CN102757676B - Low-emissivity nano-coating and preparation method and application thereof - Google Patents

Low-emissivity nano-coating and preparation method and application thereof Download PDF

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CN102757676B
CN102757676B CN201210144467.4A CN201210144467A CN102757676B CN 102757676 B CN102757676 B CN 102757676B CN 201210144467 A CN201210144467 A CN 201210144467A CN 102757676 B CN102757676 B CN 102757676B
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coating
weight part
gazo
ball
byk
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CN102757676A (en
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马天
冯新星
沈凤川
张建春
郝新敏
来侃
张华�
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Quartermaster Research Institute of General Logistics Department of CPLA
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Abstract

The invention discloses a low-emissivity nano-coating and a preparation method and an application thereof. The coating comprises a coating agent and additives, wherein the coating agent is any one of aqueous coating agents and oily coating agents; the additives include a filler, a wetting and dispersing agent, a cross-linking agent, a defoaming agent and a solvent; and the filler is GaZO nanopowder. The particle size of the coating is less than 100 nm, the viscosity is 8 to 15 cP, the surface tension is 20 to 36 mN/m, and the weight percentage content of the solid phase is 1 to 60 wt%. The coating is suitable for making thermal infrared invisible camouflages, camouflage nets, tents and the like, is invisible to visible light, near-infrared light (wavelength of 0.38 to 2.5 mum) and infrared light (wavelength of 8 to 14 mum) while retaining the original physochemical properties, has no bad impact on wear comfort, and has a significant application value.

Description

Low-launch-rate nano paint and preparation method thereof and application
Technical field
The present invention relates to a kind of low-launch-rate nano paint and preparation method thereof and application.
Background technology
Along with the development of infrared detection technique and guidance technology, the spatial resolution of the thermal infrared imaging instrument of working at infrared band (wavelength 8～14 μ m) has reached 0.1～0.2mrad, and temperature resolution reaches 0.1～0.3 ℃.Infrared stealth technology, as the important factor that improves combat unit viability, penetration ability and fighting efficiency, has caused the great attention of various countries, and the importance in present information war grows with each passing day.Infrared stealth technology roughly may be summarized to be and changes ir radiation wave band, reduction infrared intensity, adjusting three aspects of ir radiation transmitting procedure.At target surface, apply infrared stealth coating and can reduce its infrared intensity, and the research of low-launch-rate coating is the key of infrared stealth coating preparation research.Wherein, 8～14 mu m wavebands are one of important wave bands of infrared thermal imaging.
General infrared stealth coating is comprised of coating-forming agent and additive.Described coating-forming agent refers to the polymeric coating layer agent with certain infrared transparent performance; Described additive comprises: filler, wetting dispersing agent, defoamer, linking agent, solvent, thinner etc.; Described filler comprises metallic stuffing, semiconductor fills.Research shows, coating-forming agent accounts for more than 60% for the impact of coating emittance, and the infrared emittance of most of common coating-forming agents is all higher, is difficult to meet the low-launch-rate needs of infrared stealth.Have investigator to synthesize infrared transparent coating-forming agent, so as to reducing coating emittance, wherein with modified EPT rubber typical case the most, but that its shortcoming is adhesion strength is low, easily comes off in actual applications.There is non-refractory and the problem such as resistance to deterioration is poor in conductive polymer coating-forming agent.In numerous fillers, metallic stuffing is to report up to now maximum low-launch-rate fillers, and the shortcoming of its existence is that metallic stuffing reflectivity is high, is unfavorable at multiband multi-Functional Camouflages such as visible ray, radar and laser, and metallic stuffing is oxidizable in air, can make its infrared emittance significantly raise; Meanwhile, the low-launch-rate coating of being made by metallic stuffing is coated on after fabric, and feel is hardened, and adheres to fastness and can not meet actual needs.The combination of semiconductor fills and infrared transparent coating-forming agent can effectively overcome above shortcoming, thereby becomes the emphasis of research and application.Effectively selecting the semiconductor fills of different sorts, granularity and addition, with the optimum combination of infrared transparent coating-forming agent, is the key of preparing low emissivity coatings, realizing infrared stealth.
Doped semiconductor filler is one of infrared stealth material of high comprehensive performance.The more doped semiconductor materials of research is ITO (tin-doped indium oxide) and ATO (antimony doped tin oxide) at present.Owing to preparing raw material In, the Sn of ITO and ATO, belong to rare metal, cause its cost of manufacture to increase, be unfavorable for the application of ITO and ATO.ZAO (Al-Doped ZnO) is novel semi-conductor stealth material, and cost is cheaper with respect to ITO and ATO, is considered to tool doped semiconductor materials with broad prospects for development; Its shortcoming is that the coating emittance of preparing with it is higher.Zinc oxide codoped gallium aluminium (Gallium and Aluminum Co-doped Zinc Oxide, GAZO) be a kind of semiconductor material with low-launch-rate, research for GAZO both at home and abroad focuses mostly at GAZO sputtered film, and the research for infrared stealth material have not been reported using GAZO powder as filler.
Summary of the invention
The object of this invention is to provide a kind of low-launch-rate nano paint and preparation method thereof and application.
Nanometer GAZO powder provided by the invention, is prepared and is obtained by following raw material: Ga, Al, Ga 2o 3, Al 2o 3and ZnO.
In above-mentioned nanometer GAZO powder, the consumption umber of described each raw material is respectively: Ga:0.1-2 weight part, Al:0.1-2 weight part, Ga 2o 3: 0.1-3 weight part, Al 2o 3: 0.1-3 weight part, ZnO:90-99.6 weight part; Be preferably as follows each raw material of consumption umber: Ga:1 weight part, Al:1 weight part, Ga 2o 3: 1 weight part, Al 2o 3: 1 weight part, ZnO:96 weight part;
The particle diameter of described nanometer GAZO powder is 20-200nm, is specially 150-180nm.
The method of the above-mentioned nanometer GAZO powder of preparation provided by the invention, comprises the steps: under inert atmosphere protection, by after aforementioned each raw material blending, in 1000-1400 ℃ of insulation, after 0.5-3 hour, quenches again, obtains described nanometer GAZO powder.
After described quenching step, also can according to actual needs, products therefrom be ground, be filtered.Described inert atmosphere specifically can be nitrogen atmosphere or argon gas atmosphere.
Nano paint provided by the invention, comprises coating-forming agent and additive;
Wherein, described coating-forming agent is selected from any one in aqueous coating agent and oiliness coating-forming agent;
Described nano paint also can only be comprised of said components.
Described additive comprises filler, wetting dispersing agent, linking agent, defoamer and solvent;
Described filler is nanometer GAZO powder;
Described wetting dispersing agent be selected from BYK-9076, BYK-9077,
Figure BDA00001623928900021
dispers 610,
Figure BDA00001623928900022
dispers610S,
Figure BDA00001623928900023
dispers 651,
Figure BDA00001623928900024
dispers 652,
Figure BDA00001623928900025
dispers 700,
Figure BDA00001623928900026
dispers 710,
Figure BDA00001623928900027
dispers 715W,
Figure BDA00001623928900028
dispers 735W, dispers 740W,
Figure BDA000016239289000210
dispers 745W,
Figure BDA000016239289000211
dispers 750W,
Figure BDA000016239289000212
dispers 752W,
Figure BDA000016239289000213
dispers 760W, Surfynol CT-324, Surfynol CT-136, DISPERBYK-190, DISPERBYK-191, DISPERBYK-2010, DISPERBYK-2090, DISPERBYK-2091, DISPERBYK-2095, DISPERBYK-107, BYK-P105, Irgaflow tM100, Irgaflow tM110,
Figure BDA000016239289000214
wet KL245,
Figure BDA000016239289000215
wet KL280, wet250, wet 260,
Figure BDA000016239289000218
wet 265, wet 265,
Figure BDA000016239289000220
wet 270,
Figure BDA000016239289000221
wet 280,
Figure BDA000016239289000222
wet 500, AD41-5033,
Figure BDA000016239289000223
wet 505, fSO,
Figure BDA000016239289000225
fSA,
Figure BDA000016239289000226
fSN,
Figure BDA000016239289000227
fSP, Tergitol NP-10,
Figure BDA000016239289000228
4430, 4432,
Figure BDA000016239289000230
at least one in 4434, Surfynol 420, Surfynol 440, Surfynol 465, Surfynol 485, Surfynol 104E;
Described linking agent be selected from BYK-4500, BYK-4510, rad 2100,
Figure BDA000016239289000232
rad 2200N,
Figure BDA000016239289000233
rad 2250,
Figure BDA000016239289000234
rad 2300, at least one in Rad 2500, Printofix Fixing agnet ZF;
Described defoamer be selected from BYK-011, BYK-012, BYK-016, BYK-020, BYK-022, BYK-088, BYK-072, BYK-085,
Figure BDA00001623928900031
foamex 810, TEGO Foamex 825,
Figure BDA00001623928900032
foamex 822,
Figure BDA00001623928900033
foamex 845, at least one in Foamex 1488, Surfynol DF-110D, Surfynol DF-75;
Wherein, the product ShiBYK company of DISPERBYK and BYK provides;
Figure BDA00001623928900035
product by Goldschmidt chemical company, provided;
Figure BDA00001623928900036
product by E.I.Du Pont Company, provided; Tergitol NP-10 YouDow company provides; The product of Surfynol is provided by U.S. aerification chemical product company;
Figure BDA00001623928900037
product You3M company provide; Irgaflow tMproduct by BASF Ta Fuka, provided;
Described solvent is selected from deionized water, distilled water, ethyl acetate, methyl acetate, butylacetate, propylene glycol methyl ether acetate, ethylene glycol ether acetate, propylene glycol monomethyl ether, benzene,toluene,xylene, hexanaphthene, methylcyclohexane, p-chloro benzo trifluoride-99, isopropyl acetate, 1, at least one in 1,1-trichloromethane, methyl iso-butyl ketone (MIBK) and the acetic acid trimethyl carbinol;
Described aqueous coating agent is selected from
Figure BDA00001623928900038
n96101,
Figure BDA00001623928900039
n96110,
Figure BDA000016239289000310
at least one in N96111, Impranil DLC-F, MW-713;
Described oiliness coating-forming agent be selected from EEA NUC 4107, SIS 1105, SIS 1106,
Figure BDA000016239289000311
g1643MPolymer,
Figure BDA000016239289000312
d1161J,
Figure BDA000016239289000313
at least one in D1702H;
Wherein,
Figure BDA000016239289000314
product by Clariant company, provided; MW-713 Shi You Shanghai Mowang Composite Materials Co., Ltd. provides; The product of SIS is provided by Yueyang petrochemical industry;
Figure BDA000016239289000315
product by U.S. Ke Teng Polymer Company, provided; EEANUC 4107 is provided by Japanese NUC company;
Described additive is by described filler, wetting dispersing agent, linking agent, defoamer and solvent composition;
The mass ratio of described coating-forming agent and additive is 5-30: 70-95, and within preferably 15: 85, (indication quality is the total mass that belongs to all components of coating-forming agent or additive herein.)；
In described additive, the mass ratio of described filler, wetting dispersing agent, linking agent, defoamer and solvent is 1.75-14: 0.1-2: 0.1-3: 0.1-1: 65-82.95, preferably 8: 1: 0.5: 0.5: 75.
The particle diameter of described nano paint is less than 100nm, and viscosity is 8～15cP, and surface tension is 20～36mN/m, and the quality percentage composition of solid phase is 1～60%, and the normal temperature storage time is no less than 6 months; The average resistivity of coating is 4.5 * 10 -3Ω cm.
The method of the described nano paint of preparation provided by the invention, carries out ball milling after comprising the steps: aforementioned each component to mix, and obtains described nano paint.
In described ball milling step, the rotating speed of ball mill is 500～6000r/min, and the time is 1～24hr; All materials that described each component forms and the mass ratio of ball milling step abrading-ball used are 2: 1～1: 3, preferably 1: 1～1: 1.5; The material that forms described abrading-ball is silicon carbide, zirconium white or norbide; The particle diameter of described abrading-ball is 0.03～2mm, preferably 0.04～0.8mm.
In actually operating, described mixing step can specifically comprise the steps:
1) the described wetting dispersing agent of 0.1～20 part of the described solvent of 30～85 parts of weight parts, weight part is mixed and carries out ball milling with the described GAZO powder of 5～70 parts of weight parts, while making the particle diameter of described GAZO powder be 10～100nm, stop described ball milling, obtain GAZO thickened pulp;
2) coating-forming agent of 30～92 parts of described defoamer, the weight parts of 0.1～20 part of the described solvent of 30～90 parts of weight parts, weight part is mixed and carries out ball milling, obtain coating-forming agent dispersion; In described ball milling step, the rotating speed of ball mill is 500～6000r/min, and the time is 0.1～1hr, preferably 0.3～0.8hr;
3) by the described step 1 of 1～80 part of described linking agent, the weight part of 0.1～20 part of the described solvent of 1～95 part of weight part, weight part) the described step 2 of 1～80 part of gained GAZO thickened pulp and weight part) gained coating-forming agent dispersion mixes and carries out ball milling, obtains described nano paint.
Above-mentioned steps 1), in, in described GAZO thickened pulp, the quality percentage composition of solid phase is 10～80%, preferably 40～60%;
The described described wetting dispersing agent by 0.1～20 part of the described solvent of 30～85 parts of weight parts, weight part mixes and carries out in ball milling step with the described GAZO powder of 5～70 parts of weight parts, the rotating speed of ball mill is 500～6000r/min, Ball-milling Time is 2-48hr, preferably 4-32hr;
Step 2) in, described the coating-forming agent of 30～80 parts of described defoamer, the weight parts of 0.1～20 part of the described solvent of 30～90 parts of weight parts, weight part is mixed and carried out in ball milling step, the rotating speed of ball mill is 500～6000r/min, and the time is 0.1～1hr, preferably 0.3～0.8hr;
Step 3) in, described the coating-forming agent of 30～80 parts of described defoamer, the weight parts of 0.1～20 part of the described solvent of 30～90 parts of weight parts, weight part is mixed and carried out in ball milling step, the rotating speed of ball mill is 500～6000r/min, and Ball-milling Time is 1-24hr, preferably 2-18hr.
The fabric with infrared stealth function that the above-mentioned nano paint provided by the invention of take is coating; And this nano paint has the application in the fabric of infrared stealth function in preparation, also belong to protection scope of the present invention.Wherein, the body material in described fabric is selected from least one in woven fabrics, knitted fabrics, non-woven fabrics, synthetic leather, glass and metal skin; The top coat colour fastness of described fabric is 4 grades; Described fabric is that 0.38～2.5 visible light wave range of μ m is, the average transmittances of near-infrared band is more than 90% at wavelength; The average emitted rate that is 8～14 μ m infrared bands at wavelength is 0.5～0.75.
Compared with the prior art, tool has the following advantages in the present invention:
1, utilize the particle diameter of the low-launch-rate nano paint that the inventive method makes to be less than 100nm, viscosity 8～15cP, surface tension 20～36mN/m, adjustable within the scope of solid phase quality percentage composition 1～60wt%, normal temperature can store more than 6 months, and stable system is convenient to transportation.
2, the nano paint that utilizes the inventive method to make, mode is coated on woven fabric, looped fabric, non-woven fabrics or synthetic leather surface to adopt numerial code spray drawing, screen printing, blade coating, spray, pad etc., through drying or hot-pressing processing, make the low emissivity coatings fabric with infrared stealth function again.Due to nano paint of the present invention dry or hot pressing after without washing, so can significantly reduce environmental pollution, gained coating is firmly soft, and can large-scale production, has very high application prospect.
3, utilize the made coated fabric top coat colour fastness of nano paint of the present invention can reach 4 grades; Strong adhesion, wear-resistant, soft, water tolerance, thermotolerance are good; At the average transmittances of visible light wave range, near-infrared band (wavelength 0.38～2.5 μ m) up to more than 90%; Coating average resistivity is 4.5 * 10 -3Ω cm; In the average emitted rate of infrared band (wavelength 8～14 μ m), be 0.5～0.75 adjustable.The present invention can carry out the material surface application of infrared stealth at multiple need, have wide Application Areas.
Utilize the low emissivity coatings material that the inventive method is made to be suitable for making thermal infrared stealth camouflage fatigue, camouflage net and tent etc., do not reducing on the basis of existing product physicochemical property, can compatible visible ray, near infrared (wavelength 0.38～2.5 μ m) and infrared (wavelength 8～14 μ m) multispectral stealthy, and do not affect snugness of fit.The present invention can be widely used in infrared stealth and the eo stealth engineering field of individual soldier and weaponry, is also suitable for the association area such as heat insulation of building glass, vehicle glass and metal skin simultaneously.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Described method is ordinary method if no special instructions.Described starting material all can obtain from open commercial sources if no special instructions.In following embodiment ball milling step, the material that forms abrading-ball used is zirconium white, and abrading-ball particle diameter is 0.05mm.
Embodiment 1, preparation GAZO powder
Under argon gas atmosphere protection, by 1 weight part Ga, 1 weight part Al, 1 weight part Ga 2o 3, 1 weight part Al 2o 3mix with 96 weight part ZnO, after grinding, 1200 ℃ of insulations, after 1 hour, quench, grind 24 hours, filter, obtain GAZO powder provided by the invention.The particle diameter of this GAZO powder is 180nm.
Embodiment 2, preparation GAZO powder
Under argon gas atmosphere protection, by 0.1 weight part Ga, 2 weight part Al, 3 weight part Ga 2o 3, 0.1 weight part Al 2o 3mix with 94.8 weight part ZnO, after grinding, 1400 ℃ of insulations, after 0.5 hour, quench, grind 24 hours, filter, obtain GAZO powder provided by the invention.The particle diameter of this GAZO powder is 150nm.
Embodiment 3, preparation GAZO powder
Under argon gas atmosphere protection, by 2 weight part Ga, 0.1 weight part Al, 0.1 weight part Ga 2o 3, 3 weight part Al 2o 3mix with 94.8 weight part ZnO, after grinding, 1200 ℃ of insulations, after 3 hours, quench, grind 24 hours, filter, obtain GAZO powder provided by the invention.The particle diameter of this GAZO powder is 160nm.
Embodiment 4, prepare nano paint
(1) water-based GAZO thickened pulp preparation
Take 45 parts of deionized waters of weight part as solvent, the wetting dispersing agent DISPERBYK-190 that weight part is 10 parts, adds successively ball mill and mixes, drum's speed of rotation 5500r/min; Being prepared by embodiment 1 to 45 parts of GAZO powders of gained weight part again and put into grinding in ball grinder 24hr, make GAZO diameter of particle homogeneous more, is 100nm; Through suction filtration, regrind, prepares the water-based GAZO thickened pulp that solid phase quality percentage composition is 50wt%.
(2) coating-forming agent dispersion preparation
Take 10 parts of deionized waters of weight part as solvent, 88 parts of aqueous coating agent Impranil DLC-F of weight part, 2 parts of defoamers of weight part
Figure BDA00001623928900061
foamex 845 adds ball mill jointly to disperse successively, drum's speed of rotation 1000r/min, and jitter time is 0.5hr, it is standby that the coating-forming agent dispersion that obtains solid phase mass content and be 50wt% is waited until next procedure.
(3) coating preparation
Take 59 parts of deionized waters of weight part as solvent, 1 part of crosslinking agent B YK-4500 of weight part, 10 parts of water-based GAZO thickened pulp of weight part, 30 parts of coating-forming agent dispersions of weight part, put into successively ball mill ball milling, drum's speed of rotation is 5000r/min, and Ball-milling Time is 12hr.Wherein, the material of abrading-ball is zirconium white, and all materials and mill ball quality ratio are 1: 1.Through suction filtration, regrind, obtains the water-based low-launch-rate nano paint that solid phase quality percentage composition is 20wt% again.
Embodiment 5, prepare nano paint
(1) water-based GAZO thickened pulp preparation
Take 60 parts of deionized waters of weight part as solvent, the wetting dispersing agent that weight part is 3 parts
Figure BDA00001623928900062
dispers 610, add successively ball mill and mix, drum's speed of rotation 6000r/min; Being prepared by embodiment 1 to 37 parts of GAZO powders of gained weight part again and put into grinding in ball grinder 12hr, make GAZO diameter of particle homogeneous more, is 100nm; Through suction filtration, regrind, preparing solid phase mass content is the water-based GAZO thickened pulp of 40wt%.
(2) coating-forming agent dispersion preparation
Take 12 parts of deionized waters of weight part as solvent, 87 parts of aqueous coating agents of weight part n96101,1 part of defoamer BYK-011 of weight part adds ball mill jointly to disperse successively, drum's speed of rotation 800r/min, jitter time is 0.8hr, it is standby that the coating-forming agent dispersion that obtains solid phase mass content and be 50wt% is waited until next procedure.
(3) coating preparation
Take 49 parts of deionized waters of weight part as solvent, 1 part of linking agent Printofix Fixing agnet ZF of weight part, 15 parts of water-based GAZO thickened pulp of weight part, 35 parts of coating-forming agent dispersions of weight part, put into successively ball mill ball milling, drum's speed of rotation is 6000r/min, and Ball-milling Time is 4hr.Wherein, the material of abrading-ball is zirconium white, and all materials and mill ball quality ratio are 1: 1.Through suction filtration, regrind, obtains the water-based low-launch-rate nano paint that solid phase mass content is 24wt% again.
Embodiment 6, prepare nano paint
(1) water-based GAZO thickened pulp preparation
Take 35 parts of deionized waters of weight part as solvent, the wetting dispersing agent DISPERBYK-2010 that weight part is 10 parts, adds successively ball mill and mixes, drum's speed of rotation 5000r/min; Being prepared by embodiment 2 to 55 parts of GAZO powders of gained weight part again and put into grinding in ball grinder 30hr, make GAZO diameter of particle homogeneous more, is 80nm; Through suction filtration, regrind, preparing solid phase mass content is the water-based GAZO thickened pulp of 60wt%.
(2) coating-forming agent dispersion preparation
Take 8 parts of deionized waters of weight part as solvent, 91.5 parts of aqueous coating agent MW-713 of weight part, 0.5 part of defoamer of weight part foamex 822 adds ball mill jointly to disperse successively, drum's speed of rotation 1500r/min, and jitter time is 0.3hr, it is standby that the coating-forming agent dispersion that obtains solid phase mass content and be 50wt% is waited until next procedure.
(3) coating preparation
Take 39 parts of deionized waters of weight part as solvent, 1 part of linking agent Printofix Fixing agnet ZF of weight part, 15 parts of water-based GAZO thickened pulp of weight part, 35 parts of coating-forming agent dispersions of weight part, put into successively ball mill ball milling, drum's speed of rotation is 4000r/min, and Ball-milling Time is 18hr.Wherein, the material of abrading-ball is silicon carbide, and all materials and mill ball quality ratio are 1: 1.2.Through suction filtration, regrind, obtains the water-based low-launch-rate nano paint that solid phase mass content is 26wt% again.
Embodiment 7, prepare nano paint
(1) oiliness GAZO thickened pulp preparation
Take 32 parts of solvent xylenes of weight part, 14 parts of solvent hexanaphthenes, the wetting dispersing agent DISPERBYK-107 that weight part is 14 parts puts into successively ball mill and mixes, drum's speed of rotation 5800r/min; Being prepared by embodiment 2 to 40 parts of nanometer GAZO powders of gained weight part again and put into grinding in ball grinder 22hr, make GAZO diameter of particle homogeneous more, is 100nm; Through suction filtration, regrind, prepares the oiliness GAZO thickened pulp that solid phase mass content scope is 50wt%;
(2) coating-forming agent dispersion preparation
Take 48 parts of solvent xylenes of weight part, 20 parts of solvent hexanaphthenes; 2 parts of defoamer BYK-088 of weight part add ball mill pre-mixing successively, again by the oiliness coating-forming agent SIS 1106 of 30 parts of weight parts, add ball mill jointly to disperse, drum's speed of rotation 1800r/min, jitter time is 0.8hr, and it is standby that the coating-forming agent dispersion that obtains solid phase mass content and be 30wt% is waited until next procedure.
(3) coating preparation
Take 27 parts of solvent xylenes of weight part, 11 parts of solvent hexanaphthenes; 2 parts of crosslinking agent B YK-4510 of weight part, 10 parts of oiliness GAZO thickened pulp of weight part, 50 parts of coating-forming agent dispersions of weight part, put into ball mill ball milling successively, and drum's speed of rotation is 5000r/min, and Ball-milling Time is 12hr.Wherein, the material of abrading-ball is silicon carbide, and all materials and mill ball quality ratio are 1: 1.2.Through suction filtration, regrind, obtains the oiliness low-launch-rate nano paint that solid phase mass content is 20wt% again.
Embodiment 8, prepare nano paint
(1) oiliness GAZO thickened pulp preparation
Take 28 parts of solvent xylenes of weight part, 12 parts of solvent hexanaphthenes, 7 parts of DISPERBYK-2095 of the wetting dispersing agent DISPERBYK-2091 that weight part is 3 parts and weight part put into successively ball mill and mix, drum's speed of rotation 6000r/min; Being prepared by embodiment 3 to 50 parts of nanometer GAZO powders of gained weight part again and put into grinding in ball grinder 15hr, make GAZO diameter of particle homogeneous more, is 100nm; Through suction filtration, regrind, prepares the oiliness GAZO thickened pulp that solid phase mass content scope is 55wt%;
(2) coating-forming agent dispersion preparation
Take 49 parts of solvent toluenes of weight part, 20 parts of solvent hexanaphthenes; 1 part of defoamer BYK-072 of weight part adds ball mill pre-mixing successively, then by the oiliness coating-forming agent of 30 parts of weight parts
Figure BDA00001623928900081
g1643M Polymer, adds ball mill jointly to disperse, drum's speed of rotation 2000r/min, and jitter time is 0.5hr, it is standby that the coating-forming agent dispersion that obtains solid phase mass content and be 30wt% is waited until next procedure.
(3) coating preparation
Take 20 parts of solvent xylenes of weight part, 9 parts of solvent hexanaphthenes; 1 part of linking agent of weight part
Figure BDA00001623928900082
rad 2250,15 parts of oiliness GAZO thickened pulp of weight part, and 55 parts of coating-forming agent dispersions of weight part, put into ball mill ball milling successively, and drum's speed of rotation is 6000r/min, and Ball-milling Time is 4hr.Wherein, the material of abrading-ball is norbide, and all materials and mill ball quality ratio are 1: 1.5.Through suction filtration, regrind, obtains the oiliness low-launch-rate nano paint that solid phase mass content is 25wt% again.
Embodiment 9, prepare nano paint
(1) oiliness GAZO thickened pulp preparation
Take 25 parts of solvent xylenes of weight part, 25 parts of solvent acetic acid butyl esters, the wetting dispersing agent BYK-P 105 that weight part is 20 parts puts into successively ball mill and mixes, drum's speed of rotation 5600r/min; Being prepared by embodiment 3 to 40 parts of nanometer GAZO powders of gained weight part again and put into grinding in ball grinder 23hr, make GAZO diameter of particle homogeneous more, is 100nm; Through suction filtration, regrind, prepares the oiliness GAZO thickened pulp that solid phase mass content scope is 50wt%;
(2) coating-forming agent dispersion preparation
Take 33 parts of solvent xylenes of weight part, 30 parts of solvent acetic acid butyl esters; 2 parts of defoamer BYK-085 of weight part add ball mill pre-mixing successively, again by the oiliness coating-forming agent EEANUC 4107 of 35 parts of weight parts, add ball mill jointly to disperse, drum's speed of rotation 2500r/min, jitter time is 0.3hr, and it is standby that the coating-forming agent dispersion that obtains solid phase mass content and be 40wt% is waited until next procedure.
(3) coating preparation
Take 14.5 parts of solvent xylenes of weight part, 14.5 parts of solvent acetic acid butyl esters; 1 part of crosslinking agent B YK-4510 of weight part, 20 parts of oiliness GAZO thickened pulp of weight part, 50 parts of coating-forming agent dispersions of weight part, put into ball mill ball milling successively, and drum's speed of rotation is 4000r/min, and Ball-milling Time is 18hr.Wherein, the material of abrading-ball is norbide, and all materials and mill ball quality ratio are 1: 1.5.Through suction filtration, regrind, obtains the oiliness low-launch-rate nano paint that solid phase mass content is 30% again.
Above-described embodiment is prepared to gained nano paint and be coated in woven fabric, looped fabric, non-woven fabrics or synthetic leather surface, according to relevant criterion, test, after test, coated fabric physicochemical property is as shown in table 2.
The test of table 2 coated fabric physicochemical property
Figure BDA00001623928900091
As shown in Table 2, the various colour fastness indexs of coated fabric all reach more than 4 grades, hydrothermal aging continue after 28 days appearance of coat unchanged, without adhesion, can compatible visible ray, near infrared (wavelength 0.38～2.5 μ m) and infrared (wavelength 8～14 μ m) multispectral stealthy, and do not affect snugness of fit, there is important using value.

Claims (14)

1. a nanometer GAZO powder, is prepared and is obtained by following raw material: Ga, Al, Ga 2o 3, Al 2o 3and ZnO;
The consumption umber of described each raw material is respectively: Ga:0.1-2 weight part, Al:0.1-2 weight part, Ga 2o 3: 0.1-3 weight part, Al 2o 3: 0.1-3 weight part, ZnO:90-99.6 weight part.
2. nanometer GAZO powder according to claim 1, is characterized in that: the consumption umber of described each raw material is respectively: Ga:1 weight part, Al:1 weight part, Ga 2o 3: 1 weight part, Al 2o 3: 1 weight part, ZnO:96 weight part;
The particle diameter of described nanometer GAZO powder is 20-200nm.
3. a method of preparing nanometer GAZO powder described in claim 1 or 2; comprise the steps: under inert atmosphere protection; by after each raw material blending described in claim 1 or 2, in 1000-1400 ℃ of insulation, after 0.5-3 hour, quench again, grind, obtain described nanometer GAZO powder.
4. a nano paint, comprises coating-forming agent and additive;
Wherein, described coating-forming agent is selected from any one in aqueous coating agent and oiliness coating-forming agent;
Described additive comprises filler, wetting dispersing agent, linking agent, defoamer and solvent;
Described filler is the nanometer GAZO powder described in claim 1 or 2.
5. nano paint according to claim 4, is characterized in that: described wetting dispersing agent be selected from BYK-9076, BYK-9077, dispers610,
Figure FDA0000409953250000012
dispers610S, dispers651, dispers652,
Figure FDA0000409953250000015
dispers700,
Figure FDA0000409953250000016
dispers710,
Figure FDA0000409953250000017
dispers715W,
Figure FDA0000409953250000018
dispers735W,
Figure FDA0000409953250000019
dispers740W,
Figure FDA00004099532500000110
dispers745W,
Figure FDA00004099532500000111
dispers750W,
Figure FDA00004099532500000112
dispers752W,
Figure FDA00004099532500000113
dispers760W, Surfynol CT-324, Surfynol CT-136, DISPERBYK-190, DISPERBYK-191, DISPERBYK-2010, DISPERBYK-2090, DISPERBYK-2091, DISPERBYK-2095, DISPERBYK-107, BYK-P105, Irgaflow tM100, Irgaflow tM110,
Figure FDA00004099532500000114
wet KL245,
Figure FDA00004099532500000115
wet KL280,
Figure FDA00004099532500000116
wet250,
Figure FDA00004099532500000117
wet260,
Figure FDA00004099532500000118
wet265,
Figure FDA00004099532500000119
wet265,
Figure FDA00004099532500000120
wet270,
Figure FDA00004099532500000121
wet280,
Figure FDA00004099532500000122
wet500, AD41-5033,
Figure FDA00004099532500000123
wet505,
Figure FDA00004099532500000124
fSO,
Figure FDA00004099532500000125
fSA, fSN,
Figure FDA00004099532500000127
fSP, Tergitol NP-10,
Figure FDA00004099532500000128
4430,
Figure FDA00004099532500000129
4432,
Figure FDA00004099532500000130
at least one in 4434, Surfynol420, Surfynol440, Surfynol465, Surfynol485 and Surfynol104E;
Described linking agent be selected from BYK-4500, BYK-4510,
Figure FDA00004099532500000131
rad2100,
Figure FDA00004099532500000132
rad2200N,
Figure FDA00004099532500000133
rad2250, rad2300,
Figure FDA00004099532500000135
at least one in Rad2500 and Printofix Fixing agnet ZF;
Described defoamer be selected from BYK-011, BYK-012, BYK-016, BYK-020, BYK-022, BYK-088, BYK-072, BYK-085,
Figure FDA00004099532500000136
foamex810, TEGO Foamex825,
Figure FDA00004099532500000137
foamex822,
Figure FDA00004099532500000138
foamex845,
Figure FDA00004099532500000139
at least one in Foamex1488, Surfynol DF-110D and Surfynol DF-75;
Described solvent is selected from deionized water, distilled water, ethyl acetate, methyl acetate, butylacetate, propylene glycol methyl ether acetate, ethylene glycol ether acetate, propylene glycol monomethyl ether, benzene,toluene,xylene, hexanaphthene, methylcyclohexane, p-chloro benzo trifluoride-99, isopropyl acetate, 1, at least one in 1,1-trichloromethane, methyl iso-butyl ketone (MIBK) and the acetic acid trimethyl carbinol;
Described aqueous coating agent is selected from
Figure FDA0000409953250000021
n96101,
Figure FDA0000409953250000022
n96110,
Figure FDA0000409953250000023
at least one in N96111, Impranil DLC-F and MW-713;
Described oiliness coating-forming agent be selected from EEA NUC4107, SIS1105, SIS1106, g1643M Polymer, d1161J and
Figure FDA0000409953250000026
at least one in D1702H;
The particle diameter of described nanometer GAZO powder is 20-200nm;
The mass ratio of described coating-forming agent and additive is 5-30:70-95;
In described additive, the mass ratio of described filler, wetting dispersing agent, linking agent, defoamer and solvent is 1.75-14:0.1-2:0.1-3:0.1-1:65-82.95.
6. nano paint according to claim 5, is characterized in that: the mass ratio of described coating-forming agent and additive is 15:85;
In described additive, the mass ratio of described filler, wetting dispersing agent, linking agent, defoamer and solvent is 8:1:0.5:0.5:75.
7. according to the nano paint described in any one in claim 4-6, it is characterized in that: the particle diameter of described nano paint is less than 100nm, viscosity is 8～15cP, surface tension is 20～36mN/m, the quality percentage composition of solid phase is 1～60%, the normal temperature storage time is no less than 6 months, and average resistivity is 4.5 * 10 -3Ω cm.
8. prepare in claim 4-7 a method for nano paint described in any one, comprise the steps: arbitrary described each component in claim 4-6 to carry out ball milling after mixing, obtain described nano paint.
9. method according to claim 8, is characterized in that: described mixing step comprises:
1) the described wetting dispersing agent of 0.1～20 part of the described solvent of 30～85 parts of weight parts, weight part is mixed and carries out ball milling with the described GAZO powder of 5～70 parts of weight parts, while making the particle diameter of described GAZO powder be 10-100nm, stop described ball milling, obtain GAZO thickened pulp; In described GAZO thickened pulp, the quality percentage composition of solid phase is 10～80%; In described ball milling step, the rotating speed of ball mill is 500～6000r/min, and Ball-milling Time is 2-48hr;
2) coating-forming agent of 30～92 parts of described defoamer, the weight parts of 0.1～20 part of the described solvent of 30～90 parts of weight parts, weight part is mixed and carries out ball milling, obtain coating-forming agent dispersion; In described ball milling step, the rotating speed of ball mill is 500～6000r/min, and the time is 0.1～1hr;
3) by the described step 2 of 1～80 part of the described step 1) gained GAZO thickened pulp of 1～80 part of described linking agent, the weight part of 0.1～20 part of the described solvent of 1～95 part of weight part, weight part and weight part) gained coating-forming agent dispersion mixes and carries out ball milling, obtains described nano paint; In described ball milling step, the rotating speed of ball mill is 500～6000r/min, and Ball-milling Time is 1-24hr;
All materials that in described claim 4-6, arbitrary described each component forms and the mass ratio of ball milling step abrading-ball used are 2:1～1:3; The material that forms described abrading-ball is silicon carbide, zirconium white or norbide; The particle diameter of described abrading-ball is 0.03～2mm.
10. method according to claim 9, is characterized in that:
In described step 1), in described GAZO thickened pulp, the quality percentage composition of solid phase is 40～60%; In described ball milling step, Ball-milling Time is 4-32hr;
Described step 2), in, in described ball milling step, Ball-milling Time is 0.3～0.8hr;
Described step 2), in, in described ball milling step, Ball-milling Time is 2-18hr;
All materials that in described claim 4-6, arbitrary described each component forms and the mass ratio of ball milling step abrading-ball used are 1:1～1:1.5; The particle diameter of described abrading-ball is 0.04～0.8mm.
11. take the fabric with infrared stealth function that described in any one, nano paint is coating in claim 4-7.
12. fabrics according to claim 11, is characterized in that: the body material in described fabric is selected from least one in woven fabrics, knitted fabrics, non-woven fabrics, synthetic leather, glass and metal skin;
The top coat colour fastness of described fabric is 4 grades; Described fabric is that 0.38～2.5 visible ray of μ m is, the average transmittances of near-infrared band is more than 90% at wavelength; The average emitted rate that is 8～14 μ m infrared bands at wavelength is 0.5～0.75.
In 13. claim 4-7, described in any one, nano paint has the application in the fabric of infrared stealth function in preparation.
14. application according to claim 13, is characterized in that: the body material in described fabric is selected from least one in woven fabrics, knitted fabrics, non-woven fabrics, synthetic leather, glass and metal skin;
The top coat colour fastness of described fabric is 4 grades; Described fabric is that 0.38～2.5 visible ray of μ m is, the average transmittances of near-infrared band is more than 90% at wavelength; The average emitted rate that is 8～14 μ m infrared bands at wavelength is 0.5～0.75.
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