CN102951849A - Interference color glass bead and preparation method thereof - Google Patents
Interference color glass bead and preparation method thereof Download PDFInfo
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- CN102951849A CN102951849A CN2012104178979A CN201210417897A CN102951849A CN 102951849 A CN102951849 A CN 102951849A CN 2012104178979 A CN2012104178979 A CN 2012104178979A CN 201210417897 A CN201210417897 A CN 201210417897A CN 102951849 A CN102951849 A CN 102951849A
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Abstract
The invention relates to an interference color glass bead and a preparation method thereof. The interference color glass bead is characterized by comprising a spherical common glass flint glass substrate and metal oxide coatings sequentially coated on the outer surface; the metal oxide coating is one layer or more; thickness of each layer of metal oxide coating meets the following formula: 2nd + 1 / 2 lambda = k lambda; n represents the index rate of metal oxide; d represents the thickness of the coating; lambda represents wavelength of interference phase light wave and values from 350 to 770nm; and K is an natural number other than 0. The metal oxide coating on the outer surface of the interference color glass bead has advantages of smoothness, compactness, good reflection performance and diversified and adjustable color; and the preparation process is simple, and convenient for popularization and application.
Description
Technical field
The present invention relates to a kind of interference colorful glass microbead and preparation method thereof, belong to the glass microballon field.
Technical background
Glass microsphere is widely used in the fields such as road traffic label, billboard, screen, reflective heat-insulation paint.A reflecting glass microballon adularescent and silver gray are two kinds at present, if need to have other color in the actual application, then maybe need to add versicolor film or pigment, and can greatly reduce like this its reflecting effect, or adopt tinted shade to prepare, and adopt the granulated glass sphere reflecting effect of the method preparation poor, and usually only be used for the decoration field, less for the reflection field.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of reflecting properties good for the deficiency of currently available products, color-variable, adjustable interference colorful glass microbead and preparation method thereof.
A kind of interference colorful glass microbead comprises spherical common flint glass matrix and is coated on successively the coating of metal oxides of its outside surface that described coating of metal oxides is one or more layers, and the thickness of described each layer coating of metal oxides satisfies following formula:
2nd+1/2λ?=kλ
Wherein n is the specific refractory power of metal oxide;
D is the thickness of coating;
λ is for interfering mutually long optical wavelength, and value is 350～770nm;
The k value is for removing 0 natural number of thinking.
What interfere that long optical wavelength mutually reflects in visible-range is exactly the color of light.
Press such scheme, the preferred value of described k is 1-3.
Press such scheme, the metal oxide in the described coating of metal oxides is selected from titanium dioxide, ferric oxide, zirconium white, silicon oxide, cobalt oxide, chromic oxide, nickel oxide, aluminum oxide, vanadium oxide, molybdenum oxide, manganese oxide etc.
Press such scheme, the diameter of described interference colorful glass microbead is 1 μ m-5mm.
A kind of preparation method who interferes colorful glass microbead is characterized in that: may further comprise the steps:
(a) common flint glass microballon is placed in the water through pre-treatment, stirring makes its suspension, pH requirement when then basis is with the corresponding metal-salt hydrolysis of metal oxide to be covered, the pH of regulation system is to setting range, under the state that stirs, drip corresponding water-soluble metal salts solution in 20-70 ℃ again, regulating by respective acids basicity simultaneously makes system pH be stabilized in aforementioned pH setting range, and make metal-salt constantly be hydrolyzed to metal oxide or metal hydroxides, and be coated on equably the surface of glass microballon, reaching setting thickness when this coating layer at last, after presenting pre-color, stop to coat;
When described coating of metal oxides to be covered is multilayer, after the oxide compound of the first metal or metal hydroxides are coated on the glass microballon surface, the pH value of system when dripping again the corresponding water-soluble metal salts solution of other each metal oxides and corresponding regulation and control hydrolysis and coating successively;
(b) filter, wash drying;
(c) calcining gets final product to get the surperficial interference colorful glass microbead that is coated with smooth compact metal oxide coating behind the naturally cooling.
Press such scheme, described pre-treatment comprises washing, alkali cleaning or acid pickling step.
Press such scheme, the concentration of described water-soluble metal salts solution is 10-100g/L, and drop rate is 10-50mL/h.
Press such scheme, described metal oxide is selected from titanium dioxide, ferric oxide, zirconium white, silicon-dioxide, cobalt oxide, chromic oxide, nickel oxide, aluminum oxide, vanadium oxide, molybdenum oxide, manganese oxide etc.
Pressing such scheme, is titanium dioxide such as the metal oxide that coats, and used water-soluble salt is titanium tetrachloride; Metal oxide such as coating is ferric oxide, and used water-soluble salt is iron trichloride; Metal oxide such as coating is zirconium white, and used water-soluble salt is basic zirconium chloride; Metal oxide such as coating is silicon-dioxide, and used water-soluble salt is water glass; Metal oxide such as coating is cobalt oxide, and used water-soluble salt is cobalt chloride; Metal oxide such as coating is chromic oxide, and used water-soluble salt is chromium chloride; Metal oxide such as coating is nickel oxide, and used water-soluble salt is nickelous chloride or single nickel salt; Metal oxide such as coating is aluminum oxide, and used water-soluble salt is aluminum chloride or Tai-Ace S 150; Metal oxide such as coating is vanadium oxide, and used water-soluble salt is sodium metavanadate; Metal oxide such as coating is molybdenum oxide, and used water-soluble salt is Sodium orthomolybdate; Metal oxide such as coating is manganese oxide, and used water-soluble salt is Manganous chloride tetrahydrate or manganous sulfate.
Press such scheme, described metal oxide to be covered is TiO
2The time, before its corresponding water-soluble metal salts solution of dropping applies, according to SnCl
4PH requirement during hydrolysis, the pH of regulation system drips SnCl to setting range under the state that stirs
4Solution is to coat in advance one deck SnO outside glass microballon
2Crystal type promoting reagent.
Press such scheme, described SnCl
4With SnO
2Metering, the water-soluble metal salt of described titanium is with TiO
2Metering, SnCl
4Add-on be the 1%-10% of the water-soluble metal salt molar weight of titanium.
Press such scheme, the drying temperature of described step (b) is 50-200 ℃.
Press such scheme, described calcining temperature is 200-800 ℃, and calcination time is 20-100min.The coating that described calcining temperature and calcination time can coat according to stromal surface be oxide compound or the oxyhydroxide of this metal, and the metal oxide of pre-which kind of crystal formation of acquisition and selecting.
The present invention is by hydrolysis preparation metal oxide or metal hydroxides nano particle, and make this nano particle be coated on equably the surface of glass microsphere, the colorful glass microbead of the surface clad oxide coating that obtains through aftertreatment again, smooth surface is fine and close, reflecting properties is good, not only do not reduce catoptrical brightness, increased on the contrary glass microballon to the reflection of light performance.In addition, by coating different coating of metal oxides, and the control coat-thickness, can prepare the adjustable colorful glass microbead of multiple color.
Principle of the present invention is described as follows:
Take coating of metal oxides as example as individual layer: as shown in Figure 1, when incident illumination was mapped to the glass microballon surface, a part was by glass microballon surface coating layer reflection (R1), and another part sees through coating layer, at glass microballon surface reflection (R2).Because coating layer has the specific refractory power that is different from air, so this two-beam has certain phase differential, and be identical with the frequency of light beam generation, thereby produced each other interference, finally show the color of interference color.And the metal oxide by coating different refractivity or coat different coat-thicknesses can reach the purpose of the colorful glass microbead of preparation multiple color.And when being multiple coating, this glass microballon also can be different with the color that the difference of viewing angle is observed.
Beneficial effect of the present invention:
This interferes the smooth densification of coating of metal oxides of colorful glass microbead outside surface, and reflecting properties is good, and color is various adjustable;
Preparation technology is simple, and is easy to utilize.
Description of drawings
Fig. 1 is silvery white glass microballon and the simple glass microballon integrating sphere light diffuse-reflectance collection of illustrative plates that embodiment 1 makes.
Fig. 2 is the scanning electron microscope (SEM) photograph contrast of the silvery white glass microballon that makes of embodiment 1 and simple glass bead surface;
Fig. 3 is colorful glass microbead colour developing schematic diagram of the present invention.
Among the figure: I is incident light; R1 is the coating layer reflected light; R2 is the glass microballon surface reflection; D is the physical thickness of coating layer.
Embodiment
In order to further specify summary of the invention of the present invention, below in conjunction with embodiment summary of the invention of the present invention is described further.
Embodiment 1
Take by weighing the 10g glass microballon in the 250ml there-necked flask, add the 200ml deionized water, stir washing 10 minutes, leave standstill and remove supernatant liquid a moment, repeat above-mentioned steps twice, wash complete.Then add the 80ml deionized water, regulate pH value to 9 with NaOH, stirred 10 minutes, leave standstill and remove supernatant liquid a moment, alkali cleaning is complete.Add the 80ml deionized water, with salt acid for adjusting pH value to 2.5, stirred 10 minutes.Solution is heated to 60 ℃, drips the TiCl of 100g/L with the speed of 0.3ml/min
4Solution drips mass percent and is 10% NaOH solution simultaneously so that the system pH regulator is stabilized in 2.5, stops to drip TiCl when products therefrom presents silvery white
4Solution and NaOH alkaline solution.Filter out solid product, use the deionized water washes clean, with 150 ℃ of oven dry, then put into retort furnace, be heated to 650 ℃, roasting 30 minutes, naturally cooling obtains silvery white glossy glass microballon in stove.
With the silvery white glass microballon that makes with do not coat TiO
2The glass microballon of interfering layer is analyzed it to the reflection of light performance with the ultraviolet/visible light spectrophotometer, sees Fig. 1, and silvery white glass microballon will be better than the simple glass microballon far away at the reflecting properties of visible light and infrared light region as seen from Figure 1.This silvery white glass microballon ultraviolet region reflecting properties descends, and is because its TiO
2Interfering layer is very strong and the reflecting properties to UV-light is descended to some extent to the ultraviolet Optical Absorption.
Fig. 2 is the scanning electron microscope (SEM) photograph contrast of silvery white glass microballon and simple glass bead surface; As seen from Figure 2: coated behind the interfering layer surface of glass microballon more smooth, smooth, and more be conducive to reflection of light.
Embodiment 2
Take by weighing the 10g glass microballon in the 250ml there-necked flask, add the 200ml deionized water, stir washing 10 minutes, leave standstill and remove supernatant liquid a moment, repeat above-mentioned steps twice, wash complete.Add the 80ml deionized water in flask, regulate pH value to 9 with NaOH and stirred 10 minutes, leave standstill and remove supernatant liquid a moment, alkali cleaning is complete.Add the 80ml deionized water, stirred 10 minutes with salt acid for adjusting pH value to 2.5.Solution is heated to 60 ℃, drips the TiCl of 100g/L with the speed of 0.3ml/min
4Solution drips mass percent and is 10% NaOH solution simultaneously so that system pH is stabilized in 2.5, stops to drip TiCl when products therefrom presents blueness
4Solution and NaOH alkaline solution.Filter out solid product, use the deionized water washes clean, 150 ℃ of oven dry are put into retort furnace with the colorful glass microbead after the oven dry, are heated to 650 ℃, roasting 30 minutes, and naturally cooling gets blue glossy glass microballon in stove.
Embodiment 3
Take by weighing the 10g glass microballon in the 250ml there-necked flask, add the 200ml deionized water, stirring velocity is that per minute 300 turns.Stir washing 10 minutes, leave standstill and remove supernatant liquid a moment, repeat above-mentioned steps twice, wash complete.Add the 80ml deionized water in flask, regulate pH value to 9 with NaOH and stirred 10 minutes, leave standstill and remove supernatant liquid a moment, alkali cleaning is complete.Add the 80ml deionized water, regulate pH value to 2 with HCl and stirred 10 minutes.Solution is heated to 50 ℃, drips the SnCl of 35g/L with the speed of 0.2ml/min
4Solution 20ml drips 10% NaOH solution simultaneously so that system pH is stablized PH 2.Be added dropwise to complete rear stirring 10 minutes.Drip mass percent and be 10% NaOH solution with the stabilising system pH value 2.5, then drip the TiCl of 100g/L with the speed of 0.3ml/min
4Solution stops to drip TiCl when products therefrom presents redness
4Solution and NaOH alkaline solution.Filter out solid product, use the deionized water washes clean, 100 ℃ of oven dry, with 650 ℃ of roastings of colorful glass microbead after the oven dry 30 minutes, naturally cooling got red glossy glass microballon in stove.
By regulating TiCl
4The add-on of solution adds crystal type promoting reagent in case of necessity, with thickness and the titanium dioxide crystal form of control coating of titanium dioxide, can reach control glass microsphere color such as the purpose of the color such as silvery white, golden, yellow, red, purple, blue, green.
Embodiment 4
Take by weighing the 10g glass microballon in the 250ml there-necked flask, add the 200ml deionized water, stir washing 10 minutes, leave standstill and remove supernatant liquid a moment, repeat above-mentioned steps twice, wash complete.Add the 80ml deionized water in flask, regulate pH value to 9 with NaOH and stirred 10 minutes, leave standstill and remove supernatant liquid a moment, alkali cleaning is complete.Add the 80ml deionized water, regulate pH value to 3 with HCl, stirred 10 minutes.Solution is heated to 30 ℃, drips the FeCl of 30g/L
3Solution, drip simultaneously NaOH solution so that the stable system pH value 3, stops to drip solution and NaOH alkaline solution when products therefrom presents yellow.Filter out solid product, use the deionized water washes clean, 150 ℃ of oven dry are put into retort furnace with the colorful glass microbead after the oven dry, 300 ℃ of roastings after 30 minutes in stove naturally cooling obtain yellow glossy glass microballon; 600 ℃ of roastings 30 minutes, naturally cooling gets the glossy glass microballon of deep yellow in stove afterwards.
By regulating FeCl
3The amount of splashing into of solution with the thickness of control coating oxidation iron, can be controlled in conjunction with the setting of maturing temperature the crystal formation of ferric oxide simultaneously, and reach the purpose of control bead color.Available color has gold, Huang, the multiple color such as red, purple, brown, black.
Embodiment 5
Take by weighing the 10g glass microballon in the 250ml there-necked flask, add the 200ml deionized water, stir washing, leave standstill and remove supernatant liquid a moment, repeat above-mentioned steps twice, wash complete.Add the 80ml deionized water in flask, regulate pH value to 9 with sodium hydroxide and stirred 10 minutes, leave standstill and remove supernatant liquid a moment, alkali cleaning is complete.Add the 80ml deionized water, regulate pH value to 8 with hydrochloric acid and stirred 10 minutes.Solution is heated to 25 ℃, drips the CrCl of 10g/L
3Solution drips mass percent and is 3% NaOH solution simultaneously to stablize pH value 8, stops to drip solution and NaOH alkaline solution when products therefrom presents green.Filter out solid product, use the deionized water washes clean, with 80 ℃ of oven dry, the colorful glass microbead after the oven dry is put into retort furnace, 300 ℃ of roastings after 30 minutes in stove naturally cooling get green glossy glass microballon; 600 ℃ of roastings after 30 minutes in stove naturally cooling get the glossy glass microballon of deep green.
By regulating CrCl
3The amount of splashing into of solution with the thickness of control coating oxidation chromium, can be controlled in conjunction with the setting of maturing temperature the crystal formation of chromic oxide simultaneously, and reach the purpose of control bead color.Available color has the multiple colors such as green, yellowish green, blue.
Embodiment 6
Take by weighing the 10g glass microballon in the 250ml there-necked flask, add the 200ml deionized water, stir washing, leave standstill and remove supernatant liquid a moment, repeat above-mentioned steps twice, wash complete.Add the 80ml deionized water in flask, regulate pH value to 9 with sodium hydroxide and stirred 10 minutes, leave standstill and remove supernatant liquid a moment, alkali cleaning is complete.Add the 80ml deionized water, solution is heated to 60 ℃, drip the sodium silicate solution of 50g/L with the speed of 0.8ml/min, drip simultaneously mass percent and be 3% hydrochloric acid soln to stablize pH value 9, when products therefrom presents golden yellow, stop to drip solution and alkaline solution.Filter out solid product, use the deionized water washes clean, with 120 ℃ of oven dry, the colorful glass microbead after the oven dry is put into retort furnace, be heated to 600 ℃, roasting 30 minutes, naturally cooling gets golden yellow glossy glass microballon in stove.
PH value required during above-mentioned coating also can be regulated pH value to 2 with hydrochloric acid after alkali cleaning is complete, then drip sodium silicate solution, so coat, when products therefrom presents gold, stop to coat, afterwards in 600 ℃, roasting 30 minutes, naturally cooling obtains golden yellow glossy glass microballon in stove.
By regulating the amount of splashing into of sodium silicate solution, with the thickness of control coating silicon-dioxide, can reach the purpose of control bead color.Available color has silvery white, gold, Huang, the multiple color such as red, purple, blue, green.
Embodiment 7
Take by weighing the 10g glass microballon in the 250ml there-necked flask, add the 200ml deionized water, stir washing, leave standstill and remove supernatant liquid a moment, repeat above-mentioned steps twice, wash complete.Add the 80ml deionized water in flask, regulate pH value to 11 with sodium hydroxide and stirred 10 minutes, leave standstill and remove supernatant liquid a moment, alkali cleaning is complete.Add the 80ml deionized water, solution is heated to 60 ℃, drip the cobalt chloride solution of 50g/L with the speed of 0.5ml/min, drip simultaneously NaOH solution to stablize pH value 11, when products therefrom presents blueness, stop to drip cobalt chloride solution and NaOH solution.Filter out solid product, use the deionized water washes clean, with 150 ℃ of oven dry, the colorful glass microbead after the oven dry is put into retort furnace, be heated to 600 ℃, roasting 50 minutes, naturally cooling gets blue glossy glass microballon in stove.
By regulating the amount of splashing into of cobalt chloride solution, with the thickness of control coating cobalt dioxide, can reach the purpose of control bead color.Available color has indigo plant, the multiple color such as green, black.
Embodiment 8
Take by weighing the 10g glass microballon in the 250ml there-necked flask, add the 200ml deionized water, stir washing 10 minutes, leave standstill and remove supernatant liquid a moment, repeat above-mentioned steps twice, wash complete.Add the 80ml deionized water in flask, regulate pH value to 11 with sodium hydroxide and stirred 10 minutes, leave standstill and remove supernatant liquid a moment, alkali cleaning is complete.Add the 80ml deionized water, solution is heated to 60 ℃, drip the zirconium oxychloride solution of 10g/L, drip simultaneously NaOH solution to stablize pH value 11, when products therefrom presents redness, stop to drip solution and alkaline solution.Filter out solid product, use the deionized water washes clean, with 150 ℃ of oven dry, the colorful glass microbead after the oven dry is put into retort furnace, be heated to 600 ℃, roasting 80 minutes, naturally cooling gets red glossy glass microballon in stove.
By regulating the amount of splashing into of zirconium oxychloride solution, with the thickness of control coating oxidation zirconium, can reach the purpose of control bead color.Available color has silvery white, gold, Huang, the multiple color such as red, purple, blue, green.
Embodiment 9
Take by weighing the 10g glass microballon in the 250ml there-necked flask, add the 200ml deionized water, washing was stirred 10 minutes, left standstill to remove supernatant liquid a moment, repeated above-mentioned steps twice, washed complete.Add the 80ml deionized water in flask, regulate pH value to 8 with sodium hydroxide and stirred 10 minutes, leave standstill and remove supernatant liquid a moment, alkali cleaning is complete.Add the 80ml deionized water, solution is heated to 60 ℃, drip the alum liquor of 10g/L with the speed of 0.3ml/min, drip simultaneously mass percent and be 10% sodium hydroxide solution to stablize pH value 8, when products therefrom presents redness, stop to drip solution and alkaline solution.Filter out solid product, use the deionized water washes clean, with 150 ℃ of oven dry, the colorful glass microbead after the oven dry is put into retort furnace, be heated to 600 ℃, roasting, naturally cooling gets red glossy glass microballon in stove.
By regulating the amount of splashing into of alum liquor, with the thickness of control coating oxidation aluminium, can reach the purpose of control bead color.Available color has silvery white, gold, Huang, the multiple color such as red, purple, blue, green.
Embodiment 10
Take by weighing the 10g glass microballon in the 250ml there-necked flask, add the 200ml deionized water, stir washing 10 minutes, leave standstill and remove supernatant liquid a moment, repeat above-mentioned steps twice, wash complete.Add the 80ml deionized water in flask, regulate pH value to 9 with NaOH and stirred 10 minutes, leave standstill and remove supernatant liquid a moment, alkali cleaning is complete.Add the 80ml deionized water, stirred 10 minutes with salt acid for adjusting pH value to 2.5.Solution is heated to 60 ℃, drips the TiCl of 100g/L with the speed of 0.3ml/min
4Solution drips mass percent and is 10% NaOH solution simultaneously so that system pH is stabilized in 2.5, stops to drip TiCl when products therefrom presents blueness
4Solution and NaOH alkaline solution.Then regulate pH value to 3 with 10% NaOH solution, stirred 10 minutes.Keep 60 ℃ of solution, drip the FeCl of 30g/L
3Solution, drip simultaneously NaOH solution so that the stable system pH value 3, stops to drip solution and NaOH alkaline solution when products therefrom presents yellow.Filter out solid product, use the deionized water washes clean, 150 ℃ of oven dry are put into retort furnace with the colorful glass microbead after the oven dry, are heated to 600 ℃, roasting 30 minutes, and naturally cooling gets yellow slightly red gloss glass microballon in stove.
Embodiment 11
Take by weighing the 10g glass microballon in the 250ml there-necked flask, add the 200ml deionized water, stir washing 10 minutes, leave standstill and remove supernatant liquid a moment, repeat above-mentioned steps twice, wash complete.Add the 80ml deionized water in flask, regulate pH value to 9 with NaOH and stirred 10 minutes, leave standstill and remove supernatant liquid a moment, alkali cleaning is complete.Add the 80ml deionized water, stirred 10 minutes with salt acid for adjusting pH value to 2.5.Solution is heated to 60 ℃, drips the TiCl of 100g/L with the speed of 0.3ml/min
4Solution drips mass percent and is 10% NaOH solution simultaneously so that system pH is stabilized in 2.5, stops to drip TiCl when products therefrom presents blueness
4Solution and NaOH alkaline solution.Then regulate pH value to 11 with sodium hydroxide and stirred 10 minutes, leave standstill and remove supernatant liquid a moment, alkali cleaning is complete.Add the 80ml deionized water, keep 60 ℃ of solution, drip the cobalt chloride solution of 50g/L with the speed of 0.3ml/min, drip simultaneously NaOH solution to stablize pH value 11, when products therefrom presents blueness, stop to drip cobalt chloride solution and NaOH solution.Filter out solid product, use the deionized water washes clean, with 150 ℃ of oven dry, the colorful glass microbead after the oven dry is put into retort furnace, be heated to 600 ℃, roasting 30 minutes, naturally cooling gets the glass microballon of blue slightly red gloss in stove.
Claims (10)
1. interfere colorful glass microbead for one kind, it is characterized in that: comprise spherical common flint glass matrix and be coated on successively the coating of metal oxides of its outside surface, described coating of metal oxides is one or more layers, and the thickness of described each layer coating of metal oxides satisfies following formula:
2nd+1/2λ?=kλ
Wherein n is the specific refractory power of metal oxide;
D is the thickness of coating;
λ is for interfering mutually long optical wavelength, and value is 350～770nm;
The k value is for removing 0 natural number of thinking.
2. interference colorful glass microbead according to claim 1, it is characterized in that: described k value is 1-3.
3. interference colorful glass microbead according to claim 1, it is characterized in that: the metal oxide in the described coating of metal oxides is selected from titanium dioxide, ferric oxide, zirconium white, silicon oxide, cobalt oxide, chromic oxide, nickel oxide, aluminum oxide, vanadium oxide, molybdenum oxide, manganese oxide.
4. interference colorful glass microbead according to claim 1, it is characterized in that: the diameter of described interference colorful glass microbead is 1 μ m-5mm.
5. preparation method who interferes colorful glass microbead is characterized in that: may further comprise the steps:
(a) common flint glass microballon is placed in the water through pre-treatment, stirring makes its suspension, pH requirement when then basis is with the corresponding metal-salt hydrolysis of metal oxide to be covered, the pH of regulation system is to setting range, under the state that stirs, drip corresponding water-soluble metal salts solution in 20-70 ℃ again, regulating by respective acids basicity simultaneously makes system pH be stabilized in aforementioned pH setting range, and make metal-salt constantly be hydrolyzed to metal oxide or metal hydroxides, and be coated on equably the surface of glass microballon, reaching setting thickness when this coating layer at last, after presenting pre-color, stop to coat;
When described coating of metal oxides to be covered is multilayer, after the oxide compound of the first metal or metal hydroxides are coated on the glass microballon surface, the pH value of system when dripping again the corresponding water-soluble metal salts solution of other each metal oxides and corresponding regulation and control hydrolysis and coating successively;
(b) filter, wash drying;
(c) calcining gets final product to get the interference colorful glass microbead of the smooth densification of top coat behind the naturally cooling.
6. the preparation method of interference colorful glass microbead according to claim 5, it is characterized in that: the concentration of described water-soluble metal salts solution is 10-100g/L, drop rate is 10-50mL/h.
7. the preparation method of interference colorful glass microbead according to claim 5 is characterized in that: be titanium dioxide such as the metal oxide that coats, used water-soluble salt is titanium tetrachloride; Metal oxide such as coating is ferric oxide, and used water-soluble salt is iron trichloride; Metal oxide such as coating is zirconium white, and used water-soluble salt is basic zirconium chloride; Metal oxide such as coating is silicon-dioxide, and used water-soluble salt is water glass; Metal oxide such as coating is cobalt oxide, and used water-soluble salt is cobalt chloride; Metal oxide such as coating is chromic oxide, and used water-soluble salt is chromium chloride; Metal oxide such as coating is nickel oxide, and used water-soluble salt is nickelous chloride or single nickel salt; Metal oxide such as coating is aluminum oxide, and used water-soluble salt is aluminum chloride or Tai-Ace S 150; Metal oxide such as coating is vanadium oxide, and used water-soluble salt is sodium metavanadate; Metal oxide such as coating is molybdenum oxide, and used water-soluble salt is Sodium orthomolybdate; Metal oxide such as coating is manganese oxide, and used water-soluble salt is Manganous chloride tetrahydrate or manganous sulfate.
8. the preparation method of interference colorful glass microbead according to claim 5 is characterized in that, described metal oxide to be covered is TiO
2The time, before its corresponding water-soluble metal salts solution of dropping applies, according to SnCl
4PH requirement during hydrolysis, the pH of regulation system drips SnCl to setting range under the state that stirs
4Solution is to coat in advance one deck SnO on the glass microballon surface
2Crystal type promoting reagent.
9. the preparation method of interference colorful glass microbead according to claim 5 is characterized in that: described SnCl
4With SnO
2Metering, the water-soluble metal salt of described titanium is with TiO
2Metering, SnCl
4Add-on be the 1%-10% of the water-soluble metal salt molar weight of titanium.
10. the preparation method of interference colorful glass microbead according to claim 5, it is characterized in that: the drying temperature of described step (b) is 50-200 ℃; Described calcining temperature is 200-800 ℃, and calcination time is 20-100min.
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| CN116442629A (en) * | 2023-04-28 | 2023-07-18 | 深圳御光新材料有限公司 | Projection film and manufacturing method thereof |
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| CN108298824A (en) * | 2017-08-18 | 2018-07-20 | 深圳先进技术研究院 | A kind of novel heat insulation material and preparation method thereof |
| CN107903694A (en) * | 2017-10-30 | 2018-04-13 | 安徽铭能保温科技有限公司 | A kind of method that insulating moulding coating colorful hollow glass microballoon is prepared using Chemical coating method |
| CN108795256A (en) * | 2018-07-11 | 2018-11-13 | 佛山市陵谐环保科技有限公司 | A kind of heat insulation coating and preparation method thereof |
| CN109535522A (en) * | 2018-11-22 | 2019-03-29 | 杭州普信塑料包装有限公司 | A kind of packing bottle for pesticide and preparation method thereof |
| CN114437567A (en) * | 2020-10-31 | 2022-05-06 | 中国石油化工股份有限公司 | Metal oxide/hollow microsphere and preparation method thereof |
| CN114437567B (en) * | 2020-10-31 | 2023-07-04 | 中国石油化工股份有限公司 | Metal oxide/hollow microsphere and preparation method thereof |
| CN116162387A (en) * | 2022-12-09 | 2023-05-26 | 安徽拓力工程材料科技有限公司 | Durable reflective coating and preparation method and application thereof |
| CN116442629A (en) * | 2023-04-28 | 2023-07-18 | 深圳御光新材料有限公司 | Projection film and manufacturing method thereof |
| CN116442629B (en) * | 2023-04-28 | 2024-01-26 | 深圳御光新材料有限公司 | Projection film and manufacturing method thereof |
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