CN107140687B - A kind of compound nuclear shell structure nano powder - Google Patents

A kind of compound nuclear shell structure nano powder Download PDF

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Publication number
CN107140687B
CN107140687B CN201710488220.7A CN201710488220A CN107140687B CN 107140687 B CN107140687 B CN 107140687B CN 201710488220 A CN201710488220 A CN 201710488220A CN 107140687 B CN107140687 B CN 107140687B
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antimony
powder
layer
nano
shell structure
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CN107140687A (en
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杨波
李茂东
常萌蕾
黄国家
张双红
李仕平
翟伟
王志刚
何颖怡
伍振凌
常亮
潘莹
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Guangzhou Special Pressure Equipment Inspection and Research Institute
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Abstract

The invention discloses a kind of compound nuclear shell structure nano powder, including the first kernel, first kernel is the antimony doped stannic oxide nano powder that antimony mole doping concentration is 1%~10%；Middle layer, the middle layer are the silicon dioxide layer being coated on outside first kernel, and first kernel and middle layer constitute intermediate powder；Outer layer, the outer layer are the antimony doped stannic oxide nano powder layer that the antimony mole doping concentration being coated on outside the intermediate powder is 5%~15%.By in nano antimony-doped tin dioxide particle surface coated silica layer as intermediate powder medium, then one layer of nano antimony-doped tin dioxide is coated again, NEW TYPE OF COMPOSITE core-shell structure nanopowder body is prepared, experimental facilities and process are simple, and economic cost is low.

Description

A kind of compound nuclear shell structure nano powder
Technical field
The present invention relates to a kind of nano-powder, especially a kind of compound nuclear shell structure nano powder.
Background technique
In recent years, hud typed hetero nano structure material is due to having different from any single substance property and materialized It learns and field of nanometer technology has played extensive concern.Nucleocapsid hetero nano structure material can be by the material structure of different composition functions At can construct more good composite functional material and device by Material cladding, complementation and optimization, meet the needs of development. Core-shell structure material is formed in particle surface cladding shell substance, the interaction between control particle is can be very good, passes through The composition for changing the size of coating, structure and particle can assign particle with special functional characteristic, so that it be made to obtain More extensive potential application.
Stibium doping stannic oxide (Antimony tin oxide, abbreviation ATO) nano material, has combined ATO material And the advantages of nano material, it has unique photoelectric properties, ionizing radiation-resistant, good antireflective, infrared absorption, thermostabilization Property and very high ion selectivity exchange capacity is known as to certain members, can be used for insulating moulding coating, low-E glass for building, Infrared absorption heat-barrier material, anti-static plastic, Radiation-proof antistatic coating material, fiber, electrode material, gas sensor etc..? Foreign countries, especially in Japan, the U.S., the preparation and application study of ATO nano material come into the stage of large-scale production. And the research of China in this respect is started late, product relies primarily on import.So the autonomous research of ATO nano material, Become current considerable scientific research project.Huge economic benefit and social benefit, therefore, ATO have been involved among these Its preparation and application of nano material are increasingly taken seriously.
ATO nano material is a kind of excellent transparent heat-insulated filler, has excellent light-coloured transparent and infrared absorption special Property, and it is corrosion-resistant, thermal stability is high.However, it is desirable to heat-proof quality is further increased, in insulating moulding coating, researcher is by adding A certain amount of inorganic nano-particle is added to be modified coating property.For example, the Chinese invention of Publication No. CN1563231A Patent discloses a kind of be used as with nano ATO wet pulp and nano-indium stannum oxide (Indium Tin Oxide, abbreviation ITO) wet pulp and changes Property filler be added in glass coating make coating have good visible light transmittance and very high infrared shielding effect.And Nano-glass heat insulation paint need to only brush several microns of thickness, so that it may reach very good heat insulation, it is easy to operate And it is cheap.ATO nanoparticle itself has good antireflective, the functions such as anti-radiation and infrared absorption, and its is good Light transmittance, weatherability and stability and its cheap cost, so that the nanometer of its nanometer heat isolation paint for becoming present mainstream Filler.It is saturating that the Chinese invention patent of Publication No. CN106118287A discloses a kind of nano ATO/CuS filler water soluble acrylic acid It is bright heat-insulated, using nano ATO/CuS mixing filling, achieve the purpose that improving performance.
Summary of the invention
In order to overcome the drawbacks of the prior art, the present invention proposes a kind of compound core-shell structure nanopowder that heat-proof quality is good Body.
For this purpose, a kind of compound nuclear shell structure nano powder provided by the invention, including：
First kernel, first kernel are the antimony doped stannic oxide nanometer that antimony mole doping concentration is 1%~10% Powder；
Middle layer, the middle layer are the silicon dioxide layer being coated on outside first kernel, and first kernel is in Interbed constitutes intermediate powder；
Outer layer, the outer layer are that the antimony that the antimony mole doping concentration being coated on outside the intermediate powder is 5%~15% is mixed Miscellaneous stannic oxide nano powder layer.
Preferably, first kernel is the antimony doped stannic oxide nano powder that antimony mole doping concentration is 8.5%.
Preferably, the outer layer is the Sb doped two that the antimony mole doping concentration being coated on outside the intermediate powder is 5% Tin oxide nano-powder layer.
Preferably, the outer layer is the Sb doped two that the antimony mole doping concentration being coated on outside the intermediate powder is 7% Tin oxide nano-powder layer.
Preferably, the outer layer is the Sb doped two that the antimony mole doping concentration being coated on outside the intermediate powder is 10% Tin oxide nano-powder layer.
Preferably, the outer layer is the Sb doped two that the antimony mole doping concentration being coated on outside the intermediate powder is 15% Tin oxide nano-powder layer.
Preferably, the mean grain size of the compound nuclear shell structure nano powder is between 1.726nm and 2.115nm.
A kind of compound nuclear shell structure nano powder provided by the invention, preparation method includes the following steps：
S10：It is molten by antimony mole doping concentration will to be that 1%~10% weighed stannic chloride pentahydrate and antimony trichloride are dissolved in hydrochloric acid In liquid, by adding ammonium hydroxide, the first solution that pH value is 9~11 is formed；
S11：First solution is reacted 20~60 minutes under the conditions of being more than or equal to 50 DEG C of water bath with thermostatic control, formed at It is divided into the first sediment of Sb doped stannic hydroxide；
S15：First sediment is calcined, antimony doped stannic oxide nano powder is obtained；
S20：By the antimony doped stannic oxide nano powder ultrasonic disperse in dehydrated alcohol, formed by the way that ammonium hydroxide is added The second solution that pH value is 9~11；
S21：Under agitation, ethyl orthosilicate is added into second solution, sufficiently reacts, formed with the antimony Doped stannic oxide nano powder is as the first kernel, the second sediment of external sheath Silicon dioxide, hydrate；
S25：Second sediment is calcined, the intermediate powder that silicon dioxide layer coats first kernel is obtained；
S30：Stannic chloride pentahydrate and antimony trichloride are dissolved into containing levulinic for 5%~15% by antimony mole doping concentration In the dehydrated alcohol of ketone, sufficiently reaction is stirred, forms third solution, then distilled water is slowly added dropwise into the third solution, institute The volume ratio for stating distillation water consumption and the dehydrated alcohol dosage is 1.4~1.8:100, after continuing stirring 1~2 hour, display Aging obtains Sb doped stannic hydroxide colloidal sol；
S31：The intermediate powder is added to the Sb doped stannic hydroxide colloidal sol by the mass volume ratio of 2g/100ml In and carry out ultrasonic disperse, then sealing and standing is formed using the intermediate powder as the second kernel, external sheath Sb doped hydrogen The third sediment of tin oxide；
S35：It dries, calcine the third sediment and obtain nano antimony-doped tin dioxide and coat second kernel being formed Compound nuclear shell structure nano powder.
Preferably, in step slo, the molar concentration of the hydrochloric acid solution is 1~3mol/L.
Preferably, in step S10 and S20, the volumetric concentration of the ammonium hydroxide is 10%~30%.
It preferably, by antimony mole doping concentration is in step s 30 5%, 7%, 10% or 15% by stannic chloride pentahydrate It is dissolved into the dehydrated alcohol containing acetylacetone,2,4-pentanedione with antimony trichloride.
Preferably, the consumption proportion of intermediate powder and the Sb doped stannic hydroxide colloidal sol described in step S31 is Powder corresponds to 50ml Sb doped stannic hydroxide colloidal sol among 1.0g.
Preferably, in step S31, the ultrasonic disperse time is 15~30 minutes, and the sealing and standing time is 16~32 small When.
Preferably, in step S15, S25 and S35, the temperature of the calcining is 500~800 DEG C, and calcination time is 1~3 Hour.
It preferably, further include being filtered, washing to first sediment before calcination between step S11 and S15 The step of with drying.
It preferably, further include being filtered, washing to second sediment before calcination between step S21 and S25 The step of with drying.
It preferably, further include being filtered, washing to the third sediment before calcination between step S31 and S35 The step of with drying.
Beneficial effects of the present invention are：Compound nuclear shell structure nano powder provided by the invention, by nano antimony-doped Then stannic oxide particle surface coated silica layer coats one layer of nano antimony-doped titanium dioxide as intermediate powder medium again Tin prepares NEW TYPE OF COMPOSITE core-shell structure nanopowder composite material, and experimental facilities and process are simple, and economic cost is low. The compound nuclear shell structure nano powder application that this method is prepared is in insulating moulding coating, and the dispersibility of powder is than using merely Sb doped The insulating moulding coating of tin dioxide nanometer material is good, and heat insulation is also more preferably.
Detailed description of the invention
Fig. 1 is 6,000 times of SEM photographs of No. 1 nano material sample；
Fig. 2 is 10,000 times of SEM photographs of No. 1 nano material sample；
Fig. 3 is 6,000 times of SEM photographs of No. 2 nano material samples；
Fig. 4 is 10,000 times of SEM photographs of No. 2 nano material samples；
Fig. 5 is 6,000 times of SEM photographs of No. 3 nano material samples；
Fig. 6 is 10,000 times of SEM photographs of No. 3 nano material samples；
Fig. 7 is the diffracted intensity curve comparison figure of 1 to No. 6 nano material sample；
Fig. 8 is warm in the case for being thermally shielded test after the aluminium sheet covering bubble chamber of 0 to No. 6 nanometer heat isolation paint using being coated with Spend change curve comparison diagram.
Specific embodiment
Below by specific embodiment to further illustrate the technical scheme of the present invention.
Embodiment one
A kind of compound nuclear shell structure nano powder provided in this embodiment, including：
First kernel, first kernel are the antimony doped stannic oxide nano powder that antimony mole doping concentration is 8.5%；
Middle layer, the middle layer are the silicon dioxide layer being coated on outside first kernel, and first kernel is in Interbed constitutes the second kernel；
Outer layer, the outer layer are the Sb doped dioxy that the antimony mole doping concentration being coated on outside second kernel is 10% Change tin nano-powder layer.
The compound nuclear shell structure nano raw powder's production technology, includes the following steps：
S10：33g stannic chloride pentahydrate will be weighed for 8.5% by antimony mole doping concentration and 2g antimony trichloride is dissolved in 2mol/L Hydrochloric acid solution in, by addition volumetric concentration be 10% ammonium hydroxide, form the first solution of pH=9；
S11：First solution is reacted 30 minutes under the conditions of 60 DEG C of water bath with thermostatic control, forming component is Sb doped hydrogen Tin oxide (Sn (OH)4·Sb(OH)3) the first sediment of yellow, reaction equation is as follows:
SnCl4·5H2O+SbCl3+NH3·H2O→Sn(OH)4·Sb(OH)3↓+NH4Cl；
S12：It filters first solution and obtains first sediment；
S13：Obtained the first sediment ethyl alcohol will be filtered and deionized water is respectively washed 5 times；
S14：First sediment after cleaning is dried 12 hours at 80 DEG C；
S15：First sediment after cleaning is put into Muffle furnace to calcine 2 hours at 650 DEG C, to the Sb doped hydrogen Tin oxide is dehydrated, and after natural cooling, obtains navy blue antimony doped stannic oxide nano powder, by the Sb doped dioxy Change tin nano-powder as No. 1 nano material sample and be scanned electron microscope (SEM) shooting, wherein 6,000 times of SEM photographs As shown in Figure 1,10,000 times of SEM photographs are as shown in Fig. 2, by Fig. 1~2 it is found that being mixed using the antimony of above-mentioned coprecipitation synthesis The pattern of miscellaneous stannic oxide nano powder is the block of size unevenness；
S20：The navy blue antimony doped stannic oxide nano powder is added in the dehydrated alcohol of 100ml, ultrasound point It dissipates 30 minutes, it is the second solution that 10% ammonium hydroxide forms that pH value is 9 that volumetric concentration, which is then added, is stirred 30 minutes；
S21：Under agitation, ethyl orthosilicate 20ml, sufficiently reaction 3.5 hours are added into second solution, It is formed using the antimony doped stannic oxide nano powder as the first kernel, the second precipitating of external sheath Silicon dioxide, hydrate Object；
S22：It filters second solution and obtains second sediment；
S23：Obtained the second sediment ethyl alcohol will be filtered and deionized water is respectively washed 5 times；
S24：Second sediment after cleaning is dried 12 hours at 80 DEG C；
S25：Second sediment after cleaning is put into Muffle furnace and calcines 2 hours to the external sheath at 650 DEG C Silicon dioxide, hydrate be dehydrated, after natural cooling, obtain being coated in described first by silicon dioxide layer for light slate gray Karyomorphism at intermediate powder；The intermediate powder is scanned electron microscope (SEM) as No. 2 nano material samples to clap Take the photograph, wherein 6,000 times of SEM photographs as shown in figure 3,10,000 times of SEM photographs as shown in figure 4, by Fig. 3~4 it is found that having coated dioxy The particle size of namely No. 2 nano material samples of the antimony doped stannic oxide nano powder of SiClx floor obviously becomes smaller, distribution Also relatively uniform, pattern structure spherical in shape, average grain diameter is respectively less than 0.3 μm；
S30：By will be that 10% weigh 30g stannic chloride pentahydrate and 2.17g antimony trichloride is dissolved by antimony mole doping concentration In the mixed solution of 8ml acetylacetone,2,4-pentanedione and 100ml dehydrated alcohol, first ultrasonic disperse 15 minutes, then magnetic agitation 30 minutes, shape 1.6ml distilled water is slowly added dropwise at the clear third solution of clear, yellowish, then into the third solution, it is small to continue stirring 1 Shi Hou after displaying aging 24 hours, obtains Sb doped stannic hydroxide colloidal sol；
S31：The intermediate powder for weighing 1.0g light slate gray is added in Sb doped stannic hydroxide colloidal sol described in 50ml, Ultrasonic disperse 15 minutes, then sealing and standing 24 hours, formed using the intermediate powder as the second kernel, external sheath antimony is mixed The third sediment of miscellaneous stannic hydroxide；
S32：It filters the Sb doped stannic hydroxide colloidal sol and obtains the third sediment；
S33：The obtained third sediment will be filtered to be cleaned 5 times with ethyl alcohol；
S34：The third sediment after cleaning is dried 12 hours at 80 DEG C；
S35：The third sediment after cleaning is put into Muffle furnace and calcines 2 hours to the external sheath at 650 DEG C Sb doped stannic hydroxide be dehydrated, after natural cooling, obtain nano antimony-doped tin dioxide cladding described second in karyomorphism At compound nuclear shell structure nano powder；The compound nuclear shell structure nano powder is swept as No. 3 nano material samples Electron microscope (SEM) shooting is retouched, wherein 6,000 times of SEM photographs are as shown in figure 5,10,000 times of SEM photographs are as shown in Figure 6；By Fig. 5 ~6 it is found that No. 3 nano material samples that antimony mole doping concentration is 10%, powder can be clearly seen that spherical structure, be distributed Relatively uniform, cladding thickness is larger, this is because the reunion growth of nano surface stibium doping stannic oxide crystallite dimension is related.Its Size has no and significantly changes compared with No. 2 nano material sample nano-powders.
Embodiment two to four
The compound nuclear shell structure nano powder constituents and preparation method and embodiment one basic one that embodiment two to four provides It causes, the difference with embodiment one is only that the antimony mole doping concentration of the antimony doped stannic oxide nano powder layer of the outer layer And the antimony mole doping concentration in step S30 and distillation water consumption, the data comparison of specific Ingredient Amount is as shown in table 1.
Each ingredient contrast table in the step S30 of 1 embodiment one to four of table
In order to facilitate comparison various embodiments of the present invention involved in various nano materials, embodiment two to four provide three kinds Compound nuclear shell structure nano powder is respectively defined as 4 to No. 6 nano material samples secondary.Sample number into spectrum table such as table corresponding with ingredient Shown in 2.
2 sample number into spectrum of table table corresponding with ingredient
Sample ID Ingredient
No. 1 nano material sample The antimony doped stannic oxide nano powder of one step S15 of embodiment preparation
No. 2 nano material samples The intermediate powder of one step S25 of embodiment preparation
No. 3 nano material samples The compound nuclear shell structure nano powder of embodiment one
No. 4 nano material samples The compound nuclear shell structure nano powder of embodiment two
No. 5 nano material samples The compound nuclear shell structure nano powder of embodiment three
No. 6 nano material samples The compound nuclear shell structure nano powder of example IV
Referring to Fig. 7, it is found that 1 to No. 6 each diffraction maximum of nano material sample mentioned in the embodiment of the present invention one to four Tetragonal phase cassiterite structure (the JCPDS card number of data and stannic oxide：21~1250, JCPDS：Joint Committee on Powder Diffraction Standards/ Joint Committee on Powder Diffraction Standards) diffraction maximum it is consistent.There is not antimony The diffraction maximum of oxide illustrates that all antimony ions enter the tin ion in stannic oxide lattice instead of part.
Compare the diffracted intensity curve of No. 1 and No. 2 nano material sample it can be found that No. 2 nano material samples diffraction Peak is significantly broadened compared with No. 1 nano material sample, and diffraction peak intensity reduces, and shows the grain size of No. 2 nano material sample powders It is smaller.The apparent characteristic peak of silica is had no in figure, shows that the silica of cladding is unformed structure and cladding thickness It is relatively thin.It takes the highest peak of No. 2 nano material samples and No. 1 nano material sample to calculate grain size, is calculated 2 by Scherrer formula The mean grain size d=2.049nm, the mean grain size d=of No. 1 nano material sample powder of number nano material sample powder 3.919nm.The result shows that after No. 1 nano material coated silica floor, lighter and crystallite dimension becomes smaller.3~No. 6 are received The diffraction maximum of rice material sample powder does not change substantially, and crystal is still the stibium doping stannic oxide structure of rutile structure, peak Position slightly migrates.The diffraction maximum of 3~No. 6 nano material sample powders more widen compared with No. 2 nano material sample powders changed it is some, Diffraction peak intensity reduces slightly.Show that the grain size of 3~No. 6 nano material sample powders is smaller.Take 3~No. 6 nano material samples The highest peak of product calculates grain size, and the mean grain size d=of No. 3 nano material sample powders is calculated by Scherrer formula 2.115nm, the mean grain size d=1.726nm of No. 4 nano material sample powders, the average crystalline substance of No. 5 nano material sample powders Granularity 1.741nm, the mean grain size d=2.115nm of No. 6 nano material sample powders, the mean grain size d=of powder 1.856nm.The result shows that with the increase of antimony mole doping concentration in the stibium doping stannic oxide of outermost layer cladding, complex nucleus The grain size first increases and then decreases of shell structural nano powder.Compare discovery, the grain of sample obtained in the SEM photograph in Fig. 1~6 Diameter calculates resulting crystallite dimension (D much larger than by Scherrer formulaXRD), this is primarily due to DSEMIt is the size of particle, it may Be by multiple grain colony poly groups at particle, and DXRDIt is single crystallite dimension.
The antimony mole in step S30 is only had adjusted for better contrast and experiment, in the embodiment of the present invention one to four The dosage of doping concentration and distilled water.Certainly, by experimental verification, in the case where guaranteeing effect of the present invention, the present invention its In the compound nuclear shell structure nano powder preparation method that his alternate embodiment provides, various reaction conditions and ingredient are in each step It can also be adjusted in following ratios or range in rapid：
S10：Stannic chloride pentahydrate and antimony trichloride can be weighed by antimony mole doping concentration for 1%~10%, the hydrochloric acid The concentration of solution is 1~3mol/L, and the volumetric concentration of ammonium hydroxide is 10%~30%, the pH value of first solution is adjusted to 9~ 11；
S11：The temperature of water bath with thermostatic control is 50~90 DEG C, and the reaction time is 20~60 minutes；
S20：The volumetric concentration of ammonium hydroxide is 10%~30%, and the pH value of second solution is 9~11；
S30：Stannic chloride pentahydrate and antimony trichloride are weighed for 5%~15% by antimony mole doping concentration, the distilled water is used The volume ratio of amount and the dehydrated alcohol dosage is 1.4~1.8:100, continue stirring 1~2 hour after distilled water is added；
S31：The ultrasonic disperse time is 15~30 minutes, and the sealing and standing time is 16~32 hours；
S13, S23 and S33：Ethyl alcohol wash number is 3~6 times, and deionized water wash number is 0~6 time；
S14, S24 and S34：Drying temperature is 70~90 DEG C, and drying time is 10~15 hours；
S15, S25 and S35：Calcination temperature range is 500~800 DEG C, and calcination time is 1~3 hour.
Embodiment five
It is prepared for the compound nuclear shell structure nano powder preparation method that the test embodiment of the present invention one to four provides compound The heat-proof quality of core-shell structure nanopowder body, using 1 to No. 6 nano material sample as additive in coating in the present embodiment, with 0 Number nanometer heat isolation paint is major ingredient, prepares 1 to No. 6 nanometer heat isolation paint, and be thermally shielded performance test to all samples, respectively The ingredient of nanometer heat isolation paint is as shown in table 3.
3 coating sample of table table corresponding with ingredient
Wherein No. 0 nanometer heat isolation paint uses water-borne acrylic coatings, and the water-borne acrylic coatings press quality hundred Point than by 70% aqueous acrylic emulsion, 5% calcium carbonate, 5% mica powder, 1% defoaming agent, 1% thickener and 18% water composition.
Illustrate by taking No. 1 nanometer heat isolation paint as an example below, the preparation method of No. 1 insulating moulding coating provided in this embodiment includes Following steps：
S50：No. 1 nano material sample 0.2g is weighed to be added as additive in No. 0 nanometer heat isolation paint of 1.8g；
S55：Ultrasonic disperse 30 minutes, No. 1 nano material sample is made to be dispersed in No. 0 nanometer heat isolation paint In, form No. 1 nanometer heat isolation paint.
For the consistency for guaranteeing test, the preparation of 2 to No. 6 nanometer heat isolation paints is all made of the above method, and difference is only It is to replace with additive into corresponding nano material sample.
0 to No. 6 nanometer heat isolation paint is uniformly brushed into the surface of aluminum plate uniform in size respectively, forms a layer thickness For the heat insulating coating film of 0.5mm, smearing range is full aluminium sheet, is tested for heat-proof quality.Aluminium sheet having a size of 11.2 × 4.8 × 0.15cm after film, is put and forms 0 to No. 6 aluminum test under room temperature environment after desiccation, does experimental data for heat-insulated test and adopts Collection.
Heat-insulated test：
Experimental situation：Indoor test, room temperature：29℃；
Major experimental stage property：0 to No. 6 aluminum test, specification is 34 × 25 × 10cm and center of top is provided with 10 × 4cm Opening bubble chamber, the tengsten lamp of 500W, hygrosensor；
Testing procedure (illustrates) by taking No. 0 aluminum test as an example：
T10：Experiment stage property is placed on test wrapper domestic 2 hours, makes the temperature and ambient temperature equilibrium of testing stage property, test When door and window close, experimental situation wind speed be 0；
T20：No. 0 aluminum test is covered in the opening of bubble chamber, is aligned with the opening center, to guarantee bubble chamber Opening is completely covered, and the end of probe of the hygrosensor is set in the bubble chamber for detecting the sky in the bubble chamber Temperature degree, reading end are set to outside the bubble chamber；
T30：Heat source uses the tengsten lamp with 500W similar in solar spectrum, and tengsten lamp is hung over the covering bubble chamber and is opened Right above No. 0 aluminum test of mouth at 30cm；
T40：Start timing when opening tengsten lamp, records the temperature of air in the bubble chamber at intervals of two minutes；To temperature After degree variation is no more than 0.5 DEG C, (being the 26th minute in the present embodiment) stops recording data as needed.
No. 0 aluminum test is replaced with into 1 to No. 6 aluminum test respectively according to the method described above, obtains and uses 0 to No. 6 Temperature variation data in the bubble chamber that aluminum test is tested forms Fig. 8 with this data creating temperature changing curve diagram.By scheming 8 it is found that under the irradiation of tengsten lamp, and extension at any time, described foam the temperature inside the box rises with it, incipient stage ascensional range It is larger, it gradually tends to be steady, when irradiating after twenty minutes, air themperature gradually tends to balance in box.Referring to Fig. 8, wherein on to Aluminium sheet used in the corresponding test of the temperature variation curve of lower arrangement is followed successively by No. 0, No. 1, No. 2, No. 4, No. 5, No. 6 and No. 3 survey Try aluminium sheet.It can be seen that No. 2 nanometer heat isolation paints, that is, the antimony doped stannic oxide nanometer of addition coated silica layer The heat insulation of the coating sample of powder body material and No. 1 nanometer heat isolation paint, that is, addition antimony doped stannic oxide nanometer powder The coating sample of body material is compared, and heat insulation is preferable；And add the antimony doped stannic oxide nanometer powder of different Sb doped concentration Body carries out the coating sample of the compound nuclear shell structure nano powder of outermost layer cladding, i.e., the heat-insulated effect of 3 to No. 6 nanometer heat isolation paints Fruit is superior to No. 1 and No. 2 nanometer heat isolation paints, wherein the heat-proof quality of No. 3 nanometer heat isolation paints is optimal.
In conclusion the compound nuclear shell structure nano powder that the present invention supplies, by antimony doped stannic oxide nano powder Then particle surface coated silica middle layer coats one layer of antimony doped stannic oxide nano powder again, prepare novel multiple Synkaryon shell structural nano powder, Preparation equipment and process are simple, and economic cost is low.By test, the compound nucleocapsid knot Additive of the structure nano-powder as insulating moulding coating, dispersibility is more preferably than antimony doped stannic oxide nano powder；By above-mentioned reality Testing result can also verify, and add the heat insulation of the nanometer heat isolation paint of the compound nuclear shell structure nano powder than addition antimony The heat-proof quality of the heat-barrier material of doped stannic oxide nano powder is more preferable.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art The other embodiments being understood that.

Claims (7)

1. a kind of compound nuclear shell structure nano powder, it is characterised in that including：
First kernel, first kernel are the antimony doped stannic oxide nano powder that antimony mole doping concentration is 1%~10%；
Middle layer, the middle layer are the silicon dioxide layer being coated on outside first kernel, first kernel and middle layer Constitute intermediate powder；
Outer layer, the outer layer are the Sb doped two that the antimony mole doping concentration being coated on outside the intermediate powder is 5%~15% Tin oxide nano-powder layer.
2. a kind of compound nuclear shell structure nano powder according to claim 1, it is characterised in that：First kernel is antimony The antimony doped stannic oxide nano powder that mole doping concentration is 8.5%.
3. a kind of compound nuclear shell structure nano powder according to claim 1, it is characterised in that：The outer layer is to be coated on The antimony doped stannic oxide nano powder layer that antimony mole doping concentration outside the intermediate powder is 5%.
4. a kind of compound nuclear shell structure nano powder according to claim 1, it is characterised in that：The outer layer is to be coated on The antimony doped stannic oxide nano powder layer that antimony mole doping concentration outside the intermediate powder is 7%.
5. a kind of compound nuclear shell structure nano powder according to claim 1, it is characterised in that：The outer layer is to be coated on The antimony doped stannic oxide nano powder layer that antimony mole doping concentration outside the intermediate powder is 10%.
6. a kind of compound nuclear shell structure nano powder according to claim 1, it is characterised in that：The outer layer is to be coated on The antimony doped stannic oxide nano powder layer that antimony mole doping concentration outside the intermediate powder is 15%.
7. a kind of compound nuclear shell structure nano powder according to claim 1, it is characterised in that：The compound core-shell structure The mean grain size of nano-powder is between 1.726nm and 2.115nm.
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