CN107473715A - A kind of ternary system NTC thermistor material and its manufacture method - Google Patents
A kind of ternary system NTC thermistor material and its manufacture method Download PDFInfo
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention discloses a kind of ternary system NTC thermistor material and preparation method thereof, thermistor material is made of using manganese nitrate, nickel nitrate, aluminum nitrate as raw material, and the molar percentage of wherein each component is：Manganese：Nickel：Aluminium=50 80:25‑45:5‑40.The manufacture method of thermistor material comprises the following steps：Ar ion mixing liquid is configured to as raw material using manganese nitrate, nickel nitrate, aluminum nitrate；Prepare precipitant solution；The Ar ion mixing liquid is added in the precipitant solution and is allowed to react；Clean sediment repeatedly with deionized water 35 times, then filtered with ethanol dehydration, obtain powder；Powder is polished, through 450 DEG C of decomposition, then through pre-burning；After powder pre-burning, through ball milling into particle；It is sintered by idiosome isostatic pressing through being pre-formed as idiosome after ball milling, thermistor porcelain ingot is made；Thermistor porcelain ingot is cut into ceramics；Then thermistor is made in blackening electrode.
Description
Technical field
The present invention relates to a kind of thermistor, particularly a kind of ternary system NTC thermistor material and its manufacture method.
Background technology
(Negative Temperature Coefficient, negative temperature coefficient, it is very big to refer to negative temperature coefficient to NTC
Semi-conducting material or component) thermistor material is a kind of semiconductor electronic ceramics, be most to be widely applied to thermometric neck
A kind of sensitive material in domain.Its characteristic is to vary with temperature its impedance to change, and this corresponding relation determines material
Temperature coefficient, microcosmic crystal structure.Conversely, the temperature curve characteristic of thermistor be limited by itself crystal structure, composition,
The a series of microcosmic influence factors such as size, material composition.So the controllability of material structure, the uniformity of material composition are for temperature-sensitive
Repeatability, the stability of resistance chip production have vital effect.
Publication No. be CN1588576A, CN1588574A patent document in, it is necessary to strictly control coprecipitation reaction pH
The parameter such as value and concentration, it is complete to be allowed to precipitation.It is well known that on the premise of extraneous alkali ion is not introduced, pH value is one
Response parameter very rambunctious, control the completeness of reaction extremely difficult by control ph, cause the repeatability of technique
It is difficult to.
The Japanese leading manganese nickel aluminium series thermistor of Zhi Pu companies, because manganese nickel Spinel is highly stable structure, institute
It is fine with the stability of finished product, and manganese nickel system is insensitive to component requirements, is adapted to produce in enormous quantities；But depositing due to nickel
It also is difficult to ensure the repeatability of nickel precipitation in, traditional coprecipitation.PH value is adjusted with ammoniacal liquor, is prepared each time, each
Operator may have different results；Sodium ion can then be brought into by doing precipitating reagent with sodium hydroxide solution, influence the characteristic of product；
And with solid phase method, because manganese nickel synthesis temperature is higher, the incorporation of particularly aluminium make it that synthesis temperature is higher, and sintered density is generally inclined
It is low, influence properties of product.
Therefore it is quick with relatively low synthesis temperature, excellent repeatability solution manganese nickel aluminothermy it is an object of the invention to realize
The synthesis difficulty problem of resistance material system, makes it possible to industrialized production.
The content of the invention
In view of this, it is a primary object of the present invention to provide one kind to realize that technique is simple, reproducible, stability
It is high, can industrialized production manganese nickel aluminium ternary system NTC thermistor material and its manufacture method.
To reach above-mentioned purpose, the invention provides a kind of ternary system NTC thermistor material, the thermistor material
It is made of using manganese nitrate, nickel nitrate, aluminum nitrate as raw material, the molar percentage of wherein each component is：
Manganese:Nickel:Aluminium=(50-80):(25-45):(5-40).
A kind of manufacture method of ternary system NTC thermistor material, comprises the following steps：
A, manganese nitrate, nickel nitrate and aluminum nitrate are weighed in proportion as raw material, and by the preparation soluble in water of these three raw materials
Into Ar ion mixing liquid；
B, ammonium hydrogen carbonate, ammoniacal liquor, alcohol and water are subjected to mixed preparing precipitant solution；
C, precipitant solution is heated to 40-50 DEG C, and with vigorous stirring, by the Ar ion mixing liquid described in step a
It is added in the precipitant solution and is allowed to carry out precipitation reaction；
D, after precipitation reaction is complete, 4-24 hours are stood, taking precipitate cleans sediment with deionized water 3-5 times repeatedly,
Then filtered with ethanol dehydration, 80-100 DEG C of drying, obtain the presoma of powder, as thermistor material；
E, the powder of gained in step d is ground, then through 450 DEG C of decomposition 0.5-2 hours, then through 950-1150 DEG C
Pre-burning 2-4 hours；
F, after step e pre-burning, then through ball milling particle is made, particle diameter is 0.8-3 microns；
G, preformed again after ball milling is idiosome, by idiosome isostatic pressing, pressure 2-3MPa/cm2；
H, thermistor porcelain ingot is made through 1250-1300 DEG C of sintering 2-4 hour after isostatic pressed；
I, the thermistor porcelain ingot is cut into the thick ceramics of 0.3-0.6mm；
J, after the ceramics is cleaned, thermistor is made in its two sides blackening electrode.
Preferably, the concentration of the Ar ion mixing liquid is 1-1.5mol/L.
Preferably, the concentration of ammonium hydrogen carbonate is 1.5-3mol/L in the precipitant solution, and the concentration of ammoniacal liquor is 0.2-
1mol/L。
Preferably, in the Ar ion mixing liquid manganese nitrate, the summation of nickel nitrate and aluminum nitrate and ammonium hydrogen carbonate mol ratio
For 1：(2-3).
Preferably, the material of the electrode is one kind in silver paste, gold paste or palladium-silver slurry.
The invention has the advantages that：
1st, the present invention does not need the parameters such as extraneous strict control ph, concentration, it is only necessary to surfactant slightly, utilizes hydrogen
The both sexes feature of aluminum oxide, under the conditions of the stable reaction speed of control, you can obtain evengranular powder.
2nd, the present invention is under relatively low synthesis temperature, you can the high thermistor material of stability is made.
3rd, present invention process is simple, passes through the ratio of fixed cation and anion, control charging rate, control reaction temperature
Spend and then realize the repeatability of course of reaction, industrialized production can be realized.
Embodiment
The invention provides a kind of ternary system NTC thermistor material and its manufacture method method, below with specific experiment
Illustrate embodiment exemplified by case, it will be appreciated that the specific embodiments described herein are merely illustrative of the present invention,
It is not intended to limit the present invention.
Used manganese nitrate, nickel nitrate, aluminum nitrate, ammonium hydrogen carbonate, ammoniacal liquor, alcohol, anhydrous second in the embodiment of the present invention
Alcohol and silver paste are come as commercially available.
Embodiment 1：
A, deionized water is added to be configured to 1mol/L ion as raw material using 3 moles of manganese nitrate altogether, nickel nitrate, aluminum nitrate
Mixed liquor, wherein each component molar percentage are：Manganese：Nickel：Aluminium=60:30:10.
B, ammonium hydrogen carbonate, ammoniacal liquor, alcohol and water are subjected to mixed preparing precipitant solution, its formula is：Ammonium hydrogen carbonate 6 rubs
You, 1 mole of ammoniacal liquor, 100 milliliters of alcohol, the concentration of ammonium hydrogen carbonate is 2mol/L in precipitant solution.
C, reaction temperature is in 45 DEG C ± 1 DEG C of water bath, with vigorous stirring, the Ar ion mixing liquid in step a is equal
Even be added in precipitant solution is allowed to carry out precipitation reaction, and addition speed is 150ml/min.
D, after precipitation reaction is complete, 8 hours are stood, cleans precipitation repeatedly with deionized water 3-5 times, then uses ethanol dehydration
Filter, 80 DEG C of drying, obtain the presoma of powder, as thermistor material.
E, after the powder of gained in step d is ground, decomposed 1 hour through 450 DEG C, then through 1100 DEG C of pre-burnings 4 hours.
F, after powder pre-burning, through ball milling into particle, particle diameter is 1.9 microns.
G, preformed powder after ball milling is a diameter of 40mm, the highly idiosome for 20mm, then by idiosome isostatic pressed
Shaping, pressure 2.5MPa/cm2。
H, sintered 2 hours through 1280 DEG C after isostatic pressed, thermistor porcelain ingot is made.
I, thermistor porcelain ingot is cut into the thick ceramics of 0.36mm.
J, after the ceramics is cleaned, thermistor is made in its two sides blackening electrode, the material of electrode is silver paste.
Play dispensing 8 times by above-mentioned step, respectively record data 1A 1B 1C 1D 1E 1F 1G 1H.
Embodiment 2：
A, deionized water is added to be configured to 1mol/L ion as raw material using 3 moles of manganese nitrate altogether, nickel nitrate, aluminum nitrate
Mixed liquor, wherein each component molar percentage are：Manganese：Nickel：Aluminium=60:19:21.
B, ammonium hydrogen carbonate, ammoniacal liquor, alcohol and water are subjected to mixed preparing precipitant solution, its formula is：Ammonium hydrogen carbonate 8 rubs
You, 1 mole of ammoniacal liquor, 100 milliliters of alcohol, the concentration of ammonium hydrogen carbonate is 2mol/L in precipitant solution.
C, reaction temperature is in 48 DEG C ± 1 DEG C of water bath, with vigorous stirring, the Ar ion mixing liquid in step a is equal
Even be added in precipitant solution is allowed to carry out precipitation reaction, and addition speed is 150ml/min.
D, after precipitation reaction is complete, 8 hours are stood, cleans precipitation repeatedly with deionized water 3-5 times, then uses ethanol dehydration
Filter, 90 DEG C of drying, obtain the presoma of powder, as thermistor material.
E, after the powder of gained in step d is ground, decomposed 1 hour through 450 DEG C, then through 1150 DEG C of pre-burnings 4 hours.
F, after powder pre-burning, through ball milling into particle, particle diameter is 2.2 microns.
G, preformed powder after ball milling is a diameter of 40mm, the highly idiosome for 20mm, then by idiosome isostatic pressed
Shaping, pressure 2.5MPa/cm2。
H, sintered 2 hours through 1300 DEG C after isostatic pressed, thermistor porcelain ingot is made.
I, thermistor porcelain ingot is cut into the thick ceramics of 0.36mm.
J, after the ceramics is cleaned, thermistor is made in its two sides blackening electrode, the material of electrode is silver paste.
Play dispensing 8 times by above-mentioned step, respectively record data 2A 2B 2C 2D 2E 2F 2G 2H.
Embodiment 3：
A, deionized water is added to be configured to 1mol/L ion as raw material using 3 moles of manganese nitrate altogether, nickel nitrate, aluminum nitrate
Mixed liquor, wherein each component molar percentage are：Manganese：Nickel：Aluminium=56:18:26.
B, ammonium hydrogen carbonate, ammoniacal liquor, alcohol and water are subjected to mixed preparing precipitant solution, its formula is：Ammonium hydrogen carbonate 6 rubs
You, 1 mole of ammoniacal liquor, 100 milliliters of alcohol, the concentration of ammonium hydrogen carbonate is 1.5mol/L in precipitant solution.
C, reaction temperature is in 40 DEG C ± 1 DEG C of water bath, with vigorous stirring, the Ar ion mixing liquid in step a is equal
Even be added in precipitant solution is allowed to carry out precipitation reaction, and addition speed is 150ml/min.
D, after precipitation reaction is complete, 24 hours are stood, cleans precipitation repeatedly with deionized water 3-5 times, then with anhydrous second
Dehydration of alcohols filters, and 100 DEG C of drying, obtains the presoma of powder, as thermistor material.
E, after the powder of gained in step d is ground, decomposed 1 hour through 450 DEG C, then through 980 DEG C of pre-burnings 4 hours.
F, after powder pre-burning, through ball milling into particle, particle diameter is 1.0 microns.
G, preformed powder after ball milling is a diameter of 40mm, the highly idiosome for 20mm, then by idiosome isostatic pressed
Shaping, pressure 3MPa/cm2。
H, sintered 4 hours through 1250 DEG C after isostatic pressed, thermistor porcelain ingot is made.
I, thermistor porcelain ingot is cut into the thick ceramics of 0.36mm.
J, after the ceramics is cleaned, thermistor is made in its two sides blackening electrode, the material of electrode is silver paste.
By above-mentioned steps dispensing 8 times, respectively record data 3A 3B 3C 3D 3E 3F 3G 3H.
The data result of each experimental record is shown in table 1 in embodiment 1-3.Data are to seal ceramics with single-ended glass in table
The result tested after dress, its Midst density measure according to Archimedes method, and ageing rate refers to place in 200 DEG C of environment at 200 DEG C
The front and rear rate of change of resistance after 1000 hours.
Table 1
As it can be seen from table 1 in same embodiment, data Midst density, B numerical constants and the resistivity of 8 dispensing experiments
Differ small, illustrate that the present invention has excellent repeatability；Ageing rate is all non-at 200 DEG C of every group of data of embodiment 1-3
It is often low, illustrate that ternary system NTC thermistor stability of material produced by the present invention is very high.
Comparative example 1 and embodiment 2 are understood：Ar ion mixing liquid concentration is certain, improves the molar percentage of aluminium, reduces nickel
Molar percentage, B numerical constants and resistivity improve.
Finally it should be noted that：Above-described embodiments are merely to illustrate the technical scheme, rather than to it
Limitation；Although the present invention is described in detail with reference to the foregoing embodiments, it will be understood by those within the art that：
It can still modify to the technical scheme described in previous embodiment, or which part or all technical characteristic are entered
Row equivalent substitution；And these modifications or substitutions, the essence of appropriate technical solution is departed from various embodiments of the present invention technical side
The scope of case.
Claims (6)
- A kind of 1. ternary system NTC thermistor material, it is characterised in that the thermistor material be with manganese nitrate, nickel nitrate, Aluminum nitrate is made up of raw material, and the molar percentage of wherein each component is：Manganese:Nickel:Aluminium=(50-80):(25-45):(5-40).
- 2. the manufacture method of ternary system NTC thermistor material as claimed in claim 1, it is characterised in that including following step Suddenly：A, manganese nitrate, nickel nitrate and aluminum nitrate are weighed in proportion as raw material, and by these three raw materials it is soluble in water be configured to from Sub- mixed liquor；B, ammonium hydrogen carbonate, ammoniacal liquor, alcohol and water are subjected to mixed preparing precipitant solution；C, precipitant solution is heated to 40-50 DEG C, and with vigorous stirring, the Ar ion mixing liquid described in step a added It is allowed to carry out precipitation reaction into the precipitant solution；D, after precipitation reaction is complete, 4-24 hours are stood, taking precipitate cleans sediment with deionized water 3-5 times repeatedly, then Filtered with ethanol dehydration, 80-100 DEG C of drying, obtain the presoma of powder, as thermistor material；E, the powder of gained in step d is ground, then through 450 DEG C of decomposition 0.5-2 hours, then through 950-1150 DEG C of pre-burning 2-4 hours；F, after step e pre-burning, then through ball milling particle is made, particle diameter is 0.8-3 microns；G, preformed again after ball milling is idiosome, by idiosome isostatic pressing, pressure 2-3MPa/cm2；H, thermistor porcelain ingot is made through 1250-1300 DEG C of sintering 2-4 hour after isostatic pressed；I, the thermistor porcelain ingot is cut into the thick ceramics of 0.3-0.6mm；J, after the ceramics is cleaned, thermistor is made in its two sides blackening electrode.
- 3. the manufacture method of ternary system NTC thermistor material as claimed in claim 2, it is characterised in that the ion mixes The concentration for closing liquid is 1-1.5mol/L.
- 4. the manufacture method of ternary system NTC thermistor material as claimed in claim 2, it is characterised in that the precipitating reagent The concentration of ammonium hydrogen carbonate is 1.5-3mol/L in solution, and the concentration of ammoniacal liquor is 0.2-1mol/L.
- 5. the manufacture method of ternary system NTC thermistor material as claimed in claim 2, it is characterised in that the ion mixes The mol ratio for closing manganese nitrate, the summation of nickel nitrate and aluminum nitrate and ammonium hydrogen carbonate in liquid is 1:(2-3).
- 6. the manufacture method of ternary system NTC thermistor material as claimed in claim 2, it is characterised in that the electrode Material is one kind in silver paste, gold paste or palladium-silver slurry.
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| CN105753473A (en) * | 2016-02-25 | 2016-07-13 | 江苏师范大学 | Preparation method of magneto-optic terbium oxide transparent ceramic |
| CN106390981A (en) * | 2016-09-19 | 2017-02-15 | 常州大学 | Rare earth doped barium titanate nano-powder photocatalyst and preparation method thereof |
| CN106698528A (en) * | 2017-01-25 | 2017-05-24 | 中国科学院新疆理化技术研究所 | Composite oxide material with core-shell structure, and preparation method and application thereof |
| CN106977206A (en) * | 2017-02-22 | 2017-07-25 | 江苏师范大学 | Spraying codepostion prepares the continuation method of high dispersancy nano oxide powder |
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