CN105330277B - Negative tempperature coefficient thermistor raw material composition and application - Google Patents
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Abstract
The invention discloses the preparation methods of a kind of negative tempperature coefficient thermistor raw material composition, negative temperature coefficient heat-sensitive composition, the preparation method of negative temperature coefficient heat-sensitive composition and negative tempperature coefficient thermistor chip.Negative tempperature coefficient thermistor raw material composition, by percentage to the quality, including following components: Mn3O430~65%；Co3O45~45%；NiO 5~25%；Fe2O35~30%；Nd2O30.5~2.0%；And Al (NO3)3.9H2O 1~10%.Introducing Al in the form of aluminum nitrate in this temperature coefficient thermistor raw material composition3+, rather than with Al2O3Solid form is added, and aluminum nitrate is water-soluble very well, it is easy to just be evenly distributed in composition, so as to reduce the deviation of resistance value sum, improve the B value precision of resistivity sum.Additionally by the high enthalpy rare earth oxide Nd of addition2O3, which is 1783KJ/mol, this type oxide is not susceptible to chemically react at high temperature, so that the aging as caused by chemical change influences to reduce, so that its electrical stability is improved.
Description
Technical field
The present invention relates to a kind of negative tempperature coefficient thermistor raw material compositions, negative temperature coefficient heat-sensitive composition, subzero temperature
Spend the preparation method of coefficient heat-sensitive composition and the preparation method of negative tempperature coefficient thermistor chip.
Background technique
NTC thermistor (temperature coefficient thermistor) refers to the resistance that its resistance value is increased with temperature and is exponentially reduced,
Since it has many advantages, such as that temperature sensitive, small in size, response is fast, price is low and interchangeability is good, it is widely used in temperature inspection
Survey, temperature control and temperature-compensating etc..
High resistant (100K Ω or more), high B value (3900 or more) NTC thermistor material overwhelming majority formula are prepared at present
A kind of important functional material Al will be added in system2O3, additive amount is seldom (1wt%~10wt%), but its effect is compared again
Greatly, the resistivity of thermo-sensitive material can be substantially improved in it, due to Al2O3It is insoluble in water, during making temperature-sensitive powder, is difficult
It being evenly distributed in powder, the centrality for being bound to cause material unit for electrical property parameters (resistance value, material constant B value) in this way is bad,
Deviation range is very big, and generally all in J grades (± 5%), K grades (± 10%) and M grades (± 20%), electrical stability is poor.
Summary of the invention
Based on this, it is necessary to provide a kind of negative temperature coefficient that can prepare the preferable NTC themistor of electrical stability
Thermistor raw material composition, negative temperature coefficient heat-sensitive composition, the preparation method of negative temperature coefficient heat-sensitive composition and subzero temperature
Spend the preparation method of coefficient resistance chip.
A kind of negative tempperature coefficient thermistor raw material composition, by percentage to the quality, including following components:
A kind of preparation method of negative temperature coefficient heat-sensitive composition, comprising the following steps:
Above-mentioned negative tempperature coefficient thermistor raw material composition is added after deionized water progress wet grinding to dry and is obtained
Mixed powder；
Mixed powder progress pre-burning is obtained into pre-burning powder；And
Poly-vinyl alcohol solution will be added after pre-burning powder grinding, is dried obtains negative temperature coefficient heat after mixing
Sensitive composition.
In one embodiment, the temperature of the drying is 100 DEG C~150 DEG C, and the time of the drying is 2~3 hours.
In one embodiment, the temperature of the pre-burning is 900 DEG C~1000 DEG C, and the time of the pre-burning is 1~2 small
When.
In one embodiment, described to be ground to wet grinding, grinding in the operation that the pre-burning powder is ground
Pre-burning powder is dried and is sieved afterwards.
In one embodiment, in the step of pre-burning powder being dried and is sieved after the grinding, the temperature of the drying is
100 DEG C~150 DEG C, the time of the drying is 2~3 hours.
In one embodiment, the mass concentration of the poly-vinyl alcohol solution be 4~7%, the poly-vinyl alcohol solution with
The mass ratio of the pre-burning powder is 10:100~15:100.
In one embodiment, the drying process is specially to toast 10~20 minutes at 100 DEG C~150 DEG C.
The negative temperature coefficient heat-sensitive group of the preparation method preparation of negative temperature coefficient heat-sensitive composition described in any of the above embodiments
Close object.
A kind of preparation method of negative tempperature coefficient thermistor chip, comprising the following steps:
Above-mentioned negative temperature coefficient heat-sensitive composition is pressed into green compact；
The green compact are sintered 3~5 hours at 1190 DEG C~1230 DEG C and obtain tile；And
Silver paste is applied on two opposite surfaces of the tile, negative tempperature coefficient thermistor chip is obtained after sintering.
Introducing Al in the form of aluminum nitrate in above-mentioned negative tempperature coefficient thermistor raw material composition3+, rather than with
Al2O3Solid form is added, and aluminum nitrate is water-soluble very well, it is easy to just be evenly distributed in composition, so as to reduce electricity
The deviation of resistance value and B value improves the precision of resistivity and B value, so that resistivity and B value precision can achieve F grades；Additionally by
High enthalpy rare earth oxide Nd is added2O3, which is 1783KJ/mol, this type oxide is not susceptible at high temperature
Chemical reaction, so that the aging as caused by chemical change influences to reduce, so that its electrical stability is improved.
Detailed description of the invention
Fig. 1 is sample crystal grain stereoscan photograph prepared by embodiment 3；
Fig. 2 is the sample crystal grain stereoscan photograph of comparative example preparation.
Specific embodiment
Below mainly in combination with specific embodiments and drawings to negative tempperature coefficient thermistor raw material composition, negative temperature coefficient
The preparation method of heat-sensitive composition, the preparation method of negative temperature coefficient heat-sensitive composition and negative tempperature coefficient thermistor chip is made
Further details of explanation.
The negative tempperature coefficient thermistor raw material composition of one embodiment, by percentage to the quality, including following components:
NTC thermal sensitive ceramics belongs to typical spinel structure, general formula AB2O4, A is generally bivalent positive ion, B in formula
For trivalent cation, O is oxonium ion.Its electrical conduction mechanism abides by Spectrametry of Electron Exchange model theory, on the position B between aliovalent metal ion
Electron exchange.For the NTC thermal sensitive ceramics of polynary system containing manganese, usual Mn exists in the form of trivalent and tetravalence and occupies B, leads
Electric process relies primarily on the realization of the electron exchange between Mn ion, i.e. Mn3++Mn4+→Mn4++Mn3+, therefore, system carrier
Concentration is related with aliovalent Mn ion concentration.Al3+It adulterates in the system, almost all is added in spinel solid solution, a part
Cause the reduction of Mn ion concentration into lattice, lead to the reduction of system carrier concentration, resistivity increases；Another part enters crystalline substance
Boundary, inhibits growing up for crystal grain, also causes system resistivity to increase, therefore Al3+The uniformity of dopant profiles to system resistance value with
And B value precision plays very important effect.By with aluminum nitrate in above-mentioned negative tempperature coefficient thermistor raw material composition
Form introduces Al3+, rather than with Al2O3Solid form is added, and aluminum nitrate is water-soluble very well, it is easy to just be evenly distributed in group
It closes in object, so as to reduce the deviation of resistance value and B value, so that resistivity and B value precision can be from original K grades, J grades of raisings
To F grades.Additionally by the high enthalpy rare earth oxide Nd of addition2O3, which is 1783KJ/mol, this type oxide exists
It is not susceptible to chemically react under high temperature, so that the aging as caused by chemical change influences to reduce, so that its electrical stability obtains
To raising.It calculating after tested, for the resistivity of the NTC thermistor of preparation up to 3600 Ω cm or more, B value is greater than 3900K, and
Centrality is good, and precision can reach F grades (± 1%), and electrical stability is good.
Each component is uniformly mixed when prepared by above-mentioned negative tempperature coefficient thermistor raw material composition.
The preparation method of the negative temperature coefficient heat-sensitive composition of one embodiment, comprising the following steps:
Step S110, after deionized water progress wet grinding being added in above-mentioned negative tempperature coefficient thermistor raw material composition
Drying obtains mixed powder.
Preferably, the mass ratio of the deionized water of addition and negative tempperature coefficient thermistor raw material composition is 2:1~3:
1。
Preferably, wet grinding is carried out using polyurethane ball-milling pot, and ball-milling medium is zirconium ball.It is further preferred that zirconium ball
Diameter be 5~7.5mm, the mass ratio of zirconium ball and negative tempperature coefficient thermistor raw material composition is 2:1~3:1.Further
Preferably, the revolving speed of grinding is 400~500r/min.
Preferably, the time of wet grinding is 4~6 hours.
Preferably, the temperature of drying is 100 DEG C~150 DEG C, and the time of drying is 2~3 hours.
Preferably, the material after ball milling is filtered zirconium ball to pour into stainless steel disc, is placed in baking oven and toasts.
Step S120, mixed powder carries out pre-burning and obtains pre-burning powder.
Preferably, the temperature of pre-burning is 900 DEG C~1000 DEG C, and the time of pre-burning is 1~2 hour.
Step S130, poly-vinyl alcohol solution will be added after the grinding of pre-burning powder, is dried obtains negative temperature after mixing
Coefficient heat-sensitive composition.
Preferably, in the operation of pre-burning powder grinding, it is ground to wet grinding, pre-burning powder is dried and is sieved after grinding.
It is further preferred that grinding uses planetary ball mill, the time of grinding is 4~6 hours, and the temperature of drying is 100 DEG C~150
DEG C, the time of drying is 2~3 hours.
Preferably, 80 meshes will be crossed after the grinding of pre-burning powder.
Preferably, the mass concentration of poly-vinyl alcohol solution is 4~7%, and the mass ratio of poly-vinyl alcohol solution and pre-burning powder is
10:100~15:100 is preferred, and being dried is specially to toast 10~20 minutes at 100 DEG C~150 DEG C.
The preparation method of above-mentioned negative temperature coefficient heat-sensitive composition is easy to operate.
The negative temperature coefficient heat-sensitive composition of one embodiment, using the preparation side of above-mentioned negative temperature coefficient heat-sensitive composition
Method preparation.
Above-mentioned negative temperature coefficient heat-sensitive composition introduces Al in the form of aluminum nitrate3+, rather than with Al2O3Solid form adds
Enter, aluminum nitrate is water-soluble very well, it is easy to just be evenly distributed in composition, so as to reduce the inclined of resistance value and B value
Difference, so that resistivity B value precision can be increased to F grades from original K grade, J grades.Additionally by the high enthalpy rare earth oxide of addition
Nd2O3, which is 1783KJ/mol, this type oxide is not susceptible to chemically react at high temperature, so that by chemistry
Aging caused by changing influences to reduce, so that its electrical stability is improved.
The preparation method of the negative tempperature coefficient thermistor chip of one embodiment, comprising the following steps:
Step S210, above-mentioned negative temperature coefficient heat-sensitive composition is pressed into green compact.
Preferably, the pressure of compression moulding is 6~10MPa.
Preferably, it is 15.19 ± 0.01mm that green compact, which are diameter, with a thickness of the disk of 1.1 ± 0.01mm.
Step S220, green compact are sintered 3~5 hours at 1190 DEG C~1230 DEG C and obtain tile.
Preferably, green compact are sintered in Muffle furnace.
Step S230, silver paste is applied on two opposite surfaces of tile, negative tempperature coefficient thermistor core is obtained after sintering
Piece.
Preferably, sintering temperature is 650 DEG C~750 DEG C in the step, and sintering time is 10~20min.
Preferably, the two sides polishing of tile is completely first applied into silver paste again.
Step S240, temperature coefficient thermistor chip is divided into the small square piece of 1mm × 1mm × 0.9mm on scribing machine.
The preparation method of above-mentioned negative tempperature coefficient thermistor chip operates relatively simple, the negative temperature coefficient heat of preparation
Quick resistance chip high-precision, high resistivity, high B value, stability are good.
It is described in detail below in conjunction with specific embodiment.
Embodiment 1
NTC thermistor raw material include following components: Mn3O4260g、Co3O420g、NiO 20g、Fe2O388g、
Nd2O38g、Al(NO3)3·9H2O 4g。
Implementation process: each raw material is accurately weighed by the above recipe ingredient, gross weight 400g is poured into equipped with 800g Φ 7.5mm zirconium
The polyurethane ball grinder of ball, adds deionized water 800g, and wet-milling 4h, revolving speed 500r/mm will be ground on planetary ball mill after sealing
Good material pours into stainless steel disc, is put into 150 DEG C of baking oven and toasts 2h, by the pre-burning in 1000 DEG C of Muffle furnaces of the powder of drying
1h, by pre-burning powder, wet-milling 4h and the baking 2h drying in 150 DEG C of baking ovens on planetary ball mill again, crosses 80 mesh for the powder of drying
Sieve is added in the PVA solution 60g and the even baking oven for placing into 150 DEG C later that mass concentration is 4% and toasts 10min, then will dry
Dry powder crosses 80 meshes, and NTC temperature-sensitive powder is made.
Under the pressure of 10MPa, by above-mentioned powder pressing at the disk of Φ 15.19mm Х 1.10mm, burnt in Muffle furnace
Knot, keeps the temperature 5h by 1190 DEG C of sintering temperature, after cooling, the two sides of tile is polished and completely applies silver, and 650 DEG C of silver ink firing temperature, the time
Chip is divided into the small square piece of 1mm × 1mm × 0.9mm by 20min on scribing machine.
Embodiment 2
NTC thermistor raw material include following components: Mn3O4120g、Co3O4180g、NiO 20g、Fe2O336g、
Nd2O34g、Al(NO3)3.9H2O 40g。
Implementation process: each raw material is accurately weighed by the above recipe ingredient, gross weight 400g is poured into equipped with 1200g Φ 5mm zirconium ball
Polyurethane ball grinder, add deionized water 1200g, wet-milling 6h, revolving speed 400r/mm will be ground on planetary ball mill after sealing
Good material pours into stainless steel disc, is put into 100 DEG C of baking oven and toasts 3h, by the pre-burning in 900 DEG C of Muffle furnaces of the powder of drying
2h, by pre-burning powder, wet-milling 6h and the baking 3h drying in 100 DEG C of baking ovens on planetary ball mill again, crosses 80 mesh for the powder of drying
Sieve is added in the PVA solution 40g and the even baking oven for placing into 100 DEG C later that mass concentration is 7% and toasts 20min, then will dry
Dry powder crosses 80 meshes, and NTC temperature-sensitive powder is made.
Under the pressure of 6MPa, by above-mentioned powder pressing at the disk of Φ 15.19mm Х 1.10mm, burnt in Muffle furnace
Knot, keeps the temperature 3h by 1230 DEG C of sintering temperature, after cooling, the two sides of tile is polished and completely applies silver, and 750 DEG C of silver ink firing temperature, the time
Chip is divided into the small square piece of 1mm × 1mm × 0.9mm by 10min on scribing machine.
Embodiment 3
NTC thermistor raw material include following components: Mn3O4192g、Co3O4100g、NiO 60g、Fe2O320g、
Nd2O38g、Al(NO3)3.9H2O 20g。
Implementation process: each raw material is accurately weighed by the above recipe ingredient, gross weight 400g is poured into equipped with 1000g Φ 7.5mm zirconium
The polyurethane ball grinder of ball, adds deionized water 1000g, after sealing on planetary ball mill wet-milling 5h, revolving speed 450r/mm, will
The material of milled pours into stainless steel disc, is put into 125 DEG C of baking oven and toasts 2.5h, by the powder of drying in 950 DEG C of Muffle furnaces
Pre-burning 1.5h by pre-burning powder the wet-milling 5h on planetary ball mill, revolving speed 450r/mm again, and toasts 2.5h in 125 DEG C of baking ovens
The powder of drying is crossed 80 meshes by drying, and PVA solution 50g and the even baking for placing into 125 DEG C later that mass concentration is 5% is added
15min is toasted in case, then the powder of drying is crossed into 80 meshes, and NTC temperature-sensitive powder is made.
Under the pressure of 8MPa, by above-mentioned powder pressing at the disk of Φ 15.19mm Х 1.10mm, burnt in Muffle furnace
Knot, keeps the temperature 4h by 1210 DEG C of sintering temperature, after cooling, the two sides of tile is polished and completely applies silver, and 700 DEG C of silver ink firing temperature, the time
Chip is divided into the small square piece of 1mm × 1mm × 0.9mm by 15min on scribing machine.
Comparative example
Comparative example is roughly the same with embodiment 1, and difference is: NTC thermistor raw material, includes following components:
Mn3O4260g、Co3O428g、NiO 20g、Fe2O388g、Al2O34g。
Fig. 1 and Fig. 2 are please referred to, Fig. 1 is the crystal grain SEM photograph for the small square piece that embodiment 3 is prepared, and Fig. 2 is comparative example
The crystal grain SEM photograph for the small square piece being prepared.It can be seen that from Fig. 1 and Fig. 2 using the uniform of aluminum nitrate doping grain size
Property is obviously got well than alumina doped, and the centrality of its resistance value and B value so is significantly improved.
It is made using Dutch PHILIPS Co. XL30&DX-4I type scanning electronic microscope observation embodiment 1-3 and comparative example 1
The pattern of standby small square piece measures embodiment 1-3 and comparative example using Agilent34401A electric bridge in 25 DEG C and 50 DEG C of oil baths
The resistance value of the small square piece of preparation, is expressed as R25And R50.Sample is placed in aging 500h in 125 DEG C of baking ovens, is then surveyed again
R25' and R50'.Embodiment 1-3 and comparative example separately sampled 20, test the R of each sample25、R50、R25' and R50', then divide
The R of each embodiment sample is not calculated25And R25' average value, count respectivelyCalculate embodiment 1-3 and comparison
Each sample of exampleTo obtain embodiment 1-3 and comparative exampleBe averaged
Value；Calculate embodiment 1-3 and comparative exampleCalculate the B of each sample of embodiment 1-3 and comparative example25/50
[3853.89×㏑(R25/R50)] and B '25/50[3853.89×㏑(R25’/R50')], to calculate embodiment 1-3 and comparison
The B of the sample of example25/50Average value and B '25/50Average value, be denoted as respectivelyAndCalculate embodiment 1-3 and right
Each sample of ratioTo obtain embodiment 1-3 and comparative exampleAverage value, calculate the sample of embodiment 1-3 and comparative example
As a result as shown in Table 1 and Table 2 respectively.
Table 1
Note: every part 20, sample, institute's measured data is averaged.
As it can be seen from table 1 embodiment 1-3 is compared with comparative example, R25And B25/50Centrality has very big raising.
Table 2
Note: every part 20, sample, institute's measured data is averaged.
From table 2 it can be seen that embodiment 1-3, compared with comparative example, electric performance stablity has very big improvement.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of negative tempperature coefficient thermistor raw material composition, which is characterized in that by percentage to the quality, by following components group
At:
2. a kind of preparation method of negative temperature coefficient heat-sensitive composition, which comprises the following steps:
Negative tempperature coefficient thermistor raw material composition described in claim 1 is added after deionized water carries out wet grinding and is dried
Obtain mixed powder；
Mixed powder progress pre-burning is obtained into pre-burning powder；And
Poly-vinyl alcohol solution will be added after pre-burning powder grinding, is dried obtains negative temperature coefficient heat-sensitive group after mixing
Close object.
3. the preparation method of negative temperature coefficient heat-sensitive composition as claimed in claim 2, which is characterized in that the temperature of the drying
Degree is 100 DEG C~150 DEG C, and the time of the drying is 2~3 hours.
4. the preparation method of negative temperature coefficient heat-sensitive composition as claimed in claim 2, which is characterized in that the temperature of the pre-burning
Degree is 900 DEG C~1000 DEG C, and the time of the pre-burning is 1~2 hour.
5. the preparation method of negative temperature coefficient heat-sensitive composition as claimed in claim 2, which is characterized in that it is described will be described pre-
It is described to be ground to wet grinding in the operation for burning powder grinding, pre-burning powder is dried and is sieved after grinding.
6. the preparation method of negative temperature coefficient heat-sensitive composition as claimed in claim 5, which is characterized in that will after the grinding
In the step of pre-burning powder is dried and is sieved, the temperature of the drying is 100 DEG C~150 DEG C, and the time of the drying is 2~3 small
When.
7. the preparation method of negative temperature coefficient heat-sensitive composition as claimed in claim 2, which is characterized in that the polyvinyl alcohol
The mass concentration of solution is 4~7%, and the mass ratio of the poly-vinyl alcohol solution and the pre-burning powder is 10:100~15:100.
8. the preparation method of negative temperature coefficient heat-sensitive composition as claimed in claim 2, which is characterized in that the drying process
It is toasted 10~20 minutes specially at 100 DEG C~150 DEG C.
9. the negative temperature coefficient prepared such as the preparation method of the described in any item negative temperature coefficient heat-sensitive compositions of claim 2-8
Heat-sensitive composition.
10. a kind of preparation method of negative tempperature coefficient thermistor chip, which comprises the following steps:
Negative temperature coefficient heat-sensitive composition as claimed in claim 9 is pressed into green compact；
The green compact are sintered 3~5 hours at 1190 DEG C~1230 DEG C and obtain tile；And
Silver paste is applied on two opposite surfaces of the tile, negative tempperature coefficient thermistor chip is obtained after sintering.
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| CN106187184B (en) * | 2016-07-22 | 2019-06-07 | 广东风华高新科技股份有限公司 | Thermistor raw material and its preparation method and application |
| CN107200563A (en) * | 2017-06-28 | 2017-09-26 | 中南大学 | Al Li optimization Ni Zn oxide negative temperature coefficient heat-sensitive resistance materials |
| CN107607216A (en) * | 2017-09-25 | 2018-01-19 | 南京航伽电子科技有限公司 | A kind of temperature transmitter with good compensation performance |
| CN107892557A (en) * | 2017-10-12 | 2018-04-10 | 中南大学 | The nickel zinc oxide NTC thermistor material of Li/Fe modifications |
| CN107857584A (en) * | 2017-10-26 | 2018-03-30 | 中南大学 | A kind of NTC thermistor material based on nickel magnesium-zinc oxide |
| CN109741894B (en) * | 2019-01-14 | 2021-06-25 | 深圳顺络电子股份有限公司 | Method for manufacturing chip negative temperature coefficient thermistor |
| CN113087495B (en) * | 2021-03-31 | 2023-04-07 | 广东风华高新科技股份有限公司 | NTC (negative temperature coefficient) heat-sensitive material as well as preparation method and application thereof |
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| CN102249648B (en) * | 2011-04-01 | 2013-06-19 | 中国科学院新疆理化技术研究所 | Magnesium-containing quaternary system negative temperature coefficient thermistor material |
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