CN1744240A - A kind of deep low temperature oxide thermosensitive resistor material - Google Patents
A kind of deep low temperature oxide thermosensitive resistor material Download PDFInfo
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Abstract
The present invention relates to a kind of deep low temperature oxide thermosensitive resistor material, this material is with strontium carbonate or strontium oxide strontia and cobalt sesquioxide carries out direct solid phase reaction or adopt chemical method to synthesize non-stoichiometric perovskite structure oxide SrCoO with nitrate
1-xNi
xO
3-5(0≤δ≤0.1,0≤δ≤0.5) material, its parameter is compared with the existing approved product that uses under liquid oxygen, liquid nitrogen, liquid hydrogen temperature after tested, and the element that draws can use under the 4.2K-20K temperature, and use warm area than broad, also do not reduced cost owing to do not contain rare earth element.
Description
Technical field
The present invention relates to a kind of profound hypothermia NTC oxide thermosensitive resistor material of extensive use on a kind of aerospace engineering and the cryogenic technique.
Background technology
Profound hypothermia negative temperature coefficient (NTC) thermistor is used for the temperature survey and the control of aerospace engineering and cryogenic science technology, and the transducer of low-temperature measurement commonly used at present, control and liquid level indication has: platinum resistance thermometer, germanium thermometer thermometer, helium temperature meter etc.But platinum, germanium thermometer are affected by magnetic fields big, and gas thermometer can not directly produce the signal of telecommunication and be not easy to miniaturization, and that oxide thermistor has is highly sensitive, and thermal inertia is little, low price, advantage such as little affected by magnetic fields.Therefore oxide thermistor has its special status on low-temperature physics and cryogenic engineering, is that the ideal of other low-temperature test transducers substitutes device.
The basic theoretical formula of semiconductor temperature-sensitive ceramic component:
A
nDecisions such as shape and size by thermistor; B
nBe the thermistor material constant, by the physical characteristic decision of material; T is an absolute temperature.
According to above formula, in order to guarantee that resistance value is not higher than a certain use permissible value under the low temperature, must select B value materials with smaller as can be known with the reduction of serviceability temperature, the profound hypothermia thermistor requires material that less B value is arranged.
Profound hypothermia NTC thermistor has a wide range of applications on low-temperature physics, cryogenic engineering, the approved product that uses under liquid oxygen, liquid nitrogen, liquid hydrogen temperature is only arranged at present, also do not have at present the more following product that uses of low temperature, and the material of product is the composite ceramic material that transition metal synthesizes with rare earth doped modification mostly.
Non-stoichiometric perovskite structure oxide SrCoO
1-xNi
xO
3-5(0≤δ≤0.1,0≤δ≤0.5) has conductivity metal at normal temperatures, and the reduction resistivity increase with serviceability temperature has NTC semiconductive ceramic characteristic.Through measuring the resistance under liquid oxygen, the liquid nitrogen temperature, calculate the B value of its material, carry out parameter relatively with existing low temperature thermistor material (Mn-Ni-Cu-La system, Mn-Ni-Cu-Nb based material), as shown in the table:
| Material | Mn-Ni-Cu-La | Mn-Ni-Cu-Nb | SrCoO 1-xNi xO 3-5 (0≤δ≤0.1， (0≤δ≤0.5) |
| Serviceability temperature | 4.2K-20K | 20K-77K | Be lower than 20K |
| The B value | 247K | 343K | 35K |
Can estimate SrCoO thus
1-xNi
xO
3-5The NTC thermistor element that (0≤δ≤0.1,0≤δ≤0.5) material is made can use being lower than under the temperature of 20K.The present invention is according to non-stoichiometric perovskite structure oxide SrCoO
1-xNi
xO
3-5(0≤δ≤0.1,0≤δ≤0.5) this characteristic adopts distinct methods to synthesize profound hypothermia NTC thermistor material.
Summary of the invention
The objective of the invention is to, developing a kind of deep low temperature oxide thermosensitive resistor material, is with one or both carry out direct solid phase reaction or adopt the synthetic non-stoichiometric perovskite structure oxide SrCoO of chemical method with nitrate in strontium carbonate or strontium oxide strontia and cobalt sesquioxide, the nickel sesquioxide
1-xNi
xO
3-5(0≤δ≤0.1,0≤δ≤0.5) material, its parameter is compared with the existing approved product that uses under liquid oxygen, liquid nitrogen, liquid hydrogen temperature after tested, and the element that draws can use being lower than under the 4.2K-20K temperature, and use warm area than broad, also do not reduced cost owing to do not contain rare earth element.
A kind of deep low temperature oxide thermosensitive resistor material of the present invention, this material is to be raw material with stoichiometry strontium carbonate, strontium oxide strontia, cobalt sesquioxide and nickel sesquioxide, with one or both carry out direct solid phase reaction in strontium carbonate or strontium oxide strontia and cobalt sesquioxide, the nickel sesquioxide, at the levigate mixing of agate mortar, presintering grinds to form powder again; Or make raw material with nitrate and prepare powder with chemical coprecipitation or sol-gel process; Then the powder that makes is made electrode with platinum wire, the moulding of some pearl is carried out high temperature sintering and is become porcelain, the globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead, the employing glass packaging gets final product, and its electrical parameter is: B value 35K-100K, 25 ℃ of resistance 0.2-500 Ω.
A kind of preparation method of deep low temperature oxide thermosensitive resistor material follows these steps to carry out:
A, at first take by weighing by 1: 1 mol ratio that one or both carry out direct solid phase reaction in strontium carbonate or strontium oxide strontia and cobalt sesquioxide, the nickel sesquioxide, grind at agate mortar, levigate mixing then 800-900 ℃ of presintering, grinds to form powder again after the presintering;
Or adopt nitrate to make raw material to prepare powder with chemical coprecipitation, the nitric acid that 1: 1 mol ratio divides the another name strontium nitrate, contain 6 crystallizations water bores and contains the nickel nitrate of 6 crystallizations water, is dissolved in the 200ml deionized water, and magnetic agitation system is dissolved fully; Claim 0.15mol oxalic acid to be dissolved in that heating is stirred to dissolving fully in the 800ml deionized water, then nitrate mixed solution slowly added in the oxalic acid solution that the limit edged stirs, with ammoniacal liquor transfer pH value between the 9-12 till precipitation fully; With the quiet placement of precipitation solution precipitation deposition fully, till the PH=7, be deposited in 80 ℃ of oven for drying with washed with de-ionized water, grind mixing at agate mortar then, 600 ℃ of constant temperature decomposed in 2 hours, ground to form powder after the decomposition again;
Or adopt nitrate to make raw material to prepare powder with methods such as sol-gels, 1: 1 mol ratio divides the another name strontium nitrate, contain the cobalt nitrate of 6 crystallizations water and contain the nickel nitrate of 6 crystallizations water, is dissolved in the 200ml deionized water, and magnetic agitation system is dissolved fully, nitrate mixed solution adds excessive citric acid, add thermal agitation,, colloidal sol is placed on 80 ℃ of oven for drying to forming colloidal sol, form gel, grind mixing at agate mortar then, 500 ℃ of constant temperature decomposed in 2 hours, ground to form powder after the decomposition again;
B, then the powder that makes is added 5-10% starch solution as adhesive, make electrode with platinum wire, two interelectrode spacings are 0.1-0.3mm, the moulding of some pearl, pearl body size 0.8-1.2mm; Globule after the moulding is embedded in the corundum crucible that analysis pure zirconia aluminium powder is housed, becomes porcelain at 1000-1150 ℃ of high temperature sintering; Has perovskite structure through the XRD test; The globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead with spot welding machine, adopts glass packaging, measures the parameter as thermistor material.
Embodiment
Embodiment 1
A, be to take by weighing strontium oxide strontia (900 ℃ of decomposition of strontium carbonate make) at 1: 1 to creep into the direct solid phase reaction of row at first in molar ratio, grind that levigate mixing then 800 ℃ of presintering 4 hours, grinds to form powder again after the presintering at agate mortar with three oxidations two;
B, with adding 10% starch solution in the powder that makes as adhesive, make electrode with platinum wire, two interelectrode spacings are 0.2mm, the moulding of some pearl, pearl body size 0.8mm; Globule after the moulding is embedded in the corundum crucible that analysis pure zirconia aluminium powder is housed, sintered porcelain in 6 hours at 1075 ℃ of constant temperature; The globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead with spot welding machine, adopts glass packaging, measures the parameter as thermistor material, and its B value is at 35k, 25 ℃ of resistance 8 Ω.
Embodiment 2
A, be to take by weighing strontium oxide strontia (strontium carbonate 900 ℃ decomposition make) at 1: 1 and nickel sesquioxide carries out direct solid phase reaction at first in molar ratio, grind that levigate mixing then 850 ℃ of presintering 6 hours, grinds to form powder again after the presintering at agate mortar;
B, with adding 8% starch solution in the powder that makes as adhesive, make electrode with platinum wire, two interelectrode spacings are 0.1mm, the moulding of some pearl, pearl body size 1.0mm; Globule after the moulding is embedded in the corundum crucible that analysis pure zirconia aluminium powder is housed, sintered porcelain in 4 hours into through 1100 ℃ of constant temperature of high temperature; The globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead with spot welding machine, adopts glass packaging, measures the parameter as thermistor material, and its B value is at 35k, 25 ℃ of resistance 0.5 Ω.
Embodiment 3
A, be to take by weighing strontium carbonate at 1: 1 and cobalt sesquioxide grinds at agate mortar at first in molar ratio, levigate mixing then 900 ℃ of presintering 4 hours, grinds to form powder again after the presintering;
B, with adding 5% starch solution in the powder that makes as adhesive, make electrode with platinum wire, two interelectrode spacings are 0.2mm, the moulding of some pearl, pearl body size 1.2mm; Globule after the moulding is embedded in the corundum crucible that analysis pure zirconia aluminium powder is housed, sintered porcelain in 6 hours into through 1000 ℃ of constant temperature of high temperature; The globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead with spot welding machine, adopts glass packaging, measures the parameter as thermistor material, and its B value is at 35k, 25 ℃ of resistance 50 Ω.
Embodiment 4
A, be to take by weighing strontium carbonate at 1: 1 and nickel sesquioxide grinds at agate mortar at first in molar ratio, levigate mixing then 800 ℃ of presintering 5 hours, grinds to form powder again after the presintering;
B, with adding 6.5% starch solution in the powder that makes as adhesive, make electrode with platinum wire, two interelectrode spacings are 0.3mm, the moulding of some pearl, pearl body size 0.7mm; Globule after the moulding is embedded in the corundum crucible that analysis pure zirconia aluminium powder is housed, sintered porcelain in 2 hours into through 1150 ℃ of constant temperature of high temperature; The globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead with spot welding machine, adopts glass packaging, measures the parameter as thermistor material, and its B value is at 45k, 25 ℃ of resistance 0.3 Ω.
Embodiment 5
A, be to take by weighing strontium carbonate, cobalt sesquioxide and nickel sesquioxide at 1: 0.95: 0.05 to grind at agate mortar at first in molar ratio, levigate mixing then 900 ℃ of presintering 4 hours, grinds to form powder again after the presintering;
B, with adding 10% starch solution in the powder that makes as adhesive, make electrode with platinum wire, two interelectrode spacings are 0.3mm, the moulding of some pearl, pearl body size 0.8mm; Globule after the moulding is embedded in the corundum crucible that analysis pure zirconia aluminium powder is housed, sintered porcelain in 2 hours into through 1100 ℃ of constant temperature of high temperature; The globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead with spot welding machine, adopts glass packaging, measures the parameter as thermistor material, and its B value is at 57k, 25 ℃ of resistance 2.5 Ω.
Embodiment 6
A, at first in molar ratio be take by weighing strontium carbonate at 1: 0.9: 0.1, three oxidations two are bored and nickel sesquioxide grinds at agate mortar, levigate mixing then 900 ℃ of presintering 5 hours, grinds to form powder again after the presintering;
B, with adding 9.5% starch solution in the powder that makes as adhesive, make electrode with platinum wire, two interelectrode spacings are 0.15mm, the moulding of some pearl, pearl body size 0.8mm; Globule after the moulding is embedded in the corundum crucible that analysis pure zirconia aluminium powder is housed, sintered porcelain in 6 hours into through 1150 ℃ of constant temperature of high temperature; The globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead with spot welding machine, adopts glass packaging, measures the parameter as thermistor material, and its B value is at 99k, 25 ℃ of resistance 500 Ω.
Embodiment 7
A, with chemical coprecipitation method oxygenerating powder: the cobalt nitrate that divides another name 0.05mol strontium nitrate and 0.05mol to contain 6 crystallizations water is dissolved in the 200ml deionized water, magnetic agitation system is dissolved fully, title 0.15mol oxalic acid is dissolved in heating in the 800ml district ionized water and is stirred to dissolving fully, slowly add nitrate mixed solution in the oxalic acid solution then, stir while adding, transfer between the pH value 9-12 till precipitation fully with ammoniacal liquor; With the quiet placement of precipitation solution precipitation deposition fully, till the PH=7, be deposited in 80 ℃ of oven for drying with washed with de-ionized water, grind mixing at agate mortar then, 600 ℃ of constant temperature decomposed in 2 hours, ground to form powder after the decomposition again;
B, with adding 5% starch solution in the powder that makes as adhesive, make electrode with platinum wire, two interelectrode spacings are 0.2mm, the moulding of some pearl, pearl body size 0.8mm; Globule after the moulding is embedded in the corundum crucible that analysis pure zirconia aluminium powder is housed, sintered porcelain in 4 hours into through 1100 ℃ of constant temperature of high temperature; The globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead with spot welding machine, adopts glass packaging, measures the parameter as thermistor material, and its B value is at 35k, 25 ℃ of resistance 0.2 Ω.
Embodiment 8
A, with chemical coprecipitation method oxygenerating powder: the nickel nitrate that cobalt nitrate, the 0.005mol that divides another name 0.05mol strontium nitrate and 0.045mol to contain 6 crystallizations water contains 6 crystallizations water is dissolved in the 200ml deionized water, magnetic agitation system is dissolved fully, title 0.15mol oxalic acid is dissolved in heating in the 800ml district ionized water and is stirred to dissolving fully, slowly add nitrate mixed solution in the oxalic acid solution then, stir while adding, transfer between the pH value 9-12 till precipitation fully with ammoniacal liquor; With the quiet placement of precipitation solution precipitation deposition fully, till the PH=7, be deposited in 80 ℃ of oven for drying with washed with de-ionized water, grind mixing at agate mortar then, 600 ℃ of constant temperature decomposed in 2 hours, ground to form powder after the decomposition again;
B, with adding 5% starch solution in the powder that makes as adhesive, make electrode with platinum wire, two interelectrode spacings are 0.1mm, the moulding of some pearl, pearl body size 1.0mm; Globule after the moulding is embedded in the corundum crucible that analysis pure zirconia aluminium powder is housed, sintered porcelain in 4 hours into through 1100 ℃ of constant temperature of high temperature; The globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead with spot welding machine, adopts glass packaging, measures the parameter as thermistor material, and its B value is at 47k, 25 ℃ of resistance 2.0 Ω.
Embodiment 9
A, with sol-gel process oxygenerating powder: the cobalt nitrate that divides another name 0.05mol strontium nitrate and 0.05mol to contain 6 crystallizations water is dissolved in the 200ml deionized water, magnetic agitation system is dissolved fully, excessive citric acid will be added in the nitrate mixed solution, add thermal agitation,, colloidal sol is placed on 80 ℃ of oven for drying to forming colloidal sol, form gel, grind mixing at agate mortar then, 500 ℃ of constant temperature decomposed in 2 hours, ground to form powder after the decomposition again;
B, with adding 7% starch solution in the powder that makes as adhesive, make electrode with platinum wire, two interelectrode spacings are 0.3mm, the moulding of some pearl, pearl body size 1.2mm; Globule after the moulding is embedded in the corundum crucible that analysis pure zirconia aluminium powder is housed, sintered porcelain in 4 hours into through 1000 ℃ of constant temperature of high temperature; The globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead with spot welding machine, adopts glass packaging, measures the parameter as thermistor material, and its B value is at 35k, 25 ℃ of resistance 0.2 Ω.
Embodiment 10
A, with sol-gel process oxygenerating powder: the nickel nitrate that cobalt nitrate, the 0.005mol that divides another name 0.05mol strontium nitrate and 0.045mol to contain 6 crystallizations water contains 6 crystallizations water is dissolved in the 200ml deionized water, magnetic agitation system is dissolved fully, excessive citric acid will be added in the nitrate mixed solution, add thermal agitation,, colloidal sol is placed on 80 ℃ of oven for drying to forming colloidal sol, form gel, grind mixing at agate mortar then, 500 ℃ of constant temperature decomposed in 2 hours, ground to form powder after the decomposition again;
B, with adding 10% starch solution in the powder that makes as adhesive, make electrode with platinum wire, two interelectrode spacings are 0.3mm, the moulding of some pearl, pearl body size 0.8mm; Globule after the moulding is embedded in the corundum crucible that analysis pure zirconia aluminium powder is housed, sintered porcelain in 4 hours into through 1100 ℃ of constant temperature of high temperature; The globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead with spot welding machine, adopts glass packaging, measures the parameter as thermistor material, and its B value is at 46k, 25 ℃ of resistance 2.0 Ω.
Claims (2)
1, a kind of deep low temperature oxide thermosensitive resistor material, it is characterized in that this material is is raw material with stoichiometry strontium carbonate, strontium oxide strontia, cobalt sesquioxide and nickel sesquioxide, with one or both carry out direct solid phase reaction in strontium carbonate or strontium oxide strontia and cobalt sesquioxide, the nickel sesquioxide, at the levigate mixing of agate mortar, presintering grinds to form powder again; Or make raw material with nitrate and prepare powder with chemical coprecipitation or sol-gel process; Then the powder that makes is made electrode with platinum wire, the moulding of some pearl is carried out high temperature sintering and is become porcelain, the globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead, the employing glass packaging gets final product, and its electrical parameter is: B value 35K-100K, 25 ℃ of resistance 0.2-500 Ω.
2, the preparation method of a kind of deep low temperature oxide thermosensitive resistor material according to claim 1 is characterized in that following these steps to carrying out:
A, at first take by weighing by 1: 1 mol ratio that one or both carry out direct solid phase reaction in strontium carbonate or strontium oxide strontia and cobalt sesquioxide, the nickel sesquioxide, grind at agate mortar, levigate mixing is then 800-900 ℃ of presintering, time 4-6 hour, grind to form powder after the presintering again;
Or adopt nitrate to make raw material to prepare powder with chemical coprecipitation, divide the strontium nitrate that has another name called, contain the cobalt nitrate of 6 crystallizations water and contain the nickel nitrate of 6 crystallizations water by 1: 1 mol ratio, be dissolved in the 200ml deionized water, magnetic agitation system is dissolved fully; Title 0.15mol oxalic acid is dissolved in heating in the 800ml deionized water and is stirred to dissolving fully, then nitrate mixed solution is slowly added in the oxalic acid solution, and the limit edged stirs, and transfers pH value between 9-12 with ammoniacal liquor, till precipitating fully; With the quiet placement of precipitation solution precipitation deposition fully, till the PH=7, be deposited in 80 ℃ of oven for drying with washed with de-ionized water, grind mixing at agate mortar then, 600 ℃ of constant temperature decomposed in 2 hours, ground to form powder after the decomposition again;
Or adopt nitrate to make raw material to prepare powder with methods such as sol-gels, divide the another name strontium nitrate, contain the cobalt nitrate of 6 crystallizations water and contain the nickel nitrate of 6 crystallizations water by 1: 1 mol ratio, be dissolved in the 200ml deionized water, magnetic agitation system is dissolved fully, nitrate mixed solution adds excessive citric acid, add thermal agitation, to forming colloidal sol; Colloidal sol is placed on 80 ℃ of oven for drying, forms gel, grind mixing at agate mortar then, 500 ℃ of constant temperature decomposed in 2 hours, ground to form powder after the decomposition again;
B, then the powder that makes is added 5-10% starch solution as adhesive, make electrode with platinum wire, two interelectrode spacings are 0.1-0.3mm, the moulding of some pearl, pearl body size 0.8-1.2mm; Globule after the moulding is embedded in the corundum crucible that analysis pure zirconia aluminium powder is housed, becomes porcelain at 1000-1150 ℃ of high temperature sintering; Has perovskite structure through the XRD test; The globule that sinters porcelain into is welded in the platinum wire electrode points on the Dumet wire outer lead with spot welding machine, adopts glass packaging, measures the parameter as thermistor material.
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| CNB2005101065502A CN100555479C (en) | 2005-09-30 | 2005-09-30 | A kind of deep low temperature oxide thermosensitive resistor material and manufacture method thereof |
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| CN100555479C CN100555479C (en) | 2009-10-28 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104051094A (en) * | 2014-06-30 | 2014-09-17 | 句容市博远电子有限公司 | Multicomponent system thermistor with strontium oxide |
| CN105810377A (en) * | 2016-05-24 | 2016-07-27 | 怀远县金浩电子科技有限公司 | Liquid-phase preparation method of thermistor powder material |
| CN109133201A (en) * | 2018-09-19 | 2019-01-04 | 北京科技大学 | Based on the Ni-based perovskite oxide material of A codopes of multicomponent and application method |
| CN109269662A (en) * | 2018-09-19 | 2019-01-25 | 北京科技大学 | Rare-earth Ni-base perovskite oxide thermistor material applied to infrared acquisition |
| CN110698189A (en) * | 2019-11-15 | 2020-01-17 | 中国科学院新疆理化技术研究所 | Lanthanum ion doped deep low temperature thermistor material and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3996411B2 (en) * | 2002-03-05 | 2007-10-24 | Ｔｄｋ株式会社 | Composite NTC thermistor |
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2005
- 2005-09-30 CN CNB2005101065502A patent/CN100555479C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104051094A (en) * | 2014-06-30 | 2014-09-17 | 句容市博远电子有限公司 | Multicomponent system thermistor with strontium oxide |
| CN105810377A (en) * | 2016-05-24 | 2016-07-27 | 怀远县金浩电子科技有限公司 | Liquid-phase preparation method of thermistor powder material |
| CN109133201A (en) * | 2018-09-19 | 2019-01-04 | 北京科技大学 | Based on the Ni-based perovskite oxide material of A codopes of multicomponent and application method |
| CN109269662A (en) * | 2018-09-19 | 2019-01-25 | 北京科技大学 | Rare-earth Ni-base perovskite oxide thermistor material applied to infrared acquisition |
| CN110698189A (en) * | 2019-11-15 | 2020-01-17 | 中国科学院新疆理化技术研究所 | Lanthanum ion doped deep low temperature thermistor material and preparation method thereof |
| CN110698189B (en) * | 2019-11-15 | 2021-11-02 | 中国科学院新疆理化技术研究所 | Lanthanum ion doped deep low temperature thermistor material and preparation method thereof |
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