is or/and F.
12, red light fluorescent powder, its chemical formula are Y
2-x-yEu
xSr
yMe
+ 4O
4S, x=0.01～0.1 wherein, y=0.01～0.05, Me is Zn, Si, one or more among the Ti.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100759474A CN100447183C (en) | 2006-04-25 | 2006-04-25 | Day/night light conversion agricultural film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100759474A CN100447183C (en) | 2006-04-25 | 2006-04-25 | Day/night light conversion agricultural film and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1844206A true CN1844206A (en) | 2006-10-11 |
| CN100447183C CN100447183C (en) | 2008-12-31 |
Family
ID=37063176
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|---|---|---|---|
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Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1052493C (en) * | 1994-11-07 | 2000-05-17 | 青岛新桑达经济技术开发有限公司 | Light converting film |
| CN1187428C (en) * | 2001-02-12 | 2005-02-02 | 湖南师范大学 | Single-base dual-energy light-transforming agent and its preparing prcess and application |
| CN1709033A (en) * | 2005-07-08 | 2005-12-21 | 彭子飞 | Light-converting luminous high-light-energy weather-resistant agricultural film and its manufacturing method |
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