CN116970294A - Coating, quartz tube containing same and application - Google Patents

Coating, quartz tube containing same and application Download PDF

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Publication number
CN116970294A
CN116970294A CN202310951437.2A CN202310951437A CN116970294A CN 116970294 A CN116970294 A CN 116970294A CN 202310951437 A CN202310951437 A CN 202310951437A CN 116970294 A CN116970294 A CN 116970294A
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China
Prior art keywords
coating
quartz tube
sintering
temperature
parts
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Inventor
祁东
林佳继
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Jiageng Jiangsu Special Materials Co ltd
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Jiageng Jiangsu Special Materials Co ltd
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Priority to CN202310951437.2A priority Critical patent/CN116970294A/en
Publication of CN116970294A publication Critical patent/CN116970294A/en
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/008Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
    • C03C17/009Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08Anti-corrosive paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/43Thickening agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention provides a coating, a quartz tube containing the coating and application of the quartz tube. The paint comprises 90-110 parts of inorganic micro powder, 140-160 parts of water, 1-2 parts of thickener, 2.5-4 parts of high-temperature binder and 1.5-3 parts of foaming agent. The quartz tube comprises a quartz tube and a porous coating arranged on the inner wall of the quartz tube, wherein the raw materials of the porous coating comprise the coating. The coating has the advantages of high temperature resistance, uniform pores, high viscosity and high adhesive force, and the coating obtained by curing the coating has a porous structure, so that the stress difference caused by the difference of expansion coefficients can be effectively reduced, and the thermal shock performance of the coating is improved.

Description

Coating, quartz tube containing same and application
Technical Field
The invention belongs to the field of photovoltaic materials, and relates to a coating, in particular to a coating, a quartz tube containing the same and application of the coating.
Background
In the processing of photovoltaic material semiconductors, LPCVD (low pressure chemical vapor deposition) equipment is a vacuum high temperature furnace, and a quartz furnace tube is used as a cavity material of the vacuum furnace, and has the advantages of high temperature resistance, good light transmittance and good thermal stability. Therefore, the production cost is increased, and meanwhile, the damaged quartz furnace tube can damage the furnace body structure, so that larger loss and risk are caused.
Therefore, increasing the lifetime of the quartz furnace tube can create significant economic value and increase the core competitiveness of the enterprise. At present, the research direction for prolonging the service life of the quartz furnace tube is mainly in two aspects of functional coating and double-layer structure.
The functional coating of the quartz tube is mainly determined by the components of the coating, and the quartz tube is commonly used for high-temperature calcination, so that the coating needs to have good high-temperature resistance, has low thermal conductivity, and can effectively prevent the damage of high temperature to a substrate material.
The conventional high-temperature resistant coating mainly comprises an organic high-temperature resistant coating and an inorganic high-temperature resistant coating, but most high-temperature resistant coatings are applied to a static high-temperature environment, and when the high-temperature resistant coating is used in a high-temperature dynamic environment, cracks are generated on the surface of a coating obtained by curing the coating, so that the problems of cracking, peeling, breaking and the like are caused.
Therefore, how to prepare a coating curable to a coating having good thermal shock properties is an important research direction in the art.
Disclosure of Invention
The invention aims to provide a coating, a quartz tube containing the coating and application of the quartz tube. The coating has the advantages of high temperature resistance, uniform pores, high viscosity, high curing strength and high adhesive force, and the coating obtained by curing the coating has a porous structure, so that the stress difference caused by the expansion coefficient difference can be effectively reduced, and the thermal shock performance of the coating is improved.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
the invention aims at providing a coating which comprises 90-110 parts of inorganic micro powder, 140-160 parts of water, 1-2 parts of thickener, 2.5-4 parts of high-temperature binder and 1.5-3 parts of foaming agent.
The inorganic fine powder may be 90 parts, 92 parts, 94 parts, 96 parts, 98 parts, 100 parts, 102 parts, 104 parts, 106 parts, 108 parts or 110 parts, etc., the water may be 140 parts, 142 parts, 144 parts, 146 parts, 148 parts, 150 parts, 152 parts, 154 parts, 156 parts, 158 parts or 160 parts, etc., the thickener may be 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts or 2 parts, etc., the high-temperature binder may be 2.5 parts, 2.8 parts, 3.0 parts, 3.2 parts, 3.4 parts, 3.6 parts, 3.8 parts or 4 parts, etc., and the foaming agent may be 1.5 parts, 1.8 parts, 2.0 parts, 2.2 parts, 2.4 parts, 2.6 parts, 2.8 parts or 3 parts, etc., but the above range is not limited to the above range of values and other values may not be used.
The coating has the advantages of high temperature resistance, uniform pores, high viscosity and high adhesive force, and can obtain a coating with a porous structure after being cured into the coating, and the porous structure of the porous coating can effectively reduce the stress difference caused by the expansion coefficient difference, so that the thermal shock performance of the coating is improved.
The proportion of the inorganic micro powder and the foaming agent influences the size and the quantity of the pores of the coating, and excessive proportion of the foaming agent can cause that the pores of the prepared coating are more in pores, the diameter of the pore diameter is large, the pores are uneven, and even the pores are broken to form gaps; the proportion of the foaming agent is too small, the prepared coating has few pores and small diameter of pore diameter, and even has the problem of partial unfoamed structure.
The high-temperature binder is related to the sintering process of the coating, if the content of the added high-temperature binder is too high, the cost for preparing the coating can be increased, the coating obtained by curing the coating can generate cracking and falling risks, and if the content of the added high-temperature binder is too low, the curing strength of the inorganic micro powder is low, or the inorganic micro powder cannot be cured, and the phenomenon that the inorganic micro powder falls easily occurs in the curing process of the coating.
The proportion of the thickener and the water in the invention is used for influencing the viscosity and the solid content of the coating, thereby influencing the spraying construction of the coating and the adhesive force between the coating and the quartz tube wall after spraying. Therefore, on the basis of ensuring a certain solid content, the viscosity of the paint can be adjusted by adjusting the proportion of the thickening agent, if the proportion of the thickening agent is too high, the paint cannot be atomized well to form a uniform coating, and if the proportion of the thickening agent is too low, the paint cannot be adhered to the pipe wall well, and even the flow of the paint can be formed.
As a preferable technical scheme of the invention, the inorganic micro powder comprises silicon micro powder, alumina powder, talcum powder, feldspar powder and broken glass.
Preferably, the mass ratio of the silicon micropowder, the alumina powder, the talcum powder, the feldspar powder and the broken glass is
(20-40): (14-26): (5-10): (12-16): (25-35), wherein the mass ratio may be 30:26:5:14:25, 30:20:10:15:25, 35:18:5:12:30 or 40:18:5:12:25, etc., but is not limited to the recited values, other non-recited values within this range of values are equally applicable.
Preferably, the thickener comprises any one or a combination of at least two of polyacrylamide, hydroxypropyl methylcellulose or carboxymethylcellulose, wherein typical but non-limiting examples of such combinations are: a combination of polyacrylamide and hydroxypropyl methylcellulose, a combination of hydroxypropyl methylcellulose and carboxymethyl cellulose, or a combination of polyacrylamide and carboxymethyl cellulose, etc.
Preferably, the high temperature binder comprises any one or a combination of at least two of silica sol, phosphoric acid solution or aluminum dihydrogen phosphate, wherein typical but non-limiting examples of the combination are: a combination of silica sol and phosphoric acid solution, a combination of phosphoric acid solution and aluminum dihydrogen phosphate, or a combination of silica sol and aluminum dihydrogen phosphate, etc.
Preferably, the foaming agent comprises any one or a combination of at least two of calcium carbonate, sodium carbonate or silicon carbide, wherein typical but non-limiting examples of the combination are: a combination of heavy calcium powder and sodium carbonate, a combination of sodium carbonate and silicon carbide, or a combination of heavy calcium powder and silicon carbide, etc.
The second object of the invention is to provide a quartz tube, which comprises a quartz tube and a porous coating layer arranged on the inner wall of the quartz tube.
The raw materials of the porous coating comprise the coating according to one of the purposes.
In order to improve the thermal shock performance of the coating and avoid the coating from falling off at high temperature, the coating containing the foaming agent is added in the preparation process of the porous coating to prepare the porous coating, the porous structure of the coating can effectively reduce the stress difference caused by the expansion coefficient difference between the coating and the quartz tube, so that the thermal shock performance of the coating is improved, the porous coating can also effectively prevent sediment erosion and improve the average service life of the quartz tube, and in addition, the existence of the porous coating obviously reduces the heat dissipation of a hearth, thereby achieving the purposes of reducing heat loss and realizing energy conservation and emission reduction.
As a preferred embodiment of the present invention, the thickness of the porous coating layer is 0.3 to 1.0mm, wherein the thickness may be 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm, 1.0mm, etc., but is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Preferably, the pore size of the porous coating is 0.3 to 1.0mm, wherein the pore size may be 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm, or 1.0mm, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
The pores of the porous coating are of a closed pore structure with uniform size.
Another object of the present invention is to provide a method for manufacturing a quartz tube as defined in the second object, comprising:
dispersing the raw materials of the porous coating to obtain a coating, spraying the coating on the inner wall of a quartz tube, and drying and sintering to obtain the quartz tube;
the raw materials of the porous coating comprise inorganic micro powder, water, a thickening agent, a high-temperature binder and a foaming agent.
According to the invention, the foaming agent is added, the sintering temperature is controlled, and the lightweight porous coating structure is prepared, so that the stress difference generated by different expansion coefficients can be effectively relaxed.
As a preferable technical scheme of the invention, the preparation method of the coating comprises the following steps: the inorganic micro powder is prepared into inorganic micro powder slurry, and then dispersed with a thickener, a high-temperature binder and a foaming agent.
Preferably, the preparation method of the inorganic micro powder slurry comprises the following steps: and ball milling the inorganic micro powder, the grinding balls and water to obtain the inorganic micro powder slurry.
Preferably, the mass ratio of the inorganic micro powder, the grinding balls and the water is 1 (0.8-1.2): (1.2-1.7), wherein the mass ratio may be 1:0.8:1.2, 1:0.8:1.3, 1:0.8:1.4, 1:0.8:1.5, 1:0.8:1.6, 1:0.8:1.7, 1:1.0:1.2, 1:1.0:1.3, 1:1.0:1.4, 1:1.0:1.5, 1:1.0:1.6, 1:1.0:1.7, 1:1.2:1.2:1.3, 1:1.2:1.4, 1:1.2:1.5, 1:1.2:1.6 or 1:1.2:1.7, but the present invention is not limited to the same numerical values as those listed above.
Preferably, the ball milling time is 6 to 8 hours, wherein the time can be 6 hours, 6.2 hours, 6.4 hours, 6.6 hours, 6.8 hours, 7.0 hours, 7.2 hours, 7.4 hours, 7.6 hours, 7.8 hours or 8 hours, etc., but not limited to the recited values, other non-recited values within the range of values are equally applicable.
As a preferable embodiment of the present invention, the thickness of the spray coating is 0.3 to 1mm, wherein the thickness may be 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm or 1mm, etc., but is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
The coating of the invention has too thick spraying thickness, can form a three-dimensional structure, and has adverse effect on the temperature rise and fall of the quartz tube, thereby causing great difference of thermal stress and damaging the quartz tube; the coating thickness is too thin, so that the coating is unevenly distributed, the phenomenon of coating deficiency or excessive accumulation occurs, and the protection effect of the coating is reduced.
Preferably, the drying time is 2.5-3.5 h, wherein the time can be 2.5h, 2.6h, 2.7h, 2.8h, 2.9h, 3.0h, 3.1h, 3.2h, 3.3h, 3.4h or 3.5h, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the drying temperature is 10 to 35 ℃, wherein the temperature may be 10 ℃, 12 ℃, 14 ℃, 16 ℃, 18 ℃, 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃, 30 ℃, 32 ℃, 34 ℃, 35 ℃, or the like, but is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
As a preferred technical scheme of the invention, the sintering comprises a first-stage sintering, a second-stage sintering and a third-stage sintering which are sequentially carried out.
The invention is divided into three sections for sintering, wherein the first section is used for removing moisture and a small amount of organic matters, the second section is used for crystallizing and solidifying the adhesive and the micro powder, the third section is used for inducing the foaming agent to generate gas, and the coating has a certain viscosity at the temperature so as to wrap the gas and form a closed structure.
Preferably, the heating rate of the one-stage sintering is 5 to 8 ℃/min, wherein the heating rate can be 5 ℃/min, 6 ℃/min, 7 ℃/min or 8 ℃/min, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the temperature of the one-stage sintering is 100 to 140 ℃, wherein the temperature may be 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃ or the like, but is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Preferably, the heat preservation time of the sintering is 25-35 mins, wherein the heat preservation time can be 25mins, 26mins, 27mins, 28mins, 29mins, 30mins, 31mins, 32mins, 33mins, 34mins or 35mins, and the like, but is not limited to the recited values, and other non-recited values in the range of the values are equally applicable.
Preferably, the heating rate of the two-stage sintering is 8 to 10 ℃/min, wherein the heating rate can be 8 ℃/min, 9 ℃/min or 10 ℃/min, etc., but is not limited to the recited values, and other non-recited values in the range of the values are equally applicable.
Preferably, the temperature of the two-stage sintering is 350 to 400 ℃, wherein the temperature can be 350 ℃, 360 ℃, 370 ℃, 380 ℃, 390 ℃, 400 ℃ or the like, but is not limited to the recited values, and other non-recited values in the range of the values are equally applicable.
Preferably, the heat preservation time of the two-stage sintering is 15-25 mins, wherein the heat preservation time can be 15mins, 16mins, 17mins, 18mins, 19mins, 20mins, 21mins, 22mins, 23mins, 24mins or 25mins, and the like, but is not limited to the recited values, and other non-recited values in the range of the values are equally applicable.
Preferably, the temperature rising rate of the three-stage sintering is 5 to 8 ℃/min, wherein the temperature rising rate can be 5 ℃/min, 6 ℃/min, 7 ℃/min or 8 ℃/min, and the like, but is not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
Preferably, the temperature of the three-stage sintering is 1100 to 1200 ℃, wherein the temperature may be 1100 ℃, 1110 ℃, 1120 ℃, 1130 ℃, 1140 ℃, 1150 ℃, 1160 ℃, 1170 ℃, 1180 ℃, 1190 ℃ or 1200 ℃, etc., but is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Preferably, the three-stage sintering has a heat preservation time of 15-25 mins, wherein the heat preservation time can be 15mins, 16mins, 17mins, 18mins, 19mins, 20mins, 21mins, 22mins, 23mins, 24mins or 25mins, and the like, but is not limited to the recited values, and other non-recited values in the range of the values are equally applicable.
Preferably, the quartz tube is obtained by naturally cooling the sintered quartz tube to room temperature.
As a preferable technical scheme of the invention, the preparation method comprises the following steps:
dispersing the raw materials of the porous coating to obtain a coating, and spraying the coating on the inner wall of a quartz tube, wherein the thickness of the coating is 0.3-1 mm;
the porous coating quartz tube is obtained through drying at room temperature for 2.5-3.5 hours and sequentially performing primary sintering, secondary sintering and tertiary sintering, wherein the temperature rising rate of the primary sintering is 5-8 ℃/min, the temperature is 100-140 ℃ and the heat preservation time is 25-35 mins, the temperature rising rate of the secondary sintering is 8-10 ℃, the temperature is 350-400 ℃ and the heat preservation time is 15-25 mins, the temperature rising rate of the tertiary sintering is 5-8 ℃, the temperature is 1100-1200 ℃ and the heat preservation time is 15-25 mins.
It is a further object of the present invention to provide the use of a coating as defined in one of the objects, which is used in the field of photovoltaic materials.
Compared with the prior art, the invention has the following beneficial effects:
(1) The coating has the advantages of high temperature resistance, uniform pores, high viscosity and high adhesive force, and the coating obtained by curing the coating has a porous structure, so that the stress difference caused by the expansion coefficient difference can be effectively reduced, and the thermal shock performance of the coating is improved;
(2) The porous coating quartz tube with good high temperature resistance, corrosion resistance and thermal shock resistance provided by the invention has the advantages that the porous structure of the coating can effectively reduce the stress difference caused by the expansion coefficient difference between the coating and the quartz tube, so that the thermal shock resistance of the coating is improved;
(3) The heat resistance of the porous coating quartz tube can reach more than 1000 ℃, the porous coating quartz tube is heated to 800 ℃, is taken out and is quenched at room temperature after heat preservation for 20min, and is repeatedly operated for 5 times, so that peeling, cracking and layering of the coating are avoided; in addition, the porous coating quartz tube can effectively block erosion of sediment, and the service life is longer than 60 days.
Drawings
FIG. 1 is a graph showing the morphology of a porous coated quartz tube according to example 1 of the present invention.
FIG. 2 is a graph of the morphology of the porous coated quartz tube of example 2 of the present invention.
FIG. 3 is a graph of the morphology of the porous coated quartz tube of example 3 of the present invention.
FIG. 4 is a graph of the morphology of the porous coated quartz tube of example 4 of the present invention.
FIG. 5 is a graph of the coating morphology of a porous coated quartz tube according to example 6 of the present invention.
FIG. 6 is a graph of the coating morphology of a porous coated quartz tube in example 8 of the present invention.
FIG. 7 is a graph of the coating morphology of a porous coated quartz tube in example 10 of the present invention.
FIG. 8 is a graph of the coating morphology of a porous coated quartz tube in example 11 of the present invention.
FIG. 9 is a graph showing the morphology of the porous coated quartz tube of comparative example 1 of the present invention.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a preparation method of a porous coating quartz tube, which comprises the following steps:
1. preparation of inorganic micropowder slurry
Raw materials are weighed according to the specification in table 1.1, and inorganic micro powder is obtained after uniform mixing for standby.
TABLE 1.1
Raw material name Silica micropowder Alumina powder Talc powder Feldspar powder Broken glass
Weighing (g) 320 180 80 140 280
Raw material specification (mesh) 300 1000 1000 300 White glass fragments
Pouring the mixture of the inorganic micro powder into a stainless steel ball milling tank, sequentially adding 1.5kg of water and 5kg of stainless steel balls, ball milling for 8 hours at the rotating speed of 70r/min, taking out the slurry, and sieving with a 600-mesh sieve to obtain the inorganic micro powder slurry.
2. Preparation of the coating
Adding hydroxypropyl methylcellulose, silica sol, aluminum dihydrogen phosphate solution and calcium carbonate into the inorganic micro powder slurry, and stirring uniformly by an automatic stirrer to obtain the coating, wherein the addition amounts of various additives are shown in table 1.2.
TABLE 1.2
3. Preparation of porous coated quartz tube
And (3) atomizing and granulating 300ml of coating by using a high-pressure sprayer, uniformly spraying on the inner wall of a quartz tube, controlling the thickness of the coating to be 0.6mm after spraying, drying, sintering, raising the temperature to 120 ℃ according to the heating speed of 8 ℃/min, preserving heat for 30min, performing primary sintering, raising the temperature to 380 ℃ according to the heating speed of 8 ℃/min, preserving heat for 20min, performing secondary sintering, raising the temperature to 1180 ℃ according to the heating speed of 5 ℃/min, preserving heat for 20min, performing tertiary sintering, and then turning off a power supply to enable the quartz tube to be naturally cooled to room temperature along with a sintering furnace, and taking out the porous coated quartz tube. The coating morphology diagram of the porous coating quartz tube of the embodiment is shown in figure 1.
Example 2
The embodiment provides a preparation method of a porous coating quartz tube, which comprises the following steps:
1. preparation of inorganic micropowder slurry
Raw materials are weighed according to the specification in table 2.1, and inorganic micro powder is obtained after uniform mixing for standby.
TABLE 2.1
Pouring the mixture of the inorganic micro powder into a stainless steel ball milling tank, sequentially adding 1.5kg of water and 5kg of stainless steel balls, ball milling for 8 hours at the rotating speed of 70r/min, taking out the slurry, and sieving with a 600-mesh sieve to obtain the inorganic micro powder slurry.
2. Preparation of the coating
Adding hydroxypropyl methylcellulose, silica sol, phosphoric acid solution and calcium carbonate into the inorganic micro powder slurry, and uniformly stirring by using an automatic stirrer to obtain the coating, wherein the addition amounts of various additives are shown in table 2.2.
TABLE 2.2
3. Preparation of porous coated quartz tube
And (3) atomizing and granulating 300ml of coating by using a high-pressure sprayer, uniformly spraying on the inner wall of a quartz tube, controlling the thickness of the coating to be 0.3mm after spraying, drying, sintering, raising the temperature to 100 ℃ according to the heating speed of 5 ℃/min, preserving heat for 30min, performing primary sintering, raising the temperature to 350 ℃ according to the heating speed of 9 ℃/min, preserving heat for 20min, performing secondary sintering, raising the temperature to 1100 ℃ according to the heating speed of 6 ℃/min, preserving heat for 20min, performing tertiary sintering, and then turning off a power supply to enable the quartz tube to be naturally cooled to room temperature along with a sintering furnace, and taking out the porous coated quartz tube. The coating morphology diagram of the porous coated quartz tube of the embodiment is shown in fig. 2.
Example 3
The embodiment provides a preparation method of a porous coating quartz tube, which comprises the following steps:
1. preparation of inorganic micropowder slurry
Raw materials are weighed according to the specification in table 3.1, and inorganic micro powder is obtained after uniform mixing for standby.
TABLE 3.1
Silica micropowder Alumina powder Talc powder Feldspar powder Broken glass
Weighing (g) 320 180 80 140 280
Raw material specification (mesh) 300 1000 1000 300 White glass fragments
Pouring the mixture of the inorganic micro powder into a stainless steel ball milling tank, sequentially adding 1.5kg of water and 5kg of stainless steel balls, ball milling for 8 hours at the rotating speed of 70r/min, taking out the slurry, and sieving with a 600-mesh sieve to obtain the inorganic micro powder slurry.
2. Preparation of the coating
Adding hydroxypropyl methylcellulose, silica sol, phosphoric acid solution and calcium carbonate into the inorganic micro powder slurry, and uniformly stirring by using an automatic stirrer to obtain the coating, wherein the addition amounts of various additives are shown in table 3.2.
TABLE 3.2
Carboxymethyl cellulose Aluminum dihydrogen phosphate Phosphoric acid solution Silicon carbide
Content of 99.9% 30% 35% 99.5%
Additive amount (g) 10 15 5 15
3. Preparation of porous coated quartz tube
And (3) atomizing and granulating 300ml of coating by using a high-pressure sprayer, uniformly spraying on the inner wall of a quartz tube, controlling the thickness of the coating to be 1.0mm after spraying, drying, sintering, raising the temperature to 140 ℃ according to the heating speed of 8 ℃/min, preserving heat for 30min, performing primary sintering, raising the temperature to 400 ℃ according to the heating speed of 10 ℃/min, preserving heat for 20min, performing secondary sintering, raising the temperature to 1200 ℃ according to the heating speed of 8 ℃/min, preserving heat for 20min, performing tertiary sintering, and then turning off a power supply to enable the quartz tube to be naturally cooled to room temperature along with a sintering furnace, and taking out the porous coated quartz tube. The coating morphology diagram of the porous coated quartz tube of the embodiment is shown in fig. 3.
Example 4
This example was conducted under the same conditions as in example 1 except that the thickness of the coating layer was controlled to be 0.6mm instead of 0.1 mm. The coating morphology diagram of the porous coated quartz tube of the embodiment is shown in fig. 4.
Example 5
This example was conducted under the same conditions as in example 1 except that the thickness of the coating layer was controlled to 0.6mm instead of 1.2 mm.
Example 6
In this example, the conditions were the same as in example 1 except that the sintering method was replaced with a temperature rise rate of 5℃per minute and the temperature was raised to 1180℃for 20 minutes. The coating morphology diagram of the porous coated quartz tube of the embodiment is shown in fig. 5.
Example 7
In this example, the conditions were the same as in example 1 except that the sintering method was replaced with a temperature rising rate of 8 ℃/min to 120 ℃, the temperature was maintained for 30min to perform the first-stage sintering, and then the temperature rising rate of 5 ℃/min to 1180 ℃ and the temperature was maintained for 20min to perform the second-stage sintering.
Example 8
In this example, the conditions were the same as in example 1 except that the content of the fine silica powder was replaced with 280g and the content of the alumina powder was replaced with 220 g. The coating morphology graph of the porous coating quartz tube prepared in the embodiment is shown in fig. 6.
Example 9
In this example, the conditions were the same as in example 1 except that the content of the fine silica powder was changed to 240g and the content of the alumina powder was changed to 260 g.
Example 10
In this example, the conditions were the same as in example 1 except that the content of the fine silica powder was changed to 360g and the content of the alumina powder was changed to 140 g. The coating morphology diagram of the porous coated quartz tube of the embodiment is shown in fig. 7.
Example 11
In this example, the conditions were the same as in example 1 except that the content of the fine silica powder was replaced with 400g and the content of the alumina powder was replaced with 100 g. The coating morphology diagram of the porous coated quartz tube of the embodiment is shown in fig. 8.
Comparative example 1
This comparative example was conducted under the same conditions as in example 1 except that calcium carbonate was not added in the preparation of the coating.
The coating morphology graph of the porous coated quartz tube of this comparative example is shown in fig. 9.
The porous coated quartz tubes prepared in comparative example 1 of examples 1 to 11 were subjected to appearance defect analysis, adhesion test, and coating heat shock (i.e., thermal shock test) test, and the test results are shown in table 3.
Wherein, the appearance defects of the coating are mainly compared with respect to the thickness and uniformity of the coating, the pore size and the like;
the coating adhesion test method is a scribing method, a craft knife is used for scribing 6 x 6 grids, after cutting and scribing, a brush is used for sweeping the surface to remove loose particles, then an adhesive tape is used for adhering to a test part, the test part is rubbed back and forth with fingers to firmly adhere, and then the test part is pulled up. The classification is then performed against:
level 0: completely smooth without any grid layering;
stage 1: the small blocks are stripped at the crossing part, and the influence area is 5%;
2 stages: stripping the edges of the crossing points, wherein the influence area is 5% -15%;
3 stages: peeling off along the whole edge, and partially or totally different lattices, wherein the influence area is 15% -35%;
4 stages: peeling off the whole strip along the edge, wherein some grids are partially or completely peeled off, and the influence area is 35% -65%;
5 stages: any different exfoliation levels graded according to 4;
the method for testing the thermal shock of the coating comprises the following steps: heating the porous coating quartz tube to 800 ℃, preserving heat for 20min, taking out, cooling at room temperature, repeating the operation for 5 times, and testing the peeling, cracking and layering defects of the coating.
TABLE 3 Table 3
The sample in example 1 was found to be optimal by the above table, and the object of the present invention was achieved.
As is clear from the comparison of examples 1 and examples 2-3, the inorganic micro-ingredient fluctuation and the auxiliary agent for coating preparation are different, and meanwhile, the spraying thickness is changed, so that the porous coating structure is influenced. Based on the technological parameters in the embodiment 1, a coating with performance, appearance and anti-corrosion function can be prepared;
as can be seen from the comparison of the examples 1 and 4-5, the coating is too thick, and the coating is unevenly stressed in the gas foaming expansion process to form bubble structures with different sizes. The spraying thickness is too thin, so that the spraying of part of the area cannot be achieved, blank appears, bubbles are volatilized directly into the air, and a bubble structure cannot be formed in the coating;
as is evident from a comparison of example 1 and examples 6-7, the generation of a porous structure of the coating after the sintering was replaced with the primary sintering or the secondary sintering has a great influence. Drying, adhesive discharging, curing and sintering foaming are indispensable.
As is evident from a comparison of example 1 and examples 8-11, the mass ratio of the silica fume to the alumina powder has a significant effect on the high temperature characteristics of the coating. SiO (SiO) 2 As the skeleton oxide of the glass, the high-temperature viscosity, crystallization performance, chemical stability and the like of the glass can be greatly improved. Alumina is used as intermediate oxide to increase the high temperature viscosity and reduce the material property of the glass, so as to change the high temperature property of the glass. The processes of bubble generation, diffusion, wrapping and the like are all related to the high-temperature performance of the coating. Thus, suitable silica to alumina ratios can have a significant impact on the porous structure. The example shows that the silicon-aluminum ratio is 310: about 180 a, the prepared porous coating is most ideal. And the coating structure can change with the up-and-down adjustment of the silicon-aluminum ratio.
The coating compositions of example 8 and example 10 were in the range of the mass ratio of the silica fume, alumina powder, talc powder, feldspar powder and cullet of the present invention of (24-40): (14-26): (5-10): (12-16): (25-35), and the coating compositions of example 8 and example 10 were also coating compositions satisfying the requirements of the present invention. The coating ratios of example 9 and example 11 were not in the range of the mass ratio of the silica fume, alumina powder, talc powder, feldspar powder and cullet of the present invention of (24-40): (14-26): (5-10): (12-16): (25-35), and the test performance of the coating was poor.
From the comparison of example 1 and comparative example 1, it is evident that the coating failed to develop a porous structure without the addition of a foaming agent during the coating preparation.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.

Claims (10)

1. The paint is characterized by comprising 90-110 parts of inorganic micro powder, 140-160 parts of water, 1-2 parts of thickener, 2.5-4 parts of high-temperature binder and 1.5-3 parts of foaming agent.
2. The coating of claim 1, wherein the inorganic fine powder comprises silica fine powder, alumina powder, talc powder, feldspar powder, and crushed glass;
preferably, the mass ratio of the silicon micro powder to the alumina powder to the talcum powder to the feldspar powder to the broken glass is (20-40), 14-26, 5-10, 12-16 and 25-35;
preferably, the thickener comprises any one or a combination of at least two of polyacrylamide, hydroxypropyl methylcellulose or carboxymethyl cellulose;
preferably, the high temperature binder comprises any one or a combination of at least two of silica sol, phosphoric acid solution or aluminum dihydrogen phosphate;
preferably, the foaming agent comprises any one or a combination of at least two of calcium carbide, sodium carbonate or silicon carbide.
3. A quartz tube, characterized in that the quartz tube comprises a quartz tube and a porous coating arranged on the inner wall of the quartz tube;
the raw materials of the porous coating layer comprise the coating material according to claim 1 or 2.
4. A quartz tube according to claim 3, wherein the porous coating has a thickness of 0.3 to 1.0mm;
preferably, the pore diameter of the porous coating is 0.3-1.0 mm.
5. A method of producing the quartz tube of claim 3 or 4, comprising:
dispersing the raw materials of the porous coating to obtain a coating, spraying the coating on the inner wall of a quartz tube, and drying and sintering to obtain the quartz tube;
the raw materials of the porous coating comprise inorganic micro powder, water, a thickening agent, a high-temperature binder and a foaming agent.
6. The method of producing the coating according to claim 5, wherein the method of producing the coating comprises: preparing the inorganic micro powder into inorganic micro powder slurry, and then dispersing the inorganic micro powder slurry with a thickening agent, a high-temperature binder and a foaming agent to obtain the coating;
preferably, the preparation method of the inorganic micro powder slurry comprises the following steps: ball milling the inorganic micro powder, grinding balls and water to obtain inorganic micro powder slurry;
preferably, the mass ratio of the inorganic micro powder to the grinding balls to the water is 1 (2-7) (1.2-1.7);
preferably, the ball milling time is 6-8 hours.
7. The method of claim 5 or 6, wherein the sprayed thickness is 0.3-1 mm;
preferably, the drying time is 2.5-3.5 hours;
preferably, the drying temperature is 10-35 ℃.
8. The production method according to any one of claims 5 to 7, wherein the sintering comprises a first-stage sintering, a second-stage sintering, and a third-stage sintering which are performed sequentially;
preferably, the temperature rising rate of the primary sintering is 5-8 ℃/min;
preferably, the temperature of the primary sintering is 100-140 ℃;
preferably, the heat preservation time of the sintering section is 25-35 mins;
preferably, the temperature rising rate of the two-stage sintering is 8-10 ℃/min;
preferably, the temperature of the two-stage sintering is 350-400 ℃;
preferably, the heat preservation time of the two-stage sintering is 15-25 mins;
preferably, the temperature rising rate of the three-stage sintering is 5-8 ℃/min;
preferably, the temperature of the three-stage sintering is 1100-1200 ℃;
preferably, the heat preservation time of the three-stage sintering is 15-25 mins;
preferably, the porous coating quartz tube is obtained by naturally cooling the sintered quartz tube to room temperature.
9. The preparation method according to any one of claims 5 to 8, characterized in that the preparation method comprises:
dispersing the raw materials of the porous coating to obtain a coating, and spraying the coating on the inner wall of a quartz tube, wherein the thickness of the coating is 0.3-1 mm;
the quartz tube is obtained through drying and sequentially performing primary sintering, secondary sintering and tertiary sintering, wherein the heating rate of the primary sintering is 5-8 ℃/min, the temperature is 100-140 ℃ and the heat preservation time is 25-35 mins, the heating rate of the secondary sintering is 8-10 ℃/min, the temperature is 350-400 ℃ and the heat preservation time is 15-25 mins, the heating rate of the tertiary sintering is 5-8 ℃/min, the temperature is 1100-1200 ℃ and the heat preservation time is 15-25 mins.
10. Use of the coating according to claim 1 or 2, characterized in that the coating is applied in the field of photovoltaic materials.
CN202310951437.2A 2023-07-31 2023-07-31 Coating, quartz tube containing same and application Pending CN116970294A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002076719A1 (en) * 2001-03-24 2002-10-03 Cheol-Hwan Cho Method for coating ceramic on quartz surface
CN103833232A (en) * 2014-01-07 2014-06-04 湖州东科电子石英有限公司 Manufacturing method of cristobalite crystal layer net high temperature-resistant quartz tube
CN104129970A (en) * 2014-08-18 2014-11-05 攀钢集团攀枝花钢铁研究院有限公司 Heat insulation coating for molten iron jar
CN107353039A (en) * 2017-05-27 2017-11-17 倪润琴 A kind of Alumina Foam Ceramics whitewashing material formula and its production technology
CN108641418A (en) * 2018-04-28 2018-10-12 郑州华晶金刚石股份有限公司 A method of composite coating slurry, preparation method containing nanometer carbon crystal and prepare composite coating using it
CN112890300A (en) * 2021-02-05 2021-06-04 东莞市中科智恒新材料有限公司 Far infrared quartz tube applied to low-temperature non-combustible electronic cigarette atomizer and preparation method thereof
CN113122124A (en) * 2021-04-06 2021-07-16 宋成镇 Expansion type flame-retardant heat-insulating fireproof coating and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002076719A1 (en) * 2001-03-24 2002-10-03 Cheol-Hwan Cho Method for coating ceramic on quartz surface
CN103833232A (en) * 2014-01-07 2014-06-04 湖州东科电子石英有限公司 Manufacturing method of cristobalite crystal layer net high temperature-resistant quartz tube
CN104129970A (en) * 2014-08-18 2014-11-05 攀钢集团攀枝花钢铁研究院有限公司 Heat insulation coating for molten iron jar
CN107353039A (en) * 2017-05-27 2017-11-17 倪润琴 A kind of Alumina Foam Ceramics whitewashing material formula and its production technology
CN108641418A (en) * 2018-04-28 2018-10-12 郑州华晶金刚石股份有限公司 A method of composite coating slurry, preparation method containing nanometer carbon crystal and prepare composite coating using it
CN112890300A (en) * 2021-02-05 2021-06-04 东莞市中科智恒新材料有限公司 Far infrared quartz tube applied to low-temperature non-combustible electronic cigarette atomizer and preparation method thereof
CN113122124A (en) * 2021-04-06 2021-07-16 宋成镇 Expansion type flame-retardant heat-insulating fireproof coating and preparation method thereof

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