A method for preparing a glass thin film slurry by solid phase fusion gradient hyperdispersion

Abstract

This invention relates to the field of glass thin film material preparation technology, specifically disclosing a method for preparing glass thin film slurry through solid-phase fusion and gradient ultradispersion. First, metal oxides and other materials are weighed and ground to obtain mixture A, which is then calcined and crushed to obtain particles D. Particle D is then wet-milled and dried to obtain nanoparticles E. Nanoparticles E are added to ethyl acetate and stirred to obtain a mixed solution F, while citric acid and other materials are added to deionized water and stirred to obtain a mixed solution G. Then, an organic resin is mixed with F and G to obtain a precursor solution H. After ultrasonic dispersion and constant-temperature water bath stirring, the solution is repeatedly filtered 3-5 times to finally obtain the glass thin film slurry. The preparation method of the glass thin film slurry in this application integrates high-temperature solid-phase fusion and gradient ultradispersion processes, precisely controlling particle size and interface coupling to solve the material dispersion problem. Based on a multi-layer structure design, a spectral control system is constructed to achieve bidirectional dynamic temperature regulation, reducing consumption and improving efficiency. The film thickness is adjustable, lightweight, and highly flexible, adaptable to various scenarios.

Description

Technical Field

[0001] This invention relates to the field of glass thin film material preparation technology, and more specifically, to a method for preparing glass thin film slurry through solid-phase fusion gradient ultradispersion. Background Technology

[0002] Globally, building operation energy consumption accounts for 30%–40% of total energy consumption, with 40%–50% of this loss occurring through building envelopes. A key factor is glass, a critical component of building facades, which accounts for over 60% of heat loss. This indicates serious limitations in the application of existing high-energy-consuming glass in building energy conservation, including:

[0003] Low thermal performance: The U-value (heat transfer coefficient) of single-layer ordinary glass is 5.0–6.0 W / (m²). 2 ·K), the U-value of double-glazed insulated glass is 1.8~2.5W / (m²). 2 The U-value (K) is far higher than the national standard requirement (U-value of new buildings in cold regions ≤ 1.5 W / (m²)). 2 ·K), the U-value of the existing building after renovation is ≤2.0W / (m³). 2 ·K));

[0004] The single function of solar thermal regulation: It cannot dynamically adjust the solar heat gain coefficient (SHGC), resulting in excessive heat absorption in summer and serious heat loss in winter. This makes the drawbacks of demand conflict between hot and cold regions and insufficient adaptation to extreme climates more prominent, further relying on air conditioning compensation, thereby aggravating energy consumption.

[0005] Existing heat insulation films have insufficient reflectivity: although they have some reflectivity, there is a problem of insufficient control over mid-infrared (60%-70% transmittance in 3-5μm) and far-infrared (approximately 80% transmittance in 15μm-1mm) rays, which makes them unable to effectively block heat radiation.

[0006] High cost: Although existing technologies (such as commercially available glass films) can provide some heat insulation, the control of infrared blocking rate depends on imported materials (such as 3M products priced at 400 yuan / m2), and the manufacturing process makes the powder very easy to clump and disperse unevenly.

[0007] The shortcomings in intelligent materials and processes are obvious, and disassembly and assembly are time-consuming and labor-intensive.

[0008] Driven by energy conservation and emission reduction policies, the "General Specification for Building Energy Conservation and Renewable Energy Utilization" mandates that glass U-values ​​meet standards. Local pilot programs for "building energy efficiency rating" require additional fees for non-compliance, while subsidies are available for retrofitting. This underscores the urgency of developing high-performance, low-cost insulation materials. With over 6*10¹⁰ m² of existing buildings in China, and over 40% being non-energy-efficient, the market size for energy-saving retrofitting is estimated at trillions of yuan. This highlights the core role of building glass retrofitting in the global carbon reduction strategy and provides a huge market impetus for the development of new insulation materials.

[0009] Therefore, in view of the above-mentioned defects and shortcomings, the present invention provides a method for preparing glass thin film slurry by solid-phase fusion-gradient ultradispersion. Summary of the Invention

[0010] To address the aforementioned technical problems in related technologies, this invention provides a method for preparing glass thin film slurry through solid-phase fusion gradient ultradispersion, which can solve the above problems.

[0011] To achieve the above-mentioned technical objectives, the technical solution of the present invention is implemented as follows:

[0012] A method for preparing glass thin film slurry by solid-phase fusion gradient ultradispersion includes the following steps:

[0013] Step S1: Weigh the metal oxide, lanthanum hexaboride, and silicon dioxide according to the mass ratio of 2-3:0.5-0.7:1-1.5, place them in an agate mortar and grind them thoroughly into powder. After passing through a 200-mesh sieve, obtain mixture A.

[0014] The metal oxide is a combination of or all of the following: indium tin oxide, aluminum-doped zinc oxide, tungsten oxide, titanium dioxide, cerium oxide, copper oxide, silver oxide, lanthanum oxide, yttrium oxide, tellurium oxide, and aluminum oxide, wherein it contains at least indium tin oxide, tungsten oxide, titanium dioxide, copper oxide, silver oxide, and aluminum oxide, and the mass ratio of each component in the metal oxide is 1:1.

[0015] Step S2: Transfer the mixture A obtained in Step S1 to a high-purity alumina crucible (alumina purity ≥ 99%), and place the high-purity alumina crucible in a muffle furnace for calcination. The calcination temperature is increased from room temperature to 1500℃ at a heating rate of 10-20℃ / min, and held at 1500℃ for 2-3 hours. Then, the muffle furnace temperature is first reduced to 1300℃ at a cooling rate of 10-20℃ / min, and then the muffle furnace temperature is rapidly reduced to 800℃. The cooling rate is 50-100℃ / min to obtain mixture B. Then, mixture B is quickly poured onto a preheated alumina ceramic plate and allowed to cool naturally to room temperature to obtain block C. Block C is then placed in a muffle furnace for heat treatment. The heat treatment temperature is increased from room temperature to 800℃ at a heating rate of 5-10℃ / min, and held at 800℃ for 1-2 hours before being allowed to cool naturally to room temperature. Block C is then removed and crushed into fine particles to obtain particles D.

[0016] The temperature of the preheated alumina ceramic plate is 200-300℃.

[0017] Step S3: Transfer the particles D obtained in step S2 to a ball mill jar. Add anhydrous ethanol to the ball mill jar at a mass-to-volume ratio of metal oxide to anhydrous ethanol of 1 g: 1-2 ml. Then, wet mill the particles using a high-energy planetary ball mill at a speed of 600-800 rpm for 15-20 hours to obtain undried nanopowder E. Dry the undried nanopowder E using infrared drying at a temperature of 70-90℃ for 20-50 minutes to obtain nanopowder E.

[0018] The average particle size distribution of nanopowder E is 5–10 nm.

[0019] Step S4: Weigh out the following components according to the mass ratio of metal oxide, organic resin, silica aerogel powder, 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, lauramide propylamine oxide, tetrabutyl titanate, citric acid, and zinc nitrate: 1:60-80:0.7-1:0.5-0.8:0.5-0.7:0.3-0.5:0.1-0.3:0.3-0.7 respectively. Weigh out the following components according to the mass ratio of metal oxide, organic resin, silica aerogel powder, 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, lauramide propylamine oxide, tetrabutyl titanate, citric acid, and zinc nitrate: 1:60-80:0.7-1:0.5-0.8:0.5-0.7:0.3-0.5:0.1-0.3:0.3-0.7 respectively. Weigh out the following components according to the mass ratio of metal oxide, ethyl acetate, and deionized water: Ethyl acetate and deionized water were measured in a volume ratio of 1g:30-50ml:10-20ml. Then, the nanopowder E obtained in step S3, along with silica aerogel powder, 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, lauramide propylamine oxide, and tetrabutyl titanate, were added to ethyl acetate. The mixture was then stirred magnetically in a constant temperature water bath at 30-40℃ at a stirring speed of 100-200 rpm for 2-3 hours to obtain mixed solution F. At the same time, citric acid and zinc nitrate were added to deionized water and stirred mechanically at a stirring speed of 200-300 rpm for 10-30 minutes to obtain mixed solution G.

[0020] The organic resin is one or more of polyethylene, polyvinyl butyral, polyvinyl chloride, polyisobutylene, and polyurethane.

[0021] The silica aerogel powder has a particle size of 1–5 μm, a pore size of 20–50 nm, and a porosity of ≥90%.

[0022] Step S5: Mix the organic resin weighed in step S4 with the mixed solution F and mixed solution G obtained in step S4, and use mechanical stirring at a speed of 500-800 rpm. After 2-3 hours, a precursor solution H is obtained. Then, the precursor solution H is ultrasonically dispersed at a frequency of 30-50 kHz and a power of 500 W. After 2-4 hours, the ultrasonic dispersion is stopped. The precursor solution H is then placed in a constant temperature water bath at 50-80℃ and mechanically stirred at a speed of 300-500 rpm. After 5-8 hours, a glass film slurry precursor is obtained. The glass film slurry precursor is filtered repeatedly 3-5 times to obtain the glass film slurry.

[0023] The beneficial effects of this invention are:

[0024] This invention integrates high-temperature solid-phase fusion and gradient ultra-dispersion processes to achieve precise control over the particle size and interface coupling of metal oxide / silica aerogel powders. This effectively solves the technical bottlenecks of easy agglomeration and poor dispersibility of materials, ensuring uniform and stable slurry. This innovation not only balances material cost and performance but also provides reliable process assurance for large-scale production.

[0025] This invention is based on a multi-layer structure design. It embeds 5-10 nm metal oxide nanoparticles into silica aerogel to construct a spectrally selective control system: visible light transmittance ≥78% to ensure indoor lighting, infrared reflectance ≥87%, and ultraviolet reflectance ≥94% to achieve efficient heat insulation and UV protection, with a minimum U value of 0.86 W / (m²). 2 This technology (·K) breaks through the limitations of traditional passive regulation. Through bidirectional dynamic SHGC regulation of "winter heat preservation + summer heat insulation," it adapts to the climatic differences between hot and cold regions, reducing air conditioning energy consumption by 30% to 50% and significantly improving building energy efficiency. Its thermal management synergy mechanism combines localized surface plasmon resonance (LSPR) of metal oxides to reflect solar thermal energy with aerogel nanopores (20-50nm) to inhibit heat conduction / convection, forming multiple heat insulation barriers. At the same time, the photocatalytic self-cleaning function of titanium dioxide extends the service life of the film, achieving a dual improvement in performance and durability.

[0026] The film thickness of this invention is adjustable from 50 to 300 μm and can be applied to curved glass. Compared with traditional double-glazed insulated glass, it reduces weight by about 40%, combining the advantages of lightweight and flexibility. This characteristic makes it perform well in scenarios that are sensitive to structural loads, such as ultra-high-rise curtain walls and renovation of historical buildings. At the same time, it provides a temperature rise control solution for BIPV (Building Integrated Photovoltaics). Detailed Implementation

[0027] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention are within the scope of protection of the present invention.

[0028] Example 1

[0029] 10g of metal oxides (1g each of indium tin oxide, aluminum-doped zinc oxide, tungsten oxide, titanium dioxide, cerium oxide, copper oxide, silver oxide, yttrium oxide, tellurium oxide, and aluminum oxide), 2.25g of lanthanum hexaboride, and 4.82g of silicon dioxide were ground thoroughly into powder in an agate mortar and passed through a 200-mesh sieve to obtain mixture A. Mixture A was then transferred to a high-purity alumina crucible, which was placed in a muffle furnace for calcination. The calcination temperature was increased from room temperature to 1500℃ at a rate of 15℃ / min and held at 1500℃ for 2.7 hours. The muffle furnace temperature was then first reduced to 1300℃ at a rate of 13℃ / min, and then rapidly reduced to 800℃ at a rate of 80℃ / min, yielding mixture B. Mixture B was then quickly poured onto a preheated alumina ceramic plate at 220℃ and allowed to cool naturally to room temperature to obtain block C. The block C was then placed in a muffle furnace for heat treatment, with the temperature increased from room temperature to 800℃ at a rate of 8℃ / min. After holding at 800℃ for 1.3 hours, it was naturally cooled to room temperature. The block C was then removed and crushed into fine particles to obtain particles D.

[0030] Particle D was transferred to a ball mill jar, and 18 ml of anhydrous ethanol was added. The mixture was then wet-milled using a high-energy planetary ball mill at 650 rpm for 18 hours, yielding undried nanopowder E. This undried nanopowder E was then dried using infrared drying at 75°C for 30 minutes to obtain nanopowder E.

[0031] Nanopowder E, along with 8.62 g of silica aerogel powder, 6.34 g of 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, 5.63 g of lauramide propylamine oxide, and 3.96 g of tetrabutyl titanate, were added to 400 ml of ethyl acetate and stirred magnetically at 160 rpm in a 34°C water bath for 2.3 h to obtain mixed solution F. Simultaneously, 1.77 g of citric acid and 5.64 g of zinc nitrate were added to 120 ml of deionized water and stirred mechanically at 260 rpm for 17 min to obtain mixed solution G.

[0032] 720g of organic resin (a mixture of polyethylene and polyvinyl butyral, with a mass ratio of 3:1) was mixed with mixed solutions F and G and mechanically stirred at 600 rpm for 2.2 h to obtain precursor solution H. Precursor solution H was then ultrasonically dispersed at 30 kHz and 500 W for 2.3 h, after which ultrasonic dispersion was stopped. Precursor solution H was then placed in a 60℃ constant temperature water bath and mechanically stirred at 350 rpm for 5.7 h to obtain the glass film slurry precursor. The glass film slurry precursor was filtered three times to obtain the glass film slurry.

[0033] Example 2

[0034] 16g of metal oxides (2g each of indium tin oxide, tungsten oxide, titanium dioxide, cerium oxide, copper oxide, silver oxide, tellurium oxide, and aluminum oxide), 3.52g of lanthanum hexaboride, and 10.37g of silicon dioxide were ground thoroughly into powder in an agate mortar and passed through a 200-mesh sieve to obtain mixture A. Mixture A was then transferred to a high-purity alumina crucible, which was placed in a muffle furnace for calcination. The calcination temperature was increased from room temperature to 1500℃ at a rate of 12℃ / min and held at 1500℃ for 2.4 hours. The muffle furnace temperature was then lowered to 1300℃ at a rate of 17℃ / min, followed by a rapid decrease to 800℃ at a rate of 70℃ / min, yielding mixture B. Mixture B was then quickly poured onto a preheated alumina ceramic plate at 300℃ and allowed to cool naturally to room temperature, yielding block C. The block C was then placed in a muffle furnace for heat treatment, with the temperature increased from room temperature to 800℃ at a rate of 5℃ / min. After holding at 800℃ for 1.7 hours, it was naturally cooled to room temperature. The block C was then removed and crushed into fine particles to obtain particles D.

[0035] Particle D was transferred to a ball mill jar, and 25 ml of anhydrous ethanol was added. The mixture was then wet-milled using a high-energy planetary ball mill at 720 rpm for 15 hours, yielding undried nanopowder E. This undried nanopowder E was then dried using infrared spectroscopy at 85°C for 45 minutes to obtain nanopowder E.

[0036] Nanopowder E, along with 14.32 g of silica aerogel powder, 9.78 g of 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, 10.58 g of lauramide propylamine oxide, and 7.56 g of tetrabutyl titanate, were added to 650 ml of ethyl acetate and magnetically stirred in a 37°C water bath at 120 rpm for 2.6 h to obtain mixed solution F. Simultaneously, 3.25 g of citric acid and 7.53 g of zinc nitrate were added to 260 ml of deionized water and mechanically stirred at 270 rpm for 26 min to obtain mixed solution G.

[0037] 1130g of organic resin (a mixture of polyvinyl chloride and polyisobutylene, with a mass ratio of 5:3) was mixed with mixed solutions F and G and mechanically stirred at 720 rpm for 2.7 h to obtain precursor solution H. Precursor solution H was then ultrasonically dispersed at 40 kHz and 500 W for 3.7 h, after which ultrasonic dispersion was stopped. Precursor solution H was then placed in a 75℃ constant temperature water bath and mechanically stirred at 420 rpm for 6.3 h to obtain the glass film slurry precursor. The glass film slurry precursor was filtered repeatedly 5 times to obtain the glass film slurry.

[0038] Example 3

[0039] 27g of metal oxides (3g each of indium tin oxide, aluminum-doped zinc oxide, tungsten oxide, titanium dioxide, cerium oxide, copper oxide, silver oxide, lanthanum oxide, and aluminum oxide), 7.59g of lanthanum hexaboride, and 13.28g of silicon dioxide were ground thoroughly into powder in an agate mortar and passed through a 200-mesh sieve to obtain mixture A. Mixture A was then transferred to a high-purity alumina crucible, which was placed in a muffle furnace for calcination. The calcination temperature was increased from room temperature to 1500℃ at a rate of 18℃ / min and held at 1500℃ for 2.6 hours. The muffle furnace temperature was then first reduced to 1300℃ at a rate of 15℃ / min, and then rapidly reduced to 800℃ at a rate of 50℃ / min, yielding mixture B. Mixture B was then quickly poured onto a preheated alumina ceramic plate at 200℃ and allowed to cool naturally to room temperature, yielding block C. The block C was then placed in a muffle furnace for heat treatment, with the temperature increased from room temperature to 800℃ at a rate of 7℃ / min. After holding at 800℃ for 1.6 hours, it was naturally cooled to room temperature. The block C was then removed and crushed into fine particles to obtain particles D.

[0040] Particle D was transferred to a ball mill jar, and 48 ml of anhydrous ethanol was added. The mixture was then wet-milled using a high-energy planetary ball mill at 780 rpm for 17 hours, yielding undried nanopowder E. The undried nanopowder E was then dried using infrared spectroscopy at 78°C for 25 minutes to obtain nanopowder E.

[0041] Nanopowder E, along with 23.56 g of silica aerogel powder, 15.63 g of 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, 16.46 g of lauramidopropylamine oxide, and 11.52 g of tetrabutyl titanate, were added to 1200 ml of ethyl acetate. The mixture was then magnetically stirred at 170 rpm in a 35°C water bath for 2.4 h to obtain mixed solution F. Simultaneously, 6.84 g of citric acid and 15.73 g of zinc nitrate were added to 320 ml of deionized water and mechanically stirred at 250 rpm for 22 min to obtain mixed solution G.

[0042] 1860g of organic resin (a mixture of polyvinyl butyral, polyvinyl chloride, and polyisobutylene, with a mass ratio of 1:1:3) was mixed with mixed solutions F and G and mechanically stirred at 680 rpm for 2.4 h to obtain precursor solution H. Precursor solution H was then ultrasonically dispersed at 35 kHz and 500 W for 2.8 h, after which ultrasonic dispersion was stopped. Precursor solution H was then placed in a 55℃ constant temperature water bath and mechanically stirred at 380 rpm for 7.5 h to obtain the glass film slurry precursor. The glass film slurry precursor was filtered four times to obtain the glass film slurry.

[0043] Example 4

[0044] 24g of metal oxides (4g each of indium tin oxide, tungsten oxide, titanium dioxide, copper oxide, silver oxide, and aluminum oxide), 5.68g of lanthanum hexaboride, and 16.52g of silicon dioxide were ground thoroughly into powder in an agate mortar and passed through a 200-mesh sieve to obtain mixture A. Mixture A was then transferred to a high-purity alumina crucible, which was placed in a muffle furnace for calcination. The calcination temperature was increased from room temperature to 1500℃ at a rate of 14℃ / min and held at 1500℃ for 2.3 hours. The muffle furnace temperature was then first reduced to 1300℃ at a rate of 18℃ / min, and then rapidly reduced to 800℃ at a rate of 90℃ / min, yielding mixture B. Mixture B was then quickly poured onto a preheated alumina ceramic plate at 280℃ and allowed to cool naturally to room temperature, yielding block C. The block C was then placed in a muffle furnace for heat treatment, with the temperature increased from room temperature to 800℃ at a rate of 6℃ / min. After holding at 800℃ for 1.8 hours, it was naturally cooled to room temperature. The block C was then removed and crushed into fine particles to obtain particles D.

[0045] Particle D was transferred to a ball mill jar, and 36 ml of anhydrous ethanol was added. The mixture was then wet-milled using a high-energy planetary ball mill at 750 rpm for 16 hours, yielding undried nanopowder E. The undried nanopowder E was then dried using infrared spectroscopy at 82°C for 40 minutes to obtain nanopowder E.

[0046] Nanopowder E, along with 21.13 g of silica aerogel powder, 17.81 g of 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, 13.73 g of lauramide propylamine oxide, and 8.34 g of tetrabutyl titanate, were added to 950 ml of ethyl acetate and magnetically stirred in a 38°C water bath at 150 rpm for 2.8 h to obtain mixed solution F. Simultaneously, 4.39 g of citric acid and 11.56 g of zinc nitrate were added to 350 ml of deionized water and mechanically stirred at 230 rpm for 15 min to obtain mixed solution G.

[0047] 1750g of organic resin (a mixture of polyethylene, polyvinyl butyral, polyvinyl chloride, polyisobutylene, and polyurethane, wherein the mass ratio of polyethylene, polyvinyl butyral, polyvinyl chloride, polyisobutylene, and polyurethane is 3:2:1:2:2) was mixed with mixed solutions F and G and mechanically stirred at 750 rpm for 2.8 h to obtain precursor solution H. Precursor solution H was then ultrasonically dispersed at a frequency of 45 kHz and a power of 500 W for 3.3 h, after which ultrasonic dispersion was stopped. Precursor solution H was then placed in a 65℃ constant temperature water bath and mechanically stirred at 430 rpm for 6.8 h to obtain the glass film slurry precursor. The glass film slurry precursor was filtered three times to obtain the glass film slurry.

[0048] Example 5

[0049] 55g of metal oxides (including 5g each of indium tin oxide, aluminum-doped zinc oxide, tungsten oxide, titanium dioxide, cerium oxide, copper oxide, silver oxide, lanthanum oxide, yttrium oxide, tellurium oxide, and aluminum oxide), 16.85g of lanthanum hexaboride, and 38.63g of silicon dioxide were thoroughly ground into powder in an agate mortar and passed through a 200-mesh sieve to obtain mixture A. Mixture A was then transferred to a high-purity alumina crucible, which was placed in a muffle furnace for calcination. The calcination temperature was increased from room temperature to 1500℃ at a rate of 20℃ / min and held at 1500℃ for 2.1 hours. The muffle furnace temperature was then first reduced to 1300℃ at a rate of 16℃ / min, and then rapidly reduced to 800℃ at a rate of 60℃ / min, yielding mixture B. The mixture B was then quickly poured onto a preheated alumina ceramic plate at 240°C and allowed to cool naturally to room temperature, yielding block C. Block C was then placed in a muffle furnace for heat treatment, with the temperature increased from room temperature to 800°C at a rate of 10°C / min, and held at 800°C for 1.5 hours before being allowed to cool naturally to room temperature. Block C was then removed and crushed into fine particles to obtain particles D.

[0050] Particle D was transferred to a ball mill jar, and 100 ml of anhydrous ethanol was added. The mixture was then wet-milled using a high-energy planetary ball mill at 650 rpm for 20 hours, yielding undried nanopowder E. This undried nanopowder E was then dried using infrared spectroscopy at 73°C for 35 minutes to obtain nanopowder E.

[0051] Nanopowder E, along with 48.76 g of silica aerogel powder, 35.93 g of 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, 33.56 g of lauramidopropylamine oxide, and 23.85 g of tetrabutyl titanate, were added to 2500 ml of ethyl acetate and magnetically stirred in a 32°C water bath at 140 rpm for 2.5 h to obtain mixed solution F. Simultaneously, 12.47 g of citric acid and 27.85 g of zinc nitrate were added to 900 ml of deionized water and mechanically stirred at 280 rpm for 24 min to obtain mixed solution G.

[0052] 3680g of organic resin (a mixture of polyvinyl butyral, polyvinyl chloride, polyisobutylene, and polyurethane, wherein the mass ratio of polyvinyl butyral, polyvinyl chloride, polyisobutylene, and polyurethane is 2:2:3:1) was mixed with mixed solutions F and G, and mechanically stirred at 560 rpm for 2.5 h to obtain precursor solution H. Precursor solution H was then ultrasonically dispersed at 50 kHz and 500 W for 3.5 h, after which ultrasonic dispersion was stopped. Precursor solution H was then placed in an 80℃ constant temperature water bath and mechanically stirred at 450 rpm for 7.2 h to obtain the glass film slurry precursor. The glass film slurry precursor was filtered repeatedly 5 times to obtain the glass film slurry.

[0053] The glass film slurries prepared in Examples 1, 2, 3, 4, and 5 were used to prepare and test glass films by spraying or roller coating, respectively. The production cost of the glass films was calculated, and the detailed results are shown in Table 1.

[0054] Table 1. Results of Glass Thin Film Performance Testing and Cost Calculation

[0055]

[0056] The test results in Table 1 show that the glass film slurry prepared by the solid-phase fusion-gradient ultradispersion method of this invention can be used to produce glass films in various ways (spraying or roller coating), the thickness of the glass film is adjustable (50-300 μm), and the U value is <1.5 W / (m). 2 ·K), with a minimum of 0.86W / (m 2With an infrared reflectance of ≥87% and an ultraviolet reflectance of ≥96%, it possesses excellent thermal performance, enabling bidirectional dynamic SHGC adjustment for both winter heat preservation and summer heat insulation. This adapts to the conflicting needs of hot and cold regions, significantly reducing reliance on air conditioning and demonstrating excellent climate adaptability. Furthermore, it achieves a visible light transmittance of ≥78%, ensuring ample indoor lighting. Simultaneously, the cost from glass film slurry preparation to glass film production is controlled at 150-160 RMB / m², demonstrating a significant cost advantage.

[0057] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method of preparing a glass film slurry by solid phase fusion gradient hyperdispersion, characterized by, Includes the following steps: S1: Weigh out the metal oxide, lanthanum hexaboride, and silicon dioxide in a mass ratio of 2~3:0.5~0.7:1~1.5, place them in an agate mortar and grind them thoroughly into powder. After passing through a 200-mesh sieve, obtain mixture A. S2: Transfer the mixture A obtained in S1 to a high-purity alumina crucible, place the high-purity alumina crucible in a muffle furnace for calcination at 1500℃, and cool it down to 800℃ to obtain mixture B. Pour mixture B onto a preheated alumina ceramic plate and let it cool naturally. After cooling to room temperature, block C is obtained. Block C is then placed in a muffle furnace for heat treatment and held at 800℃ for 1~2 hours before being allowed to cool naturally to room temperature. Block C is then removed and crushed into fine particles D. S3: Transfer particles D from step S2 to a ball mill jar. Add anhydrous ethanol to the ball mill jar at a mass-volume ratio of metal oxide to anhydrous ethanol of 1g:1~2ml. After wet milling, undried nanopowder E is obtained. Dry the undried nanopowder E to obtain dried nanopowder E. S4: Weigh out the following components according to the mass ratio of metal oxide, organic resin, silica aerogel powder, 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, lauramide propylamine oxide, butyl titanate, citric acid, and zinc nitrate: 1:60~80:0.7~1:0.5~0.8:0.5~0.7:0.3~0.5:0.1~0.3:0.3~0.7 respectively. Weigh out the following components according to the mass ratio of metal oxide, organic resin, silica aerogel powder, 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, lauramide propylamine oxide, citric acid, butyl titanate, and zinc nitrate: metal oxide, acetic acid, ethyl acetate ... The mass-to-volume ratio of ethyl acetate to deionized water is 1g:30~50ml:10~20ml. Ethyl acetate and deionized water are measured separately. The nanopowder E obtained in step S3, along with silica aerogel powder, 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, lauramide propylamine oxide, and tetrabutyl titanate are added to ethyl acetate. The mixture is stirred in a constant temperature water bath at 30~40℃ for 2~3h to obtain mixed solution F. At the same time, citric acid and zinc nitrate are added to deionized water. The mixture is mechanically stirred at a speed of 200~300rpm for 10~30min to obtain mixed solution G. S5: The organic resin weighed in step S4 is mechanically mixed and stirred with the mixed solution F and mixed solution G obtained in step S4 to obtain precursor solution H. The precursor solution H is ultrasonically dispersed. After the ultrasonic dispersion stops, the precursor solution H is placed in a constant temperature water bath at 50~80℃ and mechanically stirred to obtain glass film slurry precursor. The glass film slurry precursor is repeatedly filtered to obtain glass film slurry. The metal oxide in step S1 is a combination or all of the following: indium tin oxide, aluminum-doped zinc oxide, tungsten oxide, titanium dioxide, cerium oxide, copper oxide, silver oxide, lanthanum oxide, yttrium oxide, tellurium oxide, and aluminum oxide. The metal oxide contains at least indium tin oxide, tungsten oxide, titanium dioxide, copper oxide, silver oxide, and aluminum oxide. The mass ratio of each component in the metal oxide is 1:

1.

2. The method of claim 1, wherein the glass film slurry is prepared by a solid phase fusion gradient hyperdispersion method. In step S2, the calcination temperature is increased from room temperature to 1500℃ at a heating rate of 10~20℃ / min, and held at 1500℃ for 2~3 hours. Then, the muffle furnace temperature is first reduced to 1300℃ at a cooling rate of 10~20℃ / min, and then the muffle furnace temperature is rapidly reduced to 800℃ at a cooling rate of 50~100℃ / min, thus obtaining mixture B. In step S2, block C is placed in a muffle furnace for heat treatment, and the heat treatment temperature is increased from room temperature to 800℃ at a heating rate of 5~10℃ / min. The temperature of the preheated alumina ceramic plate in step S2 is 200~300℃.

3. The method of claim 1, wherein the glass thin film slurry is prepared by a solid phase fusion gradient hyperdispersion method. The average particle size distribution of the dried nanopowder E in step S3 is 5~10 nm.

4. The method of claim 3, wherein the glass thin film slurry is prepared by a solid phase fusion gradient hyperdispersion method. In step S3, the grinding jar is wet-milled using a high-energy planetary ball mill at a speed of 600-800 rpm for 15-20 hours.

5. The method of claim 4, wherein the glass film slurry is prepared by a solid phase fusion gradient hyperdispersion method. In step S3, the nanopowder E is dried using infrared drying at a temperature of 70-90°C for 20-50 minutes.

6. The method of claim 1, wherein the glass film slurry is prepared by a solid phase fusion gradient hyperdispersion method. The constant temperature water bath stirring method in step S4 adopts magnetic stirring, and the stirring speed is 100~200 rpm.

7. The method for preparing glass thin film slurry by solid-phase fusion gradient ultradispersion according to claim 1, characterized in that, In step S5, the ultrasonic dispersion uses an ultrasonic frequency of 30-50 kHz, a power of 500 W, and a dispersion time of 2-4 h.

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