JP2903940B2 - Material for vapor deposition and method for producing the same - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a material for depositing Co, which is used in a process for producing a deposited VTR tape or the like.

[0002]

2. Description of the Related Art Co has recently been used particularly as a magnetic recording material for VTRs because of its excellent magnetic properties, that is, coercive force and residual magnetic flux density. Conventionally, the deposition method is 10 ^-5 ~
It is performed in a vacuum chamber evacuated to about 10 ^-6 Torr, and the deposition material in the crucible is heated to 2000 ° C. by an electron beam.
It was heated, melted and evaporated to a certain degree, and deposited on the base film. Here, the vapor deposition material must be replenished for the amount evaporated, but the replenishment is performed by about 10 mmφ × 10
A pellet of 〜30 mm or a bar material of 〜30-80 mmφ was used. In the case of pellets, they fall into the crucible melt,
In the case of a bar material, it is common to melt a part of the bar material and drop it into the molten metal to supply it.

[0003]

However, in any of the above-mentioned supply methods, in any case, the vapor deposition conditions become unstable due to replenishment of the surface of the vapor deposition material, scattering of the molten metal, and uneven temperature distribution in the molten metal. Hinders the production of tapes of stable quality.

[0004] As a countermeasure, it is conceivable that a long wire is used as the evaporating material, which is continuously supplied into a crucible to stabilize the vapor deposition conditions and produce a highly reliable tape.
In this case, there is also an advantage that a long-time continuous vapor deposition operation can be performed. Therefore, it has been desired to use Co as a wire.

However, since Co is a difficult-to-work material,
It is extremely difficult to increase the length by drawing or the like. For this reason, only the shapes such as the pellets and bar materials described above have been obtained, and there has been a problem that it is difficult to manufacture a magnetic tape with stable deposition conditions. The present invention has been made under such a technical background, and an object of the present invention is to provide a Co vapor deposition material having excellent workability and toughness so that stable vapor deposition conditions can be obtained.

[0006]

In order to achieve the above object, the vapor deposition material of the present invention is a metal comprising Co and unavoidable impurities and substantially 100% by weight of Co and having a diameter of 1.0 mm or more. , 10 mm or less, having a length of 1000 times or more of the diameter, and a tensile strength of 400 MPa or more, 150
It is characterized by having mechanical properties of 0 MPa or less, a draw of 5% or more, and an elongation of 5% or more (distance between gauges 100 mm).

[0007] The deposition material having such mechanical characteristics is Co.
And 100% by weight of Co
Metals, fcc (200), hcp (10
0) and the peak height (cps) of hcp (101) are f ₁ ,
Assuming that h ₁ and h ₂ , a crystal structure satisfying the equation of 0.1 ≦ f ₁ / (f ₁ + h ₁ + h ₂ ) ≦ 1 at room temperature can be obtained.

In the above-mentioned vapor deposition material, it is preferable to remove surface impurities by mechanical means such as surface grinding or chemical means such as pickling.

Further, the method of manufacturing the semiconductor device comprises the steps of adding a metal consisting essentially of Co and unavoidable impurities and containing substantially 100 wt% of Co to 40 wt.
At a temperature of 0 to 600 ° C., the cross-sectional reduction rate in one pass is 10
% Or more. After this processing,
It is preferable to cool at a rate of 0.1 ° C./s or more.

The reasons for limiting the characteristics of the vapor deposition material of the present invention will be described below. First, as for the composition, there is no added element in order not to impair the excellent magnetic properties of Co. Next, for the wire diameter, operability (ease of handling), supply speed, and the like are taken into consideration. That is, if it exceeds 10 mm, the handling of the wire is difficult, and the diameter of the winding coil becomes large, and the supply device itself becomes large. As a result, the peripheral equipment of the vacuum chamber is increased in size, and particularly when the supply device is provided in the vacuum chamber, a large space is required.

Conversely, if the thickness is less than 1.0 mm, handling is easy, but in addition to the problem of easy bending, high-speed supply is required. As a result of the high-speed supply, it is difficult to supply the liquid to a fixed position in the crucible, and problems such as a disorder of the molten metal surface are likely to occur. In addition, such a small diameter results in a large specific surface area and a large amount of surface impurities per unit weight.

[0012] In order to perform continuous operation, a length that is 1000 times or more the diameter is required.

[0013] On the other hand, regarding mechanical characteristics, this is also mainly in consideration of supplyability and operability. If the tensile strength is less than 400 MPa, the strength becomes insufficient, and conversely, 1500
If it exceeds MPa, it is hard and supply becomes difficult. Also, elongation,
If the aperture is less than 5%, it is also difficult to supply, as it is weak to bending and may cause breakage. More preferably, both are 1
0% or more.

The crystal structure has the above-mentioned crystal structure, so that it has the workability necessary for forming a wire and has the mechanical properties suitable for continuous supply (tensile strength: 400 MPa or more, drawing: 5% Above) can be obtained.

Furthermore, by removing surface impurities from such a deposition material by mechanical or chemical means,
A higher quality deposited film can be formed. In this case, if necessary, it is more effective to carry out washing with an organic solvent and a neutral detergent.

The manufacturing method is substantially 100 watts.
By processing t% of Co at the above-mentioned predetermined temperature and processing rate (cross-section reduction rate), a vapor-deposited material having the above-mentioned mechanical properties and crystal structure can be obtained.

[0017]

Embodiments of the present invention will be described below. (Example 1) First, substantially 100 wt% of Co was added to 1 in a vacuum melting furnace.
00 kg was produced. This is hot worked to reduce the diameter to 1
5,12,10,8,6,4,2,1,0.8,0.5
A wire having a length of at least 1000 times the diameter of each mm was manufactured. Then, it was actually supplied to a crucible in a vacuum chamber. As a result, 15 mm and 12 mm are too thick and very difficult to handle, resulting in poor workability.
Those with m and 0.8 mm were easy to handle, but could not be supplied stably due to bending during supply. On the other hand, other products could be supplied stably.

(Embodiment 2) Next, as in Embodiment 1, 100 kg of substantially 100 wt% Co was added in a vacuum melting furnace.
It was manufactured and hot-worked to produce a wire having a diameter of 5 mm. At this time, wires having various mechanical properties (tensile strength, elongation, drawing) were obtained by adjusting the processing conditions and the heat treatment conditions, and a supply test was performed in the same manner as in Example 1. The result is shown in FIG. As shown in FIG.
Those having a pressure lower than MPa were insufficient in strength and were broken. On the other hand, if the pressure exceeds 1500 MPa, the wire is hard and handling and supply are difficult. Unless the elongation (see FIG. A) and the constriction (see FIG. B) are each 5% or more, stable supply such as breakage during supply could not be achieved.

(Example 3) Further, a wire similar to that of Example 2 was manufactured, and its surface was mechanically ground and further washed with an organic solvent. The impurities on the surface of each wire before grinding, after grinding, and after cleaning were analyzed using EDS. As a result, many impurities including oxides were analyzed on the surface before grinding. After the grinding, the lubricant and the like at the time of the grinding were analyzed. Furthermore, no surface deposits were analyzed after washing with the organic solvent.

(Example 4) Co having a purity of 99.9% was converted to f ₁ / (f ₁ +) by changing processing conditions (processing temperature and degree of processing).
The value of h ₁ + h ₂ ) was varied, and the draw was measured by a tensile test at room temperature. Here, f ₁ , h ₁ , h ₂
Indicates peak heights (cps) of fcc (200), hcp (100) and hcp (101) in X-ray diffraction, respectively. The test results are shown in FIG. As shown, f ₁ / (f ₁ + h ₁ + h ₂
By controlling the value of ()) to 0.1 or more and 1.0 or less, it was confirmed that the drawing had good workability of 10% or more.

(Embodiment 5) Next, the same Co
In the above, working under different conditions (working temperature, working degree) was performed, and after cooling at a rate of 1 ° C./s, a tensile test was performed at room temperature to evaluate the drawing. The result is shown in FIG. In the same figure, × indicates that processing was impossible, Δ indicates that the drawing after processing was less than 10%, and ○ indicates 1
0% or more. As shown in the drawing, those subjected to processing at a processing temperature of 400 to 600 ° C. and a cross-sectional reduction rate of 10% or more showed a high aperture value, and it was confirmed that the workability was excellent.

(Embodiment 6) Further, the same Co
In the above, processing was performed at a processing temperature of 500 ° C. with different cross-sectional reduction rates, and a tensile test was performed at room temperature on a material obtained by changing the subsequent cooling rate, and the drawing was evaluated. The result is shown in FIG.
Shown in In the figure, ○ indicates the aperture of 10% or more,
Indicates less than 0%. As shown in the figure, even if the processing is performed at 500 ° C. with a cross-sectional reduction rate of 10% or more, the cooling rate after the processing is 0.1%.
If it is less than 1 ° C./s, the tensile properties (drawing) during the subsequent cold are low, and it was confirmed that the workability was not sufficient.

[0023]

As described above, according to the vapor deposition material of the present invention, continuous supply of Co wire is possible. As a result, deposition conditions, which have conventionally been a problem, have been stabilized, and continuous operation for a long time has become possible. For example, it is expected to be effectively used in the field of manufacturing VTR tapes and the like. Further, according to the production method of the present invention, it is possible to produce a vapor-deposited material that is easily formed into a wire in a cold state.

[Brief description of the drawings]

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 shows the results of testing the mechanical properties of a vapor deposition material, where (A) is a graph showing the relationship between elongation and tensile strength, and (B) is a graph showing the relationship between drawing and tensile strength. .

FIG. 2 is a graph showing a relationship between a crystal structure of a deposition material and an aperture value.

FIG. 3 is a graph showing a difference in an aperture value in a case where processings having different processing temperatures and cross-sectional reduction rates are performed.

FIG. 4 is a graph showing a difference in an aperture value when processing with different cross-sectional reduction rates is performed and a cooling rate after that is changed.

──────────────────────────────────────────────────の Continuation of the front page (51) Int.Cl. ⁶ identification code FI H01F 41/20 H01F 41/20 (58) Field surveyed (Int.Cl. ⁶ , DB name) C23C 14/00-14/58 C22C 19/07 C22F 1/10 G11B 5/85 H01F 10/16 H01F 41/20

Claims (5)

(57) [Claims] 1. A metal consisting essentially of Co and unavoidable impurities and containing 100% by weight of Co, having a diameter of 1.0 mm or more and 10 mm or less, a length of 1000 times or more of the diameter, and a tensile strength. A material for vapor deposition characterized by having mechanical properties of 400 MPa or more and 1500 MPa or less, an aperture of 5% or more, and an elongation of 5% or more (distance between gauges 100 mm). 2. A metal consisting essentially of Co and unavoidable impurities and containing 100% by weight of Co, and which is used in X-ray diffraction for fcc (200), hcp (100) and hcp (101).
Where f ₁ , h ₁ , and h ₂ are the peak heights (cps) of f ₁ , respectively, that a crystal structure that satisfies the expression 0.1 ≦ f ₁ / (f ₁ + h ₁ + h ₂ ) ≦ 1 at room temperature is obtained. Characteristic deposition material. 3. The vapor deposition material according to claim 1, wherein surface impurities are removed by mechanical means such as surface grinding or chemical means such as pickling. 4. A method of processing a metal consisting essentially of Co and unavoidable impurities and substantially containing 100 wt% of Co at a temperature of 400 to 600 ° C. and a cross-sectional reduction rate of 10% or more in one pass. Claims 1 through
3. The method for producing a vapor deposition material according to any one of 3 . 5. After processing at a temperature of 400 to 600 ° C. with a cross-sectional reduction rate of 10% or more in one pass, the temperature is reduced to 0.1 ° C.
Method for manufacturing a deposition material according to claim 4, wherein the cooling in / s or faster.