CN1339339A - Nanometer film material and its preparing method - Google Patents

Nanometer film material and its preparing method Download PDF

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Publication number
CN1339339A
CN1339339A CN 01122574 CN01122574A CN1339339A CN 1339339 A CN1339339 A CN 1339339A CN 01122574 CN01122574 CN 01122574 CN 01122574 A CN01122574 A CN 01122574A CN 1339339 A CN1339339 A CN 1339339A
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China
Prior art keywords
film material
metal
nano
nano film
film
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Pending
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CN 01122574
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Chinese (zh)
Inventor
卫英慧
胡兰青
姚敏琪
许并社
周禾丰
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Taiyuan University of Technology
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Taiyuan University of Technology
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Application filed by Taiyuan University of Technology filed Critical Taiyuan University of Technology
Priority to CN 01122574 priority Critical patent/CN1339339A/en
Publication of CN1339339A publication Critical patent/CN1339339A/en
Pending legal-status Critical Current

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Abstract

The present invention relates to metal material, inorganic material and other fields. The present invention features that nanometer film of metal, metal oxide and inorganic functional material may be obtained by irradiating easy to decompose large grain material with high-energy beam. The present invention solves many problems of practical production and operation, realizes the effective control on film position and shape, and opens one new way for the research and application of nanometer film technology.

Description

Nano film material and preparation method thereof
Nano film material of the present invention and preparation method thereof belongs to nano material and processing engineering technology category, relates to fields such as metal material, inorganic functional material.Specifically be nano film material of a kind of metal, metallic compound and inorganic functional material that makes with high energy beam irradiation raw material and preparation method thereof.
At present, the preparation nano film material often adopts vapor phase method: promptly under upper state (high temperature or plasma), the atom of random arrangement or molecule form also grows up into nanoparticle, general with the inorganic salts or the organic compound that are easy to volatilize, but the device therefor complexity, temperature is higher, cost is high; Also useful sol-gel processing: colloidal sol is formed film by infusion process or spining disk method on substrate, after gelation, can be transformed into amorphous state or polycrystalline attitude film by heat treatment, but the film microstructure is subjected to factor affecting such as polymer architecture, viscosity, the water yield, hoisting velocity, rotary speed and time in colloidal sol or the colloidal sol, is difficult to control.In addition, Chinese patent ZL97100952.X provides a kind of method for preparing metal, metal oxide superfine powder or metallic film with ultra-violet radiation.This method ultraviolet ray intensity is wayward, and based on the preparation superfine powder; Film is piled up by superfine powder and forms, and film thickness is thicker, exceeds nanometer range, and quality of forming film is relatively poor.At present, do not retrieve a kind of method that can the in-situ preparing nano thin-film as yet.When particularly using it for the Device element of high-tech, high request, connection status and stability thereof between the nuclear location of control composition film, growth process, crystallite dimension size, particulate have crucial meaning.And existing method still can't achieve the above object.
The purpose of nano film material of the present invention and preparation method thereof is to provide a kind of nano film material of metal, metallic compound and inorganic functional material continuous, that can have patterning and a kind of relative simple and feasible, fast, good reproducibility under the low temperature, can control the manufacture method of nucleation site, growth process, joint form and the film thickness of metal, metallic compound and inorganic functional material nano thin-film.
Nano film material of the present invention, it is characterized in that it being the metal that under high energy beam irradiation irradiation decomposition and high energy beam sputter, forms, the nano film material of metallic compound and inorganic functional material, this material is that different material forms according to preset ratio, nanoparticle is interconnective, have various decorative pattern and layout, the nano film material of composite construction, this material is the alternate composition of multiple material in same plane, different material forms compound transition layer, nano film material with continuous structure, this material are the gradient nano thin-film materials that forms in default gradient ratio on specific direction.
The preparation method of nano film material of the present invention, it is characterized in that it being that large particulate matter with metal, metallic compound and inorganic functional material is a raw material, disperse thing to dispose mutually different bulky grains by preset ratio, form nano film material under the high energy beam irradiation, its concrete processing step is:
A. be matrix with reality required sheet material or device;
B. on matrix, apply or drip the large particulate matter of thickness less than metal, metallic compound and the inorganic functional material of 10 μ m;
C. be 1 * 10 from the bulky grain top with intensity 18~1 * 10 22E/cm 2.sec high-power electron beam or power can generate continuous nano thin-film after being laser beam vertical irradiation 55~540s of 700W.
The preparation method of nano thin-film of the present invention is characterized in that it being that described metal, metallic compound and inorganic functional material are ZnS, H 2SnO 3, H 2TiO 3, Fe 2O 3XH 2O, Zn (OH) 2, NiCO 3, CuC 2O 4Deng metal oxide, fluoride and most of metallo-organic compound, the content of said components is advisable with 75~95%.
The preparation method of nano thin-film of the present invention is characterized in that it being that described high energy beam is electron beam, ion beam, laser etc., and its exposure intensity is advisable so that the energy that large particulate matter can be activated, reacts the required target product of generation to be provided.
Description of drawings:
[Fig. 1] individual layer nano film material preparation method schematic diagram
[Fig. 2] nano thin-film composite material and preparation method thereof schematic diagram
The nano film material preparation method schematic diagram of the alternate composition of [Fig. 3] multiple material
[Fig. 4] has the nano film material preparation method schematic diagram of layout
Symbol description:
A-matrix F-nano thin-film 2
B-bulky grain 1 G-nano compound film
C-high energy beam H-baffle plate
D-nano thin-film 1 I-multiple metal or the alternate nanometer of metal
E-bulky grain 2 films
Embodiment 1
As shown in Figure 1,50mg ZnS bulky grain B being added in the absolute ethyl alcohol of 30ml, after ultrasonic wave disperses 5 minutes, drip and having on the Cu net A of the thick carbon film of 20nm, be placed on the room temperature objective table in the vacuum chamber dripping A drying behind the B, is 1 * 10 with intensity 18E/cm 2The high-power electron beam C vertical irradiation of sec was observed under TEM after 55 seconds, can see thick, the uniform film D of the about 10nm of carbon film surface formation one deck that the Cu net is supported, through energy spectrum analysis, confirmed as ZnS.
Embodiment 2
As shown in Figure 2, in embodiment 1, drip deposited one deck warp and the same H that handles of B on the formed ZnS nano thin-film 2SnO 3Bulky grain E is placed on the room temperature objective table in the vacuum chamber again, and the exposure intensity of adjusting high-power electron beam is 1 * 10 22, shine after 540 seconds, covered by film F above under TEM, observing ZnS film D, through energy spectrum analysis, confirm as SnO 2D and F form nano-multilayer film G on A.
Embodiment 3
With ZnS bulky grain B and the H after handling similarly to Example 1 2SnO 3Bulky grain E is alternate to be coated in the surface of aluminum plate that thickness is 3mm, and coating layer thickness is 1 μ m.With special baffle plate H bulky grain E top is blocked earlier, with power is the laser beam vertical irradiation 300 seconds of 700W, with H the top of B is blocked again, after laser beam irradiation 360 seconds, producing diameter is the thick sample of 3mm, observes under TEM, forms the film I that thickness is about 35nm, through confirming, by ZnS nano thin-film D and SnO 2The alternate composition of nano thin-film F.
Embodiment 4
As shown in Figure 4, will be coated in aluminium plate matrix A through the ZnS bulky grain B with embodiment 1 same treatment equably and go up formation one annulus, coating layer thickness is 5 μ m.With power is the laser beam vertical irradiation of 700W after 300 seconds, produces the sample that diameter is 3mm, observes under TEM, and the A surface has a layer thickness to be about the film D of 40nm, through confirming as ZnS.

Claims (4)

1. nano film material, it is characterized in that it being the metal that under high energy beam irradiation irradiation decomposition and high energy beam sputter, forms, the nano film material of metallic compound and inorganic functional material, this material is that different material forms according to preset ratio, nanoparticle is interconnective, have various decorative pattern and layout, the nano film material of composite construction, this material is the alternate composition of multiple material in same plane, different material forms compound transition layer, nano film material with continuous structure, this material are the gradient nano thin-film materials that forms in default gradient ratio on specific direction.
2. press the preparation method of the described nano film material of claim 1, it is characterized in that it being that large particulate matter with metal, metallic compound and inorganic functional material is a raw material, disperse thing to dispose mutually different bulky grains by preset ratio, form nano film material under the high energy beam irradiation, its concrete processing step is:
A. be matrix with reality required sheet material or device;
B. on matrix, apply or drip the large particulate matter of thickness less than metal, metallic compound and the inorganic functional material of 10 μ m;
C. be 1 * 10 from the bulky grain top with intensity 18~1 * 10 22E/cm 2.sec behind high-power electron beam or the laser beam vertical irradiation 55~540s, can generate continuous nano thin-film.
3. by the preparation method of the described nano film material of claim 2, it is characterized in that it being that described metal, metallic compound and inorganic functional material are ZnS, H 2SnO 3, H 2TiO 3, Fe 2O 3XH 2O, Zn (OH) 2, NiCO 3, CuC 2O 4Deng metal oxide, fluoride and most of metallo-organic compound, the content of said components is advisable with 75~95%.
4. press the preparation method of the described nano film material of claim 2, it is characterized in that it being that described high energy beam is electron beam, ion beam, laser etc., its exposure intensity is advisable so that the energy that large particulate matter can be activated, reacts the required target product of generation to be provided.
CN 01122574 2001-07-12 2001-07-12 Nanometer film material and its preparing method Pending CN1339339A (en)

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CN 01122574 CN1339339A (en) 2001-07-12 2001-07-12 Nanometer film material and its preparing method

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Application Number Priority Date Filing Date Title
CN 01122574 CN1339339A (en) 2001-07-12 2001-07-12 Nanometer film material and its preparing method

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100434353C (en) * 2006-01-24 2008-11-19 南京大学 Gas phase synthesis process of nanometer particle array with one-dimensional diameter and number density gradient
CN100438990C (en) * 2006-08-21 2008-12-03 泉耀新材料科技(上海)有限公司 Method for preparing nano film through a low temperature procedure
CN101137898B (en) * 2005-03-07 2011-05-18 3M创新有限公司 Thermoplastic film having metallic nanoparticle coating

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101137898B (en) * 2005-03-07 2011-05-18 3M创新有限公司 Thermoplastic film having metallic nanoparticle coating
CN100434353C (en) * 2006-01-24 2008-11-19 南京大学 Gas phase synthesis process of nanometer particle array with one-dimensional diameter and number density gradient
CN100438990C (en) * 2006-08-21 2008-12-03 泉耀新材料科技(上海)有限公司 Method for preparing nano film through a low temperature procedure

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