CN105622066B - A kind of preparation method of micro emulsion-hydro-thermal method synthesis thermistor powder body material - Google Patents
A kind of preparation method of micro emulsion-hydro-thermal method synthesis thermistor powder body material Download PDFInfo
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Abstract
本发明涉及一种微乳‑水热法合成热敏电阻粉体材料的制备方法，该方法是由Mn、Mg、Ni和Co金属元素的硝酸盐组成，是以反相微乳法制备出热敏电阻的氢氧化物；将氢氧化物与去离子水混合，超声搅拌形成热敏电阻悬浮液；将悬浮液密封于高压水热釜后，放进恒温箱中进行水热合成，待反应完成冷却至室温，将反应所得的粉体用去离子水洗涤，最后干燥研磨即得热敏电阻纳米粉体。本发明所述方法制备工艺重复性好，材料成分配比准确，粉体均匀度好，纯度高，晶粒发育完整且分布均匀。为解决传统热敏电阻粉体粒度形貌分布不均匀、反应活性较差等问题，提供一种效果优良、便于推广应用的热敏电阻粉体制备方法。
The invention relates to a preparation method for synthesizing a thermistor powder material by a microemulsion-hydrothermal method. The method is composed of nitrates of Mn, Mg, Ni and Co metal elements. Hydroxide of the varistor; mix the hydroxide with deionized water, and ultrasonically stir to form the thermistor suspension; seal the suspension in a high-pressure hydrothermal kettle, put it into a thermostat for hydrothermal synthesis, and wait for the reaction to complete Cool to room temperature, wash the powder obtained by the reaction with deionized water, and finally dry and grind the thermistor nano-powder. The method of the invention has good preparation process repeatability, accurate material composition ratio, good powder uniformity, high purity, complete development of crystal grains and uniform distribution. In order to solve the problems of uneven particle size and morphology distribution and poor reactivity of traditional thermistor powder, a method for preparing thermistor powder with excellent effect and easy popularization and application is provided.
Description
Technical field
The present invention relates to a kind of preparation method of electronic component, specifically micro emulsion-hydro-thermal method synthesizes thermistor powder
The preparation method of material.
Background technique:
Inkjet printing technology is a kind of contactless digital printing technologies succeeded in developing late 1970s.Refer to
Ceramic ink is ejected on various dielectric surfaces by the nozzle of print head, such as ceramic glazed brick, acrylic, timber, paper,
To realize a kind of non-contact, high speed, the new material preparation method of low noise.And utilize inkjet printing technology preparation pottery
Ceramic material, the crucial preparation for being ceramic ink, and the good ceramic ink of stable dispersion and wherein thermistor ceramic powder
The synthesis of body is closely bound up.
Currently, the preparation of high-volume NTC thermistor powder mostly be by long-time grinding and high-temperature calcination made of,
Its raw material is mostly metal oxide, and the calcination temperature of presoma is higher, and general calcination temperature is prepared all at 1000 degree or more
Powder granularity it is uneven and powder active is low, so preparing high-precision NTC thermistor powder existing one using this method
Fixed limitation.In order to produce the NTC thermistor element of precision height, good reliability, one of key is sought to from material
Synthetic method improved, obtain that component is uniform, active powder granule higher, partial size is tiny.
Therefore seek simple process, new method that is easily operated and can effectively improving thermistor material quality becomes
It is particularly significant.Micro emulsion method is a kind of effective ways for preparing nanoparticle developed in recent years, and there is the method experiment to set
The features such as standby simple, operation is easy, particle size is controllable, scattered, narrowly distributing.It makes two kinds of mutual not phases using surfactant
Molten solvent forms a kind of uniform and stable microemulsion, and wherein the size of micelle is mainly by ω0It is worth (ω0=[aqueous solution]/[table
Face activating agent], molar ratio) influence, therefore can by adjust be added water and surfactant amount, control microemulsion in glue
The size of group.Using the micelle in microemulsion as " microreactor ", the processes such as nucleation, growth, coalescence, reunion can be made to be confined to
It is carried out in one small spherical droplets, so as to form spheric granules, in turn avoids further reuniting between particle, to reach
Nanometer scale ceramics powder granule can be prepared to control particle size, the purpose of shape, therefore using reverse microemulsion method.And hydro-thermal method
Refer in high pressure water heating kettle using aqueous solution as reaction system, by heating, pressurizeing to system or the creation of spontaneous vapour pressure
The reaction environment of one relatively-high temperature, high pressure, so that usually indissoluble or insoluble substance dissolves and recrystallize and carry out inorganic
Synthetic method.
And the ceramic powder in traditional hydro-thermal method, there are particle diameter distributions it is uneven, dispersibility is poor the problems such as,
Therefore many researchers are dedicated to optimizing in hydro-thermal method preparation nano material.This patent is for the first time by reverse microemulsion method and hydro-thermal method
In conjunction with, utilize micro emulsion method to solve the problems such as ceramic powder particle diameter distribution is irregular, pattern is different in hydro-thermal method, it is simultaneously synthesizing go out pottery
Porcelain powder requires no high-temperature calcination, is directly placed into high pressure water heating kettle and carries out hydro-thermal reaction, available crystallization same in this way
Property good, with very strongly hydrophilic, nano level superfine thermistor powder body material.
Therefore, micro emulsion-hydro-thermal method is a kind of novel chemical method for preparing superfine nano ceramic powder, shows and surmounts
The many advantages of conventional hydrothermal method, including synthesis cycle is short, accurate composition control and due to liquid phase method metal salt powder mix
Excellent homogeneity etc. on bring molecular level.In addition, the thermistor powder body material synthesized by micro emulsion-hydro-thermal method is just
It is combined in hydrophilic solvent, dispersion effect is good in its solvent, convenient for preparing the ceramic ink of high solids content and stable dispersion
Water.
Summary of the invention
Present invention aims at provide a kind of preparation method of micro emulsion-hydro-thermal method synthesis thermistor powder body material, the party
Method is made of the nitrate of Mn, Co, Ni and Mg metallic element, is the hydroxide that thermistor is prepared with reverse microemulsion method
Object；Hydroxide is mixed with deionized water, ultrasonic agitation forms thermistor suspension；Suspension is sealed in high pressure hydro-thermal
It after kettle, puts into and carries out hydrothermal synthesis in insulating box, completion to be reacted is cooled to room temperature, and will react resulting powder deionized water
Washing, last drying and grinding is up to thermistor nano-powder.The method of the invention preparation process is reproducible, material composition
Proportion speed, powder good evenness, purity is high, grain development is complete and is evenly distributed.To solve conventional thermistor powder grain
It spends that topographic profile is uneven, the problems such as reactivity is poor, a kind of excellent effect, thermistor powder easy to promote and utilize is provided
Preparation.
A kind of micro emulsion of the present invention-hydro-thermal method synthesis thermistor powder body material preparation method, follows these steps
It carries out: preparing the hydroxide of thermistor:
It a, is that Mn-Co-Ni-O, Mn-Mg-Ni-O or Mn-Co-Ni-Mg-O are weighed respectively by the system of thermistor powder
The nitrate mixing of cobalt, manganese, nickel and magnesium, is dissolved in uniform stirring in deionized water for mixture, and being configured to concentration is 0.5-4mol/
L, ω0Value is the nitrate mixed solution of 0.5-4, while being by volume triton x-100: n-hexyl alcohol: hexamethylene=0.5-
2.5: 2.5-4: 7-10 measures triton x-100, n-hexyl alcohol and hexamethylene mixing respectively is configured to organic phase solution；Again will
Nitrate mixed solution is gradually added drop-wise in organic phase solution, magnetic agitation 1-2h, forms microemulsion；Ammonium hydroxide is weighed again to add dropwise
Enter in microemulsion, at room temperature magnetic agitation 1-12h, adds 100-300ml dehydrated alcohol, magnetic agitation demulsification, then stand old
Change 12-48h, filters or centrifuge separation washing is to neutrality, dry 6-12h at 50-100 DEG C of temperature, obtain black precipitate temperature-sensitive
The hydroxide of resistance；
Hydro-thermal method synthesizes thermistor powder:
B, the quality of the hydroxide of the obtained thermistor of step a is mixed for 1.5-5g with deionized water 60-80mL,
5-30min is stirred by ultrasonic, forms thermistor suspension, then suspension is put into high pressure water heating kettle, is 160-250 in temperature
DEG C, the time is to carry out hydrothermal synthesis under 6-18h, resulting powder will be reacted and be washed with deionized 2-3 times, last drying and grinding
Up to thermistor nano-powder.
The molar ratio of Mn-Co-Ni-O is Mn: Co: Ni=0.8-1.5: 1- in the system of thermistor powder in step a
2.1:0.1-0.5；The molar ratio of Mn-Mg-Ni-O is Mn: Mg: Ni=1.2-2.05: 0.15-0.3: 0.8-1.5 in system；Body
The molar 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 in system.
The additional amount of ammonium hydroxide in step a is 1-5 times of Mn, Co, Ni and Mg nitrate integral molar quantity.
High pressure water heating kettle liner in step b is that volume is 100mL polytetrafluoroethylene (PTFE) material, and reaction kettle is stainless steel
Matter；
Thermistor diameter of particle obtained in step b is distributed in 45-95nm.
The wherein ω of the nitrate mixed solution in step a0It is worth (ω0=[aqueous metal salt]/[surfactant], rubs
That ratio) it is 0.5-4.
A kind of micro emulsion of the present invention-hydro-thermal method synthesis thermistor powder body material preparation method, this method feature
Are as follows:
The formula and content of thermistor powder are varied, can be adjusted, can make with market and experiment demand
The thermistor superfine powder of different systems.
The thermistor powder that micro emulsion-hydro-thermal method synthesizes has even particle size distribution, reactivity high, good hydrophilic property
Advantage, and this method is simple and convenient practical, promotes convenient for the marketization.
The thermistor ceramic powder that micro emulsion-hydro-thermal method is prepared easily facilitates height since it is with extremely strong hydrophily
The preparation of solid content ceramic ink.
Detailed description of the invention
Fig. 1 is 1 gained thermistor powder SEM image of the embodiment of the present invention；
Fig. 2 is 2 gained thermistor powder XRD diagram picture of the embodiment of the present invention.
Specific embodiment
Embodiment 1
Prepare the hydroxide of thermistor:
A, by Mn-Co-Ni-O molar ratio in the system of thermistor powder be 0.8: 2.1: 0.1 weigh respectively manganese nitrate,
Cobalt nitrate and nickel nitrate mixing, and be dissolved in deionized water, uniform stirring, being configured to concentration is 0.5mol/L, ω0Value is 0.5
Nitrate mixed solution；Triton x-100 is measured respectively for 2: 3: 10 by volume simultaneously, and n-hexyl alcohol and hexamethylene mixing are stirred
It mixes and is configured to organic phase solution；Nitrate mixed solution is gradually added drop-wise in organic phase solution again, magnetic agitation 1h, is formed micro-
Lotion；Manganese nitrate, cobalt nitrate and 5 times of nickel nitrate integral molar quantity of ammonium hydroxide are weighed again, are added dropwise in microemulsion, at room temperature
Magnetic agitation 1h adds the demulsification of 100ml dehydrated alcohol magnetic agitation, then still aging 12h, filters or centrifuge separation is washed extremely
Neutrality dries 12h under temperature 50 C, obtains the hydroxide of black precipitate thermistor；
Hydro-thermal method synthesizes thermistor powder:
B, obtained thermistor hydroxide 4g and deionized water 76ml is mixed, 30min is stirred by ultrasonic, form temperature-sensitive
Resistance suspension, it is 100mL polytetrafluoroethylene (PTFE) material, the high pressure water heating kettle of stainless steel material that by suspension, to be put into liner, which be volume,
In, it is 250 DEG C in reaction temperature, carries out hydrothermal synthesis under reaction time 18h, resulting powder will be reacted and be washed with deionized
It 2-3 times, finally dries, grinds the thermistor nano-powder material to get partial size in 45nm.
Embodiment 2
Prepare the hydroxide of thermistor:
A, manganese nitrate, nitre are weighed respectively for 1.5: 1: 0.5 by Mn-Co-Ni-O molar ratio in the system of thermistor powder
Sour cobalt and nickel nitrate mixing, and be dissolved in deionized water, uniform stirring, being configured to concentration is 4mol/L, ω0The nitric acid that value is 1
Mixed salt solution；Triton x-100 is measured respectively for 0.5: 2.5: 7 by volume simultaneously, and n-hexyl alcohol and hexamethylene are mixed
It is configured to organic phase solution；Nitrate mixed solution is gradually added drop-wise in organic phase solution again, magnetic agitation 2h, forms micro emulsion
Liquid；Manganese nitrate, cobalt nitrate and 3 times of nickel nitrate integral molar quantity of ammonium hydroxide are weighed again, are added dropwise in microemulsion, at room temperature magnetic
Power stirs 12h, adds the demulsification of 300ml dehydrated alcohol magnetic agitation, then still aging 48h, filters or centrifuge separation is washed extremely
Neutrality dries 6h at 100 DEG C of temperature, obtains the hydroxide of black precipitate thermistor；
Hydro-thermal method synthesizes thermistor powder:
B, the hydroxide 3g of obtained thermistor and deionized water 60ml is mixed, 5min is stirred by ultrasonic, form heat
Quick resistance suspension, it is 100mL polytetrafluoroethylene (PTFE) material, the high pressure hydro-thermal of stainless steel material that by suspension, to be put into liner, which be volume,
It is 160 DEG C in reaction temperature in kettle, the reaction time is to carry out hydrothermal synthesis under 16h, will react resulting powder deionized water
Washing 2-3 times, is finally dried, and grinds the thermistor nano-powder material to get partial size in 65nm.
Embodiment 3
Prepare the hydroxide of thermistor:
A, by Mn-Mg-Ni-O molar ratio in the system of thermistor powder be 1.2: 0.3: 1.5 weigh respectively manganese nitrate,
Magnesium nitrate and nickel nitrate mixing, and it is dissolved in uniform stirring in deionized water, being configured to concentration is 1.5mol/L, ω0The nitre that value is 4
Hydrochlorate mixed solution；Triton x-100 is measured respectively for 2.5: 4: 10 by volume simultaneously, and n-hexyl alcohol and hexamethylene are mixed
It is configured to organic phase solution；Nitrate mixed solution is gradually added drop-wise in organic phase solution again, magnetic agitation 1h, forms micro emulsion
Liquid；The ammonium hydroxide that manganese nitrate, magnesium nitrate and nickel nitrate integral molar quantity amount are 4 times is weighed again, is added dropwise in microemulsion, room temperature
Lower magnetic agitation 2h, add 200ml dehydrated alcohol magnetic agitation demulsification, then it is still aging for 24 hours, filter or centrifuge separation washing
To neutrality, 6h is dried at 80 DEG C of temperature, obtains the hydroxide of black precipitate thermistor；
Hydro-thermal method synthesizes thermistor powder:
B, the hydroxide 1.5g of obtained thermistor and deionized water 80ml is mixed, 15min is stirred by ultrasonic, formed
Thermistor suspension, it is 100mL polytetrafluoroethylene (PTFE) material, the high pressure water of stainless steel material that by suspension, to be put into liner, which be volume,
It is 220 DEG C in reaction temperature in hot kettle, the reaction time is to carry out hydrothermal synthesis under 12h, will react resulting powder deionization
Water washing 2-3 times is finally dried, and grinding is to get partial size in 85nm thermistor nano-powder material.
Embodiment 4
Prepare the hydroxide of thermistor:
A, nitric acid is weighed respectively for 2.05: 0.15: 0.8 by Mn-Mg-Ni-O molar ratio in the system of thermistor powder
Manganese, magnesium nitrate and nickel nitrate mixing, and be dissolved in deionized water, uniform stirring, being configured to concentration is 2.5mol/L, ω0Value
For 3 nitrate mixed solution；Triton x-100, n-hexyl alcohol and hexamethylene mixing are measured respectively for 1: 3: 8 by volume simultaneously
Stirring is configured to organic phase solution；Nitrate mixed solution is gradually added drop-wise in organic phase solution again, magnetic agitation 1.5h, shape
At microemulsion；Manganese nitrate, magnesium nitrate and 3 times of nickel nitrate integral molar quantity of ammonium hydroxide are weighed again, are added dropwise in microemulsion, room
The lower magnetic agitation 1h of temperature, adds the demulsification of 150ml dehydrated alcohol magnetic agitation, then still aging 12h, filters or centrifuge separation is washed
It washs to neutrality, dries 8h under temperature 60 C, obtain the hydroxide of black precipitate thermistor；
Hydro-thermal method synthesizes thermistor powder:
B, the hydroxide 5g of obtained thermistor and deionized water 75ml is mixed, 25min is stirred by ultrasonic, form heat
Quick resistance suspension, it is 100mL polytetrafluoroethylene (PTFE) material, the high pressure hydro-thermal of stainless steel material that by suspension, to be put into liner, which be volume,
It is 240 DEG C in reaction temperature in kettle, the reaction time is to carry out hydrothermal synthesis under 10h, will react resulting powder deionized water
Washing 2-3 times, is finally dried, and grinds the thermistor nano-powder material to get partial size in 65nm.
Embodiment 5
Prepare the hydroxide of thermistor:
A, claim respectively by Mn-Co-Ni-Mg-O molar ratio in the system of thermistor powder for 0.8: 1.95: 0.15: 0.1
Manganese nitrate, cobalt nitrate, nickel nitrate and magnesium nitrate mixing are taken, and is dissolved in deionized water, uniform stirring, being configured to concentration is
6mol/L, ω0The nitrate mixed solution that value is 2；Triton x-100, n-hexyl alcohol are measured respectively for 2: 4: 9 by volume simultaneously
Organic phase solution is configured to hexamethylene mixing；Nitrate mixed solution is gradually added drop-wise in organic phase solution again, magnetic
Power stirs 2h, forms microemulsion；The ammonium hydroxide that manganese nitrate, cobalt nitrate, nickel nitrate and magnesium nitrate integral molar quantity are 5 times is weighed again, it will
It is added dropwise in microemulsion, at room temperature magnetic agitation 2h, adds the demulsification of 100ml dehydrated alcohol magnetic agitation, then stand old
Change for 24 hours, filters or centrifuge separation washing is to neutrality, dry 8h under temperature 60 C, obtain the hydrogen-oxygen of black precipitate thermistor
Compound；
Hydro-thermal method synthesizes thermistor powder:
B, the hydroxide 3g of obtained thermistor and deionized water 60ml is mixed, 20min is stirred by ultrasonic, form heat
Quick resistance suspension, it is 100mL polytetrafluoroethylene (PTFE) material, the high pressure hydro-thermal of stainless steel material that by suspension, to be put into liner, which be volume,
It is 200 DEG C in reaction temperature in kettle, the reaction time is to carry out hydrothermal synthesis under 14h, will react resulting powder deionized water
Washing 2-3 times, is finally dried, and grinds the thermistor nano-powder material to get partial size in 75nm.
Embodiment 6
Prepare the hydroxide of thermistor:
A, it is weighed respectively by Mn-Co-Ni-Mg-O molar ratio in the system of thermistor powder for 1.5: 0.9: 0.3: 0.3
Manganese nitrate, cobalt nitrate, nickel nitrate and magnesium nitrate mixing, and be dissolved in deionized water, uniform stirring, being configured to concentration is
0.5mol/L, ω0The nitrate mixed solution that value is 4；Measure triton x-100 respectively by volume simultaneously for 2: 4: 8, just oneself
Pure and mild hexamethylene mixing is configured to organic phase solution；Nitrate mixed solution is gradually added drop-wise in organic phase solution again,
Magnetic agitation 2h forms microemulsion；The ammonium hydroxide that manganese nitrate, cobalt nitrate, nickel nitrate and magnesium nitrate integral molar quantity are 1 times is weighed again,
It is added dropwise in microemulsion, at room temperature magnetic agitation 2h, adds the demulsification of 150ml dehydrated alcohol magnetic agitation, then stand
It is aged 15h, filters or centrifuge separation washing is to neutrality, dry 6h under temperature 60 C, obtain the hydrogen of black precipitate thermistor
Oxide；
Hydro-thermal method synthesizes thermistor powder:
B, the hydroxide 5g of obtained thermistor and deionized water 70ml is mixed, 15min is stirred by ultrasonic, form heat
Quick resistance suspension, it is 100mL polytetrafluoroethylene (PTFE) material, the high pressure hydro-thermal of stainless steel material that by suspension, to be put into liner, which be volume,
It is 220 DEG C in reaction temperature in kettle, the reaction time is to carry out hydrothermal synthesis under 12h, will react resulting powder deionized water
Washing 2-3 times, is finally dried, and grinds the thermistor nano-powder material to get partial size in 95nm.
Embodiment 7
By any one thermistor nano-powder material obtained in embodiment 1-6, analyzed through scanning electron microscope (SEM),
Diameter of particle can be intuitively found out between 30-100nm, and according to the XRD data after hydro-thermal, it will be seen that show good point
Spinel structure.
Claims (1)
1. a kind of micro emulsion-hydro-thermal method synthesis thermistor powder body material preparation method, it is characterised in that follow these steps to carry out:
Prepare the hydroxide of thermistor:
A, by the system of thermistor powder be Mn-Co-Ni-O, Mn-Mg-Ni-O or Mn-Co-Ni-Mg-O weigh respectively cobalt,
The nitrate of manganese, nickel and magnesium mixes, and mixture is dissolved in uniform stirring in deionized water, and being configured to concentration is 0.5-4 mol/L
And ω0Value is aqueous metal salt/surfactant molar ratio 0.5-4 nitrate mixed solution, while being by volume song
Draw logical X-100: n-hexyl alcohol: hexamethylene=0.5-2.5: 2.5-4: 7-10 measures triton x-100, n-hexyl alcohol and hexamethylene respectively
Alkane mixing is configured to organic phase solution；Nitrate mixed solution is gradually added drop-wise in organic phase solution again, magnetic agitation
1-2 h forms microemulsion；It weighs ammonium hydroxide again to be added dropwise in microemulsion, magnetic agitation 1-12 h, adds 100- at room temperature
300 mL dehydrated alcohols, magnetic agitation demulsification, then still aging 12-48 h, filter or centrifuge separation washing is to neutrality, in temperature
6-12 h is dried at 50-100 DEG C of degree, obtains black precipitate-thermistor hydroxide, wherein the Mn- of thermistor powder
Molar ratio in Co-Ni-O system is Mn: Co: Ni=0.8-1.5: 1-2.1: 0.1-0.5；Mole in Mn-Mg-Ni-O system
Than being Mn: Mg: Ni=1.2-2.05: 0.15-0.3: 0.8-1.5；Molar ratio in Mn-Co-Ni-Mg-O system is Mn: Co: Ni
: Mg=0.8-1.5: 0.9-1.95: 0.15-0.3:0.1-0.3；The additional amount of ammonium hydroxide is Mn, Co, Ni and Mg nitrate total moles
1-5 times of amount；
Hydro-thermal method synthesizes thermistor powder:
B, the hydroxide of the obtained thermistor of step a is mixed for 1.5-5 g with deionized water 60-80 mL by quality, is surpassed
Sound stirs 5-30 min, forms thermistor suspension, then suspension is put into liner volume is 100 mL, liner material is poly-
It is 160-250 DEG C in temperature, the time is 6-18 h in tetrafluoroethene material, the high pressure water heating kettle that reaction kettle is stainless steel material
Lower carry out hydrothermal synthesis, will react resulting powder and is washed with deionized 2-3 times, last drying and grinding exists up to particle diameter distribution
45-95 nm thermistor nano-powder.
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| CN101318814A (en) * | 2008-07-10 | 2008-12-10 | 中国计量学院 | Preparation Method of Negative Temperature Coefficient Heat Sensitive Powder——Hydrothermal Reaction Method |
| 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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| CN101318814A (en) * | 2008-07-10 | 2008-12-10 | 中国计量学院 | Preparation Method of Negative Temperature Coefficient Heat Sensitive Powder——Hydrothermal Reaction Method |
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