CN1768914A - Method for preparing nano-titanium oxide electroheological fluid by combination of carbamide and formamide - Google Patents
Method for preparing nano-titanium oxide electroheological fluid by combination of carbamide and formamide Download PDFInfo
- Publication number
- CN1768914A CN1768914A CN 200410073225 CN200410073225A CN1768914A CN 1768914 A CN1768914 A CN 1768914A CN 200410073225 CN200410073225 CN 200410073225 CN 200410073225 A CN200410073225 A CN 200410073225A CN 1768914 A CN1768914 A CN 1768914A
- Authority
- CN
- China
- Prior art keywords
- formamide
- urea
- fluid
- solution
- obtains
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Lubricants (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for preparing nanometer composite titanium oxide current-change liquid with high current-change effect, which is characterized in that: via the hydrolyzation of alcoholic solution of butyl titanate and formamide in the water solution of carbamide at the condition of ice water bath, attaining the nanometer butyl titanate particle of carbamide/formamide; than milling said nanometer particles and silicon methyl oil to attain the current-change liquid, whose yield stress can reach 70kPa at the direct current electric field of 4kV/mm. compared with traditional micron particle current-change liquid and pure butyl titanate current-change liquid, its has significantly improved property as figure. The invention has the characters as better anti-deposition, simple design, easy operation and lower cost.
Description
Technical field the present invention relates to the preparation method that a kind of high-performance current becomes liquid, particularly is compounded with the preparation method of the nanometer titanium oxide electrorheological fluid of urea/formamide polar molecule.
The background technology ER fluid has crucial application prospect as a kind of new intelligent soft material.It normally is scattered in the insulating oil of low-k and the suspension system that forms by the solid particle of high-k, low conductivity.This system can realize liquid-solid transformation in moment under effect of electric field, and this transformation behavior has advantages such as quick, reversible, adjustable, so there is important use to be worth on automation, shock absorber, clutch, damper, stepless speed-regulating device and optics and printing equipment.Traditional micron particles ER fluid has the operation temperature area of broad, and leakage current density is little, and energy consumption is little etc., but exist also that the mechanics value is not high, resistance to settling is poor, problems such as complicated process of preparation or cost height, still hindered it and be extensive use of.The nanometer ER fluid material has fundamentally overcome above-mentioned shortcoming, its the most outstanding advantage is that yield value of stress is significantly improved, substantially exceeded the micron particles ER fluid, simultaneously, resistance to settling can also increase, as opening the surfactant composite titanic acid strontium ER fluid that waits invention, the compound barium titanyl oxalate ER fluid of urea of report such as Wen.Yet we find these with the compound ER fluid of normal temperature solid polar molecule when the high-temperature process overlong time, electric current becomes active decline in various degree, this also certainly will influence its extensive use.
Summary of the invention the purpose of this invention is to provide a kind of preparation method of novel nano ER fluid, it is characterized in that urea and liquid formamide that decentralized photo has selected for use normal temperature to be in solid carry out composite modified to nano-titanium oxide, here formamide and urea are strong polar organic matter, and self can produce effective polarization response to extra electric field; High boiling liquid formamide is difficult for volatilizing as water after high-temperature process simultaneously, thereby still can provide the carrier transport environment, reaches the purpose that the strong interface polarization is provided, and urea then can reduce current density, thereby obtains high stable electric rheological effect.The present invention has adopted simple wet-chemical to prepare technology in addition; adopt 0～5 ℃ of ice-water bath that the reactant tetrabutyl titanate is protected in the preparation process; suppress its hydrolysis, can control the titan oxide particles particle diameter effectively, obviously reduce than the particle diameter of traditional preparation method's products therefrom.
Description of drawings
Fig. 1 (a) is the relation curve of the static yield strength and the electric-field intensity of the ER fluid of gained among the embodiment one to four, (b) is corresponding current density curve;
Fig. 2 (a) is the relation curve of the static yield strength and the electric-field intensity of the ER fluid of gained among the embodiment five to eight, (b) is corresponding current density curve.
The object of the present invention is achieved like this for the specific embodiment:
(1) takes by weighing 5 milliliters of chemical pure tetrabutyl titanates, the ethanolic solution that under stirring condition, adds 150 milliliters of ethanol preparation tetrabutyl titanates, the ice-water bath reduction environment temperature that is between 0～5 ℃ with temperature when stirring obtain solution is protected, remain on the unlikely hydrolysis change of tetrabutyl titanate muddiness in the dropping process, influence particle size;
(2) the pure formamide of given quantitative analysis is added in the above-mentioned tetrabutyl titanate solution of having prepared, stir and make it even mixing;
(3) the pure urea of given quantitative analysis is dissolved in 800 ml distilled waters, is mixed with solution;
(4) under 0～5 ℃ of ice-water bath and stirring condition, the alcoholic solution of the tetrabutyl titanate/formamide of acquisition in the step (2) dropwise is added drop-wise in the aqueous solution of being prepared in the step (3) that contains urea, continued stirring 20 hours so that react completely again after dropwising, and the ageing of spending the night obtains milky sol solutions;
(5) the milky sol solutions that the reaction that obtains in the step (4) is obtained obtains filter cake after suction filtration, washing and ethanol washing, and filter cake places vacuum drying chamber to take out after 6 hours 120 ℃ of vacuum drying;
(6) the compound nano-titanium oxide (powder) of the urea/formamide of the drying that obtains of step (5) and methyl-silicone oil are to mix at 3: 1 according to particle/silicone oil mass ratio, and grind with agate mortar and to make ER fluid after 6 hours, this ER fluid after smoking 12 hours under 120 ℃ of infrared lamps, is measured its rheologic behavio(u)r with NXS-11 plate plate viscosimeter again.
So that relatively, when not adding formamide in advance in the above-mentioned steps (2), just can make the compound nanometer titanium oxide electrorheological fluid of simple urea; When not adding formamide and urea simultaneously in above-mentioned steps (2) and (3), just can make simple nanometer titanium oxide electrorheological fluid.
Implementation procedure of the present invention and material property are described in detail by following examples:
Embodiment one:
Take by weighing 5 milliliters of chemical pure tetrabutyl titanates, the ethanolic solution that under stirring condition, adds 150 milliliters of ethanol preparation tetrabutyl titanates, the ice-water bath reduction environment temperature that is between 0～5 ℃ with temperature when stirring obtain solution is protected, remain on the unlikely hydrolysis change of tetrabutyl titanate muddiness in the dropping process, influence particle size; Analyze pure formamide with 1.5 milliliters and add in the above-mentioned tetrabutyl titanate solution of having prepared, stir and make it even mixing; 5 grams are analyzed pure urea be dissolved in 800 ml distilled waters, be mixed with solution; Under 0～5 ℃ of ice-water bath and stirring condition, the alcoholic solution of tetrabutyl titanate/formamide dropwise is added drop-wise in the aqueous solution of being prepared that contains urea, continued stirring 20 hours so that react completely again after dropwising, and the ageing of spending the night obtains milky sol solutions; Will this sol solutions suction filtration, washing and ethanol washing back obtain filter cake, filter cake places the compound nano-titanium oxide (powder) of urea/formamide of the drying that vacuum drying chamber obtains after 6 hours 120 ℃ of vacuum drying; Is to mix at 2: 1 this powder and methyl-silicone oil according to particle/silicone oil mass ratio, and grinds with agate mortar and to make ER fluid after 6 hours, is named as LB-ERF.This ER fluid after smoking 12 hours under 120 ℃ of infrared lamps, is measured its rheologic behavio(u)r with NXS-11 plate plate viscosimeter again.The static yield strength of this ER fluid and the relation curve of electric-field intensity and corresponding current density curve are as shown in Figure 1.
Embodiment two
Take by weighing 5 milliliters of chemical pure tetrabutyl titanates, the ethanolic solution that under stirring condition, adds 150 milliliters of ethanol preparation tetrabutyl titanates, the ice-water bath reduction environment temperature that is between 0～5 ℃ with temperature when stirring obtain solution is protected, remain on the unlikely hydrolysis change of tetrabutyl titanate muddiness in the dropping process, influence particle size; Analyze pure formamide with 4 milliliters and add in the above-mentioned tetrabutyl titanate solution of having prepared, stir and make it even mixing; 5 grams are analyzed pure urea be dissolved in 800 ml distilled waters, be mixed with solution; Under 0～5 ℃ of ice-water bath and stirring condition, the alcoholic solution of tetrabutyl titanate/formamide dropwise is added drop-wise in the aqueous solution of being prepared that contains urea, continued stirring 20 hours so that react completely again after dropwising, and the ageing of spending the night obtains milky sol solutions; Will this sol solutions suction filtration, washing and ethanol washing back obtain filter cake, filter cake places the compound nano-titanium oxide (powder) of urea/formamide of the drying that vacuum drying chamber obtains after 6 hours 120 ℃ of vacuum drying; Is to mix at 2: 1 this powder and methyl-silicone oil according to particle/silicone oil mass ratio, and grinds with agate mortar and to make ER fluid after 6 hours, is named as MB-ERF.This ER fluid after smoking 12 hours under 120 ℃ of infrared lamps, is measured its rheologic behavio(u)r with NXS-11 plate plate viscosimeter again.The static yield strength of this ER fluid and the relation curve of electric-field intensity and corresponding current density curve are as shown in Figure 1.
Embodiment three:
Take by weighing 5 milliliters of chemical pure tetrabutyl titanates, the ethanolic solution that under stirring condition, adds 150 milliliters of ethanol preparation tetrabutyl titanates, the ice-water bath reduction environment temperature that is between 0～5 ℃ with temperature when stirring obtain solution is protected, remain on the unlikely hydrolysis change of tetrabutyl titanate muddiness in the dropping process, influence particle size; 5 grams are analyzed pure urea be dissolved in 800 ml distilled waters, be mixed with solution; Under 0～5 ℃ of ice-water bath and stirring condition, the alcoholic solution of tetrabutyl titanate/formamide dropwise is added drop-wise in the aqueous solution of being prepared that contains urea, continued stirring 20 hours so that react completely again after dropwising, and the ageing of spending the night obtains milky sol solutions; Will this sol solutions suction filtration, washing and ethanol washing back obtain filter cake, filter cake places the compound nano-titanium oxide (powder) of pure urea of the drying that vacuum drying chamber obtains after 6 hours 120 ℃ of vacuum drying; Is to mix at 2: 1 this powder and methyl-silicone oil according to particle/silicone oil mass ratio, and grinds with agate mortar and to make ER fluid after 6 hours, is named as UB-ERF.This ER fluid after smoking 12 hours under 120 ℃ of infrared lamps, is measured its rheologic behavio(u)r with NXS-11 plate plate viscosimeter again.The static yield strength of this ER fluid and the relation curve of electric-field intensity and corresponding current density curve are as shown in Figure 1.
Embodiment four:
Take by weighing 5 milliliters of chemical pure tetrabutyl titanates, the ethanolic solution that under stirring condition, adds 150 milliliters of ethanol preparation tetrabutyl titanates, the ice-water bath reduction environment temperature that is between 0～5 ℃ with temperature when stirring obtain solution is protected, remain on the unlikely hydrolysis change of tetrabutyl titanate muddiness in the dropping process, influence particle size; Under 0～5 ℃ of ice-water bath and stirring condition, the alcoholic solution of tetrabutyl titanate dropwise is added drop-wise in the aqueous solution, continue again after dropwising to stir 20 hours so that react completely, and the ageing of spending the night obtains milky sol solutions; Will this sol solutions suction filtration, washing and ethanol washing back obtain filter cake, filter cake places the pure nano-titanium oxide (powder) of the drying that vacuum drying chamber obtains after 6 hours 120 ℃ of vacuum drying; Is to mix at 2: 1 this powder and methyl-silicone oil according to particle/silicone oil mass ratio, and grinds with agate mortar and to make ER fluid after 6 hours, is named as PB-ERF.This ER fluid after smoking 12 hours under 120 ℃ of infrared lamps, is measured its rheologic behavio(u)r with NXS-11 plate plate viscosimeter again.The static yield strength of this ER fluid and the relation curve of electric-field intensity and corresponding current density curve are as shown in Figure 1.
Embodiment five
The ER fluid of ER fluid gained after smoking 24 hours again under 120 ℃ of infrared lamps of embodiment one gained is named as LA-ERF.The static yield strength of this ER fluid and the relation curve of electric-field intensity and corresponding current density curve are as shown in Figure 2.
Embodiment six
The ER fluid of ER fluid gained after smoking 24 hours again under 120 ℃ of infrared lamps of embodiment two gained is named as MA-ERF.The static yield strength of this ER fluid and the relation curve of electric-field intensity and corresponding current density curve are as shown in Figure 2.
Embodiment seven
The ER fluid of ER fluid gained after smoking 24 hours again under 120 ℃ of infrared lamps of embodiment three gained is named as UA-ERF.The static yield strength of this ER fluid and the relation curve of electric-field intensity and corresponding current density curve are as shown in Figure 2.
Embodiment eight
The ER fluid of ER fluid gained after smoking 24 hours again under 120 ℃ of infrared lamps of embodiment four gained is named as PA-ERF.The static yield strength of this ER fluid and the relation curve of electric-field intensity and corresponding current density curve are as shown in Figure 2.
Claims (4)
1. the preparation method of urea/formamide composite Nano titanium oxide electrorheological fluid, it is characterized in that: hydrolysis obtains to be compounded with the TiOx nano particle of urea/formamide in the aqueous solution that is containing urea under the ice-water bath condition by the alcoholic solution that contains tetrabutyl titanate and formamide, and then common grinding of this nano particle and methyl-silicone oil obtains ER fluid.
2. the preparation method of a kind of urea as claimed in claim 1/formamide composite Nano titanium oxide electrorheological fluid is characterized in that this method may further comprise the steps:
(1) takes by weighing 5 milliliters of chemical pure tetrabutyl titanates, the ethanolic solution that under stirring condition, adds 150 milliliters of ethanol preparation tetrabutyl titanates, the ice-water bath reduction environment temperature that is between 0～5 ℃ with temperature when stirring obtain solution is protected, remain on the unlikely hydrolysis change of tetrabutyl titanate muddiness in the dropping process, influence particle size;
(2) the pure formamide of given quantitative analysis is added in the above-mentioned tetrabutyl titanate solution of having prepared, stir and make it even mixing;
(3) the pure urea of given quantitative analysis is dissolved in 800 ml distilled waters, is mixed with the aqueous solution that contains urea;
(4) under 0～5 ℃ of ice-water bath and stirring condition, the alcoholic solution of the tetrabutyl titanate/formamide of acquisition in the step (2) dropwise is added drop-wise in the aqueous solution of being prepared in the step (3) that contains urea, continued stirring 20 hours so that react completely again after dropwising, the ageing of spending the night obtains milky sol solutions;
(5) the milky sol solutions that the reaction that obtains in the step (4) is obtained obtains filter cake after suction filtration, washing and ethanol washing, and filter cake places vacuum drying chamber to take out after 6 hours 120 ℃ of vacuum drying;
(6) the compound nano-titanium oxide (powder) of the urea/formamide of the drying that obtains of step (5) and methyl-silicone oil are to mix at 2: 1 according to particle/silicone oil mass ratio, and grind with agate mortar and to make ER fluid after 6 hours, this ER fluid is measured its rheologic behavio(u)r with NXS-11 plate plate viscosimeter after smoking 12 hours under 120 ℃ of infrared lamps.
3. method as claimed in claim 2 is characterized in that: the amount of used formamide is between 1.0 milliliters and 5.0 milliliters in the step (2).
4. method as claimed in claim 2 is characterized in that: the amount of used urea is 5 grams in the step (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100732256A CN100413570C (en) | 2004-11-03 | 2004-11-03 | Method for preparing nano-titanium oxide electroheological fluid by combination of carbamide and formamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100732256A CN100413570C (en) | 2004-11-03 | 2004-11-03 | Method for preparing nano-titanium oxide electroheological fluid by combination of carbamide and formamide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1768914A true CN1768914A (en) | 2006-05-10 |
| CN100413570C CN100413570C (en) | 2008-08-27 |
Family
ID=36750603
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100732256A Expired - Fee Related CN100413570C (en) | 2004-11-03 | 2004-11-03 | Method for preparing nano-titanium oxide electroheological fluid by combination of carbamide and formamide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100413570C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100412177C (en) * | 2006-09-01 | 2008-08-20 | 中国科学院物理研究所 | Blended titanium dioxide electric rheological liquid and its preparing method |
| JP2009540067A (en) * | 2006-06-15 | 2009-11-19 | 中國科學院物理研究所 | Polar molecular-type electrorheological fluid |
| CN101486948B (en) * | 2008-12-31 | 2012-05-02 | 中国科学院宁波材料技术与工程研究所 | Titanium dioxide electrorheological liquid having heavy electrorheological effect under low field |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05194973A (en) * | 1992-01-22 | 1993-08-03 | Toyohisa Fujita | Electric-field-responsive fluid |
| CN1094636C (en) * | 1999-12-21 | 2002-11-20 | 西北工业大学 | Electric rheopectic liquid containing TiO2 modified by doping rare earth and its preparing process |
-
2004
- 2004-11-03 CN CNB2004100732256A patent/CN100413570C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009540067A (en) * | 2006-06-15 | 2009-11-19 | 中國科學院物理研究所 | Polar molecular-type electrorheological fluid |
| CN100412177C (en) * | 2006-09-01 | 2008-08-20 | 中国科学院物理研究所 | Blended titanium dioxide electric rheological liquid and its preparing method |
| CN101486948B (en) * | 2008-12-31 | 2012-05-02 | 中国科学院宁波材料技术与工程研究所 | Titanium dioxide electrorheological liquid having heavy electrorheological effect under low field |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100413570C (en) | 2008-08-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102513079B (en) | Controllable crystalline form titanium dioxide and graphite alkene composite material with high efficient photoelectricity activity and preparation method thereof | |
| CN101693196B (en) | Preparation method of silver/titanium dioxide compound | |
| CN101089164B (en) | Polar molecule type electric rheologic liquid | |
| CN1872787A (en) | Method for preparing Nano composite material of stannic oxide / titanium dioxide | |
| CN1240287C (en) | Attapulgite-argentum nanometer composite antibiotic material and preparation method thereof | |
| CN105665737A (en) | Biosynthesis method of nano Ag | |
| CN101469286B (en) | Polyaniline intercalated titanium oxide nano-tube ER fluid | |
| CN1768914A (en) | Method for preparing nano-titanium oxide electroheological fluid by combination of carbamide and formamide | |
| CN101768503B (en) | Titanium oxyoxalate electrorheological fluid and preparation method thereof | |
| CN101066776A (en) | Zinc oxide synthesizing process | |
| CN1622283A (en) | Method for preparing composite oxide semiconductor nano material | |
| CN109181815B (en) | Electrorheological fluid and preparation method thereof | |
| CN101575544B (en) | Surface modified titanium-calcium oxyoxalate electrorheological fluid and preparation method thereof | |
| CN100396760C (en) | Intercalation kaolin/modified titanium oxide nano composite particles electrorheological fluid | |
| CN1055111C (en) | Composite strontium titanate electrically rheological liquid and its preparation | |
| CN1094636C (en) | Electric rheopectic liquid containing TiO2 modified by doping rare earth and its preparing process | |
| CN100340488C (en) | Method for preparing high dispersibility antimony doped stannic hydroxide nanometer powder | |
| CN101486948B (en) | Titanium dioxide electrorheological liquid having heavy electrorheological effect under low field | |
| CN1239684C (en) | Current variable fluid material of Nano composite granules between kaoline and oxide of titanium, and preparation method | |
| CN1332003C (en) | Kaolin/TiO2 nanotube composite particle electrorheological fluid materials | |
| CN1539934A (en) | Current variable fluid material of modified Nano composite granules between kaoline and oxide of titanium, and prepration method | |
| CN1607179A (en) | Preparation technology of size controllable incompact superfine alumina powder material | |
| CN100370009C (en) | Calcium titanate electric rheological liquid and preparing process thereof | |
| CN1285714C (en) | Kaolin/dimethyl sulphoxide/carboxymethyl starch ternary system nanotube composite electrorheological fluid materials | |
| CN102617044B (en) | Method for preparing vertical orientation anatase titanium oxide film by using hydrothermal method and gas sensor thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |