CN102674820B - Insulating material, ceramic heating element containing insulating material, preparation and application - Google Patents
Insulating material, ceramic heating element containing insulating material, preparation and application Download PDFInfo
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- CN102674820B CN102674820B CN2012101793567A CN201210179356A CN102674820B CN 102674820 B CN102674820 B CN 102674820B CN 2012101793567 A CN2012101793567 A CN 2012101793567A CN 201210179356 A CN201210179356 A CN 201210179356A CN 102674820 B CN102674820 B CN 102674820B
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Abstract
The invention relates to an insulating material, a ceramic heating element using the insulating material and a preparation process and application of the ceramic heating element. The insulating material is a ceramic material with alumina serving as a main body, and the insulating material comprises, by mass, 95-98% of nano-alumina, 0.5-2% of titanium dioxide, 0.4-2% of silicon dioxide, 0.2-0.7% of calcium oxide and 0.1-0.3% of yttrium oxide. The ceramic heating element using the insulating material comprises a lower ceramic substrate, a lower insulating layer, a heating electrode, an upper insulating layer and an upper ceramic substrate from bottom to top sequentially, wherein the lower insulating layer and the upper insulating layer are made of the insulating material, and the heating electrode is connected with an electrode lead. The insulating material has the advantages of low in sintering temperature, good in insulating performance, good in compatibility with a heating resistance material and a ceramic support part, long in service life, environment-friendly and harmless to human bodies.
Description
Technical field
The present invention relates to a kind of insulating material, also relate to ceramic heating element of applying this insulating material and preparation method thereof, also relate in addition the application of this ceramic heating element.
Background technology
Ceramic heating element is the heater that a kind of high efficiency, heat distribution are even, have insulation property, it is direct printing conductive resistance slurry on ceramic green, after lamination, binder removal, at high temperature burn till altogether the product be integrated, product itself and production process meet environmental requirement.With the conventional alloys heating wire, the PTC heating element is compared and is had simple in structure, the plurality of advantages such as intensification is rapid, power density is large, it is safe, corrosion-resistant to use, long service life, so be widely used in daily life, industrial technology, military affairs, science, communication, medical treatment, environmental protection, the multiple fields such as aerospace.
Soya-bean milk has high nutritive value, in soya-bean milk, contains the necessary amino acid of multiple high-quality protein, multivitamin, multiple human body and various trace elements etc., is a kind of ideal healthy food.No matter adult, the elderly and children, drink as long as adhere to, for improving physique, prevention and treatment illness, all benefits.Along with the enhancing of health of people understanding, for health, that drinks is relieved, selects one after another family's self-control soya-bean milk, thereby pulls household soy milk machine market.
But the heater of the soy bean milk making machine on market is for being mainly the Resistant heating pipe now, and existing heat generation device has following weak point:
1. metal directly contacts with soya-bean milk, and kish and corrosion of metals thing in soya-bean milk make soya-bean milk that the metal residual flavor be arranged, and affect the delicious food of soya-bean milk, and also can cause certain injury to health;
2. heat-generating pipe is difficult for cleaning up, easily breed bacteria;
3. the heating uniformity of heat-generating pipe is poor, produces localized hyperthermia, easily occurs being charred on the heater surface, is difficult to clean.
Existing ceramic heater is mainly used in the fields such as gas sensor, and application is rare in the kitchen appliance field.
Number of patent application CN200580016753.0 discloses a kind of ceramic heater and has adopted its lambda sensor and hair-waving to cut, and number of patent application CN200520043672.7 discloses a kind of heating plate of Novel aluminum oxide ceramic with the high sensitivity temperature sensor.The pottery of above ceramic heating element is all aluminium oxide ceramics, and alumina surface is coarse, and brittleness of ceramics is large, poor with human compatibility, is not suitable for doing the heater of soy bean milk making machine.
Summary of the invention
First technical problem that the present invention will solve is to provide a kind of new insulation material, this insulating material has advantages of that sintering temperature is low, good insulation preformance, with the heating resistor material and the ceramic supporting body matching is good, long service life, environmental protection, to human body without injury.
Second technical problem that the present invention will solve is to provide a kind of ceramic heating element of applying this insulating material.This ceramic heating element heats up rapidly, power density is large, homogeneous heating, corrosion-resistant, easy cleaning,, long service life pollution-free to food, and cost is low.
The 3rd technical problem that the present invention will solve is to provide the preparation method of above-mentioned ceramic heating element.
The 4th technical problem that the present invention will solve is to provide the concrete application of this ceramic heating element.
Technical problem to be solved by this invention is achieved by the following technical programs:
A kind of insulating material, be the ceramic material of main body for take aluminium oxide, and each component and mass percent be, nano aluminium oxide 95 ~ 98%, titanium dioxide 0.5 ~ 2%, silicon dioxide 0.4 ~ 2%, calcium oxide 0.2 ~ 0.7%, yttria 0.1 ~ 0.3%.
A kind of ceramic heating element of applying above-mentioned insulating material, be followed successively by from top to bottom upper insulating barrier, upper ceramic matrix that lower insulating barrier, heating electrode, described insulating material that lower ceramic matrix, described insulating material make are made, described heating electrode is connected with contact conductor.
Described lower ceramic matrix and upper ceramic matrix are the cubic polycrystal nanometer zirconium oxide ceramic of 2 ~ 4mo1% stabilized with yttrium oxide.
The thickness of described lower ceramic matrix and upper ceramic matrix is 0.1 ~ 2mm.
Described heating electrode material used is mixed with and is formed by the component of following mass percent: Aludirome 60 ~ 85%, nano aluminium oxide 8 ~ 20%, titanium dioxide 1 ~ 4%, silicon dioxide 0.4 ~ 2%, calcium oxide 0.2 ~ 1.0%, yttria 0.1 ~ 0.4%.
Described Aludirome is mixed by the component of following mass percent: chromium 16 ~ 21%, and aluminium 2 ~ 5%, rhenium 0.5 ~ 2%, molybdenum 1.4 ~ 2.5%, niobium 0.4 ~ 0.8%, surplus is iron.
The thickness of described lower insulating barrier (4) and upper insulating barrier (2) is 10 ~ 120 μ m.
A kind of preparation method of above-mentioned ceramic heating element, preparation process is followed successively by:
(1) prepare respectively the material of heating electrode, upper insulating barrier and lower insulating barrier, upper ceramic matrix and lower ceramic matrix;
(2) printing of layers of material: on the green compact of lower ceramic matrix, adopt silk-screen printing technique print successively under insulating barrier, heating electrode, on insulating barrier; The printed layers thickness that wherein descends insulating barrier and upper insulating barrier is 15 ~ 160 μ m; Heating electrode (3) printed layers thickness is 15 ~ 25 μ m;
Step 3: superimposed after printing
By the green compact of step 2 resulting materials and the green compact of upper ceramic matrix, under the pressure condition of the temperature of 50 ~ 120 ℃ and 10 ~ 60MPa, carry out superimposed;
Step 4: high temperature sintering
Superimposed body is put into to vacuum degreasing sintering furnace and carry out binder removal degreasing and high temperature sintering, the high temperature sintering temperature is 1350 ~ 1550 ℃, and temperature retention time is 1 ~ 3h;
Step 5: the welding of contact conductor
Adopt soldering processes that heating electrode is connected with lead-in wire, prepare required ceramic heating element.
The preparation method of described upper ceramic matrix and lower ceramic matrix is: adopt casting technique to prepare green compact, the thickness of green compact is 0.12 ~ 2.5mm;
The preparation method of heating electrode screen printing sizing agent is: the powder of heating resistor material needed raw material material and the organic carrier that contains adhesive are mixed; The powder of described heating resistor material needed raw material material is 0.6 ~ 1.5:1 with the mass ratio that contains the organic carrier of adhesive.
The preparation method of upper insulating barrier (2) and lower insulating barrier (4) screen printing sizing agent is: the powder of insulating barrier needed raw material material and the organic carrier that contains adhesive are mixed; The powder of described insulating barrier needed raw material material is 0.6 ~ 1.5:1 with the mass ratio that contains the organic carrier of adhesive.
A kind of ceramic heating element is as the application of soy bean milk making machine heater block.
Compared to existing technology, the present invention has following beneficial effect:
1, new insulation material of the present invention have advantages of that sintering temperature is low, good insulation preformance, with the heating resistor material and the ceramic supporting body matching is good, long service life, environmental protection, to human body without injury.
2, the present invention has applied the ceramic heating element that this insulating material is made, and after tested, have following advantage: (1) efficiency of heating surface is high, and reaching 300 ℃ only needs 50 seconds; (2) heating uniformity is high, and the temperature difference maximum of 5 points is less than 5 ℃; (3) durability is high, after 3000 circulation cold shock testings, there is no crackle, comes off, layering, and resistance change rate is less than 8%; (4) outward appearance does not have crackle, there is no stain, any surface finish.
3, the present invention has applied the ceramic heating element that this heating resistor material makes and has been applied in soy bean milk making machine, comparing existing Resistant heating pipe has the following advantages: (1) does not produce metal residue and corrosion of metals thing, in soya-bean milk, without the metal residual flavor, human body is not produced to harm; (2) ceramic heating element easy cleaning more, do not have bacteria breed; (3) heating uniformity due to ceramic heating element is good, can not be charred because localized hyperthermia causes soya-bean milk, reduces taste and the nutritive value of soya-bean milk.
The accompanying drawing explanation
Fig. 1 is the explosive view of ceramic heating element of the present invention.
Embodiment
For the ease of it will be appreciated by those skilled in the art that the present invention will be further described below in conjunction with embodiment.Embodiment is only the preferred embodiment of the present invention, is not limitation of the present invention.
A kind of insulating material, each component and mass percent be, nano aluminium oxide 97%, titanium dioxide 1.2%, silica 1 %, calcium oxide 0.5%, yttria 0.3%.
As shown in Figure 1, a kind of ceramic heating element of applying above-mentioned insulating material, be followed successively by from top to bottom upper insulating barrier 2, upper ceramic matrix 1 that lower insulating barrier 4, heating electrode 3, above-mentioned insulating material that lower ceramic matrix 6, above-mentioned insulating material make are made, described heating electrode 3 is connected with contact conductor 5.
Described upper ceramic matrix 1 and lower ceramic matrix 6 are the cubic polycrystal nanometer zirconium oxide ceramic of 3mo1% stabilized with yttrium oxide.
Preparation heating electrode 3 heating resistor material used, mixed by the component of following mass percent: Aludirome 80%, nano aluminium oxide 13%, titanium dioxide 4%, silica 1 .8%, calcium oxide 0.8%, yttria 0.4%.
Wherein Aludirome is mixed by the component of following mass percent: chromium (Cr) is 19%, and aluminium (Al) is 5%, rhenium (Re) 2%, and molybdenum (Mo) 2%, niobium (Nb) 0.8%, surplus is iron (Fe).
Below the preparation method of ceramic heating element elaborated.
Step 1: the preparation of layers of material
(1) preparation of ceramic matrix
Adopt casting technique to prepare the green compact of the nanometer zirconium oxide ceramic matrix of 3mo1% stabilized with yttrium oxide, the length of green compact is 80mm, and width is 30mm, and thickness is 0.8mm.
(2) preparation of heating electrode 3
100 parts of the heating electrode weight of take take the powder of following umber as benchmark: 80 parts of Aludiromes, 13 parts of nano aluminium oxides, 4 parts of titanium dioxide, silica 1 .8 part, 0.8 part, calcium oxide, 0.4 part of yttria; Wherein in Aludirome, the mass percent of each component is: chromium (Cr) is 19%, and aluminium (Al) is 5%, rhenium (Re) 2%, and molybdenum (Mo) 2%, niobium (Nb) 0.8%, all the other content are iron (Fe).Above powder and the organic carrier that contains adhesive are mixed with to the heating electrode screen printing sizing agent.
(3) preparation of insulating barrier
100 parts of the weight of insulating barrier of take are benchmark, take 97 parts of nano aluminium oxides, 1.2 parts of titanium dioxide, silica 1 part, 0.5 part, calcium oxide, 0.3 part of yttria.Above powder and the organic carrier that contains adhesive are mixed with to the insulating barrier screen printing sizing agent.
Step 2: the printing of layers of material
On the green compact of zirconia matrix 6, adopt silk-screen printing technique to print successively insulating barrier 4, heating electrode 5, insulating barrier 2; Wherein insulating barrier 2 and 4 printed layers length are 70mm, and width is 20mm, and thickness is 25-30 μ m, and heating electrode printed layers thickness is 20 μ m.
Step 3: superimposed after printing
By being printed with the green compact of zirconia matrix 6 of insulating barrier and heating electrode and the green compact of zirconia matrix 1, under the pressure condition of the temperature of 80 ℃ and 30MPa, carry out superimposed.
Step 4: high temperature sintering
Superimposed body is put into to vacuum degreasing sintering furnace and carry out binder removal degreasing and high temperature sintering, the high temperature sintering temperature is 1450 ℃, and temperature retention time is 2h.
Step 5: the welding of contact conductor
Adopt soldering processes that heating electrode is connected with contact conductor, prepare required ceramic heating element.
Ceramic heating element prepared by the present embodiment carries out Performance Detection.
The detection data of insulation property index:
Dielectric strength (or being called DC breakdown intensity): be greater than 20Kv/mm (GB-T 5593-1996 electronic devices and components structural ceramic material .5.13)
Specific insulation: in the time of 20 ℃, ρ ν>=1 * 10
14Ω cm; In the time of 100 ℃, ρ ν>=1 * 10
14Ω cm; In the time of 300 ℃, ρ ν>=1 * 10
12Ω cm; In the time of 500 ℃, ρ ν>=1 * 10
10Ω cm.(GB-T 5594.5-1985 electronic devices and components structural ceramic material performance test methods specific insulation method of testing).
It is below corrosion resistance test (GB-T 5594.6-1985 electronic devices and components structural ceramic material performance test methods chemical stability method of testing)
Acid proof test: H≤7 mg/cm2,
Alkaline-resisting test: N≤0.2 mg/cm2
The detection of other index, detection method is as follows:
1, outward appearance detects: whether employing visually observes ceramic surface crackle, stain;
2, the efficiency of heating surface detects: heating electrode is connected to the domestic circuit of 220V, test heating element surface reaches 300 ℃ of needed times;
3, heating uniformity detects: when the test ceramic heating element reaches stable temperature point, and the Temperature numerical of four angles of periphery and center, the temperature difference maximum of 5 points of calculating.
4, durability test: to the ceramic heating element applied voltage, make the temperature of ceramic heating element reach 300 ℃, then off voltage, to ceramic heating element, blow air, ceramic heating element integral body is cooled to below 40 ℃, 3000 circulation cold shock testings like this, observe whether ceramic heating element crackle occurs, come off, layering, the resistance variations of test heating element.
The present embodiment ceramic heating element the performance test results is in Table 1.
Table 1 ceramic heating element the performance test results
| Test event | Test case |
| Outward appearance | There is no crackle, there is no stain, any surface finish |
| The efficiency of heating surface | Reach 300 ℃ of needed time 5S |
| Heating uniformity | The temperature difference maximum of 5 points is less than 5 ℃ |
| Durability | After 3000 circulation cold shock testings, there is no crackle, come off, layering, resistance change rate is less than 8%. |
The present invention also provides a kind of application of above-mentioned ceramic heating element, is about to above-mentioned ceramic heating element and replaces the heater block of existing Resistant heating pipe as soy bean milk making machine.The structure of soy bean milk making machine, the accessory of soy bean milk making machine, program control, be assembled into conventionally known to one of skill in the artly, also do not repeat herein.Ceramic heating element prepared in embodiment 1 by the heater in the soy bean milk making machine of the present embodiment is made into, and a soy bean milk making machine contains 3 ceramic heating elements, is evenly arranged in cup.
This soy bean milk making machine is charred, does not have metal residual flavor, free of contamination soya-bean milk owing to possessing the described ceramic heating element of the embodiment of the present invention 1, can not prepare; Soy bean milk making machine is easily cleaned, long service life.
Embodiment 2
A kind of insulating material, each component and mass percent be, nano aluminium oxide 95%, titanium dioxide 2%, silicon dioxide 2%, calcium oxide 0.7%, yttria 0.3%.
Having applied the present embodiment insulating material, to prepare the method for ceramic heating element with embodiment 1 identical, do not do and be repeated in this description at this.
It is as follows that the insulation property of having applied insulating barrier in the ceramic heating element that the present embodiment insulating material makes detect index:
Dielectric strength (or being called DC breakdown intensity): be greater than 20Kv/mm (GB-T 5593-1996 electronic devices and components structural ceramic material .5.13)
Specific insulation: in the time of 20 ℃, ρ ν>=1 * 10
14Ω cm; In the time of 100 ℃, ρ ν>=1 * 10
14Ω cm; In the time of 300 ℃, ρ ν>=1 * 10
12Ω cm; In the time of 500 ℃, ρ ν>=1 * 10
10Ω cm.(GB-T 5594.5-1985 electronic devices and components structural ceramic material performance test methods specific insulation method of testing).
It is below corrosion resistance test (GB-T 5594.6-1985 electronic devices and components structural ceramic material performance test methods chemical stability method of testing)
Acid proof test: H≤7 mg/cm
2,
Alkaline-resisting test: N≤0.2 mg/cm
2
Embodiment 3
Nano aluminium oxide 98%, titanium dioxide 0.5%, silicon dioxide 0.6%, calcium oxide 0.6%, yttria 0.3%.
Having applied the present embodiment insulating material, to prepare the method for ceramic heating element with embodiment 1 identical, do not do and be repeated in this description at this.
It is as follows that the insulation property of having applied the ceramic heating element that the present embodiment insulating material makes detect index:
Dielectric strength (or being called DC breakdown intensity): be greater than 20Kv/mm (GB-T 5593-1996 electronic devices and components structural ceramic material .5.13)
Specific insulation: in the time of 20 ℃, ρ ν>=1 * 10
14Ω cm; In the time of 100 ℃, ρ ν>=1 * 10
14Ω cm; In the time of 300 ℃, ρ ν>=1 * 10
12Ω cm; In the time of 500 ℃, ρ ν>=1 * 10
10Ω cm.(GB-T 5594.5-1985 electronic devices and components structural ceramic material performance test methods specific insulation method of testing).
It is below corrosion resistance test (GB-T 5594.6-1985 electronic devices and components structural ceramic material performance test methods chemical stability method of testing)
Acid proof test: H≤7 mg/cm
2,
Alkaline-resisting test: N≤0.2 mg/cm
2.
Claims (1)
1. ceramic heating element, it is characterized in that: be followed successively by from top to bottom upper insulating barrier (2), upper ceramic matrix (1) that lower insulating barrier (4), heating electrode (3), described insulating material that lower ceramic matrix (6), insulating material make are made, described heating electrode (3) is connected with contact conductor (5);
Described insulating material is the ceramic material of main body for take aluminium oxide, and each component and mass percent be, nano aluminium oxide 95 ~ 98%, titanium dioxide 0.5 ~ 2%, silicon dioxide 0.4 ~ 2%, calcium oxide 0.2 ~ 0.7%, yttria 0.1 ~ 0.3%;
Wherein, described heating electrode (3) material used is mixed with and is formed by the component of following mass percent: Aludirome 60 ~ 85%, nano aluminium oxide 8 ~ 20%, titanium dioxide 1 ~ 4%, silicon dioxide 0.4 ~ 2%, calcium oxide 0.2 ~ 1.0%, yttria 0.1 ~ 0.4%, the mass percent sum of described each component of heating electrode material therefor is 100%;
Described Aludirome is mixed by the component of following mass percent: chromium 16 ~ 21%, and aluminium 2 ~ 5%, rhenium 0.5 ~ 2%, molybdenum 1.4 ~ 2.5%, niobium 0.4 ~ 0.8%, surplus is iron;
Described lower ceramic matrix (6) and upper ceramic matrix (1) are the cubic polycrystal nanometer zirconium oxide ceramic of 2 ~ 4mo1% stabilized with yttrium oxide.
2. ceramic heating element according to claim 1, it is characterized in that: the thickness of described lower ceramic matrix (6) and upper ceramic matrix (1) is 0.1 ~ 2mm.
3. ceramic heating element according to claim 1, the thickness that it is characterized in that described lower insulating barrier (4) and upper insulating barrier (2) is 10 ~ 120 μ m.
4. the preparation method of a ceramic heating element claimed in claim 1 is characterized in that preparation process is followed successively by:
(1) prepare respectively the material of heating electrode (3), upper insulating barrier (2) and lower insulating barrier (4), upper ceramic matrix (1) and lower ceramic matrix (6);
(2) printing of layers of material: adopt silk-screen printing technique to print successively lower insulating barrier (4), heating electrode (3), upper insulating barrier (2) on the green compact of lower ceramic matrix (6); The printed layers thickness that wherein descends insulating barrier (4) and upper insulating barrier (2) is 15 ~ 160 μ m; Heating electrode (3) printed layers thickness is 15-25 μ m;
Step 3: superimposed after printing
Green compact by the green compact of step 2 resulting materials and upper ceramic matrix (1), carry out superimposed under the pressure condition of the temperature of 50 ~ 120 ℃ and 10 ~ 60MPa;
Step 4: high temperature sintering
Superimposed body is put into to vacuum degreasing sintering furnace and carry out binder removal degreasing and high temperature sintering, the high temperature sintering temperature is 1350 ~ 1550 ℃, and temperature retention time is 1 ~ 3h;
Step 5: the welding of contact conductor
Adopt soldering processes that heating electrode is connected with lead-in wire, prepare required ceramic heating element.
5. the preparation method of ceramic heating element according to claim 4 is characterized in that:
The preparation method of upper ceramic matrix (1) and lower ceramic matrix (6) is: adopt casting technique to prepare green compact, the thickness of green compact is 0.12 ~ 2.5mm;
The preparation method of heating electrode screen printing sizing agent is: the powder of heating resistor material needed raw material material and the organic carrier that contains adhesive are mixed; The powder of described heating resistor material needed raw material material is 0.6 ~ 1.5:1 with the mass ratio that contains the organic carrier of adhesive;
The preparation method of upper insulating barrier (2) and lower insulating barrier (4) screen printing sizing agent is: the powder of insulating barrier needed raw material material and the organic carrier that contains adhesive are mixed; The powder of described insulating barrier needed raw material material is 0.6 ~ 1.5:1 with the mass ratio that contains the organic carrier of adhesive.
6. a ceramic heating element claimed in claim 1 is as the application of soy bean milk making machine heater block.
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