CN108381956B - Preparation method of laser blinding protective lens - Google Patents
Preparation method of laser blinding protective lens Download PDFInfo
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- CN108381956B CN108381956B CN201810176516.XA CN201810176516A CN108381956B CN 108381956 B CN108381956 B CN 108381956B CN 201810176516 A CN201810176516 A CN 201810176516A CN 108381956 B CN108381956 B CN 108381956B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D11/00—Producing optical elements, e.g. lenses or prisms
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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
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
- C08K2201/011—Nanostructured additives
Abstract
The invention relates to a preparation method of a laser blinding protective lens, belonging to the technical field of functional materials. The invention takes a graphene-like two-dimensional material molybdenum disulfide nanosheet as a substrate, utilizes the advantages of large in-plane carrier mobility, small indirect band gap, high fluorescence quantum yield, large surface area, good photoelectrochemical stability and the like, synthesizes ternary quantum dots in the interlayer spacing, and obtains a nonlinear optical amplitude limiting material which is good in dispersity and strong in stability and is not easy to deteriorate through the synergistic effect of the blocking effect of the molybdenum disulfide and the quantum dots.
Description
Technical Field
The invention relates to a preparation method of a laser blinding protective lens, belonging to the technical field of functional materials.
Background
Laser has the advantages of strong directivity, good monochromaticity and coherence, and the like, and is widely applied to the fields of military affairs, medical treatment, industry and the like. Laser protective materials have become a great concern in military and civil fields. The protection principle is divided into two types, namely linear and nonlinear laser protection, of the laser protection materials and the protection technology adopted at home and abroad at present.
The linear protection is mainly classified into absorption type, reflection type and absorption/reflection composite type. The absorption type protective material is prepared by adding light absorption dye into a polycarbonate base material. The advantage is that the protection effect has no angle dependence, but the visible light transmittance is lower. The reflective protective material is formed by plating a plurality of reflective medium layers on the surface of the optical glass substrate. The advantages are high visible light transmittance, angle dependence of protection effect, easy shedding of the coating and complex processing technology. Although the absorption/reflection composite material overcomes the defects of the two protective materials to a certain extent, the defects of the two products still exist to a certain extent only by combining the two types of physical materials. For example, the preparation process is complex, and the vapor deposition layer reaches dozens of layers or even hundreds of layers; the preparation conditions are harsh, and the adopted film evaporation technology needs conditions of high temperature, high vacuum and the like. Not only increases the processing difficulty and cost, but also reduces the transmittance of the light which should transmit through the wave band.
The most excellent protective performance in the nonlinear protective material is the optical amplitude limiting material which is most practical, and typical protective materials such as carbon material-fullerene, graphene, carbon nano tube and the like all have large conjugated structures, poor solubility characteristics and unsatisfactory protective effect. In addition, the adopted matrix is generally a liquid solvent, is volatile, easy to leak and difficult to prepare into a protective device, and greatly limits the practical application of the nonlinear protection technology. Therefore, it is urgently needed to develop an excellent laser protection material to meet the huge market demand.
disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems of narrow absorption bandwidth, poor sharp cutoff, dark field and low light transmittance of the existing laser protection material, the preparation method of the laser blinding protection lens is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
(1) Adding molybdenum disulfide and sodium cholate into deionized water, and performing ultrasonic dispersion for 6-8 hours at 40-50 ℃ to obtain a molybdenum disulfide dispersion liquid;
(2) putting the molybdenum disulfide dispersion liquid into a centrifugal machine, performing centrifugal separation at 3000-4000 r/min to obtain supernatant, performing centrifugal separation on the supernatant at 12000-12500 r/min to obtain precipitate, performing ultrasonic cleaning on the precipitate with absolute ethyl alcohol, performing centrifugal separation, and drying to obtain pretreated molybdenum disulfide nanosheets;
(3) Putting cadmium oxide, zinc oxide, oleic acid and octadecylene into a flask, heating and stirring, and cooling to 150-160 ℃ to obtain a mixed solution;
(4) Adding selenium powder and a pretreated molybdenum disulfide nanosheet into N-formylmorpholine, heating to 150-160 ℃, stirring for 20-30 min, adding into the mixed solution, continuing stirring for 20-30 min, heating to 220-240 ℃, keeping the temperature, stirring for 1.5-2.5 h, cooling, filtering, washing with alcohol, and drying to obtain a nonlinear optical amplitude limiting material;
(5) Drying polycarbonate, then loading the polycarbonate into a mixing barrel, adding a nonlinear optical amplitude limiting material and liquid paraffin into the mixing barrel, uniformly mixing, and then loading the mixture into a roller mill for mixing for 2-3 hours to obtain composite polycarbonate master batches;
(6) Filling the composite polycarbonate master batch into an injection molding machine for melting, injecting the molten composite polycarbonate into a mold for injection molding, and cooling to room temperature to obtain a filter lens;
(7) polishing the filter lens to remove burrs, washing and drying to obtain the laser blinding protective lens.
the mass ratio of the molybdenum disulfide to the sodium cholate in the step (1) is (2.2-5.0): 1.
the cadmium oxide, the zinc oxide, the oleic acid and the octadecene in the step (3) are 2-3 parts by weight of cadmium oxide, 0.4-0.6 part by weight of zinc oxide, 10-15 parts by weight of oleic acid and 10-15 parts by weight of octadecene.
and (3) heating and stirring to 220-240 ℃ in a nitrogen atmosphere, and stirring for 20-30 min at 200-300 r/min.
the selenium powder, the pretreated molybdenum disulfide nanosheet and the N-formyl morpholine in the step (4) are 1.6-2.4 parts by weight of the selenium powder, 5-8 parts by weight of the pretreated molybdenum disulfide nanosheet and 20-30 parts by weight of the N-formyl morpholine.
The dosage of the nonlinear optical amplitude limiting material in the step (5) is 0.1-0.3% of the mass of the polycarbonate, and the dosage of the liquid paraffin is 0.05-0.20% of the mass of the polycarbonate.
and (6) melting and injection molding at 250-310 ℃, injecting the molten composite polycarbonate into a mold at 100-120 ℃ under the injection pressure of 80-120 MPa, and injection molding under the pressure of 80-100 MPa.
Compared with other methods, the method has the beneficial technical effects that:
the invention takes a graphene-like two-dimensional material molybdenum disulfide nanosheet as a substrate, utilizes the advantages of large in-plane carrier mobility, small indirect band gap, high fluorescence quantum yield, large surface area, good photoelectrochemical stability and the like of the two-dimensional material molybdenum disulfide nanosheet, synthesizes ternary quantum dots in the interlayer spacing thereof, obtains a nonlinear optical amplitude limiting material which is good in dispersity, strong in stability and not easy to deteriorate through the synergistic effect of the blocking effect of the molybdenum disulfide and the quantum dots, shows the increase of polarizability and the increase of absorption coefficient through the surface effect, the quantum size effect, the quantum confinement effect, the macroscopic quantum tunneling effect and the like of the quantum effect, has larger nonlinear optical parameters, has light intensity smaller than the nonlinear absorption threshold of the material when the laser energy is low, does not generate the nonlinear absorption effect, the incident laser almost completely penetrates through the material, and after the light intensity of the laser is increased, when the material is far away from the focus, the laser energy is still weaker, the normalized transmittance of the material is still close to 1, the light beam transmittance is rapidly reduced along with the continuous approach of the material to the focus, the laser energy is the largest when the material reaches the focus, the normalized transmittance is reduced to the minimum, and after the material is far away from the focus, the laser transmittance gradually rises along with the reduction of the light intensity, so that a reliable and efficient protection means can be provided for laser operators.
Detailed Description
adding 10-15 g of molybdenum disulfide and 3.0-4.5 g of sodium cholate into 2-3L of deionized water, ultrasonically dispersing for 6-8 h by using 500W of ultrasonic wave under a constant-temperature water bath of 40-50 ℃ to obtain a molybdenum disulfide dispersion liquid, loading the molybdenum disulfide dispersion liquid into a centrifugal machine, centrifugally separating for 20-30 min by using 3000-4000 r/min, collecting supernatant, centrifugally separating for 30-40 min by using 12000-12500 r/min, collecting precipitate to obtain molybdenum disulfide nanosheets, adding the molybdenum disulfide nanosheets into 500-600 mL of anhydrous ethanol, ultrasonically cleaning for 20-30 min by using 300W of ultrasonic wave, centrifugally separating for 30-40 min by using 12000-12500 r/min, collecting precipitate, placing the precipitate into a drying box, drying for 3-5 h at 105-110 ℃ to obtain pretreated molybdenum disulfide nanosheets, taking 2-3 g of cadmium oxide, 0.4-0.6 g of zinc oxide and 10-15 g of oleic acid, putting 10-15 g of octadecene into a flask, heating to 220-240 ℃ in a nitrogen atmosphere, stirring for 20-30 min at 200-300 r/min, cooling to 150-160 ℃ to obtain a reaction liquid, taking 1.6-2.4 g of selenium powder and 5-8 g of pretreated molybdenum disulfide nanosheet, adding the pretreated molybdenum disulfide nanosheet into 20-30 g of N-formylmorpholine, heating to 150-160 ℃, stirring for 20-30 min at 200-300 r/min, adding the mixture into the reaction liquid, continuing stirring for 20-30 min, heating to 220-240 ℃, keeping the temperature, stirring for 1.5-2.5 h, cooling to room temperature, filtering to obtain a filter cake, washing the filter cake with absolute ethyl alcohol for 3-5 times, then placing the filter cake into a drying box, drying for 4-5 h at 105-110 ℃ to obtain a nonlinear optical material, taking 1-2 kg of polycarbonate, placing the polycarbonate into a drying box, drying for 8-10 h at 105-110 ℃ with an amplitude limit, then placing into a mixing barrel, adding 2-3 g of the nonlinear optical material, 1-2 g of liquid paraffin, uniformly mixing, putting into a roller mill, mixing for 2-3 h to obtain composite polycarbonate master batches, putting the composite polycarbonate master batches into an injection molding machine, melting at 250-310 ℃, injecting the molten composite polycarbonate into a 100-120 ℃ mold under 80-120 MPa injection pressure, injection molding under 80-100 MPa pressure maintaining pressure, cooling to room temperature to obtain a filter lens, polishing and polishing the filter lens to remove burrs, washing the filter lens for 3-5 times with deionized water, transferring into a vacuum drying oven, and drying at 60-80 ℃ for 1-2 h to obtain the laser blinding protective lens.
example 1
Adding 10g of molybdenum disulfide and 3.0g of sodium cholate into 2L of deionized water, ultrasonically dispersing for 6h by using 500W of ultrasonic waves in a constant-temperature water bath at 40 ℃ to obtain a molybdenum disulfide dispersion liquid, loading the molybdenum disulfide dispersion liquid into a centrifugal machine, centrifugally separating for 20min at 3000r/min, collecting supernatant, centrifugally separating for 30min at 12000r/min, collecting precipitate to obtain molybdenum disulfide nanosheets, adding the molybdenum disulfide nanosheets into 500mL of absolute ethyl alcohol, ultrasonically cleaning for 20min by using 300W of ultrasonic waves, centrifugally separating for 30min at 12000r/min, collecting precipitate, placing the precipitate in a drying box, drying for 3h at 105 ℃ to obtain pretreated molybdenum disulfide nanosheets, loading 2g of cadmium oxide, 0.4g of zinc oxide, 10g of oleic acid and 10g of octadecene into a flask, heating to 220 ℃ under the nitrogen atmosphere, stirring for 20min at 200r/min, cooling to 150 ℃ to obtain a reaction liquid, taking 1.6g of selenium powder and 5g of pretreated molybdenum disulfide nanosheet, adding the selenium powder and the pretreated molybdenum disulfide nanosheet into 20g of N-formylmorpholine, heating to 150 ℃, stirring for 20min at 200r/min, adding the mixture into the reaction liquid, continuously stirring for 20min, heating to 220 ℃, keeping the temperature and stirring for 1.5h, cooling to room temperature, filtering to obtain a filter cake, washing the filter cake with absolute ethyl alcohol for 3 times, placing the filter cake into a drying box, drying for 4h at 105 ℃ to obtain a nonlinear optical limiting material, placing 1kg of polycarbonate into the drying box, drying for 8h at 105 ℃, placing into a mixing barrel, adding 2g of the nonlinear optical limiting material and 1g of liquid paraffin into the mixing barrel, uniformly mixing, placing into a roller mill for mixing for 2h to obtain a composite polycarbonate master batch, placing the composite polycarbonate master batch into an injection molding machine, melting at 250 ℃, injecting under 80MPa, injecting the molten composite polycarbonate into a 100 ℃ mold, performing injection molding under the pressure of 80MPa, cooling to room temperature to obtain a filter lens, polishing and grinding the filter lens to remove burrs, washing the filter lens for 3 times by using deionized water, transferring the filter lens into a vacuum drying oven, and drying at 60 ℃ for 1h to obtain the laser blinding protective lens.
example 2
Adding 13g of molybdenum disulfide and 3.7g of sodium cholate into 2.5L of deionized water, ultrasonically dispersing for 7h under 500W of ultrasonic waves in a constant-temperature water bath at 45 ℃ to obtain a molybdenum disulfide dispersion liquid, loading the molybdenum disulfide dispersion liquid into a centrifugal machine, centrifugally separating for 25min at 3500r/min, collecting supernatant, centrifugally separating for 35min at 12250r/min, collecting precipitate to obtain molybdenum disulfide nanosheets, adding the molybdenum disulfide nanosheets into 550mL of absolute ethyl alcohol, ultrasonically cleaning for 25min under 300W of ultrasonic waves, centrifugally separating for 35min at 12250r/min, collecting precipitate, drying the precipitate in a drying box at 107 ℃ for 4h to obtain pretreated molybdenum disulfide nanosheets, loading 2.5g of cadmium oxide, 0.5g of zinc oxide, 13g of oleic acid and 13g of octadecene into a flask, heating to 230 ℃ under the atmosphere of nitrogen, stirring for 25min at 250r/min, cooling to 155 ℃ to obtain reaction liquid, taking 2.0g of selenium powder and 7g of pretreated molybdenum disulfide nanosheet, adding the mixture into 25g of N-formylmorpholine, heating to 155 ℃, stirring for 25min at 250r/min, adding the mixture into the reaction liquid, continuously stirring for 25min, heating to 230 ℃, keeping the temperature and stirring for 2.0h, cooling to room temperature, filtering to obtain a filter cake, washing the filter cake with absolute ethyl alcohol for 4 times, placing the filter cake into a drying box, drying for 4h at 107 ℃ to obtain a nonlinear optical limiting material, placing 1.5kg of polycarbonate into the drying box, drying for 9h at 107 ℃, placing into a mixing barrel, adding 2.5g of the nonlinear optical limiting material and 1.5g of liquid paraffin into the mixing barrel, uniformly mixing, placing into a roller mill for mixing for 2h to obtain composite polycarbonate master batches, placing the composite polycarbonate master batches into an injection molding machine, melting at 280 ℃ and injecting under 100MPa, injecting the molten composite polycarbonate into a 110 ℃ mold, performing injection molding under the pressure of 90MPa, cooling to room temperature to obtain a filter lens, polishing and grinding the filter lens to remove burrs, washing the filter lens with deionized water for 4 times, transferring the filter lens into a vacuum drying oven, and drying at 70 ℃ for 2 hours to obtain the laser blinding protective lens.
Example 3
Adding 15g of molybdenum disulfide and 4.5g of sodium cholate into 3L of deionized water, ultrasonically dispersing for 8h by using 500W of ultrasonic waves in a constant-temperature water bath at 50 ℃ to obtain a molybdenum disulfide dispersion liquid, loading the molybdenum disulfide dispersion liquid into a centrifugal machine, centrifugally separating for 30min at 4000r/min, collecting supernatant, centrifugally separating for 40min at 12500r/min, collecting precipitate to obtain molybdenum disulfide nanosheets, adding the molybdenum disulfide nanosheets into 600mL of absolute ethyl alcohol, ultrasonically cleaning for 30min by using 300W of ultrasonic waves, centrifugally separating for 40min at 12500r/min, collecting precipitate, drying the precipitate in a drying box at 110 ℃ for 5h to obtain pretreated molybdenum disulfide nanosheets, loading 3g of cadmium oxide, 0.6g of zinc oxide, 15g of oleic acid and 15g of octadecene into a flask, heating to 240 ℃ under the nitrogen atmosphere, stirring for 30min at 300r/min, cooling to 160 ℃ to obtain a reaction liquid, taking 2.4g of selenium powder and 8g of pretreated molybdenum disulfide nanosheet, adding the selenium powder and the pretreated molybdenum disulfide nanosheet into 30g of N-formylmorpholine, heating to 160 ℃, stirring for 30min at 300r/min, adding the mixture into the reaction liquid, continuously stirring for 30min, heating to 240 ℃, keeping the temperature and stirring for 2.5h, cooling to room temperature, filtering to obtain a filter cake, washing the filter cake with absolute ethyl alcohol for 5 times, placing the filter cake into a drying box, drying for 5h at 110 ℃ to obtain a nonlinear optical limiting material, placing 2kg of polycarbonate into the drying box, drying for 10h at 110 ℃, placing into a mixing barrel, adding 3g of the nonlinear optical limiting material and 2g of liquid paraffin into the mixing barrel, uniformly mixing, placing into a roller mill, mixing for 3h to obtain a composite polycarbonate master batch, placing the composite polycarbonate master batch into an injection molding machine, melting at 310 ℃, injecting under 120MPa, injecting the molten composite polycarbonate into a 120 ℃ mold, performing injection molding under the pressure of 100MPa, cooling to room temperature to obtain a filter lens, polishing and grinding the filter lens to remove burrs, washing the filter lens for 5 times by using deionized water, transferring the filter lens into a vacuum drying oven, and drying at 80 ℃ for 2 hours to obtain the laser blinding protective lens.
the laser blinding protective lens prepared by the invention and the protective lens produced by Guangdong company are detected, and the specific detection results are shown in the following table 1:
Table 1 characterization of laser blinding protective lens performance
As can be seen from Table 1, the laser blinding protective lens prepared by the invention has larger nonlinear optical parameters, when the laser energy is low, the light intensity is smaller than the nonlinear absorption threshold value of the material, and the laser transmittance gradually rises along with the reduction of the light intensity, so that a reliable and efficient protective means can be provided for laser operators.
Claims (3)
1. A preparation method of a laser blinding protective lens is characterized by comprising the following specific preparation steps:
(1) adding molybdenum disulfide and sodium cholate into deionized water, and performing ultrasonic dispersion for 6-8 hours at 40-50 ℃ to obtain a molybdenum disulfide dispersion liquid; the mass ratio of the molybdenum disulfide to the sodium cholate is (2.2-5.0): 1;
(2) Putting the molybdenum disulfide dispersion liquid into a centrifugal machine, performing centrifugal separation at 3000-4000 r/min to obtain supernatant, performing centrifugal separation on the supernatant at 12000-12500 r/min to obtain precipitate, performing ultrasonic cleaning on the precipitate with absolute ethyl alcohol, performing centrifugal separation, and drying to obtain pretreated molybdenum disulfide nanosheets;
(3) Putting cadmium oxide, zinc oxide, oleic acid and octadecylene into a flask, heating and stirring, and cooling to 150-160 ℃ to obtain a mixed solution; the cadmium oxide, the zinc oxide, the oleic acid and the octadecene are 2-3 parts by weight of cadmium oxide, 0.4-0.6 part by weight of zinc oxide, 10-15 parts by weight of oleic acid and 10-15 parts by weight of octadecene;
(4) Adding selenium powder and a pretreated molybdenum disulfide nanosheet into N-formylmorpholine, heating to 150-160 ℃, stirring for 20-30 min, adding into the mixed solution, continuing stirring for 20-30 min, heating to 220-240 ℃, keeping the temperature, stirring for 1.5-2.5 h, cooling, filtering, washing with alcohol, and drying to obtain a nonlinear optical amplitude limiting material; the selenium powder, the pretreated molybdenum disulfide nanosheet and the N-formyl morpholine are 1.6-2.4 parts by weight of the selenium powder, 5-8 parts by weight of the pretreated molybdenum disulfide nanosheet and 20-30 parts by weight of the N-formyl morpholine;
(5) Putting 1-2 kg of polycarbonate in a drying oven, drying at 105-110 ℃ for 8-10 h, then putting into a mixing barrel, adding a nonlinear optical amplitude limiting material and liquid paraffin into the mixing barrel, uniformly mixing, and then putting into a roller mill for mixing for 2-3 h to obtain composite polycarbonate master batch; the dosage of the nonlinear optical amplitude limiting material is 0.1-0.3% of the mass of the polycarbonate, and the dosage of the liquid paraffin is 0.05-0.20% of the mass of the polycarbonate;
(6) filling the composite polycarbonate master batch into an injection molding machine for melting, injecting the molten composite polycarbonate into a mold for injection molding, and cooling to room temperature to obtain a filter lens;
(7) Polishing the filter lens to remove burrs, washing and drying to obtain the laser blinding protective lens.
2. The method for preparing a laser blinding protective lens according to claim 1, wherein the heating and stirring in step (3) is heating to 220-240 ℃ in a nitrogen atmosphere, and stirring at 200-300 r/min for 20-30 min.
3. The method for preparing a laser blind protective lens according to claim 1, wherein the melting injection molding process in the step (6) is melting at 250-310 ℃, injecting the molten composite polycarbonate into a 100-120 ℃ mold under an injection pressure of 80-120 MPa, and injection molding under a pressure of 80-100 MPa.
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| US7063151B2 (en) * | 2004-03-05 | 2006-06-20 | Halliburton Energy Services, Inc. | Methods of preparing and using coated particulates |
| CN102849798B (en) * | 2012-08-29 | 2014-02-26 | 北京化工大学 | Molybdenum disulfide nano-sheet film material and its preparation methods |
| CN103203463A (en) * | 2013-03-21 | 2013-07-17 | 上海大学 | Preparation method of molybdic sulfide nanosheet/sliver nanoparticle composite material |
| CN104103829B (en) * | 2014-07-17 | 2016-06-29 | 浙江大学 | MoS2Nanometer sheet/graphene composite nano material with holes and preparation method |
| CN105623227A (en) * | 2014-11-04 | 2016-06-01 | 刘和超 | Optical glass with high hardness |
| CN104525938B (en) * | 2014-12-23 | 2017-02-22 | 国家纳米科学中心 | Molybdenum disulfide/gold nanorod composite, preparation method and application |
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Effective date of registration: 20191114 Address after: No.2-1, No.152 Zhongrun Avenue, high tech Zone, Zibo City, Shandong Province Applicant after: Zibo Langsi Photoelectric Co., Ltd. Address before: 213000 Room 401, Unit A, 6 Blocks, Baiyun East Court, Zhonglou District, Changzhou City, Jiangsu Province Applicant before: Guo Yingqing |
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