CN101894641B - Method for improving thermosensitive resistor production efficiency - Google Patents
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- CN101894641B CN101894641B CN2010102077705A CN201010207770A CN101894641B CN 101894641 B CN101894641 B CN 101894641B CN 2010102077705 A CN2010102077705 A CN 2010102077705A CN 201010207770 A CN201010207770 A CN 201010207770A CN 101894641 B CN101894641 B CN 101894641B
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- 238000004519 manufacturing process Methods 0.000 title abstract description 19
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- 238000002360 preparation method Methods 0.000 claims abstract description 30
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000005303 weighing Methods 0.000 claims description 15
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 8
- 229910052712 strontium Inorganic materials 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052788 barium Inorganic materials 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
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- 238000003466 welding Methods 0.000 claims description 2
- 229910010252 TiO3 Inorganic materials 0.000 claims 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
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- 239000003795 chemical substances by application Substances 0.000 description 7
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Abstract
The invention discloses a preparation method of a positive temperature coefficient thermosensitive resistor (PTCR), which comprises: synthesizing a primary chip material with a Curie temperature of 40 DEG C and a secondary chip material with a Curie temperature of 140 DEG C by pre-sintering; and mixing the materials according to the Curie temperature required by the customers of the PTCR product. As material preparation production can be performed in advanced, the production period from order receiving to delivery is shortened effectively.
Description
Technical field
(Positive Temperature Coefficient of Resistance, preparation method PTCR), and particularly a kind ofly help enhancing productivity practice thrift the PTCR preparation method of cost to the invention relates to positive temperature coefficient thermistor.
Background technology
The development of PTCR material started from the eighties in last century; Through painstaking efforts for many years; The PTC thermo-sensitive material has developed into the another large-scale electronic material except that capacitor, piezoelectric in China's electronic material, devices field, its output value, output are all in swift and violent increase.
Current, the PTCR performance is the most stable, and that obtain extensive use is BaTiO
3The PTC themistor of system.BaTiO behind the doping vario-property
3Being PTCR the transition of resistance value occurs at its phase transformation temperature points, and this transformation temperature is the Curie temperature of PTCR.The Curie point of PTCR changes with its different purposes, Curie point＜120 of using like demagnetization, current limliting ℃; Motor starting and heating are with the Curie temperature of PTCR then＞120 ℃.Pure BaTiO
3The Curie point of material is 120 ℃.Therefore, obtain the PTC themistor of different Curie points, just should add and can make its Curie point, promptly the phase transition temperature of crystal boundary ferroelectric media layer produces the additive that moves, and is called to move the peak admixture or Curie point moves agent.It gets into the lattice lattice point with the substituted form of solid solution.Usually the peak additive that moves of usefulness has Pb, Sr, Zr, Sn etc.After Pb replaces the Ba position, Curie point is shifted to＞120 ℃ high temperature side; And Sr, Zr, Hf and Sn replace elements corresponding Ba or Ti, and Curie point is moved to＜120 ℃ low temperature direction.
Each moves the peak agent and all has certain mobile efficient.The so-called efficient that moves, promptly refer to every interpolation molar fraction be 1% move the peak additive after, make BaTiO
3The number of degrees that move of Curie point.The common in theory mobile efficient of moving the peak agent is as shown in table 1.But in the actual production, the mobile efficient of moving the peak agent is influenced by several factors, such as other dopant and doping content, sintering condition or the like.
The common mobile efficient of moving the peak agent of table 1.
| Element term | Pb | Sr | Zr | Sn | Hf |
| Efficient (℃/(10 -2mol)) | 4 | -3.7 | -5.3 | -8.0 | -5.0 |
Seeing that the linear relationship of the replacement amount of Sn, Zr, Hf and Curie point is bad, porcelain body crystal grain is thick, causes proof voltage to reduce, old friends Pb and the Sr of adopting more.Known pure SrTiO
3Curie temperature be-250 ℃, pure PbTiO
3Curie temperature be 490 ℃.Practical production experience shows that in certain Curie temperature scope, the mobile efficient of Pb and Sr is suitable, all in (3.5～3.7) ℃/(10
-2Mol).
Move the peak agent except adding Curie temperature, also need add multiple dopant in the preparation process of PTCR, comprising: alms giver, acceptor dopants, sintering aid etc.
Donor dopant makes BaTiO
3Pottery is semi-conductive dopant from insulator transition.ABO
3Type BaTiO
3Be that ptc material donor adulterant commonly used can divide two types: one type is and Ba
2+Ionic radius is close, and chemical valence is higher than Ba
2+Alms giver's element is served as in the replacement A position of ion, and La is generally arranged
3+, Ce
4+, Y
3+Deng rare earth and Bi
3+, Sb
3+Deng; Another kind ofly be and Ti
4+Radius is close, chemical valence is higher than Ti
4+Replacement B position serve as alms giver's element, Nb is generally arranged
5+Ta
5+, Sb
5+Deng.Acceptor impurities such as transition elements Fe, Mn, Cr, Zn, Ni, Co, Cu and Alkali-Metal Na and K all are known obstruction BaTiO
3The impurity of pottery semiconducting.But the kick amplitude when the adding recipient element just can effectively improve sudden change of resistivity in high-purity raw material.Therefore, be to be worth using to preparation PTC thermistor, but addition is answered strict controlling, because the excessive master that receives can make material lose semiconduction.
At BaTiO
3Matrix PTC material prepares in the process, except the alms giver that improves the required adding of its electrical property, led and the admixture of equal value, for each item performance of optimizing resistor and improve sintering process, needs to add certain sintering aid.Because sintering aid at high temperature forms liquid phase, can objectionable impurities be received in crystal boundary, be beneficial to the purifying of crystal grain, can also improve the microstructure of barium titanate, improve proof voltage, reduce voltage effects.Sintering aid also can enlarge the sintering warm area, reduces sintering temperature.The adding of sintering aid can suppress crystal grain misgrowth, and uniform crystal particles is grown up: simultaneously the segregation in crystal boundary of some impurity is come out, material is played the effect of " detoxifcation ", thereby optimize the performance of material.Sintering aid commonly used is SiO
2, Al
2O
3, TiO
2
These additives also influence each other except separately effect of performance, therefore, obtain the PTCR product of function admirable, need debugging constantly, repeatedly research material compositing formula and grope various process conditions.
At present, the PTC resistor has been widely used in every field, relates to the use in green illumination, electric ballast, household electrical appliances, communication, mainly plays overcurrent, overtemperature protection, effects such as preheating delayed startup.
Various, the various performance of products parameter request of PTC resistor product is also different.With the green illumination field is example: owing to be applied in the electronic energy-saving lamp of different occasions, different model, different capacity different startup requirements is arranged, this just needs the corresponding pipeline start up by preheating element PTCR that satisfies the demands.Usually, the Curie temperature of pipeline start up by preheating element PTCR at 50 ℃～120 ℃, room temperature resistance value between 100 Ω～7000 Ω.It is thus clear that the performance of products parameter area is very wide.
This has brought challenge for the production of PTC resistor.Various additives were various during the prescription of PTCR was formed on the one hand, and influenced each other; The production process of PTCR is complicated simultaneously, and the cycle long (referring to Fig. 1, the conventional production process flow process of PTCR); On the other hand, product demand is again multifarious, and client's demand has uncertainty usually, and the client hopes that the delivery cycle is short more good more most the time.If rise that time receiving order, begin tissue production from the development prescription again, usually can affect adversely delivery date, lose confidence and business opportunity.Therefore, how improving the production technology of PTCR, to the client qualified product is provided as scheduled, for enterprise wins benefit and development, is the difficult problem that each PTCR production firm is faced.
Summary of the invention
The present invention proposes a kind of preparation method who helps improving PTCR production efficiency, and it may further comprise the steps:
(1) the synthetic Curie temperature of pre-burning is the negative film material that 40 ℃ main leaf material and Curie temperature is 140 ℃;
(2) according to the quality of following linear equation in two unknowns set of calculated main leaf material and negative film material:
Wherein a is the quality of main leaf material, quality, the T that b is the negative film material
cFor the PTCR product that will prepare Curie temperature, m for the powder quality that will feed intake;
(3) with the main leaf material and the negative film material process ball mill mixing → granulation → moulding → sintering → electrode of institute's weighing, make the PTCR chip;
(4) to the PTCR chip carry out welding lead, seal, test, finished product packing.
Among the preparation method proposed by the invention, the preparation Curie temperature is that 40 ℃ main leaf material may further comprise the steps:
1. form according to following material: (Ba
0.783Sr
0.217) TiO
3+ 3%molTiO
2+ 0.105%molMn
2++ (1.9～2.5) gY
2O
3/ kg+ (4.6～5.5) gSiO
2/ kg, weighing raw materials comprises: BaCO
3, SrCO
3, TiO
2, Mn (NO
3)
2Or MnCO
3, Y
2O
3, SiO
2
2. each raw material that will take by weighing is by material: ball (agate ball): the weight ratio of water (deionized water)=1: 1.5: 1.2～1.5; Ball milling is 24 hours in the Place mill equipment; Discharging oven dry back sintering in high temperature furnace is incubated 2～4 hours under the maximum temperature about 1150 ± 20 ℃, promptly obtain Curie temperature and be 40 ℃ main leaf pre-burning material; Its principal crystalline phase is (Ba, Sr) TiO
3
Among the preparation method proposed by the invention, the preparation Curie temperature is that 140 ℃ negative film material may further comprise the steps:
1. form according to following material: (Ba
0.93Pb
0.05Ca
0.02) TiO
3+ 2.6%molTiO
2+ 0.085%molMn
2++ (1.9～2.5) gY
2O
3/ kg+ (4.6～5.5) gSiO
2/ kg, weighing raw materials comprises: BaCO
3, Pb
3O
4Or PbO or Pb
2O
3, TiO
2, Mn (NO
3)
2Or MnCO
3, Y
2O
3, SiO
2
2. each raw material that will take by weighing is by material: ball (agate ball): the weight ratio of water (deionized water)=1: 1.5: 1.2～1.5; Ball milling is 24 hours in the Place mill equipment; Discharging oven dry back sintering in high temperature furnace is incubated 2～4 hours under the maximum temperature about 1150 ± 20 ℃, promptly obtain Curie temperature and be 140 ℃ negative film pre-burning material; Its principal crystalline phase is (Ba, Pb) TiO
3
Among the preparation method proposed by the invention, purity of raw materials is: the BaCO more than analysis is pure
3, SrCO
3, Y
2O
3, TiO
2The Pb of purity more than chemical pure
3O
4Or PbO or Pb
2O
3
Among the preparation method proposed by the invention, when also being included in for the second time mixing and ball milling, carry out trace doped, with adjustment performance of products parameter.
Among the preparation method proposed by the invention, the production that can feed intake simultaneously of main leaf material and negative film material.
Utilize preparation method proposed by the invention, have following significant advantage:
At first, because main leaf material and negative film material have specific composition and preparation technology, so when the final required product parameters of unknown client, the production of can getting the raw materials ready; And when receiving order, only need the main leaf material after the pre-burning and negative film material are carried out easy configuration, since the second time mixing and ball milling produce, make the production cycle shortened near half, improved efficient greatly, reduced production cost.
Secondly, the present invention has utilized Pb and Sr as moving the peak agent, mixes in the time of Pb and Sr, not only can obtain stable Curie temperature, can also play the effect of crystal grain thinning, has improved the anti-anti-rush of current ability of product significantly.
At last, in the preparation of PTCR, Dope Additive is of a great variety.If to each product, material engineering Shi Doucong component design begins to develop, and wherein from the lab scale to the scale, goes into operation, and need constantly test and grope, and length, the workload in its cycle are big, is difficult to the imagination.But utilize preparation method proposed by the invention, material engineering teacher can carry out the secondary doping of trace in the second time when mixing and ball milling main leaf material and negative film material, reaches the purpose of adjustment product parameters, has significantly alleviated its operating pressure.
Description of drawings
Fig. 1 is existing PTCR technological process of production figure.
Fig. 2 is PTCR technological process of production figure proposed by the invention.
Fig. 3 is that prepared Curie temperature is the resistance temperature curve of 55 ℃ PTCR in the specific embodiment of the invention.
Fig. 4 is that prepared Curie temperature is the resistance temperature curve of 70 ℃ PTCR in the specific embodiment of the invention.
Fig. 5 is that prepared Curie temperature is the resistance temperature curve of 85 ℃ PTCR in the specific embodiment of the invention.
Fig. 6 is that prepared Curie temperature is the resistance temperature curve of 110 ℃ PTCR in the specific embodiment of the invention.
Embodiment
(1) the preparation Curie temperature is 40 ℃ a main leaf material
1. form according to following material: (Ba
0.783Sr
0.217) TiO
3+ 3%molTiO
2+ 0.105%Mn (NO
3)
2+ 2.1gY
2O
3/ kg+5gSiO
2/ kg, weighing raw materials comprises: BaCO
3, SrCO
3, TiO
2, Mn (NO
3)
2, Y
2O
3, SiO
2
2. each raw material that will take by weighing is by material: ball (agate ball): the weight ratio of water (deionized water)=1: 1.5: 1.2～1.5; Ball milling is 24 hours in the Place mill equipment; Discharging oven dry back sintering in high temperature furnace is incubated 2～4 hours under the maximum temperature about 1150 ± 20 ℃, promptly obtain Curie temperature and be 40 ℃ main leaf pre-burning material; Its principal crystalline phase is (Ba, Sr) TiO
3
(2) the preparation Curie temperature is 140 ℃ a negative film material
1. form according to following material: (Ba
0.93Pb
0.05Ca
0.02) TiO
3+ 2.6%molTiO
2+ 0.085%molMn (NO
3)
2+ 2.5gY
2O
3/ kg+5gSiO
2/ kg, weighing raw materials comprises: BaCO
3, CaCO
3, PbO, TiO
2, Mn (NO
3)
2, Y
2O
3, SiO
2
2. each raw material that will take by weighing is by material: ball (agate ball): the weight ratio of water (deionized water)=1: 1.5: 1.2～1.5; Ball milling is 24 hours in the Place mill equipment; Discharging oven dry back sintering in high temperature furnace is incubated 2～4 hours under the maximum temperature about 1150 ± 20 ℃, promptly obtain Curie temperature and be 140 ℃ negative film pre-burning material; Its principal crystalline phase is (Ba, Pb) TiO
3
(3) the preparation Curie temperature is 50～130 ℃ a PTCR resistor
1. according to the quality of following linear equation in two unknowns set of calculated main leaf material and negative film material:
Wherein a is the quality of main leaf material, quality, the T that b is the negative film material
cFor the PTCR product that will prepare Curie temperature, m for the powder quality that will feed intake.
The present invention is that 55 ℃, 70 ℃, 85 ℃, 110 ℃ PTCR product is an example with Curie temperature, and one feeding 100kg distinguishes as shown in table 2 through the quality of calculating its main leaf material and negative film material:
The main leaf material of several kinds of different Curie temperature of table 2. and the quality that feeds intake of negative film material (100kg always feeds intake)
2. according to the amount that table 1 calculated, weighing main leaf material and negative film material, according to material: ball (agate ball): the mass ratio of water (deionized water)=1: 1.5: 1.2～1.5, ball milling is 16～24 hours in the Place mill equipment, carries out granulation after the discharging.
3. powder compression moulding on former that granulation is good.
4. the ceramic chips layering of above-mentioned forming is put on load bearing board, interlayer is used ZrO
2The pad powder separates, and puts in the high temperature furnace, and sintering under air atmosphere, its maximum sintering temperature are 1320～1360 ℃, and insulation 40～60min reduces to 1000 ℃ by the cooling rate of 150～250 ℃/h then.Close the sintering furnace attemperating unit, treat that furnace temperature reduces to room temperature naturally and can take out ceramics.
5. the PTCR ceramics that will accomplish high temperature sintering carries out drying behind surface grinding, shakeout, the wash clean, seal is coated with Al electrode (bottom electrode; 610 ± 10 ℃ of sintering temperatures) or Ag electrode (bottom electrode; 550 ± 10 ℃ of sintering temperatures) and Ag electrode (top layer electrode, 520 ± 10 ℃ of sintering temperatures).
With the magnetic sheet of printed electrode burn-on lead-in wire (immersed solder), seal, testing, sorting, packing.
This instance prepared PTC R element is tested, and its resistance temperature curve is shown in Fig. 3-6.Can know that by test result its Curie temperature Tc25 is respectively: 55.6 ℃, 70.7 ℃, 84.4 ℃, 112.6 ℃
This instance prepared PTC R element is tested, and its traditional performance parameter is following:
1. chip size: Φ 5.0 * 3.0mm, Curie point: Tc=55 ± 5 ℃, room temperature resistivity: (4.0～8.0) * 10
2Ω, temperature coefficient of resistance: about+13%, electric strength:>=1200 volts.
2. chip size: Φ 5.0 * 3.0mm, Curie point: Tc=70 ± 5 ℃, room temperature resistivity: (4.0～8.0) * 10
2Ω, temperature coefficient of resistance: about+14%, electric strength:>=1200 volts.
3. chip size: Φ 5.0 * 3.0mm, Curie point: Tc=85 ± 5 ℃, room temperature resistivity: (4.0～8.0) * 10
2Ω, temperature coefficient of resistance: about+20%, electric strength:>=1200 volts.
4. chip size: Φ 5.0 * 3.0mm, Curie point: Tc=110 ± 5 ℃, room temperature resistivity: (4.0～8.0) * 10
2Ω, temperature coefficient of resistance: about+21%, electric strength:>=1000 volts.
Claims (9)
1. the preparation method of a positive temperature coefficient thermistor PTCR, it may further comprise the steps:
(1) the synthetic Curie temperature of pre-burning is the negative film material that 40 ℃ main leaf material and Curie temperature is 140 ℃;
(2) according to the quality of following linear equation in two unknowns set of calculated main leaf material and negative film material:
Wherein a is the quality of main leaf material, quality, the T that b is the negative film material
cFor the PTCR product that will prepare Curie temperature, m for the powder quality that will feed intake;
(3) with the main leaf material and the negative film material process ball mill mixing → granulation → moulding → sintering → electrode of institute's weighing, make the PTCR chip.
2. positive temperature coefficient thermistor PTCR preparation method as claimed in claim 1 comprises also wherein that the PTCR chip carries out welding lead, seals, test, finished product packing.
3. according to claim 1 or claim 2 PTCR preparation method, the main leaf material that wherein prepares Curie temperature and be 40 ℃ may further comprise the steps:
(1) forms according to following material: (Ba
0.783Sr
0.217) TiO
3+ 3%molTiO
2+ 0.105%molMn
2++ (1.9～2.5) gY
2O
3/ kg+ (4.6～5.5) gSiO
2/ kg, weighing raw materials comprises: BaCO
3, SrCO
3, TiO
2, Mn (NO
3)
2Or MnCO
3, Y
2O
3, SiO
2
Each raw material that (2) will take by weighing is by material: ball: the weight ratio of water=1: 1.5: 1.2～1.5; Ball milling is 16～24 hours in the Place mill equipment; Discharging oven dry back sintering in high temperature furnace is incubated 2～4 hours under 1150 ± 20 ℃ maximum temperature, promptly obtain Curie temperature and be 40 ℃ main leaf pre-burning material; Its principal crystalline phase is (Ba, Sr) TiO
3
4. according to claim 1 or claim 2 positive temperature coefficient thermistor PTCR preparation method, the negative film material that wherein prepares Curie temperature and be 140 ℃ may further comprise the steps:
(1) forms according to following material: (Ba
0.93Pb
0.05Ca
0.02) TiO3+2.6%molTiO2+0.085%molMn
2++ (1.9～2.5) gY
2O
3/ kg+ (4.6～5.5) gSiO
2/ kg, weighing raw materials comprises: BaCO
3, CaCO
3, Pb
3O
4Or PbO or Pb
2O
3, TiO
2, Mn (NO
3)
2Or MnCO
3, Y
2O
3, SiO
2
Each raw material that (2) will take by weighing is by material: ball: the weight ratio of water=1: 1.5: 1.2～1.5; Ball milling is 16～24 hours in the Place mill equipment; Discharging oven dry back sintering in high temperature furnace is incubated 2～4 hours under 1150 ± 20 ℃ maximum temperature, promptly obtain Curie temperature and be 140 ℃ negative film pre-burning material; Its principal crystalline phase is (Ba, Pb) TiO
3
5. positive temperature coefficient thermistor PTCR preparation method as claimed in claim 3, wherein raw material BaCO
3, SrCO
3, Y
2O
3, TiO
2, Mn (NO
3)
2Or MnCO
3, SiO
2Purity for analyze pure more than.
6. positive temperature coefficient thermistor PTCR preparation method as claimed in claim 4, wherein raw material BaCO
3, CaCO
3, TiO
2, Mn (NO
3)
2Or MnCO
3, Y
2O
3, SiO
2Purity for analyze pure more than, and Pb
3O
4Or PbO or Pb
2O
3Purity be more than the chemical pure.
7. positive temperature coefficient thermistor PTCR preparation method as claimed in claim 3, wherein ball is an agate ball, water is deionized water.
8. positive temperature coefficient thermistor PTCR preparation method as claimed in claim 4, wherein ball is an agate ball, water is deionized water.
9. according to claim 1 or claim 2 positive temperature coefficient thermistor PTCR preparation method, wherein main leaf material and negative film material can be produced simultaneously.
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|---|---|---|---|
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|---|---|---|---|
| CN2010102077705A CN101894641B (en) | 2010-06-23 | 2010-06-23 | Method for improving thermosensitive resistor production efficiency |
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|---|---|---|---|---|
| CN102617134A (en) * | 2012-03-26 | 2012-08-01 | 常熟市林芝电子有限责任公司 | Thermal sensitive ceramic material, thermal resistor made of thermal sensitive ceramic material and used for heating, and manufacture method for thermal resistor |
| CN102617136A (en) * | 2012-03-26 | 2012-08-01 | 常熟市林芝电子有限责任公司 | Thermosensitive ceramic material and electromobile thermosensitive resistor made of thermosensitive ceramic material and manufacturing method of thermosensitive resistor |
| CN103971870A (en) * | 2014-02-19 | 2014-08-06 | 贵州凯里经济开发区中昊电子有限公司 | Polymer thermosensitive resistor core material and product preparation method thereof |
| CN106145933A (en) * | 2016-06-12 | 2016-11-23 | 上海大学 | A kind of high-curie temperature (Tc > 190 DEG C) low lead PTCR ceramic material preparation method |
| CN108164252A (en) * | 2017-12-12 | 2018-06-15 | 孝感华工高理电子有限公司 | A kind of PTC raw powder's production technologies |
| CN113651612A (en) * | 2021-08-13 | 2021-11-16 | 湖州南木纳米科技有限公司 | Barium titanate PTC thermal sensitive ceramic material and application thereof in lithium battery |
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| CN1160273A (en) * | 1997-02-26 | 1997-09-24 | 清华大学 | Medium- and low-temp. sintered combined characteristic thermosensitive resistor material composition and preparing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1160273A (en) * | 1997-02-26 | 1997-09-24 | 清华大学 | Medium- and low-temp. sintered combined characteristic thermosensitive resistor material composition and preparing method |
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