JPH0325508B2 - - Google Patents

Description

[Detailed Description of the Invention] <Industrial Application Field> The present invention relates to an evaporation source device for generating a large amount of steam flow for applying ion plating treatment to a long plate to be treated, particularly a unidirectional silicon steel plate. It is.

<Prior art and its problems> In recent years, remarkable development efforts to improve the electrical and magnetic properties of unidirectional silicon steel sheets, especially to meet the extreme requirements of reducing iron loss, are gradually bearing fruit. However, as a serious damage caused by the implementation, when unidirectional silicon steel sheets are subjected to so-called strain-relief annealing after processing and assembly, they will not suffer from deterioration of characteristics. It has been pointed out that there are disadvantages due to restrictions on how it can be used.

This specification relates to new manufacturing equipment that can advantageously meet the above requirements, whether or not after undergoing a high temperature thermal history such as strain relief annealing, particularly equipment for bulk deposition during ion plating. This is explained below.

As is well known, unidirectional silicon steel sheets are products in which secondary recrystallized grains are integrated in the (110) [001], or Goss, orientation, and are mainly used as iron cores for transformers and other electrical equipment. electricity,
As for magnetic properties, products are required to have high magnetic flux density (represented by B ₁₀ value) and low iron loss (represented by W _17/50 value).

This unidirectional silicon steel plate is manufactured through a wide variety of complicated processes, but numerous inventions and improvements have been made so far, and today products with a thickness of 0.3 mm have magnetic properties of B ₁₀ : 1.90T or more, W _{17 /50} : 1.05W/
Kg or less, and the magnetic properties of products with a plate thickness of 0.23 mm are
Ultra-low core loss unidirectional silicon steel sheets with B ₁₀ : 1.89T or more and W _17/50 : 0.90W/Kg or less are being manufactured.

In particular, recently there has been a marked increase in the demand for reducing power loss as a top priority from the standpoint of energy conservation. The ``evaluation'' (iron loss evaluation) system is becoming widespread.

Under these circumstances, recently, research has been conducted to introduce micro-strain locally by irradiating the surface of a unidirectional silicon steel sheet after final annealing with a laser in a direction approximately perpendicular to the rolling direction to subdivide the magnetic domains and thereby reduce iron loss. (See Japanese Patent Publication No. 59-2252, Japanese Patent Publication No. 57-53419, Japanese Patent Publication No. 58-26405, and Japanese Patent Publication No. 58-26406).

This magnetic domain refining technology is effective for transformer materials for laminated cores that are not subjected to strain relief annealing, but in materials for wound core transformers that are subjected to strain relief annealing, the local minute strain introduced by laser irradiation is Since the annealing process opens the magnetic domain width and widens it, there is a drawback that the laser irradiation effect is lost.

Recently, the present inventors have succeeded in manufacturing an ultra-low core loss unidirectional silicon steel sheet that does not suffer from the deterioration of properties during the above-mentioned high temperature treatment (Japanese Patent Application No. 1381/1981). In other words, this manufacturing method involves removing oxides on the surface of a grain-oriented silicon steel sheet that has been finish annealed, or polishing it to a mirror-like state, and then ion plating Ti, Zr, V, Nb, Ta, Cr, Mo, W, Mn,
Forming an ultra-thin tensile coating made of at least one selected from nitrides and/or carbonates of Co, Ni, Al, B, and Si and oxides of Al, Ni, Cu, W, Si, and Zn. It was discovered that it is possible to reduce iron loss in unidirectional silicon steel sheets.

The present invention deals with long and wide plates, particularly after removing oxides on the surface of a grain-oriented silicon steel plate that has been finish annealed based on the above-mentioned method, or by polishing the steel plate surface using a continuous line to create a mirror-like surface. The present invention relates to a series of continuous processing equipment that immediately forms ultra-thin tensile coatings of the carbides, nitrides, and oxides by ion plating after the oxidation process.

Conventionally, a method for vacuum-depositing Zn, etc. on the surface of a steel plate in a continuous line is disclosed in Japanese Patent Application Laid-Open No. 158379/1983. Normally, in order to uniformly evaporate a wide plate-shaped object, it is necessary to use a crucible corresponding to each crucible, but if the evaporation surface is not made uniform in terms of temperature distribution, the amount of evaporation may change in position. In particular, a uniform deposited film cannot be obtained across the width of the plate. In addition, regarding the evaporation of melted materials, Zn, which has a high vapor pressure,
Limited to substances with a low melting point such as Al, which have a high melting point,
There was no development at all regarding the vapor deposition of metals such as Ti, which have low vapor pressure. Especially when the plate to be treated is wide,
The technology for continuous ion plating at relatively high line speeds has remained a research topic for a long time.

The present inventors have discovered that in order to manufacture ultra-low core loss electrical steel sheets on a continuous line by forming an ultra-thin tensile film such as TiN on the surface of the steel sheet, a large amount of
As a result of numerous research experiments based on the recognition that it is important to generate a Ti vapor flow, we have found that the following conditions must be met in order to manufacture ultra-low core loss unidirectional silicon steel sheets. made clear that it was necessary.

In other words, when continuously ion plating an ultra-thin tension film (0.5 μ thick) such as TiN, if it is formed at a line speed of 50 m/min, if the width of the object to be deposited is 2 m, the deposition rate will be as short as 25 μ/min. It is necessary to adhere a large amount in time.

As a result of various studies based on the above basic points, we found that it is possible to continuously mass-produce ultra-low core loss unidirectional silicon steel sheets by forming a tension coating using a method different from conventional methods. They discovered this and completed the present invention.

<Object of the Invention> Therefore, the object of the present invention is to solve the above-mentioned drawbacks of the prior art and to provide a large amount of steam for forming a uniform vapor deposition film on a long and wide object to be treated, especially a unidirectional silicon steel plate. The present invention aims to provide an evaporation source device for stream generation.

<Structure of the Invention> That is, the present invention provides an evaporation source device for a high vacuum ion plating apparatus that continuously performs ion plating on the surface of a long and wide plate to be processed. at least one electron beam generator for simultaneously irradiating the melted and evaporated material in the crucible linearly over the length of the crucible;
The present invention provides an evaporation source device for generating a large amount of vapor flow, which is characterized by comprising:

The invention will be explained in detail below with reference to the accompanying drawings.

Figure 4 shows a schematic diagram of the ion plating method using a conventional 270° deflected electron beam {Co-authored by Siegfried Schiller and Ulrich Heisitzig (translated by Nippon Vacuum Technology Co., Ltd.), Vacuum Deposition, May 1, 1983. Publication date, see page 50}.

In FIG. 4, 40 is an evaporation material crucible, 41
is a cathode, 42 is an accelerating electrode, 43 is an electron beam, 44 is a cooling means, 45 is an electrode 46, and a winding 47
and a deflection magnet consisting of a core 48, 4
9 is a steam flow, 50 is N ₂ gas, and 51 is a substrate.

This ion plating method using an electron beam is optimal for depositing on small batch-type substrates, but it requires a continuous line to deposit a large amount of material, and it is not possible to deposit uniformly across the width of the steel sheet.

For this reason, a continuous ion plating apparatus as shown in FIG. 1 has been developed. The present invention provides an evaporation source device that can perform ion plating uniformly in the width direction of a long and wide plate to be processed using such a device and in a short time.

To briefly explain this Fig. 1, 1 is a coil of grain-oriented silicon steel finish annealing plate after MgO on the surface has been removed, 21 is a shear, 3 is a pickling tank, 4 is a cleaning tank, 5 is a first Electrolytic tank, 6 is a second electrolytic tank, 7 is a cleaning tank, 8 is a drying tank, 9 is a looper, 10 is a high vacuum processing tank, 11, 11', 11'' is a preliminary evacuation tank before ion plating, 12 is a High vacuum exhaust, 13
is a gas inlet, 14, 14', 14'' is a preliminary exhaust tank after ion plating, 15 is an evaporation source, 16
18 is a coil after ion plating, 19 is an ion bombardment and preheating tank, and 20 is an ultrasonic cleaning and drying tank.

In the high vacuum ion plating apparatus shown in Fig. 1, which performs continuous ion plating, a steel plate is passed vertically, and evaporation sources are provided on both sides of the steel plate, so that ion plating is performed on both sides of the steel plate at the same time. Also good. Usually for dissolving evaporated materials
A 270° deflection electron beam is used, but since the vapor of the melted evaporated material is isotropically dispersed, very few evaporated atoms adhere to the steel plate, and 1
Even if the evaporation atoms are accelerated using the ionization electrode No. 6, the evaporation efficiency is low. Therefore, in such continuous ion plating equipment, the important issue is how to generate a large amount of evaporation atomic vapor flow from the evaporation source and uniformly plate ions across the width direction of the steel plate in the passing plate. It is.

FIG. 2 shows a schematic diagram of the evaporation source of the continuous ion plating apparatus 15 shown in FIG. In order to generate ion plating, uniform ion plating is performed in the width direction of the steel plate by using a device 34 that generates an electron beam 33 that simultaneously irradiates linearly over the length of the crucible using a magnetic field. be able to.

In addition, in order to deposit a large amount on the steel plate being passed, it can be achieved by using an electron beam generator that simultaneously irradiates multiple linear electron beams, as shown at 34a, 34b, 34c, and 34d in Figure 3. . This linearly radiated polarized beam is
By deflecting from 220 to 280 degrees, it is possible to vary the steam flow and also to generate a large amount of steam flow.

By newly introducing the steam source device for generating a large amount of steam flow according to the present invention into such continuous ion plating, it is possible to continuously perform ion plating treatment by mass deposition.

Further, this evaporation source device that generates a large amount of vapor flow can also be used for general ceramic coating of low carbon cold rolled steel sheets, stainless steel sheets, etc.

<Example> A description will be given based on a specific example using the evaporation source device of the present invention.

After finish annealing of unidirectional silicon steel plate (0.23mm thickness)
A coil (width 1000 mm, weight 7 tons) from which MgO was removed was used. Using continuous ion plating as shown in Figure 1, a 0.8 μm thick TiN tension film was formed on the surface of the steel plate at a line speed of 35 m/min. At this time, the length of the melt storage part of the crucible was 1200 mm, the linear irradiation width of the electron beam was 1200 mm, and a total of 4 electron beam generators were installed in the third It was used in the same way as in the figure.

The coating is uniform in both the length and width directions of the steel plate,
The magnetic properties at that time were as follows.

B ₁₀ = 1.92T, W _17/50 = 0.63W/Kg <Effects of the Invention> The present invention is equipped with a crucible for accommodating an evaporated material having a length greater than the width of the object to be processed, and the melting part in the crucible is The present invention provides an apparatus for ion plating a long and wide workpiece, which has at least one electron beam generating device that simultaneously irradiates linearly over its length.

According to this device, even when processing a wide material, 1
Since steam is supplied from multiple linear locations along the length of the two long crucibles, steam is supplied uniformly over the entire width of the object to be processed, and the beam polarization angle of the electron beam generator or the number thereof can be adjusted. This allows the amount of steam to be adjusted freely.

When this apparatus is applied to the vapor deposition of unidirectional silicon steel sheets, the unidirectional silicon steel sheets with better properties can be obtained.

[Brief explanation of drawings]

FIG. 1 is a schematic diagram of a continuous ion plating line. FIGS. 2 and 3 are schematic diagrams showing an example of the configuration of the evaporation source for generating a large amount of steam according to the present invention. FIG. 4 is a schematic diagram of a conventional ion plating apparatus. Explanation of symbols 1, 18...Coil, 3...Pickling layer,
4, 7... Washing layer, 5, 6... Electrolytic layer, 8... Drying layer,
9,9′...looper, 10...high vacuum processing layer, 11,
11', 11'', 14, 14', 14''...Preliminary exhaust layer, 12...High vacuum exhaust, 13...Gas inlet, 15
...Evaporation source, 19...Ion bombardment and preheating tank, 16...Ionization electrode, 17...Guide roll,
20... Ultrasonic cleaning and drying tank, 21... Shear,
31... Melting and evaporating material, 32... Crucible, 33... Electron beam, 34... Electron beam generator, 40... Crucible, 41... Cathode, 42... Accelerating electrode, 43... Electron beam, 44... Cooling device, 45... Polarizing magnet, 46... Electrode, 47... Winding wire, 48... Core, 49
...vapor flow, 50... _N2 gas, 51...substrate.

Claims (1)

[Claims] 1. An evaporation source device of a high vacuum ion plating apparatus that continuously performs ion plating on the surface of a long and wide plate to be processed, comprising an evaporation material containing crucible having a length equal to or longer than the width of the plate to be processed,
An evaporation source device for generating a large amount of vapor flow, comprising at least one electron beam generator that simultaneously irradiates the melted and evaporated material in the crucible linearly over the length of the crucible.