CN111995229B - Composite light-storing ceramic for fire indication and preparation method thereof - Google Patents
Composite light-storing ceramic for fire indication and preparation method thereof Download PDFInfo
- Publication number
- CN111995229B CN111995229B CN202010941267.6A CN202010941267A CN111995229B CN 111995229 B CN111995229 B CN 111995229B CN 202010941267 A CN202010941267 A CN 202010941267A CN 111995229 B CN111995229 B CN 111995229B
- Authority
- CN
- China
- Prior art keywords
- light
- sintering
- storing
- powder
- ceramic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
- B32B7/023—Optical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/10—Interconnection of layers at least one layer having inter-reactive properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B1/00—Preparing the batches
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/026—Pelletisation or prereacting of powdered raw materials
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7792—Aluminates
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Ceramic Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Glass Compositions (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a composite light-storing ceramic for fire indication and a preparation method thereof, wherein light-storing powder and glass powder are respectively weighed according to the proportion and are put into a granulator to be directly stirred and granulated to obtain mixed materials; the mixed material is directly sieved and tiled in a mould through a screen mesh in the distributing machine, and then a ground glass sheet printed with patterns is covered on the surface of the mixed material and sent into a roller kiln together for firing; dividing the roller kiln into a preheating zone, three sintering zones, a quenching zone and a slow cooling zone, wherein the sintering step of the roller kiln comprises a pre-sintering stage, three sintering stages and two cooling stages; the ceramic product obtained by sintering is further processed according to requirements. After 20min light accumulation, the composite light-accumulating ceramic prepared by the invention can realize continuous luminescence for 18 hours (0.32 mcd/m2) at most, and the initial 1min intensity is 4800mcd/m 2; 60min intensity is more than 44mcd/m2 (20 min direct outdoor sunlight, 30min daylight lamp, 5min ultraviolet ray, 25 ℃ test at room temperature).
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic nonmetallic materials, relates to a preparation method of light-storing ceramic, and particularly relates to composite light-storing ceramic for fire indication and a preparation method thereof.
Background
The light storage material is a material which can emit light by itself within a certain time after the light source disappears through the irradiation of the light source. The special material can emit light at night or in dark places after being irradiated by sunlight or lamplight and the like, so that the special material has the excellent physical and chemical properties of no energy consumption and battery hidden danger, no need of laying a circuit, good chemical stability, long light-emitting time and the like, and is widely applied to the indication fields of architectural decoration, transportation, fire safety, subway tunnels and the like.
At present, in the research of light-storing materials for fire indication, the carrier materials of light-storing products commonly used at home and abroad are thin aluminum plates (light-storing material patterns are printed on the thin aluminum plates), plastics, printing ink, resin and other materials which can be shaped by normal temperature or lower temperature treatment. However, these materials tend to suffer from low luminance, short duration and poor weatherability.
Therefore, a light-storing material based on glass has been produced. The glass material has the advantages of high strength, good weather resistance, easy cleaning of the surface, long service life and the like. The advantages of the light-storing material and the advantages of the quartz glass material are integrated, namely the light-storing glass, so that the performance of the light-storing material product is further improved. CN110240472A discloses a light-storing ceramic based on glass prepared by mixing and sintering glass (quartz) powder and light-storing powder. The preparation process of the light-storing ceramic has the characteristics of low energy consumption, simple steps, low cost and the like. However, in the firing process of the light-storing ceramic, the light-storing powder on the surface of the light-storing ceramic is better than the light-storing powder without the protection of the initial melting glass powder, so that the surface is failed; meanwhile, the larger refractive index difference between the refractive index (larger than 1.45) and the air (the refractive index is 1.0) generates a total internal reflection effect when fluorescence is generated after the fluorescence is excited by external energy and is emitted from the upper surface of the ceramic, the calculated total reflection critical angle is 44 degrees, namely only 24.4 percent of the fluorescence can be emitted from the upper surface of the ceramic, and the rest of the fluorescence is limited by the total internal reflection effect and is transmitted in the ceramic in a waveguide effect mode until the fluorescence is completely lost. This inherent drawback limits the widespread use of light-storing ceramics.
Recently, a fluorescent ceramic with a characteristic microstructure is introduced with pores in the ceramic by adding pore-forming agents (such as starch, polyvinyl alcohol, dextrin, etc.), so that fluorescence is incident to the pores and then propagates in the ceramic in a scattering or reflection manner, thereby improving light extraction rate and absorption rate (such as patents CN109467453A and CN 110204321A). Different from naturally occurring air holes, the active introduction of scattering points increases the mean free path of photon propagation on one hand, and is beneficial to the full absorption of luminescent ions on natural light; and the waveguide effect and the total internal reflection effect of the fluorescence are effectively weakened, so that the extraction efficiency and the emergence efficiency of the fluorescence are improved.
However, the pore-forming agent is decomposed at a high temperature to generate a gas, but the pore-forming agent is often accompanied by a severe oxidation-reduction reaction or pyrolysis reaction, resulting in a case where the pore shape deviates from a normal spherical shape or the pore size is not uniform. Therefore, in order to prepare the light-storing ceramic with the micro-characteristic structure, a pore-forming agent and specific other additives need to be accurately selected according to the characteristics of raw materials and the requirements of products, and a specific ball milling and sintering process and the like are also needed. This will undoubtedly put great demands on workers in the field, and finally result in unstable light-emitting efficiency and low yield of the product.
Disclosure of Invention
The invention aims to provide the composite light-storing ceramic for fire indication, which is not added with a pore-forming agent and has high light efficiency.
The invention also aims to provide a method for preparing the composite light-storing ceramic for fire fighting indication, which has simple steps and short sintering time.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the composite light storage ceramic is prepared by sintering an upper layer of ground glass layer and a lower layer of light storage functional layer, wherein the lower layer of light storage functional layer is formed by sintering light storage powder and glass powder, the upper layer of glass layer is double-sided ground glass, and the components of the upper layer of glass layer are consistent with those of the glass powder in the lower layer of light storage functional layer.
Preferably, the roughness of the double-sided frosted glass is 7-13 microns, and the thickness of the double-sided frosted glass is 1-3 millimeters.
Fig. 1 shows the optical transmission path of the glass-air interface plane and rough surface. The figure shows a simple route by which the complete internal reflected light loss extraction can be significantly improved by the ground glass surface, and the innovative composite structure can increase the escape probability of the emergent rays and redirect photons originally emitted back to the glass substrate. In other words, the ground glass substrate can minimize total internal reflection light at the glass-air interface, thereby improving optical uniformity and luminous efficacy.
The invention also provides a preparation method of the composite light-storing ceramic for fire fighting indication, which comprises the following steps:
1) weighing raw materials: respectively weighing 10-30 parts of light-storing powder and 90-70 parts of glass powder by 100 parts by weight;
2) and (3) granulation: putting the raw materials weighed in the step 1) into a granulator, and directly stirring and granulating to obtain a mixed material;
3) stacking powder and forming: directly sieving the mixed material obtained in the step 2) through a screen in a distributing machine, flatly paving the mixed material in a mould, covering a ground glass sheet printed with patterns on the surface of the mixed material, wherein the shape of the mould and the ground glass sheet is required by the product requirement, and then feeding the mixed material into a roller kiln for firing;
4) sintering in a roller kiln: divide a preheating zone, three firing district, a quench zone and a slow cooling district with roller kilns, wherein, the preheating zone: the temperature ranges from room temperature to 720 ℃, and the sintering time is 20-35 min; a first firing zone: only opening a lower roller burner, controlling the temperature to be 800-810 ℃, and controlling the sintering time to be 10-20 min; a second sintering area: opening an upper roller burner at the temperature of 750-780 ℃, opening a lower roller nozzle at the temperature of 800-810 ℃, and sintering for 10-20 min; a third sintering area: opening an upper roller nozzle at the temperature of 860-900 ℃, opening a lower roller nozzle at the temperature of 890-930 ℃, and sintering for 15-25 min; a quenching zone: the temperature is 930-700 ℃, and the cooling time is 3-5 min; a slow cooling area: the temperature range is 700-room temperature, and the cooling time is 10-15 min;
5) product treatment: and 4) carrying out edge cutting treatment on the ceramic product obtained by sintering in the step 4) according to requirements.
Preferably, the particle size of the light-storing powder in the step 1) is 60-100 meshes, and the particle size of the glass powder is 80-200 meshes.
Preferably, the light-storing powder in the step 1) is rare earth doped alkaline earth metal aluminate.
Preferably, in the step 2), the rotating speed of the granulator in the whole stirring process is 80-250 rad/min, and the stirring time is 1-3 h.
Preferably, in the step 3), the aperture of the screen is 20-60 meshes; the pattern is formed by screen printing.
In the preparation process, a simple and convenient powder stacking process is adopted, any additive and water which can cause failure of light-storing powder are not needed in the powder mixing process, and the firing area is creatively and reasonably divided by combining the characteristic that the roller kiln can rapidly and continuously fire, and the opening sequence and firing time of the burners are arranged, so that the green body is sintered from bottom to top.
The invention is not only beneficial to the shrinkage sintering and the exhaust of the piled powder green body, but also can shorten the sintering time as much as possible, improve the productivity, simultaneously avoid damaging the initial brightness and afterglow time of the luminous center in the green body, and keep the luminous efficiency of the luminous center as much as possible; and the surface viscosity of the blank can be rapidly reduced in the third sintering area, a vitrified layer is formed in the quenching area, and the surface brightness and the glossiness are increased.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the adhesion degree of the ground glass layer and the glass can be increased in the sintering process of the glass powder and the light-storing powder from the lower side in the earlier stage, so that the combination of the molten fine glass powder and the glass sheet can protect the glass sheet before the oxidation temperature of the light-storing powder; meanwhile, the surface energy of the glass powder is higher than that of the ground glass sheet, so that the glass powder is prior to the ground glass sheetAnd melting, and under a proper temperature, the glass powder can be sintered, and the ground glass sheet can keep the original shape and structure. Compared with the prior art, the composite light-storing ceramic prepared by the invention can store light for 20min, and can realize 18 hours (at most)>0.32mcd/m 2 ) Continuous luminescence, initial 1min intensity>9700mcd/m 2 (ii) a Strength at 60min>1820mcd/m 2 (direct outdoor sunlight for 20min, fluorescent lamp for 30min, ultraviolet ray for 5min, room temperature 25 deg.C).
2. The rough frosted glass surface can enhance diffuse reflection light, and improve the visual comfort degree while improving the lighting effect. Compared with the prior art, the light efficiency of the surface of the product is improved by 20-38%.
3. The roller kiln is adopted for sintering, the discharge of air holes is promoted by reasonably arranging the opening sequence and the combustion temperature of the burners, and meanwhile, the glossiness of the surface of the ceramic can be increased. According to the actual statistics of the production line, the yield of the light-storing ceramic produced by the process reaches over 80 percent.
4. Compared with the prior art, the roller kiln has the production line operation characteristic of continuous sintering, the longest sintering time only needs 98min under the condition of achieving the product effect of the prior art, and the sintering time is saved by nearly 50 percent compared with the prior art. Under the full load working state, the yield can reach 9500 square meters after 24 hours by adopting the process.
Drawings
FIG. 1 is a graph showing the optical transmission paths of the glass-air interface plane and the rough surface in the composite light-storing ceramic of the present invention;
FIG. 2 is a diagram of a composite structure light-storing ceramic as prepared in example 1.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
In the following examples, the procedures are generally carried out under conventional conditions or conditions recommended by the manufacturer, unless otherwise specified, and the starting materials and reagents used are commercially available.
Example 1
The specific process comprises the following steps:
1) weighing raw materials: respectively weighing the particle sizes60 mesh light-storing powder (CaAl) 2 O 4 : eu and Nd)10 parts, and 90 parts of glass powder with the particle size of 80 meshes.
2) Powder preparation and treatment: putting the weighed raw materials into a granulator, directly stirring and granulating, and stirring for 1 hour to obtain a mixed material; the rotating speed of the granulator is 80rad/min in the whole stirring process.
3) Stacking powder and forming: directly sieving and flatly paving the mixed material obtained in the step 2) into a mould through a screen (the aperture is 20 meshes) in a distributing machine, then covering a rough glass sheet (the roughness is 13 microns and the thickness is 3 millimeters) printed with a left-turn outlet indication pattern through a screen printing machine on the surface of the mixed material, enabling one surface printed with the pattern to face downwards, enabling the mould and the rough glass sheet to be rectangular (10cm 20cm), and then feeding the mixture into a roller kiln for firing.
4) Firing: a preheating zone: the temperature ranges from room temperature to 720 ℃, and the sintering time is 20 min; a first firing zone: only opening a lower roller burner, controlling the temperature range at 800 ℃, and sintering for 10 min; a second sintering area: opening an upper roller burner at the temperature of 750 ℃ and a lower roller nozzle at the temperature of 800 ℃ for 10 min; a third firing zone: opening an upper roller nozzle, wherein the temperature range is 860 ℃, opening a lower roller nozzle, the temperature range is 890 ℃, and the sintering time is 15 min; a quenching zone: the temperature range is 930 ℃, and the cooling time is 3 min; a slow cooling area: the temperature range is 700-room temperature, and the cooling time is 15 min.
5) Product treatment: and (5) trimming the product according to requirements. As shown in FIG. 2, the ceramic material object can be seen to have a ground glass layer as the upper layer and a light-storing functional layer as the lower layer.
The test of the product shows that after 20min of light storage, 17 hours can be realized>0.32mcd/m 2 ) The initial 1min intensity of 9357mcd/m 2 (ii) a The strength at 60min was 1542mcd/m 2 (direct outdoor sunlight for 20min, fluorescent lamp for 30min, ultraviolet ray for 5min, room temperature for 25 deg.C); the luminous efficiency of the emitted light is improved by 20%.
Example 2
The specific process comprises the following steps:
1) weighing raw materials: respectively weighing the light-storing powder (Sr) with the grain diameter of 80 meshes 4 Al 14 O 25 ：Eu，Dy)25 parts of glass powder with the particle size of 100 meshes and 75 parts of glass powder.
2) Powder preparation and treatment: putting the weighed raw materials into a granulator, directly stirring and granulating, and stirring for 2 hours to obtain a mixed material; the rotating speed of the granulator is 100rad/min in the whole stirring process.
3) Stacking powder and forming: directly sieving and flatly paving the mixed material obtained in the step 2) into a mould through a screen (with the aperture of 40 meshes) in a distributing machine, covering a frosted glass sheet (with the roughness of 10 micrometers and the thickness of 2 millimeters) printed with a right-turn outlet indication pattern through a screen printing machine on the surface of the mixed material, enabling one surface printed with the pattern to face downwards, enabling the mould and the frosted glass sheet to be square (25cm × 25cm), and then feeding the mixed material into a roller kiln for firing.
4) Firing: a preheating zone: the temperature ranges from room temperature to 720 ℃, and the sintering time is 30 min; a first firing zone: only opening a lower roller burner, controlling the temperature range at 805 ℃ and the sintering time at 15 min; a second sintering area: opening an upper roller burner at 760 ℃ and opening a lower roller nozzle at 805 ℃ for 15 min; a third sintering area: opening an upper roller nozzle, wherein the temperature range is 880 ℃, opening a lower roller nozzle, the temperature range is 900 ℃, and the sintering time is 20 min; a quenching zone: the temperature range is 900-700 ℃, and the cooling time is 4 min; a slow cooling area: the temperature range is 700-room temperature, and the cooling time is 13 min.
5) Product treatment: and (5) trimming the product according to requirements.
The test result of the product shows that after 20min light storage, 18 hours can be realized>0.32mcd/m 2 ) The initial 1min intensity of 9670mcd/m 2 (ii) a The intensity at 60min is 1783mcd/m 2 (direct outdoor sunlight for 20min, fluorescent lamp for 30min, ultraviolet ray for 5min, room temperature for 25 deg.C); the luminous efficiency of the emitted light is improved by 27%.
Example 3
The specific process comprises the following steps:
1) weighing raw materials: respectively weighing light-storing powder (SrAl) with the particle size of 100 meshes 2 O 4 : eu and Dy)30 parts and glass powder with the particle size of 200 meshes 70 parts.
2) Powder preparation and treatment: putting the weighed raw materials into a granulator, directly stirring and granulating, and stirring for 3 hours to obtain a mixed material; the granulator speed is 250rad/min during the whole stirring process.
3) Stacking powder and forming: directly sieving and flatly paving the mixed material obtained in the step 2) into a mould through a screen (with the aperture of 60 meshes) in a distributing machine, then covering a frosted glass sheet (with the roughness of 7 micrometers and the thickness of 0.5 millimeter) printed with an emergency exit indication pattern through a screen printing machine on the surface of the mixed material, enabling one surface printed with the pattern to face downwards, enabling the mould and the frosted glass sheet to be square (25cm × 25cm), and then feeding the mixed material into a roller kiln for firing.
4) Firing: a preheating zone: the temperature ranges from room temperature to 720 ℃, and the sintering time is 35 min; a first firing zone: only opening a lower roller burner, controlling the temperature range at 810 ℃ and the sintering time at 20 min; a second sintering area: opening an upper roller burner at 780 ℃ and a lower roller nozzle at 810 ℃ for 20 min; a third firing zone: opening an upper roller nozzle at 900 ℃ and a lower roller nozzle at 930 ℃ for 25 min; a quenching zone: the temperature is 930-700 ℃, and the cooling time is 5 min; a slow cooling area: the temperature range is 700-room temperature, and the cooling time is 15 min.
5) Product treatment: and (5) trimming the product according to requirements.
The test on the product shows that the light accumulation can be realized for 18 hours at most after 20 min: (>0.32mcd/m 2 ) The initial 1min intensity of 9700mcd/m 2 (ii) a The strength at 60min was 1820mcd/m 2 (direct outdoor sunlight for 20min, fluorescent lamp for 30min, ultraviolet ray for 5min, room temperature for 25 deg.C); the luminous efficiency of the emitted light is improved by 38%.
Comparative example 1
The specific process comprises the following steps:
1) weighing raw materials: respectively weighing light-storing powder (SrAl) with the particle size of 100 meshes 2 O 4 : eu and Dy)30 parts, and glass powder with the particle size of 200 meshes 70 parts.
2) Powder preparation and treatment: putting the weighed raw materials into a granulator, directly stirring and granulating, and stirring for 3 hours to obtain a mixed material; the granulator speed is 250rad/min during the whole stirring process.
3) Stacking powder and forming: directly sieving and flatly paving the mixed material obtained in the step 2) into a mold through a screen (with the aperture of 60 meshes) in a distributing machine, wherein the mold is square (25cm x 25cm), and then feeding into a roller kiln for firing.
4) Firing: a preheating zone: the temperature ranges from room temperature to 720 ℃, and the sintering time is 35 min; a first firing zone: only opening a lower roller burner, controlling the temperature range at 810 ℃ and the sintering time at 20 min; a second sintering area: opening an upper roller burner at 780 ℃ and a lower roller nozzle at 810 ℃ for 20 min; a third sintering area: opening an upper roller nozzle at 900 ℃ and a lower roller nozzle at 930 ℃ for 25 min; a quenching zone: the temperature is 930-700 ℃, and the cooling time is 5 min; a slow cooling area: the temperature range is 700-room temperature, and the cooling time is 15 min.
5) Product treatment: and (5) trimming the product according to requirements.
The test on the product shows that the light accumulation can be realized for 18 hours at most after 20 min: (>0.32mcd/m 2 ) The initial 1min intensity of 7185mcd/m 2 (ii) a The intensity at 60min is 1793mcd/m 2 (direct outdoor sunlight for 20min, fluorescent lamp for 30min, ultraviolet ray for 5min, room temperature 25 deg.C).
Claims (6)
1. The composite light-storing ceramic for fire fighting indication is characterized by being prepared by sintering an upper layer of ground glass layer and a lower layer of light-storing functional layer, wherein the lower layer of light-storing functional layer is prepared by sintering light-storing powder and glass powder, the upper layer of ground glass layer is double-sided ground glass, and the components of the upper layer of ground glass layer are consistent with those of the glass powder in the lower layer of light-storing functional layer; the preparation method of the composite light-storing ceramic for fire fighting indication comprises the following steps:
1) weighing raw materials: respectively weighing 10-30 parts of light-storing powder and 90-70 parts of glass powder by 100 parts by weight;
2) and (3) granulation: putting the raw materials weighed in the step 1) into a granulator, and directly stirring and granulating to obtain a mixed material;
3) stacking powder and forming: directly sieving the mixed material obtained in the step 2) through a screen in a distributing machine, flatly paving the mixed material in a mould, covering a ground glass sheet printed with patterns on the surface of the mixed material, wherein the shape of the mould and the ground glass sheet is required by the product requirement, and then feeding the mixed material into a roller kiln for firing;
4) sintering in a roller kiln: divide a preheating zone, three firing district, a quench zone and a slow cooling district with roller kilns, wherein, the preheating zone: the temperature ranges from room temperature to 720 ℃, and the sintering time is 20-35 min; a first firing zone: only opening a lower roller burner, controlling the temperature to be 800-810 ℃, and controlling the sintering time to be 10-20 min; a second firing zone: opening an upper roller burner at the temperature of 750-780 ℃, opening a lower roller nozzle at the temperature of 800-810 ℃, and sintering for 10-20 min; a third sintering area: opening an upper roller nozzle at the temperature of 860-900 ℃, opening a lower roller nozzle at the temperature of 890-930 ℃, and sintering for 15-25 min; a quenching zone: the temperature is 930-700 ℃, and the cooling time is 3-5 min; a slow cooling area: the temperature range is 700-room temperature, and the cooling time is 10-15 min;
5) product treatment: and 4) carrying out edge cutting treatment on the ceramic product obtained by sintering in the step 4) according to requirements.
2. The composite light-storing ceramic for fire fighting indication according to claim 1, wherein the roughness of the double-sided frosted glass is 7-13 μm, and the thickness is 1-3 mm.
3. The composite light-storing ceramic for fire fighting indication as defined in claim 1, wherein the particle size of the light-storing powder in step 1) is 80-200 mesh, and the particle size of the glass powder is 60-100 mesh.
4. The composite light-storing ceramic for fire fighting indication according to claim 1, wherein the light-storing powder in step 1) is rare earth doped alkaline earth metal aluminate.
5. The composite light-storing ceramic for fire fighting indication according to claim 1, wherein in the step 2), the rotating speed of the granulator in the whole stirring process is 80-250 rad/min, and the stirring time is 1-3 h.
6. The composite light-storing ceramic for fire fighting indication according to claim 1, wherein in step 3), the mesh has a pore size of 20-60 mesh.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010941267.6A CN111995229B (en) | 2020-09-09 | 2020-09-09 | Composite light-storing ceramic for fire indication and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010941267.6A CN111995229B (en) | 2020-09-09 | 2020-09-09 | Composite light-storing ceramic for fire indication and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111995229A CN111995229A (en) | 2020-11-27 |
| CN111995229B true CN111995229B (en) | 2022-08-02 |
Family
ID=73469086
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010941267.6A Active CN111995229B (en) | 2020-09-09 | 2020-09-09 | Composite light-storing ceramic for fire indication and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111995229B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114464384B (en) * | 2022-03-02 | 2022-10-14 | 深圳安培龙科技股份有限公司 | Gold electrode NTC thermistor chip, preparation method and temperature sensor |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070948A (en) * | 2007-05-11 | 2007-11-14 | 杨毅男 | Environment-protection energy-accumulated self-illuminating and light-reflecting structure |
| CN101428974B (en) * | 2008-12-24 | 2012-01-18 | 葛利民 | High-brightness extinction, light-storing, luminescent glass and method of producing the same |
| CN103880273A (en) * | 2012-12-19 | 2014-06-25 | 湖北春永明亮科技有限公司 | Light-retaining self-luminous multilayered glass |
| CN103837916B (en) * | 2014-03-19 | 2017-01-18 | 张家港康得新光电材料有限公司 | Retro-reflective film |
| CN106517816A (en) * | 2016-10-21 | 2017-03-22 | 武汉理工大学 | Fluorescent glass with gradient refractive index and preparation method thereof |
| CN107804974B (en) * | 2017-11-01 | 2020-02-21 | 上海应用技术大学 | Preparation method of remote fluorescent sheet based on low-melting-point lead-free glass powder |
| CN110357424A (en) * | 2019-06-26 | 2019-10-22 | 中国计量大学 | A kind of complex phase fluorescent glass and its cryogenic high pressure sintering preparation method |
-
2020
- 2020-09-09 CN CN202010941267.6A patent/CN111995229B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN111995229A (en) | 2020-11-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4765525B2 (en) | Luminescent color conversion member | |
| CN102633440B (en) | Glass coating containing fluorophor and method for producing glass coating, and light-emitting device and method for manufacturing light-emitting device | |
| US20130049575A1 (en) | Phosphor composite member, led device and method for manufacturing phosphor composite member | |
| JP3311254B2 (en) | Inorganic artificial ceramic granular product having luminous fluorescent properties and method for producing the same | |
| WO2011111462A1 (en) | Wavelength conversion member, optical device, and process for production of wavelength conversion member | |
| JP2009524235A (en) | Sheet-like antibody, method for producing the same, and light-emitting device using the same | |
| CN109301057A (en) | Wavelength conversion member and use luminescent device made of the component | |
| KR20110003377A (en) | Conversion material, especially for a white or colored light source comprising a semiconductor light source, method for producing the same and light source comprising said conversion material | |
| JP2008169348A (en) | Phosphor composite material | |
| CN101696085A (en) | Yttrium aluminum garnet fluorescent glass, manufacturing method thereof and use thereof | |
| CN107304984A (en) | Wavelength convert part and Projecting Lamp | |
| JP7212319B2 (en) | Wavelength conversion member and light emitting device | |
| CN111995229B (en) | Composite light-storing ceramic for fire indication and preparation method thereof | |
| US20220089498A1 (en) | Multicolor light-storing ceramic for fire-protection indication and preparation method thereof | |
| CN102464450A (en) | Green and energy-saving fluorescent powder/glass compound luminous material and preparation method thereof | |
| US20160033679A1 (en) | Light reflective substrate and light emitting device using the same | |
| JP6004250B2 (en) | Wavelength conversion member and light emitting device | |
| JP2011222751A (en) | Wavelength conversion member and semiconductor light-emitting element device having and using the wavelength conversion member | |
| TW201422555A (en) | White glass | |
| CN112863328A (en) | Diffusion plate, backlight module and preparation method of diffusion plate | |
| EP2814072A1 (en) | Light-emitting device | |
| US20060214134A1 (en) | Luminescent glass article and method of manufacturing the same | |
| CN110540728A (en) | energy-storage self-luminous material, preparation method and application thereof, self-luminous particles and self-luminous brick | |
| CN101723588B (en) | Long-persistence luminous enameled plate and preparation method thereof | |
| CN110783471A (en) | Perovskite quantum dot light-emitting device and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |