CN109136852B

CN109136852B - Method for plating tungsten film on metal-based lining

Info

Publication number: CN109136852B
Application number: CN201811178490.9A
Authority: CN
Inventors: 樊启文; 孟波; 胡跃明
Original assignee: China Institute of Atomic of Energy
Current assignee: China Institute of Atomic of Energy
Priority date: 2018-10-10
Filing date: 2018-10-10
Publication date: 2020-10-09
Anticipated expiration: 2038-10-10
Also published as: CN109136852A

Abstract

The invention belongs to the technical field of nuclear technology application, and discloses a method for plating a tungsten film on a metal-based liner. The method comprises two steps of plating a tungsten transition layer on metal vapor vacuum pulse arc ion implantation equipment and plating a tungsten deposition layer on single 90-degree bent tube filtering cathode vacuum pulse arc equipment. The method can plate a tungsten film with the thickness of thousands of nanometers and good bonding force with the metal substrate on the metal substrate.

Description

Method for plating tungsten film on metal-based lining

Technical Field

The invention belongs to the technical field of nuclear technology application, and particularly relates to a method for plating a tungsten film on a metal substrate.

Background

In the nuclear physics experiment process, a tungsten film is often used as a target nucleus of a nuclear reaction experiment and is required to be plated on a certain metal substrate. Common methods for plating such tungsten films include magnetron sputtering, focused heavy ion sputtering, chemical vapor deposition, and the like. Other impurities can be introduced in the chemical vapor deposition, so that the method is not suitable for nuclear targets with higher purity requirements; the binding force between the tungsten film deposited by magnetron sputtering and a metal-based liner, in particular to a titanium-based liner is poor, and the tungsten film can obviously fall off when the thickness of the tungsten film reaches more than 500 nm. Therefore, a plating method with good bonding force between the tungsten film and the metal substrate is required to be found.

Disclosure of Invention

Objects of the invention

According to the problems existing in the prior art, the invention provides a preparation method of a tungsten film, which has the thickness of thousands of nanometers and good bonding force with a metal-based liner.

(II) technical scheme

In order to solve the problems existing in the prior art, the invention is realized by the following technical scheme:

a method of plating a tungsten film on a metal-based substrate, the method comprising the steps of:

(1) tungsten-plated transition layer

Placing the pretreated substrate into metal vapor vacuum pulsed arc ion implantation equipment (MEVVPA); adjusting the trigger voltage of the pulse MEVVPA ion source to be 6-8 KV, the trigger current to be 20-30A and the trigger pulse width to be 6-8 us; the main arc voltage is 80-100V, the main arc current is 85-100A, and the main arc pulse width is 1.2-1.6 ms; injecting high voltage of 30-50 KV and injected beam current of 5-7 mA; the injection count is 500-1000 mC; the purpose of this step is to make a tungsten transition layer on the metal substrate;

(2) preparation of tungsten deposit

Placing the metal-based liner plated with the transition layer obtained in the step (1) into single 90-degree bent pipe Filtering Cathode Vacuum Pulsed Arc (FCVPA) equipment; adjusting the pulse trigger voltage to be 6-8 KV, the trigger current to be 25-35A and the trigger pulse width to be 6-8 us; the pulse arc voltage is 150-180V, the pulse arc current is 20-40 mA, and the arc pulse width is 2.5-3 ms; the deflection voltage is 20-40V; the deflection current is 2.1-2.3A; a base liner bias voltage of 80V; the deposition count is 2C-1000C to obtain a tungsten film with a thickness of several nanometers to several thousands of nanometers.

Preferably, the material of the metal substrate is titanium, stainless steel or copper.

Preferably, in the step (1), the trigger voltage of an ion source in the metal vapor vacuum pulse arc ion implantation equipment is adjusted to be 7KV, the trigger current is 25A, and the trigger pulse width is 6 us; arc pulse width 1.2 ms; injecting high voltage of 50KV and beam current of 5 mA.

Preferably, in the step (2), the pulse trigger voltage is 6KV, the trigger current is 30A, and the trigger pulse width is 6 us; the pulse arc voltage is 150V, the pulse arc current is 20mA, and the arc pulse width is 2.5 ms; a deflection voltage of 20V; the deflection current is 2.1A.

(III) advantageous effects

According to the method provided by the application, the MEVVA and FCVPA equipment is used in a combined mode to prepare the tungsten film, particularly the tungsten film with the thickness more than 500nm, on the metal substrate in a two-step mode, the tungsten film is prevented from falling off from the substrate due to the fact that the required tungsten film is too thick in the preparation process, and the success rate of preparing the tungsten film is up to 100%. The method comprises the following steps that the first step is carried out on MEVVA equipment, a small amount of plasmas are generated on the surface of a cathode by adjusting trigger voltage between a trigger electrode and the cathode, the plasmas are rapidly diffused, cathode vacuum arc discharge is generated through a main arc power supply loop between the cathode and an anode, after the pulse of a main arc power supply is finished, the plasmas are triggered again to generate next arc discharge, and the first step is to prepare a tungsten transition layer with the thickness ranging from 5 nm to 10 nm. The second part is to plate a tungsten film with the required target thickness on a tungsten transition layer by using FCVPA equipment, and the specific principle is to generate plasma by using FCVPA discharge, guide the plasma to move to a target chamber substrate through a curved magnetic field, and filter liquid drops or large particles generated by pulse arc discharge so as to realize the deposition of a high-quality tungsten film. The step avoids the shedding phenomenon caused by directly adopting a filtered cathode vacuum pulse arc plasma pulse arc or other methods (such as focused heavy ion sputtering and magnetron sputtering) to prepare a thicker tungsten film.

Detailed Description

The present application will be further described with reference to specific embodiments.

Example 1

(1) tungsten-plated transition layer

(2) preparation of tungsten deposit

The metal-based lining is stainless steel.

The process is stable and reliable, the binding force between the plated tungsten film and the titanium foil is good, and the experimental requirements are completely met.

Example 2

Unlike example 1, the material of the metal-based liner was titanium. In the step (1), the trigger voltage of an ion source in the metal vapor vacuum pulse arc ion implantation equipment is adjusted to be 7KV, the trigger current is adjusted to be 25A, and the trigger pulse width is adjusted to be 6 us; arc pulse width 1.2 ms; injecting high voltage of 50KV and beam current of 5 mA.

In the step (2), the pulse trigger voltage is 6KV, the trigger current is 30A, and the trigger pulse width is 6 us; the pulse arc voltage is 150V, the pulse arc current is 20mA, and the arc pulse width is 2.5 ms; a deflection voltage of 20V; the deflection current is 2.1A.

Example 3

Unlike in example 1, the material of the metal-based liner is copper.

Claims

1. A method for plating a tungsten film on a metal substrate is characterized in that the method belongs to the technical field of nuclear technology application, and comprises the following steps:

(1) tungsten-plated transition layer

Placing the pretreated substrate into metal vapor vacuum pulse arc ion implantation equipment; adjusting the trigger voltage of the pulse ion source to be 6-8 KV, the trigger current to be 20-30A and the trigger pulse width to be 6-8 us; the main arc voltage is 80-100V, the main arc current is 85-100A, and the main arc pulse width is 1.2-1.6 ms; injecting high voltage of 30-50 KV and injected beam current of 5-7 mA; the injection count is 500-1000 mC; the step can obtain a tungsten transition layer on the metal substrate;

(2) preparation of tungsten deposit

Placing the metal substrate lining plated with the transition layer obtained in the step (1) into single 90-degree bent pipe filtering cathode vacuum pulse arc equipment; adjusting the pulse trigger voltage to be 6-8 KV, the trigger current to be 25-35A and the trigger pulse width to be 6-8 us; the pulse arc voltage is 150-180V, the pulse arc current is 20-40 mA, and the arc pulse width is 2.5-3 ms; the deflection voltage is 20-40V; the deflection current is 2.1-2.3A; a base liner bias voltage of 80V; the deposition count is 2C-1000C to obtain a tungsten film with a thickness of several nanometers to several thousands of nanometers.

2. The method of claim 1, wherein the metal substrate is made of titanium, stainless steel or copper.

3. The method for plating the tungsten film on the metal substrate according to the claim 1, wherein the trigger voltage of the ion source in the metal vapor vacuum pulse arc ion implantation equipment is adjusted to 7KV, the trigger current is 25A, and the trigger pulse width is 6us in the step (1); arc pulse width 1.2 ms; injecting high voltage of 50KV and beam current of 5 mA.

4. The method for plating the tungsten film on the metal substrate according to claim 1, wherein in the step (2), the pulse trigger voltage is 6KV, the trigger current is 30A, and the trigger pulse width is 6 us; the pulse arc voltage is 150V, the pulse arc current is 20mA, and the arc pulse width is 2.5 ms; a deflection voltage of 20V; the deflection current is 2.1A.