CN1094636C - Electric rheopectic liquid containing TiO2 modified by doping rare earth and its preparing process - Google Patents
Electric rheopectic liquid containing TiO2 modified by doping rare earth and its preparing process Download PDFInfo
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- CN1094636C CN1094636C CN 99115944 CN99115944A CN1094636C CN 1094636 C CN1094636 C CN 1094636C CN 99115944 CN99115944 CN 99115944 CN 99115944 A CN99115944 A CN 99115944A CN 1094636 C CN1094636 C CN 1094636C
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Abstract
The present invention introduces electrorheological fluid material and a preparative technique thereof and particularly relates to rare earth doped modification titanium dioxide anhydrous electrorheological fluid material. Compared with the existing material, obtained rare earth modification titanium dioxide of electrorheological fluid discrete state material of the present invention, namely RE-TiO2, is prepared by a sol-gel method at normal temperature; raw material is easily acquired, and components and performance are easy to control; the doping of a trace amount of rare-earth elements can greatly increase the dielectric property and the conductance characteristic of the material, so electrorheological fluid prepared from the material and methyl silicone oil has high mechanical value and favorable temperature effect. An accompanying diagram displays the relation curve of the shearing stress and the direct-current electric field strength of the titanium dioxide electrorheological fluid modified by rare earth at 25 DEG C and at the shearing speed of 1.441S<-1>.
Description
The present invention relates to a kind of electrorheological fluid material and technology of preparing thereof, particularly rareearth doped modified titanium dioxide anhydrous electric rheological liquid material.
Electrorheological fluid is extremely paid attention in recent years as a kind of novel intelligent material.It is the suspension system that is formed in the insulating oil of low-k by the easy polarized dielectric Dispersion of Particles that high-k, low electricity are led.
At present, the performance of electrorheological fluid does not also reach the practicability requirement, about the research of electrorheological discrete state material mainly concentrates on moisture er material and the polymer semiconductor's anhydrous electric rheological material: the former is (as J.E.Stangroom and I.Harness, German Patent, 3310959 (1983)) be that the macromolecular material that will have certain water absorbing capacity is dispersed in the insulating oil and forms.But this material requires under the very wide occasion in variations in temperature, because the icing or vaporization of water can make the performance of material seriously descend; And leakage current is big, to the metal device seriously corroded.The latter makes mostly polymer semiconductor is dispersed in the insulating oil and forms, (as H.Block andJ.P.Kelly, U.K.Patent, 2170510 (1985)), the electrorheological fluid that polymer semiconductor obtains as decentralized photo has better solved the former limitation on serviceability temperature.But this material is under high electric field, and leakage current is big near and have influence on mechanical property, and complicated process of preparation, toxicity is big, cost is high, therefore is difficult to realize commercialization and industrialization.
For addressing these problems, part Study person begins to turn in the research and development of inorganic electrorheological fluid material, and mainly be to utilize oxide or ceramic-like to prepare electrorheological fluid (as Gillites D, et al.U.K.Patent 2219598 (1989)) as decentralized photo and insulating oil.But, there are shortcomings such as the mechanics value is low, resistance to settling is poor, operating temperature range is still narrow partially from the combination property of gained material.
The purpose of this invention is to provide a kind of rare earth modified titanium dioxide anhydrous electric rheological liquid that utilizes.It not only can effectively improve the mechanical property of pure titinium dioxide electrorheological fluid, also has temperature effect preferably; And preparation is simple, and product component and performance are easy to control.
The concrete enforcement of purpose of the present invention is as follows:
Adopt colloidal sol-gel reaction technology.
With the above grade raw material of chemical pure: tetrabutyl titanate (Ti (O-Bu)
4) make the chloride monohydrate (RECl that matrix material, absolute ethyl alcohol (EtOH) are made organic solvent, rare earth
37H
2O (RE=La, Ce etc.)) is the speed that dopant, a certain amount of hydrochloric acid are done catalyst and control hydrolysis and polycondensation reaction.
The mole proportioning of reactant: Ti (O-Bu)
4: EtOH: H
2O: HCl=1: 18～20: 0.625: 0.1～0.2, take by weighing RECl by RE/Ti=0～0.2 mol ratio
37H
2O.
At first, with Ti (O-Bu)
4Mix as first component with the anhydrous ethanol solvent of half amount; With a certain amount of secondary deionized water, hydrochloric acid with RECl
37H
2O dissolves and mixes as second component with second half amount absolute ethyl alcohol.Then, under room temperature and the vigorous stirring second component slowly is being added drop-wise to dropper among first component, dropwising that the back continues to stir 5～10 minutes, and forming the crocus clear solution so that reactant mixes more evenly; Then this clear solution being put into fume hood leaves standstill 12～48 hours (gel time will be subjected to amount of water, hydrochloric acid content and RECl
37H
2O measures influence), allow its gelling.After treating that gel forms, put it into 80 ℃ of vacuum drying chamber inner dryings 7～8 hours, taking off organic solvent and water, and the xerogel blocky-shaped particle that obtains loosening.With mortar it is ground into fine powder, changes crucible over to and put into chamber type electric resistance furnace, handled continuously 4 hours, treat that furnace temperature drops to 100 ℃ and takes out powders and put into drier, promptly obtained the yellow cerium titanium dioxide composite powder of mixing by 400 ℃/2h+500 ℃/2h.At last, with mixing by particle/silicone oil volume ratio 35% with the methyl-silicone oil of smoking through 150 ℃/2h after 150 ℃/4h of this particle drying, promptly obtain the doped with rare-earth elements electric titania rheological liquid.
The present invention only can effectively improve the dielectric property and the conductance property of titanium dioxide by the doping trace rare-earth element, cause the raising of gained electrorheological fluid mechanics value and the significantly improvement of temperature effect, and preparation is simple, cost is lower; Simultaneously, because the traditional sol gel reaction of employing, so preparation manipulation is not had specific (special) requirements, reaction can be carried out at low temperatures, and the doping of trace element and even distribution the thereof are more easily realized, and be easier of product component and performance enforcement control.
The performance of implementation procedure of the present invention and material is by following examples and description of drawings.Embodiment one: (pure TiO
2Electrorheological fluid)
With 15ml Ti (O-Bu)
4(density is about 1.0g/cm
3) join in the 20ml absolute ethyl alcohol, and constantly stirring makes it to mix as first component; A certain amount of hydrochloric acid and 0.5ml secondary deionized water mixed to join in addition partly measure in the 20ml absolute ethyl alcohol as second component.Under room temperature and the vigorous stirring second component slowly being added drop-wise to dropper among first component, adjust pH value=3～4.After waiting to dropwise, continue to stir 5～10 minutes, reactant is mixed, and put into fume hood and leave standstill hour, allow its gelling.After treating that gel forms, put into the dry 80 ℃/8h of baking oven, the dry gel particle that obtains loosening is put into crucible with mortar after with its porphyrize and is changed chamber type electric resistance furnace over to, by 400 ℃/2h+500 ℃/2h heat treatment 4 hours, treating furnace temperature to drop to 100 ℃ of taking-ups, to put into drier stand-by.The pure titinium dioxide powder that obtains white mixed by the volume ratio 35% of particle/silicone oil promptly obtain electric titania rheological liquid.The relation of measuring its shear stress and electric field strength as shown in Figure 1.
(25 ℃, shear rate is 1.441S to the relation curve of Fig. 1 rare earth modified back electric titania rheological liquid shear stress and electric field strength (direct current)
-1)
Embodiment two:
With 15ml Ti (O-Bu)
4Join in the 20ml absolute ethyl alcohol, and constantly stirring makes it to mix as first component; With a certain amount of hydrochloric acid, 0.5ml secondary deionized water, CeCl
37H
2O 1.095 grams mix to join in addition partly to be measured in the 20ml absolute ethyl alcohol as second component.Under room temperature and the vigorous stirring second component slowly being added drop-wise to dropper among first component, adjust pH value=3～4.After waiting to dropwise, continue to stir 5～10 minutes, reactant is mixed, and put into fume hood and leave standstill hour, allow its gelling.After treating that gel forms, put into the dry 80 ℃/8h of baking oven, the dry gel particle that obtains loosening is put into crucible with mortar after with its porphyrize and is changed chamber type electric resistance furnace over to, by 400 ℃/2h+500 ℃/2h heat treatment 4 hours, treating furnace temperature to drop to 100 ℃ of taking-ups, to put into drier stand-by.Make and mix cerium titanium dioxide granule material, and be mixed with electrorheological fluid by above-mentioned particle/silicone oil volume ratio 35%.The relation of measuring its shear stress and electric field strength as shown in Figure 1, the relation of current density and electric field strength as shown in Figure 2, the relation of shear strength and shear rate as shown in Figure 3, the relation of apparent viscosity and shear rate as shown in Figure 4, its temperature effect is by shown in Figure 5.
(25 ℃, shear rate is 1.441S to the relation curve of Fig. 1 rare earth modified back electric titania rheological liquid shear stress and electric field strength (direct current)
-1)
The relation curve of a kind of modifying titanium dioxide of Fig. 2 (RE/Ti=0.085) electrorheological fluid current density and electric field strength (direct current) (25 ℃)
The relation (25 ℃) of the shear strength of titanium dioxide (RE/Ti=0.085) electrorheological fluid and shear rate after a kind of modification of Fig. 3
The relation curve of titanium dioxide (RE/Ti=0.085) electrorheological fluid apparent viscosity and shear rate (25 ℃) after a kind of modification of Fig. 4
Fig. 5 not same electric field next plant the shear strength of modifying titanium dioxide (RE/Ti=0.07) electrorheological fluid and the relation curve of temperature (direct current, shear rate be 1.441S
-1)
Embodiment three:
Press the preparation process of embodiment two, CeCl is mixed in preparation3·7H
2O 0.902 gram mix cerium titanium dioxide Granular materials, and be mixed with ER fluid by above-mentioned particle/silicone oil volume ratio 35%. Measure its shear stress with The relation of electric-field intensity as shown in Figure 1.
(25 ℃, shear rate is 1.441S to the relation curve of the rare earth modified rear electric titania rheological liquid shear stress of Fig. 1 and electric-field intensity (direct current)-1)
Embodiment four:
Press the preparation process of embodiment two, CeCl is mixed in preparation3·7H
2O 2.575 gram mix cerium titanium dioxide Granular materials, and be mixed with ER fluid by above-mentioned particle/silicone oil volume ratio 35%. Measure its shear stress with The relation of electric-field intensity as shown in Figure 1.
(25 ℃, shear rate is 1.441S to the relation curve of Fig. 1 rare earth modified back electric titania rheological liquid shear stress and electric field strength (direct current)
-1)
Embodiment five:
Press the preparation process of embodiment two, utilize LaCl
37H
2Lanthanum titanium dioxide granule material is mixed in the O preparation, and is mixed with electrorheological fluid by above-mentioned particle/silicone oil volume ratio 35%.
Claims (5)
1, the electric rheopectic liquid containing TiO 2 modified material of a kind of doped with rare-earth elements, the decentralized photo of this material are doped with rare-earth elements modifying titanium dioxide dielectric particle material, and the continuous phase base fluid is a methyl-silicone oil.
2, the electric rheopectic liquid containing TiO 2 modified material of doped with rare-earth elements according to claim 1 is characterized in the dispersion particle titanium dioxide as base matter, and rare earth element is as modifier, i.e. RE-TiO
2, wherein RE is rare earth elements such as La, Ce.
3, the electric rheopectic liquid containing TiO 2 modified material of doped with rare-earth elements according to claim 1 is characterized in that: RE/Ti=0 in the dispersion particle material～0.2 (mol ratio).
4, the electric rheopectic liquid containing TiO 2 modified material of doped with rare-earth elements according to claim 1, the volume ratio that it is characterized in that dispersion particle material and methyl-silicone oil is 35%.
5, the preparation method of a kind of doped with rare-earth elements modifying titanium dioxide er material as claimed in claim 1 is characterized in that the preparation method may further comprise the steps:
1. select tetrabutyl titanate (Ti (O-Bu) for use
4), the rare earth chloride monohydrate is (as CeCl
37H
2O), secondary deionized water is made reaction raw materials.Absolute ethyl alcohol is made organic solvent.Hydrochloric acid is made the pH value conditioning agent;
2. by (Ti (O-Bu)
4): Et (OH): H
2O: RECl
37H
2O: HCl=1: 18～20: 0.625: 0.1～0.2 (mol ratio) batching;
3. tetrabutyl titanate and ethanol are mixed composition first component; H
2O, CeCl
37H
2O, hydrochloric acid and ethanol mix forms second component, under the normal temperature second component is added drop-wise in first component, and constantly stirs, and to form homogeneous transparent solution, the control pH value is 3～5, leaves standstill 12～48h under the normal temperature, treats its gelling;
4. with gel with baking oven 80 ℃ of drying 7～8h, obtain xerogel, be ground into certain fineness with mortar, change in the chamber type electric resistance furnace, by 400 ℃/2h+500 ℃/2h heat treatment 4 hours, obtain white or yellow doped with rare-earth elements modifying titanium dioxide subparticle;
5. particle and methyl-silicone oil 35% are mixed by volume, it is electric rheopectic liquid containing TiO 2 modified promptly to have made doped with rare-earth elements.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99115944 CN1094636C (en) | 1999-12-21 | 1999-12-21 | Electric rheopectic liquid containing TiO2 modified by doping rare earth and its preparing process |
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|---|---|---|---|
| CN 99115944 CN1094636C (en) | 1999-12-21 | 1999-12-21 | Electric rheopectic liquid containing TiO2 modified by doping rare earth and its preparing process |
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|---|---|
| CN1301027A CN1301027A (en) | 2001-06-27 |
| CN1094636C true CN1094636C (en) | 2002-11-20 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358618C (en) * | 2004-11-03 | 2008-01-02 | 西北工业大学 | Method for preparing nano-titanium oxide/amide derivative electrorheological fluid |
| CN100393857C (en) * | 2005-10-28 | 2008-06-11 | 重庆大学 | Anhydrous electric rheological liquid and preparing process thereof |
| CN100413570C (en) * | 2004-11-03 | 2008-08-27 | 西北工业大学 | Method for preparing nano-titanium oxide electroheological fluid by combination of carbamide and formamide |
| CN100448962C (en) * | 2003-10-13 | 2009-01-07 | 西北工业大学 | Transition metal ion doped titanium dioxide electrorheological materials |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1769403B (en) * | 2004-11-03 | 2010-12-08 | 西北工业大学 | Acetamide modified nanometer titanium oxide electrorheological fluid |
| CN102108315A (en) * | 2009-12-23 | 2011-06-29 | 西北工业大学 | Multinuclear rare earth doped titanium oxide/hierarchical porous carbon electrorheological fluid material |
| CN114075068B (en) * | 2020-08-21 | 2023-01-13 | 大莲电瓷（福建）有限公司 | Preparation process of alumina electric porcelain |
| CN115160932B (en) * | 2022-06-12 | 2023-07-14 | 西北工业大学深圳研究院 | Composite oxide electrorheological fluid, preparation method and polishing method |
-
1999
- 1999-12-21 CN CN 99115944 patent/CN1094636C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100448962C (en) * | 2003-10-13 | 2009-01-07 | 西北工业大学 | Transition metal ion doped titanium dioxide electrorheological materials |
| CN100358618C (en) * | 2004-11-03 | 2008-01-02 | 西北工业大学 | Method for preparing nano-titanium oxide/amide derivative electrorheological fluid |
| CN100413570C (en) * | 2004-11-03 | 2008-08-27 | 西北工业大学 | Method for preparing nano-titanium oxide electroheological fluid by combination of carbamide and formamide |
| CN100393857C (en) * | 2005-10-28 | 2008-06-11 | 重庆大学 | Anhydrous electric rheological liquid and preparing process thereof |
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|---|---|
| CN1301027A (en) | 2001-06-27 |
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