CN106876069A - The uniform co-precipitation preparation method of manganese cobalt nickel based negative temperature coefficient thermistor material - Google Patents
The uniform co-precipitation preparation method of manganese cobalt nickel based negative temperature coefficient thermistor material Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/008—Thermistors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/04—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having negative temperature coefficient
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Abstract
The present invention relates to the uniform co-precipitation preparation method of manganese cobalt nickel based negative temperature coefficient thermistor material.The method is first using manganese sulfate, nickel sulfate, two or three of cobaltous sulfate as metal ion source, oxalic acid diethyl fat is used as reaction precipitation agent, ammoniacal liquor or NaOH are used as complexant, chemical precipitation reaction is carried out, precipitated product is then obtained into manganese, nickel, cobalt-based binary or ternary thermistor powder body material after filtering and washing, drying and grinding, calcining and grinding.The characteristics of the method has easy to operate, low cost, cycle is short, yield high, gained thermistor powder is spinel structure, and particle diameter is small, shapeliness, good dispersion, quality better.
Description
Technical field
The present invention relates to a kind of uniform co-precipitation preparation method of manganese cobalt nickel based negative temperature coefficient thermistor material.
Background technology
Negative temperature coefficient (Negative Temperature coefficient, NTC) thermal resistor is a kind of application
Extensive measurement and control of temperature element, the quality of its performance will directly affect whole temperature monitoring system, to the overall performance equipped and
Normal operation has very important significance.Manganese cobalt nickel base spinel structure NTC thermistor material has B values height, resistivity
The good advantage of low and heat endurance, therefore, it is widely used in the fields such as household electrical appliances, automobile, Internet of Things, Aero-Space, ocean
Temperature survey.With the development of modern science and technology, each field proposes requirement higher to the uniformity and stability of element,
This is accomplished by each key technique that continuous lifting prepares thermistor element.
Thermo-sensitive material synthesis is first important step for preparing thermistor element.Preparation particle uniformity is good, particle diameter
Size is small, the NTC thermistor powder body material of stoichiometric proportion stabilization is to obtain to have good stability and a straightforward temperature-sensitive electricity
The premise of resistance element.Therefore, the good NTC thermistor powder of synthesis uniformity, extremely intentional for preparing NTC themistor
Justice.
At present, the preparation method of common thermistor powder body material has ball-milling method, coprecipitation, sol-gal process etc..
Ball-milling method prepares powder has a process is simple, low cost and other advantages, but due to the limitation of ball-milling method equipment, therefore use the method
It is difficult to obtain the good material of uniformity.Coprecipitation and sol-gal process complete reaction under uniform chemical solvent environment,
And then uniform heat-sensitive powder can be obtained, but have the shortcomings that complex process, experiment variable element are more.
The content of the invention
Present invention aim at, there is provided a kind of uniform co-precipitation of manganese cobalt nickel based negative temperature coefficient thermistor powder body material
Preparation method, the method is first using manganese sulfate, nickel sulfate, two or three of cobaltous sulfate as metal ion source, oxalic acid diethyl
Used as reaction precipitation agent, ammoniacal liquor or NaOH carry out chemical precipitation reaction, then by precipitated product through taking out to fat as complexant
Manganese, nickel, cobalt-based binary or ternary thermistor powder body material are obtained after filter washing, drying and grinding, calcining and grinding.The method has
The characteristics of easy to operate, low cost, cycle is short, yield high, gained thermistor powder is spinel structure, and particle diameter is small, shape
Good, good dispersion, quality better.
A kind of uniform co-precipitation preparation method of manganese cobalt nickel based negative temperature coefficient thermistor material of the present invention, presses
The following steps are carried out：
A, it is to press ion mol ratio manganese two or three in manganese sulfate, nickel sulfate, cobaltous sulfate by sulfate:Nickel:Cobalt=
1-4:0-1:0-5 is weighed and is dissolved in deionized water, and 30-60min is stirred at 40 DEG C of temperature, forms concentration for 0.5-5mol/L
Homogeneous mixture solotion；
B, precise analyze pure diethy-aceto oxalate, and the diethy-aceto oxalate for being configured to 1mol/L with deionized water is molten
Liquid, and 30-60min is stirred at 40 DEG C of temperature, hydrolyze diethy-aceto oxalate；
C, ammoniacal liquor or NaOH are configured to the ammoniacal liquor or sodium hydroxide solution that concentration is 1mol/L with deionized water, and
30-60min is stirred at 40 DEG C of temperature；
D, the diethy-aceto oxalate solution for configuring step b are added in the mixed solution of step a configurations, are gradually heated up, and are controlled
Reaction temperature stirs 30-60min at 70-90 DEG C so that solution is well mixed；
E, keep step D-shaped into mixed solution stir speed (S.S.) it is constant, by step c configure ammoniacal liquor or NaOH it is molten
Liquid separatory funnel be added dropwise over step D-shaped into mixed solution in, titration terminate after, the pH value of solution is between 6-10；
F, step e resulting solutions are continued to stop stirring after stirring 4-8h, are then aged 12-24h, formed supernatant liquor and
Lower sediment；
G, filtering and washing is carried out 4-10 times to lower sediment in step f with deionized water, then use absolute ethanol washing 1-2
It is secondary, it is precipitated thing；
H, sediment in step g is placed in 100-120 DEG C of temperature is dried, 30-60min is ground after drying, sunk
Starch flour, by precipitation powder, 450-600 DEG C of temperature thermally decomposes 1-10h in Muffle furnace；
I, by step h thermally decompose after powder continue grind 1-4h, then at temperature, 700-1000 DEG C carries out pre-burning, pre-burning
Grind 1h again afterwards, you can obtain manganese, nickel, cobalt-based binary or ternary thermistor powder body material.
The addition of step b medium-height grass diethyl phthalates is 1-2 with the mol ratio of sulfate mixture in step a:1.
The uniform co-precipitation preparation method of manganese cobalt nickel based negative temperature coefficient thermistor powder body material of the present invention, should
The advantage of method is：
1) the strict controllable manganese cobalt nickel base thermistor powder body material of stoichiometric proportion can be obtained；
2) homogeneous co-precipitation prepares manganese cobalt nickel based oxide powder has process is simple, and low cost, grain diameter is small, equal
The advantages of even property is good；
3) homogeneous co-precipitation prepares manganese cobalt nickel based oxide powder, with more than 96% yield.
Brief description of the drawings
Fig. 1 is the XRD spectrums that the present invention prepares manganese cobalt nickel oxide powder；
Fig. 2 is the SEM spectrums that the present invention prepares nickel manganese oxide powder；
Fig. 3 is the size distribution spectrum that the present invention prepares manganese cobalt/cobalt oxide powder.
Specific embodiment
Embodiment 1
A, in molar ratio Mn:Ni:Co=4:1:5 are dissolved in deionized water manganese sulfate, nickel sulfate and cobaltous sulfate, in temperature
30-60min is stirred at 40 DEG C, the homogeneous mixture solotion that concentration is 0.5mol/L is formed；
B, precise analyze pure diethy-aceto oxalate 20ml, addition and manganese sulfate, the sulfuric acid in step a of diethy-aceto oxalate
The mol ratio of nickel and cobaltous sulfate mixture is 2:1, it is configured to the diethy-aceto oxalate solution of 1mol/L with deionized water, and
30min is stirred at 40 DEG C of temperature, diethy-aceto oxalate is hydrolyzed；
C, ammoniacal liquor is configured to the ammoniacal liquor or sodium hydroxide solution that concentration is 1mol/L with deionized water, and in 40 DEG C of temperature
Lower stirring 30-60min；
D, the diethy-aceto oxalate solution for configuring step b are added in the mixed solution of step a configurations, are gradually heated up, and are controlled
Reaction temperature stirs 30min at 70 DEG C so that solution is well mixed；
E, keep step D-shaped into mixed solution stir speed (S.S.) it is constant, the ammonia spirit that step c is configured point liquid leaks
Bucket be added dropwise over step D-shaped into mixed solution in, titration terminate after, the pH value of solution is 6；
F, will step e resulting solutions continue stir 4h after stop stirring, be aged 12h, formed supernatant liquor and lower sediment；
G, filtering and washing is carried out 4 times to lower sediment in step f with deionized water, then with absolute ethanol washing 1 time, obtained
Sediment；
H, sediment in step g be placed in 100 DEG C of temperature dried, 30min is ground after drying, be precipitated powder,
Will precipitation powder 450 DEG C of thermal decomposition 1h of temperature in Muffle furnace；
I, by step h thermally decompose after powder continue grind 1h, then at temperature, 700 DEG C carry out pre-burning, are ground again after pre-burning
Mill 1h, you can obtain manganese, nickel, cobalt-based ternary thermistor powder body material.
Embodiment 2
A, in molar ratio Mn:Ni=1:0.5 is dissolved in deionized water manganese sulfate and nickel sulfate, is stirred at 40 DEG C of temperature
60min, forms the homogeneous mixture solotion that concentration is 5mol/L；
B, precise analyze pure diethy-aceto oxalate 10ml, and the addition of diethy-aceto oxalate mixes with manganese sulfate and nickel sulfate
The mol ratio of thing is 1:1, it is configured to the diethy-aceto oxalate solution of 1mol/L with deionized water, and stirred at 40 DEG C of temperature
60min, hydrolyzes diethy-aceto oxalate；
C, NaOH is configured to the sodium hydroxide solution that concentration is 1mol/L with deionized water, and at 40 DEG C of temperature
Stirring 60min；
D, the diethy-aceto oxalate solution for configuring step b are added in the mixed solution of step a configurations, are gradually heated up, and are controlled
Reaction temperature stirs 60min at 90 DEG C so that solution is well mixed；
E, keep step D-shaped into mixed solution stir speed (S.S.) it is constant, by step c configure ammoniacal liquor or NaOH it is molten
Liquid separatory funnel be added dropwise over step D-shaped into mixed solution in, titration terminate after, the pH value of solution is 10；
F, step e resulting solutions are continued to stop stirring after stirring 8h, be then aged 24h, form supernatant liquor and lower floor
Precipitation；
G, filtering and washing is carried out 10 times to lower sediment in step f with deionized water, then with absolute ethanol washing 2 times, obtained
To sediment；
H, sediment in step g be placed in 120 DEG C of temperature dried, 60min is ground after drying, be precipitated powder,
Will precipitation powder 600 DEG C of thermal decomposition 10h of temperature in Muffle furnace；
I, by step h thermally decompose after powder continue grind 4h, then at temperature, 1000 DEG C carry out pre-burning, are ground again after pre-burning
Mill 1h, you can obtain manganese, Ni-based binary thermistor powder body material.
Embodiment 3
A, in molar ratio Mn:Co=3:1 is dissolved in deionized water manganese sulfate and cobaltous sulfate, is stirred at 40 DEG C of temperature
45min, forms the homogeneous mixture solotion that concentration is 3mol/L；
B, precise analyze pure diethy-aceto oxalate 15ml, and the addition of diethy-aceto oxalate mixes with manganese sulfate and cobaltous sulfate
The mol ratio of thing is 1.5:1, it is configured to the diethy-aceto oxalate solution of 1mol/L with deionized water, and stirred at 40 DEG C of temperature
40min is mixed, diethy-aceto oxalate is hydrolyzed；
C, NaOH is configured to the ammoniacal liquor or sodium hydroxide solution that concentration is 1mol/L with deionized water, and in temperature
50min is stirred at 40 DEG C；
D, the diethy-aceto oxalate solution for configuring step b are added in the mixed solution of step a configurations, are gradually heated up, and are controlled
Reaction temperature stirs 40min at 80 DEG C so that solution is well mixed；
E, keep step D-shaped into mixed solution stir speed (S.S.) it is constant, by step c configure sodium hydroxide solution with point
Liquid funnel be added dropwise over step D-shaped into mixed solution in, titration terminate after, the pH value of solution is 8；
F, step e resulting solutions are continued to stop stirring after stirring 7h, be then aged 20h, form supernatant liquor and lower floor
Precipitation；
G, filtering and washing is carried out 8 times to lower sediment in step f with deionized water, then with absolute ethanol washing 2 times, obtained
Sediment；
H, sediment in step g be placed in 110 DEG C of temperature dried, 50min is ground after drying, be precipitated powder,
Will precipitation powder 500 DEG C of thermal decomposition 8h of temperature in Muffle furnace；
I, by step h thermally decompose after powder continue grind 3h, then at temperature, 800 DEG C carry out pre-burning, are ground again after pre-burning
Mill 1h, you can obtain manganese, cobalt-based binary thermistor powder body material.
Embodiment 4
A, in molar ratio Mn:Ni:Co=2:0.75:2 are dissolved in deionized water manganese sulfate, nickel sulfate and cobaltous sulfate,
45min is stirred at 40 DEG C of temperature, the homogeneous mixture solotion that concentration is 3mol/L is formed；
B, precise analyze pure diethy-aceto oxalate 16ml, addition and manganese sulfate, nickel sulfate, the sulfuric acid of diethy-aceto oxalate
The mol ratio of cobalt mixture is 1.6:1, the diethy-aceto oxalate solution of 1mol/L is configured to deionized water, and in temperature 40
40min is stirred at DEG C, diethy-aceto oxalate is hydrolyzed；
C, NaOH is configured to the ammoniacal liquor or sodium hydroxide solution that concentration is 1mol/L with deionized water, and in temperature
50min is stirred at 40 DEG C；
D, the diethy-aceto oxalate solution for configuring step b are added in the mixed solution of step a configurations, are gradually heated up, and are controlled
Reaction temperature stirs 40min at 80 DEG C so that solution is well mixed；
E, keep step D-shaped into mixed solution stir speed (S.S.) it is constant, by step c configure sodium hydroxide solution with point
Liquid funnel be added dropwise over step D-shaped into mixed solution in, titration terminate after, the pH value of solution is 8；
F, step e resulting solutions are continued to stop stirring after stirring 7h, be then aged 20h, form supernatant liquor and lower floor
Precipitation；
G, filtering and washing is carried out 8 times to lower sediment in step f with deionized water, then with absolute ethanol washing 2 times, obtained
Sediment；
H, sediment in step g be placed in 110 DEG C of temperature dried, 50min is ground after drying, be precipitated powder,
Will precipitation powder 500 DEG C of thermal decomposition 8h of temperature in Muffle furnace；
I, by step h thermally decompose after powder continue grind 3h, then at temperature, 800 DEG C carry out pre-burning, are ground again after pre-burning
Mill 1h, you can obtain manganese, cobalt-based binary thermistor powder body material.
Embodiment 5
A, in molar ratio Mn:Co:Ni=1:1:1 is dissolved in deionized water manganese sulfate, cobaltous sulfate and nickel sulfate, in temperature
30-60min is stirred at 40 DEG C, the homogeneous mixture solotion that concentration is 0.5mol/L is formed；
B, precise analyze pure diethy-aceto oxalate 20ml, addition and manganese sulfate, cobaltous sulfate and the sulphur of diethy-aceto oxalate
The mol ratio of sour nickel mixture is 2:1, the diethy-aceto oxalate solution of 1mol/L is configured to deionized water, and in temperature 40
30min is stirred at DEG C, diethy-aceto oxalate is hydrolyzed；
C, ammoniacal liquor is configured to the ammoniacal liquor or sodium hydroxide solution that concentration is 1mol/L with deionized water, and in 40 DEG C of temperature
Lower stirring 30-60min；
D, the diethy-aceto oxalate solution for configuring step b are added in the mixed solution of step a configurations, are gradually heated up, and are controlled
Reaction temperature stirs 30min at 70 DEG C so that solution is well mixed；
E, keep step D-shaped into mixed solution stir speed (S.S.) it is constant, the ammonia spirit that step c is configured point liquid leaks
Bucket be added dropwise over step D-shaped into mixed solution in, titration terminate after, the pH value of solution is 6；
F, will step e resulting solutions continue stir 4h after stop stirring, be aged 12h, formed supernatant liquor and lower sediment；
G, filtering and washing is carried out 4 times to lower sediment in step f with deionized water, then with absolute ethanol washing 1 time, obtained
Sediment；
H, sediment in step g be placed in 100 DEG C of temperature dried, 30min is ground after drying, be precipitated powder,
Will precipitation powder 450 DEG C of thermal decomposition 1h of temperature in Muffle furnace；
I, by step h thermally decompose after powder continue grind 1h, then at temperature, 700 DEG C carry out pre-burning, are ground again after pre-burning
Mill 1h, you can obtain manganese, nickel, cobalt-based ternary thermistor powder body material.
Embodiment 6
Any one powder body material that embodiment 1-5 is obtained carries out XRD, SEM, Laser particle-size distribution test, as a result as schemed
It is shown, it can be seen that the manganese cobalt nickel ternary prepared using homogeneous co-precipitation or manganese nickel binary or manganese cobalt binary are aoxidized
Powder is respectively provided with good crystallinity and dispersiveness.
Claims (2)
1. a kind of uniform co-precipitation preparation method of manganese cobalt nickel based negative temperature coefficient thermistor material, it is characterised in that by following
Step is carried out：
A, it is to press ion mol ratio manganese two or three in manganese sulfate, nickel sulfate, cobaltous sulfate by sulfate:Nickel:Cobalt=1-4:0-
1:0-5 is dissolved in deionized water, and 30-60min is stirred at 40 DEG C of temperature, forms the uniformly mixing that concentration is 0.5-5mol/L molten
Liquid；
B, precise analyze pure diethy-aceto oxalate, and the diethy-aceto oxalate solution of 1mol/L is configured to deionized water, and
30-60min is stirred at 40 DEG C of temperature, diethy-aceto oxalate is hydrolyzed；
C, ammoniacal liquor or NaOH are configured to the ammoniacal liquor or sodium hydroxide solution that concentration is 1mol/L with deionized water, and in temperature
30-60min is stirred at 40 DEG C of degree；
D, the diethy-aceto oxalate solution for configuring step b are added in the mixed solution of step a configurations, are gradually heated up, control reaction
Temperature stirs 30-60min at 70-90 DEG C so that solution is well mixed；
E, keep step D-shaped into mixed solution stir speed (S.S.) it is constant, by step c configure ammoniacal liquor or sodium hydroxide solution use
Separatory funnel be added dropwise over step D-shaped into mixed solution in, titration terminate after, the pH value of solution is between 6-10；
F, step e resulting solutions are continued to stop stirring after stirring 4-8h, be aged 12-24h, form supernatant liquor and lower floor heavy
Form sediment；
G, filtering and washing is carried out 4-10 times to lower sediment in step f with deionized water, then with absolute ethanol washing 1-2 times, obtained
To sediment；
H, sediment in step g is placed in 100-120 DEG C of temperature is dried, 30-60min is ground after drying, be precipitated powder
End, by precipitation powder, 450-600 DEG C of temperature thermally decomposes 1-10h in Muffle furnace；
I, by step h thermally decompose after powder continue grind 1-4h, then at temperature, 700-1000 DEG C carries out pre-burning, after pre-burning again
Grinding 1h, you can obtain manganese, nickel, cobalt-based binary or ternary thermistor powder body material.
2. method according to claim 1, it is characterised in that in the addition of step b medium-height grass diethyl phthalates and step a
The mol ratio of sulfate mixture is 1-2:1.
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| CN110230029A (en) * | 2019-06-27 | 2019-09-13 | 西安邮电大学 | A kind of preparation method of spinel structure nickel manganese oxide film |
| CN110372336A (en) * | 2019-08-19 | 2019-10-25 | 陈龙 | A kind of CoNiO2The co-precipitation method of thermistor powder |
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Application publication date: 20170620 |
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