CN103045180B - Low-conductivity nanofluid and preparation method thereof - Google Patents

Low-conductivity nanofluid and preparation method thereof Download PDF

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Publication number
CN103045180B
CN103045180B CN201210573980.5A CN201210573980A CN103045180B CN 103045180 B CN103045180 B CN 103045180B CN 201210573980 A CN201210573980 A CN 201210573980A CN 103045180 B CN103045180 B CN 103045180B
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nano
conductivity
exchange resin
suspension
oxide
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CN103045180A (en
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朱海涛
雷清泉
吴大雄
苏静文
王连刚
张灿英
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Qingdao University of Science and Technology
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Abstract

The invention relates to a low-conductivity nanofluid and a preparation method thereof, belonging to the field of electrical and electronic equipment cooling. The conductivity of the nanofluid is less than 1 microsecond/cm; and the nanofluid comprises the following components in mass percentage: 40.0-99.0% of ultrapure water, 0.0-60.0% of dihydric alcohol, 0.1-10.0% of nanopowder and 0.01-3.0% of dispersing agent. The preparation method comprises the following steps of: dispersing the calcined nanopowder into ultrapure water, removing charged foreign ions, coating the dispersing agent on the surfaces of nanoparticles, and removing foreign ions again to obtain the low-conductivity nanofluid. Compared with the conventional cooling liquid, the nanofluid is high in heat exchanging capability and significant in technical advantages.

Description

A kind of Low-conductivity nanofluid and preparation method thereof
Technical field:
The present invention relates to a kind of Low-conductivity nanofluid and preparation method thereof, belong to power electronic equipment cooling field.
Background technology:
Along with the develop rapidly of Power Electronic Technique, high-power, high power density device is by a large amount of development and application.Power electronic equipment is while power increases, and its hear rate is also in increase, and the surface heat flux during work of some power electronic devices has reached tens of watts and even upper hectowatt every square centimeter.If a large amount of hear rates can not distribute in time, will greatly affect the reliability of electronics.Therefore, how effectively to be emitted by the waste heat in power electronic equipment, thus extend its life-span, enhancing reliability, tool is of great significance.At present, the type of cooling that power electronic equipment is conventional mainly contains natural air cooled, forced air cooling and forces liquid cooling three major types.Wherein, natural air cooled limited with cooling power that is forced air cooling, often can only be used for the lower occasion of heat flow density; The heat flow density that liquid cooling is born is large, and radiating efficiency is high, and heat load thermograde is little, the occasion that applicable heat flow density is higher.The cooling fluid that liquid cooling adopts mainly contains water, ethylene glycol, wet goods, but its thermal conductivity of these liquid is low, exchange capability of heat is poor, and oneself, through not meeting the cooling requirements of high loading power electronic equipment, is necessary the cooling fluid of development of new, high efficient heat exchanging.The appearance of nano-fluid technology, the development for engine-cooling system provides new thinking.Nano-fluid is metal or the particle stabilized a kind of novel heat exchange working medium being suspended to formation in conventional fluid (water, ethylene glycol etc.) of non pinetallic nano.Existing research shows, compared with conventional fluid, nano-fluid has higher thermal conductivity and excellent heat exchange property, and thus nano-fluid is expected to the cooling requirements solving power electronic equipment high loading.
As everyone knows, most power electronic equipments is in operation and often there is higher electric field, have up to several kilovolts, several ten thousand volts even hundreds of thousands of volt.And nano grain surface has scission of link, particle surface is usually with electric charge.In the electric field, the nano particle in nano-fluid very easily produces electrostatic interaction with electrode, thus produces absorption and deposition, causes heat exchange efficiency to reduce even cooling failure.Therefore, nano-fluid is applied to the cooling of power electronic equipment, how eliminate the surface charge of nano particle, reduce the specific conductivity of nano-fluid, prepare and stablize under the electric field and the excellent nano-fluid of heat exchange property is key.The method can preparing nano-fluid in enormous quantities of current report mainly contains dispersion method and wet chemistry method.Dispersion method being pH value by changing system, adding positively charged ion or anionic dispersing agents etc., and is aided with ultrasonic or mechanical stirring and nano-powder is distributed in basal liquid forms nano-fluid.As Zhu Dongsheng etc. has prepared Al by changing pH value and adding anionic dispersing agents Sodium dodecylbenzene sulfonate 2o 3/ water nano-fluid (Materials Science and Engineering, 2008,1,56-61); Peng little Fei etc. utilize anionic dispersing agents Sodium dodecylbenzene sulfonate, and are aided with ultrasonic disperse, nanometer Al 2o 3, nanometer CuO, Nano-meter SiO_2 2, the powder such as nanometer Cu is distributed in distilled water, ethylene glycol, propylene glycol and obtains multiple nano-fluid (Peng little Fei, nano-fluid high temperature heat transfer underlying issue research in car radiator, Zhejiang University Ph.D. Dissertation, 2007).Changing pH value, adding the object of positively charged ion or anionic dispersing agents is improve the zeta current potential of nano grain surface, thus improves the standard stability of nano-fluid.But the raising of zeta current potential, can cause the increase of nano-fluid specific conductivity, the nano-fluid of thus preparation like this cannot be used for the cooling of the power electronic equipment having electric field to exist.Wet chemistry method utilizes the chemical reaction in liquid phase directly in liquid phase medium, to prepare nano particle, thus obtain nano-fluid, and the method combines the preparation of the preparation of nano particle and nano-fluid.Such as, Zhu etc. add reductive agent in the ethylene glycol solution of copper sulfate, adopt microwave heating directly to obtain Cu/ ethylene glycol nano-fluid (J.Colloid Interf.Sci.2004,277,100); Zhu etc. copper hydroxide nanoparticulate dispersed in water, employing ammonium citrate is dispersion agent, makes copper hydroxide be decomposed into cupric oxide by ultrasonic and microwave heating, thus obtains CuO/ water nano-fluid (J.Phys.Chem.C 2007,111,1646-1650).In the nano-fluid adopting wet chemistry method to prepare, owing to there is the foreign ion that raw material is introduced, its specific conductivity is higher, cannot stablize under the electric field, also just cannot meet the requirement of power electronic equipment cooling.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of Low-conductivity nanofluid and preparation method thereof, the requirement of the power electronic equipment cooling having electric field to exist can be met.
To achieve these goals, the present invention adopts following technical measures:
Low-conductivity nanofluid of the present invention, its specific conductivity is less than 1 μ s/cm, and by mass percent, nano-fluid comprises following component: ultrapure water 40.0 ~ 99.0%, dibasic alcohol 0.0 ~ 60.0%, nano-powder 0.1 ~ 10.0%, dispersion agent 0.01 ~ 3.0%.
Wherein, described ultrapure resistivity of water is greater than 15M Ω cm.Described nano-powder is any one or arbitrary combination in nano silicon oxide, nanometer silicon carbide, nano aluminium oxide, nano zine oxide, nano cupric oxide, nano titanium oxide; The particle diameter of nano-powder is 10 ~ 100nm.Described dispersion agent is any one or its arbitrary combination in polyoxyethylene-type non-ionic dispersing agent, polyol type non-ionic dispersing agent, alkylol amide type non-ionic dispersing agent; By mass percent, the add-on of dispersion agent is 1 ~ 30% of nano particle.Described dibasic alcohol is any one or arbitrary combination in ethylene glycol, propylene glycol, Diethylene Glycol.
The preparation method of Low-conductivity nanofluid of the present invention, comprises following consecutive steps:
(1) nano-powder is carried out calcination processing;
(2) by mass, mixed by the nano-powder after 1 part of calcination processing with 5 ~ 30 parts of ultrapure waters, ultrasonic or powerful mechanical stirring 0.5 ~ 12 hour, obtains finely dispersed suspension;
(3) suspension of gained is passed through ion exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 5 μ s/cm;
(4) in the suspension of low conductivity, add dispersion agent, stir 1 ~ 24 hour, make dispersion agent evenly be coated on nano grain surface;
(5) nano granule suspension after coated again by ion exchange resin, is removed charged foreign ion, is made the specific conductivity of suspension be less than 1 μ s/cm;
(6) in the suspension of step (5), add ultrapure water or dibasic alcohol, mix the nano-fluid obtaining low conductivity, its specific conductivity is less than 1 μ s/cm.
Wherein, the calcination processing temperature of described nano-powder is 300 ~ 600 DEG C.Described ion exchange resin is that hydrogen type cation exchange resin mixes with hydroxyl type anion exchange resin the Ion Exchange Resin In The Mixing Bed formed; The mass ratio of hydrogen type cation exchange resin and hydroxyl type anion exchange resin is 1:0.5 ~ 3.
In preparation process of the present invention, by calcining in certain temperature and atmosphere nano-powder, to eliminate nano grain surface defect and adsorbing contaminant, thus reduce nanoparticle surface charge; Utilize ion exchange resin to the adsorption of charged impurity ion, remove foreign ion, thus reduce the specific conductivity of nano-fluid further; Utilize the dissemination of specific dispersant, the dispersion stabilization of nano particle in nano-fluid can be improved, reduce the specific conductivity of nano-fluid simultaneously further.
Compared with prior art, the present invention has following positively effect:
1, the specific conductivity of nano-fluid of the present invention is less than 1 μ s/cm, in the electric field can stable existence, does not adsorb, does not deposit, can be used in the cooling of power electronic equipment;
2, cool liquid phase ratio with tradition, its exchange capability of heat improves 5 ~ 30%, thus has obvious technical superiority.
Embodiment
Below in conjunction with embodiment, set forth the present invention further.
Embodiment 1
By the nano aluminium oxide of particle diameter 50 nanometer at 600 DEG C, H 2calcination processing 3h under atmosphere;
After cool to room temperature, get the ultrapure water that 1 kilogram of nano aluminium oxide and 10 kilograms of resistivity are 16M Ω cm and mix, ultrasonic disperse 12 hours, obtains finely dispersed suspension;
The suspension of gained is mixed the Ion Exchange Resin In The Mixing Bed (mass ratio of the two is 1:2) formed with hydroxyl type anion exchange resin by hydrogen type cation exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 5 μ s/cm;
In the suspension of low conductivity, add 100 grams of polyoxyethylene-type non-ionic dispersing agents, stir 4 hours, make dispersion agent evenly be coated on nano grain surface;
Nano granule suspension after coated mixes the Ion Exchange Resin In The Mixing Bed (mass ratio of the two is 1:1) formed again with hydroxyl type anion exchange resin by hydrogen type cation exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 1 μ s/cm;
In above-mentioned suspension, add the ultrapure water that 10 kilograms of resistivity are 17M Ω cm, mix the nano-fluid obtaining low conductivity, its specific conductivity is 0.1 ~ 0.5 μ s/cm;
Compared with pure water, its exchange capability of heat improves 25%.
Embodiment 2
By the nanometer silicon carbide of particle diameter 40 nanometer at 450 DEG C, calcination processing 1h under oxygen atmosphere;
After cool to room temperature, get the ultrapure water that 1 kilogram of nanometer silicon carbide and 20 kilograms of resistivity are 16M Ω cm and mix, ultrasonic disperse 6 hours, obtains finely dispersed suspension;
The suspension of gained is mixed the Ion Exchange Resin In The Mixing Bed (mass ratio of the two is 1:1) formed with hydroxyl type anion exchange resin by hydrogen type cation exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 5 μ s/cm;
In the suspension of low conductivity, add 300 grams of alkylol amide type non-ionic dispersing agents, stir 12 hours, make dispersion agent evenly be coated on nano grain surface;
Nano granule suspension after coated mixes the Ion Exchange Resin In The Mixing Bed (mass ratio of the two is 1:0.8) formed again with hydroxyl type anion exchange resin by hydrogen type cation exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 1 μ s/cm;
In above-mentioned suspension, add ultrapure water and 10 kilograms of ethylene glycol that 10 kilograms of resistivity are 17M Ω cm, mix the nano-fluid obtaining low conductivity, its specific conductivity is 0.05 ~ 0.3 μ s/cm;
With the water/ethylene glycol basis liquid phase ratio of equal proportion, its exchange capability of heat improves 30%.
Embodiment 3
By the nano titanium oxide of particle diameter 20 nanometer at 300 DEG C, calcination processing 6h under nitrogen atmosphere;
After cool to room temperature, get the ultrapure water that 1 kilogram of nano titanium oxide and 30 kilograms of resistivity are 16M Ω cm and mix, ultrasonic disperse 6 hours, obtains finely dispersed suspension;
The suspension of gained is mixed the Ion Exchange Resin In The Mixing Bed (mass ratio of the two is 1:1) formed with hydroxyl type anion exchange resin by hydrogen type cation exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 5 μ s/cm;
In the suspension of low conductivity, add 100 grams of polyol type non-ionic dispersing agents, stir 3 hours, make dispersion agent evenly be coated on nano grain surface;
Nano granule suspension after coated mixes the Ion Exchange Resin In The Mixing Bed (mass ratio of the two is 1:1) formed again with hydroxyl type anion exchange resin by hydrogen type cation exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 1 μ s/cm;
In above-mentioned suspension, add ultrapure water and 15 kilograms of propylene glycol that 15 kilograms of resistivity are 17M Ω cm, mix the nano-fluid obtaining low conductivity, its specific conductivity is 0.1 ~ 0.8 μ s/cm;
With the water/propylene glycol basis liquid phase ratio of equal proportion, its exchange capability of heat improves 10%.
Embodiment 4
By the nano zine oxide of particle diameter 60 nanometer at 500 DEG C, calcination processing 2h under oxygen atmosphere;
After cool to room temperature, get the ultrapure water that 1 kilogram of nano zine oxide and 25 kilograms of resistivity are 16M Ω cm and mix, ultrasonic disperse 12 hours, obtains finely dispersed suspension;
The suspension of gained is mixed the Ion Exchange Resin In The Mixing Bed (mass ratio of the two is 1:3) formed with hydroxyl type anion exchange resin by hydrogen type cation exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 5 μ s/cm;
In the suspension of low conductivity, add 300 grams of polyoxyethylene-type non-ionic dispersing agents, stir 6 hours, make dispersion agent evenly be coated on nano grain surface;
Nano granule suspension after coated mixes the Ion Exchange Resin In The Mixing Bed (mass ratio of the two is 1:2) formed again with hydroxyl type anion exchange resin by hydrogen type cation exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 1 μ s/cm;
In above-mentioned suspension, add ultrapure water and 15 kilograms of Diethylene Glycols that 10 kilograms of resistivity are 17M Ω cm, mix the nano-fluid obtaining low conductivity, its specific conductivity is 0.3 ~ 0.8 μ s/cm;
Compared with the water/Diethylene Glycol basal liquid of equal proportion, its exchange capability of heat improves 12%.
Embodiment 5
By the nano silicon oxide of particle diameter 30 nanometer at 600 DEG C, calcination processing 6h under oxygen atmosphere;
After cool to room temperature, get the ultrapure water that 1 kilogram of nano silicon oxide and 30 kilograms of resistivity are 16M Ω cm and mix, ultrasonic disperse 12 hours, obtains finely dispersed suspension;
The suspension of gained is mixed the Ion Exchange Resin In The Mixing Bed (mass ratio of the two is 1:1.5) formed with hydroxyl type anion exchange resin by hydrogen type cation exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 5 μ s/cm;
In the suspension of low conductivity, add 300 grams of polyol type non-ionic dispersing agents, stir 6 hours, make dispersion agent evenly be coated on nano grain surface;
Nano granule suspension after coated mixes the Ion Exchange Resin In The Mixing Bed (mass ratio of the two is 1:1.2) formed again with hydroxyl type anion exchange resin by hydrogen type cation exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 1 μ s/cm;
In above-mentioned suspension, add ultrapure water and 30 kilograms of ethylene glycol that 20 kilograms of resistivity are 17M Ω cm, mix the nano-fluid obtaining low conductivity, its specific conductivity is 0.3 ~ 0.8 μ s/cm;
With the water/ethylene glycol basis liquid phase ratio of equal proportion, its exchange capability of heat improves 8%.
Embodiment 6
By the nano cupric oxide of particle diameter 60 nanometer at 350 DEG C, calcination processing 1h under nitrogen atmosphere;
After cool to room temperature, get the ultrapure water that 1 kilogram of nano cupric oxide and 10 kilograms of resistivity are 16M Ω cm and mix, ultrasonic disperse 3 hours, obtains finely dispersed suspension;
The suspension of gained is mixed the Ion Exchange Resin In The Mixing Bed (mass ratio of the two is 1:0.8) formed with hydroxyl type anion exchange resin by hydrogen type cation exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 5 μ s/cm;
In the suspension of low conductivity, add 50 grams of alkylol amide type non-ionic dispersing agents, stir 2 hours, make dispersion agent evenly be coated on nano grain surface;
Nano granule suspension after coated mixes the Ion Exchange Resin In The Mixing Bed (mass ratio of the two is 1:1) formed again with hydroxyl type anion exchange resin by hydrogen type cation exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 1 μ s/cm;
In above-mentioned suspension, add the ultrapure water that 10 kilograms of resistivity are 17M Ω cm, mix the nano-fluid obtaining low conductivity, its specific conductivity is 0.05 ~ 0.5 μ s/cm;
Compared with pure water, its exchange capability of heat improves 15%.

Claims (7)

1. a Low-conductivity nanofluid, it is characterized in that, the specific conductivity of nano-fluid is less than 1 μ s/cm, by mass percent, nano-fluid comprises following component: ultrapure water 40.0 ~ 99.0%, dibasic alcohol 0.0 ~ 60.0%, the nano-powder 0.1 ~ 10.0% in certain temperature and atmosphere after calcination processing, dispersion agent 0.01 ~ 3.0%; Described nano-powder is any one or arbitrary combination in nano silicon oxide, nanometer silicon carbide, nano aluminium oxide, nano zine oxide, nano cupric oxide, nano titanium oxide;
The temperature of described calcination processing is 300 ~ 600 DEG C;
The atmosphere of described nano silicon oxide, nanometer silicon carbide, nano zine oxide calcination processing is oxygen;
The atmosphere of described nano cupric oxide, nano titanium oxide calcination processing is nitrogen;
The atmosphere of described nano aluminium oxide calcination processing is hydrogen.
2. Low-conductivity nanofluid as claimed in claim 1, is characterized in that: described ultrapure resistivity of water is greater than 15M Ω cm.
3. Low-conductivity nanofluid as claimed in claim 1, is characterized in that: the particle diameter of described nano-powder is 10 ~ 100nm.
4. Low-conductivity nanofluid as claimed in claim 1, is characterized in that: described dispersion agent is any one or its arbitrary combination in polyoxyethylene-type non-ionic dispersing agent, polyol type non-ionic dispersing agent, alkylol amide type non-ionic dispersing agent; By mass percent, the add-on of dispersion agent is 1 ~ 30% of nano particle.
5. Low-conductivity nanofluid as claimed in claim 1, is characterized in that: described dibasic alcohol is any one or arbitrary combination in ethylene glycol, propylene glycol, Diethylene Glycol.
6. the preparation method of Low-conductivity nanofluid as claimed in claim 1, is characterized in that: the method comprises following consecutive steps:
(1) nano-powder is carried out calcination processing in certain temperature and atmosphere; Described nano-powder is any one or arbitrary combination in nano silicon oxide, nanometer silicon carbide, nano aluminium oxide, nano zine oxide, nano cupric oxide, nano titanium oxide;
The temperature of described calcination processing is 300 ~ 600 DEG C;
The atmosphere of described nano silicon oxide, nanometer silicon carbide, nano zine oxide calcination processing is oxygen;
The atmosphere of described nano cupric oxide, nano titanium oxide calcination processing is nitrogen;
The atmosphere of described nano aluminium oxide calcination processing is hydrogen;
(2) by mass, mixed by the nano-powder after 1 part of calcination processing with 5 ~ 30 parts of ultrapure waters, ultrasonic or powerful mechanical stirring 0.5 ~ 12 hour, obtains finely dispersed suspension;
(3) suspension of gained is passed through ion exchange resin, remove charged foreign ion, make the specific conductivity of suspension be less than 5 μ s/cm;
(4) in the suspension of low conductivity, add dispersion agent, stir 1 ~ 24 hour, make dispersion agent evenly be coated on nano grain surface;
(5) nano granule suspension after coated again by ion exchange resin, is removed charged foreign ion, is made the specific conductivity of suspension be less than 1 μ s/cm;
(6) in the suspension of step (5), add ultrapure water or dibasic alcohol, mix the nano-fluid obtaining low conductivity, its specific conductivity is less than 1 μ s/cm.
7. Low-conductivity nanofluid preparation method as claimed in claim 6, is characterized in that: described ion exchange resin is that hydrogen type cation exchange resin mixes with hydroxyl type anion exchange resin the Ion Exchange Resin In The Mixing Bed formed; The mass ratio of hydrogen type cation exchange resin and hydroxyl type anion exchange resin is 1:0.5 ~ 3.
CN201210573980.5A 2012-12-26 2012-12-26 Low-conductivity nanofluid and preparation method thereof Expired - Fee Related CN103045180B (en)

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