CN1274737A - Room temperature solid-phase reaction of thermosensitive powder with negative temperature coefficient - Google Patents
Room temperature solid-phase reaction of thermosensitive powder with negative temperature coefficient Download PDFInfo
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- CN1274737A CN1274737A CN 99106687 CN99106687A CN1274737A CN 1274737 A CN1274737 A CN 1274737A CN 99106687 CN99106687 CN 99106687 CN 99106687 A CN99106687 A CN 99106687A CN 1274737 A CN1274737 A CN 1274737A
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Abstract
Powdered material is first obtained by means of full grinding manganese acetate, nickel acetate, cobalt acetate, and mangesium acetate, mixing the ground material with oxalic acid, and subsequent treatment including drying, pre-decomposition, thermal decomposition and grinding, and then mixed with organic adhesive, sieved, pelletized, tableted, sintered and heat treated to obtain the thermosensitive powder. Compared with couventional ball grinding process, co-precipitation process and sol-gel process, the said process has the features of low reaction temperature, no need of solvent for reaction, high yield, short synthetic period, easy-to-control reaction condition, wide application range, etc.
Description
The present invention relates to a kind of preparation method-room temperature solid-phase coordination chemical reaction method of negative temperature coefficient heat-sensitive powder
The preparation method of negative temperature coefficient heat-sensitive powder usually adopts ball milled, coprecipitation method, sol-gel processing etc., and these methods when reaction the temperature height, synthesis cycle is long, reaction conditions is difficult to control and a large amount of solvent of needs when reaction.The present invention is directed to the problem of existence,, develop room temperature solid-phase coordination chemical reaction method is adopted in the preparation of negative temperature coefficient heat-sensitive powder through a large amount of experiments.
The object of the invention is, preparation method-room temperature the solid state reaction of the negative temperature coefficient heat-sensitive powder of development, be manganese acetate, nickel acetate, Cobaltous diacetate, magnesium acetate fully to be ground the back mix with oxalic acid, handle then, drying, predecomposition, thermolysis, grinding promptly get powder, add organic binder bond again, the granulation of sieving, be pressed into steps such as disk, sintering, thermal treatment and make; Adopt this method to compare, have characteristics such as temperature of reaction is low, reaction need not solvent, productive rate height, synthesis cycle weak point, easily-controlled reaction conditions, applied widely with ball milled, coprecipitation method, sol-gel processing.
Preparation method-room temperature the solid state reaction of the negative temperature coefficient heat-sensitive powder of the present invention's development, the branch following steps are carried out:
At first manganese acetate, nickel acetate, Cobaltous diacetate, magnesium acetate are fully ground, manganese acetate after will grinding, nickel acetate, Cobaltous diacetate, magnesium acetate mix with the oxalic acid of equimolar amount, fully grind 1 hour, put into microwave oven then and handle 2 minutes, place 70 ℃ of dryings again, grind and be powder.
Powder after will grinding is again put into muffle furnace 150-250 ℃ of predecomposition 4 hours, then 800-900 ℃ of thermolysis 4 hours, fully grinds and obtains the negative temperature coefficient heat-sensitive powder.
Mix the granulation of sieving, dry-pressing formed sequin with adding 3% polyvinyl alcohol organic binder bond in the gained temperature-sensitive powder again, then the disk biscuit is put into the globars box-type furnace, at 1150-1300 ℃ of sintering, sintering time is 3-6 hour, and heating-cooling speed is 60 ℃/hour; Adopt palladium-silver conductive paste to prepare electrode on the sintered sheets two sides, 150 ℃ of following thermal treatments 200 hours, the lead-in wire of burn-oning, R25 ℃ of mensuration, R50 ℃ obtain B value, resistivity, resistance varying-ratio and get final product in thermostatic oil bath.
Embodiment 1 (content is unit with the mole)
At first 3.6mol manganese acetate, 2.4mol nickel acetate are fully ground, mix, fully ground 1 hour, put into microwave oven then and handled 2 minutes, place 70 ℃ of dryings again, grind and be powder with the oxalic acid of equimolar amount.
Powder after will grinding is again put into muffle furnace 150-250 ℃ of predecomposition 4 hours, then 800-900 ℃ of thermolysis 4 hours, fully grinds and obtains the negative temperature coefficient heat-sensitive powder.
Mix the granulation of sieving, dry-pressing formed sequin with adding 3% polyvinyl alcohol organic binder bond in the gained temperature-sensitive powder again, then the disk biscuit is put into the globars box-type furnace, at 1150-1300 ℃ of sintering, sintering time is 3-6 hour, and heating-cooling speed is 60 ℃/hour; Adopt palladium-silver conductive paste to prepare electrode on the sintered sheets two sides, 150 ℃ of following thermal treatments 200 hours, the lead-in wire of burn-oning, the B value of R25 ℃ of mensuration, R50 ℃ is 3780K in thermostatic oil bath, resistivity P is 2100 Ω .cm, resistance varying-ratio+1.2%.
Embodiment 2 (content is unit with the mole)
At first 4mol manganese acetate, 2mol nickel acetate are fully ground, mix, fully ground 1 hour, put into microwave oven then and handled 2 minutes, place 70 ℃ of dryings again, grind and be powder with the oxalic acid of equimolar amount.
Powder after will grinding is again put into muffle furnace 150-250 ℃ of predecomposition 4 hours, then 800-900 ℃ of thermolysis 4 hours, fully grinds and obtains the negative temperature coefficient heat-sensitive powder.
Mix the granulation of sieving, dry-pressing formed sequin with adding 3% polyvinyl alcohol organic binder bond in the gained temperature-sensitive powder again, then the disk biscuit is put into the globars box-type furnace, at 1150-1300 ℃ of sintering, sintering time is 3-6 hour, and heating-cooling speed is 60 ℃/hour; Adopt palladium-silver conductive paste to prepare electrode on the sintered sheets two sides, 150 ℃ of following thermal treatments 200 hours, the lead-in wire of burn-oning, the B value of R25 ℃ of mensuration, R50 ℃ is 3820K in thermostatic oil bath, resistivity P is 2400 Ω .cm, resistance varying-ratio+1.4%
Embodiment 3 (content is unit with the mole)
At first 3.7mol manganese acetate, 1.7mol nickel acetate, 0.6mol Cobaltous diacetate are fully ground, mix, fully ground 1 hour, put into microwave oven then and handled 2 minutes, place 70 ℃ of dryings again, grind and be powder with the oxalic acid of equimolar amount.
Powder after will grinding is again put into muffle furnace 150-250 ℃ of predecomposition 4 hours, then 800-900 ℃ of thermolysis 4 hours, fully grinds and obtains the negative temperature coefficient heat-sensitive powder.
Mix the granulation of sieving, dry-pressing formed sequin with adding 3% polyvinyl alcohol organic binder bond in the gained temperature-sensitive powder again, then the disk biscuit is put into the globars box-type furnace, at 1150-1300 ℃ of sintering, sintering time is 3-6 hour, and heating-cooling speed is 60 ℃/hour; Adopt palladium-silver conductive paste to prepare electrode on the sintered sheets two sides, 150 ℃ of following thermal treatments 200 hours, the lead-in wire of burn-oning, the B value of R25 ℃ of mensuration, R50 ℃ is 3615K in thermostatic oil bath, resistivity P is 1680 Ω .cm, resistance varying-ratio+0.8%.
Embodiment 4 (content is unit with the mole)
At first 3.1mol manganese acetate, 2.3mol nickel acetate, 0.6mol Cobaltous diacetate are fully ground, mix, fully ground 1 hour, put into microwave oven then and handled 2 minutes, place 70 ℃ of dryings again, grind and be powder with the oxalic acid of equimolar amount.
Powder after will grinding is again put into muffle furnace 150-250 ℃ of predecomposition 4 hours, then 800-900 ℃ of thermolysis 4 hours, fully grinds and obtains the negative temperature coefficient heat-sensitive powder.
Mix the granulation of sieving, dry-pressing formed sequin with adding 3% polyvinyl alcohol organic binder bond in the gained temperature-sensitive powder again, then the disk biscuit is put into the globars box-type furnace, at 1150-1300 ℃ of sintering, sintering time is 3-6 hour, and heating-cooling speed is 60 ℃/hour; Adopt palladium-silver conductive paste to prepare electrode on the sintered sheets two sides, 150 ℃ of following thermal treatments 200 hours, the lead-in wire of burn-oning, the B value of R25 ℃ of mensuration, R50 ℃ is 3550K in thermostatic oil bath, resistivity P is 1070 Ω .cm, resistance varying-ratio+0.8%.
Embodiment 5 (content is unit with the mole)
At first 3mol manganese acetate, 1mol nickel acetate, 2mol magnesium acetate are fully ground, mix, fully ground 1 hour, put into microwave oven then and handled 2 minutes, place 70 ℃ of dryings again, grind and be powder with the oxalic acid of equimolar amount.
Powder after will grinding is again put into muffle furnace 150-250 ℃ of predecomposition 4 hours, then 800-900 ℃ of thermolysis 4 hours, fully grinds and obtains the negative temperature coefficient heat-sensitive powder.
Mix the granulation of sieving, dry-pressing formed sequin with adding 3% polyvinyl alcohol organic binder bond in the gained temperature-sensitive powder again, then the disk biscuit is put into the globars box-type furnace, at 1150-1300 ℃ of sintering, sintering time is 3-6 hour, and heating-cooling speed is 60 ℃/hour; Adopt palladium-silver conductive paste to prepare electrode on the sintered sheets two sides, 150 ℃ of following thermal treatments 200 hours, the lead-in wire of burn-oning, the B value of R25 ℃ of mensuration, R50 ℃ is 4190K in thermostatic oil bath, resistivity P is 35500 Ω .cm, resistance varying-ratio+0.4%.
Embodiment 6 (content is unit with the mole)
At first 3.2mol manganese acetate, 0.8mol nickel acetate, 2.2mol magnesium acetate are fully ground, mix, fully ground 1 hour, put into microwave oven then and handled 2 minutes, place 70 ℃ of dryings again, grind and be powder with the oxalic acid of equimolar amount.
Powder after will grinding is again put into muffle furnace 150-250 ℃ of predecomposition 4 hours, then 800-900 ℃ of thermolysis 4 hours, fully grinds and obtains the negative temperature coefficient heat-sensitive powder.
Mix the granulation of sieving, dry-pressing formed sequin with adding 3% polyvinyl alcohol organic binder bond in the gained temperature-sensitive powder again, then the disk biscuit is put into the globars box-type furnace, at 1150-1300 ℃ of sintering, sintering time is 3-6 hour, and heating-cooling speed is 60 ℃/hour; Adopt palladium-silver conductive paste to prepare electrode on the sintered sheets two sides, 150 ℃ of following thermal treatments 200 hours, the lead-in wire of burn-oning, the B value of R25 ℃ of mensuration, R50 ℃ is 4280K in thermostatic oil bath, resistivity P is 14300 Ω .cm, resistance varying-ratio+0.3%.
Claims (1)
1, a kind of preparation method of negative temperature coefficient heat-sensitive powder-room temperature solid state reaction is characterized in that, the branch following steps are carried out:
At first manganese acetate, nickel acetate, Cobaltous diacetate, magnesium acetate are fully ground, manganese acetate after will grinding, nickel acetate, Cobaltous diacetate, magnesium acetate mix with the oxalic acid of equimolar amount, fully grind 1 hour, put into microwave oven then and handle 2 minutes, place 70 ℃ of dryings again, grind and be powder.
Powder after will grinding is again put into muffle furnace 150-250 ℃ of predecomposition 4 hours, then 800-900 ℃ of thermolysis 4 hours, fully grinds and obtains the negative temperature coefficient heat-sensitive powder.
Mix the granulation of sieving, dry-pressing formed sequin with adding 3% polyvinyl alcohol organic binder bond in the gained temperature-sensitive powder again, then the disk biscuit is put into the globars box-type furnace, at 1150-1300 ℃ of sintering, sintering time is 3-6 hour, and heating-cooling speed is 60 ℃/hour; Adopt palladium-silver conductive paste to prepare electrode on the sintered sheets two sides, 150 ℃ of following thermal treatments 200 hours, the lead-in wire of burn-oning, R25 ℃ of mensuration, R50 ℃ obtain B value, resistivity, resistance varying-ratio and get final product in thermostatic oil bath.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99106687 CN1093159C (en) | 1999-05-24 | 1999-05-24 | Room temperature solid-phase reaction of thermosensitive powder with negative temperature coefficient |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99106687 CN1093159C (en) | 1999-05-24 | 1999-05-24 | Room temperature solid-phase reaction of thermosensitive powder with negative temperature coefficient |
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| CN1274737A true CN1274737A (en) | 2000-11-29 |
| CN1093159C CN1093159C (en) | 2002-10-23 |
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| CN 99106687 Expired - Fee Related CN1093159C (en) | 1999-05-24 | 1999-05-24 | Room temperature solid-phase reaction of thermosensitive powder with negative temperature coefficient |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7887713B2 (en) | 2003-01-24 | 2011-02-15 | Epcos Ag | Method for producing an electronic component |
| CN102249648A (en) * | 2011-04-01 | 2011-11-23 | 中国科学院新疆理化技术研究所 | Magnesium-containing quaternary system negative temperature coefficient thermistor material |
| CN101318814B (en) * | 2008-07-10 | 2012-03-21 | 中国计量学院 | Hydrothermal reaction method for manufacturing negative temperature coefficient heat-sensitive powder |
-
1999
- 1999-05-24 CN CN 99106687 patent/CN1093159C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7887713B2 (en) | 2003-01-24 | 2011-02-15 | Epcos Ag | Method for producing an electronic component |
| CN101318814B (en) * | 2008-07-10 | 2012-03-21 | 中国计量学院 | Hydrothermal reaction method for manufacturing negative temperature coefficient heat-sensitive powder |
| CN102249648A (en) * | 2011-04-01 | 2011-11-23 | 中国科学院新疆理化技术研究所 | Magnesium-containing quaternary system negative temperature coefficient thermistor material |
| 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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| Publication number | Publication date |
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| CN1093159C (en) | 2002-10-23 |
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