CN106631011A - Thermosensitive conductive composite ceramic material and preparation method thereof - Google Patents
Thermosensitive conductive composite ceramic material and preparation method thereof Download PDFInfo
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- CN106631011A CN106631011A CN201611112536.8A CN201611112536A CN106631011A CN 106631011 A CN106631011 A CN 106631011A CN 201611112536 A CN201611112536 A CN 201611112536A CN 106631011 A CN106631011 A CN 106631011A
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Abstract
The invention discloses a thermosensitive conductive composite ceramic material and a preparation method thereof. The thermosensitive conductive composite ceramic material is prepared from the following raw materials in parts by weight: 35 to 50 parts of zirconium dioxide ceramic powder, 5 to 9 parts of aggregate, 5 to 10 parts of boron carbide, 5 to 8 parts of magnesium aluminate spinel, 2 to 5 parts of polyvinylidene fluoride, 3 to 6 parts of polyfluortetraethylene, 4 to 7 parts of polyaluminosiloxane, 1 to 3 parts of dilauryl thiodipropionate, 4 to 8 parts of sodium tetraborate, 2 to 4 parts of absolute ethyl alcohol, 1 to 4 parts of polyethylene glycol, 1 to 2 parts of tin dioxide, 1 to 4 parts of copper oxide, 2 to 5 parts of ferric oxide, 2 to 6 parts of calcium hydroxide, 3 to 5 parts of silicon carbide, 1 to 2 parts of antimony trioxide, 1 to 4 parts of antioxidants, 2 to 5 parts of stabilizing agents and 1 to 2 parts of coupling agents. The prepared thermosensitive conductive composite ceramic material has the advantages that the performance is stable; the hardness is high; the temperature-resistant performance and the electric performance are good. Meanwhile, the invention also discloses the corresponding preparation method.
Description
Technical field
The present invention relates to Material Field, is related specifically to a kind of thermo-sensitive conductive composite ceramic material and preparation method thereof.
Background technology
Thermal sensitive ceramics is the ceramic material that a kind of resistance is varied with temperature and changed.Positive temperature coefficient thermal sensitive ceramic generally exists
The resistance ratio of near room temperature is relatively low, after applied voltage.Generated heat rapidly due to low resistance, when temperature rises to certain critical-temperature
（Vicinity of Curie temperatures）, resistance rises to several orders of magnitude, and electric current therefore reduces, and heating and temperature rise weaken again, and temperature is constant Curie
Near point.Between from resistance minimum of a value to maximum, resistance is raised with temperature and linearly increased.Negative temperature coefficient thermosensitive ceramics
Resistance is then raised and linear reduction with temperature.Thermal sensitive ceramics is that current production rate is maximum, most widely used class sensitive material.Just
Temperature coefficient thermistor is used for constant temp. automatic control heater, is widely used in colour TV degaussing component, automatic constant-temperature electric iron, electronics volume
Send out device, motor overheating protection, temperature alarm and temperature compensating element.Negative tempperature coefficient thermistor is used for TEMP
Device, thermo detector, electromagnetic stove, electric cooker etc..
The content of the invention
To solve above-mentioned technical problem, the present invention provides a kind of thermo-sensitive conductive composite ceramic material and preparation method thereof, leads to
Cross and be combined using specified raw material, coordinate corresponding production technology, the thermo-sensitive conductive composite ceramic material for obtaining, its performance is steady
Fixed, hardness height, high temperature resistant, electrical property are good, the requirement of industry are disclosure satisfy that, with preferable application prospect.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of thermo-sensitive conductive composite ceramic material, is prepared by the raw materials in：Zirconia ceramics powder 35-50 part, aggregate
5-9 parts, boron carbide 5-10 parts, magnesium aluminate spinel 5-8 parts, Kynoar 2-5 parts, polytetrafluoroethylene (PTFE) 3-6 parts, polyaluminosiloxane
4-7 parts, thiodipropionic acid dilauryl cinnamic acid ester 1-3 parts, sodium tetraborate 4-8 parts, absolute ethyl alcohol 2-4 parts, polyethylene glycol 1-4 parts, two
Tin oxide 1-2 parts, cupric oxide 1-4 parts, iron oxide 2-5 parts, calcium hydroxide 2-6 parts, carborundum 3-5 parts, antimony oxide 1-2
Part, antioxidant 1-4 parts, stabilizer 2-5 parts, coupling agent 1-2 parts.
Preferably, the antioxidant is 2,2'- methylene bis (4- methyl -6- tert-butyl phenols), 4- hydroxy-dodecanoic acids
One or more in anilid, the t-octyl diphenylamines of 4,4'- bis-, 4- hydroxyoctadecanoic acid anilids.
Preferably, the stabilizer is any one in 2- ethyl acetic acid lead, calcium ricinoleate, zinc stearate, orange osmanthus acid barium
Kind.
Preferably, the coupling agent is selected from three iso stearate isopropyl titanates, isopropyl three（Dioctyl pyrophosphoryl base) titanium
Acid esters, two (dioctyl pyrophosphoryl bases) close any in fluoroacetic acid ester titanium, isopropyl three (positive ethylamino-ethylamino) titanate esters
One or more.
The preparation method of described thermo-sensitive conductive composite ceramic material, comprises the following steps：
（1）Each raw material is weighed according to weight portion；
（2）Zirconia ceramics powder, aggregate, boron carbide, magnesium aluminate spinel are added and is ground in raymond mill, flour mill work(
Rate is 22KW, and mixture granularity is 200-300 mesh;
（3）By polytetrafluoroethylene (PTFE), polyaluminosiloxane, tin ash, cupric oxide, iron oxide, calcium hydroxide, carborundum, three oxidations
Two antimony, antioxidant, step（2）Mixture of powders add together hot test electric furnace sinter, by the high temperature sintering thing for obtaining
Water quenching, cooling obtains ceramic block, and high temperature sintering temperature is 550-650 DEG C, and the high temperature sintering time is 20-30 minutes；
（4）By step（3）Ceramic block, sodium tetraborate, absolute ethyl alcohol, polyethylene glycol add the ball mill, pellet ratio to be together
1：5, Ball-milling Time is 3-5 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture；
（6）By step（5）The mixture that sieves, Kynoar, thiodipropionic acid dilauryl cinnamic acid ester, stabilizer, coupling agent note
Enter in high pressure homogenizer and stir, 1000-1500 rev/min of rotating speed, pressure is 0.5-1MPa, mix 15-25 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is solid in 4-10 DEG C of nitrogen incubator
Calmly, degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered shaping, calcining heat is 850-900 DEG C, very
Pneumatics is by force 0.2-0.5Pa, and the vacuum-sintering time is 60-90 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen incubators and conserve 2-
4 hours, get product.
Preferably, the condition of the water quenching is：Enter coolant-temperature gage for 10-15 DEG C, the water quenching time is 45 seconds.
Preferably, the mesh size is 200 mesh.
Compared with prior art, its advantage is the present invention：
（1）The thermo-sensitive conductive composite ceramic material of the present invention, with zirconia ceramics powder, aggregate, boron carbide, magnesium aluminate spinel, poly-
Tetrafluoroethene, polyaluminosiloxane, tin ash, cupric oxide, iron oxide, calcium hydroxide, carborundum, antimony oxide for it is main into
Point, by adding sodium tetraborate, absolute ethyl alcohol, polyethylene glycol, Kynoar, thiodipropionic acid dilauryl cinnamic acid ester, anti-oxidant
Agent, stabilizer, coupling agent, are aided with mechanical crushing, high temperature sintering, Water Quenching, ball milling sorting, the homogeneous, mold that pressurizes and fix, very
The techniques such as sky calcining, mould from dewaxing, maintenance shaping so that the thermo-sensitive conductive composite ceramic material being prepared from, its stable performance,
Hardness height, high temperature resistant, electrical property are good, the requirement of industry are disclosure satisfy that, with preferable application prospect.
（2）The thermo-sensitive conductive composite ceramic material raw material of the present invention is cheap, process is simple, is suitable to heavy industrialization fortune
With practical.
Specific embodiment
The technical scheme invented is described in detail with reference to specific embodiment.
Embodiment 1
（1）35 parts of zirconia ceramics powder, 5 parts of aggregate, 5 parts of boron carbide, 5 parts of magnesium aluminate spinel, poly- inclined fluorine are weighed according to weight portion
It is 2 parts of ethene, 3 parts of polytetrafluoroethylene (PTFE), 4 parts of polyaluminosiloxane, 1 part of thiodipropionic acid dilauryl cinnamic acid ester, 4 parts of sodium tetraborate, anhydrous
2 parts of ethanol, 1 part of polyethylene glycol, 1 part of tin ash, 1 part of cupric oxide, 2 parts of iron oxide, 2 parts of calcium hydroxide, 3 parts of carborundum, three
Aoxidize 1 part of two antimony, 1 part of 2,2'- methylene bis (4- methyl -6- tert-butyl phenols), 2 parts of 2- ethyl acetic acids lead, three iso stearates
1 part of isopropyl titanate；
（2）Zirconia ceramics powder, aggregate, boron carbide, magnesium aluminate spinel are added and is ground in raymond mill, flour mill work(
Rate is 22KW, and mixture granularity is 200-300 mesh;
（3）By polytetrafluoroethylene (PTFE), polyaluminosiloxane, tin ash, cupric oxide, iron oxide, calcium hydroxide, carborundum, three oxidations
Two antimony, 2,2'- methylene bis (4- methyl -6- tert-butyl phenols), step（2）Mixture of powders add together hot test electricity
Stove is sintered, and by the high temperature sintering thing water quenching for obtaining, cooling obtains ceramic block, and high temperature sintering temperature is 550 DEG C, the high temperature sintering time
For 20 minutes, water quenching entered coolant-temperature gage for 10 DEG C, and the water quenching time is 45 seconds；
（4）By step（3）Ceramic block, sodium tetraborate, absolute ethyl alcohol, polyethylene glycol add the ball mill, pellet ratio to be together
1：5, Ball-milling Time is 3 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture, and mesh size is 200 mesh；
（6）By step（5）The mixture that sieves, Kynoar, thiodipropionic acid dilauryl cinnamic acid ester, 2- ethyl acetic acid lead, three
Stir in iso stearate isopropyl titanate injection high pressure homogenizer, 1000 revs/min of rotating speed, pressure is 0.5MPa, mixing
Stirring 15 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is fixed in 4 DEG C of nitrogen incubators,
Degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered shaping, calcining heat is 850 DEG C, vacuum pressure
It is by force 0.2Pa, the vacuum-sintering time is 60 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen incubators and conserve 2
Hour, get product.
The performance test results of obtained thermo-sensitive conductive composite ceramic material are as shown in table 1.
Embodiment 2
（1）40 parts of zirconia ceramics powder, 6 parts of aggregate, 7 parts of boron carbide, 6 parts of magnesium aluminate spinel, poly- inclined fluorine are weighed according to weight portion
It is 3 parts of ethene, 4 parts of polytetrafluoroethylene (PTFE), 5 parts of polyaluminosiloxane, 1 part of thiodipropionic acid dilauryl cinnamic acid ester, 5 parts of sodium tetraborate, anhydrous
3 parts of ethanol, 2 parts of polyethylene glycol, 1 part of tin ash, 2 parts of cupric oxide, 3 parts of iron oxide, 3 parts of calcium hydroxide, 4 parts of carborundum, three
Aoxidize 1 part of two antimony, 2 parts of 4- hydroxy-dodecanoic acids anilid, 3 parts of calcium ricinoleate, isopropyl three（Dioctyl pyrophosphoryl base) titanium
1 part of acid esters；
（2）Zirconia ceramics powder, aggregate, boron carbide, magnesium aluminate spinel are added and is ground in raymond mill, flour mill work(
Rate is 22KW, and mixture granularity is 250 mesh;
（3）By polytetrafluoroethylene (PTFE), polyaluminosiloxane, tin ash, cupric oxide, iron oxide, calcium hydroxide, carborundum, three oxidations
Two antimony, 4- hydroxy-dodecanoic acid anilids, step（2）Mixture of powders add together hot test electric furnace sinter, will
The high temperature sintering thing water quenching arrived, cooling obtains ceramic block, and high temperature sintering temperature is 580 DEG C, and the high temperature sintering time is 23 minutes, water
It is 12 DEG C to quench into coolant-temperature gage, and the water quenching time is 45 seconds；
（4）By step（3）Ceramic block, sodium tetraborate, absolute ethyl alcohol, polyethylene glycol add the ball mill, pellet ratio to be together
1：5, Ball-milling Time is 3.5 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture, and mesh size is 200 mesh；
（6）By step（5）The mixture that sieves, Kynoar, thiodipropionic acid dilauryl cinnamic acid ester, calcium ricinoleate, isopropyl
Three（Dioctyl pyrophosphoryl base) stir in titanate esters injection high pressure homogenizer, 1200 revs/min of rotating speed, pressure is
0.7MPa, mixes 18 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is fixed in 6 DEG C of nitrogen incubators,
Degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered shaping, calcining heat is 860 DEG C, vacuum pressure
It is by force 0.3Pa, the vacuum-sintering time is 70 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen incubators conserve
2.5 hours, get product.
The performance test results of obtained thermo-sensitive conductive composite ceramic material are as shown in table 1.
Embodiment 3
（1）45 parts of zirconia ceramics powder, 8 parts of aggregate, 9 parts of boron carbide, 7 parts of magnesium aluminate spinel, poly- inclined fluorine are weighed according to weight portion
It is 4 parts of ethene, 5 parts of polytetrafluoroethylene (PTFE), 6 parts of polyaluminosiloxane, 2 parts of thiodipropionic acid dilauryl cinnamic acid ester, 7 parts of sodium tetraborate, anhydrous
3 parts of ethanol, 3 parts of polyethylene glycol, 2 parts of tin ash, 3 parts of cupric oxide, 4 parts of iron oxide, 5 parts of calcium hydroxide, 4 parts of carborundum, three
Aoxidize 2 parts of two antimony, 3 parts of 4,4'-, bis- t-octyl diphenylamines, 4 parts of zinc stearate, two (dioctyl pyrophosphoryl bases) and close fluoroacetic acid ester titanium
2 parts；
（2）Zirconia ceramics powder, aggregate, boron carbide, magnesium aluminate spinel are added and is ground in raymond mill, flour mill work(
Rate is 22KW, and mixture granularity is 250 mesh;
（3）By polytetrafluoroethylene (PTFE), polyaluminosiloxane, tin ash, cupric oxide, iron oxide, calcium hydroxide, carborundum, three oxidations
Two antimony, the t-octyl diphenylamines of 4,4'- bis-, step（2）Mixture of powders add together hot test electric furnace sinter, by what is obtained
High temperature sintering thing water quenching, cooling obtains ceramic block, and high temperature sintering temperature is 620 DEG C, and the high temperature sintering time is 27 minutes, and water quenching enters
Coolant-temperature gage is 14 DEG C, and the water quenching time is 45 seconds；
（4）By step（3）Ceramic block, sodium tetraborate, absolute ethyl alcohol, polyethylene glycol add the ball mill, pellet ratio to be together
1：5, Ball-milling Time is 4 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture, and mesh size is 200 mesh；
（6）By step（5）The mixture that sieves, Kynoar, thiodipropionic acid dilauryl cinnamic acid ester, zinc stearate, two (two is pungent
Base pyrophosphoryl base) close and stirred in fluoroacetic acid ester titanium injection high pressure homogenizer, 1400 revs/min of rotating speed, pressure is 0.9MPa,
Mix 22 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is fixed in 8 DEG C of nitrogen incubators,
Degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered shaping, calcining heat is 880 DEG C, vacuum pressure
It is by force 0.4Pa, the vacuum-sintering time is 80 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen incubators and conserve 3
Hour, get product.
The performance test results of obtained thermo-sensitive conductive composite ceramic material are as shown in table 1.
Embodiment 4
（1）50 parts of zirconia ceramics powder, 9 parts of aggregate, 10 parts of boron carbide, 8 parts of magnesium aluminate spinel, poly- inclined fluorine are weighed according to weight portion
It is 5 parts of ethene, 6 parts of polytetrafluoroethylene (PTFE), 7 parts of polyaluminosiloxane, 3 parts of thiodipropionic acid dilauryl cinnamic acid ester, 8 parts of sodium tetraborate, anhydrous
4 parts of ethanol, 4 parts of polyethylene glycol, 2 parts of tin ash, 4 parts of cupric oxide, 5 parts of iron oxide, 6 parts of calcium hydroxide, 5 parts of carborundum, three
Aoxidize 2 parts of two antimony, 4 parts of 4- hydroxyoctadecanoic acids anilid, orange osmanthus 5 parts of barium of acid, isopropyl three (positive ethylamino-ethylamino)
2 parts of titanate esters；
（2）Zirconia ceramics powder, aggregate, boron carbide, magnesium aluminate spinel are added and is ground in raymond mill, flour mill work(
Rate is 22KW, and mixture granularity is 300 mesh;
（3）By polytetrafluoroethylene (PTFE), polyaluminosiloxane, tin ash, cupric oxide, iron oxide, calcium hydroxide, carborundum, three oxidations
Two antimony, 4- hydroxyoctadecanoic acid anilids, step（2）Mixture of powders add together hot test electric furnace sinter, will
The high temperature sintering thing water quenching arrived, cooling obtains ceramic block, and high temperature sintering temperature is 650 DEG C, and the high temperature sintering time is 30 minutes, water
It is 15 DEG C to quench into coolant-temperature gage, and the water quenching time is 45 seconds；
（4）By step（3）Ceramic block, sodium tetraborate, absolute ethyl alcohol, polyethylene glycol add the ball mill, pellet ratio to be together
1：5, Ball-milling Time is 5 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture, and mesh size is 200 mesh；
（6）By step（5）The mixture that sieves, Kynoar, thiodipropionic acid dilauryl cinnamic acid ester, orange osmanthus acid barium, isopropyl
Three (positive ethylamino-ethylamino) titanate esters are injected and are stirred in high pressure homogenizer, 1500 revs/min of rotating speed, and pressure is
1MPa, mixes 25 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is solid in 10 DEG C of nitrogen incubators
Calmly, degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered shaping, calcining heat is 900 DEG C, vacuum pressure
It is by force 0.5Pa, the vacuum-sintering time is 90 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen incubators and conserve 4
Hour, get product.
The performance test results of obtained thermo-sensitive conductive composite ceramic material are as shown in table 1.
Comparative example 1
（1）35 parts of zirconia ceramics powder, 5 parts of aggregate, 5 parts of magnesium aluminate spinel, 2 parts of Kynoar, poly- is weighed according to weight portion
It is 3 parts of tetrafluoroethene, 4 parts of polyaluminosiloxane, 1 part of thiodipropionic acid dilauryl cinnamic acid ester, 4 parts of sodium tetraborate, 2 parts of absolute ethyl alcohol, poly-
1 part of ethylene glycol, 1 part of tin ash, 1 part of cupric oxide, 2 parts of calcium hydroxide, 3 parts of carborundum, 1 part of antimony oxide, 2,2'- first
1 part of support double (4- methyl -6- tert-butyl phenols), 2 parts of 2- ethyl acetic acids lead, 1 part of three iso stearate isopropyl titanate；
（2）Zirconia ceramics powder, aggregate, magnesium aluminate spinel are added and is ground in raymond mill, milling acc power is
22KW, mixture granularity is 200-300 mesh;
（3）By polytetrafluoroethylene (PTFE), polyaluminosiloxane, tin ash, cupric oxide, calcium hydroxide, carborundum, antimony oxide, 2,
2'- methylene bis (4- methyl -6- tert-butyl phenols), step（2）Mixture of powders add together hot test electric furnace sinter,
By the high temperature sintering thing water quenching for obtaining, cooling obtains ceramic block, and high temperature sintering temperature is 550 DEG C, and the high temperature sintering time is 20 points
Clock, water quenching enters coolant-temperature gage for 10 DEG C, and the water quenching time is 45 seconds；
（4）By step（3）Ceramic block, sodium tetraborate, absolute ethyl alcohol, polyethylene glycol add the ball mill, pellet ratio to be together
1：5, Ball-milling Time is 3 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture, and mesh size is 200 mesh；
（6）By step（5）The mixture that sieves, Kynoar, thiodipropionic acid dilauryl cinnamic acid ester, 2- ethyl acetic acid lead, three
Stir in iso stearate isopropyl titanate injection high pressure homogenizer, 1000 revs/min of rotating speed, pressure is 0.5MPa, mixing
Stirring 15 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is fixed in 4 DEG C of nitrogen incubators,
Degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered shaping, calcining heat is 850 DEG C, vacuum pressure
It is by force 0.2Pa, the vacuum-sintering time is 60 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen incubators and conserve 2
Hour, get product.
The performance test results of obtained thermo-sensitive conductive composite ceramic material are as shown in table 1.
Comparative example 2
（1）50 parts of zirconia ceramics powder, 9 parts of aggregate, 10 parts of boron carbide, 8 parts of magnesium aluminate spinel, poly- inclined fluorine are weighed according to weight portion
5 parts of ethene, 6 parts of polytetrafluoroethylene (PTFE), 7 parts of polyaluminosiloxane, 3 parts of thiodipropionic acid dilauryl cinnamic acid ester, 4 parts of absolute ethyl alcohol, poly- second
4 parts of glycol, 5 parts of iron oxide, 6 parts of calcium hydroxide, 5 parts of carborundum, 2 parts of antimony oxide, 4- hydroxyoctadecanoic acid anilids
4 parts, orange osmanthus acid 5 parts of barium, isopropyl three (positive ethylamino-ethylamino) 2 parts of titanate esters；
（2）Zirconia ceramics powder, aggregate, boron carbide, magnesium aluminate spinel are added and is ground in raymond mill, flour mill work(
Rate is 22KW, and mixture granularity is 300 mesh;
（3）By polytetrafluoroethylene (PTFE), polyaluminosiloxane, iron oxide, calcium hydroxide, carborundum, antimony oxide, 4- hydroxyoctadecanoics
Sour anilid, step（2）Mixture of powders add together hot test electric furnace sinter, by the high temperature sintering thing water for obtaining
Quench, cooling obtains ceramic block, high temperature sintering temperature is 650 DEG C, and the high temperature sintering time is 30 minutes, and water quenching enters coolant-temperature gage for 15
DEG C, the water quenching time is 45 seconds；
（4）By step（3）Ceramic block, absolute ethyl alcohol, polyethylene glycol add ball mill together, pellet ratio is 1：5, during ball milling
Between be 5 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture, and mesh size is 200 mesh；
（6）By step（5）The mixture that sieves, Kynoar, thiodipropionic acid dilauryl cinnamic acid ester, orange osmanthus acid barium, isopropyl
Three (positive ethylamino-ethylamino) titanate esters are injected and are stirred in high pressure homogenizer, 1500 revs/min of rotating speed, and pressure is
1MPa, mixes 25 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is solid in 10 DEG C of nitrogen incubators
Calmly, degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered shaping, calcining heat is 900 DEG C, vacuum pressure
It is by force 0.5Pa, the vacuum-sintering time is 90 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen incubators and conserve 4
Hour, get product.
The performance test results of obtained thermo-sensitive conductive composite ceramic material are as shown in table 1.
The obtained thermo-sensitive conductive composite ceramic material of embodiment 1-4 and comparative example 1-2 is carried out into resistivity, bending resistance strong
Degree, hardness, this several performance tests of thermal conductivity.
Table 1
| Resistivity（Ω.cm） | Bending strength, Mpa | Hardness, HV | Thermal conductivity（W/m.K） | |
| Embodiment 1 | 2.92*106 | 1027 | 2390 | 136.2 |
| Embodiment 2 | 2.87*106 | 1069 | 2339 | 135.5 |
| Embodiment 3 | 2.79*106 | 1038 | 2370 | 137.9 |
| Embodiment 4 | 2.82*106 | 1048 | 2401 | 138.4 |
| Comparative example 1 | 7.87*106 | 661 | 1767 | 87.3 |
| Comparative example 2 | 6.31*106 | 755 | 1912 | 95.6 |
The thermo-sensitive conductive composite ceramic material of the present invention, with zirconia ceramics powder, aggregate, boron carbide, magnesium aluminate spinel, polytetrafluoro
Ethene, polyaluminosiloxane, tin ash, cupric oxide, iron oxide, calcium hydroxide, carborundum, antimony oxide are main component,
By add sodium tetraborate, absolute ethyl alcohol, polyethylene glycol, Kynoar, thiodipropionic acid dilauryl cinnamic acid ester, antioxidant,
Stabilizer, coupling agent, be aided with mechanical crushing, high temperature sintering, Water Quenching, ball milling sorting, the homogeneous, mold that pressurizes fix, vacuum
The techniques such as calcining, mould from dewaxing, maintenance shaping so that the thermo-sensitive conductive composite ceramic material being prepared from, it is its stable performance, hard
Degree height, high temperature resistant, electrical property are good, the requirement of industry are disclosure satisfy that, with preferable application prospect.The thermo-sensitive conductive of the present invention
Composite ceramic material raw material is cheap, process is simple, is suitable to heavy industrialization utilization, practical.
Embodiments of the invention are the foregoing is only, the scope of the claims of the present invention is not thereby limited, it is every using this
Equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, is included within the scope of the present invention.
Claims (7)
1. a kind of thermo-sensitive conductive composite ceramic material, it is characterised in that：It is prepared by the raw materials in：Zirconia ceramics powder
35-50 parts, aggregate 5-9 parts, boron carbide 5-10 parts, magnesium aluminate spinel 5-8 parts, Kynoar 2-5 parts, polytetrafluoroethylene (PTFE) 3-6
Part, polyaluminosiloxane 4-7 parts, thiodipropionic acid dilauryl cinnamic acid ester 1-3 parts, sodium tetraborate 4-8 parts, absolute ethyl alcohol 2-4 parts, poly- second
Glycol 1-4 parts, tin ash 1-2 parts, cupric oxide 1-4 parts, iron oxide 2-5 parts, calcium hydroxide 2-6 parts, carborundum 3-5 parts, three
Aoxidize two antimony 1-2 parts, antioxidant 1-4 parts, stabilizer 2-5 parts, coupling agent 1-2 parts.
2. thermo-sensitive conductive composite ceramic material according to claim 1, it is characterised in that：The antioxidant is 2,2'-
Methylene bis (4- methyl -6- tert-butyl phenols), 4- hydroxy-dodecanoic acid anilids, the t-octyl diphenylamines of 4,4'- bis-, 4- hydroxyls
One or more in base octadecanoid acid anilid.
3. thermo-sensitive conductive composite ceramic material according to claim 1, it is characterised in that：The stabilizer is 2- ethyl second
Any one in lead plumbate, calcium ricinoleate, zinc stearate, orange osmanthus acid barium.
4. thermo-sensitive conductive composite ceramic material according to claim 1, it is characterised in that：The coupling agent is different hard selected from three
Ester acid isopropyl titanate, isopropyl three（Dioctyl pyrophosphoryl base) titanate esters, two (dioctyl pyrophosphoryl bases) close fluoroacetic acid ester titanium,
Any one or a few in isopropyl three (positive ethylamino-ethylamino) titanate esters.
5. according to the preparation method of the arbitrary described thermo-sensitive conductive composite ceramic material of claim 1-4, it is characterised in that include
Following steps：
（1）Each raw material is weighed according to weight portion；
（2）Zirconia ceramics powder, aggregate, boron carbide, magnesium aluminate spinel are added and is ground in raymond mill, flour mill work(
Rate is 22KW, and mixture granularity is 200-300 mesh;
（3）By polytetrafluoroethylene (PTFE), polyaluminosiloxane, tin ash, cupric oxide, iron oxide, calcium hydroxide, carborundum, three oxidations
Two antimony, antioxidant, step（2）Mixture of powders add together hot test electric furnace sinter, by the high temperature sintering thing for obtaining
Water quenching, cooling obtains ceramic block, and high temperature sintering temperature is 550-650 DEG C, and the high temperature sintering time is 20-30 minutes；
（4）By step（3）Ceramic block, sodium tetraborate, absolute ethyl alcohol, polyethylene glycol add the ball mill, pellet ratio to be together
1：5, Ball-milling Time is 3-5 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture；
（6）By step（5）The mixture that sieves, Kynoar, thiodipropionic acid dilauryl cinnamic acid ester, stabilizer, coupling agent note
Enter in high pressure homogenizer and stir, 1000-1500 rev/min of rotating speed, pressure is 0.5-1MPa, mix 15-25 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is solid in 4-10 DEG C of nitrogen incubator
Calmly, degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered shaping, calcining heat is 850-900 DEG C, very
Pneumatics is by force 0.2-0.5Pa, and the vacuum-sintering time is 60-90 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen incubators and conserve 2-
4 hours, get product.
6. the preparation method of thermo-sensitive conductive composite ceramic material according to claim 5, it is characterised in that the step
（3）In, the condition of water quenching is：Enter coolant-temperature gage for 10-15 DEG C, the water quenching time is 45 seconds.
7. the preparation method of thermo-sensitive conductive composite ceramic material according to claim 5, it is characterised in that the step
（5）In, mesh size is 200 mesh.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108218291A (en) * | 2018-02-02 | 2018-06-29 | 付主枝 | A kind of preparation method for the bioceramic material for adulterating dicalcium silicate nano powder |
| CN113880555A (en) * | 2021-11-23 | 2022-01-04 | 景德镇市苏氏瓷业有限公司 | Preparation method of blue and white ceramic |
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| CN102682942A (en) * | 2012-06-04 | 2012-09-19 | 句容市博远电子有限公司 | Thermistor with low resistance value, high B value and negative temperature coefficient |
| CN103578675A (en) * | 2012-07-27 | 2014-02-12 | 苏州星火电子科技有限公司 | Making method of NTC thermo-sensitive resistor |
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| JPS62230006A (en) * | 1986-03-31 | 1987-10-08 | 松下電器産業株式会社 | Temperature sensitive resistance element |
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| CN108218291A (en) * | 2018-02-02 | 2018-06-29 | 付主枝 | A kind of preparation method for the bioceramic material for adulterating dicalcium silicate nano powder |
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