CN103613088A

CN103613088A - Method for preparing carbon nanotube brush with consistent hole pitch

Info

Publication number: CN103613088A
Application number: CN201310601612.1A
Authority: CN
Inventors: 杨志; 朱兴忠; 程应武; 苏言杰; 张亚非
Original assignee: Shanghai Jiaotong University
Current assignee: Shanghai Jiaotong University
Priority date: 2013-11-25
Filing date: 2013-11-25
Publication date: 2014-03-05
Anticipated expiration: 2033-11-25
Also published as: CN103613088B

Abstract

The invention discloses a method for preparing carbon nanotube brush with consistent hole pitch. The method comprises the following steps of: putting a hole duct template with consistent hole pitch into a tubular furnace, growing a carbon nanotube array by adopting a chemical vapor deposition method, wherein one carbon nanotube grows in each hole duct; grinding the template in which the carbon nanotube array grows through abrasive paper, then binding to a silicon chip, glass or a flexible polyimide substrate, and curing at room temperature; finally removing the skeleton ingredients of the hole duct templates, cleaning with deionized water and drying, and exposing brush hairs to form the carbon nanotube brush. The method is simple in technology and strong in practicability, the density of brush hairs of the prepared carbon nanotube brush is controllable, the length of the brush hairs of the prepared carbon nanotube brush is consistent, and the carbon nanotube brush is convenient for large-scale industrial production, and has tremendous application potential on the aspect of cleaning in the field of microelectronics.

Description

A kind of method of preparing the carbon nanotube brush that pitch of holes is consistent

Technical field

The present invention relates to a kind of preparation method of nano material, be specifically related to a kind of method of preparing the carbon nanotube brush that pitch of holes is consistent.

Background technology

Carbon nanotube is a kind of monodimension nanometer material of excellent performance, and it can be divided into Single Walled Carbon Nanotube, double-walled carbon nano-tube and multi-walled carbon nano-tubes.A large amount of research work has in recent years disclosed carbon nanotube and has had unique electricity, physics, chemistry and mechanical property.Research at present finds that the potential Application Areas of carbon nanotube mainly comprises: nano electron device, sensor, a transmitting, battery, Chu Qing, demonstration and matrix material etc.Carbon nanotube has that size is little, density is low, aspect ratio is large, thermostability is strong, resistance to compression and high resilience, unreactiveness and excellent heat-conductivity conducting performance, be one of ideal material of preparing bristle, prepared carbon nanotube brush has very large application potential at microelectronic aspect clean.

Carbon nanotube based on carbon nano pipe array is brushed with a small amount of research report (Nature Materials2005 in recent years, 4,540-545), it is mainly directly being loaded with carbon nano-tube on the silicon carbide fiber of catalyzer by chemical Vapor deposition process, but because carbon nano pipe array super-high density is closely arranged in parallel, between tube bank, spacing is very little, can not regulate and control " bristle " soft durometer, be difficult to realize the consistent hair brush structure of pitch of holes truly and seriously restricted its performance and application.

Therefore, those skilled in the art is devoted to develop a kind of method of preparing the carbon nanotube brush that pitch of holes is consistent.

Summary of the invention

Technical problem to be solved by this invention is: overcome above-mentioned the deficiencies in the prior art, propose a kind of method of preparing the carbon nanotube brush that pitch of holes is consistent.

For achieving the above object, the invention provides a kind of method of preparing pitch of holes carbon nanotube always, utilize duct template chemical vapour deposition that pitch of holes is consistent to obtain regular carbon nano pipe array and prepare carbon nanotube brush, fully guaranteed that the interval of bristle is all even in good order.

A method of preparing the carbon nanotube brush that pitch of holes is consistent, comprises the following steps:

Step 1, carbon nano-tube on duct and the consistent template of pitch of holes, the described carbon nanotube of growing in duct described in each, forms carbon nano pipe array.

Step 2, will adhere in substrate and solidify after described template polishing, and carbon nanotube and substrate are fixed together; Solidify and at room temperature carry out.

Step 3, removes described template, and the carbon nanotube staying and substrate are cleaned and dried, and forms carbon nanotube brush.Clean and use deionized water.Carbon nanotube is exactly the bristle of carbon nanotube brush.

Preferably, in step 1, the pore diameter range of template is 30～200nm, and the thickness of template is 30～150 μ m.Template is selected the interconnected template of anodised aluminium duct template, unicircuit or the TSV duct template of stereo integrated circuit.

Preferably, use chemical Vapor deposition process carbon nano-tube in template in step 1, carbon source is a kind of in acetylene, ethene, methane; Temperature of reaction is 650～900 ℃; Reaction times is 1～3h.Chemical Vapor deposition process carries out in tube furnace.By the reaction times, control the growth of carbon nanotube, play the effect of pilot brush staple length.

Preferably, in step 2, polishing adopts sand papering, and sand paper is 1000～2000 object sand paper.

More preferably, the time of the sand papering in step 2 is 3～5min.

Preferably, the substrate in step 2 is silicon chip, sheet glass or flexible polyimide plate.Other materials smooth and acid-alkali-corrosive-resisting also can be used as substrate and uses.

Preferably, the employing of the adhesion in step 2 epoxy resin is adhesive agent.

Preferably, in step 2, the curing time is 24～48h.

Preferably, remove described template and dissolve with sodium hydroxide or potassium hydroxide solution in step 3, strength of solution is 1～3mol/L.

Preferably, the time of dissolving is 12～36h.

Compared with prior art, the present invention has following beneficial effect: technique is simple, practical, and the bristle density of making carbon nanotube brush is controlled, and length is consistent, is convenient to large-scale commercial production.

Below with reference to accompanying drawing, the technique effect of design of the present invention, specific examples and generation is described further, to understand fully the present invention.Provide the object of these explanations to be only to help to explain the present invention, should not be used for limiting the scope of claim of the present invention.

Accompanying drawing explanation

Fig. 1 is the schematic diagram of the carbon nanotube brush prepared of a preferred embodiment of the present invention;

Fig. 2 is the stereoscan photograph of the bristle of carbon nanotube brush in Fig. 1.

Embodiment

Below in conjunction with accompanying drawing, embodiments of the invention are elaborated, the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.

Embodiment 1

Step 1, gets an aperture and is that 80nm, pitch of holes are consistent, thickness is the anodised aluminium duct template of 30 μ m, puts into tube furnace, with acetylene as carbon source, chemical vapour deposition reaction 3h carbon nano-tube at 650 ℃.The carbon nanotube of growing in each duct forms carbon nano pipe array in template.

Step 2, cuts into the template of the carbon nano pipe array of having grown in the sample of 2 * 2mm size, with the 1000 object sand paper 3min that polishes gently, uses deionized water washes clean.On sample being sticked to epoxy resin at the bottom of the silicon wafer-based of 3 * 20mm size, be placed in dry 24h under room temperature, guarantee bonding firmly.

Step 3, the sodium hydroxide solution that the sample brush of preparation is placed in to 1mol/L dissolves 24h, guarantees that alumina formwork is dissolved completely, then uses washed with de-ionized water three times.At the bottom of leaving silicon wafer-based and carbon nanotube, on even carbon nanotube is distributed at the bottom of silicon wafer-based, form the carbon nanotube brush that pitch of holes is consistent, carbon nanotube quality is soft, plays the effect of bristle.Can replace sodium hydroxide solution with potassium hydroxide solution.

Above-mentioned preparation process, can control the thickness of bristle by aperture, control the spacing of bristle by pitch of holes, controls the length of bristle by the chemical vapour deposition reaction time.This method is prepared carbon nanotube brush, and technique is simple, practical, and the bristle density of making carbon nanotube brush is controlled, and length is consistent, is convenient to large-scale commercial production.

Fig. 1 is the schematic diagram of the carbon nanotube brush of preparation, and carbon nanotube brush comprises bristle 1 and substrate 2, and bristle 1 is formed by the consistent carbon nanotube of spacing, and substrate 2 is materials of silicon chip or other surfacings acid-alkali-corrosive-resisting.

Fig. 2 is the stereoscan photograph of the bristle of carbon nanotube brush.As can be seen from Figure 2, the bristle of carbon nanotube brush is soft, and the spacing of bristle is more consistent, and prepared carbon nanotube brush has very large application potential at microelectronic aspect clean.

Embodiment 2

Step 1, getting an aperture is that 120nm, thickness are the anodised aluminium duct template of 50 μ m, puts into tube furnace, with ethene as carbon source, chemical vapour deposition reaction 3h carbon nano-tube at 700 ℃.The carbon nanotube of growing in each duct forms carbon nano pipe array in template.

Step 2, cuts into the template of the carbon nano pipe array of having grown in the sample of 2 * 2mm size, with the 2000 object sand paper 5min that polishes gently, uses deionized water washes clean.On sample being sticked to epoxy resin at the bottom of the silicon wafer-based of 3 * 20mm size, be placed in dry 24h under room temperature, guarantee bonding firmly.

Step 3, the sodium hydroxide solution that the sample brush of preparation is placed in to 2mol/L dissolves 12h, guarantees that alumina formwork is dissolved completely, then uses washed with de-ionized water three times, obtains carbon nanotube brush.

Embodiment 3

Step 1, getting an aperture is that 150nm, thickness are the interconnected template of the unicircuit of 80 μ m, puts into tube furnace, with methane as carbon source, chemical vapour deposition reaction 2h carbon nano-tube at 750 ℃.The carbon nanotube of growing in each duct forms carbon nano pipe array in template.

Step 2, cuts into the template of the carbon nano pipe array of having grown in the sample of 2 * 2mm size, with the 1000 object sand paper 3min that polishes gently, uses deionized water washes clean.With epoxy resin, sample is sticked in the glass sheet substrate of 3 * 20mm size, be placed in dry 48h under room temperature, guarantee bonding firm.

Step 3, the sodium hydroxide solution that the sample brush of preparation is placed in to 1mol/L dissolves 24h, guarantees that the interconnected template of unicircuit is dissolved completely, then uses washed with de-ionized water three times, obtains carbon nanotube brush.

Embodiment 4

Step 1, getting an aperture is that 200nm, thickness are the TSV duct template of the stereo integrated circuit of 120 μ m, puts into tube furnace, with acetylene as carbon source, chemical vapour deposition reaction 1h carbon nano-tube at 850 ℃.

Step 2, cuts into the template of the carbon nano pipe array of having grown in the sample of 2 * 2mm size, with the 1000 object sand paper 4min that polishes gently, uses deionized water washes clean.With epoxy resin, sample is sticked in the flexible polyimide plate substrate of 3 * 20mm size, be placed in dry 48h under room temperature, guarantee bonding firm.

Step 3, the sodium hydroxide solution that the sample brush of preparation is placed in to 3mol/L dissolves 36h, guarantees that the TSV duct template of stereo integrated circuit is dissolved completely, then uses washed with de-ionized water three times, obtains carbon nanotube brush.

More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just can design according to the present invention make many modifications and variations without creative work.Therefore, all technician in the art, all should be in the determined protection domain by claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.

Claims

1. a method of preparing the carbon nanotube brush that pitch of holes is consistent, is characterized in that, comprises the following steps:

Step 1, carbon nano-tube on duct and the consistent template of pitch of holes, the described carbon nanotube of growing in duct described in each, forms carbon nano pipe array;

Step 2, will adhere in substrate and solidify after described template polishing, and carbon nanotube and substrate are fixed together;

Step 3, removes described template, and the carbon nanotube staying and substrate are cleaned, and forms carbon nanotube brush.

2. according to a kind of method of preparing the carbon nanotube brush that pitch of holes is consistent described in claim 1, it is characterized in that, the pore diameter range of template described in described step 1 is 30～200nm, and the thickness of described template is 30～150 μ m.

3. according to a kind of described in claim 1, prepare the method for the carbon nanotube brush that pitch of holes is consistent, it is characterized in that, use chemical Vapor deposition process carbon nano-tube in described template in described step 1, carbon source is a kind of in acetylene, ethene, methane; Temperature of reaction is 650～900 ℃, and the reaction times is 1～3h.

4. according to a kind of method of preparing the carbon nanotube brush that pitch of holes is consistent described in claim 1, it is characterized in that, polishing described in described step 2 adopts sand papering, and described sand paper is 1000～2000 object sand paper.

5. according to a kind of method of preparing the carbon nanotube brush that pitch of holes is consistent described in claim 4, it is characterized in that, the time of the described sand papering in described step 2 is 3～5min.

6. according to a kind of method of preparing the carbon nanotube brush that pitch of holes is consistent described in claim 1, it is characterized in that, the described substrate in described step 2 is silicon chip, sheet glass or flexible polyimide plate.

7. according to a kind of method of preparing the carbon nanotube brush that pitch of holes is consistent described in claim 1, it is characterized in that, it is adhesive agent that the described adhesion in described step 2 adopts epoxy resin.

8. according to a kind of method of preparing the carbon nanotube brush that pitch of holes is consistent described in claim 1, it is characterized in that, the curing time described in described step 2 is 24～48h.

9. according to a kind of method of preparing the carbon nanotube brush that pitch of holes is consistent described in claim 1, it is characterized in that, in described step 3, remove described template and dissolve with sodium hydroxide or potassium hydroxide solution, strength of solution is 1～3mol/L.

10. according to a kind of method of preparing the carbon nanotube brush that pitch of holes is consistent described in claim 9, it is characterized in that, the time of described dissolving is 12～36h.