CN103476155A - Mica heating substrate coated with inorganic thick film, preparing method therefore and heating assembly - Google Patents

Mica heating substrate coated with inorganic thick film, preparing method therefore and heating assembly Download PDF

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CN103476155A
CN103476155A CN201310418175XA CN201310418175A CN103476155A CN 103476155 A CN103476155 A CN 103476155A CN 201310418175X A CN201310418175X A CN 201310418175XA CN 201310418175 A CN201310418175 A CN 201310418175A CN 103476155 A CN103476155 A CN 103476155A
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thick film
mica
inorganic thick
substrate carrier
base plate
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CN103476155B (en
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李琴
简伟雄
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Abstract

The invention provides a mica heating substrate coated with an inorganic thick film. The mica heating substrate comprises a mica substrate carrier, the face-type inorganic thick film, electrodes, wire leading ends and a mica cover plate, wherein the face-type inorganic thick film is arranged on the first surface of the mica substrate carrier in a high-temperature sintering mode, the electrodes enable the inorganic thick film to be connected into a circuit, the wire leading ends are used for being connected with power source lead wires, and the mica cover plate is attached to the mica substrate carrier to cover the inorganic thick film, the electrodes and the wire leading ends. The inorganic thick film comprises graphite powder, bismuth oxide, boric oxide, silicon dioxide, antimonous oxide, zinc oxide, strontium carbonate and the like. The mica heating substrate which is healthy and environmentally friendly is obtained, short circuits, ignition and the excessively high oxidation speed of an electric heating wire are prevented from being caused by the excessively large partial expansion coefficient of mica, and the defects that a rubber layer of a traditional mica heating substrate is prone to aging, blistering and layering are partially generated, the resistance is damped, and the temperature is uneven are overcome. The invention further provides a preparing method of the mica heating substrate and a mica heating assembly with the mica heating substrate.

Description

Scribble mica heating base plate and preparation method thereof and the heat generating component of inorganic thick film
Technical field
The invention belongs to the electric heating field of new, relate in particular to a kind of mica heating base plate that scribbles inorganic thick film and preparation method thereof and heat generating component.
Background technology
Mica heating plate is traditional electrical heating elements, it adopts conventional board production technique, alloy sheet is arranged or be wound around heating wire or ribbon heater on mica substrate at the micarex back etched, the mica heating plate that also to have the transparent electric heating film preparation be thermal source at the first-class composite construction of mica substrate, its product defects is used the harmful substances such as strong acid in a large number due to needs while being to produce (etch process), there are the three wastes to produce, harmful serious with environmental pollution.During product work, because product is " linearity " thermal source heating arrangement, the unit cross-sectional area power density is large, surface temperature is high, and the differential expansion coefficient is large, yielding, sound is arranged during work, in the place that is prepared with line with heating function, temperature is very high, causes mica differential expansion coefficient excessive and produce the abnormal conditions such as heating wire short circuit, sparking, too fast oxidation and occur; The glue that is used for combined mica due to product is that organic material is made, and peculiar smell is arranged during work and discharge a large amount of gas and be harmful to smog to produce; Because product is composite construction, the easy aging layering of long term high temperature intermediate rubber adhesion coating, cause the aging layering of mica carrier and heater and produce the air thermal resistance and cause fire, the aging of product too fast.
The micarex of current commercially available transparent electric heating film production, because monolithic product area is large, the product square resistance is inhomogeneous, poor repeatability, therefore the single chip architecture technical target of the product can't be realized.The existing product structure is the multi-disc splicing structure, but each piece resistance is different again, and causes the product surface non-uniform temperature, after the work certain hour, and product gross power 20% left and right of decaying, this product is eliminated gradually.
Above-mentioned series technique is with respect to today of scientific and technological high development, and the continuous pursuit of people to healthy and environmental protection is obviously inapplicable.
Summary of the invention
The purpose of the embodiment of the present invention is to provide a kind of heating base plate of the mica with inorganic thick film, is intended to solve the defect existed in prior art, obtains the mica heating base plate of a kind of health and environmental protection.
The embodiment of the present invention is to realize like this, a kind of mica heating base plate that scribbles inorganic thick film, it comprises the mica substrate carrier, described mica substrate carrier has first surface and the second surface relative with described first surface, the described mica heating base plate that scribbles inorganic thick film also comprises the planar inorganic thick film of high temperature sintering on the first surface of described mica substrate carrier, the electrode that described inorganic thick film is connected in circuit reaches the lead ends for connecting power supply lead wire and is affixed on described mica substrate carrier to cover described inorganic thick film, the mica emulsion sheet of described electrode and described lead ends, described lead ends and described electrode are electrically connected, described electrode and described inorganic thick film are electrically connected, described inorganic thick film high temperature sintering is on described mica substrate carrier, described inorganic thick film, the component that comprises following weight fraction:
Figure BDA0000381833280000021
Further, the weight fraction of described bismuth oxide is 70-75 part.
Another order of the embodiment of the present invention is to provide a kind of above-mentioned preparation method who scribbles the mica heating base plate of inorganic thick film, and it comprises the steps:
S1) provide the mica substrate carrier;
S2) print successively described electrode, described lead ends and described inorganic thick film on the described first surface of described mica substrate carrier, and described lead ends and described electrode are electrically connected, described inorganic thick film and described electrode are electrically connected;
S3) the mica substrate carrier that is printed with described electrode, described lead ends and described inorganic thick film is carried out to sintering processes;
S4) described mica emulsion sheet is affixed on described mica substrate carrier to cover described inorganic thick film, described electrode and described lead ends.
Further, in step S2) in, also comprising the step a) for preparing described inorganic thick film, it comprises the steps:
Described graphite powder, bismuth oxide, boron oxide, silicon dioxide, antimonous oxide, zinc oxide and strontium carbonate are provided by weight ratio;
By described bismuth oxide, boron oxide, silicon dioxide, antimonous oxide, zinc oxide and strontium carbonate heating and melting, fused mass is ground to below 350 orders after cooling, add described graphite powder to mix, obtain the first mixture;
Described the first mixture is mixed for 65-80: 20-35 by weight with organic carrier, obtain the second mixture;
Described the second mixture is coated on described mica substrate carrier and obtained inorganic thick film.
Further, the weight fraction of the bismuth oxide of described inorganic thick film is 70-75 part.
Further, the temperature of described bismuth oxide, described boron oxide, described silicon dioxide, described antimonous oxide, described zinc oxide and described strontium carbonate heating and melting is 900-1200 ℃.
Further, in step S3) in, the temperature of described sintering is 400-700 ℃.
Further, described organic carrier comprises the component of following percentage by weight:
Terpinol 85-95%
Ethyl cellulose 5-15%.
Further, also comprise step S5), wherein another mica emulsion sheet is affixed on the described second surface of described mica substrate carrier.
A purpose again of the embodiment of the present invention is to provide a kind of heat generating component, it comprises the above-mentioned mica heating base plate that scribbles inorganic thick film, be affixed on another mica emulsion sheet on the described second surface of described mica substrate carrier, be located in described mica substrate carrier surrounding the metal hemming edge bar and be connected in thermostat and the fuse on described power supply lead wire.
The mica heating base plate that scribbles inorganic thick film of the embodiment of the present invention, preparation method reach and heat generating component at least has following advantage:
1, inorganic thick film is not due to leaded, and material is environmental protection not only, and is rich in far infrared, reduced environmental pollution, useful health, overcome product and due to needs, use in a large number the harmful substance such as strong acid to produce the three wastes, the harmful and serious defect of environmental pollution.
2, the material granule degree of inorganic thick film is meticulousr, and the resistance dispersion is little, and the material sheet resistance is reproducible, and conforming product rate is high, has saved the energy, has lowered production cost, has improved quality and the precision of product, has promoted product competitiveness in the market.
3, the inorganic thick film of the present invention's application, by using bismuth oxide as framework material, be used in conjunction with again the components such as boron oxide, silicon dioxide, zinc oxide, antimonous oxide and strontium carbonate, both realized the performance of inorganic thick film, simultaneously, realize zero content of lead oxide with respect to existing inorganic thick film, prevented people's lead poisoning and to the pollution of environment when the use inorganic thick film; And, due to the use of bismuth oxide, the serviceability temperature of inorganic thick film is improved greatly, enlarged the scope of application of inorganic thick film.
4, the inorganic thick film of mica heating base plate of the present invention is " planar " heater, its heating area is the several times of traditional product " linearity " heater area, reduced the unit power density of heater, reduced the coefficient of expansion of mica part, thereby while having avoided product work because product is " linearity " thermal source heating arrangement, the unit cross-sectional area power density is large, surface temperature is high, the differential expansion coefficient is large, yielding, sound is arranged during work, very high and cause excessive the brought heating wire short circuit of mica differential expansion coefficient at the local Yin Wendu that is prepared with line with heating function, sparking, the problems such as too fast oxidation,
5, the inorganic thick film of mica heating base plate of the present invention adopts silk-screen printing technique and imposes high-sintering process, and heater and mica substrate carrier are forever made to integral structure, there are not stratified, non-foaming, fast, the characteristics such as temperature is even, resistance stabilization of conducting heat, the glue-line that has overcome traditional mica heating base plate is easily aging, the defects such as local foaming, layering, resistance decrement, non-uniform temperature.
The accompanying drawing explanation
Fig. 1 is the structure chart of the mica heating base plate that scribbles inorganic thick film that provides of the embodiment of the present invention.
Fig. 2 is the longitudinal section of the mica heating base plate that scribbles inorganic thick film of Fig. 1.
Fig. 3 is preparation method's the block diagram of the mica heating base plate that scribbles inorganic thick film of Fig. 1.
Fig. 4 is the heat generating component structure chart of the mica heating base plate that scribbles inorganic thick film of application drawing 1.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Refer to Fig. 1 and Fig. 2, the mica heating base plate 10 that scribbles inorganic thick film 13 that the embodiment of the present invention provides comprises mica substrate carrier 11, and described mica substrate carrier 11 has first surface 16 and the second surface 17 relative with described first surface 16.The described mica heating base plate 10 that scribbles inorganic thick film also comprises the planar inorganic thick film 13 of high temperature sintering on the first surface 16 of described mica substrate carrier 11, the electrode 14 that described inorganic thick film 13 is connected in circuit reaches the lead ends 15 for connecting power supply lead wire and is affixed on described mica substrate carrier 11 to cover described inorganic thick film 13, the mica emulsion sheet 18 of described electrode 14 and described lead ends 15, described lead ends 15 is electrically connected with described electrode 14, described electrode 14 is electrically connected with described inorganic thick film 13, described inorganic thick film 13 high temperature sinterings are on described mica substrate carrier 11, described inorganic thick film 13, the component that comprises following weight fraction:
The mica heating base plate 10 that scribbles inorganic thick film 13 of the present invention at least has following advantage:
1, inorganic thick film 13 is not due to leaded, and material is environmental protection not only, and is rich in far infrared, reduced environmental pollution, useful health, overcome product and due to needs, use in a large number the harmful substance such as strong acid to produce the three wastes, the harmful and serious defect of environmental pollution.
2, the material granule degree of inorganic thick film 13 is meticulousr, and the resistance dispersion is little, and the material sheet resistance is reproducible, and conforming product rate is high, has saved the energy, has lowered production cost, has improved quality and the precision of product, has promoted product competitiveness in the market.
3, the inorganic thick film 13 of the present invention's application, by using bismuth oxide as framework material, be used in conjunction with again the components such as boron oxide, silicon dioxide, zinc oxide, antimonous oxide and strontium carbonate, both realized the performance of inorganic thick film 13, simultaneously, realize zero content of lead oxide with respect to existing inorganic thick film 13, prevented people's lead poisoning and to the pollution of environment when the use inorganic thick film 13; And, due to the use of bismuth oxide, the serviceability temperature of inorganic thick film 13 is improved greatly, enlarged the scope of application of inorganic thick film 13.
4, the inorganic thick film 13 of mica heating base plate 10 of the present invention is " planar " heaters, its heating area is the several times of traditional product " linearity " heater area, reduced the unit power density of heater, reduced the coefficient of expansion of mica substrate carrier 11, thereby while having avoided product work because product is " linearity " thermal source heating arrangement, the unit cross-sectional area power density is large, surface temperature is high, the differential expansion coefficient is large, yielding, sound is arranged during work, very high and cause excessive the brought heating wire short circuit of mica differential expansion coefficient at the local Yin Wendu that is prepared with line with heating function, sparking, the problems such as too fast oxidation,
5, the inorganic thick film 13 of mica heating base plate 10 of the present invention adopts silk-screen printing technique and imposes high-sintering process, and heater and mica substrate carrier 11 are forever made to integral structure, there are not stratified, non-foaming, fast, the characteristics such as temperature is even, resistance stabilization of conducting heat, the glue-line that has overcome traditional mica heating base plate 10 is easily aging, the defects such as local foaming, layering, resistance decrement, non-uniform temperature.
The inorganic thick film 13 of the mica heating base plate 10 of the embodiment of the present invention, comprise two large components, the one, and graphite powder, another pottery formed by metal oxide, glass granules.This pottery, glass granules form after by bismuth oxide, boron oxide, silicon dioxide, zinc oxide, antimonous oxide and strontium carbonate melting.
Concrete, this graphite is a kind of non-metallic conducting material, it is a kind of of carbon simple substance, inorganic thick film 13 is under electric field action, in inorganic thick film 13, the carbon micel produces " Brownian movement ", violent friction and shock occur between the carbon molecule, and the heat energy of generation is mainly with far infrared radiation with to streamed external transmission.Therefore the inorganic thick film 13 of mica heating base plate 10 of the present invention, have the feature place of the far infrared of being rich in.The weight fraction of this graphite powder is 15-30 part, is preferably 20-30 part.The particle diameter of this graphite powder (is less than 200 orders) below 200 orders.
The weight fraction of this bismuth oxide is 60-75 part, is preferably 70-75 part, and this bismuth oxide is the framework material of inorganic thick film 13.Because bismuth oxide has higher softening point temperature (with respect to lead oxide), a large amount of uses of bismuth oxide make the film-forming temperature of inorganic thick film 13, coating maximum operation (service) temperature all obtain larger raising, and the scope of application of inorganic thick film 13 is significantly widened.
The weight fraction of this boron oxide is 5-15 part, and this boron oxide supplements as bismuth oxide, plays the skeleton function of inorganic thick film 13;
The weight fraction of this silicon dioxide is 0.5-2 part, and this silica is also supplementing of bismuth oxide, plays the skeleton function of inorganic thick film 13.
This bismuth oxide, boron oxide and silicon dioxide are all framework materials in inorganic thick film 13, and the three cooperatively interacts, and in inorganic thick film 13, play a supporting role.Simultaneously, by the regulating action of strontium carbonate, three kinds of adhesions between framework material are significantly increased.
The weight fraction of this strontium carbonate is 3-5 part, because the content of bismuth oxide is higher, makes the caking property between inorganic thick film 13 each components greatly reduce, and by adding a small amount of strontium carbonate, the adhesion between bismuth oxide and other components is increased greatly; By cooperatively interacting between this strontium carbonate and bismuth oxide, improved the adhesion of inorganic thick film 13, prevented that the problems such as crackle, explosion from appearring in inorganic thick film 13 in preparation technology's calcination process.
The weight portion of this zinc oxide is 3-6 part.Adding of zinc oxide, can improve the coefficient of expansion of inorganic thick film 13, make the coefficient of expansion of inorganic thick film 13 consistent with glass, regulate the adhesion between inorganic thick film 13 and glass, make inorganic thick film 13 better in adhesion on glass.
The weight fraction of this antimonous oxide is 3-5 part.This antimonous oxide coordinates the effect of strontium carbonate and zinc oxide, improves the adhesive force of pottery, glass granules and substrate, promotes the cohesive force between pottery, glass granules, strengthens the binding ability between pottery, glass granules and carbon dust simultaneously.
By using the various metal oxides of above-mentioned weight fraction, improve on the one hand temperature applicable range, reach the surface conjunction power between pottery, glass granules and carbon dust between improvement pottery, glass granules on the other hand, the adhesion of raising semiconductor thick film inside reaches the adhesive force with carrier.Simultaneously, each component is coordinated mutually, improves the thermal coefficient of expansion of inorganic thick film, improves its thermal stability.
In existing resistive coating material, lead occupies very large amount, and the plumbous skeleton as material has very important significance.But plumbous meeting produce very large impact to human body, environment.Those skilled in the art are attempting plumbous content is reduced always, with other material, substitute, but prepared its electric stability energy of resistive coating out, heat tolerance energy etc. are all undesirable.Particularly use new material as framework material, the adhesive force of resistive coating and thermal stability, all can not well solve.
The inorganic thick film 13 of mica heating base plate 10 of the present invention is by being used bismuth oxide as framework material, be used in conjunction with again the components such as boron oxide, silicon dioxide, zinc oxide, antimonous oxide and strontium carbonate, both realized the performance of inorganic thick film 13, simultaneously, greatly reduce the content of lead oxide with respect to existing inorganic thick film 13, prevented people's lead poisoning when using inorganic thick film 13; And, due to the use of bismuth oxide, the serviceability temperature of inorganic thick film 13 is improved greatly, enlarged the scope of application of inorganic thick film 13.
The embodiment of the present invention also provides a kind of above-mentioned preparation method who scribbles the mica heating base plate 10 of inorganic thick film 13, and it comprises the steps:
S1) provide mica substrate carrier 11;
S2) print successively described electrode 14, described lead ends 15 and described inorganic thick film 13 on the described first surface 16 of described mica substrate carrier 11, and described lead ends 15 and described electrode 14 are electrically connected, described inorganic thick film 13 is electrically connected with described electrode 14;
S3) the mica substrate carrier 11 that is printed with described electrode 14, described lead ends 15 and described inorganic thick film 13 is carried out to sintering processes;
S4) described mica emulsion sheet 18 is affixed on described mica substrate carrier 11 to cover described inorganic thick film 13, described electrode 14 and described lead ends 15.
Please consult Fig. 3, Fig. 3 shows the preparation method's of the above-mentioned mica heating base plate 10 that scribbles inorganic thick film 13 step more specifically simultaneously.Wherein,
Step S2) by the rapid S02 of each small step), S12), S22), S32), S42), S52), S62) complete, particularly, step S02) be the described electrode 14 of silk-screen, step S12) for drying electrode 14, the temperature of this oven dry is 180 ℃~250 ℃, and baking time is 30min.Step S22) be the outward appearance of inspecting electrode 14, be mainly inspecting electrode 14 whether bubble, whether have the slag point, whether regular, whether have and lack to print and bite.Step S32) be the described lead ends 15 of silk-screen; Step S42) be the described inorganic thick film 13 of silk-screen; Step S52) for drying described lead ends 15 and described inorganic thick film 13, its bake out temperature is 180 ℃~250 ℃, and baking time is 15min-20min; Step S62) be checking procedure, the outward appearance that it checks described lead ends 15 and described inorganic thick film 13, be mainly check whether bubble, whether have the slag point, whether regular, whether have and lack to print and bite.
Understandably, if conditions permit can be printed described electrode 14, described lead ends 15 and described inorganic thick film 13 successively continuously, the step of doing again afterwards oven dry, check, sintering and pasting mica emulsion sheet 18.
Understandably, print described lead ends 15 and dried successively and check processing afterwards, and then print described inorganic thick film 13, dried successively and check again processing after being completed for printing, and then carry out sintering processes.At step S4) also comprise afterwards step S5), wherein another mica emulsion sheet 19 is affixed on the described second surface 17 of described mica substrate carrier 11.This another mica emulsion sheet 19 is identical or different with above-mentioned mica emulsion sheet 18.
In step S2) in, also comprising the step a) for preparing described inorganic thick film 13, it comprises the steps:
Step SA), provide raw material:
Described graphite powder, bismuth oxide, boron oxide, silicon dioxide, antimonous oxide, zinc oxide and strontium carbonate are provided by weight ratio;
Step SB), prepare the first mixture:
By described bismuth oxide, boron oxide, silicon dioxide, antimonous oxide, zinc oxide and strontium carbonate heating and melting, fused mass is ground to below 350 orders after cooling, add described graphite powder to mix, obtain the first mixture;
Step SC), prepare the second mixture:
Described the first mixture is mixed for 65-80: 20-35 by weight with organic carrier, obtain the second mixture; Described the second mixture is coated on described mica substrate carrier 11 and obtained inorganic thick film 13.
Concrete, step SA) in, this graphite powder, bismuth oxide, boron oxide, silicon dioxide, zinc oxide, antimonous oxide and strontium carbonate and aforesaid identical, do not repeat to set forth at this.
Step SB) in, above-mentioned bismuth oxide, boron oxide, silicon dioxide, zinc oxide, antimonous oxide and strontium carbonate are mixed, be heated to 900-1200 ℃, make the above-mentioned raw materials melting, obtain glass, ceramic-like material grain after cooling; This glass, ceramic-like material grain are carried out to milled processed (pulverizing and ball milling), make the particle diameter of powder below 350 orders, then add above-mentioned graphite powder, obtain the first mixture after mixing; By controlling the particle diameter of the first mixture, improve the resistance dispersion of inorganic thick film 13, improve its sheet resistance repeatability.
Step SC), in, this organic carrier comprises the component of following percentage by weight:
Terpinol 85-95%
Ethyl cellulose 5-15%.
Because the boiling point of organic carrier is lower, guarantee that, in follow-up dry run, this organic material can be evaporated fully.
In this step, by step SB) in the first mixture of obtaining with this organic carrier, mix, make slurry, obtain the second mixture;
The silk screen printing on mica substrate carrier 11 of this second mixture is become to one deck membranoid substance, the 40-120 order.Then dry 15-20 minute under 180-250 ℃ of condition, be sintering 15-20 minute under 400-700 ℃ of condition in temperature after drying, obtains inorganic thick film 13.
The preparation of the inorganic thick film 13 of the present invention's application is by being used bismuth oxide as framework material, be used in conjunction with again the components such as boron oxide, silicon dioxide, zinc oxide, antimonous oxide and strontium carbonate, prepared inorganic thick film 13 environmental-protecting performances have been realized, enlarged the scope of application of inorganic thick film 13, inorganic thick film 13 preparation methods of the present invention's application, simple to operate, with low cost, be very suitable for suitability for industrialized production.
The prepared inorganic thick film 13 of the present invention is core parts of various electric heating products and heating system, characteristic with planar infrared radiation heating, be widely used in the various Space, Places that the various requirements such as various household heaters, far infrared light wave sauna house, medical infant incubator are good to thermal stability and electric heating appliance, medical treatment, care appliance and needs environmental protection heat.Inorganic thick film 13 is that to take bismuth oxide (not leaded), graphite powder (being rich in far infrared) be Main Ingredients and Appearance, add a small amount of strontium carbonate, silicon dioxide, boron oxide, zinc oxide and other trace mineral supplements, under 400 ℃ of-1200 ℃ of serial high temperature, the techniques such as sintering and printing are made.Inorganic thick film 13 materials in the present invention are not due to leaded, and material environment friendly, produce and use procedure produces without the three wastes; Graphite powder is the resistive conductor material, and health, be rich in far infrared, useful health; The thick film main framework material is that the inorganic high-temp metal oxide materials is made, and resistance, electric property are more stable, are easy to industrialization, large-scale production; It is framework material that inorganic thick film 13 be take the materials such as bismuth oxide, silicon dioxide, and material softening point temperature obviously improves, the thick film that it is prepared, and range of application is more extensive.
Please again consult Fig. 1 and 2, Fig. 1 and 2 has shown mica heating base plate 10 structure charts of applying above-mentioned inorganic thick film, this mica heating base plate 10 comprises mica substrate carrier 11, be formed at successively electrode 14, lead ends 15 and described inorganic thick film 13 on this mica substrate carrier 11, and described lead ends 15 and described electrode 14 are electrically connected, described inorganic thick film 13 is electrically connected with described electrode 14.
Below in conjunction with specific embodiment, the above-mentioned preparation method who scribbles the mica heating base plate 10 of inorganic thick film 13 is described in detail.
Embodiment 1
Get the rectangle mica substrate carrier 11 of a block length 600mm, wide 200mm, thick 0.5mm;
Then respectively apply a long 170mm with conductive silver slurry on the surface of 11 two minor faces of this rectangle mica substrate carrier, the electrode 14 of wide 10mm, and then coat as shown in Figure 1 lead ends 15, and then following formula material is provided:
Figure BDA0000381833280000111
6 kinds of compositions except graphite powder in above-mentioned formula are stirred, by this mixture in 1200 ℃ of lower meltings 60 minutes, after obtained mixed material piece is cooling by its fragmentation, then use the ball mill ball milling 48 hours, make particle diameter be less than 350 purposes Powdered, toward wherein adding graphite powder, obtain the first mixture again; Then the liquid organic carrier that adds 120g-150g to be comprised of 95% weight terpinol and 5% weight diethylene cellulose, be modulated into uniform slurry, obtains the second mixture;
Adopt silk-screen printing technique that slurry is printed on above-mentioned mica substrate carrier 11 and the side surface with electrode 14 and lead ends 15.Should note during printing by Fig. 1 and as shown in Figure 2, make 2/3 part of inorganic thick film 13 coated electrodes 14, with preventing poor contact the reserved lead ends of attention 15 positions, so that power line connects.It is dried 15 minutes under 200 ℃, then, 620 ℃ of lower sintering 15 minutes, made inorganic thick film 13 of the present invention, the thickness of coating is about 0.25mm.Thereby having formed an area is 55 * 17=935Cm 2tabular mica heating base plate 10.The resistance that obtains 14, two electrode with the resistance instrumentation is 345 Ω, and being equivalent to its square resistance is 106 Ω.
Embodiment 2
In embodiment 2, except replacing the mica base plate with ceramic bottom board, other are all tested by the condition of embodiment 1, have obtained the substantially the same result of embodiment 1.
Embodiment 3
In embodiment 3, except replacing ceramic bottom board with the devitrified glass base plate, other are all tested by the condition of embodiment 2, have obtained the result substantially the same with embodiment 1-2.
Comparative Examples 1
In Comparative Examples 1, except not containing strontium carbonate, other are all tested by the condition of embodiment 1.
Comparative Examples 2
In Comparative Examples 2, except not containing zinc oxide, other are all tested by the condition of embodiment 1.
Performance test
Stability test 1(storage stability):
Each 10 of the resistive elements (for example mica resistance element, ceramic resistor element, devitrified glass resistive element) of 3 kinds of application inorganic thick films that above-described embodiment 1-3 is obtained are placed on (relative humidity 80%-90%) in moist experimental box and store 1 year, and result is not found any one resistive element moisture absorption or gone mouldy.The resistance value testing result shows, the rate of change of its resistance value≤1%.
Stability test 2(thermal stability):
(virtual voltage: 253V), its current strength reaches 0.85 ampere, its gross power and reaches 185W, and its thermal equilibrium temperature reaches 220 ℃ or slightly high to apply 1.15 times of alternating voltage of 220V between the two end electrodes 14 of 3 kinds of above-mentioned resistive elements.Under this extra-heavy operating state, continuous operation is 5000 hours.Then stop energising, carry out resistance measurement after it is cooled to room temperature.Result shows, the rate of change of its resistance value≤1%.
Temperature homogeneity test 3(measures being uniformly distributed of inorganic thick-film resistance component temperature in service, i.e. the uniformity of square resistance):
This is an iron case that peripheral sealing is good for test.Divide 3 test periods by 3 kinds of above-mentioned resistive elements, test respectively each resistive element.At first, resistive element is lain on the bottom insulation support of iron case, 6 temperature sensing probes are placed on the different position of resistive element face coat.Resistive element is with 220 ℃ of operations 300 minutes, the average temperature value that records temperature sensing probe in 30 minutes.Its temperature high-low temperature difference should be in 5 ℃.In addition, the surface temperature of conductive electrode 14 and lead ends 15 should be higher than the temperature of resistive element face coat.Result shows, the temperature of resistive element face coat is that high-low temperature difference, in 5 ℃, can be obtained by above-mentioned test: the square resistance of resistive element face coat is uniform uniformly.
Far infrared performance test 4: each 10 of above-mentioned 3 kinds of inorganic thick-film resistance elements are delivered to: the infrared and industrial electroheat product quality supervision and inspection center of country is according to GB/T4654-2008 " requirements of nonmetal basal body infrared radiation heater current techique " and GB/T7287-2008 " infrared radiation heater test method " detection, and the indices such as its relative radiant-energy spectrum, electricity-thermal radiation conversion efficiency, normal direction total emissivity all meet above-mentioned standard-required.
Environmental-protecting performance test 5: each 10 of above-mentioned 3 kinds of inorganic thick-film resistance elements are delivered to: An Mute detection technique Co., Ltd, in accordance with the 2011/65/EU of European Union (ROHS) instruction, detect plumbous (pb), cadmium (cd), mercury (Hg), Cr VI (Cr 6+), the indices such as content of Polybrominated biphenyl (PBBs), Poly Brominated Diphenyl Ethers (PBDEs) all meet above-mentioned ROHS command request.
After inorganic thick-film resistance coating adhesion test 6(test run, the adhesive force of inorganic thick-film resistance coating).
By respectively 10 of above-mentioned mica, ceramic wafer, 3 kinds of inorganic resistance thick film resistance elements of micro-crystal plate, carry out again the adhesion test of inorganic thick-film resistance component resistance coating respectively after stability test, far infrared performance test, environmental-protecting performance test, the test of temperature temperature homogeneity.
Experimental condition: carry out in room temperature 23C ° ± 2C ° and relative humidity 50 ± 5 ﹪.
Concrete grammar is as follows: draw 10 * 10 little grids of (100) 1mm * 1mm with cutter on the inorganic thick-film resistance coating surface of test, each line should reach the bottom of coating deeply; With hairbrush, the fragment of test zone is cleaned down; With 3M600 or 3M610 gummed paper or be equal to the tested little grid of gummed paper stick fast of effect, and with the erasing rubber wiping adhesive tape of exerting oneself, to strengthen contact area and the dynamics in adhesive tape and tested zone; Catch adhesive tape one end with hand, (90 °) shut down rapidly gummed paper in the vertical direction, and same position carries out identical test 2 times.Through above-mentioned test, estimate the intersection of its otch, the smooth of the edge of otch, the grid edge is without any peeling off.The adhesion test of its inorganic thick-film resistance component resistance coating is qualified.
Refer to Fig. 4, the embodiment of the present invention also provides a kind of mica heat generating component 100, it comprises the above-mentioned mica heating base plate 10 that scribbles inorganic thick film 13, be affixed on another mica emulsion sheet 19 on the described second surface 17 of described mica substrate carrier 11, be located in described mica substrate carrier 11 surrounding metal hemming edge bar 40 and be connected in thermostat (not shown) and the fuse (not shown) on described power supply lead wire.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.

Claims (10)

1. a mica heating base plate that scribbles inorganic thick film, it is characterized in that: the described mica heating base plate that scribbles inorganic thick film comprises the mica substrate carrier, described mica substrate carrier has first surface and the second surface relative with described first surface, the described mica heating base plate that scribbles inorganic thick film also comprises the planar inorganic thick film of high temperature sintering on the first surface of described mica substrate carrier, the electrode that described inorganic thick film is connected in circuit reaches the lead ends for connecting power supply lead wire and is affixed on described mica substrate carrier to cover described inorganic thick film, the mica emulsion sheet of described electrode and described lead ends, described lead ends and described electrode are electrically connected, described electrode and described inorganic thick film are electrically connected, described inorganic thick film high temperature sintering is on described mica substrate carrier, described inorganic thick film, the component that comprises following weight fraction:
Figure FDA0000381833270000011
2. the mica heating base plate that scribbles inorganic thick film as claimed in claim 1, is characterized in that, the weight fraction of described bismuth oxide is 70-75 part.
3. the preparation method as the mica heating base plate that scribbles inorganic thick film of claim 1 or 2, it comprises the steps:
S1) provide the mica substrate carrier;
S2) print successively described electrode, described lead ends and described inorganic thick film on the described first surface of described mica substrate carrier, and described lead ends and described electrode are electrically connected, described inorganic thick film and described electrode are electrically connected;
S3) the mica substrate carrier that is printed with described electrode, described lead ends and described inorganic thick film is carried out to sintering processes;
S4) described mica emulsion sheet is affixed on described mica substrate carrier to cover described inorganic thick film, described electrode and described lead ends.
4. the preparation method who scribbles the mica heating base plate of inorganic thick film as claimed in claim 3, is characterized in that, in step S2) in, also comprising the step a) for preparing described inorganic thick film, it comprises the steps:
Described graphite powder, bismuth oxide, boron oxide, silicon dioxide, antimonous oxide, zinc oxide and strontium carbonate are provided by weight ratio;
By described bismuth oxide, boron oxide, silicon dioxide, antimonous oxide, zinc oxide and strontium carbonate heating and melting, fused mass is ground to below 350 orders after cooling, add described graphite powder to mix, obtain the first mixture; Described the first mixture is mixed for 65-80: 20-35 by weight with organic carrier, obtain the second mixture; Described the second mixture is coated on described mica substrate carrier and obtained inorganic thick film.
5. the preparation method who scribbles the mica heating base plate of inorganic thick film as claimed in claim 4, is characterized in that, the weight fraction of the bismuth oxide of described inorganic thick film is 70-75 part.
6. the preparation method who scribbles the mica heating base plate of inorganic thick film as claimed in claim 4, it is characterized in that, the temperature of described bismuth oxide, described boron oxide, described silicon dioxide, described antimonous oxide, described zinc oxide and described strontium carbonate heating and melting is 900-1200 ℃.
7. the preparation method who scribbles the mica heating base plate of inorganic thick film as claimed in claim 3, is characterized in that, in step S3) in, the temperature of described sintering is 400-700 ℃.
8. the preparation method who scribbles the mica heating base plate of inorganic thick film as claimed in claim 4, is characterized in that, described organic carrier comprises the component of following percentage by weight:
Terpinol 85-95%
Ethyl cellulose 5-15%.
9. the preparation method who scribbles the mica heating base plate of inorganic thick film as claimed in claim 3, is characterized in that, also comprises step S5), wherein another mica emulsion sheet is affixed on the described second surface of described mica substrate carrier.
10. a mica heat generating component is characterized in that: described mica heat generating component comprises the mica heating base plate that scribbles inorganic thick film as claim 1 or 2, be affixed on as described in the mica substrate carrier as described in another mica emulsion sheet on second surface, be located in as described in the mica substrate carrier surrounding the metal hemming edge bar and be connected in as described in thermostat and fuse on power supply lead wire.
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CN111132395A (en) * 2019-12-31 2020-05-08 陆建华 Heating body with mica sheet and graphene coating and preparation process thereof
CN113260098A (en) * 2021-05-10 2021-08-13 广东温道百镒健康科技有限公司 Far infrared heating plate structure and manufacturing process thereof
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CN111132395A (en) * 2019-12-31 2020-05-08 陆建华 Heating body with mica sheet and graphene coating and preparation process thereof
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