CN1978517A - Method for preparing metal silver molybdenum disulfide hybrid composite material - Google Patents
Method for preparing metal silver molybdenum disulfide hybrid composite material Download PDFInfo
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- CN1978517A CN1978517A CN 200510126586 CN200510126586A CN1978517A CN 1978517 A CN1978517 A CN 1978517A CN 200510126586 CN200510126586 CN 200510126586 CN 200510126586 A CN200510126586 A CN 200510126586A CN 1978517 A CN1978517 A CN 1978517A
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Abstract
This invention discloses a preparation method of the complex material with an insert layer of metal silver and molybdenum disulfide. The method is based on the condition of macromolecule protecting so that the metal element can be inserted. Firstly, the solution containing metal ions and the polymers were mixed so as to form the colloidal sols system. Then the colloidal sols were inserted into the monolayer of molybdenum disulfide. Finally, the metal ions were deoxidized and the complex material with an insert layer of metal silver and molybdenum disulfide was obtained. This method inaugurated a new approach for synthesizing the complex material with inserted layers. The metal ions in the complex material were deoxidized totally to metal elements, so there was no mixture of metal ions and metal elements. The inserted method under the condition of macromolecule protecting is simple and practical, and has expansive application prospect. Compared with molybdenum disulfide, the electric conductivity of the material in this invention was increased by 6 orders of magnitude. The material has potential application values in the area of conductive materials, lubricative materials and micro-electronics mechanism.
Description
Technical field
The present invention relates to a kind of preparation method of metal silver molybdenum disulfide hybrid composite material, specially refer to the preparation method of the matrix material of polymkeric substance and mineral filler composition.
Background technology
Molybdenumdisulphide is solid lubricant and the semiconductor material with good lubrication performance, it has two-dimensional layered structure, there are intensive ionic linkage and covalent linkage effect in the layer, interlayer is with weak Van der Waals force combination, utilize this characteristics, different ions, molecule and polymkeric substance can be inserted into its interlayer and form intercalation composite material.People such as Allen insert the molybdenumdisulphide interlayer with some metal ions, as Hg
2+, Ag
+, Co
2+, Mn
2+, Ru
2+, Ni
2+Deng, prepared the metal ion molybdenum disulfide hybrid composite material.In order to make the metal ion that is inserted into the molybdenumdisulphide interlayer be converted into metal simple-substance, the human heat-treating methods is arranged, experimental results show that this method can make Ag
0.61MoS
2The middle MoS that inserts
2The Ag of interlayer
+Be reduced to argent, but cause easily and take off slottingly, the research of therefore carrying out metal dithionite molybdenum intercalation composite material new synthetic process is very necessary, also is the focus of current research.Metallic nano-particle is inserted into the molybdenumdisulphide interlayer, can prepare have electroconductibility, magnetic, self-lubricating, low abrasive functional molybdenum disulfide hybrid composite material, application prospect is boundless.Existing Chinese patent 02124645.9,02150059.2,03127931.7 grade has reported that in-situ inserted polymerization is equipped with the method for polymkeric substance molybdenum disulfide hybrid composite material.In these patents, obtain polystyrene, polyimide and polyoxymethylene molybdenum disulfide hybrid composite material, but do not related to argent and molybdenum disulfide hybrid composite material and preparation method thereof.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of metal silver molybdenum disulfide hybrid composite material.
The present invention is a kind of intercalation method based on the metal simple-substance under the polymer protection condition; total invention thought is that polymkeric substance and the aqueous solution that contains metal ion are formed the uniform sol system; then colloidal sol is inserted into the molybdenumdisulphide interlayer, metal ion is reduced handle the molybdenum disulfide hybrid composite material that promptly obtains pbz polymer and metal simple-substance at last.By selecting different polymkeric substance, can obtain different metal-containing polymer molybdenum disulfide hybrid composite materials.
A kind of preparation method of metal silver molybdenum disulfide hybrid composite material, it is characterized in that this method in the following order step carry out:
A adds equimolar aqueous sodium hydroxide solution in silver nitrate aqueous solution, Silver Nitrate is converted into silver suboxide, then with being dissolved in behind the deionized water wash in the ammoniacal liquor; Mix with aqueous solutions of polymers again and obtain mixing solutions; Polymkeric substance is selected from polyvinyl alcohol, polyvinylpyrrolidone or polymethyl acrylic acid;
B adds LiMoS with above-mentioned mixing solutions
2In the aqueous solution, stir after 6～30 hours, add excessive 0.1M aqueous formic acid, reaction product is behind centrifugation and deionized water wash, and vacuum-drying promptly obtains metal silver molybdenum disulfide hybrid composite material.
Molybdenumdisulphide is a kind of compound of layered metal structure, each individual layer molybdenumdisulphide includes two-layer S atom therebetween one deck Mo atom, form sandwich sandwich structure, this flaggy is piled up up and down in crystal, make the S atomic shell of the S atomic shell of a flaggy and another flaggy adjacent, therebetween by weak Van der Waals force combination.6 the S atoms of arranging around the Mo atom in the laminate structure, between them with the strong covalent bond combination.The Mo atom is taked the triangular prism coordination generally speaking, forms 2H type or 3R type structure, and shows metal or metalloid.This structure of molybdenumdisulphide provides advantageous conditions for the preparation intercalation composite material, but, the object positively charged ion that some volumes are bigger can not form intercalation compound by direct reaction, alkalimetal ion can only be inserted in advance, and then remove to exchange out alkalimetal ion, thereby obtain expecting intercalation compound with bigger positively charged ion.
The used polymkeric substance of the present invention is the polymkeric substance with good aqueous solubility, can select polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP) or polymethyl acrylic acid (PMAA).
The metal silver molybdenum disulfide hybrid composite material of the present invention's preparation, metal ion has been reformed completely into metal simple-substance, rather than the mixture of metal ion and metal simple-substance, and its conductivity has improved 6 orders of magnitude than molybdenumdisulphide.This method realized the compound of metal simple-substance silver and molybdenum disulfide nano yardstick, and this method has solved the problem that metal simple-substance is inserted into molybdenumdisulphide sheet interlayer.
The metal silver molybdenum disulfide hybrid composite material of the present invention's preparation, solved the problem that the metal ion that is inserted into the molybdenumdisulphide interlayer among other preparation method can not be converted into metal simple-substance fully, preparation method's technology is simple, easy to operate, be easy to industrialization, at electro-conductive material, lubricant and microelectron-mechanical field have potential using value.
The present invention is a kind of intercalation method based on the metal simple-substance under the polymer protection condition; this method has been opened up the new way of synthetic metal intercalation composite material; metal ion has been reformed completely into metal simple-substance in the prepared intercalation composite material, rather than the mixture of metal ion and metal simple-substance.Molybdenumdisulphide is semiconductor material, and the specific conductivity of prepared metal silver molybdenum disulfide hybrid composite material has improved 6 orders of magnitude than molybdenumdisulphide, has the potential using value aspect electro-conductive material, lubricant and the microelectronic material.The intercalation method of the metal simple-substance under this polymer protection condition is simple and practical, has broad application prospects.
Embodiment
Embodiment 1
Take by weighing the Silver Nitrate of 0.5g, water-soluble 10% the aqueous solution of being made into, add equimolar aqueous sodium hydroxide solution, Silver Nitrate is converted into silver suboxide, with the deionized water wash number all over after be dissolved in 15% the weak ammonia and even with 15% the aqueous solution that contains the 1g polyvinyl alcohol, the gained mixing solutions is added the LiMoS that contains 0.75g
2In the aqueous solution, stir after 24 hours, dropwise add the aqueous formic acid of excessive 0.1M, reaction product behind centrifugation and deionized water wash, vacuum-drying.
Embodiment 2
Take by weighing the Silver Nitrate of 0.4g, water-soluble 18% the aqueous solution of being made into, add equimolar aqueous sodium hydroxide solution, Silver Nitrate is converted into silver suboxide, with the deionized water wash number all over after be dissolved in 20% the weak ammonia and even with 15% the aqueous solution that contains the 1.3g polyvinyl alcohol, the gained mixing solutions is added the LiMoS that contains 0.75g
2In the aqueous solution, stir after 30 hours, dropwise add the aqueous formic acid of excessive 0.1M, reaction product behind centrifugation and deionized water wash, vacuum-drying.
Embodiment 3
Take by weighing the Silver Nitrate of 2.0g, water-soluble 40% the aqueous solution of being made into, add equimolar aqueous sodium hydroxide solution, Silver Nitrate is converted into silver suboxide, with the deionized water wash number all over after be dissolved in 25% the weak ammonia and even with 16% the aqueous solution that contains the 5g polyvinylpyrrolidone, the gained mixing solutions is added the LiMoS that contains 2.5g
2In the aqueous solution, stir after 30 hours, dropwise add the aqueous formic acid of excessive 0.1M, reaction product behind centrifugation and deionized water wash, vacuum-drying.
Embodiment 4
Take by weighing the Silver Nitrate of 1.5g, water-soluble 10% the aqueous solution of being made into, add equimolar aqueous sodium hydroxide solution, Silver Nitrate is converted into silver suboxide, with the deionized water wash number all over after be dissolved in 20% the weak ammonia and even with 1% the aqueous solution that contains the 1.5g polyvinylpyrrolidone, the gained mixing solutions is added the LiMoS that contains 3.0g
2In the aqueous solution, stir after 8 hours, dropwise add the aqueous formic acid of excessive 0.1M, reaction product behind centrifugation and deionized water wash, vacuum-drying.
Embodiment 5
Take by weighing the Silver Nitrate of 0.3g, water-soluble 15% the aqueous solution of being made into, add equimolar aqueous sodium hydroxide solution, Silver Nitrate is converted into silver suboxide, with the deionized water wash number all over after be dissolved in 25% the weak ammonia and even with 30% the aqueous solution that contains the 2.0g polymethyl acrylic acid, the gained mixing solutions is added the LiMoS that contains 1.0g
2In the aqueous solution, stir after 10 hours, dropwise add the aqueous formic acid of excessive 0.1M, reaction product behind centrifugation and deionized water wash, vacuum-drying.
Claims (1)
1, a kind of preparation method of metal silver molybdenum disulfide hybrid composite material, it is characterized in that this method in the following order step carry out:
A adds equimolar aqueous sodium hydroxide solution in silver nitrate aqueous solution, Silver Nitrate is converted into silver suboxide, then with being dissolved in behind the deionized water wash in the ammoniacal liquor; Mix with aqueous solutions of polymers again and obtain mixing solutions; Polymkeric substance is selected from polyvinyl alcohol, polyvinylpyrrolidone or polymethyl acrylic acid;
B adds LiMoS with above-mentioned mixing solutions
2In the aqueous solution, stir after 6～30 hours, add excessive 0.1M aqueous formic acid, reaction product is behind centrifugation and deionized water wash, and vacuum-drying promptly obtains metal silver molybdenum disulfide hybrid composite material.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102944907A (en) * | 2012-11-10 | 2013-02-27 | 清华大学 | Modified composite material for layered intercalation and method for realizing negative refraction |
| CN103497473A (en) * | 2013-08-30 | 2014-01-08 | 哈尔滨工业大学 | Preparation method of nano-grade silver particle/two-dimensional layered nano-structure composite film |
| CN104525938A (en) * | 2014-12-23 | 2015-04-22 | 国家纳米科学中心 | Molybdenum disulfide/gold nanorod composite, preparation method and application |
| CN105271411A (en) * | 2015-11-04 | 2016-01-27 | 太原理工大学 | Preparation method for molybdenum disulfide quantum dot |
| CN106964372A (en) * | 2017-04-16 | 2017-07-21 | 合肥国轩高科动力能源有限公司 | A kind of metal nanoparticle asymmetry one side inlays the synthetic method of molybdenum disulfide nano sheet |
| WO2018013055A1 (en) * | 2016-07-12 | 2018-01-18 | National University Of Singapore | Composite materials and processes of manufacturing the same for use as high performance catalysts for water splitting |
| CN109627413A (en) * | 2018-12-07 | 2019-04-16 | 上海应用技术大学 | A kind of high abrasion polyurethane material and preparation method thereof |
| CN112777585A (en) * | 2019-11-01 | 2021-05-11 | 清华大学 | Two-dimensional composite material, preparation method and application thereof |
-
2005
- 2005-11-30 CN CN 200510126586 patent/CN1978517A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102944907A (en) * | 2012-11-10 | 2013-02-27 | 清华大学 | Modified composite material for layered intercalation and method for realizing negative refraction |
| CN103497473A (en) * | 2013-08-30 | 2014-01-08 | 哈尔滨工业大学 | Preparation method of nano-grade silver particle/two-dimensional layered nano-structure composite film |
| CN104525938A (en) * | 2014-12-23 | 2015-04-22 | 国家纳米科学中心 | Molybdenum disulfide/gold nanorod composite, preparation method and application |
| CN104525938B (en) * | 2014-12-23 | 2017-02-22 | 国家纳米科学中心 | Molybdenum disulfide/gold nanorod composite, preparation method and application |
| CN105271411A (en) * | 2015-11-04 | 2016-01-27 | 太原理工大学 | Preparation method for molybdenum disulfide quantum dot |
| WO2018013055A1 (en) * | 2016-07-12 | 2018-01-18 | National University Of Singapore | Composite materials and processes of manufacturing the same for use as high performance catalysts for water splitting |
| CN106964372A (en) * | 2017-04-16 | 2017-07-21 | 合肥国轩高科动力能源有限公司 | A kind of metal nanoparticle asymmetry one side inlays the synthetic method of molybdenum disulfide nano sheet |
| CN106964372B (en) * | 2017-04-16 | 2019-04-19 | 合肥国轩高科动力能源有限公司 | A kind of metal nanoparticle asymmetry single side inlays the synthetic method of molybdenum disulfide nano sheet |
| CN109627413A (en) * | 2018-12-07 | 2019-04-16 | 上海应用技术大学 | A kind of high abrasion polyurethane material and preparation method thereof |
| CN109627413B (en) * | 2018-12-07 | 2021-05-28 | 上海应用技术大学 | High-wear-resistance polyurethane material and preparation method thereof |
| CN112777585A (en) * | 2019-11-01 | 2021-05-11 | 清华大学 | Two-dimensional composite material, preparation method and application thereof |
| CN112777585B (en) * | 2019-11-01 | 2022-10-04 | 清华大学 | Two-dimensional composite material, preparation method and application thereof |
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