CN1296945C - Method of using acetate to prepare heat sensitire resistance oxide nano-powder - Google Patents
Method of using acetate to prepare heat sensitire resistance oxide nano-powder Download PDFInfo
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- CN1296945C CN1296945C CNB031542611A CN03154261A CN1296945C CN 1296945 C CN1296945 C CN 1296945C CN B031542611 A CNB031542611 A CN B031542611A CN 03154261 A CN03154261 A CN 03154261A CN 1296945 C CN1296945 C CN 1296945C
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Abstract
The present invention relates to a method of using acetate to prepare heat sensitive resistance oxide nano-powder. The method takes Co, Mn and Ni as raw materials of acetates, oxalic acid is used as a precipitating agent, and finally, mixing heat resistance oxide nano-powder of the acetates of Co, Mn and Ni can be prepared through the processes of mixing, coprecipitation, washing, distributed processing, drying and calcining. Granular size of the powder is usually in a range of 50 to 150 nm. The powder prepared by the method is a high-performance NTC heat sensitive resistor with the advantages of high resistance value consistency, high B value consistency and good interchanging performance.
Description
Technical field
The present invention relates to a kind of method for preparing NTC thermistor nm-class oxide powder with acetate.
Background technology
Coprecipitation is meant in containing the mixed solution of multiple metal cation salt and adds precipitation reagent, makes the method for all ion coprecipitations, can obtain composition and precipitate uniformly.It is the important method that preparation contains the composite oxides of two or more metallic elements.At present, coprecipitation is widely used in preparing the super-fine powder or the nano-powder material of functional ceramic such as sensitive material, ferrite, fluorescent material.The present invention compares through the analysis-by-synthesis to many preparation methods according to the liquid phase coprecipitation technology, has found out a kind of method of using acetate to prepare the thermistor nm-class oxide powder.
Summary of the invention
The object of the invention is to study a kind of method for preparing the thermistor nm-class oxide powder with acetate.It is raw material that this method adopts the acetate of Co, Mn, Ni, and oxalic acid is precipitation reagent, handles through operations such as stirring, co-precipitation, washing, dispersion treatment, oven dry, calcinings and prepares the thermistor nano-powder at last.The powder granule size as occurs soft-agglomeratedly generally in the 50-150nm scope, and the agglomerated particle size does not generally wait at the 0.1-4 mu m range.Powder is the spinel structure phase.
The general traditional handicraft of oxide powder of preparation thermistor is a mechanical milling method, is not easy mixing with the powder component of this method preparation and reaches very even, and thermistor element resistance value consistency and the B value consistent performance manufactured are relatively poor.Have component and mix and adopt liquid-phase coprecipitation to prepare oxide powder, purity, controllable granularity, the powder granule degree is thinner, can realize that particle evenly mixes at atom, molecular level, preparation technology is fairly simple, equipment requirements is few, NTC thermistor with low cost, preparation can have high electrical resistance value consistency and B value consistency, exchange advantages such as better performances, therefore good practical value and application prospect are arranged.
Of the present inventionly prepare the method for thermistor nm-class oxide powder, press routine step and carry out with acetate:
A, take by weighing the acetate of Co, Mn, Ni as raw material at first respectively, its ratio is: Co: Mn: Ni=30-65: 20-40: 10-30, mix and dissolve in the deionized water, control metal ion acetate molar concentration is 0.05-0.4mol/L, is configured to the major constituent mixed solution;
B, usefulness oxalic acid are configured to precipitant solution as precipitation reagent, take by weighing with metal ion acetate mole ratio to be 1-2.0: the pure oxalic acid of 1 analysis dissolves in the deionized water, abundant stirring and dissolving, and the control molar concentration is 0.05-0.2mol/L;
C, Co, Mn, Ni acetate mixed solution slowly poured into carry out coprecipitation reaction in the oxalic acid precipitation agent solution, temperature is 10 ℃-80 ℃, constantly stirs in the time of reaction, with ammoniacal liquor pH value is controlled at 5-6;
D, the solution left standstill that reaction is finished fully deposit it, suction filtration or topple over the clear liquid of sediment top, with the sediment that deposits, wash with deionized water, clean dispersion treatment with absolute ethyl alcohol then, put into baking oven and carry out dried, to remove moisture in the powder at 60 ℃-100 ℃;
E, taking-up powder, grind dispersion treatment, powder is carried out calcination processing at 360-600 ℃, time 40-50 minute, promptly obtain Co-Mn-Ni ternary system thermistor nm-class oxide powder, the powder granule size is in the 50-150 nanometer, calcining heat is not being reunited below 400 ℃, and calcining heat is having soft-agglomeratedly more than 400 ℃, as occur soft-agglomeratedly, and the agglomerated particle size is at 0.1-4 μ m.
Embodiment
Embodiment 1
A, at first by Co: Mn: Ni=30: take by weighing at 40: 30 and to analyze pure cobalt acetate, manganese acetate, nickel acetate chemical reagent, mix and dissolve in the deionized water, control metal ion acetate molar concentration is 0.05mol/L, is configured to the major constituent mixed solution;
B, with oxalic acid as precipitation reagent, be configured to precipitant solution, take by weighing with metal ion acetate mole ratio be that 1.2: 1 the pure oxalic acid of analysis dissolves in the deionized water, abundant stirring and dissolving, the control molar concentration is 0.05mol/L;
C, Co, Mn, Ni acetate mixed solution slowly poured into carry out coprecipitation reaction in the oxalic acid precipitation agent solution, temperature is 10 ℃, constantly stirs in the time of reaction, with ammoniacal liquor pH value is controlled at 5;
D, the solution left standstill that reaction is finished fully deposit it, suction filtration or topple over the clear liquid of sediment top, with the sediment that deposits, wash with deionized water, clean dispersion treatment with absolute ethyl alcohol then, put into baking oven and carry out dried, to remove moisture in the powder at 60 ℃;
E, take out powder, grind dispersion treatment, powder is carried out calcination processing at 360 ℃, 40 minutes time, promptly obtain Co-Mn-Ni ternary system thermistor nm-class oxide powder, the powder granule size is in the 50-150 nanometer, no agglomerated particle.
Embodiment 2
A, at first by Co: Mn: Ni=50: take by weighing at 40: 10 and to analyze pure cobalt acetate, manganese acetate, nickel acetate chemical reagent, mix and dissolve in the deionized water, control metal ion acetate molar concentration is 0.2mol/L, is configured to the major constituent mixed solution;
B, with oxalic acid as precipitation reagent, be configured to precipitant solution, take by weighing with metal ion acetate mole ratio be that 1.5: 1 the pure oxalic acid of analysis dissolves in the deionized water, abundant stirring and dissolving, the control molar concentration is 0.1mol/L;
C, Co, Mn, Ni acetate mixed solution slowly poured into carry out coprecipitation reaction in the oxalic acid precipitation agent solution, temperature is 50 ℃, constantly stirs in the time of reaction, with ammoniacal liquor pH value is controlled at 6;
D, the solution left standstill that reaction is finished fully deposit it, suction filtration or topple over the clear liquid of sediment top, with the sediment that deposits, wash with deionized water, clean dispersion treatment with absolute ethyl alcohol then, put into baking oven and carry out dried, to remove moisture in the powder at 80 ℃;
E, taking-up powder grind dispersion treatment, and powder is carried out calcination processing at 460 ℃, 45 minutes time promptly obtained Co-Mn-Ni ternary system thermistor nm-class oxide powder, and the powder granule size is in the 60-120 nanometer, have soft-agglomeratedly, the agglomerated particle size is at 0.5-2 μ m.
Embodiment 3
A, at first by Co: Mn: Ni=65: take by weighing at 20: 15 and to analyze pure cobalt acetate, manganese acetate, nickel acetate chemical reagent, mix and dissolve in the deionized water, control metal ion acetate molar concentration is 0.4mol/L, is configured to the major constituent mixed solution;
B, with oxalic acid as precipitation reagent, be configured to precipitant solution, take by weighing with metal ion acetate mole ratio be that 2.0: 1 the pure oxalic acid of analysis dissolves in the deionized water, abundant stirring and dissolving, the control molar concentration is 0.2mol/L;
C, Co, Mn, Ni acetate mixed solution slowly poured into carry out coprecipitation reaction in the oxalic acid precipitation agent solution, temperature is 80 ℃, constantly stirs in the time of reaction, with ammoniacal liquor pH value is controlled at 6;
D, the solution left standstill that reaction is finished fully deposit it, suction filtration or topple over the clear liquid of sediment top, with the sediment that deposits, wash with deionized water, clean dispersion treatment with absolute ethyl alcohol then, put into baking oven and carry out dried, to remove moisture in the powder at 100 ℃;
E, taking-up powder grind dispersion treatment, and powder is carried out calcination processing at 600 ℃, 50 minutes time promptly obtained Co-Mn-Ni ternary system thermistor nm-class oxide powder, and the powder granule size is in the 80-150 nanometer, occur soft-agglomeratedly, the agglomerated particle size is at 1-4 μ m.
Claims (1)
1, a kind ofly prepare the method for thermistor nm-class oxide powder, it is characterized in that pressing routine step and carry out with acetate:
A, take by weighing the acetate of Co, Mn, Ni as raw material at first respectively, its ratio is: Co: Mn: Ni=30-65: 20-40: 10-30, mix and dissolve in the deionized water, control metal ion molar concentration is 0.05-0.4mol/L, is configured to the major constituent mixed solution;
B, usefulness oxalic acid are configured to precipitant solution as precipitation reagent, take by weighing with metal ion acetate mole ratio to be 1-2.0: the pure oxalic acid of 1 analysis dissolves in the deionized water, abundant stirring and dissolving, and the control molar concentration is 0.05-0.2mol/L;
C, Co, Mn, Ni acetate mixed solution slowly poured into carry out coprecipitation reaction in the oxalic acid precipitation agent solution, temperature is 10 ℃-80 ℃, constantly stirs in the time of reaction, with ammoniacal liquor pH value is controlled at 5-6;
D, the solution left standstill that reaction is finished fully deposit it, suction filtration or topple over the clear liquid of sediment top, with the sediment that deposits, wash with deionized water, clean dispersion treatment with absolute ethyl alcohol then, put into baking oven and carry out dried, to remove moisture in the powder at 60 ℃-100 ℃;
E, taking-up powder, grind dispersion treatment, powder is carried out calcination processing at 360 1 600 ℃, time 40-50 minute, promptly obtain Co-Mn-Ni ternary system thermistor nm-class oxide powder, the powder granule size is in the 50-150 nanometer, calcining heat is not being reunited below 400 ℃, and calcining heat is having soft-agglomeratedly more than 400 ℃, as occur soft-agglomeratedly, and the agglomerated particle size is at 0.1-4 μ m.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB031542611A CN1296945C (en) | 2003-08-16 | 2003-08-16 | Method of using acetate to prepare heat sensitire resistance oxide nano-powder |
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| CNB031542611A CN1296945C (en) | 2003-08-16 | 2003-08-16 | Method of using acetate to prepare heat sensitire resistance oxide nano-powder |
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| CN1514448A CN1514448A (en) | 2004-07-21 |
| CN1296945C true CN1296945C (en) | 2007-01-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110372336A (en) * | 2019-08-19 | 2019-10-25 | 陈龙 | A kind of CoNiO2The co-precipitation method of thermistor powder |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104347202B (en) * | 2013-07-30 | 2017-12-08 | 中国振华集团云科电子有限公司 | A kind of preparation method of thick-film negative temp coefficient resistance slurry |
| CN109516780A (en) * | 2018-11-29 | 2019-03-26 | 镇江爱豪科思电子科技有限公司 | A kind of high-stability negative temperature coefficient heat-sensitive resistance material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0869903A (en) * | 1994-08-30 | 1996-03-12 | Tokin Corp | Manufacture of ntc thermistor |
| CN1185631A (en) * | 1996-12-14 | 1998-06-24 | 中国科学院新疆物理研究所 | Oxidate semi-condcutor thermo-sensitive resistance and mfg. method thereof |
-
2003
- 2003-08-16 CN CNB031542611A patent/CN1296945C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0869903A (en) * | 1994-08-30 | 1996-03-12 | Tokin Corp | Manufacture of ntc thermistor |
| CN1185631A (en) * | 1996-12-14 | 1998-06-24 | 中国科学院新疆物理研究所 | Oxidate semi-condcutor thermo-sensitive resistance and mfg. method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110372336A (en) * | 2019-08-19 | 2019-10-25 | 陈龙 | A kind of CoNiO2The co-precipitation method of thermistor powder |
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