CN113829471A - Heating ceramic tile with stable resistance and preparation method thereof - Google Patents

Heating ceramic tile with stable resistance and preparation method thereof Download PDF

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Publication number
CN113829471A
CN113829471A CN202111174161.9A CN202111174161A CN113829471A CN 113829471 A CN113829471 A CN 113829471A CN 202111174161 A CN202111174161 A CN 202111174161A CN 113829471 A CN113829471 A CN 113829471A
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China
Prior art keywords
ceramic tile
width
conductive
resistance
extrusion groove
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CN202111174161.9A
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Chinese (zh)
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CN113829471B (en
Inventor
苏伟劲
区邦熙
朱联烽
邓波
梁观列
李志豪
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Guangdong Jianyi Group Ceramics Co ltd
Qingyuan Jianyi Ceramics Co Ltd
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Guangdong Jianyi Group Ceramics Co ltd
Qingyuan Jianyi Ceramics Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B3/00Producing shaped articles from the material by using presses; Presses specially adapted therefor
    • B28B3/02Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein a ram exerts pressure on the material in a moulding space; Ram heads of special form
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B17/00Details of, or accessories for, apparatus for shaping the material; Auxiliary measures taken in connection with such shaping
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04FFINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F13/00Coverings or linings, e.g. for walls or ceilings
    • E04F13/07Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor
    • E04F13/08Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements
    • E04F13/0875Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements having a basic insulating layer and at least one covering layer
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04FFINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F15/00Flooring
    • E04F15/02Flooring or floor layers composed of a number of similar elements
    • E04F15/10Flooring or floor layers composed of a number of similar elements of other materials, e.g. fibrous or chipped materials, organic plastics, magnesite tiles, hardboard, or with a top layer of other materials
    • E04F15/107Flooring or floor layers composed of a number of similar elements of other materials, e.g. fibrous or chipped materials, organic plastics, magnesite tiles, hardboard, or with a top layer of other materials composed of several layers, e.g. sandwich panels
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04FFINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F15/00Flooring
    • E04F15/18Separately-laid insulating layers; Other additional insulating measures; Floating floors
    • E04F15/181Insulating layers integrally formed with the flooring or the flooring elements
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/02Details
    • H05B3/06Heater elements structurally combined with coupling elements or holders
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/10Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/20Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04FFINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F2290/00Specially adapted covering, lining or flooring elements not otherwise provided for
    • E04F2290/02Specially adapted covering, lining or flooring elements not otherwise provided for for accommodating service installations or utility lines, e.g. heating conduits, electrical lines, lighting devices or service outlets
    • E04F2290/023Specially adapted covering, lining or flooring elements not otherwise provided for for accommodating service installations or utility lines, e.g. heating conduits, electrical lines, lighting devices or service outlets for heating
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04FFINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F2290/00Specially adapted covering, lining or flooring elements not otherwise provided for
    • E04F2290/04Specially adapted covering, lining or flooring elements not otherwise provided for for insulation or surface protection, e.g. against noise, impact or fire

Abstract

The invention discloses a heating ceramic tile with stable resistance and a preparation method thereof, wherein the preparation method comprises the following steps: pressing and molding the ceramic tile blank on a mold, and sintering to obtain a ceramic substrate with an extrusion groove; detecting the width of the extrusion groove by a detector, if the width of the extrusion groove does not meet the rated width, coating a filling agent in the extrusion groove, and executing the next step after drying; printing conductive resistance slurry in the extrusion groove, preheating at the temperature of 180 ℃ and 200 ℃ for 30-35min, and curing at the temperature of 250 ℃ and 280 ℃ for 25-30 min; applying an insulating layer on the surface of the ceramic substrate; and pressing the heat insulation board and the ceramic substrate to obtain the heating ceramic tile with stable resistance. Through detecting the ceramic substrate after firing, detect out the extrusion recess that does not conform to the standard, inject the filler into the extrusion recess and make it keep rated size throughout, guarantee that the application volume change range of conductive resistance thick liquids is less when screen printing each time, the ceramic tile that generates heat has stable resistance, and the effect that generates heat is invariable.

Description

Heating ceramic tile with stable resistance and preparation method thereof
Technical Field
The invention relates to the technical field of heating ceramic tiles, in particular to a heating ceramic tile with stable resistance and a preparation method thereof.
Background
The heating tile is a functional tile which heats a tile body through an external heat source and transfers heat to an external environment in contact with the tile body, so that space heating is achieved. Current heating tiles generally consist of the following structure: ceramic tile base member layer, the material and the thermal insulation layer that generate heat of taking insulating encapsulation, the ceramic tile back is hugged closely on the layer that generates heat, and the heat direct transfer of production reaches the ceramic tile body, and the insulating layer has then ensured the security of ceramic tile in the circular telegram use, and thermal loss can be avoided to the heated board.
When preparing novel heating ceramic tile, consider the problem of cost and area that generates heat, studied out and printed resistance thick liquids in the recess, formed the resistance strip after the solidification to realize the scheme that the ceramic tile generates heat. However, in the above scheme, although the groove size of the die used in pressing can be kept consistent in actual production, the problem of inconsistent volume change after firing of tiles with different components or different proportions can exist, so that the sizes of the extrusion grooves formed after pressing are inconsistent, and the internal volumes of the extrusion grooves with different sizes are inconsistent, so that the width and thickness of the resistance paste for screen printing cannot be controlled within a certain range, the prepared heating tile resistor is unstable, and the heating effect cannot be kept within a constant range.
Disclosure of Invention
The invention mainly aims to provide a heating ceramic tile with stable resistance and a preparation method thereof, aiming at solving the technical problems that the width and thickness of the resistance paste printed by the heating ceramic tiles of different batches cannot be controlled within a set range and the resistance of the heating ceramic tile is unstable.
In order to achieve the purpose, the invention provides a preparation process of a heating ceramic tile with stable resistance, which comprises the following steps:
s1, pressing and forming a ceramic tile blank on a mold with a groove, and obtaining a ceramic substrate with an extrusion groove after sintering;
s2, detecting the width of the extrusion groove by a detector;
s21, if the difference value between the width of the extrusion groove and the rated width is larger than 0.4, sorting out the ceramic substrates, controlling the glue injection head to brush the filler on the side wall of the extrusion groove until the filler reaches the rated width by using the controller, and executing the step S3;
s22, if the difference between the width of the extrusion groove and the rated width is less than or equal to 0.4, executing a step S4;
s3, drying for the first time at 120-150 ℃ for 15-30min, drying for the second time at 280-325 ℃ for 10-30min, and executing step S4;
s4, printing conductive resistance slurry in the extrusion groove, preheating for 30-35min at the temperature of 180-200 ℃, and curing for 25-30min after preheating at the temperature of 250-280 ℃;
s5, applying an insulating layer on the surface of the ceramic substrate printed with the conductive resistance paste;
and S6, pressing the heat insulation plate and the ceramic substrate subjected to the step S5 to obtain the heating ceramic tile with the stable resistance.
Firstly, a plurality of parallel extrusion grooves with width are pressed on the back surface of the ceramic substrate when the ceramic substrate is pressed and formed through a mould, and then the ceramic substrate is fired according to the conventional manufacturing process of the ceramic tile. The ceramic substrate can shrink after being fired, the part of the ceramic substrate, which is not provided with the extrusion groove, can cause the extrusion groove to expand towards two sides due to the shrinkage, so that the extrusion groove is larger than the initial size, even the inside of part of the groove is slightly uneven, therefore, the scheme firstly detects the deformation degree of the extrusion groove through a detector, when the extrusion groove changes too much after being fired, namely the width is larger than the rated width, a controller controls an adhesive injection head to brush a filling agent towards the inside along the inner wall of the extrusion groove, the filling agent is directly coated on any inner wall or the bottom of the extrusion groove, the filling agent can be polytetrafluoroethylene, the heating efficiency can be improved while the heat insulation effect is achieved, the extrusion groove is filled to the rated width through the brushed filling agent, therefore, the extrusion groove of each batch can be ensured to be kept at the rated size, and as the extrusion groove is filled with conductive resistance slurry, therefore, the printing sizes of the conductive resistance paste of different batches are kept constant, so that the resistance of each batch is kept in a stable range, and the heating effect is stable; and after the filling is finished, drying twice to ensure a better curing effect of the filling agent. The printing length of the conductive resistance paste in the scheme is usually 300-1000mm, the change of about 0.4mm has small overall influence on the length, and the influence on the resistance can be ignored; the depth is not limited because the depth of the groove is larger than the printing thickness of the conductive resistance paste, and the change of the depth of about 0.4mm cannot influence the printing thickness, so that the resistance value cannot be influenced.
The detector can be a radar detector, an infrared detector or an ultrasonic detector, and can detect the distance and the interval below a millimeter level. The controller may be a PLC controller or the like.
After the conductive resistance paste is prepared, the conductive resistance paste is printed into the extrusion groove through screen printing, pre-sintering is carried out firstly, and then curing is carried out, so that the conductive electronic paste is ensured to be stably attached to the ceramic substrate, organic components in the conductive resistance paste are thoroughly volatilized, the resistance tends to be stable, and at the moment, the conductive resistance paste is cured to form the resistance heating strip. The setting of insulating layer can prevent conductive resistance thick liquids and external direct contact, avoids steam and other pollutants to cause the influence to the effect of generating heat of ceramic tile, sets up the polyurethane heated board at ceramic substrate bottommost layer again at last, makes the ceramic tile can maintain the effect of generating heat of a long time, and heated board and ceramic tile need pass through the pressfitting to guarantee firm the connection between them, obtain the ceramic tile that generates heat that has stable resistance after the pressfitting.
Preferably, in the step S2, the nominal width is 5-15 mm; the filler is polytetrafluoroethylene. When the rated width is limited in the range, the size of the conductive resistance paste can be ensured to be in a proper range, the resistance is small, the heating power is large, and the heating effect of the heating ceramic tile is optimal.
Preferably, the heat insulation plate is provided with sunken parts which correspond to the extrusion grooves one by one, and the depth of each sunken part is 0.2-0.4 mm. The arrangement of the concave part can improve the heat preservation effect of the heating ceramic tile. The one-to-one correspondence here means that the depressed part is just in the range of the vertical extension line of the extrusion groove, the heat of the heating ceramic tile is maximum in the region, and the depressed part arranged at the position can enable the heat preservation effect to be optimal.
Preferably, in the step S2, preparing the conductive resistance paste includes the following steps: s21, putting 2.0-5.0% of graphene, 1.0-3.0% of carbon black, 2.0-5.0% of nickel, 0.2-1.2% of dispersing agent, 0.3-1.6% of binder, 0.4-1.3% of auxiliary agent and 85-95% of water in a ball milling device in sequence according to weight percentage, and performing ball milling dispersion for 100 plus materials for 150min to obtain the conductive resistance slurry.
The conductive resistance paste in the scheme mainly comprises graphene, carbon black and nickel, and plays a role in conducting electricity, the addition of water is used as a solvent to facilitate the dispersion of each component, in addition, a dispersing agent is additionally added into the conductive resistance paste to further promote the uniform dispersion of each component, the addition of a binder is used for ensuring that the conductive resistance paste is stably bonded on a ceramic substrate, the raw materials are sequentially placed into a planetary ball milling tank for ball milling and dispersing for 100-150min, and the conductive resistance paste with uniform liquid quality can be obtained and can be subjected to screen printing.
Preferably, the dispersant is at least one of polyethylene glycol, sodium polycarboxylate, polyacrylamide or glyceryl monostearate; the adhesive is titanate, the auxiliary agent is a silane coupling agent with the types of KH-550, KH-792, KH-570 and Si-69.
Preferably, the step S4 is followed by the following steps: s42, printing conductive silver paste layers at two ends of the cured conductive resistance paste, curing at the temperature of 280-300 ℃ and cooling to normal temperature, covering a conductive copper foil electrode above the conductive silver paste layers, and electrically connecting the conductive copper foil electrode with an external power supply. The conductive resistance paste, the conductive silver paste layer and the conductive copper foil electrode are combined to realize conductivity, and the heating effect is stable. The conductive copper foil electrode is electrically connected with the wiring terminal and fixed in a tin soldering mode, and the wiring terminal is electrically connected with an external power supply.
Preferably, the width of the conductive silver paste layer is 1-10mm, and the width of the conductive copper foil electrode is 10-30 mm. The heating is uniform, and the effect is better.
Preferably, in step S5, the step of applying the insulating layer on the surface of the ceramic substrate printed with the conductive resistance paste includes the steps of: s51, covering glass fiber mesh cloth on the surface of the ceramic substrate printed with the conductive resistance paste, coating epoxy resin to enable the glass fiber mesh cloth to be soaked in the epoxy resin, and curing at the temperature of 120-150 ℃ for 25-40min to obtain the insulating layer.
The back of the ceramic substrate layer after the step S23 is covered by glass fiber mesh cloth with the thickness of 1-2mm, the glass fiber mesh cloth is mainly alkali-resistant glass fiber mesh cloth, the glass fiber mesh cloth is formed by twisting medium-alkali-free glass fiber yarns (the main component is silicate and has good chemical stability) through a special tissue structure-leno tissue, the glass fiber mesh cloth is subjected to high-temperature heat setting treatment such as alkali resistance and reinforcing agent, the size and specification of the glass fiber mesh cloth are consistent with those of a ceramic substrate layer, a conductive back bolt screw is exposed and leaked, a wiring terminal is sleeved on the back bolt screw, the whole structure on the wiring terminal and the conductive back bolt screw is completely wrapped by a plastic rubber sleeve and encapsulated by epoxy resin, and the ceramic tile circuit is more stable and waterproof, and the heating ceramic tile circuit is effectively connected, and the situations of line breakage, electric leakage or poor contact can not be caused. And then coating insulating epoxy resin on the position covered by the glass fiber mesh cloth to ensure that the glass fiber mesh cloth is completely wetted and impregnated, and curing for 25-40min at 120-150 ℃ to obtain the insulating layer.
Preferably, after the step S5, the method further includes the following steps:
s52, pasting aluminum foil glass fiber cloth on the insulating layer, and electrically connecting the ground wire with an aluminum foil layer of the aluminum foil glass fiber cloth to obtain a ground layer;
s53, covering 1-2mm of glass fiber mesh cloth on the grounding layer, and coating epoxy resin to obtain a protective layer;
s54, coating epoxy resin on the protective layer, and then pasting aluminum foil glass fiber cloth to obtain the sealing layer.
The aluminum foil glass fiber cloth is a compact film formed by using glass fibers as basic raw materials and laminating and bonding the aluminum foil with the aluminum foil, the surface of one side where the aluminum foil is compounded is smooth, the aluminum foil layer of the aluminum foil glass fiber cloth faces upwards (the side close to the insulating layer) and the glass fiber layer faces downwards, then the ground wire is connected with the aluminum foil layer to obtain a ground layer, and the ground wire can be detected in a conducting state. And a protective layer is required to be arranged on the grounding layer to prevent electric leakage, the grounding layer is continuously covered by glass fiber gridding cloth with the thickness of 1-2mm, and the position covered by the glass fiber gridding cloth is coated with insulating potting resin to obtain the protective layer. After the protective layer is obtained, priming with epoxy insulating resin, and then attaching aluminum foil glass fiber cloth, wherein the aluminum foil layer faces upwards (the side close to the protective layer) and the glass fiber layer faces downwards to obtain a sealing layer; then, sticking a polyurethane insulation board by using ceramic tile glue, wherein the polyurethane insulation board is provided with concave parts which correspond to the extrusion grooves one by one; the ceramic substrate and the polyurethane insulation board after being attached are arranged on the pressing frame and pressed under the pressure of 2 tons, so that the insulation board is tightly combined with the ceramic substrate, and in other embodiments, the pressure of pressing can be 1 ton, 3 tons or 4 tons and the like. And pressing to obtain the heating ceramic tile with the stable resistance, and cleaning and decontaminating the front and back sides of the heating ceramic tile with the stable resistance to obtain a finished product.
The invention also provides a heating ceramic tile which is prepared by the preparation method of the heating ceramic tile with the stable resistance. Referring to the above embodiments, since the heating tile adopts all technical solutions of all the above embodiments, at least all effects brought by the technical solutions of the above embodiments are achieved, and no further description is given here.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1. the conductive resistance paste is printed in the extrusion groove on the back of the ceramic tile base body and is solidified as a heating source, the heating layer is in direct contact with the ceramic tile base body, and no thick film or insulating rubber layer is arranged in the middle of the heating layer, so that the heat transfer efficiency is high, the consumption of the heating resistance paste is low, and the cost is low. The size of detector real-time detection extrusion recess, width promptly, when the width of extrusion recess and rated width's difference were too big, with the filler with inside packing of too big extrusion recess to unanimous with rated width, guarantee that the inside volume of each batch of extrusion recess is unanimous to the printing size of conductive resistance thick liquids can keep invariable, resistance also can keep in invariable within range, the effect of generating heat of the ceramic tile is comparatively stable.
2. The glass fiber mesh cloth and epoxy resin are filled and sealed to serve as an insulating layer, the glass fiber mesh cloth soaked by the resin is tightly attached to the conductive resistance slurry, the insulating layer with good sealing performance is formed after the resin is cured, and the insulating layer has a certain heat preservation effect while insulating. The polyurethane insulation board with the depressed part is adopted, the depressed part is particularly arranged on the insulation board and corresponds to the extrusion grooves of the ceramic substrate one to one, an air layer is further separated between the region where the depressed part of the insulation board is located and the next layer, and the heat conductivity of air is small, so that the heat loss is reduced, and the insulation effect of the insulation board is further enhanced.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other related drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural view of a heating tile with stable resistance provided herein;
FIG. 2 is a schematic cross-sectional view of a heating tile with stable resistance provided herein;
fig. 3 is a schematic structural diagram of the insulation board provided by the present application.
In the drawings: 1-ceramic substrate, 11-extrusion groove, 2-conductive resistance paste, 21-conductive silver paste layer, 22-conductive copper foil electrode, 3-insulating layer, 4-insulation board, 41-recess, 5-grounding layer, 6-protective layer and 7-sealing layer.
The implementation, functional features and advantages of the objectives of the present application will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
A preparation method of a heating ceramic tile with stable resistance comprises the following steps:
s1, pressing and forming a ceramic tile blank on a mold with a groove, and obtaining a ceramic substrate 1 with an extrusion groove 11 after sintering;
s2, detecting the width of the extrusion groove 11 by a detector;
s21, if the difference value between the width of the extrusion groove 11 and the rated width is larger than 0.4, sorting out the ceramic substrates 1, controlling a glue injection head (not shown in the figure) to paint a filler on the side wall of the extrusion groove 11 by a controller (not shown in the figure) until the filler reaches the rated width, and executing step S3;
s22, if the difference between the width of the extrusion groove 11 and the rated width is less than or equal to 0.4, executing a step S4; the rated width is 5-15 mm;
s3, drying for the first time at 120-150 ℃ for 15-30min, drying for the second time at 280-325 ℃ for 10-30min, and executing step S4;
s4, printing the conductive resistance paste 2 in the extrusion groove 11, preheating for 30-35min at the preheating temperature of 180-200 ℃, and curing for 25-30min after preheating at the curing temperature of 250-280 ℃; printing conductive silver paste layers 21 at two ends of the cured conductive resistance paste 2, curing and cooling to normal temperature at the temperature of 280-300 ℃, covering conductive copper foil electrodes 22 above the conductive silver paste layers 21, wherein the conductive copper foil electrodes 22 are electrically connected with an external power supply, the width of the conductive silver paste layers 21 is 1-10mm, and the width of the conductive copper foil electrodes 22 is 10-30 mm;
the preparation of the conductive resistance paste 2 comprises the following steps: s41, sequentially putting 2.0-5.0% of graphene, 1.0-3.0% of carbon black, 2.0-5.0% of nickel, 0.2-1.2% of dispersing agent, 0.3-1.6% of binder, 0.4-1.3% of auxiliary agent and 85-95% of water into ball milling equipment according to weight percentage, and performing ball milling dispersion for 100 plus materials for 150min to obtain conductive resistance slurry 2;
the dispersing agent is at least one of polyethylene glycol, sodium polycarboxylate, polyacrylamide or glyceryl monostearate; the adhesive is titanate, the auxiliary agent is a silane coupling agent, and the following types are adopted specifically: KH-550, KH-792, KH-570, Si-69;
s51, covering glass fiber mesh cloth on the surface of the ceramic substrate 1 printed with the conductive resistance paste 2, coating epoxy resin to immerse the glass fiber mesh cloth in the epoxy resin, and curing at the temperature of 120-150 ℃ for 25-40min to obtain an insulating layer;
s52, pasting aluminum foil glass fiber cloth on the insulating layer, and electrically connecting the ground wire with an aluminum foil layer of the aluminum foil glass fiber cloth to obtain a ground layer 5;
s53, covering 1-2mm of glass fiber mesh cloth on the grounding layer 5, and coating epoxy resin to obtain a protective layer 6;
s54, coating epoxy resin on the protective layer 6, and then pasting aluminum foil glass fiber cloth to obtain a sealing layer 7;
s6, pressing the heat insulation board 4 and the ceramic substrate 1 subjected to the step S54 to obtain the heating ceramic tile with the stable resistance; the heat insulation plate is provided with concave parts 41 which are in one-to-one correspondence with the extrusion grooves 11, and the depth of each concave part 41 is 0.2-0.4 mm.
The technical solutions of the present invention are further described in detail with reference to the following specific examples, which should be understood as merely illustrative and not limitative.
Example 1
A preparation method of a heating ceramic tile with stable resistance comprises the following steps:
s1, pressing and forming a ceramic tile blank on a mold with a groove, and obtaining a ceramic substrate 1 with an extrusion groove 1111 after sintering;
s2, detecting the width of the extrusion groove 11 by a detector, wherein the difference value between the width (12.6mm) of the extrusion groove 11 and the rated width (12mm) is 0.6 mm; sorting out the ceramic substrates 1, controlling the glue injection head to brush the filler on the side wall of the extrusion groove 11 by the controller until the filler reaches the rated width, and executing the step S3;
s3, drying for the first time at 120 ℃ for 30min, drying for the second time at 300 ℃ for 30min, and executing the step S4;
s4, printing the conductive resistance paste 2 in the extrusion groove 11, preheating for 34min at 185 ℃, and curing for 28min after preheating at 270 ℃; printing conductive silver paste layers 21 at two ends of the cured conductive resistance paste 2, curing at 300 ℃ and cooling to normal temperature, covering conductive copper foil electrodes 22 on the conductive silver paste layers 21, wherein the conductive copper foil electrodes 22 are electrically connected with an external power supply, the width of the conductive silver paste layers 21 is 8.5mm, and the width of the conductive copper foil electrodes 22 is 22 mm;
the preparation of the conductive resistance paste 2 comprises the following steps: s41, sequentially putting 3% of graphene, 1% of carbon black, 4% of nickel, 0.8% of sodium polycarboxylate dispersant, 1.2% of KH-550 binder and 90% of water in a ball milling device according to weight percentage, and performing ball milling dispersion for 135min to obtain conductive resistance slurry 2;
s51, covering glass fiber mesh cloth on the surface of the ceramic substrate 1 printed with the conductive resistance paste 2, coating epoxy resin to immerse the glass fiber mesh cloth in the epoxy resin, and curing at 140 ℃ for 30min to obtain an insulating layer 3;
s52, pasting aluminum foil glass fiber cloth on the insulating layer 3, and electrically connecting the ground wire with an aluminum foil layer of the aluminum foil glass fiber cloth to obtain a ground layer 5;
s53, covering 2mm of glass fiber mesh cloth on the grounding layer 5, and coating epoxy resin to obtain a protective layer 6;
s54, coating epoxy resin on the protective layer 6, and then pasting aluminum foil glass fiber cloth to obtain a sealing layer 7;
s6, pressing the heat insulation board 4 and the ceramic substrate 1 subjected to the step S54 to obtain the heating ceramic tile with the stable resistance; the heat insulation plate 4 is provided with concave parts 41 corresponding to the extrusion grooves 11 one by one, and the depth of each concave part 41 is 0.4 mm.
Comparative example 1
The comparative example has the same parameters as example 1 except that: the steps S2-S3 are not performed, that is, the steps of detecting and applying the filler are not performed, and the width of the pressing groove 11 is 12.6 mm.
Example 2
The parameters of this embodiment are consistent with those of embodiment 1, and the differences are only that:
s2, detecting the width of the extrusion groove 11 by a detector, wherein the difference value between the width (12.2mm) of the extrusion groove 11 and the rated width (12mm) is 0.2mm, and executing the step S4;
examples 1-2 and comparative example 1 were subjected to performance tests, the results of which are given in the following table:
table 1 results of performance testing
Detecting items Resistance/omega
Example 1 1005
Example 2 984
Comparative example 1 957
As can be seen from the test results in table 1, the heating tile with stable resistance of the present invention has stable resistance, and when the dimensional parameters of the extrusion grooves are adjusted within the limited range, the resistance value does not change excessively.
Example 3
A preparation method of a heating ceramic tile with stable resistance comprises the following steps:
s1, pressing and forming a ceramic tile blank on a mold with a groove, and obtaining a ceramic substrate 1 with an extrusion groove 11 after sintering;
s2, detecting the width of the extrusion groove 11 by a detector, wherein the difference value between the width (12.5mm) of the extrusion groove 11 and the rated width (12mm) is 0.5 mm; sorting out the ceramic substrates 1, controlling the glue injection head to brush the filler on the side wall of the extrusion groove 11 by the controller until the filler reaches the rated width, and executing the step S3;
s3, drying for the first time at 130 ℃ for 25min, drying for the second time at 310 ℃ for 25min, and executing the step S4;
s4, printing conductive resistance paste 2 in the extrusion groove 11, preheating for 33min at 200 ℃, and curing for 25min after preheating at 260 ℃; printing conductive silver paste layers 21 at two ends of the cured conductive resistance paste 2, curing at 280 ℃ and cooling to normal temperature, covering conductive copper foil electrodes 22 on the conductive silver paste layers 21, wherein the conductive copper foil electrodes 22 are electrically connected with an external power supply, the width of the conductive silver paste layers 21 is 3mm, and the width of the conductive copper foil electrodes 22 is 30 mm;
the preparation of the conductive resistance paste 2 comprises the following steps: s41, sequentially putting 2% of graphene, 3% of carbon black, 5% of nickel, 1% of sodium polycarboxylate dispersant, 1% of KH-550 binder and 88% of water into ball milling equipment according to weight percentage, and performing ball milling dispersion for 150min to obtain conductive resistance slurry 2;
s51, covering glass fiber mesh cloth on the surface of the ceramic substrate 1 printed with the conductive resistance paste 2, coating epoxy resin to immerse the glass fiber mesh cloth in the epoxy resin, and curing at 120 ℃ for 30min to obtain an insulating layer 3;
s52, pasting aluminum foil glass fiber cloth on the insulating layer 3, and electrically connecting the ground wire with an aluminum foil layer of the aluminum foil glass fiber cloth to obtain a ground layer 5;
s53, covering 1mm of glass fiber mesh cloth on the grounding layer 5, and coating epoxy resin to obtain a protective layer 6;
s54, coating epoxy resin on the protective layer 6, and then pasting aluminum foil glass fiber cloth to obtain a sealing layer 7;
s6, pressing the heat insulation board 4 and the ceramic substrate 1 subjected to the step S54 to obtain the heating ceramic tile with the stable resistance; the heat insulation board 4 is provided with the concave parts 41 which are in one-to-one correspondence with the extrusion grooves 11, and after the heat insulation board 4 is pressed with the ceramic substrate 1, gaps with the height of 0.3mm are formed between the concave parts 41 and the extrusion grooves 11.
Example 4
The parameters of this example are consistent with those of example 3, and the difference is only that:
s2, detecting the width of the extrusion groove 11 by using a detector, wherein the difference value between the width (12.15mm) of the extrusion groove 11 and the rated width (12mm) is 0.15 mm; step S4 is executed.
Comparative example 2
The comparative example has the same parameters as example 3 except that: the heat insulating plate 4 is not provided with the recess 41.
Examples 3-4 and comparative example 2 were tested for performance and the results are given in the following table:
table 2 results of performance testing
Detecting items Resistance/omega Holding time/min
Example 3 922 32
Example 4 914 /
Comparative example 2 / 25
The detection of the heat preservation time is to connect all the prepared tiles with a power supply and continuously heat for 40min, and then detect the time required for the tiles to naturally cool to the normal temperature (25 ℃) in the closed space.
As can be seen from the test results in table 2, the heating tile with stable resistance of the present invention has stable resistance, and the resistance value does not change too much when other parameters are adjusted. In addition, this ceramic tile that generates heat still has comparatively excellent heat preservation effect.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the present specification and directly/indirectly applied to other related technical fields within the spirit of the present invention are included in the scope of the present invention.

Claims (10)

1. A preparation process of a heating ceramic tile with stable resistance is characterized by comprising the following steps:
s1, pressing and forming a ceramic tile blank on a mold with a groove, and obtaining a ceramic substrate (1) with an extrusion groove (11) after sintering;
s2, detecting the width of the extrusion groove (11) by a detector;
s21, if the difference value between the width of the extrusion groove (11) and the rated width is larger than 0.4, sorting out the ceramic substrate (1), controlling the glue injection head to brush the filler on the side wall of the extrusion groove (11) until the filler reaches the rated width by using the controller, and executing the step S3;
s22, if the difference value between the width of the extrusion groove (11) and the rated width is less than or equal to 0.4, executing a step S4;
s3, drying for the first time at 120-150 ℃ for 15-30min, drying for the second time at 280-325 ℃ for 10-30min, and executing step S4;
s4, printing the conductive resistance paste (2) in the extrusion groove (11), preheating for 30-35min at the preheating temperature of 180-200 ℃, and curing for 25-30min after preheating at the curing temperature of 250-280 ℃;
s5, applying an insulating layer (3) on the surface of the ceramic substrate (1) printed with the conductive resistance paste (2);
and S6, pressing the heat insulation plate (4) and the ceramic substrate (1) subjected to the step S5 to obtain the heating ceramic tile with the stable resistance.
2. A process for producing a heat-generating ceramic tile having stabilized electric resistance according to claim 1, wherein in said step S2, the rated width is 5-15 mm; the filler is polytetrafluoroethylene.
3. A process for preparing a heat-generating ceramic tile with stabilized electrical resistance as claimed in claim 1, wherein: the heat insulation plate (4) is provided with sunken parts (41) which correspond to the extrusion grooves (11) one by one, and the depth of each sunken part is 0.2-0.4 mm.
4. The process for preparing a heat-generating ceramic tile with stabilized electric resistance according to claim 1, wherein in the step S4, the preparation of the conductive resistance paste (2) comprises the steps of:
s41, sequentially putting 2-5% of graphene, 1-3% of carbon black, 2-5% of nickel, 0.2-1.2% of dispersing agent, 0.3-1.6% of binder, 0.4-1.3% of auxiliary agent and 85-95% of water into ball milling equipment according to weight percentage, and performing ball milling dispersion for 100-150min to obtain the conductive resistance slurry (2).
5. The process for preparing a heat-generating ceramic tile having stable electric resistance as claimed in claim 4, wherein the dispersant is at least one of polyethylene glycol, sodium polycarboxylate, polyacrylamide or glyceryl monostearate;
the adhesive is titanate, and the auxiliary agent is a silane coupling agent.
6. A process for preparing a heating ceramic tile with stable resistance according to claim 1, wherein said step S4 is followed by the following steps:
s42, printing conductive silver paste layers (21) at two ends of the cured conductive resistance paste (2), curing and cooling to normal temperature at the temperature of 280-300 ℃, covering conductive copper foil electrodes (22) above the conductive silver paste layers (21), and electrically connecting the conductive copper foil electrodes (22) with an external power supply.
7. The process for preparing a heat-generating ceramic tile with stable resistance according to claim 6, wherein the width of the conductive silver paste layer (21) is 1-10mm, and the width of the conductive copper foil electrode (22) is 10-30 mm.
8. The process for preparing a heat-generating ceramic tile with stable resistance according to claim 6, wherein in step S5, the step of applying the insulating layer (3) on the surface of the ceramic substrate (1) printed with the conductive resistance paste (2) comprises the steps of:
s51, covering glass fiber mesh cloth on the surface of the ceramic substrate (1) printed with the conductive resistance slurry (2), coating epoxy resin to enable the glass fiber mesh cloth to be soaked in the epoxy resin, and curing at the temperature of 120-150 ℃ for 25-40min to obtain the insulating layer (3).
9. A process for preparing a heating ceramic tile with stable resistance according to claim 6, wherein after the step S5, the process further comprises the following steps:
s52, pasting aluminum foil glass fiber cloth on the surface of the insulating layer (3), and electrically connecting the ground wire with an aluminum foil layer of the aluminum foil glass fiber cloth to obtain a ground layer (5);
s53, covering 1-2mm of glass fiber mesh cloth on the surface of the grounding layer (5), and coating epoxy resin to obtain a protective layer (6);
s54, coating epoxy resin on the surface of the protective layer (6), and then attaching aluminum foil glass fiber cloth to obtain the sealing layer (7).
10. A heat-generating ceramic tile characterized by being produced by the method for producing a heat-generating ceramic tile having a stable electric resistance according to any one of claims 1 to 9.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102108779A (en) * 2009-12-25 2011-06-29 李增清 Electric heating terrestrial heat floor board
US20120094083A1 (en) * 2010-10-18 2012-04-19 Nitto Denko Corporation Light emissive ceramic laminate and method of making same
CN106313287A (en) * 2016-11-03 2017-01-11 景德镇全球亮科技有限公司 Multifunctional ceramic tile and manufacturing method thereof
CN110056163A (en) * 2019-05-29 2019-07-26 上海热丽科技集团有限公司 A kind of spontaneous heating ceramic tile, preparation process and its method for paving
CN112477313A (en) * 2020-12-11 2021-03-12 广东康烯科技有限公司 Porous titanium carbide MXene/reduced graphene oxide base heating brick

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102108779A (en) * 2009-12-25 2011-06-29 李增清 Electric heating terrestrial heat floor board
US20120094083A1 (en) * 2010-10-18 2012-04-19 Nitto Denko Corporation Light emissive ceramic laminate and method of making same
CN106313287A (en) * 2016-11-03 2017-01-11 景德镇全球亮科技有限公司 Multifunctional ceramic tile and manufacturing method thereof
CN110056163A (en) * 2019-05-29 2019-07-26 上海热丽科技集团有限公司 A kind of spontaneous heating ceramic tile, preparation process and its method for paving
CN112477313A (en) * 2020-12-11 2021-03-12 广东康烯科技有限公司 Porous titanium carbide MXene/reduced graphene oxide base heating brick

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