A kind of preparation method of porous ceramics positive temperature coefficient thermistor
Technical field
The present invention relates to preparation method of a kind of porous ceramics positive temperature coefficient thermistor and products thereof, relate in particular to the preparation method for the ceramic positive temperature coefficient thermosensitive resistor of overcurrent protection series.
Background technology
Ceramic positive temperature coefficient thermosensitive resistor (abbreviation ceramic PTC) is widely used in overcurrent, overvoltage, the overheat protector field of electronic circuit owing to its good self-healing. But because the restriction of material itself, ceramic PTC is very easy to produce when bearing high voltage, large current cycle and lost efficacy, and concrete failure characteristics is: zero power resistance raises or the element cracking. Cause the main cause of these two kinds of failure characteristics to be: element generates heat rapidly when bearing heavy current impact, cause material to pass through fast its Curie's warm area, because larger change in volume occurs in material when passing through curie point, and because the heat conduction factor of material causes inside and outside non-uniform temperature, whole element produces huge stress when passing through curie point. Ceramic material itself is fragile material, and huge stress makes material internal produce trickle crackle. Under heavy current impact repeatedly, crackle is expanded gradually, until ceramics splits, the gross feature of this inefficacy is exactly that resistance raises gradually until the element cracking. Therefore, existing ceramic PTC haves much room for improvement.
Summary of the invention
In order to overcome defects, the object of the present invention is to provide a kind of new ceramic PTC preparation method, the ceramic PTC that makes in this way can suppress the expansion of crackle, thereby improves the anti-high current surge withstanding capability of ceramic PTC.
The present invention is achieved through the following technical solutions: a kind of preparation method of porous ceramics positive temperature coefficient thermistor, with the raw material of preparation pottery prepare burden in proportion, after the grinding, pre-burning, carry out again carrying out batch mixing after second batch namely adds the carbon black of 0.1-10%, add simultaneously surfactant, make it to mix, granulation after the oven dry, compacting, sinter molding, form ceramics, the ceramics of making by said method, owing to mixed a large amount of carbon blacks, when sintering, can produce a large amount of pores and reducing atmosphere, cause the PTC effect of ceramics significantly to reduce, withstand voltage properties worsens, and therefore needs above-mentioned ceramics is carried out re-oxidation in air, is namely made the porous ceramics PTC of anti-heavy current impact by good electrode.
The particle size range of wherein said carbon black is 10-200 μ m.
Wherein said mixing method refers to ball milling method or agitating mode.
Wherein said re-oxidation temperature is 600-1200 ℃, and the time is 0.5-24 hour.
According to the prepared porous ceramics PTC of the inventive method, structure is cellular, and the diameter of its hole is 3-15 times of crystal grain diameter, and this structure can well suppress the expansion of crackle, thereby improves the performance of the anti-heavy current impact of ceramic PTC.
The advantage of the preparation method of a kind of porous ceramics positive temperature coefficient thermistor of the present invention is: owing to add a certain proportion of carbon black in manufacturing process, when sintering, can produce a large amount of pores, and the uniformity of hole is fine, this structure can well suppress the expansion of crackle, thereby improve the anti-high current surge withstanding capability of ceramic PTC, can bear the circulation impact of high voltage, large electric current.
Description of drawings
Accompanying drawing is process chart of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing of the present invention process chart of the present invention, specify the present invention and how to realize:
Embodiment 1
The raw material of preparation pottery is prepared burden in proportion, ball milling, pre-burning, carried out second batch again and namely add the carbon black that the 0.5wt% particle diameter is 50 μ m, the n-butanol that adds simultaneously 1wt%, take ball milling method to carry out batch mixing, make it to mix, granulation after the oven dry, compacting, sinter molding under 1350C, form ceramics, with ceramics re-oxidation in 1000 ℃ air, oxidization time is to be made ceramic PTC by good electrode again in 1 hour.
The properties of product of testing, method of testing and testing equipment see Table shown in (1); The ceramics that the inventive method makes is cooked same test with carbon dope is not black with the ceramics that does not carry out re-oxidation, and comparative result sees Table shown in (2).
Table (1):
Properties of product | Method of testing | Testing equipment |
Zero power resistance | To in 25 ± 2 ℃ environment, be placed one by the later ceramics of good electrode and as a child measure its resistance. Measure altogether 50, calculate its average electrical resistance. | The zero power resistance table |
Lift-drag ratio | Measure the R-T curve of 10 ceramics, get the resistance calculations lift-drag ratio of its highest electricity and minimum point, calculate its mean value. | Resistance temperature (R-T) curve tester |
Anti-rush of current | Voltage 650Vac, electric current 1.1A kept 1 second, had a rest 1 minute, circulated 20 times. Survey altogether 50. Test rear placement measuring resistance after 1 hour, before repetition measurement resistance and the test | The anti-current tester of PTC thermistor |
| Resistance differs and is no more than ± and 10%, otherwise for losing efficacy. | |
High withstand voltage | 600V, 1A kept 5 minutes, and every 5 minutes boosted voltage 20V, until till ceramics burns, record burnt the high withstand voltage that former test voltage is ceramics. | PTC thermistor withstands voltage tester |
Table (2):
Properties of product | Test result |
Process to get ceramics without the present invention | Process to get ceramics through the present invention |
Zero power resistance |
50.55Ω
|
51.32Ω
|
Lift-drag ratio |
7.22
|
7.09
|
Anti-rush of current | 36 inefficacies | 50 complete good |
High withstand voltage |
920V
|
920V
|
Embodiment 2:
The raw material of preparation pottery is prepared burden in proportion, ball milling, pre-burning, carried out second batch again and namely add the carbon black that the 5wt% particle diameter is 50 μ m, the n-butanol that adds simultaneously 2wt%, take to stir the mill mode and carry out batch mixing, make it to mix, granulation, compacting after the oven dry, 1320 ℃ of lower sinter moldings, form ceramics, with ceramics re-oxidation in 1100 ℃ air, oxidization time is 5 hours, is made ceramic PTC by good electrode again.
The properties of product of testing, method of testing and testing equipment see Table shown in (3); To do same test with carbon dope is not black with the ceramics that does not carry out re-oxidation according to the ceramics that the inventive method makes, comparative result sees Table shown in (4).
Table (3):
Properties of product | Method of testing | Testing equipment |
Zero power resistance | To in 25 ± 2 ℃ environment, be placed one by the later ceramics of good electrode and as a child measure its resistance. Measure altogether 50, calculate its average electrical resistance. | The zero power resistance table |
Lift-drag ratio | Measure the R-T curve of 10 ceramics, get the resistance calculations lift-drag ratio of its highest electricity and minimum point, calculate its mean value. | Resistance temperature (R-T) curve tester |
Anti-rush of current | Voltage 250Vac, electric current 3A kept 1 minute, had a rest 10 minutes, circulated 20 times. Survey altogether 50. Test rear placement measuring resistance after 1 hour, before repetition measurement resistance and the test resistance differ be no more than ± 10%, otherwise for losing efficacy. | The anti-current tester of PTC thermistor |
High withstand voltage | 200V, 1A kept 5 minutes, and every 5 minutes boosted voltage 20V, until till ceramics burns, record burnt the high withstand voltage that former test voltage is ceramics. | PTC thermistor withstands voltage tester |
Table (4)
Properties of product | Test result |
Process to get ceramics without the present invention | Process to get ceramics through the present invention |
Zero power resistance |
10.23Ω
|
10.45Ω
|
Lift-drag ratio |
6.89
|
6.93
|
Anti-rush of current | 45 inefficacies | 50 complete good |
High withstand voltage |
520V
|
540V
|