CN105622066A - Method for preparing thermistor powdered material by microemulsion-hydrothermal synthesis - Google Patents
Method for preparing thermistor powdered material by microemulsion-hydrothermal synthesis Download PDFInfo
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- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3279—Nickel oxides, nickalates, or oxide-forming salts thereof
Abstract
The invention relates to a method for preparing a thermistor powdered material by micro-emulsion-hydrothermal synthesis. The method comprises the following steps: preparing hydroxide of thermistor from nitrate of Mn, Mg, Ni and Co metal elements by a reverse microemulsion method; mixing the hydroxide with deionized water, and performing ultrasonic stirring to form thermistor suspension; sealing the suspension in a high-pressure hydrothermal kettle, performing hydrothermal synthesis in a constant-temperature tank, cooling to room temperature after the reaction is completed, and washing the powder obtained in the reaction with deionized water; and finally, drying and grinding to obtain the thermistor nano-powder. The method has good process repeatability; the material has an accurate ingredient proportion, good powder uniformity, high purity, complete grain growth and uniform distribution. The preparation method of the thermistor powder which is excellent in effect and convenient to popularize and apply can be used for solving the problems of non-uniform granularity and appearance distribution, poor reaction activity and the like of traditional thermistor powder.
Description
Technical field
The preparation method that the present invention relates to a kind of electronic devices and components, the specifically preparation method of microemulsion-water heat transfer critesistor powder body material.
Background technology:
Inkjet technology is a kind of contactless digital printing technologies succeeded in developing late 1970s. Refer to and ceramic ink be ejected on various dielectric surface by the nozzle of printhead, such as pottery glazed brick, acrylic, timber, paper etc., it is achieved thereby that a kind of noncontact, at high speed, the new material preparation method of low noise. And utilize inkjet technology to prepare ceramic material, it is critical only that the preparation of ceramic ink, and the good ceramic ink of stable dispersion is closely bound up with the synthesis of wherein critesistor ceramic powder.
At present, mostly the preparation of high-volume NTC thermistor powder body is by grinding for a long time and high-temperature calcination, its raw material mostly is metal-oxide, the calcining heat of presoma is higher, general calcining heat is all more than 1000 degree, and the powder granularity prepared is uneven and powder active is low, so using the method to prepare high-precision NTC thermistor powder body have certain limitation. In order to produce the NTC thermistor element of precision height, good reliability, the synthetic method that one of its key seeks to from material is improved, and obtains component higher, powder granule that particle diameter is tiny homogeneous, active.
Therefore technique is sought simple, easily operated and the new method of thermistor material quality can be effectively improved and become particularly significant. Microemulsion method is a kind of effective ways preparing nanoparticle that development in recent years is got up, and the method has the features such as simple, controlled, scattered, the narrowly distributing of processing ease, size of experimental facilities. It utilizes surfactant to make solvent two kinds immiscible form a kind of uniform, stable microemulsion, and wherein the size of micelle is limited mainly by ��0Value (��0=[aqueous solution]/[surfactant], mol ratio) impact, therefore can pass through to regulate the amount of water and the surfactant added, control the size of micelle in microemulsion. Utilize the micelle in microemulsion as " microreactor ", the processes such as nucleation, growth, coalescence, reunion can be made to be confined in a small spherical droplets to carry out, thus spheroidal particle can be formed, turn avoid and reunite further between granule, thus reaching to control the purpose of particle size, shape, therefore adopt reverse microemulsion method can prepare nanometer scale ceramics powder granule. And hydro-thermal method refers to and adopts aqueous solution as reaction system in high pressure water heating kettle, by system is heated, pressurization or spontaneous vapour pressure create the reaction environment of relatively-high temperature, high pressure so that generally indissoluble or insoluble material dissolve and recrystallization and the method that carries out Inorganic synthese.
And the ceramic powder in traditional hydro-thermal method, there is the problems such as particle size distribution is uneven, dispersibility is poor, therefore many researchers are devoted to optimize hydro-thermal method and prepare in nano material. Reverse microemulsion method and hydro-thermal method are combined by this patent first, ceramic powder particle size distribution in hydro-thermal method is irregular, the not first-class problem of pattern to utilize microemulsion method to solve, simultaneously synthesizing go out ceramic powder require no high-temperature calcination, it is directly placed in high pressure water heating kettle to carry out hydro-thermal reaction, so equally possible obtains that crystallinity is good, there is very strongly hydrophilic, nano level superfine critesistor powder body material.
Therefore, microemulsion-hydro-thermal method is the chemical method preparing superfine nano ceramic powder of a kind of novelty, demonstrate many advantages of beyond tradition hydro-thermal method, accurate composition control short including synthesis cycle and the excellent homogeneity etc. on the molecular level due to liquid phase method slaine powder body mixed zone. It addition, the critesistor powder body material gone out by microemulsion-water heat transfer is easy to and hydrophilic solvent combines, in its solvent, dispersion effect is good, it is simple to the ceramic ink of preparation high solids content and stable dispersion.
Summary of the invention
Present invention aim at, it is provided that the preparation method of a kind of microemulsion-water heat transfer critesistor powder body material, the method is made up of the nitrate of Mn, Co, Ni and Mg metallic element, is the hydroxide preparing critesistor with reverse microemulsion method; Being mixed with deionized water by hydroxide, ultrasonic agitation forms critesistor suspension; After suspension is sealed in high pressure water heating kettle, putting into and carry out Hydrothermal Synthesis in calorstat, question response completes to be cooled to room temperature, and by the powder body deionized water wash of reaction gained, critesistor nano-powder is ground and obtained to final drying. The method of the invention preparation technology is reproducible, material composition proportion speed, powder body good evenness, and purity is high, and grain development is complete and is evenly distributed. For solving the problems such as conventional thermistor powder granularity topographic profile is uneven, reactivity is poor, it is provided that a kind of excellent effect, critesistor powder preparation method easy to utilize.
The preparation method of a kind of microemulsion of the present invention-water heat transfer critesistor powder body material, follows these steps to carry out: prepare the hydroxide of critesistor:
A, being Mn-Co-Ni-O, Mn-Mg-Ni-O or Mn-Co-Ni-Mg-O nitrate mixing of weighing cobalt, manganese, nickel and magnesium respectively by the system of critesistor powder body, be dissolved in deionized water by mixture uniform stirring, being configured to concentration is 0.5-4mol/L, ��0Value is the nitrate mixed solution of 0.5-4, simultaneously by volume for triton x-100: hexanol: hexamethylene=0.5-2.5: 2.5-4: 7-10 measures triton x-100, hexanol and hexamethylene mix and blend respectively and be configured to organic phase solution; Again nitrate mixed solution is added drop-wise in organic phase solution gradually, magnetic agitation 1-2h, forms microemulsion; Weigh ammonia again and be added dropwise in microemulsion, magnetic agitation 1-12h under room temperature, add 100-300ml dehydrated alcohol, magnetic agitation breakdown of emulsion, still aging 12-48h again, sucking filtration or centrifugation washing, to neutral, dried 6-12h at temperature 50-100 DEG C, are obtained the hydroxide of black precipitate critesistor;
Water heat transfer critesistor powder body:
B, the critesistor that step a is obtained the quality of hydroxide be that 1.5-5g mixes with deionized water 60-80mL, ultrasonic agitation 5-30min, form critesistor suspension, again suspension is put in high pressure water heating kettle, it is 160-250 DEG C in temperature, time is carry out Hydrothermal Synthesis under 6-18h, and by powder body deionized water wash 2-3 time of reaction gained, critesistor nano-powder is ground and obtained to final drying.
In step a, in the system of critesistor powder body, the mol ratio of Mn-Co-Ni-O is Mn: Co: Ni=0.8-1.5: 1-2.1: 0.1-0.5; In system, the mol ratio of Mn-Mg-Ni-O is Mn: Mg: Ni=1.2-2.05: 0.15-0.3: 0.8-1.5; In system, the mol ratio of Mn-Co-Ni-Mg-O is Mn: Co: Ni: Mg=0.8-1.5: 0.9-1.95: 0.15-0.3:0.1-0.3.
The addition of the ammonia in step a be Mn, 1-5 times of Co, Ni and Mg nitrate integral molar quantity.
High pressure water heating kettle liner in step b is volume is 100mL politef material, and reactor is stainless steel;
The critesistor diameter of particle obtained in step b is distributed in 45-95nm.
The wherein �� of the nitrate mixed solution in step a0Value (��0=[aqueous metal salt]/[surfactant], mol ratio) for 0.5-4.
The preparation method of a kind of microemulsion of the present invention-water heat transfer critesistor powder body material, the method feature is:
Formula and the content of critesistor powder body are varied, can be adjusted with market and experiment demand, can make the critesistor superfine powder of different system.
The critesistor powder body that microemulsion-water heat transfer goes out has that even particle size distribution, reactivity be high, the advantage of good hydrophilic property, and the simple and convenient practicality of the method, it is simple to the marketization is promoted.
The critesistor ceramic powder that microemulsion-hydro-thermal method is prepared, owing to it has extremely strong hydrophilic, easily facilitates the preparation of high solids content ceramic ink.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 gained critesistor powder body SEM image;
Fig. 2 is the embodiment of the present invention 2 gained critesistor powder body XRD figure picture.
Detailed description of the invention
Embodiment 1
Prepare the hydroxide of critesistor:
A, being respectively weigh manganese nitrate, cobalt nitrate and nickel nitrate mixing at 0.8: 2.1: 0.1 by Mn-Co-Ni-O mol ratio in the system of critesistor powder body, and be dissolved in deionized water, uniform stirring, being configured to concentration is 0.5mol/L, ��0Value is the nitrate mixed solution of 0.5; It is simultaneously respectively measure triton x-100, hexanol and hexamethylene mix and blend be configured to organic phase solution at 2: 3: 10 by volume; Again nitrate mixed solution is added drop-wise in organic phase solution gradually, magnetic agitation 1h, forms microemulsion; Weigh the ammonia of manganese nitrate, cobalt nitrate and nickel nitrate integral molar quantity 5 times again, it is added dropwise in microemulsion, magnetic agitation 1h under room temperature, add 100ml dehydrated alcohol magnetic agitation breakdown of emulsion, still aging 12h again, sucking filtration or centrifugation washing, to neutral, dried 12h under temperature 50 C, are obtained the hydroxide of black precipitate critesistor;
Water heat transfer critesistor powder body:
B, the critesistor hydroxide 4g obtained and deionized water 76ml are mixed, ultrasonic agitation 30min, forming critesistor suspension, it be volume is 100mL politef material that suspension is put into liner, in the high pressure water heating kettle of stainless steel, it it is 250 DEG C in reaction temperature, Hydrothermal Synthesis is carried out, by powder body deionized water wash 2-3 time of reaction gained, final drying under response time 18h, grind, obtain the particle diameter critesistor nano-powder material at 45nm.
Embodiment 2
Prepare the hydroxide of critesistor:
A, being respectively weigh manganese nitrate, cobalt nitrate and nickel nitrate mixing at 1.5: 1: 0.5 by Mn-Co-Ni-O mol ratio in the system of critesistor powder body, and be dissolved in deionized water, uniform stirring, being configured to concentration is 4mol/L, ��0Value is the nitrate mixed solution of 1; It is simultaneously respectively measure triton x-100, hexanol and hexamethylene mix and blend be configured to organic phase solution at 0.5: 2.5: 7 by volume; Again nitrate mixed solution is added drop-wise in organic phase solution gradually, magnetic agitation 2h, forms microemulsion; Weigh the ammonia of manganese nitrate, cobalt nitrate and nickel nitrate integral molar quantity 3 times again, it is added dropwise in microemulsion, magnetic agitation 12h under room temperature, add 300ml dehydrated alcohol magnetic agitation breakdown of emulsion, still aging 48h again, sucking filtration or centrifugation washing, to neutral, dried 6h at temperature 100 DEG C, are obtained the hydroxide of black precipitate critesistor;
Water heat transfer critesistor powder body:
B, by hydroxide 3g and the deionized water 60ml mixing of the critesistor that obtains, ultrasonic agitation 5min, forming critesistor suspension, it be volume is 100mL politef material that suspension is put into liner, in the high pressure water heating kettle of stainless steel, it it is 160 DEG C in reaction temperature, response time is carry out Hydrothermal Synthesis under 16h, by powder body deionized water wash 2-3 time of reaction gained, final drying, grind, obtain the particle diameter critesistor nano-powder material at 65nm.
Embodiment 3
Prepare the hydroxide of critesistor:
A, being respectively weigh manganese nitrate, magnesium nitrate and nickel nitrate mixing at 1.2: 0.3: 1.5 by Mn-Mg-Ni-O mol ratio in the system of critesistor powder body, and be dissolved in deionized water uniform stirring, being configured to concentration is 1.5mol/L, ��0Value is the nitrate mixed solution of 4; It is simultaneously respectively measure triton x-100, hexanol and hexamethylene mix and blend be configured to organic phase solution at 2.5: 4: 10 by volume; Again nitrate mixed solution is added drop-wise in organic phase solution gradually, magnetic agitation 1h, forms microemulsion; Weigh manganese nitrate, magnesium nitrate and ammonia that nickel nitrate integral molar quantity amount is 4 times again, it is added dropwise in microemulsion, magnetic agitation 2h under room temperature, add 200ml dehydrated alcohol magnetic agitation breakdown of emulsion, still aging 24h again, sucking filtration or centrifugation washing, to neutral, dried 6h at temperature 80 DEG C, are obtained the hydroxide of black precipitate critesistor;
Water heat transfer critesistor powder body:
B, by hydroxide 1.5g and the deionized water 80ml mixing of the critesistor that obtains, ultrasonic agitation 15min, forming critesistor suspension, it be volume is 100mL politef material that suspension is put into liner, in the high pressure water heating kettle of stainless steel, it it is 220 DEG C in reaction temperature, response time is carry out Hydrothermal Synthesis under 12h, by powder body deionized water wash 2-3 time of reaction gained, final drying, grind, obtain particle diameter at 85nm critesistor nano-powder material.
Embodiment 4
Prepare the hydroxide of critesistor:
A, being respectively weigh manganese nitrate, magnesium nitrate and nickel nitrate mixing at 2.05: 0.15: 0.8 by Mn-Mg-Ni-O mol ratio in the system of critesistor powder body, and be dissolved in deionized water, uniform stirring, being configured to concentration is 2.5mol/L, ��0Value is the nitrate mixed solution of 3; It is simultaneously respectively measure triton x-100, hexanol and hexamethylene mix and blend be configured to organic phase solution at 1: 3: 8 by volume; Again nitrate mixed solution is added drop-wise in organic phase solution gradually, magnetic agitation 1.5h, forms microemulsion; Weigh the ammonia of manganese nitrate, magnesium nitrate and nickel nitrate integral molar quantity 3 times again, it is added dropwise in microemulsion, magnetic agitation 1h under room temperature, add 150ml dehydrated alcohol magnetic agitation breakdown of emulsion, still aging 12h again, sucking filtration or centrifugation washing, to neutral, dried 8h under temperature 60 C, are obtained the hydroxide of black precipitate critesistor;
Water heat transfer critesistor powder body:
B, by hydroxide 5g and the deionized water 75ml mixing of the critesistor that obtains, ultrasonic agitation 25min, forming critesistor suspension, it be volume is 100mL politef material that suspension is put into liner, in the high pressure water heating kettle of stainless steel, it it is 240 DEG C in reaction temperature, response time is carry out Hydrothermal Synthesis under 10h, by powder body deionized water wash 2-3 time of reaction gained, final drying, grind, obtain the particle diameter critesistor nano-powder material at 65nm.
Embodiment 5
Prepare the hydroxide of critesistor:
A, being respectively weigh manganese nitrate, cobalt nitrate, nickel nitrate and magnesium nitrate mixing at 0.8: 1.95: 0.15: 0.1 by Mn-Co-Ni-Mg-O mol ratio in the system of critesistor powder body, and be dissolved in deionized water, uniform stirring, being configured to concentration is 6mol/L, ��0Value is the nitrate mixed solution of 2; It is simultaneously respectively measure triton x-100, hexanol and hexamethylene mix and blend be configured to organic phase solution at 2: 4: 9 by volume; Again nitrate mixed solution is added drop-wise in organic phase solution gradually, magnetic agitation 2h, forms microemulsion; Weigh manganese nitrate, cobalt nitrate, nickel nitrate and ammonia that magnesium nitrate integral molar quantity is 5 times again, it is added dropwise in microemulsion, magnetic agitation 2h under room temperature, add 100ml dehydrated alcohol magnetic agitation breakdown of emulsion, still aging 24h again, sucking filtration or centrifugation washing, to neutral, dried 8h under temperature 60 C, are obtained the hydroxide of black precipitate critesistor;
Water heat transfer critesistor powder body:
B, by hydroxide 3g and the deionized water 60ml mixing of the critesistor that obtains, ultrasonic agitation 20min, forming critesistor suspension, it be volume is 100mL politef material that suspension is put into liner, in the high pressure water heating kettle of stainless steel, it it is 200 DEG C in reaction temperature, response time is carry out Hydrothermal Synthesis under 14h, by powder body deionized water wash 2-3 time of reaction gained, final drying, grind, obtain the particle diameter critesistor nano-powder material at 75nm.
Embodiment 6
Prepare the hydroxide of critesistor:
A, being respectively weigh manganese nitrate, cobalt nitrate, nickel nitrate and magnesium nitrate mixing at 1.5: 0.9: 0.3: 0.3 by Mn-Co-Ni-Mg-O mol ratio in the system of critesistor powder body, and be dissolved in deionized water, uniform stirring, being configured to concentration is 0.5mol/L, ��0Value is the nitrate mixed solution of 4; It is simultaneously respectively measure triton x-100, hexanol and hexamethylene mix and blend be configured to organic phase solution at 2: 4: 8 by volume; Again nitrate mixed solution is added drop-wise in organic phase solution gradually, magnetic agitation 2h, forms microemulsion; Weigh manganese nitrate, cobalt nitrate, nickel nitrate and ammonia that magnesium nitrate integral molar quantity is 1 times again, it is added dropwise in microemulsion, magnetic agitation 2h under room temperature, add 150ml dehydrated alcohol magnetic agitation breakdown of emulsion, still aging 15h again, sucking filtration or centrifugation washing, to neutral, dried 6h under temperature 60 C, are obtained the hydroxide of black precipitate critesistor;
Water heat transfer critesistor powder body:
B, by hydroxide 5g and the deionized water 70ml mixing of the critesistor that obtains, ultrasonic agitation 15min, forming critesistor suspension, it be volume is 100mL politef material that suspension is put into liner, in the high pressure water heating kettle of stainless steel, it it is 220 DEG C in reaction temperature, response time is carry out Hydrothermal Synthesis under 12h, by powder body deionized water wash 2-3 time of reaction gained, final drying, grind, obtain the particle diameter critesistor nano-powder material at 95nm.
Embodiment 7
Any one critesistor nano-powder material that will obtain in embodiment 1-6, scanned Electronic Speculum (SEM) is analyzed, can intuitively find out that diameter of particle is between 30-100nm, and according to the XRD data after hydro-thermal, it will be seen that all present good spinel structure.
Claims (5)
1. the preparation method of microemulsion-water heat transfer critesistor powder body material, it is characterised in that follow these steps to carry out:
Prepare the hydroxide of critesistor:
A, being Mn-Co-Ni-O, Mn-Mg-Ni-O or Mn-Co-Ni-Mg-O nitrate mixing of weighing cobalt, manganese, nickel and magnesium respectively by the system of critesistor powder body, be dissolved in deionized water by mixture uniform stirring, being configured to concentration is 0.5-4mol/L, ��0Value is the nitrate mixed solution of 0.5-4, simultaneously by volume for triton x-100: hexanol: hexamethylene=0.5-2.5: 2.5-4: 7-10 measures triton x-100, hexanol and hexamethylene mix and blend respectively and be configured to organic phase solution; Again nitrate mixed solution is added drop-wise in organic phase solution gradually, magnetic agitation 1-2h, forms microemulsion; Weigh ammonia again and be added dropwise in microemulsion, magnetic agitation 1-12h under room temperature, add 100-300ml dehydrated alcohol, magnetic agitation breakdown of emulsion, still aging 12-48h again, sucking filtration or centrifugation washing, to neutral, dried 6-12h at temperature 50-100 DEG C, are obtained the hydroxide of black precipitate critesistor;
Water heat transfer critesistor powder body:
B, the critesistor that step a is obtained the quality of hydroxide be that 1.5-5g mixes with deionized water 60-80mL, ultrasonic agitation 5-30min, form critesistor suspension, again suspension is put in high pressure water heating kettle, it is 160-250 DEG C in temperature, time is carry out Hydrothermal Synthesis under 6-18h, and by powder body deionized water wash 2-3 time of reaction gained, critesistor nano-powder is ground and obtained to final drying.
2. the preparation method of microemulsion according to claim 1-water heat transfer critesistor powder body material, it is characterised in that in step a, in the system of critesistor powder body, the mol ratio of Mn-Co-Ni-O is Mn: Co: Ni=0.8-1.5: 1-2.1: 0.1-0.5; In system, the mol ratio of Mn-Mg-Ni-O is Mn: Mg: Ni=1.2-2.05: 0.15-0.3: 0.8-1.5; In system, the mol ratio of Mn-Co-Ni-Mg-O is Mn: Co: Ni: Mg=0.8-1.5: 0.9-1.95: 0.15-0.3: 0.1-0.3.
3. the preparation method of microemulsion according to claim 1-water heat transfer critesistor powder body material, it is characterised in that the addition of the ammonia in step a be Mn, 1-5 times of Co, Ni and Mg nitrate integral molar quantity.
4. the preparation method of microemulsion according to claim 1-water heat transfer critesistor powder body material, it is characterised in that the high pressure water heating kettle liner in step b is volume is 100mL politef material, and reactor is stainless steel.
5. the preparation method of microemulsion according to claim 1-water heat transfer critesistor powder body material, it is characterised in that the critesistor diameter of particle obtained in step b is distributed in 45-95nm.
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Cited By (2)
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| CN109437324A (en) * | 2018-09-17 | 2019-03-08 | 石河子大学 | A kind of spinel structure material and preparation method thereof using microreactor preparation |
| CN110372336A (en) * | 2019-08-19 | 2019-10-25 | 陈龙 | A kind of CoNiO2The co-precipitation method of thermistor powder |
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| CN1526648A (en) * | 2003-09-19 | 2004-09-08 | 中国科学院上海硅酸盐研究所 | Wet chemical process of preparing low-dimensional nano nickel sulfide crystal |
| CN101318814A (en) * | 2008-07-10 | 2008-12-10 | 中国计量学院 | Hydrothermal reaction method for manufacturing negative temperature coefficient heat-sensitive powder |
| CN101785982A (en) * | 2010-02-05 | 2010-07-28 | 北京化工大学 | Method for preparing hollow nanospheres by a hot emulsion method |
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|---|---|---|---|---|
| CN109437324A (en) * | 2018-09-17 | 2019-03-08 | 石河子大学 | A kind of spinel structure material and preparation method thereof using microreactor preparation |
| CN110372336A (en) * | 2019-08-19 | 2019-10-25 | 陈龙 | A kind of CoNiO2The co-precipitation method of thermistor powder |
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