CN108239398B - Method for producing optical element - Google Patents
Method for producing optical element Download PDFInfo
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- CN108239398B CN108239398B CN201611203763.1A CN201611203763A CN108239398B CN 108239398 B CN108239398 B CN 108239398B CN 201611203763 A CN201611203763 A CN 201611203763A CN 108239398 B CN108239398 B CN 108239398B
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- carbon black
- optical element
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention provides a plastic composition and a preparation method thereof. The plastic composition comprises about 98.5-99.995 parts by weight of base material powder, about 0.005-1 part by weight of carbon black powder and about 0.00025-0.5 part by weight of solid dispersing agent. The substrate powder comprises polyetherimide. The particle size of the carbon black powder is less than or equal to about 500 nanometers. Also provided is an optical element manufactured using the plastic composition. The optical element prepared by the invention has extremely low black spot generation rate and excellent optical property.
Description
Technical Field
The present invention relates to a composition, a method for preparing the same, and applications thereof, and more particularly, to a plastic composition, a method for preparing the same, and an optical element using the same.
Background
Since the optical device industry has been developed for a long time, it is mature in terms of theory and production technology, and only the issues of quality, yield and price, and specifications of various application products remain. In optical fiber communication systems, optical fiber connectors are essential components for connecting various devices, and are the most widely used optical fiber components at present. Therefore, attention has been paid to how to rapidly mass-produce optical fiber connectors with good quality and high yield, which meet various product specifications.
Disclosure of Invention
In view of the above, the present invention provides a plastic composition, a method for preparing the same, and an optical element using the same. The preparation method of the invention is easy, and can be used for quickly producing optical elements with good quality and high yield in mass production and meeting the requirements of various product specifications.
The invention provides a plastic composition, which comprises about 98.5-99.995 parts by weight of base material powder, about 0.005-1 part by weight of carbon black powder and about 0.00025-0.5 part by weight of solid dispersing agent. The substrate powder includes Polyetherimide (PEI). The particle size of the carbon black powder is less than or equal to about 500 nanometers.
In an embodiment of the invention, the particle size of the base material powder is not greater than 300 μm.
In an embodiment of the invention, the solid dispersant includes a paraffin dispersant.
In an embodiment of the present invention, the surface area of the carbon black powder is greater than or equal to about 50m2/g。
The invention also provides an optical element which is made by using the plastic composition.
In an embodiment of the invention, a black spot generation rate of the optical element is about 10% or less.
In an embodiment of the invention, the optical attenuation of the optical element is in a range of about-0.5 to-10.0.
The invention also provides a preparation method of the plastic composition, which comprises the following steps. And (3) carrying out liquid grinding on the carbon black powder. After the liquid grinding step, a drying step is performed. After the drying step, a solid-state grinding step is performed on the carbon black powder to form refined carbon black powder, wherein the grain diameter of the refined carbon black powder is less than 500 nanometers. Mixing 0.005-1 weight part of the refined carbon black powder, 0.00025-0.5 weight part of a solid dispersant and 98.5-99.995 weight parts of a base material powder, and performing a dispersion step to form the plastic composition.
In an embodiment of the invention, the substrate powder includes Polyetherimide (PEI).
In an embodiment of the invention, the particle size of the base material powder is less than or equal to about 300 μm.
In an embodiment of the invention, the solid dispersant includes a paraffin dispersant.
In an embodiment of the present invention, the surface area of the refined carbon black powder is greater than or equal to about 50m2/g。
In an embodiment of the invention, the liquid polishing step includes: mixing about 85-98 parts by weight of water, about 1-10 parts by weight of the carbon black powder and about 1-5 parts by weight of a liquid dispersant; and grinding the mixture for about 0.5 to 4 hours at a rotational speed of about 250 to 350rpm by a planetary ball mill.
In one embodiment of the present invention, the solid-state milling step comprises milling with a high-speed mill at a speed of about 2,000rpm or more for about 0.03 hours or more.
In an embodiment of the present invention, the method further comprises feeding the plastic composition to an extruder for melt-kneading, wherein the kneading temperature is in a range of 290 ℃ to 350 ℃.
Based on the above, the method of the present invention can easily prepare optical grade materials with different specifications of light transmittance (transmittance) and different specifications of optical attenuation values, so as to rapidly produce optical elements with good quality and high yield, and which can meet various product specifications. In addition, the optical element prepared by the invention has extremely low black spot generation rate and excellent optical properties.
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below.
Drawings
FIG. 1 is a flow chart illustrating a method of preparing a plastic composition in accordance with one embodiment of the present invention.
FIG. 2 is a flow chart of a method for preparing a carbon black masterbatch, according to an embodiment of the present invention.
Description of the symbols
100. 102, 104, 106, 200, 202, 204: operation of
Detailed Description
The invention provides a plastic composition, which is prepared by uniformly mixing carbon black powder with the particle size of less than 1 micron and base material powder with the particle size of less than 300 microns. In the invention, the optical grade material with different specifications of light transmittance (transmittance) and optical attenuation values can be easily prepared by diluting the carbon black master batch A with the base material particles B, so that optical elements meeting various product specifications can be rapidly produced in a large scale, and the optical elements have high quality and yield.
In the optical element prepared by the prior method, because the carbon black particles are not refined, the carbon black is easy to aggregate to generate a plurality of black spots with the size of more than 40 microns, and the optical transmission signal of the optical element is caused to be problematic. On the contrary, the optical element prepared by the plastic composition of the invention does not have the problem of black spots, and the key technology is to prepare and disperse carbon black powder with the particle size of less than 1 micron so that the plastic composition containing carbon black and the optical element prepared by the composition in the following process hardly have black spots.
Hereinafter, a method for preparing the plastic composition of the present invention will be described. FIG. 1 is a flow chart illustrating a method of preparing a plastic composition in accordance with one embodiment of the present invention.
Referring to fig. 1, in operation 100, a liquid grinding step is performed on carbon black powder. In one embodiment, the liquid grinding step includes mixing about 85-98 parts by weight of water, about 1-10 parts by weight of carbon black powder, and about 1-5 parts by weight of a liquid dispersant to form a carbon black dispersion. In one embodiment, the liquid dispersant comprises a non-ionic dispersant. Then, the mixture is ground by a planetary ball mill at a rotational speed of about 250 to 350rpm for about 0.5 to 4 hours. In one embodiment, the planetary ball mill is, for example, a planetary zirconium bead mill.
In operation 102, a drying step is performed after the liquid milling step. In one embodiment, the water in the carbon black dispersion is removed at about 105-115 ℃. After the drying step, a part of the carbon black is aggregated by removing water and heating, so another grinding step is required to disperse the aggregated carbon black.
In operation 104, the carbon black powder is subjected to a solid state grinding step to form a refined carbon black powder, wherein the particle size of the refined carbon black powder is less than 500 nanometers. In one embodiment, performing the solid-state milling step comprises milling with a high-speed mill at a speed of greater than or equal to about 2,000rpm for about 0.03 hours or more. In one embodiment, the surface area of the carbon black powder after the solid-state grinding step is, for example, about 50m or more2G, e.g. greater than or equal to about150m2And the particle diameter of the carbon black powder is refined to be less than or equal to about 1 micron, such as less than or equal to about 500 nanometers.
In operation 106, about 0.005 to 1 part by weight of the refined carbon black powder, about 0.00025 to 0.5 part by weight of the solid dispersant, and about 98.5 to 99.995 parts by weight of the base material powder are mixed and subjected to a dispersion step to form the plastic composition of the present invention. In one embodiment, the solid dispersant comprises a paraffin-based dispersant. In one embodiment, the substrate powder includes Polyetherimide (PEI) or the like. In one embodiment, the plastic particles are ground to reduce the particle size of the substrate powder to less than or equal to about 300 microns. For example, the plastic grinding step is performed on the plastic particles, which includes grinding the plastic particles for about 2 to 10 seconds at a rotation speed of about 10,000rpm or more with a high-speed grinder to obtain a substrate powder having a particle size of about 300 μm or less. In one embodiment, the dispersing step comprises milling with a solid state mixing disperser at a speed of greater than or equal to about 500rpm for about 0.5 hours or more.
In one embodiment, the plastic composition prepared by the above method includes about 98.5 to 99.995 parts by weight of the base material powder, about 0.005 to 1 part by weight of the carbon black powder, and about 0.00025 to 0.5 part by weight of the solid dispersant. In one embodiment, the base powder comprises Polyetherimide (PEI) and the solid dispersant comprises paraffin dispersant. The carbon black powder has a particle size of about 500 nm or less, and the base powder has a particle size of about 300 μm or less. The surface area of the carbon black powder is about 50m or more2G, e.g. greater than or equal to about 150m2/g。
Hereinafter, the method for producing the carbon black master batch of the present invention will be described. FIG. 2 is a flow chart of a method for preparing a carbon black masterbatch, according to an embodiment of the present invention.
In operation 200, the plastic composition of the present invention is fed to an extruder for a melt-kneading step to form plastic moldings. In one embodiment, the plastic composition of the present invention is manufactured by the above operations 100 to 106, for example. In one embodiment, the extruder is a twin screw extruder and the kneading temperature is in the range of about 290 ℃ to about 350 ℃.
In operation 202, a cooling step is performed after the melt-kneading step to solidify the heated plastic bead. In one embodiment, the plastic bead is cooled with cold water at about 25 ℃.
In operation 204, a granulation step is performed after the cooling step. In one embodiment, the plastic molding is pelletized at a speed of about 200 to 300rpm to form the carbon black masterbatch A of the present invention.
In one embodiment, the concentration of carbon black in the carbon black masterbatch A can be controlled within a range of about 50ppm to 10,000ppm, but the invention is not limited thereto. More specifically, the carbon black concentration of the carbon black master batch a may be adjusted to 50ppm, 100ppm, 200ppm, 250ppm, or any desired concentration within any two of the above numerical ranges, as desired by the process.
In one embodiment, the base material contained in the base material particle B is the same as the base material powder contained in the carbon black master particle a. In the invention, the optical grade material with different specifications of light transmittance (transmittance) and optical attenuation values can be easily prepared by diluting the carbon black master batch A with the base material particles B, so that the optical element with high quality and high yield can be rapidly produced in a large scale and can meet various product specifications.
In one embodiment, the present invention provides an optical element, which is formed by blending a carbon black master batch A made from the plastic composition of the present invention and a pure base material batch B. In one embodiment, the optical element of the present invention comprises a fiber optic connector.
In one embodiment, the carbon black concentration of the optical element of the present invention is in the range of about 5ppm to 50ppm, but the present invention is not limited thereto. More specifically, the carbon black concentration of the optical element can be adjusted to 5ppm, 6ppm, 7ppm, 8ppm, 9ppm, 10ppm, 11ppm, 12ppm, 13ppm, 14ppm, 15ppm, 16ppm, 17ppm, 18ppm, 19ppm, 20ppm, 25ppm, 30ppm, 35ppm, 40ppm, 45ppm, 50ppm or any desired concentration within any two of the above numerical ranges, depending on the process requirements.
In one embodiment, the optical element of the present invention has a light transmittance in a range of about 30% to 85%, but the present invention is not limited thereto. More specifically, the light transmittance of the optical device can be adjusted to 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85% or any desired light transmittance within any two of the above numerical ranges according to the process requirement.
In one embodiment, the black spot generation rate of the optical element is about 10% or less. More specifically, the generation rate of black dots having a size of 40 microns or more is about 10% or less, the generation rate of black dots having a size of 20 microns or more is about 10% or less, the generation rate of black dots having a size of 10 microns or more is about 10% or less, and/or the generation rate of black dots having a size of 5 microns or more is about 10% or less.
In one embodiment, the optical attenuation of the optical element is in the range of about-0.5 to-10.0, but the invention is not limited thereto. More specifically, the optical attenuation of the optical element can be adjusted to be-0.5, -1.0, -1.5, -2.0, -2.5, -3.0, -3.5, -4.0, -4.5, -5.0, -5.5, 6.0, -6.5, -7.0, -7.5, -8.0, -8.5, -9.0, -9.5, -10.0, or any desired optical attenuation between any two values, as desired by the process.
Hereinafter, a comparative example and a plurality of examples are listed to verify the efficacy of the present invention. According to the experimental parameters in the table I and the table II, the carbon black master batch A with different carbon black concentrations is prepared, and then the carbon black master batch A and the base material particles B with different proportions are mixed to prepare the optical element which meets the specifications of various products. The comparative example 1 and the example 1 are both products with the same specification, wherein the comparative example 1 uses carbon black powder which is not ground, and the particle size of the carbon black is 1-200 microns; in example 1, the carbon black powder of the present invention was used, and the particle size of the carbon black was less than 500 nm.
Watch 1
Watch two
As can be seen from the tables I and II, the method of the present invention can easily prepare optical elements with different light transmittance and different optical attenuation values to satisfy various requirements of customers. In addition, the optical element provided by the embodiment of the invention has an extremely low black spot generation rate (less than or equal to 5%) and a qualification rate of 95-100%.
On the contrary, in comparative example 1, since the carbon black powder is used without being ground, since the particle size of the carbon black is 1 to 200 μm or more, the produced product has many black spots with a size of 40 μm or more, the black spot generation rate is 75%, the yield is only 25%, the yield is low, and the cost is wasted.
In summary, the method of the present invention can easily prepare optical grade materials with different light transmittance and different optical attenuation values, so as to achieve fast mass production of optical devices meeting various product specifications, and the mass-produced optical devices have high quality and yield. In addition, the optical element of the present invention has fewer black spots and excellent optical properties. In addition, the Minimum Order Quantity (MOQ) of the optical element is small, the delivery period is short (1-2 months), and the product competitiveness can be greatly improved.
Although the present invention has been described with reference to the above embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (4)
1. A method for producing an optical element, characterized by comprising:
carrying out liquid grinding on the carbon black powder;
after the liquid grinding step, performing a drying step;
after the drying step, performing a solid-state grinding step on the carbon black powder to form refined carbon black powder, wherein the grain diameter of the refined carbon black powder is less than 500 nanometers;
mixing 0.005-1 part by weight of the refined carbon black powder, 0.00025-0.5 part by weight of a solid dispersant and 98.5-99.995 parts by weight of a base material powder, and performing a dispersion step to form a plastic composition;
feeding the plastic composition into an extruder to perform a melt-mixing step to form a plastic molding; and
dicing the plastic batten to form carbon black master batch which is mixed with the base material particles to prepare the optical element,
wherein the grain diameter of the base material powder is less than or equal to 300 microns,
the solid dispersant includes a paraffin-based dispersant,
the surface area of the refined carbon black powder is more than or equal to 50m2/g，
The base material powder comprises polyetherimide, and the base material contained in the base material particles is the same as the base material powder contained in the carbon black master batch.
2. The method for producing an optical element according to claim 1, wherein the liquid-state grinding step comprises:
mixing 85-98 parts by weight of water, 1-10 parts by weight of carbon black powder and 1-5 parts by weight of liquid dispersant; and
grinding the mixture for 0.5 to 4 hours at a rotation speed of 250 to 350rpm by a planetary ball mill.
3. The method for producing an optical element according to claim 1, wherein the solid-state milling step comprises milling with a high-speed mill at a rotation speed of 2,000rpm or more for 0.03 hours or more.
4. The method for producing an optical element according to claim 1, wherein a kneading temperature of the melt-kneading step is in a range of 290 ℃ to 350 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611203763.1A CN108239398B (en) | 2016-12-23 | 2016-12-23 | Method for producing optical element |
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| CN201611203763.1A CN108239398B (en) | 2016-12-23 | 2016-12-23 | Method for producing optical element |
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| CN108239398A CN108239398A (en) | 2018-07-03 |
| CN108239398B true CN108239398B (en) | 2021-02-26 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1795231A (en) * | 2003-05-29 | 2006-06-28 | 通用电气公司 | Method for making a conductive thermoplastic composition |
| CN104419205A (en) * | 2013-09-09 | 2015-03-18 | 达迈科技股份有限公司 | Black polyimide film and processing method thereof |
| CN104553183A (en) * | 2013-10-22 | 2015-04-29 | 达迈科技股份有限公司 | Multilayer polyimide film containing polyimide powder matting agent and method for producing same |
| CN105085956A (en) * | 2015-09-08 | 2015-11-25 | 宁波今山电子材料有限公司 | Preparation method of black polyimide film with static electricity prevention and shielding functions |
| WO2016052412A1 (en) * | 2014-09-29 | 2016-04-07 | 株式会社クラレ | Polyetherimide-based fiber, method for manufacturing same, and fiber structure containing same |
-
2016
- 2016-12-23 CN CN201611203763.1A patent/CN108239398B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1795231A (en) * | 2003-05-29 | 2006-06-28 | 通用电气公司 | Method for making a conductive thermoplastic composition |
| CN104419205A (en) * | 2013-09-09 | 2015-03-18 | 达迈科技股份有限公司 | Black polyimide film and processing method thereof |
| CN104553183A (en) * | 2013-10-22 | 2015-04-29 | 达迈科技股份有限公司 | Multilayer polyimide film containing polyimide powder matting agent and method for producing same |
| WO2016052412A1 (en) * | 2014-09-29 | 2016-04-07 | 株式会社クラレ | Polyetherimide-based fiber, method for manufacturing same, and fiber structure containing same |
| CN105085956A (en) * | 2015-09-08 | 2015-11-25 | 宁波今山电子材料有限公司 | Preparation method of black polyimide film with static electricity prevention and shielding functions |
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