CN100568408C - A kind of low resistance/high B value slice heat sensitive resistor and manufacture method thereof - Google Patents
A kind of low resistance/high B value slice heat sensitive resistor and manufacture method thereof Download PDFInfo
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- CN100568408C CN100568408C CNB2007101137730A CN200710113773A CN100568408C CN 100568408 C CN100568408 C CN 100568408C CN B2007101137730 A CNB2007101137730 A CN B2007101137730A CN 200710113773 A CN200710113773 A CN 200710113773A CN 100568408 C CN100568408 C CN 100568408C
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 238000005516 engineering process Methods 0.000 claims abstract description 20
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 14
- 238000005755 formation reaction Methods 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 239000012528 membrane Substances 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 7
- 238000010276 construction Methods 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 3
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 18
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 4
- 238000003746 solid phase reaction Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 description 8
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920002689 polyvinyl acetate Polymers 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241001504664 Crossocheilus latius Species 0.000 description 1
- 229910017945 Cu—Ti Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention discloses the slice heat sensitive resistor in a kind of sensor technology of areas of information technology, disclose a kind of low resistance/high B value slice heat sensitive resistor and manufacture method thereof especially.This low resistance/high B value slice heat sensitive resistor, its special character is: the chip of element is by the composite construction of folder one floor height B value heat-sensitive layer between two conductive formations, and conductive formation is made of Mn-Ni-Cu-Ca, and high B value layer is made of Mn-Co-Cu-Ti-Nb; Make low resistance diaphragm that forms conductive formation and the high B value diaphragm that forms high B value heat-sensitive layer respectively with pricking membrane technology, and coincide and make compound film sheet, high-temperature calcination forms the temperature-sensitive chip, through cutting and chip NTCR is made in the termination electrode making.The present invention has adopted low resistivity layer and stacking the closing of high B value, has reduced the resistance of element widely.It is simple to have technology, low cost of manufacture, the characteristics of being convenient to produce in enormous quantities.
Description
(1) technical field
The present invention relates to the slice heat sensitive resistor in the sensor technology of areas of information technology, particularly a kind of low resistance/high B value slice heat sensitive resistor and manufacture method thereof.
(2) background technology
Slice heat sensitive resistor is the indispensable basic element of mechanics of communication, computer technology and instrument and meter industry.Slice heat sensitive resistor also is the important directions of thermistor industry development.At present both at home and abroad the slice heat sensitive resistor of producing (0805,0603,0402) all is to be raw material with transition metal oxide, and the use casting technique is made.The B value is the material constant of thermistor, and promptly the chip of thermistor forms the material with certain resistivity through behind the high temperature sintering.The B value can be calculated after measuring the resistance value when 25 degrees centigrade and 50 degrees centigrade (or 85 degrees centigrade); B value and the positive correlation of product temperature coefficient of resistance that is to say that the B value is big more, and its temperature coefficient of resistance is also just big more; Temperature coefficient just is meant every rising 1 degree of temperature, the rate of change of resistance value; Along with variation of temperature, its resistance change of product that the B value is big is bigger, that is to say sensitiveer.In order to realize the low resistance/high B value element, use sandwich construction usually.Yet the diffusion of metal ion when the costliness of the inner electrode that sandwich construction brings and high temperature sintering causes the material B value to descend, and resistance is dispersed to be increased; And termination electrode when electroplating extension and the corrosion of porcelain body, make the strong variation of machinery of element, the reliability of element degenerates.The casting technique apparatus expensive, complex process, the production cycle is long, makes and the manufacturing cost of product increases.
In recent years, people have done the thermo-sensitive material that all attempts attempt preparations have low-resistivity and high B value, realize the slice heat sensitive resistor of low-resistance/high B value with single chip architecture.Also there is the method for human protection porcelain body to prepare termination electrode, exempt from the extension that it is corroded and stop electrode, but problem just fails still fundamentally to be resolved so far.
(3) summary of the invention
The present invention provides the low resistance/high B value slice heat sensitive resistor and the manufacture method thereof of a kind of precision height, low cost of manufacture in order to remedy the deficiencies in the prior art.
The present invention is achieved through the following technical solutions:
A kind of low resistance/high B value slice heat sensitive resistor, its special character is: the chip of element is by the composite construction of folder one floor height B value heat-sensitive layer between two conductive formations, and conductive formation is made of Mn-Ni-Cu-Ca, and high B value layer is made of Mn-Co-Cu-Ti-Nb; Make low resistance diaphragm that forms conductive formation and the high B value diaphragm that forms high B value heat-sensitive layer respectively with rolling membrane technology, and coincide and make compound film sheet, high-temperature calcination forms the temperature-sensitive chip, through cutting and chip NTCR is made in the termination electrode making.
Low resistance/high B value slice heat sensitive resistor of the present invention, the material of conductive formation is the oxide of Mn-Ni-Cu-Ca, the mol ratio between it is: Mn: Ni: Cu: Ca=2.6: 1.3: 1.8: 0.3.Conductive formation is to be MnO by percentage by weight
2: NiO: CuO: CaO=43.845%: 18.834%: 34.058%: 3.263% composition, oxide synthesizes the heat-sensitive powder with low-resistivity for the powder solid phase reaction, and its granularity is 5-10um.
Low resistance/high B value slice heat sensitive resistor of the present invention, the material of high B value layer is the oxide of Mn-Co-Cu-Ti-Nb, the mol ratio between it is: Mn: Co: Cu: Ti: Nb=3.6: 1.4: 0.6: 0.2: 0.2.High B value layer is to be MnO by percentage by weight
2: Co
3O
4: CuO: TiO
2: Nb
2O
3Form at=62.222%: 22.338%: 9.505%: 3.168%: 2.767%, and high B value layer material is made the thermo-sensitive material powder with high B value for the powder solid phase reaction.
The manufacture method of low resistance/high B value slice heat sensitive resistor of the present invention, employing is rolled membrane technology and is prepared low resistance diaphragm and high B value diaphragm, synthetic powder and PVA glue with low resistance synthesis material and high B value is made into slurry respectively, respectively it is rolled the diaphragm that grinds into institute's required thickness on roll forming machine; The thickness of low resistance film is 5-10 times of high B value thickness.
The manufacture method of low resistance/high B value slice heat sensitive resistor of the present invention, slurry are polyvinyl alcohol, and the weight proportion between powder and the polyvinyl alcohol is: powder: polyvinyl alcohol=(90-92): (10-8).Composite membrane at high temperature burns till the temperature-sensitive chip with low-resistance and high B value, and sintering process comprises shaping, binder removal, sintering, and the shaping temperature is 150 ℃, and dump temperature is 200-500 ℃, and sintering temperature is 1100-1250 ℃.
Principle of the present invention and concrete scheme:
1, the preparation of low resistance/low B value diaphragm
Low resistance/low B value diaphragm is to utilize the Mn-Ni-Cu-Ca material, and this material forms spinel structure when high temperature sintering, and the Cu ion is in the B position in the AB2O4 structure, provides a large amount of 4d electronics to participate in conduction, makes the resistivity of material very low; The 4S electronics of Ca ion out orbit directly enters conduction band, the progressive resistance that reduces.Low resistance/low B value thin slice is with above-mentioned material, by prescription: MnO
2: the ratio ground and mixed of NiO: CuO: CaO=43.845%: 18.834%: 34.058%: 3.26%wt, 700 ℃/(2.5-3) hour pre-burning, grind to form for the second time the powder that granularity is 1-5um, 4-5%PVA glue mixed roll film in the powder and make, its thickness requires to decide according to element.
2, high B value preparation of sections
High B value thin slice utilizes the Mn-Co-Cu-Ti material.Form spinel structure during this material at high temperature sintering, Co is in the B position of AB2O4, forms higher activation energy higher B value is provided.Add the Ti ion simultaneously, make it to assemble, improve the crystal boundary potential barrier, further improve the B value at the edge of crystalline substance.MnO is pressed in the preparation of diaphragm
2: Co
3O
4: CuO: TiO
2: Nb
2O
3=62.222%: 22.338%: 9.505%: 3.168%: 2.767% batching adopts the identical manufacture method of low-resistance web preparation, and the thickness of high B value film is 1/5 or 1/10 of low resistance diaphragm thickness.The common burning temperature of two kinds of diaphragms depends on the content of Cu, if the content of Cu is identical, then sintering temperature is identical.
3, the preparation of compound chip
Compound chip is that its gross thickness is (2 * 5)+0.5=10.5mm with low resistance diaphragm (is 5mm such as thickness) therebetween one floor height B value diaphragm (such as 0.5mm).The composite sheet roll compacting of 10.5mm thickness is become the composite membrane base sheet of 1mm with roll forming machine.This moment, the thickness of high B value film became 0.05mm, and behind the sintering, chip thickness will become 0.8mm (shrinkage 20%).Element to 0603, compacting thickness should be controlled at about 1.0mm is advisable.Make 0402 chip NTCR according to this method, nominal resistance is 100, B25/50=3400-3600K; 0603 chip NTCR, nominal resistance are 47 Ω, and the B value is 3600-3800K.
The present invention utilizes oxide semiconductor low-resistance/low B value and high resistant/high B value inherent characteristic, with low-resistivity/low B value layer one one as electrode, high resistant/high B value layer is made responsive to temperature partly, with two-layer series connection, realize low resistance/high B value slice heat sensitive resistor, 0402 chip NTCR, nominal resistance are 100 Ω, B25/50=3400-3600K; 0603 chip NTCR, nominal resistance are 47 Ω, and the B value is 3600-3800K.This is that sandwich construction is incomparable.
The present invention has overcome an interior electrode difficult problem and the contradiction of element low resistance and high B value and the problem that element exchanges low precision that exists on the existing slice heat sensitive resistor technology of preparing.The present invention has adopted low resistivity layer and stacking the closing of high B value, and the equal proportion thinning technique can be thinned to 0.001mm with high B value layer, has reduced the resistance of element widely.Low resistivity layer and high B value are homogeneous material, can not produce ion diffusion and thermal stress mutually during high temperature sintering.Low resistivity layer is done the shielding of high B value, can not cause during plating that electrode extends the resistance that changes element, thereby guarantee the precision of element.It is simple that the present invention has technology, low cost of manufacture, the characteristics of being convenient to produce in enormous quantities.
(4) embodiment
Embodiment 1:
1. the preparation of low-resistance diaphragm
Get the MnO of chemical pure (C.R)
2, NiO, CuO and CaO be by weight 43.845%: 18.834%: 34.058%: 3.267% weighing is the ZrO of Φ 6 with diameter
2Ball, by expecting: water: ball=1.0: 1.1: 1.5 (wt) ground 12 hours on planetary ball mill, 90 ℃ of oven dry down, and crossed 200 mesh sieves, and the powder that sieves is contained in the ceramic alms bowl in pre-burning in 700 ℃/2 hours; Powder after the pre-burning advanced for the second time ball milling 16-18 hour (method with the first time ball milling identical).Powder behind the ball milling was dried 250 mesh sieves for the second time.
2. roll film
With adding the PVA sol solution (solution concentration is 20%) of 40-50%wt in the powder, fully stir, and place the normal temperature of relative humidity 95% to keep fermentation in 12 hours down.Slurry after fermentation is directly put into to roll and is rolled stone roller on the film, constantly adjusts the gap of roll forming machine, till diaphragm thickness reaches 5mm.
Use the same method high B value material, MnO
2: Co
3O
4: CuO: TiO
2: Nb
2O
3Make diaphragm that thickness be 0.3mm at=62.222%: 22.338%: 9.505%: 3.168%: 2.767%.
3. preparation compound film sheet
On smooth glass plate, put one deck low-resistance diaphragm, put a floor height B value diaphragm then thereon, put one deck low-resistance diaphragm above again, form the Sandwich structure, on compound film sheet, press a plate glass and weight; Behind the static pressure 30min, take off compound film sheet and on roll forming machine, it is ground into the chip green compact that gross thickness is 1.0mm.
4. sintering
The compound chip green compact are cut into the square sheet of 40m * 40mm, mix ZrO
2Powder (bonding die when preventing sintering) overlays in the porcelain alms bowl, presses pouring weight (pouring weight weight is decided on the base sheet).Sintering temperature curve is
5. element is made
The element chip that the rear sheet is cut into 0402 size will be burnt.Closed-end technology manufacturing terminal electrode with chip NTCR commonly used.Promptly with silver slurry end-blocking, electroplated Ni and Sn then.
6. test result (with 100 chips statistics)
R25/Ω B25/50/K H/mw C/sec ΔR/R/％ ΔB/B/％
103.1 3520 3.0 8.0 ±8 ±0.8
Embodiment 2:
With the identical technology of embodiment 1, the green compact thickness of low-resistance diaphragm is taken as 8mm, high B value diaphragm green compact thickness is taken as 0.2mm, gross thickness after compound is 1.0mm, be cut into 0603 chip behind the sintering, the manufacturing terminal electrode is measured result such as following table (with 100 chip statistics) in thermostat according to a conventional method
R25/Ω B25/50/K H/mw C/sec ΔR/R/％ ΔB/B/％
50.8 3485 3.58 ±7 ±0.7
Embodiment 3:
With embodiment 1 same technology and method, the prescription of high B value diaphragm is taken as MnO
2: Co
3O
4: CuO: TiO: Nb
2O
3=62.5%: 23.565%: 8.0%: 3.168%: 2.767%, the green compact thickness of low-resistance diaphragm is 5mm, the green compact thickness of high B value film is that the green compact thickness of 0.1mm compound film sheet is 1.1mm, the chip that is cut into 0402 size behind the sintering is the manufacturing terminal electrode according to a conventional method, test result such as following table (with 100 chips statistics)
R25/Ω B25/50/K H/mw C/sec ΔR/R/％ ΔB/B/％
302.2 3942 2.5 8.0 ±7.2 ±1.0
The foregoing description 1, the result of embodiment 2 and embodiment 3 shows that technology provided by the invention can realize low resistance/high B value slice formula NTCR easily.Compare with the chip NTCR of sandwich construction, it has the more B value of low resistance and Geng Gao, and technology is simple, low cost of manufacture.The technology of the present invention is applicable to production in enormous quantities.
Claims (8)
1, a kind of low resistance/high B value slice heat sensitive resistor, it is characterized in that: the chip of element is by the composite construction of folder one floor height B value heat-sensitive layer between two conductive formations, conductive formation is made of the Mn-Ni-Cu-Ca oxide, and high B value layer is made of the Mn-Co-Cu-Ti-Nb oxide; Make the low resistance diaphragm of conductive formation and the high B value diaphragm of high B value heat-sensitive layer respectively with rolling membrane technology, and coincide and make compound film sheet, high-temperature calcination forms the temperature-sensitive chip, makes chip negative temperature coefficient thermistor through cutting and termination electrode making.
2, low resistance/high B value slice heat sensitive resistor according to claim 1 is characterized in that: conductive formation Mn-Ni-Cu-Ca oxide, the mol ratio between it is: Mn: Ni: Cu: Ca=2.6: 1.3: 1.8: 0.3.
3, low resistance/high B value slice heat sensitive resistor according to claim 2 is characterized in that: oxide synthesizes the heat-sensitive powder with low-resistivity for the powder solid phase reaction, and its granularity is 5-10um.
4, low resistance/high B value slice heat sensitive resistor according to claim 1 is characterized in that: high B value layer Mn-Co-Cu-Ti-Nb oxide, the mol ratio between it is: Mn: Co: Cu: Ti: Nb=3.6: 1.4: 0.6: 0.2: 0.2.
5, low resistance/high B value slice heat sensitive resistor according to claim 4 is characterized in that: high B value layer material is made the thermo-sensitive material powder with high B value for the powder solid phase reaction.
6, according to the manufacture method of the described low resistance/high B value slice heat sensitive resistor of claim 1, it is characterized in that: employing is rolled membrane technology and is prepared low resistance diaphragm and high B value diaphragm, synthetic powder and polyvinyl alcohol with low resistance synthesis material and high B value is made into slurry respectively, respectively it rolled the diaphragm that grinds into institute's required thickness on roll forming machine; The thickness of low resistance film is 5-10 times of high B value thickness.
7, the manufacture method of low resistance/high B value slice heat sensitive resistor according to claim 6 is characterized in that: the weight proportion between powder and the polyvinyl alcohol is: powder: polyvinyl alcohol=(90-92): (10-8).
8, the manufacture method of low resistance/high B value slice heat sensitive resistor according to claim 6, it is characterized in that: composite membrane at high temperature burns till the temperature-sensitive chip with low-resistance and high B value, sintering process comprises shaping, binder removal, sintering, the shaping temperature is 150 ℃, dump temperature is 200-500 ℃, and sintering temperature is 1100-1250 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101137730A CN100568408C (en) | 2007-09-12 | 2007-09-12 | A kind of low resistance/high B value slice heat sensitive resistor and manufacture method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101137730A CN100568408C (en) | 2007-09-12 | 2007-09-12 | A kind of low resistance/high B value slice heat sensitive resistor and manufacture method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101123134A CN101123134A (en) | 2008-02-13 |
| CN100568408C true CN100568408C (en) | 2009-12-09 |
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|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101618959B (en) * | 2009-07-28 | 2012-05-23 | 四川西汉电子科技有限责任公司 | Low-resistivity and high-B-value negative temperature coefficient thermosensitive material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4531110A (en) * | 1981-09-14 | 1985-07-23 | At&T Bell Laboratories | Negative temperature coefficient thermistors |
| JP2000357603A (en) * | 1999-06-16 | 2000-12-26 | Mitsubishi Materials Corp | Chip type thermistor and manufacturing method thereof |
| CN1405798A (en) * | 2002-11-06 | 2003-03-26 | 祝翌 | Chip negative temperature coefficient thermistor and its pure wet manufacturing method |
| CN101022048A (en) * | 2007-03-23 | 2007-08-22 | 上海维安热电材料股份有限公司 | Sheet type NTC and producing method thereof |
-
2007
- 2007-09-12 CN CNB2007101137730A patent/CN100568408C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4531110A (en) * | 1981-09-14 | 1985-07-23 | At&T Bell Laboratories | Negative temperature coefficient thermistors |
| JP2000357603A (en) * | 1999-06-16 | 2000-12-26 | Mitsubishi Materials Corp | Chip type thermistor and manufacturing method thereof |
| CN1405798A (en) * | 2002-11-06 | 2003-03-26 | 祝翌 | Chip negative temperature coefficient thermistor and its pure wet manufacturing method |
| CN101022048A (en) * | 2007-03-23 | 2007-08-22 | 上海维安热电材料股份有限公司 | Sheet type NTC and producing method thereof |
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