CN103361613A - Method for preparing column-shaped nano-tungsten - Google Patents

Abstract

The invention discloses a method for preparing column-shaped nano-tungsten. The method enables tungsten to grow on a graphite substrate in a tilted column shape, and can be used for studying the radiation performance of a first wall material. The method mainly comprises the following steps of: (1) manufacturing a sample rack, namely manufacturing a cylinder, and clamping four substrates at different angles inside the cylinder for simultaneously sputtering; (2) preparing the graphite substrate, namely preparing the graphite substrate with the size of 1cm*1cm, and washing the substrate to a certain extent; and (3) preparing the column-shaped nano-tungsten by a direct-current magnetron sputtering glancing angle deposition method, namely sputtering a pure tungsten target material on the graphite conductive substrate by changing the included angle alpha between the normal direction of the substrate and an incident particle flow so as to prepare a column-shaped nano-tungsten membrane.

Description

A kind of method for preparing nano columnar metal tungsten

technical field

The patent of the invention belongs to the field of nanomaterials and material manufacturing, and relates to a method for preparing nano-columnar metal tungsten by DC magnetron sputtering. the

Background technique

Magnetron sputtering is to perform high-speed sputtering under low pressure, and the ionization rate of the gas must be effectively increased. By introducing a magnetic field on the surface of the target cathode, using the magnetic field to confine the charged particles to increase the plasma density and increase the sputtering rate. The DC sputtering method requires the target to be able to transfer the positive charge obtained from the ion bombardment process to the cathode that is in close contact with it, so this method can only sputter conductive materials and is not suitable for insulating materials. Commonly used metal materials are W, Au, Ag, Ti, Cr, etc. The methods commonly used at present usually include: the sputtering direction of the substrate and the metal particles is vertical, and when a certain vacuum degree and ion concentration are reached, the metal particles will deposit a uniform film on the surface of the substrate, the thickness of the film and the sputtering time and the nature of ions. the

Purpose of the invention

The purpose of the present invention is to form a uniformly distributed nano columnar tungsten film on the surface of the substrate through the technique of direct current magnetron sputtering grazing angle deposition. the

Contents of the invention

The technical problem proposed by the invention is to provide a new method capable of forming a nano columnar tungsten film on the surface of a substrate. the

(1) Design and manufacture a sample holder with a certain inclination angle

A cylinder was made, the inside of which can hold four substrates with different angles and sputter at the same time. the

(2) Magnetron sputtering coating

There are many methods for preparing metal thin films, including sol-gel method, L-B film method, chemical vapor deposition (CVD), vacuum evaporation method, molecular beam and atomic beam epitaxy, sputtering deposition and other methods. The thickness of the metal film is tens of nanometers to several micrometers. Sputtering deposition was performed under the conditions of DC magnetron sputtering duty cycle 50%, current 0.15A, and voltage 300V. the

(3) Preparation of nano-columnar tungsten by grazing angle deposition

DC magnetron sputtering can ensure uniform and orderly deposition of particles under a certain duty cycle and a relatively small current. In addition, the substrate has a certain inclination angle, which can ensure that the grains grow along a certain direction. , and at a certain angle to the substrate, sputtering for about 3 hours can produce nano-columnar tungsten with an aspect ratio of about 10:1. the

Detailed ways

The embodiments of the present invention are described in detail below. This embodiment is implemented under the premise of the technical solution of the present invention, and detailed implementation methods and specific operation processes are provided, but the protection scope of the present invention is not limited to the following embodiments. . the

Example 1

This embodiment comprises the following steps:

(1) Production of sample holder

Car out an aluminum cylinder with a specified size, with an outer diameter of 5.8cm and an inner diameter of 5.1cm. The wall of the cylinder is divided into four rows of holes. The distance between the two holes in each row is 2.0cm, and the sample holder is 2.5cm. In the well, the sample is fixed on the sample holder. the

(2) Cleaning of the substrate

The 1cm*1cm graphite substrate was ultrasonically cleaned in ethanol, acetone, and deionized water for 10 minutes, and then dried with high-pressure airflow. Finally it is fixed at a specific angle on the sample holder. the

(3) Preparation of nano-columnar tungsten film

Using the method of grazing angle deposition and oblique growth, under the conditions of background vacuum 3*10-4Pa, current 0.15A, and voltage 300V, by changing the angle α between the normal direction of the substrate and the incident particle flow, the graphite conductive Nanocolumnar tungsten films were prepared by sputtering pure tungsten targets on the substrate. After several hours of sputtering, nano-columnar tungsten is finally grown. the

Description of drawings

Figure 1 is a diagram of a simple device in a vacuum chamber. the

Claims (7)

1. method for preparing nanometer column tungsten, its characterization step is: by dc magnetron sputtering method, change the normal direction and the angle α that projectile flows of substrate, prepare nanometer column W film at the graphite substrate with the pure tungsten target as sputter.

2. the method for magnetically controlled DC sputtering according to claim 1, thus it is characterized in that reaching the tilt purpose of growth of crystal grain by the direction that changes substrate.

According to claim 1 with the method for 2 described magnetically controlled DC sputterings, generally be used for preparing various films, but mainly be electro-conductive material.

4. according to claim 1, the 2 and 3 described methods that prepare nanometer column crystal film, metal targets can be the metallic substance of the conduction such as W, Au, Ag, Ti, Cr.

5. according to claim 1, the preparation method of 2,3 and 4 described nano-crystal films, the preparation method can have any one in the method for manufacturing thin film such as method of method, sol-gel of method, the sputter of evaporation.

6. according to claim 1,2,3,4 and 5 described nanometer column crystals method, thin brilliant length dimension can make tens nanometers to several microns.

7. the described method for preparing nanometer column tungsten according to claim 1, preparations of nanomaterials can adopt the preparation methods such as chemical vapour deposition (CVD or PECVD), evaporation.

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