CN102757676A - Low-emissivity nano-coating and preparation method and application thereof - Google Patents
Low-emissivity nano-coating and preparation method and application thereof Download PDFInfo
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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
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, reached 0.1～0.2mrad in the spatial resolution of the thermal infrared imaging instrument of infrared band (wavelength 8～14 μ m) work, temperature resolution reaches 0.1～0.3 ℃.Infrared stealth technology has caused the great attention of various countries as the important factor that improves combat unit viability, penetration ability and fighting efficiency, and the importance in the information war grows with each passing day in modern times.Infrared stealth technology roughly may be summarized to be and changes ir radiation wave band, reduction infrared intensity, three aspects of adjusting ir radiation transmission course.Apply the infrared stealth coating at target surface and can reduce its infrared intensity, and the research of low-launch-rate coating is the key of infrared stealth coating prepn research.Wherein, 8～14 mu m wavebands are one of important wave bands of infrared thermal imaging.
General infrared stealth coating is made up of coating-forming agent and additive.Described coating-forming agent is meant the polymeric coating layer agent with certain infrared transparent performance; Described additive comprises: filler, wetting dispersing agent, skimmer, linking agent, solvent, thinner etc.; Described filler comprises metallic stuffing, semiconductor fills.Research shows that coating-forming agent accounts for more than 60% for the influence of coating emittance, and the infrared emittance of most of common coating-forming agents is difficult to satisfy the low-launch-rate needs of infrared stealth all than higher.Have the investigator to synthesize the infrared transparent coating-forming agent, so as to reducing the coating emittance, wherein with modified EPT rubber typical case the most, but that its shortcoming is an adhesion strength is low, in practical application, comes off easily.Then there are problems such as non-refractory and resistance to deterioration difference in the conductive polymer coating-forming agent.In numerous fillers; Metallic stuffing is to report maximum low-launch-rate fillers up to now, and the shortcoming of its existence is that the metallic stuffing reflectivity is high, is unfavorable in multiband compatibilities such as visible light, radar and laser stealthy; And metallic stuffing is prone to oxidation in air, its infrared emittance is significantly raise; Simultaneously, after the low-launch-rate coating of being processed by metallic stuffing was coated on fabric, feel was hardened, and adhered to fastness and can not satisfy actual needs.The combination of semiconductor fills and infrared transparent coating-forming agent can effectively overcome above shortcoming, thereby the emphasis that becomes research and use.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 preparation low emissivity coatings, realization infrared stealth.
The 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.Because raw material In, the Sn of preparation 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 the 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 higher with the coating emittance of its preparation.Zinc oxide codoped gallium aluminium (Gallium and Aluminum Co-doped Zinc Oxide; GAZO) be a kind of semiconductor material with low-launch-rate; Research to GAZO both at home and abroad focuses mostly at the GAZO sputtered film, and the GAZO powder is not also appeared in the newspapers as the research that filler is used for the infrared stealth material.
Summary of the invention
The purpose 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 got by following feedstock production: Ga, Al, Ga
2O
3, Al
2O
3And ZnO.
In the above-mentioned nanometer GAZO powder, the consumption umber of said 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; Each raw material of preferred following 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 said 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, behind aforementioned each raw material blending, quenches after 0.5-3 hour in 1000-1400 ℃ of insulation again, obtains said nanometer GAZO powder.
After said quenching step, also can according to actual needs products therefrom be ground, filter.Said inert atmosphere specifically can be nitrogen atmosphere or argon gas atmosphere.
Nano paint provided by the invention comprises coating-forming agent and additive;
Wherein, said coating-forming agent is selected from any one in aqueous coating agent and the oiliness coating-forming agent;
Said nano paint also can only be made up of said components.
Said additive comprises filler, wetting dispersing agent, linking agent, skimmer and solvent;
Said filler is a nanometer GAZO powder;
Said wetting dispersing agent be selected from BYK-9076, BYK-9077,
Dispers 610,
Dispers610S,
Dispers 651,
Dispers 652,
Dispers 700,
Dispers 710,
Dispers 715W,
Dispers 735W,
Dispers 740W,
Dispers 745W,
Dispers 750W,
Dispers 752W,
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,
Wet KL245,
Wet KL280,
Wet250,
Wet 260,
Wet 265,
Wet 265,
Wet 270,
Wet 280,
Wet 500, AD41-5033,
Wet 505,
FSO,
FSA,
FSN,
FSP, Tergitol NP-10,
4430,
4432,
4434, at least a among Surfynol 420, Surfynol 440, Surfynol 465, Surfynol 485, the Surfynol 104E;
Said linking agent is selected from BYK-4500; BYK-4510;
Rad 2100;
Rad 2200N;
Rad 2250;
Rad 2300;
Rad 2500; At least a among the Printofix Fixing agnet ZF;
Said skimmer is selected from BYK-011; BYK-012; BYK-016; BYK-020; BYK-022; BYK-088; BYK-072; BYK-085;
Foamex 810; TEGO Foamex 825;
Foamex 822;
Foamex 845;
Foamex 1488; Surfynol DF-110D; At least a among the Surfynol DF-75;
Wherein, the product of DISPERBYK and BYK is that BYK company provides;
Product provide by Goldschmidt chemical company;
Product provide by E.I.Du Pont Company; Tergitol NP-10 is provided by Dow company; The product of Surfynol is provided by U.S. aerification chemical product company;
Product provide by 3M company; Irgaflow
TMProduct provide by BASF Ta Fuka;
Said solvent is selected from deionized water, zero(ppm) water, ETHYLE 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; 1, at least a in 1-trichloromethane, MIBK and the acetate trimethyl carbinol;
Said aqueous coating agent is selected from
N96101;
N96110;
N96111; Impranil DLC-F; At least a among the MW-713;
Said oiliness coating-forming agent is selected from EEA NUC 4107; SIS 1105; SIS 1106;
G1643MPolymer;
D1161J; At least a among
D1702H;
Wherein, the product of
is provided by Clariant company; MW-713 is provided by Shanghai Mowang Composite Materials Co., Ltd.; The product of SIS is provided by Yueyang petrochemical industry; The product of
is risen Polymer Company by U.S. section to be provided; EEANUC 4107 is provided by Japanese NUC company;
Said additive is by said filler, wetting dispersing agent, linking agent, skimmer and solvent composition;
The mass ratio of said coating-forming agent and additive is 5-30: 70-95, and (the indication quality was the total mass that belongs to all components of coating-forming agent or additive here in preferred 15: 85.)；
In the said additive, the mass ratio of said filler, wetting dispersing agent, linking agent, skimmer and solvent is 1.75-14: 0.1-2: 0.1-3: 0.1-1: 65-82.95, preferred 8: 1: 0.5: 0.5: 75.
The particle diameter of said 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 said nano paint of preparation provided by the invention comprises the steps: to obtain said nano paint with carrying out ball milling after aforementioned each component mixing.
In the said ball milling step, the rotating speed of ball mill is 500～6000r/min, and the time is 1～24hr; All materials that said each component is formed and the mass ratio of the used abrading-ball of ball milling step are 2: 1～1: 3, preferred 1: 1～1: 1.5; The material that constitutes said abrading-ball is silit, zirconium white or norbide; The particle diameter of said abrading-ball is 0.03～2mm, preferred 0.04～0.8mm.
In actually operating, said mixing step can specifically comprise the steps:
1) the said wetting dispersing agent of 0.1～20 part of said solvent, the weight part of 30～85 parts of weight parts is mixed with the said GAZO powder of 5～70 parts of weight parts carries out ball milling; Stop said ball milling when making the particle diameter of said GAZO powder be 10～100nm, obtain the GAZO thickened pulp;
2) coating-forming agent of 30～92 parts of said skimmer, the weight parts of 0.1～20 part of said solvent, the weight part of 30～90 parts of weight parts is mixed carry out ball milling, obtain the coating-forming agent dispersion-s; In the said ball milling step, the rotating speed of ball mill is 500～6000r/min, and the time is 0.1～1hr, preferred 0.3～0.8hr;
3) with the said step 2 of 1～80 part of the said step 1) gained GAZO thickened pulp of 1～80 part of said linking agent, the weight part of 0.1～20 part of said solvent, the weight part of 1～95 part of weight part and weight part) gained coating-forming agent dispersion-s mixes and carries out ball milling, obtains said nano paint.
Above-mentioned steps 1) in, the quality percentage composition of solid phase is 10～80% in the said GAZO thickened pulp, preferred 40～60%;
The said wetting dispersing agent that said said solvent with 30～85 parts of weight parts, weight part are 0.1～20 part mixes with the said GAZO powder of 5～70 parts of weight parts and carries out in the ball milling step; The rotating speed of ball mill is 500～6000r/min; The ball milling time is 2-48hr, preferred 4-32hr;
Step 2) in; The coating-forming agent that said skimmer, the weight part that said said solvent with 30～90 parts of weight parts, weight part are 0.1～20 part is 30～80 parts mixes and carries out in the ball milling step; The rotating speed of ball mill is 500～6000r/min, and the time is 0.1～1hr, preferred 0.3～0.8hr;
In the step 3); The coating-forming agent that said skimmer, the weight part that said said solvent with 30～90 parts of weight parts, weight part are 0.1～20 part is 30～80 parts mixes and carries out in the ball milling step; The rotating speed of ball mill is 500～6000r/min, and the ball milling time is 1-24hr, preferred 2-18hr.
With above-mentioned nano paint provided by the invention is the fabric with infrared stealth function of coating; And this nano paint has the application in the fabric of infrared stealth function in preparation, also belongs to protection scope of the present invention.Wherein, the body material in the said fabric is selected from least a in woven fabrics, knitted fabrics, non-woven fabrics, synthetic leather, glass and the metal skin; The top coat colour fastness of said fabric is 4 grades; Said fabric is that the visible light wave range of 0.38～2.5 μ m, the average transmittances of near-infrared band are more than 90% at wavelength; At wavelength is that the average emitted rate of 8～14 μ m infrared bands is 0.5～0.75.
Compared with present technology the present invention has following advantage:
1, the particle diameter that utilizes the low-launch-rate nano paint that the inventive method makes is less than 100nm, viscosity 8～15cP, surface tension 20～36mN/m; Adjustable in solid phase quality percentage composition 1～60wt% scope; Normal temperature can store more than 6 months, and system is stable, was convenient to transportation.
2, the nano paint that utilizes the inventive method to make; Mode is coated on woven cloth, looped fabric, non-woven fabrics or synthetic leather surface to adopt numerial code spray drawing, screen printing, blade coating, spray, pad etc.; Through oven dry or hot-pressing processing, promptly process low emissivity coatings fabric again with infrared stealth function.Owing to need not washing after nano paint of the present invention oven dry or the hot pressing, so can reduce environmental pollution significantly, the 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%; The coating average resistivity is 4.5 * 10
-3Ω cm; In the average emitted rate of infrared band (wavelength 8～14 μ m) is 0.5～0.75 adjustable.The present invention can carry out the material surface application of infrared stealth at multiple need, has wide Application Areas.
The low emissivity coatings material that utilizes the inventive method to process is suitable for making thermal infrared stealth camouflage fatigue, camouflage net and tent etc.; On the basis that does not reduce the existing product physicochemical property; Can compatible visible light, near infrared (wavelength 0.38～2.5 μ m) and infrared (wavelength 8～14 μ m) multispectral stealthy, and do not influence snugness of fit.The present invention can be widely used in the infrared stealth and the eo stealth engineering field of individual soldier and weaponry, also is suitable for simultaneously the association area such as heat insulation of building glass, vehicle glass and metal skin.
Embodiment
Below in conjunction with specific embodiment the present invention is done further elaboration, but the present invention is not limited to following examples.Said method is ordinary method if no special instructions.Said starting material all can get from open commercial sources if no special instructions.In the following embodiment ball milling step, the material that constitutes used abrading-ball is zirconium white, and the abrading-ball particle diameter is 0.05mm.
Embodiment 1, preparation GAZO powder
Under the argon gas atmosphere protection, with 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 the grinding, after 1 hour, quench, ground 24 hours, filter, obtain GAZO powder provided by the invention 1200 ℃ of insulations.The particle diameter of this GAZO powder is 180nm.
Embodiment 2, preparation GAZO powder
Under the argon gas atmosphere protection, with 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 the grinding, after 0.5 hour, quench, ground 24 hours, filter, obtain GAZO powder provided by the invention 1400 ℃ of insulations.The particle diameter of this GAZO powder is 150nm.
Embodiment 3, preparation GAZO powder
Under the argon gas atmosphere protection, with 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 the grinding, after 3 hours, quench, ground 24 hours, filter, obtain GAZO powder provided by the invention 1200 ℃ of insulations.The particle diameter of this GAZO powder is 160nm.
Embodiment 4, preparation nano paint
(1) water-based GAZO thickened pulp preparation
Take by weighing 45 parts of deionized waters of weight part as solvent, the wetting dispersing agent DISPERBYK-190 that weight part is 10 parts adds ball mill successively and mixes drum's speed of rotation 5500r/min; Again 45 parts of GAZO powders of embodiment 1 preparation gained weight part are put into grinding in ball grinder 24hr, make GAZO diameter of particle homogeneous more, be 100nm; Through suction filtration, the water-based GAZO thickened pulp that solid phase quality percentage composition is 50wt% is prepared in regrind.
(2) coating-forming agent dispersion-s preparation
Take by weighing 10 parts of deionized waters of weight part as solvent; 88 parts of aqueous coating agent Impranil of weight part DLC-F; 2 parts of skimmers of weight part
Foamex 845 adds the ball mill co-dispersed successively; Drum's speed of rotation 1000r/min; Jitter time is 0.5hr, and it is subsequent use that the coating-forming agent dispersion-s that obtains the solid phase mass content and be 50wt% is waited until next procedure.
(3) coating preparation
Take by weighing 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 of weight part thickened pulp; 30 parts of coating-forming agent dispersion-ss of weight part; Put into the ball mill ball milling successively, drum's speed of rotation is 5000r/min, and the ball milling time is 12hr.Wherein, the material of abrading-ball is a zirconium white, and all materials and mill ball quality ratio are 1: 1.Again through suction filtration, regrind, obtaining solid phase quality percentage composition is the water-based low-launch-rate nano paint of 20wt%.
Embodiment 5, preparation nano paint
(1) water-based GAZO thickened pulp preparation
Take by weighing 60 parts of deionized waters of weight part as solvent; The wetting dispersing agent that weight part is 3 parts
Dispers 610; Add ball mill successively and mix drum's speed of rotation 6000r/min; Again 37 parts of GAZO powders of embodiment 1 preparation gained weight part are put into grinding in ball grinder 12hr, make GAZO diameter of particle homogeneous more, be 100nm; Through suction filtration, regrind, preparing the solid phase mass content is the water-based GAZO thickened pulp of 40wt%.
(2) coating-forming agent dispersion-s preparation
Take by weighing 12 parts of deionized waters of weight part as solvent; 87 parts of aqueous coating agents of weight part
N96101; 1 part of skimmer BYK-011 of weight part adds the ball mill co-dispersed successively; Drum's speed of rotation 800r/min; Jitter time is 0.8hr, and it is subsequent use that the coating-forming agent dispersion-s that obtains the solid phase mass content and be 50wt% is waited until next procedure.
(3) coating preparation
Take by weighing 49 parts of deionized waters of weight part as solvent, 1 part of linking agent Printofix of weight part Fixing agnet ZF, 15 parts of water-based GAZO of weight part thickened pulp; 35 parts of coating-forming agent dispersion-ss of weight part; Put into the ball mill ball milling successively, drum's speed of rotation is 6000r/min, and the ball milling time is 4hr.Wherein, the material of abrading-ball is a zirconium white, and all materials and mill ball quality ratio are 1: 1.Again through suction filtration, regrind, obtaining the solid phase mass content is the water-based low-launch-rate nano paint of 24wt%.
Embodiment 6, preparation nano paint
(1) water-based GAZO thickened pulp preparation
Take by weighing 35 parts of deionized waters of weight part as solvent, the wetting dispersing agent DISPERBYK-2010 that weight part is 10 parts adds ball mill successively and mixes drum's speed of rotation 5000r/min; Again 55 parts of GAZO powders of embodiment 2 preparation gained weight parts are put into grinding in ball grinder 30hr, make GAZO diameter of particle homogeneous more, be 80nm; Through suction filtration, regrind, preparing the solid phase mass content is the water-based GAZO thickened pulp of 60wt%.
(2) coating-forming agent dispersion-s preparation
Take by weighing 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 skimmer of weight part
Foamex 822 adds the ball mill co-dispersed successively; Drum's speed of rotation 1500r/min; Jitter time is 0.3hr, and it is subsequent use that the coating-forming agent dispersion-s that obtains the solid phase mass content and be 50wt% is waited until next procedure.
(3) coating preparation
Take by weighing 39 parts of deionized waters of weight part as solvent, 1 part of linking agent Printofix of weight part Fixing agnet ZF, 15 parts of water-based GAZO of weight part thickened pulp; 35 parts of coating-forming agent dispersion-ss of weight part; Put into the ball mill ball milling successively, drum's speed of rotation is 4000r/min, and the ball milling time is 18hr.Wherein, the material of abrading-ball is a silit, and all materials and mill ball quality ratio are 1: 1.2.Again through suction filtration, regrind, obtaining the solid phase mass content is the water-based low-launch-rate nano paint of 26wt%.
Embodiment 7, preparation nano paint
(1) oiliness GAZO thickened pulp preparation
Take by weighing 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 ball mill successively and mixes, drum's speed of rotation 5800r/min; Again 40 parts of nanometer GAZO of embodiment 2 preparation gained weight parts powder is put into grinding in ball grinder 22hr, make GAZO diameter of particle homogeneous more, be 100nm; Through suction filtration, the oiliness GAZO thickened pulp that solid phase mass content scope is 50wt% is prepared in regrind;
(2) coating-forming agent dispersion-s preparation
Take by weighing 48 parts of solvent xylenes of weight part, 20 parts of solvent hexanaphthenes; 2 parts of skimmer BYK-088 of weight part add the ball mill pre-mixing successively; Again with the oiliness coating-forming agent SIS 1106 of 30 parts of weight parts; Add the ball mill co-dispersed; Drum's speed of rotation 1800r/min, jitter time is 0.8hr, it is subsequent use that the coating-forming agent dispersion-s that obtains the solid phase mass content and be 30wt% is waited until next procedure.
(3) coating preparation
Take by weighing 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 of weight part thickened pulp, 50 parts of coating-forming agent dispersion-ss of weight part are put into the ball mill ball milling successively, and drum's speed of rotation is 5000r/min, and the ball milling time is 12hr.Wherein, the material of abrading-ball is a silit, and all materials and mill ball quality ratio are 1: 1.2.Again through suction filtration, regrind, obtaining the solid phase mass content is the oiliness low-launch-rate nano paint of 20wt%.
Embodiment 8, preparation nano paint
(1) oiliness GAZO thickened pulp preparation
Take by weighing 28 parts of solvent xylenes of weight part, 12 parts of solvent hexanaphthenes, 7 parts of DISPERBYK-2095 of wetting dispersing agent DISPERBYK-2091 that weight part is 3 parts and weight part put into ball mill successively and mix drum's speed of rotation 6000r/min; Again 50 parts of nanometer GAZO of embodiment 3 preparation gained weight parts powder is put into grinding in ball grinder 15hr, make GAZO diameter of particle homogeneous more, be 100nm; Through suction filtration, the oiliness GAZO thickened pulp that solid phase mass content scope is 55wt% is prepared in regrind;
(2) coating-forming agent dispersion-s preparation
Take by weighing 49 parts of solvent toluenes of weight part, 20 parts of solvent hexanaphthenes; 1 part of skimmer BYK-072 of weight part adds the ball mill pre-mixing successively; Again with oiliness coating-forming agent
the G1643M Polymer of 30 parts of weight parts; Add the ball mill co-dispersed; Drum's speed of rotation 2000r/min; Jitter time is 0.5hr, and it is subsequent use that the coating-forming agent dispersion-s that obtains the solid phase mass content and be 30wt% is waited until next procedure.
(3) coating preparation
Take by weighing 20 parts of solvent xylenes of weight part, 9 parts of solvent hexanaphthenes; 1 part of linking agent of weight part
Rad 2250; 15 parts of oiliness GAZO of weight part thickened pulp; 55 parts of coating-forming agent dispersion-ss of weight part; Put into the ball mill ball milling successively, drum's speed of rotation is 6000r/min, and the ball milling time is 4hr.Wherein, the material of abrading-ball is a norbide, and all materials and mill ball quality ratio are 1: 1.5.Again through suction filtration, regrind, obtaining the solid phase mass content is the oiliness low-launch-rate nano paint of 25wt%.
Embodiment 9, preparation nano paint
(1) oiliness GAZO thickened pulp preparation
Take by weighing 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 ball mill successively and mixes, drum's speed of rotation 5600r/min; Again 40 parts of nanometer GAZO of embodiment 3 preparation gained weight parts powder is put into grinding in ball grinder 23hr, make GAZO diameter of particle homogeneous more, be 100nm; Through suction filtration, the oiliness GAZO thickened pulp that solid phase mass content scope is 50wt% is prepared in regrind;
(2) coating-forming agent dispersion-s preparation
Take by weighing 33 parts of solvent xylenes of weight part, 30 parts of solvent acetic acid butyl esters; 2 parts of skimmer BYK-085 of weight part add the ball mill pre-mixing successively; Again with the oiliness coating-forming agent EEANUC 4107 of 35 parts of weight parts; Add the ball mill co-dispersed; Drum's speed of rotation 2500r/min, jitter time is 0.3hr, it is subsequent use that the coating-forming agent dispersion-s that obtains the solid phase mass content and be 40wt% is waited until next procedure.
(3) coating preparation
Take by weighing 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 of weight part thickened pulp, 50 parts of coating-forming agent dispersion-ss of weight part are put into the ball mill ball milling successively, and drum's speed of rotation is 4000r/min, and the ball milling time is 18hr.Wherein, the material of abrading-ball is a norbide, and all materials and mill ball quality ratio are 1: 1.5.Again through suction filtration, regrind obtains the solid phase mass content and is 30% oiliness low-launch-rate nano paint.
The foregoing description is prepared the gained nano paint be coated in woven cloth, looped fabric, non-woven fabrics or synthetic leather surface, test according to relevant criterion, test back coated fabric physicochemical property is as shown in table 2.
The test of table 2 coated fabric physicochemical property
Can know by table 2; The various colour fastness indexs of coated fabric all reach more than 4 grades; Hydrothermal aging continues appearance of coat no change, no adhesion after 28 days; Can compatible visible light, near infrared (wavelength 0.38～2.5 μ m) and infrared (wavelength 8～14 μ m) multispectral stealthy, and do not influence snugness of fit, have important use and be worth.
Claims (10)
1. a nanometer GAZO powder is got by following feedstock production: Ga, Al, Ga
2O
3, Al
2O
3And ZnO.
2. nanometer GAZO powder according to claim 1 is characterized in that: the consumption umber of said 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; Each raw material of preferred following 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 said nanometer GAZO powder is 20-200nm.
3. method for preparing the arbitrary said nanometer GAZO powder of claim 1-2; Comprise the steps: under inert atmosphere protection; Behind arbitrary said each raw material blending of claim 1-3, quench again after 0.5-3 hour in 1000-1400 ℃ of insulation, obtain said nanometer GAZO powder.
4. a nano paint comprises coating-forming agent and additive;
Wherein, said coating-forming agent is selected from any one in aqueous coating agent and the oiliness coating-forming agent;
Said additive comprises filler, wetting dispersing agent, linking agent, skimmer and solvent;
Said filler is a nanometer GAZO powder.
5. nano paint according to claim 4 is characterized in that: said wetting dispersing agent be selected from BYK-9076, BYK-9077,
Dispers 610,
Dispers 610S,
Dispers 651,
Dispers652,
Dispers 700,
Dispers 710,
Dispers 715W,
Dispers 735W,
Dispers 740W,
Dispers 745W,
Dispers 750W,
Dispers 752W,
Dispers 760W, Surfynol CT-324, Surfynol CT-136, DISPERBYK-190, DISPERBYK-191, DISPERBYK-2010, DISPERBYK-2090, DISPERBYK-2091, DISPERBYK-2095, DISPERBYK-107, BYK-P 105, Irgaflow
TM100, Irgaflow
TM110,
Wet KL245,
Wet KL280,
Wet 250,
Wet 260,
Wet 265,
Wet 265,
Wet 270,
Wet 280,
Wet 500, AD41-5033,
Wet505,
FSO,
FSA,
FSN,
FSP, Tergitol NP-10,
4430,
4432,
4434, at least a among Surfynol 420, Surfynol 440, Surfynol 465, Surfynol 485 and the Surfynol104E;
Said linking agent is selected from BYK-4500; BYK-4510;
Rad 2100;
Rad 2200N;
Rad 2250;
Rad 2300; At least a among
Rad 2500 and the Printofix Fixing agnet ZF; Said skimmer is selected from BYK-011; BYK-012; BYK-016; BYK-020; BYK-022; BYK-088; BYK-072; BYK-085;
Foamex 810; TEGO Foamex 825;
Foamex 822;
Foamex 845;
Foamex 1488; At least a among Surfynol DF-110D and the Surfynol DF-75;
Said solvent is selected from deionized water, zero(ppm) water, ETHYLE 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; 1, at least a in 1-trichloromethane, MIBK and the acetate trimethyl carbinol;
The aqueous coating agent selected from the group
N96101,
N96110,
N96111, Impranil? DLC-F and MW-713 is at least one;
Said oiliness coating-forming agent is selected from EEA NUC 4107; SIS 1105; SIS 1106;
G1643MPolymer; At least a among
D1161J and
D1702H;
The particle diameter of said nanometer GAZO powder is 20-200nm;
The mass ratio of said coating-forming agent and additive is 5-30:70-95, preferred 15:85;
In the said additive, the mass ratio of said filler, wetting dispersing agent, linking agent, skimmer and solvent is 1.75-14: 0.1-2: 0.1-3: 0.1-1: 65-82.95, preferred 8: 1: 0.5: 0.5: 75.
6. according to claim 4 or 5 described nano paints, it is characterized in that: the particle diameter of said nano paint is less than 100nm, and viscosity is 8～15cP; Surface tension is 20～36mN/m; The quality percentage composition of solid phase is 1～60%, and the normal temperature storage time is no less than 6 months, and average resistivity is 4.5 * 10
-3Ω cm.
7. a method for preparing the arbitrary said nano paint of claim 4-6 comprises the steps: to obtain said nano paint with carrying out ball milling after arbitrary said each component mixing of claim 4-5.
8. method according to claim 7 is characterized in that: said mixing step comprises:
1) the said wetting dispersing agent of 0.1～20 part of said solvent, the weight part of 30～85 parts of weight parts is mixed with the said GAZO powder of 5～70 parts of weight parts carries out ball milling; Stop said ball milling when making the particle diameter of said GAZO powder be 10～100nm, obtain the GAZO thickened pulp; In the said GAZO thickened pulp, the quality percentage composition of solid phase is 10～80%, preferred 40～60%; In the said ball milling step, the rotating speed of ball mill is 500～6000r/min, and the ball milling time is 2-48hr, preferred 4-32hr;
2) coating-forming agent of 30～92 parts of said skimmer, the weight parts of 0.1～20 part of said solvent, the weight part of 30～90 parts of weight parts is mixed carry out ball milling, obtain the coating-forming agent dispersion-s; In the said ball milling step, the rotating speed of ball mill is 500～6000r/min, and the time is 0.1～1hr, preferred 0.3～0.8hr;
3) with the said step 2 of 1～80 part of the said step 1) gained GAZO thickened pulp of 1～80 part of said linking agent, the weight part of 0.1～20 part of said solvent, the weight part of 1～95 part of weight part and weight part) gained coating-forming agent dispersion-s mixes and carries out ball milling, obtains said nano paint; In the said ball milling step, the rotating speed of ball mill is 500～6000r/min, and the ball milling time is 1-24hr, preferred 2-18hr;
All materials that arbitrary said each component of said claim 1-4 is formed and the mass ratio of the used abrading-ball of ball milling step are 2: 1～1: 3, preferred 1: 1～1: 1.5; The material that constitutes said abrading-ball is silit, zirconium white or norbide; The particle diameter of said abrading-ball is 0.03～2mm, preferred 0.04～0.8mm.
9. be the fabric with infrared stealth function of coating with the arbitrary said nano paint of claim 4-6;
The arbitrary said nano paint of claim 4-6 has the application in the fabric of infrared stealth function in preparation.
10. fabric according to claim 9 or application is characterized in that: the body material in the said fabric is selected from least a in woven fabrics, knitted fabrics, non-woven fabrics, synthetic leather, glass and the metal skin;
The top coat colour fastness of said fabric is 4 grades; Said fabric is that the visible light of 0.38～2.5 μ m, the average transmittances of near-infrared band are more than 90% at wavelength; At wavelength is that the average emitted rate of 8～14 μ m infrared bands is 0.5～0.75.
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