CN102627445A - 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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- CN102627445A CN102627445A CN2012101265513A CN201210126551A CN102627445A CN 102627445 A CN102627445 A CN 102627445A CN 2012101265513 A CN2012101265513 A CN 2012101265513A CN 201210126551 A CN201210126551 A CN 201210126551A CN 102627445 A CN102627445 A CN 102627445A
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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, particularly a kind of NTC thermistor that is used to prepare the compsn of NTC thermistor chip and uses the chip that said composition makes.
Background technology
Thermistor is a type of sensor; Be divided into PTC (Positive Temperature Coefficient according to the temperature factor difference; PTC) thermistor and NTC (Negative Temperature CoeffiCient, NTC) thermistor.The typical feature of thermistor is to temperature sensitive, shows different resistance values under the different temperature.PTC thermistor resistance value when temperature is high more is big more, and NTC thermistor resistance value when temperature is high more is low more, and they belong to semiconducter device.
That the NTC thermistor has is highly sensitive, response speed is fast, volume is little, be easy to realize advantages such as teletype control and measurement, is widely used in fields such as refrigerator, air-conditioning, electric water heater, integral bathroom, electronic calendar, microwave oven, barn temperature measuring, dishwasher, electric cooker, electronics sanitation, refrigerator-freezer, soybean milk maker, battery of mobile phone, charger, electromagnetic oven, bread producing machine, sterilizing-cabinet, water dispenser, temperature control instrument, Medical Instruments, automobile thermometric, electric oven, fire alarm.
In realizing process of the present invention; The contriver finds that there is following problem at least in prior art: the influence that NTC thermistor is in the market changed by the chip material property in use; Be easy to generate aging drift; Influence its work-ing life and measuring accuracy, when especially at high temperature working, be prone to produce resistance and export unstable phenomenon; Because chip thickness and density are not enough, repeatedly through electric current the time, the easy breakdown inefficacy of chip.
Summary of the invention
In order to solve prior art problems, the embodiment of the invention provides a kind of compsn of the NTC of being used for thermistor chip and has used the resistance of this chip.Said technical scheme is following:
On the one hand, the invention provides a kind of compsn that is used to prepare the NTC thermistor chip, component that wherein comprises and content thereof are:
More than each component be nano-powder, purity is CP,
And process the chip slurry through following step by above-mentioned compsn:
(1) takes by weighing raw material according to said components and content;
(2) pour said raw materials mix into ball mill after evenly, add entry, grinding 30-50 hour;
(3) the said raw material behind the grinding is carried out dewatered drying;
(4) add tackiness agent in the said raw material after oven dry and stir, form the chip slurry.
Preferably, component that wherein comprises and content thereof are:
On the other hand, the invention provides a kind of method of the chip manufacturing NTC thermistor of processing with above-mentioned compsn, said method comprising the steps of:
(1) component and the content according to above-mentioned compsn takes by weighing raw material;
(2) pour said raw materials mix into ball mill after evenly, add entry, grinding 30-50 hour;
(3) the said raw material behind the grinding is carried out dewatered drying;
(4) add tackiness agent in the said raw material after oven dry and stir, form the chip slurry;
(5) said chip slurry is pressed into thin slice;
(6) said thin slice is polished, form ganoid embryo sheet;
(7) with said embryo sheet 1290-1310 ℃ of following high temperature sintering 48 hours, form ceramic plate;
(8) give said ceramic plate coated on both sides silver slurry, process electrode;
(9) require to cut the said ceramic plate that has adhered to silver-colored slurry according to resistance, obtain electroded NTC thermistor chip;
(10) give said electroded NTC thermistor chip welding lead, process the NTC thermistor.Wherein:
After step (10) is processed the NTC thermistor, also comprise:
Give epoxy resin rubber powder on chip and the wire bonds point parcel dipping of said NTC thermistor through the powder impregnation machine,, process the NTC thermistor of epoxy encapsulation 150 ℃ of following baking-curings 2 hours.
Tackiness agent is dibutyl phthalate and Z 150PH milky white adhesive described in the step (4) that said chip slurry and NTC thermistor are made; Its concrete operations comprise: adding dibutyl phthalate and Z 150PH milky white adhesive stir in the said raw material after oven dry; Form the chip slurry; The weight of wherein said dibutyl phthalate is 4% of the said raw material weight after drying, and the weight of said Z 150PH milky white adhesive is 1.5% of the said raw material weight after drying.
Step (5), (6) specifically comprise: through repeatedly punching press-dry and repeatedly punching press subsequently-bake operation, said chip slurry is pressed into the thick thin slice of 0.6-0.7mm; Through sander said thin slice is polished into the thick ganoid embryo sheet of 0.6mm.
The present invention also provides a kind of usefulness NTC thermistor that above-mentioned making method is made.
The B of said NTC thermistor
25/50Value is 4050K ± 3%.
The beneficial effect that the technical scheme that the embodiment of the invention provides is brought is: the proportioning that is used for each component of compsn of NTC thermistor through adjustment; The NTC thermistor chip that it is processed 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 surface smooth property and consistence; Prevent resistance drift that resistance long term operation generation performance change causes even the problem that lost efficacy, prolonged the work-ing life of resistance, improved its measuring accuracy; Simultaneously, because 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 invention provides has resistance to elevated temperatures preferably, and is stable 120 ℃ of following resistance outputs, is applicable to high temperature service fields such as water-heater.
Description of drawings
In order to be illustrated more clearly in the technical scheme in the embodiment of the invention; The accompanying drawing of required use is done to introduce simply in will describing embodiment below; Obviously, the accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills; Under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the ceramic plate that the embodiment of the invention provides;
Fig. 2 is the ceramic plate that has adhered to silver-colored slurry that the embodiment of the invention provides;
Fig. 3 is the NTC thermistor without epoxy encapsulation that the embodiment of the invention provides;
Fig. 4 be the embodiment of the invention provide through the NTC of epoxy encapsulation thermistor.
Embodiment
For making the object of the invention, technical scheme and advantage clearer, will combine accompanying drawing that embodiment of the present invention is done to describe in detail further below.
One, material therefor and instrument in the embodiment of the 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 thinner complete sets of products; Product type is SR402H) all buy CO. from KOJUNDO CHEMICAL LABORATORY; LTD (Japanese high-purity chemical institute), the purity of each nano-powder all reaches CP; Dibutyl phthalate (B oil) is bought from Korea S OCI company, and model is (C
16H
22O
4)=278.35; Z 150PH milky white adhesive model is C-501, buys from Korea S OKONG company; The epoxy resin powder model is EPR-620, buys the chemical ltd in new normal river from Shanghai.
Ball mill is bought from Korea S DAE WHA TECH company; The powder impregnation machine is bought from Korea S TWO-A system company.
The making method of the NTC thermistor that two, is adopted in the embodiment of the invention
Step (1): take by weighing raw material by following weight part 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 said raw materials mix that will weigh up is even, pours in the ball mill, in ball mill, adds 2500ml water, grinding 30-50 hour.
Step (3): the raw material behind the taking-up grinding, put into baking oven, under 125 ℃, bake 10-12 hour to the raw material dewatered drying.
Step (4): take out the raw material of oven dry, take by weighing 500g in the said raw material after oven dry, add tackiness agent and stir, form the chip slurry.The tackiness agent that in this step, uses is 20g dibutyl phthalate and 7.5g Z 150PH milky white adhesive.According to the tackiness agent bounding force of this method proportioning by force, not volatile, the chemical property of raw material is not had influence, and its material viscosity is moderate, helps and the raw material uniform mixing.
Step (5): said chip slurry is pressed into thin slice.
Earlier through repeatedly punching press-dry, operations such as the punching press through repeatedly subsequently-bake are pressed into the thick thin slice of 0.6-0.7mm with said chip slurry in the embodiment of the invention.For example, concrete operations step is:
A, the chip slurry is pressed into the thick thin slice of 0.7mm with tabletting machine;
B, fix, hang 20min at ambient temperature thin slice is dried with the big clip thin slice that 0.7mm is thick;
C, the thin slice that 0.7mm is thick are pressed into the thick thin slice of 0.65mm;
D, the thin slice that 0.65mm is thick are cut into the rectangular of wide about 44mm, and with rectangular the coming on the stainless (steel) wire of being cut into, pros and cons respectively dried in the air 10 minutes at ambient temperature;
E, the rectangular thin slice that 0.65mm is thick are 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 that is cut into is come on the stainless (steel) wire, put into baking oven and bake 10min;
G, the square sheets that 0.63mm is thick are pressed into the thick thin slice of 0.62mm;
H, the thin slice that 0.62mm is thick are placed on the sheet glass, under 60 ℃, bake 12 hours in that PID (PID) unit control is first down, are cooled to carry out secondary behind the normal temperature and cure; When secondary cured, PID unit temperature control baked 1 hour under 60 ℃, under 70 ℃, baked 1 hour; Under 80 ℃, baked 1 hour, under 90 ℃, baked 1 hour, under 100 ℃, baked 1 hour; Under 110 ℃, baked 1 hour, under 125 ℃, baked 6 hours.
Step (6): said thin slice is polished, form ganoid embryo sheet.
These step concrete operations are following: bake and finish the thick thin slice of back taking-up 0.62mm, with sander polished in its two sides, process the thick ganoid embryo sheet of 0.6mm.
Step (7): said embryo sheet 1290-1310 ℃ of following high temperature sintering 48 hours, is formed ceramic plate shown in Figure 1.
Step (8): give said ceramic plate coated on both sides silver slurry, process electrode (referring to Fig. 2).
These step concrete operations are following:
Dilution silver slurry: the silver slurry is 100: 5 with the weight ratio of silver slurry thinner;
Print electrode: after treating that ceramic plate cools off fully, to the silver slurry after the ceramic plate printing dilution, printing is carried out at twice, and the ceramic plate that all will be brushed with the silver slurry after each printing finishes is arranged on the stainless (steel) wire, under 125 ℃, bakes 10-15 minute until drying;
Roasting: the fire-resistant box of packing into of the ceramic plate after will drying, put into sintering oven 850 ℃ of following sintering 8 hours, process electrode.Step (9): require to cut the said ceramic plate 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 following:
The ceramic plate that will have electrode is cut into the fritter of 1.02*1.00mm, and the formation resistance is R
25 ℃=100K Ω ± 3%, B
25/50The electroded NTC thermistor chip of=4050K ± 3%.
Step (10): give said electroded NTC thermistor chip welding lead, process the NTC thermistor.
All adopt the scolding tin welding lead in the concrete operations.
For better protection NTC thermistor chip, improve the work-ing life of chip, the making method that the embodiment of the invention provides also comprises the steps:
Step (11): wrap up the epoxy resin-impregnated rubber powder for the chip of said NTC thermistor and wire bonds point through the powder impregnation machine,, process the NTC thermistor (as shown in Figure 4) of epoxy encapsulation 150 ℃ of following baking-curings 2 hours.
These step concrete operations are following:
3 powder grooves are arranged respectively on the powder impregnation machine, and each powder groove back all is provided with the zone that is heating and curing, and travelling belt drives said NTC thermistor running; Said NTC thermistor is stained with epoxy powder in the powder groove; Solidify through hot setting zone then, realizes epoxy resin impregnatedly, flood through second powder box and consolidation zone, the 3rd powder box and consolidation zone successively again; After dipping finishes; The powder impregnation machine is rolled onto said NTC thermistor on the dish automatically, in baking box, 150 ℃ of following baking-curings 2 hours, processes the NTC thermistor of epoxy encapsulation.
Three, the performance test methods of the NTC thermistor chip that provides of the embodiment of the invention comprises rush of current test, high temperature test, stability test etc., and three samples are chosen in every kind of performance test, and concrete testing method is following:
(1) rush of current test: the NTC thermistor chip that under 120 ℃, the embodiment of the invention is provided (the benchmark resistance is 3.490K Ω) carries out the direct current energizing test; The volts DS that the NTC thermistor chip is loaded raises from 5V gradually; In galvanization, detect the resistance output of resistance; Choose resistance or B value respectively and change above the current point of original value 3% and the current point of chip puncture, test data is referring to table 1;
(2) high temperature test: under the 5V volts DS, resistance toasted 1000 hours in the environment of 120 ℃ ± 2 ℃ of high temperature, and the variation of its resistance and B value is at room temperature tested in baking back cooling 2 hours, and test data is referring to table 2;
(3) stability test: under the 5V volts DS, with the thermal shock machine NTC thermistor chip that the embodiment of the invention provides is carried out impact experiment ,-40 ℃ following 20 minutes; 120 ℃ following 20 minutes; 2 minutes buffering time, carry out 1000 circulations, test data is referring to table 3.
The making of 1 one kinds of NTC thermistors of embodiment
Said NTC thermistor makes according to above-mentioned two said making methods, and wherein: the raw material that takes by weighing in the step (1) is: Mn
3O
4590g, Co
3O
413g, Fe
2O
3115g, SiO
215g, NiO265g.
The performance perameter of said NTC thermistor is referring to table 1-3.
The making of 2 one kinds of NTC thermistors of embodiment
Said NTC thermistor makes according to above-mentioned two said making methods, and wherein: the raw material that takes by weighing in the step (1) is: Mn
3O
4600g, Co
3O
414g, Fe
2O
3109g, SiO
216g, NiO 262g.
The performance perameter of said NTC thermistor is referring to table 1-3.
The making of 3 one kinds of NTC thermistors of embodiment
Said NTC thermistor makes according to above-mentioned two said making methods, and wherein: the raw material that takes by weighing in the step (1) is: Mn
3O
4610g, Co
3O
415g, Fe
2O
3105g, SiO
217g, NiO 260g.
The performance perameter of said NTC thermistor is referring to table 1-3.
The making of 4 one kinds of NTC thermistors of embodiment
Said NTC thermistor makes according to above-mentioned two said making methods, and wherein: the raw material that takes by weighing in the step (1) is: Mn
3O
41100g, Co
3O
425g, Fe
2O
3200g, SiO
230g, NiO 480g.The performance perameter of said NTC thermistor is referring to table 1-3.
The data parameters of the NTC thermistor performance test that embodiment 1-4 provides is following:
The rush of current test data of the NTC thermistor chip that table 1 embodiment of the invention 1-4 provides
The high temperature test data of the NTC thermistor chip that table 2 embodiment of the invention 1-4 provides
The stability test data of the NTC thermistor chip that table 3 embodiment of the invention 1-4 provides
Referring to table 1; The chip of the NTC thermistor that embodiment of the invention 1-4 provides all can tolerate the above electric current of 17mA; Embodiment 2 all can tolerate the above electric current of 19mA with the chip that embodiment 4 provides; And can know that according to the specification sheets with 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 invention provides has good anti-rush of current property;
Referring to table 2, the NTC thermistor chip that the embodiment of the invention provides toasted 1000 hours under 120 ℃ of hot environments, and change in resistance is no more than 1%, and resistance is stable, and having good temperature resistance can;
Referring to table 3; The NTC thermistor chip that the embodiment of the invention is provided carries out cold shock testing; Test back resistance varying-ratio and B value velocity of variation are all less than 1%; Especially the chip that provides of embodiment 2 and embodiment 4, resistance varying-ratio is far superior to 3% of the sector standard-required all less than 0.3%.
Test the yield rate of the NTC thermistor that the embodiment of the invention provides as follows:
The NTC thermistor that embodiment of the invention 1-4 is provided is divided into 5 batches respectively, detects the resistance and the B value of each batch resistance, and resistance and B value change and be no more than 1% product and be qualified finished product.
The NTC thermistor yield rate that the embodiment of the invention is made reaches 98.7%; And at present the yield rate of the NTC thermistor of other domestic production enterprise production mostly about 90%; The present invention has improved the yield rate of NTC thermistor greatly, has reduced production cost, has tangible price advantage.
The above is merely preferred embodiment of the present invention, and is in order to restriction the present invention, not all within spirit of the present invention and principle, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. compsn that is used to prepare the NTC thermistor chip, component that wherein comprises and content thereof are:
More than each component be nano-powder, purity is CP,
And process the chip slurry by following step:
(1) takes by weighing raw material according to said components and content;
(2) pour said raw materials mix into ball mill after evenly, add entry, grinding 30-50 hour;
(3) the said raw material behind the grinding is carried out dewatered drying;
(4) add tackiness agent in the said raw material after oven dry and stir, form the chip slurry.
2. the compsn that is used to prepare the NTC thermistor chip according to claim 1 is characterized in that, component that wherein comprises and content thereof are:
3. method of making the NTC thermistor with the described compsn of claim 1 is characterized in that said method comprises:
(1) component and the content according to the described compsn of claim 1 takes by weighing raw material;
(2) pour said raw materials mix into ball mill after evenly, add entry, grinding 30-50 hour;
(3) the said raw material behind the grinding is carried out dewatered drying;
(4) add tackiness agent in the said raw material after oven dry and stir, form the chip slurry;
(5) said chip slurry is pressed into thin slice;
(6) said thin slice is polished, form ganoid embryo sheet;
(7) with said embryo sheet 1290-1310 ℃ of following high temperature sintering 48 hours, form ceramic plate;
(8) give said ceramic plate coated on both sides silver slurry, process electrode;
(9) require to cut the said ceramic plate that has adhered to silver-colored slurry according to resistance, obtain electroded NTC thermistor chip;
(10) give said electroded NTC thermistor chip welding lead, process the NTC thermistor.
4. the method for making NTC thermistor according to claim 3 is characterized in that said step (10) also comprises afterwards:
Give epoxy resin rubber powder on chip and the wire bonds point parcel dipping of said NTC thermistor through the powder impregnation machine,, process the NTC thermistor of epoxy encapsulation 150 ℃ of following baking-curings 2 hours.
5. the method for making NTC thermistor according to claim 3 is characterized in that the tackiness agent described in the step (4) is dibutyl phthalate and Z 150PH milky white adhesive, and its operation specifically comprises:
Adding dibutyl phthalate and Z 150PH milky white adhesive stir in the said raw material after oven dry; Form the chip slurry; The weight of wherein said dibutyl phthalate is 4% of the said raw material weight after drying, and the weight of said Z 150PH milky white adhesive is 1.5% of the said raw material weight after drying.
6. the method for making NTC thermistor according to claim 5 is characterized in that said step (5), (6) specifically comprise:
Through punching press-dry and punching press subsequently-bake operation said chip slurry is pressed into the thick thin slice of 0.6-0.7mm; Through sander said thin slice is polished into the thick ganoid embryo sheet of 0.6mm.
7. with any NTC thermistor that described making method is made among the claim 3-6.
8. NTC thermistor according to claim 7 is characterized in that, the B of said NTC thermistor
25/50Value is 4050K ± 3%.
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| 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 |
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| CN108147790A (en) * | 2017-12-26 | 2018-06-12 | 珠海爱晟医疗科技有限公司 | Medical NTC heat sensitive chips of the high precision high stability containing gold and preparation 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 |
| CN113454736A (en) * | 2019-02-22 | 2021-09-28 | 三菱综合材料株式会社 | Method for manufacturing thermistor |
| 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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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| CN108147790A (en) * | 2017-12-26 | 2018-06-12 | 珠海爱晟医疗科技有限公司 | Medical NTC heat sensitive chips of the high precision high stability containing gold and preparation method thereof |
| 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 |
| CN113454736A (en) * | 2019-02-22 | 2021-09-28 | 三菱综合材料株式会社 | Method for manufacturing thermistor |
| CN113454736B (en) * | 2019-02-22 | 2023-02-17 | 三菱综合材料株式会社 | Method for manufacturing thermistor |
| US11763967B2 (en) | 2019-02-22 | 2023-09-19 | Mitsubishi Materials Corporation | Method of manufacturing thermistor |
| 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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| CN102627445B (en) | 2013-12-18 |
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