CN102627445B - Composition for preparing negative temperature coefficient (NTC) thermistor chip and NTC thermistor made by using composition - Google Patents
Composition for preparing negative temperature coefficient (NTC) thermistor chip and NTC thermistor made by using composition Download PDFInfo
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- CN102627445B CN102627445B CN 201210126551 CN201210126551A CN102627445B CN 102627445 B CN102627445 B CN 102627445B CN 201210126551 CN201210126551 CN 201210126551 CN 201210126551 A CN201210126551 A CN 201210126551A CN 102627445 B CN102627445 B CN 102627445B
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Abstract
The invention discloses a composition for preparing a negative temperature coefficient (NTC) thermistor chip and an NTC thermistor made by using the composition, belonging to the field of thermistors. The composition comprises the following components in parts by weight: 590-610 parts of Mn3O4, 13-15 parts of Co3O4, 105-115 parts of Fe2O3, 15-17 parts of SiO2 and 260-265 parts of NiO, wherein all components are nano-powder and are chemically pure. The composition is made into chip slurry through the following steps of: weighing the raw materials according to the components and the content; evenly mixing the raw materials, pouring the mixture into a ball mill, adding water and grinding for 30-50 hours; dewatering and drying the ground raw materials; and adding adhesive into the dried raw materials and evenly agitating to form the chip slurry. The invention additionally discloses a method for making the NTC thermistor by using the chip slurry. By adjusting the proportions of all components in the combination for the NTC thermistor, the service life of the thermistor is prolonged, the measurement accuracy of the thermistor is improved and the NTC thermistor is suitable for the field of high-temperature equipment such as water heaters.
Description
Technical field
The present invention relates to the thermistor field, the NTC thermistor of the chip that particularly a kind of composition for the preparation of the NTC thermistor chip and use said composition are made.
Background technology
Thermistor is a class of senser, be divided into PTC (Positive Temperature Coefficient according to the temperature coefficient difference, positive temperature coefficient) thermistor and NTC (Negative Temperature CoeffiCient, negative temperature coefficient) thermistor.The typical feature of thermistor is to responsive to temperature, shows different resistance values at different temperature.PTC thermistor resistance value when temperature is higher is larger, and NTC thermistor resistance value when temperature is higher is lower, and they belong to semiconductor device.
That the NTC thermistor has is highly sensitive, fast response time, volume are little, be easy to realize the advantages such as far distance controlled and measurement, is widely used in the fields such as refrigerator, air-conditioning, electric heater, integral bathroom, electronic calendar, microwave oven, barn temperature measuring, dishwasher, electric cooker, electronics toilet facility, refrigerator-freezer, soy bean milk making machine, battery of mobile phone, charger, electromagnetic oven, bread producing machine, disinfection cabinet, water dispenser, temperature control instrument, Medical Instruments, automobile thermometric, roaster, fire alarm.
In realizing process of the present invention, the inventor finds that at least there is following problem in prior art: the impact that NTC thermistor is in the market changed by the chip material property in use, easily produce aging drift, affect its useful life and certainty of measurement, while especially at high temperature working, easily produce resistance and export unstable phenomenon; Due to chip thickness and density inadequate, repeatedly when the electric current, the easy breakdown inefficacy of chip.
Summary of the invention
In order to solve the problem of prior art, the embodiment of the present invention provides a kind of composition for the NTC thermistor chip and has used the resistance of this chip.Described technical scheme is as follows:
On the one hand, the invention provides a kind of composition for the preparation of the NTC thermistor chip, the component wherein comprised and content thereof are:
Above each component is nano-powder, and purity is chemical pure,
And make the chip slurry by above-mentioned composition by following step:
(1) take raw material according to said components and content;
(2) pour ball mill into after described raw material is mixed, add water, grinding 30-50 hour;
(3) the described raw material after grinding is carried out to dewatered drying;
(4) in the described raw material after oven dry, add adhesive to stir, form the chip slurry.
Preferably, the component wherein comprised and content thereof are:
On the other hand, the invention provides a kind of method of the chip manufacturing NTC thermistor made from above-mentioned composition, said method comprising the steps of:
(1) component and the content according to above-mentioned composition takes raw material;
(2) pour ball mill into after described raw material is mixed, add water, grinding 30-50 hour;
(3) the described raw material after grinding is carried out to dewatered drying;
(4) in the described raw material after oven dry, add adhesive to stir, form the chip slurry;
(5) described chip slurry is pressed into to thin slice;
(6) described thin slice is polished, formed ganoid embryo sheet;
(7) by described embryo sheet 1290-1310 ℃ of lower high temperature sintering 48 hours, form potsherd;
(8) give described potsherd coated on both sides silver slurry, make electrode;
(9) require to cut the described potsherd that has adhered to silver-colored slurry according to resistance, obtain electroded NTC thermistor chip;
(10) give described electroded NTC thermistor chip welding lead, make the NTC thermistor.Wherein:
After step (10) is made the NTC thermistor, also comprise:
By the powder impregnator, go up the epoxy resin rubber powder to the chip of described NTC thermistor and wire bonds point parcel dipping, 150 ℃ of lower baking-curings 2 hours, make the NTC thermistor of epoxy encapsulation.
Described in the step (4) that said chip slurry and NTC thermistor are made, adhesive is dibutyl phthalate and polyvinyl alcohol milky white adhesive, its concrete operations comprise: in the described raw material after oven dry, add dibutyl phthalate and polyvinyl alcohol milky white adhesive to stir, form the chip slurry, the weight of wherein said dibutyl phthalate is 4% of the described raw material weight after drying, and the weight of described polyvinyl alcohol milky white adhesive is 1.5% of the described raw material weight after drying.
Step (5), (6) specifically comprise: by Multi-step forming-dry and Multi-step forming subsequently-bake operation, described chip slurry is pressed into to the thin slice that 0.6-0.7mm is thick; By sander, described thin slice is polished into to the ganoid embryo sheet that 0.6mm is thick.
The present invention also provides a kind of use NTC thermistor that above-mentioned manufacture method is made.
The B of described NTC thermistor
25/50value is 4050K ± 3%.
The beneficial effect that the technical scheme that the embodiment of the present invention provides is brought is: the proportioning that is used for each component of composition of NTC thermistor by adjustment, the NTC thermistor chip that it is made is thicker than the chip of identical B value, thereby can in the resistance manufacture craft, increase the surface grinding operation of chip embryo sheet, guarantee chip embryo sheet smoothness of the surface and consistency, prevent that the resistance long-term work from producing the problem that resistance drift that performance change causes was even lost efficacy, extend the useful life of resistance, improved its certainty of measurement; Simultaneously, due to the chip thickening, electric current is resistance to sparking easily, has improved the anti-rush of current performance of resistance; The NTC thermistor that the embodiment of the present invention provides has resistance to elevated temperatures preferably, at 120 ℃ of lower resistance stable outputs, is applicable to the high temperature apparatus field such as water heater.
The accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, in below describing embodiment, the accompanying drawing of required use is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the potsherd that the embodiment of the present invention provides;
Fig. 2 is the potsherd that has adhered to silver-colored slurry that the embodiment of the present invention provides;
Fig. 3 is the thermistor of the NTC without epoxy encapsulation that the embodiment of the present invention provides;
Fig. 4 is the thermistor of the NTC through epoxy encapsulation that the embodiment of the present invention provides.
Embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing, embodiment of the present invention is described further in detail.
One, material therefor and instrument in the embodiment of the present invention
Mn
3o
4nano-powder, Co
3o
4nano-powder, Fe
2o
3nano-powder, SiO
2nano-powder, NiO nano-powder, silver slurry (comprise silver slurry and silver slurry diluent complete sets of products, product type is SR402H) all buy the CO. from KOJUNDO CHEMICAL LABORATORY, LTD (Japanese high-purity chemical research institute), the purity of each nano-powder all reaches chemical pure; Dibutyl phthalate (B oil) is bought from Korea S OCI company, and model is (C
16h
22o
4)=278.35; Polyvinyl alcohol milky white adhesive model is C-501, buys from Korea S OKONG company; The epoxy resin powder model is EPR-620, buys from Xin Chang river, Shanghai chemistry Co., Ltd.
Ball mill is bought from Korea S DAE WHA TECH company; The powder impregnator is bought from Korea S TWO-A system company.
The manufacture method of the NTC thermistor two, adopted in the embodiment of the present invention
Step (1): take raw material by following weight portion proportioning: Mn
3o
4590-600 part, Co
3o
413-15 part, Fe
2o
3105-115 part, SiO
215-17 part, NiO 260-265 part.
Step (2): the described raw material weighed up is mixed, pour in ball mill, add 2500ml water in ball mill, grinding 30-50 hour.
Step (3): the raw material after the taking-up grinding, put into baking oven, bake 10-12 hour to the raw material dewatered drying under 125 ℃.
Step (4): take out the raw material of drying, in the described raw material after oven dry, take 500g, add adhesive to stir, form the chip slurry.The adhesive used in this step is 20g dibutyl phthalate and 7.5g polyvinyl alcohol milky white adhesive.According to the adhesive bonding force of the method proportioning by force, not volatile, on the chemical property of raw material without impact, and its material viscosity is moderate, is conducive to evenly mix with raw material.
Step (5): described chip slurry is pressed into to thin slice.
In the embodiment of the present invention, first by Multi-step forming-dry, the operation such as punching press by repeatedly subsequently-bake is pressed into by described chip slurry the thin slice that 0.6-0.7mm is thick.For example, concrete operation step is:
A, with tablet press machine, the chip slurry is pressed into to the thin slice that 0.7mm is thick;
B, thin slice 0.7mm is thick with large clip are fixed, and hang at ambient temperature 20min thin slice is dried;
C, by 0.7mm, thick thin slice is pressed into the thin slice that 0.65mm is thick;
D, by 0.65mm, thick thin slice is cut into the rectangular of wide about 44mm, and by rectangular the coming on stainless (steel) wire of being cut into, positive and negative respectively dries in the air 10 minutes at ambient temperature;
E, by 0.65mm, thick rectangular thin slice is pressed into thick rectangular of 0.63mm;
F, the rectangular thin slice that 0.63mm is thick are cut into the square sheets that the length of side is 44mm, and the square sheets be cut into is come on stainless (steel) wire, put into baking oven and bake 10min;
G, by 0.63mm, thick square sheets is pressed into the thin slice that 0.62mm is thick;
H, by 0.62mm, thick thin slice is placed on glass plate, under controlling, PID (proportional-integral-differential) controller first under 60 ℃, bakes 12 hours, be cooled to after normal temperature to carry out secondary and cure, when secondary cures, PID controller temperature control bakes 1 hour under 60 ℃, bake 1 hour under 70 ℃, bake 1 hour under 80 ℃, under 90 ℃, bake 1 hour, under 100 ℃, bake 1 hour, bake 1 hour under 110 ℃, under 125 ℃, bake 6 hours.
Step (6): described thin slice is polished, form ganoid embryo sheet.
These step concrete operations are as follows: bake and finish the thick thin slice of the rear 0.62mm of taking-up, with sander, polished in its two sides, make the ganoid embryo sheet that 0.6mm is thick.
Step (7): described embryo sheet, 1290-1310 ℃ of lower high temperature sintering 48 hours, is formed to potsherd shown in Fig. 1.
Step (8): give described potsherd coated on both sides silver slurry, make electrode (referring to Fig. 2).
These step concrete operations are as follows:
Dilution silver slurry: the silver slurry is 100: 5 with the weight ratio of silver slurry diluent;
Print electrode: after potsherd is fully cooling, to the silver slurry after potsherd printing dilution, printing is carried out at twice, and the potsherd that all will be brushed with the silver slurry after each printing finishes is arranged on stainless (steel) wire, bakes 10-15 minute until dry under 125 ℃;
Roasting: by the fire-resistant box of packing into of the potsherd after drying, put into sintering furnace 850 ℃ of lower sintering 8 hours, make electrode.Step (9): require to cut the described potsherd that has adhered to silver-colored slurry according to resistance, obtain electroded NTC thermistor chip (as shown in Figure 3).These step concrete operations are as follows:
To be cut into the potsherd of electrode the fritter of 1.02*1.00mm, the formation resistance is R
25 ℃=100K Ω ± 3%, B
25/50the electroded NTC thermistor chip of=4050K ± 3%.
Step (10): give described electroded NTC thermistor chip welding lead, make the NTC thermistor.
All adopt the scolding tin welding lead in concrete operations.
In order better to protect the NTC thermistor chip, in the useful life of improving chip, the manufacture method that the embodiment of the present invention provides also comprises the steps:
Step (11): wrap up the epoxy resin-impregnated rubber powder to the chip of described NTC thermistor and wire bonds point by the powder impregnator, 150 ℃ of lower baking-curings 2 hours, make the NTC thermistor (as shown in Figure 4) of epoxy encapsulation.
These step concrete operations are as follows:
3 powder grooves are arranged respectively on the powder impregnator, each powder groove back is provided with the zone that is heating and curing, conveyer belt drives described NTC thermistor running, described NTC thermistor is stained with epoxy powder in the powder groove, then through the hot setting zone, solidify, realize epoxy resin impregnated, again successively through the second powder box and consolidation zone, the 3rd powder box and consolidation zone dipping, after dipping, the powder impregnator is rolled onto on dish by described NTC thermistor automatically, 150 ℃ of lower baking-curings 2 hours, make the NTC thermistor of epoxy encapsulation in baking box.
The performance test methods of the NTC thermistor chip that three, the embodiment of the present invention provides, comprise rush of current test, high temperature test, stability test etc., and three samples are chosen in every kind of performance test, and concrete method of testing is as follows:
(1) rush of current test: the NTC thermistor chip under 120 ℃, the embodiment of the present invention provided (the benchmark resistance is 3.490K Ω) carries out the direct current energizing test, the direct voltage that the NTC thermistor chip is loaded raises gradually from 5V, detect the resistance output of resistance in galvanization, choose respectively resistance or B value and change the current point that surpasses original value 3% and the current point that chip punctures, test data is referring to table 1;
(2) high temperature test: under the 5V direct voltage, resistance, in the environment of high temperature of 120 DEG C ± 2 ℃, toasts 1000 hours, and after baking, cooling is 2 hours, at room temperature tests the variation of its resistance and B value, and test data is referring to table 2;
(3) stability test: under the 5V direct voltage, the NTC thermistor chip embodiment of the present invention provided with the thermal shock machine carries out impact experiment, and-40 ℃ lower 20 minutes, 120 ℃ lower 20 minutes, 2 minutes intermediate conversion time, carry out 1000 circulations, test data is referring to table 3.
The making of 1 one kinds of NTC thermistors of embodiment
Described NTC thermistor makes according to above-mentioned two described manufacture methods, and wherein: the raw material taken in step (1) is: Mn
3o
4590g, Co
3o
413g, Fe
2o
3115g, SiO
215g, NiO265g.
The performance parameter of described NTC thermistor is referring to table 1-3.
The making of 2 one kinds of NTC thermistors of embodiment
Described NTC thermistor makes according to above-mentioned two described manufacture methods, and wherein: the raw material taken in step (1) is: Mn
3o
4600g, Co
3o
414g, Fe
2o
3109g, SiO
216g, NiO 262g.
The performance parameter of described NTC thermistor is referring to table 1-3.
The making of 3 one kinds of NTC thermistors of embodiment
Described NTC thermistor makes according to above-mentioned two described manufacture methods, and wherein: the raw material taken in step (1) is: Mn
3o
4610g, Co
3o
415g, Fe
2o
3105g, SiO
217g, NiO 260g.
The performance parameter of described NTC thermistor is referring to table 1-3.
The making of 4 one kinds of NTC thermistors of embodiment
Described NTC thermistor makes according to above-mentioned two described manufacture methods, and wherein: the raw material taken in step (1) is: Mn
3o
41100g, Co
3o
425g, Fe
2o
3200g, SiO
230g, NiO 480g.The performance parameter of described NTC thermistor is referring to table 1-3.
The data parameters of the NTC thermistor performance test that embodiment 1-4 provides is as follows:
The rush of current test data of the NTC thermistor chip that table 1 embodiment of the present invention 1-4 provides
The high temperature test data of the NTC thermistor chip that table 2 embodiment of the present invention 1-4 provides
The stability test data of the NTC thermistor chip that table 3 embodiment of the present invention 1-4 provides
Referring to table 1, the chip of the NTC thermistor that embodiment of the present invention 1-4 provides all can tolerate the above electric current of 17mA, the chip that embodiment 2 and embodiment 4 provide all can tolerate the above electric current of 19mA, and it is known according to the specification of same quasi-resistance, the resistance chip of most of like products generally tolerates the electric current of 5mA only, so the NTC thermistor chip that the embodiment of the present invention provides has good anti-rush of current;
Referring to table 2, the NTC thermistor chip that the embodiment of the present invention provides toasts 1000 hours under 120 ℃ of hot environments, and change in resistance is no more than 1%, and resistance is stable, has good resistance to elevated temperatures;
Referring to table 3, the NTC thermistor chip that the embodiment of the present invention is provided carries out cold shock testing, after test, resistance varying-ratio and B value rate of change all are less than 1%, especially the chip that embodiment 2 and embodiment 4 provide, resistance varying-ratio all is less than 0.3%, is far superior to 3% of the sector standard-required.
Test as follows the rate of finished products of the NTC thermistor that the embodiment of the present invention provides:
The NTC thermistor that embodiment of the present invention 1-4 is provided is divided into respectively 5 batches, detects resistance and the B value of each batch of resistance, and resistance and B value change the product that is no more than 1% and be qualified finished product.
The NTC thermistor rate of finished products that the embodiment of the present invention is made reaches 98.7%, and the rate of finished products of the NTC thermistor that other domestic production enterprise produces at present is mostly in 90% left and right, the present invention has improved the rate of finished products of NTC thermistor greatly, has reduced production cost, has obvious price advantage.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (6)
1. a method of making the NTC thermistor, is characterized in that, the component and the content thereof that for the preparation of the composition of the chip of described NTC thermistor, comprise are:
Above each component is nano-powder, and purity is chemical pure,
Described method comprises:
(1) component and the content according to described composition takes raw material;
(2) pour ball mill into after described raw material is mixed, add water, grinding 30-50 hour;
(3) the described raw material after grinding is carried out to dewatered drying;
(4) in the described raw material after oven dry, add adhesive to stir, form the chip slurry;
(5) described chip slurry is pressed into to thin slice, specifically comprises: by punching press-dry and punching press subsequently-bake operation described chip slurry is pressed into to the thin slice that 0.6-0.7mm is thick;
(6) described thin slice is polished, formed ganoid embryo sheet, specifically comprised: by sander, described thin slice is polished into to the ganoid embryo sheet that 0.6mm is thick;
(7) by described embryo sheet 1290-1310 ℃ of lower high temperature sintering 48 hours, form potsherd;
(8) give described potsherd coated on both sides silver slurry, make electrode;
(9) require to cut the described potsherd that has adhered to silver-colored slurry according to resistance, obtain electroded NTC thermistor chip;
(10) give described electroded NTC thermistor chip welding lead, make the NTC thermistor.
2. the method for making according to claim 1 NTC thermistor, is characterized in that, the component and the content thereof that for the preparation of the composition of the chip of described NTC thermistor, comprise are:
3. the method for making NTC thermistor according to claim 1, is characterized in that, described step (10) afterwards, also comprises:
By the powder impregnator, go up the epoxy resin rubber powder to the chip of described NTC thermistor and wire bonds point parcel dipping, 150 ℃ of lower baking-curings 2 hours, make the NTC thermistor of epoxy encapsulation.
4. the method for making NTC thermistor according to claim 1, is characterized in that, the adhesive described in step (4) is dibutyl phthalate and polyvinyl alcohol milky white adhesive, and its operation specifically comprises:
In described raw material after oven dry, add dibutyl phthalate and polyvinyl alcohol milky white adhesive to stir, form the chip slurry, the weight of wherein said dibutyl phthalate is 4% of the described raw material weight after drying, and the weight of described polyvinyl alcohol milky white adhesive is 1.5% of the described raw material weight after drying.
5. use the NTC thermistor that in claim 1-4, the described manufacture method of any one is made.
6. NTC thermistor according to claim 5, is characterized in that, the B of described NTC thermistor
25/50value is 4050K ± 3%.
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| CN105152644A (en) * | 2015-07-10 | 2015-12-16 | 明光旭升科技有限公司 | NTC thermistor chip material, chip, resistor and sensor, and making methods thereof |
| CN105130412A (en) * | 2015-07-10 | 2015-12-09 | 明光旭升科技有限公司 | NTC thermistor chip material, chip, thermistor, sensor and preparation method |
| CN108147790B (en) * | 2017-12-26 | 2021-04-30 | 珠海爱晟医疗科技有限公司 | Medical gold-containing high-precision high-stability NTC (negative temperature coefficient) thermosensitive chip and manufacturing method thereof |
| CN109320211A (en) * | 2018-10-29 | 2019-02-12 | 惠州嘉科实业有限公司 | Thermometric NTC thermistor and preparation method thereof |
| JP7268393B2 (en) * | 2019-02-22 | 2023-05-08 | 三菱マテリアル株式会社 | Thermistor manufacturing method |
| CN113896512A (en) * | 2021-11-03 | 2022-01-07 | 句容市博远电子有限公司 | Composition for preparing NTC thermistor chip and NTC thermistor prepared from composition |
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