CN102718500A - Method for preparing rare earth modified graphene ceramic composite film on glass substrate - Google Patents
Method for preparing rare earth modified graphene ceramic composite film on glass substrate Download PDFInfo
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Abstract
The invention relates to a method for preparing a rare earth modified graphene ceramic composite film on a glass substrate. The method includes: (1) subjecting the surface of the glass substrate to hydroxylation pretreatment to obtain a treated glass substrate; (2) preparing rare earth sol solution and placing graphene into the obtained rare earth sol solution for treatment for 4-10h to obtain rare earth modified graphene sol; (3) immersing the treated glass substrate into the rare earth modified graphene sol, standing, upwardly lifting the glass substrate out of the sol, and drying; and (4) preserving the glass substrate obtained at the step (3) at 80-120 DEG C for 30-90min, heating to 600-800 DEG C, preserving heat for 1-5h and naturally cooling to the room temperature. The method is simple in preparation process, low in cost, free of environment pollution and fine in film forming. The composite ceramic film prepared by the method is uniform and compact and has excellent characteristics of friction reduction and abrasion resistance.
Description
Technical field
The invention belongs to the preparation field of Ceramic Composite film, particularly a kind of method that on glass substrate, prepares the grapheme modified Ceramic Composite film of rare earth.
Background technology
MEMS (MEMS) is meant the transmitter that integrates microstructure, miniature performer and signal processing and pilot circuit, forms to have intelligent micro device or the microsystem that function was obtained, handles and carried out to information simultaneously.The finish size of total system is the micron number magnitude, and the manufactured materials multiselect is with monocrystalline or polysilicon.Micromachine has that volume is little, light weight, energy consumption is low, integrated level is high and characteristics such as intelligent degree height; Have broad application prospects in biomedicine, aerospace, military affairs and industrial or agricultural each side, and receive the great attention of countries in the world scientific circles, industrial community and government department.In recent years, the tribology research of relevant composite ceramic film has become one of advanced subject of tribological field, and the ceramic membrane material has characteristics such as the high and chemicalstability of hardness is good, is expected under severe rugged environment, to use as the tribology parts.Graphene is that the monolayer carbon atom is closely arranged and a kind of carbonaceous novel material of formation, has individual layer bi-dimensional cellular shape crystalline network.Because its special microtexture, Graphene shows the physical properties of many uniquenesses.Its Young's modulus is up to 1TPa, and breaking tenacity is the highest material of intensity known today up to 130GPa.Its heat-conduction coefficient is about 2000-5000W/mK, is the excellence conductor of heat.Therefore, Graphene has fabulous mechanics, heat conductance and electric property, in fields such as microelectronics, the energy, novel material and biological medicines the major application prospect is arranged.Graphene has superpower wear resistance and self lubricity, and this has great importance for the micro-system Tribological Study.Obtained considerable progress about silicon materials surface-treated and microcosmic mechanical property thereof and Study on Friction and Wear, relevant with it material has broad application prospects in MEMS with technology.Yet, also reach perfection far away with relevant understanding with the research of lubricated essence to the wearing and tearing of the Micro Lub of MEMS, still await going deep into about the research of silicon materials process for modifying surface and modified layer Micro Lub performance; Understanding to inner link between modified layer microtexture and its micromechanics and the tribological property still awaits in-depth; The research of relevant micro-nanoization of silicon face be should strengthen emphatically from now on, thereby the application and the development need of high-tech sectors such as MEMS satisfied.
Application number is that 03114751.8 Chinese patent discloses a kind of titanium dioxide nano-film and method for making thereof that contains rare earth and silicon-dioxide.Adopt this kind prescription to make the titanium deoxid film that contains REE and silicon-dioxide, can improve the wetting ability and the photocatalytic of titanium deoxid film,, be not suitable for the purposes of antifriction than being more suitable for catalyzer.
It is a kind of with sol-gel technology preparing alumina-ceramic membrane method that application number is that 94112148.8 Chinese patent discloses, though the film of this method system has good gas permeability, do not relate to for the antifriction performance of film.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method that on glass substrate, prepares the grapheme modified Ceramic Composite film of rare earth; This method technology is simple; Cost is low, efficient is high; Can on hydroxylated glass substrate, make one or more layers ceramic thin sheet, this ceramic thin sheet has even, fine and close characteristics, has good antifriction and wear-resistant characteristics.
A kind of method that on glass substrate, prepares the grapheme modified Ceramic Composite film of rare earth of the present invention comprises:
(1) the hydroxylation pre-treatment is carried out on the surface of glass substrate, the glass substrate after obtaining handling;
(2) titanate is dissolved in the ethanol, adds diethylolamine, mix under the room temperature, add aqueous ethanolic solution again, behind 15～25 ℃ of hydrolysis 1～3h, add rare earth compound, stir, add N again, the N'-N obtains rare-earth sol solution; Place the rare-earth sol solution of gained to handle 4-10h Graphene, obtain containing the Graphene colloidal sol of rare earth modified;
(3) glass substrate after the above-mentioned processing is immersed in the above-mentioned Graphene colloidal sol that contains the rare earth modified, leave standstill, glass substrate is upwards lifted out colloidal sol, in moisture eliminator after the drying, oven dry;
(4) glass substrate with step (3) gained is incubated 30～90min at 80～120 ℃; Speed with 1～5 ℃/min is warming up to 600～800 ℃; Behind insulation 1～5h, naturally cool to room temperature, on glass substrate, form the grapheme modified Ceramic Composite film of doped with rare-earth elements.
The pretreated concrete steps of the described hydroxylation of step (1) are: glass substrate is immersed in the Pirahan solution, at room temperature left standstill 10～60 minutes, after deionized water drip washing, place inherent 100～120 ℃ of drying 0.5～1h of a dust keeper.The glass substrate hydroxylation that deals is very complete and substrate of glass is very smooth, is not corroded.
Described Pirahan solution is 98% the H of 70:30 by volume ratio
2SO
4Solution and 30% H
2O
2Solution composition.
Titanate is dissolved in the mol ratio of ethanol and titanate is 2～6:1 in the ethanol described in the step (2).
The mol ratio of diethylolamine described in the step (2) and titanate is 0.2～5:1.
Aqueous ethanolic solution described in the step (2) is that the water and the absolute ethyl alcohol of 1:8.5～9.5 is formulated by volume ratio, and the water in the aqueous ethanolic solution and the mol ratio of titanate are 1～2:1.
Rare earth compound described in the step (2) is Lanthanum trichloride, Cerium II Chloride, Lanthanum trinitrate or cerous nitrate.
The mol ratio of rare earth compound described in the step (2) and titanate is 2～5:10.
N described in the step (2), the N'-N accounts for 0.2～1% of rare-earth sol overall solution volume.
The concentration of Graphene in rare-earth sol solution described in the step (2) is 0.5-5mg/ml.
Behind the completing steps (3), repetitive operation step (3) 1-5 time is carried out step (4) again, on glass substrate, to form the grapheme modified Ceramic Composite film of multi-layer doping REE.
The present invention be employed in sol-gel method on hydroxylated glass substrate, obtain densification, evenly, the grapheme modified Ceramic Composite film of doped with rare-earth elements of surface smoothing; Because the grapheme modified existence of REE is arranged; Can improve mechanical properties in films and tribological properties, improve the antifriction quality of film.
Beneficial effect:
(1) preparation technology of the present invention is simple, and cost is low, environmentally safe, good film-forming property;
(2) ceramic thin sheet that obtains of the present invention is even, fine and close, has good antifriction and wear-resistant characteristic.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
The grapheme modified Ceramic Composite film of preparation doped with rare-earth elements on glass substrate, concrete steps are:
(1) the hydroxylation pre-treatment is carried out on the surface of glass substrate: glass substrate is immersed Pirahan solution, and (by volume ratio is 98% the H of 70:30
2SO
4Solution and 30% H
2O
2Solution constitutes) in, at room temperature left standstill 30 minutes, with a large amount of deionized water drip washing, place with the stainless material preparation, be used for preventing dry 1h in 100 ℃ of baking ovens in dust keeper inherence of contamination by dust sample.The glass substrate hydroxylation that above-mentioned condition deals is very complete and substrate of glass is very smooth, is not corroded.
(2) with the liposoluble of metatitanic acid fourth in ethanol, the mol ratio of ethanol and metatitanic acid fourth fat is 3:1, adds diethylolamine as sequestrant, the mol ratio of diethylolamine and metatitanic acid fourth fat is 1:1, stirring 10h is to mix under the room temperature; In the solution of gained, adding by volume ratio is the water of 1:9 and the aqueous ethanolic solution that absolute ethyl alcohol is mixed with, and the mol ratio of water in the aqueous ethanolic solution and metatitanic acid fourth fat is 2:1, at 20 ℃ of hydrolysis 1h; Add Lanthanum trichloride; The mol ratio of Lanthanum trichloride and metatitanic acid fourth fat is 0.5:10, stirs 1h, adds N; The N'-N obtains containing the colloidal sol of rare earth; N, N'-N are 1% of colloidal sol TV; Add Graphene, leave standstill 8h, the concentration of Graphene in colloidal sol is 1mg/ml.
(3) glass substrate after will handling immerses and contains the grapheme modified colloidal sol of rare earth; Leave standstill 5min; Speed with 3cm/min upwards lifts out colloidal sol with glass substrate; Drying at room temperature is after 30 minutes in moisture eliminator, and oven dry is 2 hours in 100 ℃ baking oven, makes the colloidal sol substantially dry of glass substrate surface;
(4) glass substrate is put into retort furnace,, be warming up to 600 ℃, behind the insulation 3h, in stove, naturally cool to room temperature, on glass substrate, form the grapheme modified Ceramic Composite film of rare earth doped lanthanum with the speed of 2 ℃/min at 100 ℃ of insulation 60min.
The grapheme modified Ceramic Composite film of rare earth doped lanthanum that forms on the glass substrate that aforesaid method is obtained is tested as follows:
Adopt the little frictional behaviour survey meter of the point pure slip of contact MEASUREMENTS OF THIN frictional coefficient.At the grapheme modified Ceramic Composite film of the rare earth doped lanthanum of measuring clean glass substrate respectively on contact pure slip little frictional behaviour survey meter and on glass substrate, form and the silicon nitride ball frictional coefficient when grinding.The grapheme modified ceramic membrane of rare earth of glass substrate surface preparation can be with frictional coefficient 0.6 during from no film be reduced to about 0.1, have fairly obvious antifriction function.
Embodiment 2
The grapheme modified Ceramic Composite film of preparation doped with rare-earth elements on glass substrate, concrete steps are:
(1) the hydroxylation pre-treatment is carried out on the surface of glass substrate: glass substrate is immersed Pirahan solution, and (by volume ratio is 98% the H of 70:30
2SO
4Solution and 30% H
2O
2Solution constitutes) in, at room temperature left standstill 30 minutes, with a large amount of deionized water drip washing, place with the stainless material preparation, be used for preventing dry 1h in 100 ℃ of baking ovens in dust keeper inherence of contamination by dust sample.The glass substrate hydroxylation that above-mentioned condition deals is very complete and substrate of glass is very smooth, is not corroded.
(2) with the liposoluble of metatitanic acid fourth in ethanol, the mol ratio of ethanol and metatitanic acid fourth fat is 6:1, adds diethylolamine as sequestrant, the mol ratio of diethylolamine and metatitanic acid fourth fat is 1:1, stirring 10h is to mix under the room temperature; In the solution of gained, adding by volume ratio is the water of 1:9 and the aqueous ethanolic solution that absolute ethyl alcohol is mixed with, and the mol ratio of water in the aqueous ethanolic solution and metatitanic acid fourth fat is 1:1, at 20 ℃ of hydrolysis 3h; Add Cerium II Chloride; The mol ratio of Cerium II Chloride and metatitanic acid fourth fat is 1:10, stirs 1h, adds N; The N'-N obtains containing the colloidal sol of rare earth; N, N'-N are 2% of colloidal sol TV; Add Graphene, leave standstill 6h, the concentration of Graphene in colloidal sol is 2mg/ml.
(3) glass substrate after will handling immerses and contains the grapheme modified colloidal sol of rare earth; Leave standstill 5min; Speed with 3cm/min upwards lifts out colloidal sol with glass substrate; Drying at room temperature is after 30 minutes in moisture eliminator, and oven dry is 3 hours in 100 ℃ baking oven, makes the colloidal sol substantially dry of glass substrate surface;
(4) glass substrate is put into retort furnace,, be warming up to 700 ℃, behind the insulation 3h, in stove, naturally cool to room temperature, on glass substrate, form the Ceramic Composite film of doped with cerium with the speed of 3 ℃/min at 100 ℃ of insulation 60min.
The grapheme modified Ceramic Composite film of rare earth cerium doping that forms on the glass substrate that aforesaid method is obtained is tested as follows:
Adopt the little frictional behaviour survey meter of the point pure slip of contact MEASUREMENTS OF THIN frictional coefficient.At the grapheme modified Ceramic Composite film of the rare earth cerium doping of measuring clean glass substrate respectively on contact pure slip little frictional behaviour survey meter and on glass substrate, form and the silicon nitride ball frictional coefficient when grinding.The grapheme modified ceramic membrane of rare earth cerium of glass substrate surface preparation can be with frictional coefficient 0.6 during from no film be reduced to about 0.1, have fairly obvious antifriction function.
Embodiment 3
The grapheme modified Ceramic Composite film of preparation doped with rare-earth elements on glass substrate, concrete steps are:
(1) the hydroxylation pre-treatment is carried out on the surface of glass substrate: glass substrate is immersed Pirahan solution, and (by volume ratio is 98% the H of 70:30
2SO
4Solution and 30% H
2O
2Solution constitutes) in, at room temperature left standstill 30 minutes, with a large amount of deionized water drip washing, place with the stainless material preparation, be used for preventing drying (0.5) h in inherent (120) ℃ baking oven of dust keeper of contamination by dust sample.The glass substrate hydroxylation that above-mentioned condition deals is very complete and substrate of glass is very smooth, is not corroded.
(2) with the liposoluble of metatitanic acid fourth in ethanol, the mol ratio of ethanol and metatitanic acid fourth fat is 8:1, adds diethylolamine as sequestrant, the mol ratio of diethylolamine and metatitanic acid fourth fat is 1:1, stirring 10h is to mix under the room temperature; In the solution of gained, adding by volume ratio is the water of 1:9 and the aqueous ethanolic solution that absolute ethyl alcohol is mixed with, and the mol ratio of water in the aqueous ethanolic solution and metatitanic acid fourth fat is 1:1, at 20 ℃ of hydrolysis 1h; Add Lanthanum trinitrate; The mol ratio of Lanthanum trinitrate and metatitanic acid fourth fat is 2:10, stirs 1h, adds N; The N'-N obtains containing the colloidal sol of rare earth; N, N'-N are 1% of colloidal sol TV; Add Graphene, leave standstill 2h, the concentration of Graphene in colloidal sol is 5mg/ml.
(3) glass substrate after will handling immerses and contains the grapheme modified colloidal sol of rare earth; Leave standstill 5min; Speed with 3cm/min upwards lifts out colloidal sol with glass substrate; Drying at room temperature is after 30 minutes in moisture eliminator, and oven dry is 3 hours in 100 ℃ baking oven, makes the colloidal sol substantially dry of glass substrate surface; Repeat aforesaid operations 3 times;
(4) glass substrate is put into retort furnace,, be warming up to 700 ℃, behind the insulation 3h, in stove, naturally cool to room temperature, on glass substrate, form the grapheme modified Ceramic Composite film of rare earth doped lanthanum with the speed of 3 ℃/min at 100 ℃ of insulation 60min.
The grapheme modified Ceramic Composite film of rare earth doped lanthanum that forms on the glass substrate that aforesaid method is obtained is tested as follows:
Adopt the little frictional behaviour survey meter of the point pure slip of contact MEASUREMENTS OF THIN frictional coefficient.The Ceramic Composite film of the Graphene of modifying at the doping lanthanum of measuring clean glass substrate respectively on contact pure slip little frictional behaviour survey meter and on glass substrate, form and the silicon nitride ball frictional coefficient when grinding.The grapheme modified ceramic membrane of rare earth of glass substrate surface preparation can be with frictional coefficient 0.6 during from no film be reduced to about 0.1, have fairly obvious antifriction function.
Claims (10)
1. the method for the grapheme modified Ceramic Composite film of preparation rare earth on glass substrate comprises:
(1) the hydroxylation pre-treatment is carried out on the surface of glass substrate, the glass substrate after obtaining handling;
(2) titanate is dissolved in the ethanol, adds diethylolamine, mix under the room temperature, add aqueous ethanolic solution again, behind 15～25 ℃ of hydrolysis 1～3h, add rare earth compound, stir, add N again, the N'-N obtains rare-earth sol solution; Place the rare-earth sol solution of gained to handle 4-10h Graphene, obtain containing the Graphene colloidal sol of rare earth modified;
(3) glass substrate after the above-mentioned processing is immersed in the above-mentioned Graphene colloidal sol that contains the rare earth modified, leave standstill, glass substrate is upwards lifted out colloidal sol, drying;
(4) with the glass substrate of step (3) gained at 80～120 ℃ of insulation 30～90min, be warming up to 600～800 ℃ with the speed of 1～5 ℃/min, behind insulation 1～5h, naturally cool to room temperature, get final product.
2. a kind of method that on glass substrate, prepares the grapheme modified Ceramic Composite film of rare earth according to claim 1; It is characterized in that: the pretreated concrete steps of the described hydroxylation of step (1) are: glass substrate is immersed in the Pirahan solution; At room temperature left standstill 10～60 minutes; After deionized water drip washing, at 100～120 ℃ of drying 0.5～1h.
3. according to claim 2 a kind of on glass substrate the method for the grapheme modified Ceramic Composite film of preparation rare earth, it is characterized in that: described Pirahan solution is 98% the H of 70:30 by volume ratio
2SO
4Solution and 30% H
2O
2Solution composition.
4. according to claim 1 a kind of on glass substrate the method for the grapheme modified Ceramic Composite film of preparation rare earth, it is characterized in that: titanate is dissolved in the mol ratio of ethanol and titanate is 2～6:1 in the ethanol described in the step (2).
5. a kind of method that on glass substrate, prepares the grapheme modified Ceramic Composite film of rare earth according to claim 1, it is characterized in that: the mol ratio of diethylolamine described in the step (2) and titanate is 0.2～5:1.
6. a kind of method that on glass substrate, prepares the grapheme modified Ceramic Composite film of rare earth according to claim 1; It is characterized in that: the aqueous ethanolic solution described in the step (2) is that the water and the absolute ethyl alcohol of 1:8.5～9.5 is formulated by volume ratio, and the water in the aqueous ethanolic solution and the mol ratio of titanate are 1～2:1.
7. a kind of method that on glass substrate, prepares the grapheme modified Ceramic Composite film of rare earth according to claim 1, it is characterized in that: the rare earth compound described in the step (2) is Lanthanum trichloride, Cerium II Chloride, Lanthanum trinitrate or cerous nitrate.
8. a kind of method that on glass substrate, prepares the grapheme modified Ceramic Composite film of rare earth according to claim 1, it is characterized in that: the mol ratio of rare earth compound described in the step (2) and titanate is 2～5:10.
9. a kind of method that on glass substrate, prepares the grapheme modified Ceramic Composite film of rare earth according to claim 1 is characterized in that: the N described in the step (2), and the N'-N accounts for 0.2～1% of rare-earth sol overall solution volume; The concentration of described Graphene in rare-earth sol solution is 0.5-5mg/mL.
10. a kind of method that on glass substrate, prepares the grapheme modified Ceramic Composite film of rare earth according to claim 1, it is characterized in that: behind the completing steps (3), repetitive operation step (3) 1-5 time is carried out step (4) again.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924118A (en) * | 2012-11-12 | 2013-02-13 | 东华大学 | Method for preparing tombarthite-modifying-graphene ceramic composite film on monocrystalline silicon piece |
| CN102936139A (en) * | 2012-11-12 | 2013-02-20 | 东华大学 | Method for preparing rare earth modification carbon nano tube ceramic composite film on glass substrate |
| CN102942369A (en) * | 2012-11-12 | 2013-02-27 | 东华大学 | Method to prepare ceramic composite film of rare earth modification carbon nanometer tube-graphene on glass substrate |
| CN103693963A (en) * | 2013-11-18 | 2014-04-02 | 武汉理工大学 | Ti3SiC2-TiC-graphene self-lubricating composite material and in situ synthesis preparation method thereof |
| CN108004649A (en) * | 2017-12-28 | 2018-05-08 | 赵文立 | A kind of graphene nanocomposite material and preparation method thereof |
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| CN1736926A (en) * | 2005-07-14 | 2006-02-22 | 上海交通大学 | Method for preparing sulfhydryl silane-rare earth self-lubricating composite film on glass substrate surface |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924118A (en) * | 2012-11-12 | 2013-02-13 | 东华大学 | Method for preparing tombarthite-modifying-graphene ceramic composite film on monocrystalline silicon piece |
| CN102936139A (en) * | 2012-11-12 | 2013-02-20 | 东华大学 | Method for preparing rare earth modification carbon nano tube ceramic composite film on glass substrate |
| CN102942369A (en) * | 2012-11-12 | 2013-02-27 | 东华大学 | Method to prepare ceramic composite film of rare earth modification carbon nanometer tube-graphene on glass substrate |
| CN103693963A (en) * | 2013-11-18 | 2014-04-02 | 武汉理工大学 | Ti3SiC2-TiC-graphene self-lubricating composite material and in situ synthesis preparation method thereof |
| CN103693963B (en) * | 2013-11-18 | 2015-12-09 | 武汉理工大学 | A kind of Ti 3siC 2-TiC-Graphene self-lubricating composite and synthesizing preparation method in situ thereof |
| CN108568218A (en) * | 2017-03-13 | 2018-09-25 | 苏州市迈尔特材料科技有限公司 | The preparation method of porous graphene film and its application in terms of collecting carbonic anhydride |
| CN108568218B (en) * | 2017-03-13 | 2021-02-02 | 苏州市迈尔特材料科技有限公司 | Preparation method of porous graphene membrane and application of porous graphene membrane in aspect of carbon dioxide capture |
| CN108004649A (en) * | 2017-12-28 | 2018-05-08 | 赵文立 | A kind of graphene nanocomposite material and preparation method thereof |
| CN110420568A (en) * | 2019-09-03 | 2019-11-08 | 北京林业大学 | A method of promoting ceramic membrane permeant flux improves strainability |
| CN110420568B (en) * | 2019-09-03 | 2022-11-29 | 北京林业大学 | Method for improving water production flux of ceramic membrane and improving filtration performance |
| CN112795273A (en) * | 2020-12-31 | 2021-05-14 | 安徽鑫铂铝业股份有限公司 | Wear-resistant and corrosion-resistant aluminum profile for automobile luggage rack |
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Application publication date: 20121010 |