JPH01298155A - Magneto-optical recording medium, sputtering target, and manufacture of sputtering target - Google Patents

Abstract

PURPOSE:To obtain a target for manufacturing a magneto-optical recording medium causing no component distribution within a film-forming plane by placing a powder of transition metal and an ingot of rare earth-transition metal alloy into a mold, heating the inside of the mold at a temp. between respective melting points of both, cooling the above, and then working the resulting formed body. CONSTITUTION:A powder of transition metal, such as Fe and Co, and an ingot of an alloy of rare earth element, such as Nd and Dy, and the transition metal are placed into a mold. The inside of the mold is heated at a temp. between the melting points of both and then cooled. The resulting formed body is worked into a sputtering target. By using this target, a magneto-optical recording medium in which a magneto-optical recording film exists on a transparent substrate is manufactured. This target has a structure consisting of three phases of a simple-substance phase of rare earth metal, a simple-substance phase of transition metal, and a rare earth-transition metal alloy phase. When this target is used, oxygen content is reduced and filling density is increased, and sputtering can be stabilized from the initial stage.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to the structure and composition of a sputtering target for rare earth transition metal alloys, and to a manufacturing method.

[Conventional technology]

Conventional sputtering targets for producing rare earth transition metal-based magneto-optical recording films include casting methods, sintering methods, and semi-melting methods. The casting method referred to here is a method in which the cast ingot is used as a target by external diameter processing, and the sintering method is a method in which the cast ingot is crushed and sintered to form a target shape. It is. Also, the semi-melting method is described in Japanese Patent Application Laid-Open No. 1986-1995.
No. 788 and JP-A-61-99640.

[Problem to be solved by the invention]

However, the above-mentioned sintering method is not suitable for rare earth transition metal systems which inherently contain a large amount of oxygen (2000 ppm is the limit) and are easily oxidized. On the other hand, the casting method is preferable because it has a small amount of oxygen (approximately 500 ppm), but it has the problem that compositional distribution occurs within the film-forming surface.

In addition, targets made by the semi-melting method have the advantage that compositional distribution is less likely to occur within the substrate surface, but since the semi-melting method is also basically manufactured by sintering, the target is completely dense. The voids are continuous to the inside of the target, and if the target is left in the atmosphere, oxidation will progress from the surface to the inside of the target, resulting in an oxide layer that cannot be cleaned by preliminary sputtering. It ends up.

The present invention is intended to solve these problems, and its purpose is to overcome the drawback of conventional cast alloy targets that compositional distribution occurs within the film formation surface, and also to It is an object of the present invention to provide rare earth transition metal targets and various methods for producing the same, which overcome the disadvantage of oxidation susceptibility of process targets.

[Means to solve the problem]

(1) In a cast alloy target for producing a magneto-optical recording layer made of a rare earth-transition metal alloy by sputtering, the metal structure in the cast alloy target is a rare-earth total bending phase, a transition metal simple phase, and a rare-earth-transition metal alloy phase. It is characterized by consisting of.

(2) The main composition of the Couget for sputtering is at least one light rare earth metal (LR) among Sm, Nd, Pr, and Ce, and at least one heavy rare earth metal among Gd, Tb, and Dy. (HR), and further contains at least one transition metal (TM) among Fe and Co.

(3) The main composition of the sputtering target includes at least one heavy rare earth metal (HR) among Gd, Tb, and Dy, and at least one transition metal (TM) among Fe and Co. It is characterized by

(4) The sputtering target is made by placing a transition metal powder and a rare earth transition metal alloy ingot into a mold, heating the inside of the mold to a temperature between the melting point of the transition metal and the melting point of the ingot, and then cooling it. It is characterized in that it is produced by processing a molded body made of

(5) For the sputtering target, a foamed transition metal sheet and a rare earth transition metal alloy ingot are placed in a mold, and the inside of the mold is heated at a temperature between the melting point of the transition metal sheet and the melting point of the ingot. , and is characterized in that it is produced by processing a molded body that is then cooled.

(6) A sputtering target is placed in a mold as a mixed powder of a transition metal powder and a rare earth transition metal alloy powder, and the inside of the mold is heated to a melting point between the transition metal and the rare earth transition metal alloy. It is characterized in that it is produced by processing a molded body that is then cooled.

(7) The sputtering target has a porosity of 30
% or more and 80% or less of transition metal powder.

(8) The sputtering target has a porosity of 30
% or more and 80% or less of a foamed transition metal sheet.

(9) A method for producing a sputtering target, characterized in that the transition metal powder has an average particle size of 10 μm or more and 3.0 μm or less.

QO) In the method for manufacturing a sputtering target, the average pore diameter of the foamed transition metal sheet is 10μ.
It is characterized by having a length of not less than m and not more than 3.0 mm.

(11) In the method for manufacturing a sputtering target, the composition of the ingot of rare earth transition metal is such that the melting point is 1200°C.
It is characterized by using the ingot having the following composition.

(+23) A method for producing a sputtering target is characterized in that the molded body is heat treated.

(13) In a magneto-optical recording medium in which at least one dielectric film and at least one magneto-optical recording film are present on a transparent substrate, the sputtering target according to item 1, 2 or 3 is used. It is characterized by being manufactured using

[Effect]

In the case of the composite target method conventionally used in laboratories, in which rare earth metal (RE) chips are arranged on a transition metal (TM) target to form a film, the composition distribution within the substrate plane is opposite to that of a cast alloy target. It shows the tendency of

In other words, in the case of a composite target, the more directly above the target there are, the more RE there are, and the sides have more TM.

On the other hand, in the case of a cast alloy target, there are more TMs directly above the target, and there are more REs on the sides. It can be seen that there is a complementary relationship between the flight of RE and TM sputter particles in the cast alloy target and the composite target.

In other words, if a target containing an appropriate mixture of RE single phase, TM single phase, and RE-7M alloy phase is created, it becomes possible to form a uniform film without compositional distribution within the substrate surface.

The following two methods are mainly considered as manufacturing methods for creating a target with a packing density of 100% that is difficult to oxidize.

One method is to mix RE grains and 7M grains by placing them in a RE-TM alloy bath with a low melting point. Another method is to disperse TM powder (sheet) in an RE-TM alloy bath in which an RE single phase appears during solidification. What is common to both is that the RE-TM alloy bath completely surrounds the powder or sheet, and the resulting compact does not have the microscopic pores found in fired crystals. Even if the pores of the product of the present invention exist, they are like cavities found in cast products, and the pores themselves are not connected, so that surface oxidation does not progress to the inside.

[Example 1-1] First, an NdDy ingot with N d Z:lD y t7at% is prepared as a raw material, and the ingot is crushed to have an average particle size of about 500 μm to produce NdDy powder. And F
A FeCo ingot with eso, sCO+q, sat% is made, and the ingot is crushed to have an average particle size of 200 μm to make FeCo powder.

Then N d +o, oD )' ss, oF e aa
, oCO++, bat%, Nd,
Dy, Fe, and Co are introduced, the temperature is raised once to 1550″C to completely dissolve, and then the temperature is lowered to 1200°C.

Then, in this NdDyFeCo molten alloy, the above N
dDy powder and FeCo powder were put into a crucible.

This NdDy has a melting point of 1400'C, and FeC0
Since the temperature is 1530°C, they will not dissolve in hot water at 1200°C, so NdDy and FeCo will exist as powders. And these NdDyFeCo, NdDy,
FeCo1 has the following proportions.

(NdDyFeCo)A ((NdDy)c (Fe
Co)D)B A:B=25: 75wt% C:D=28: 72at% (NdDyFeCo)-(NdDy
)-(FeCo)? -117? Figure 1 shows a schematic diagram of the surface texture of a 4"φ x 6 sputtering target. Phase 1 is (NdD)')ff3(FeCo). )6.
3 is an at% composition phase, this phase is a FeCo composition phase, and 3 is an NdDy composition phase. In other words, the RE single phase of NdDy, the TM single phase of FeCo, and the RE-
It can be seen that it consists of three phases: TM alloy phase.

This NdDyFeCo target was installed in a sputtering apparatus as shown in FIG. 2, and a film was formed to examine its magnetic properties and composition distribution. 21 in FIG. 2 is a sputtering target, and 22 is a substrate holder (300φ). Film forming conditions are Ar pressure 2.5 mTorr, initial vacuum degree 3.
X10-'T.

rr, power was supplied at 1°0A340■ using a DC power supply. FIG. 3 is a diagram showing the composition distribution and magnetic property distribution in the substrate holder using the target of the present invention. As shown in this figure, the composition is uniform with an RE of 28.0 to 28.5 at%, and the magnetic properties are also uniform with an Hc of 9.7 to 10.5 KOe. A nearly uniform film was formed inside the substrate holder. Naturally, since this target was a cast alloy, the amount of oxygen was small, 350 ppm.

A magneto-optical recording medium was produced by sputtering using the target of the present invention. A structural diagram of the medium is shown in FIG.

351 is a polycarbonate board, 352 is AfS
The iN dielectric film 353 is an N dielectric film prepared using the target of the present invention.
dDyFeCo film, 354 is Af! It is a SiN dielectric film. This medium has a linear velocity of 5.7 m/sec, Doma i
A very high C/N value of 59 dB was obtained with an n length of 1.4 μm, and in a reliability test, no pitting corrosion occurred for as long as 3,000 hours under constant temperature and humidity at 90"C and 90% RH. Ta.

On the other hand, for comparison, NdDyFeCo was manufactured using the conventional manufacturing method.
Created a target. That is, the entire composition of NdDyFeCo was melted in a Ruhozu at 1500°C, and poured into a mold to form an ingot. After that, the ingot was cut and polished to 4″φ
A 6t NdDyFeCo target was created. FIG. 4 is a schematic diagram of the surface structure of this target.

41 is (Ndo, +zD)'o, gs)zs (F e
o,eC.

o, z) vsa t% composition phase, 42 is (N do, J
)'0.7) ss, 3(F eo, s COo, z)
hb, tat% composition phase.

That is, both phases are NdD'FeCo alloy phases.

Overall Ndb, s D>'21.5F esscO1
The composition was 4 at%. A film was formed using this target using a spanking device shown in FIG. FIG. 5 shows a diagram of the composition distribution and magnetic property distribution in the substrate holder using a casting base NdDyFeCo target produced by this conventional manufacturing method. As shown in this figure, the composition has an RE of 29.8 to 26.
At 8at%, the closer you go to the center of the substrate holder, the more RE there is.
Conversely, RE decreases toward the outer periphery of the holder.

In addition, the magnetic properties are such that Hc is 12 to 6 KOe, and Hc increases toward the center of the holder. This also agrees with the composition distribution.

A magneto-optical recording medium was created by sputtering using this conventional target. The structure of the medium is the same as that shown in FIG. 35, in which the magneto-optical recording layer is sandwiched between A, f2 SiN dielectric films. This medium has a linear velocity of 5.7 m/
sec Domain length 1.4μmT:c/N55d
It was a slightly low value of B. This is an effect of the composition distribution within the medium. In the reliability test, 90℃90%RH
No pitting corrosion occurred even after 3000 hours at constant temperature and humidity.

Furthermore, for comparison, NdDyF by the semi-melting method shown in JP-A-61-95788 and JP-A-61-99640
An eCo target was prepared and film formation was evaluated. The target composition is Ndb,s D3'! +, 5FesscO+4a
t%, NdDy, NdDyFeCo, FeCo1
is the same as above. The amount of oxygen in this target is 150
It was 0 ppm. This target was installed in the sputtering apparatus shown in FIG. 2, and preliminary sputtering was sufficiently performed to form a film after the target surface was in a sufficiently clean state. The film forming conditions are the same as described above. FIG. 6 shows the composition distribution and magnetic property distribution in the substrate holder using a semi-molten NdDyFeCo target. Although the composition distribution is comparable to that of the target of the present invention shown in FIG. 3, it can be seen that the magnetic property distribution is generally shifted in the direction of smaller coercive force (Hc).

This is a phenomenon that occurs because the semi-molten target has a higher amount of oxygen than the target of the present invention because it is sintered, and the rare earth metal is partially oxidized by oxygen.

Using this semi-molten target, a magneto-optical recording medium was created by sputtering. The structure of the medium is the same as that shown in FIG. 35, and the magneto-optical recording layer is made of AI! , a SiN fused composite film is used. This medium has a linear velocity of 5.7 m/sec
c, Domain length was 1°4 μm, and the C/N was 57 dB, which was a slightly low value.

This is because oxygen in the Couget was also taken into the film. In addition, in the reliability test, 90℃90%RH
Pitting corrosion occurred from the 200th hour under constant temperature and humidity, and Err.
or Rate started to deteriorate. This is also because oxygen in the target was taken into the film.

The above-mentioned NdDyFeCo target of the present invention and semi-? The NdDyFeCo target was removed after sputtering, and both targets were left in the atmosphere for 24 hours. The rear target was again attached to the sputtering apparatus shown in FIG. 2, and film formation was attempted.

Table 1 shows the discharge state during sputtering.

Table 1 As shown in the above table, the target of the present invention maintained the DC sputtering Ar pressure of 2.5 mTorr from the initial stage, and the discharge was very stable, but the semi-molten target could not be DC sputtered at the initial stage. This is because the surface of the semi-molten target completely became an insulator because it was left in the atmosphere for a long time. After 1 hour, DC sputtering became possible, but the Ar pressure had to be set to 1Q mTorr, and DC sputtering became possible at 2.5 mTorr only after 7 hours.

FIG. 7 shows the relationship between the sputtering time and the magnetic properties of the films for both targets after being left in the atmosphere.

71 is a target according to the present invention, and 72 is a target made by a semi-melting method. As is clear from this figure, the target according to the present invention exhibits stable film characteristics immediately after sputtering even if it is exposed to the atmosphere for a long time. On the other hand, if a semi-molten target is exposed to the atmosphere for a long time, sputtering itself will be very difficult at the initial stage, and even after a long preliminary sputtering, the film properties will not be stable at all temperatures, and the film will By the time the characteristics stabilize, the number of targets will decrease and disappear. The magnetic properties of the films shown above are based on the compensation composition,
Since the composition (characteristics) is on the TMrich side, the coercive force (H
The larger c) means better film properties.

Next, we investigated how much exposure of the semi-molten target to the atmosphere would affect the film properties. After the target has been sufficiently cleaned by preliminary sputtering and the H characteristics have stabilized, the target is removed and placed in the atmosphere for 10 minutes.
Minutes, 30 minutes, 1 hour.

It was left for 5 and 10 hours. Thereafter, an experiment similar to that shown in FIG. 7 was conducted to examine the dependence of the film magnetic properties on Svantha time. Figure 8 shows this. 81 was left in the atmosphere for 10 minutes,
82 was left in the atmosphere for 30 minutes, 83 was left in the atmosphere for 1 hour, 84 was left in the atmosphere for 5 hours, 85 was left in the atmosphere 1
It is from 0 hours. As is clear from the figure, if the target produced by the semi-molten method is left in the atmosphere for even 10 minutes, surface oxidation of the target occurs, which affects the film magnetic properties. It can be seen that the longer the exposure time in the atmosphere, the more oxidation from the target surface progresses, and the more severe the effect on the magnetic properties of the Tn film becomes.

These adverse effects of leaving the media in the atmosphere pose a major problem in terms of yield costs when mass producing magneto-optical recording media. The target according to the present invention is also highly effective in this respect.

The created medium has a substrate of A/2S on a PCr dielectric film.
jN was used, but in addition to the PC board, any material such as PMMA, APO, glass, etc. may be used.
The effect of the present invention was found with any dielectric film such as Na, SiC, AffSiNO, ZnS, etc.

[Example 1-2] Next, a PrTb ingot with a concentration of P rzzT b 7q a t% was prepared as a raw material, and PrT was ingot as in Example 1-1.
b Make powder. Similarly, F eso, sCOIq,
Make 5a t% powder.

Furthermore, P r+oTbssF e44cO11a t%
Each element is placed in a crucible so that the temperature is raised once to 1550°C to completely melt it, and then lowered to 1200°C. Then, the above PrTb powder and FeCo powder were added to this PrTbFeCo molten alloy into a crucible. This PrTb has a melting point of 1370°C and FeCo has a melting point of 1530°C, so it will not dissolve in hot water at 1200°C, so the PrTb powder and FeCo powder will exist as they are.

And these PrTbFeCo, PrTb, FeCo
The amounts are in the following proportions:

(PrTbFeCo)t ((PrTb)c (F
eCo)H)F E: F=25: 75wt% G:H-28 near 2at% (PrTbFeCo)-(PrTb
)-Example 1 using (FeCo) cast alloy target
As a result of evaluating the composition distribution and magnetic property distribution in the substrate holder using the same film forming apparatus and film forming method as in 1, the RE was 28.
Hc is 18.0 to 19.0 KOe at 0 to 28.5 at%
It was uniform. In addition, the amount of oxygen was as low as 380 PPM, and the sputtering discharge was stable from the beginning even after being left in the atmosphere for 24 hours, and the film magnetic properties were similarly stable from the beginning.

The effect of the present invention was also confirmed in the P r T b Fe Co Ml composition.

[Example 1-3] Next, a SmGd ingot with Smz: +Gd77at% is produced, and SmGd powder is produced. And similarly Fe.

Make Co, at% powder. Furthermore, Sm+aGdasF
Each element is placed in a crucible in such a manner that the amounts are eaq, sc Os, and sat%, the temperature is raised once to 1550°C to melt it completely, and then the temperature is lowered to 1200°C. Then, the above-mentioned SmGd powder and FeCo powder were added to this SmCydFeCo molten alloy into a crucible.

This SmGd has a melting point of 1270°C, and FeC0 has a melting point of 1270°C.
Since it is 530"C, it will not dissolve in hot water at 1200°C, so it will exist as SmGd powder and FeCo powder.And these SmGdFeCo, SmGd, F
The eCo amount has the following proportions.

(SmG d Fe Co) + ((SmG d) x (
F e C0) L) JI: J=25: 75wt
%: L = 28 near 2at% (Srr + C; dFeCo) - (S
mGd) (FeCo) cast alloy target, as in Example 1-1.1-2, was a target that allowed film formation without compositional distribution or magnetic property distribution within the substrate holder. Hc is 5-5.5KOe, RE is 28-28
．． It was uniform at 5 at%.

The amount of oxygen was 300 ppm, and the sputtering discharge was stable from the beginning even after being left in the atmosphere for 24 hours, and the film magnetic properties were also stable from the beginning.

The effect of the present invention was also confirmed with the SmGdFeCo composition.

[Example 1-4] Next, Ce ++, sP r ++, sD Y7 a t
% CePrDy ingot is made and CePrDy powder is made.

Then, F eso, sCO + q, sat t% powders were prepared in the same way, and Ces, o P rs, o D)'x
s, oF ea4. Each element is put into a crucible so as to be ocOz, oat%, the temperature is raised to 1550°C to completely dissolve, and then lowered to 1200°C. Then, the above CePrDy
The powder and FeCo powder were put into a crucible. This CeP
rDy has a melting point of 1350°c, and FeC0 has a melting point of 153
Since the temperature is 0℃, it will not dissolve in hot water at 1200℃, so C
ePrDy will exist as FeCo powder. And these CePrDyFeCo, CePrDy
, the amount of FeCo is in the following proportions.

((CePrDyFeCo)H((CePrDy)r(
FeCo). ) HM: N = 25: 75 wt%P: Q=
28: 72a t% (CePrDyFeCo)-(Ce
PrDy) (FeCo) casting alloy target is
As in Example 1-1.1-2.1-3, this target was able to form a film without causing compositional distribution within the substrate holder. In addition, the oxygen content was 420 ppm, and the sputtering discharge was stable from the beginning even after being left in the atmosphere for 24 hours.
The film magnetic properties were similarly stable from the beginning.

The effect of the present invention was also confirmed for the CePrDyFeCo composition.

In addition to the composition systems shown in Example 1-1.1-2.1-3.1-4, NdTbFeCo, NdGdFeCo,
NdDyFeCo, NdTbGdFe, NdTb
GdFeCo, NdDyGdFeCo, NdD
yGdTbFeCo, PrDyFeCo, Pr
GdFeCo, NdPrDyFeCo.

NdCeDyFeCo, NdTbCo, NdP
rCeDyFeCo, NdSmDyFeCo,
CeSmPrD)'FeCo, CePrNdDyT
bFeCo, CeNdPrDyGdFeCo, etc.
, at least one kind of light rare earth among Nd, Pr, and Ce, at least one kind of heavy rare earth among Gd, Tb, and Dy, and at least one kind of transition metal among Fe and Co. It was confirmed that the effects of the present invention existed for all composition systems including.

Next, an example will be described in which the target composition does not contain a light rare earth metal, that is, it contains a heavy rare earth metal (HR) and a transition metal (TM).

[Example 2-1] First, Tb powder with an average particle size of about 300 μm was prepared as a raw material, and F eqzc O? a t% of FeCo
The ingot is crushed to an average particle size of about 150μm, and F
Make eCo powder.

Next, it is placed in a crucible in a vacuum so that Tb4sF es+cOs a t% is obtained, the temperature is raised once to 1650°C to completely melt, and then the temperature is lowered to 1200°C.

Then, the above-mentioned Tb powder and FeCo powder were added to this TbFeCo molten alloy into a crucible.

Tb has a melting point of 1450°C, and FeCo has a melting point of 1530°C.
Therefore, Tb does not dissolve in hot water at 1200°C.
, it will exist as FeCo powder. And these T b Fe Co , T b, Fec
oi has the following proportions.

(T b F e Co) A(T bc(F e Co
) o) aA:B=25: 75wt% C:D=22 near 8at% (TbFeCo)-Tb-(FeC
o) The molten metal was poured into a mold, and the resulting cast alloy was then processed to create a 4" φ x 6t subinterning target. The surface structure of the target thus created was the same as that shown in Fig. 1, and the TbFeCo RE of
There were three phases: -7M alloy phase, RE single phase of Tb, and TM single phase of FeCo.

This TbFeCo target according to the present invention was mounted on the same sputtering apparatus as shown in FIG. 2 to form a film, and its magnetic properties and composition distribution were investigated. Film forming conditions are Ar pressure 2.5m
Torr, the initial vacuum level was 3 x 10-' Torr, and the input power was 1° OA and 340 cm using a DC power supply. FIG. 9 is a diagram showing the composition distribution and magnetic property distribution in the substrate holder using the target of the present invention. As shown in this figure, the composition is uniform with RE ranging from 22.0 to 22.5 at%, and the magnetic properties are also uniform with Hc ranging from 14.7 to 15.5 KOe. A nearly uniform film was formed inside the substrate holder. Naturally, since this target was a cast alloy, the oxygen content was low, at 350 ppm.

The magneto-optical recording medium produced using the target of the present invention is
A very high value of C/N 60 dB was obtained at a linear velocity of 5.7 m/sec and a Domain length of 1.4 μm. or,
In reliability tests, no pitting corrosion was observed even after 3000 hours at a constant temperature of 90°C and 90% RF.
There was also no increase in rate.

On the other hand, for comparison, a TbFeC0 target was produced using a conventional manufacturing method. That is, the total composition of TbFeC0 is T
bzzF e7sc Os a t% in a crucible at 1650'C? The mixture was melted and poured into a mold to form an ingot. Then, this ingot was cut and polished to 4"φ
A TbFeCo target of X6t was created. 10th
The figure shows the composition distribution and magnetic property distribution in the substrate holder using a cast alloy TbFeCo target produced by this conventional manufacturing method.

As shown in this figure, the composition has an RE of 22.8 to 19°8at.
%, the closer you go to the center of the substrate holder, the more RE there is, and conversely, the more you go to the outer periphery of the holder, the less RE there is. Also,
As for the magnetic properties, Hc is 17 to 11 KOe, and HC increases as you move toward the center of the holder. This also goes against the composition distribution. In other words, cast alloy TbFe by conventional manufacturing method
A Co target exhibits characteristics in which the TM (transition metal) in the upper direction of the target tends to fly off, and the RE in the lateral direction tends to rust, resulting in a compositional distribution within the substrate holder.

The magneto-optical recording medium created using this target has a linear velocity of 5.7 m/sec and a Doma in length of 1.4 μm.
T:C/N was a slightly low value of 57 dB.

This is an effect of the composition distribution within the medium. In the reliability test, 3000
No pitting corrosion occurred even after hours.

Furthermore, for comparison, TbFeC by the semi-melting method shown in JP-A-61-95788 and JP-A-61-99640
o Target was prepared and film formation was evaluated. The target composition is T bzzF e73c os a t%;
The amounts of b, TbFeCo, and FeCo are the same as described above. The oxygen content of this target was 1300 ppm.

This target was also installed in the sputtering apparatus shown in FIG. 2, and preliminary sputtering was sufficiently performed to form a film after the target surface was in a sufficiently clean state.

The film forming conditions are the same as described above. Figure 11 shows the semi-melting method Tb.
The composition distribution and magnetic property distribution diagram in the substrate holder using a FeCo target are shown. Although the composition distribution is comparable to that of the target of the present invention shown in Part 9, it can be seen that the magnetic property distribution is generally shifted in the direction of smaller coercive force (Hc). This is a phenomenon that occurs because the semi-molten target has a larger amount of oxygen than the target of the present invention because it is sintered, and the rare earth metal is partially oxidized by oxygen.

The magneto-optical recording medium created using this target has a linear velocity of 5.7 m/sec and a doma in length of 1.4 μm.
m, the C/N was 58 dB, which was a slightly low value.

This is because oxygen in the target was also incorporated into the film. In addition, in reliability tests, 90℃90%RH
Pitting corrosion occurs from the 200th hour under constant temperature and humidity, and Ero
or Rate started to deteriorate. This is also because oxygen in the target was taken into the film.

Further, the above-described TbFeCo target of the present invention and the semi-molten TbFeCo target were removed after sputtering, and both targets were left in the atmosphere for 24 hours. The rear target was again attached to the sputtering apparatus shown in FIG. 2, and film formation was attempted. Table 2 shows the discharge state during sputtering.

Table 2 As shown in the above table, the target of the present invention has a DC sputtering Ar pressure of 2.5 mTorr and the discharge is very stable from the initial stage, but the semi-molten target cannot be DC sputtered at the initial stage. This is because the surface of the semi-molten TbFeC0 target completely became an insulator because it was left in the atmosphere for a long time. And after an hour, D
C sputtering becomes possible, but the Ar pressure must be 8 mTorr, and it is only 2.5 mT after 5 hours.

DC sputtering became possible with rr.

FIG. 12 shows the relationship between the sputtering time and the magnetic properties of the films for both targets after being left in the atmosphere. 121 is a target according to the present invention, and 122 is a target made by a semi-melting method. As is clear from this figure, the target according to the present invention exhibits stable film characteristics immediately after sputtering even if it is exposed to the atmosphere for a long time. On the other hand, if a target made by a semi-molten method is exposed to the atmosphere for a long time, sputtering itself will be very difficult in the initial stage, and even after a long preliminary sputtering, the film properties will not be stable at all temperatures, and the film properties By the time it stabilizes, the number of targets will decrease and disappear. Since the magnetic properties of the film shown in these are compositions (characteristics) on the TMrich side with the compensation composition as a boundary, the larger the coercive force (Hc), the better the film properties.

Next, we investigated how long the semi-molten target should be left in the atmosphere to affect its film properties. After the target was sufficiently cleaned by preliminary sputtering and the film properties were stable, the target was removed and exposed to the atmosphere for 10 minutes, 30 minutes, and 1 hour.

I left it for 3 hours. Thereafter, an experiment similar to that shown in FIG. 12 was conducted to examine the sputtering time dependence of the film magnetic properties. 13th
The figure shows that, 131 is the one left in the atmosphere for 10 minutes, 13
2 is the one left in the atmosphere for 30 minutes, 133 is the one left in the atmosphere for 1 hour, and 134 is the one left in the atmosphere for 3 hours. As is clear from the figure, the target produced by the semi-molten method is
If left for even 0 minutes, surface oxidation of the target will occur, affecting the magnetic properties of the film. It can be seen that the longer the exposure time in the atmosphere, the more oxidation progresses from the target surface, and the more severe the degree of shadow V that affects the magnetic properties of the film becomes.

The effect of the present invention was confirmed even with TbFeCo that does not contain light rare earth metals.

[Example 2-2] Next, Dy powder with an average particle size of about 300 μm was prepared as a raw material, and a FeCo ingot containing Fe, Co, at% was crushed so that the average particle size was about 150 μm. Make FeCo powder.

Next, D) The mixture is placed in a crucible under vacuum so that the concentration becomes 4sF es + COs a t%, the temperature is raised once to 1650°C to completely melt, and then the temperature is lowered to 1200°C.

Then, the above-mentioned Dy powder and FeCo powder were added to this D y Fe Co molten alloy into a crucible.

Dy has a melting point of 1450°C, and FeCo has a melting point of 1530°C.
Therefore, it will not dissolve in a vortex at 1200'C, so
The Dy and FeCo powders will remain as powders. The proportions of these DyFeCo and DyFeCo amounts are as follows.

(D y F e Co)t(D ya(F e CO
) + 4) FD: F = 25 nia 5 wt% G: H = 22 nia 8 at% (DyFeCo) -Dy- (FeC
o) The molten metal was poured into a mold, and the resulting cast alloy was processed, and the composition distribution and magnetic properties in the substrate holder were measured using the same film forming apparatus and film forming method as in Example 2-1 using a 4"φ x 6t sputtering target. As a result of evaluating the distribution,
The RE was uniform at 22.0 to 22.5 at%, and the magnetic properties were uniform at HC of 12.0 to 13.0 KOe.

The amount of oxygen was also as low as 350 ppm. Also, leave it in the atmosphere 2
Even after 4 hours, the sputtering discharge remained stable from the beginning, and the film magnetic properties were similarly stable from the beginning.

The effect of the present invention was also confirmed for the DyFeCo composition.

[Example 2-3] Next, as a raw material, a GdTb ingot having T bsoG dsoat% is made, and GdTb powder is made. And likewise F eqyc O? Make a t% powder. Further G
dzz, sT bzz, sF es+COa a t%
Each element is placed in a crucible so that the temperature is raised once to 1650°C to completely dissolve, and then lowered to 1200°C. Then, the above-mentioned GdTb powder and FeCo powder were added to this G d T b Fe Co molten alloy in a crucible. This C, dTb powder has a melting point of 1400℃
Since the temperature of FeCo is 1530°C, it will not melt in hot water at 1200°C, so the C, dTb, and FeCo powders will exist as powders. And these Gd
TbFeCo, GdTb, and FeCo11 have the following proportions.

(GdTbFeCo)+((GdTb)K(FeCo)
t) Jl: J=25: 75wt%: L=22 near 8at% (GdTbFeCo)-(GdTb
)-(FeCo) casting alloy target is Example 2-1
．． 1.Similar to 2-2. After all, it was a target that could be used to form a film without compositional distribution or magnetic property distribution within the substrate holder. Hc is 11-13KOe, RE is 22-22.53t
% was uniform.

The amount of oxygen was sooppm.

Further, even after 24 hours of being left in the atmosphere, the sputtering discharge remained stable from the beginning, and the film magnetic properties were similarly stable from the beginning.

The effect of the present invention was also confirmed for GdTbFeCo.

These Example 2-1. 2-2. In addition to the composition system shown in 2-3, TbDyFeCo, DyGdFeCo, Gd
FeCo, GdTbFe, TbDyFe, TbCo, D
Gd, Tb such as yGdCo, etc.

at least one heavy rare earth metal of Dy;
It is confirmed that the effect of the present invention exists for all composition systems containing at least one transition metal of e, Co.
I approved.

Next, as another example, another method for manufacturing the target of the present invention will be described. This manufacturing method is called an impregnation method or an infiltration method. An outline of this manufacturing method will be explained.

Spread TM powder in the mold and place the RE-TM alloy ingot (
(called the mother alloy). This mother alloy composition is near the eutectic composition on the rare earth metal side in the phase diagram, and is a low melting point alloy with a melting point of 1200° C. or less. This powder and master alloy are heated to melt the master alloy, and the melted master alloy is made to infiltrate into the pores of the powder. When the molten master alloy solidifies, it separates into RE, RE, and TM phases.
The metal structure of the target that is inevitably created is a TM phase,
There are three phases: RE alloy phase and RE-TM alloy phase.

[Example 3-1] First, as a raw material (Ndo,zD)'0.11)
7□, 2 (Feo, e C00, 2) z'+, ea
A t% ingot is made (hereinafter this ingot is referred to as R+R, Tz master alloy). The melting point of this master alloy is as low as 830°C.
The shape is 4″φX2t.And then Fee.CO□
. A powder having a particle size of 200 at% was prepared. The melting point of this powder is as high as approximately 1500°C, and the porosity of this powder is 62
．． It is 4%.

Place this powder in a crucible with an inner diameter of 4#φ, and place R+
Add mother alloy to R+T. FIG. 14 is a schematic diagram showing this state. 141 is a crucible, 142 is a high frequency induction heating coil, 143 is an R+R+T2 master alloy, 144
is Fe, oco, at% powder. This state is evacuated, and then the temperature is raised to 1050° C. (heated in a non-pressurized state).

At this time, the R+R+Tz master alloy is melted and Fe-
Co powder exists in a powder state without being dissolved.

In other words, the molten metal in which the ingot melts R+ R+ T is Fe-
It penetrates into the pores of the Co powder and fills the pores.

After that, it is cooled, the molded body in the crucible is taken out, the outer periphery is processed,
A sputtering target of 4″φ×3t was prepared by polishing.The target composition was Nds, sD)’zz,
. Nd5a,. C0Ia, sat%. A schematic diagram of the surface structure of this target is shown in FIG. 15
Phase 1 is Fe-Co particles, phase 152 is a rare earth single phase of Nd-Dy, and phase 153 is (NdDy) + (NdCo)z
is a rare earth transition metal alloy phase. In other words, there are three phases: a rare earth single phase, a rare earth transition metal phase, and a transition metal single phase.

This NdDyFeCo target was installed in a sputtering apparatus similar to that shown in FIG. 2, and a film was formed to examine its magnetic properties and composition distribution. Film forming conditions were Ar pressure of 1.5mTor.
r, initial vacuum level 3X10-'Torr, input power is DC
The power supply was 1.0A340. FIG. 16 is a diagram showing the composition distribution and magnetic property distribution in the substrate holder using the target of the present invention. As shown in this figure, the composition is uniform with an RE of 28°0 to 28.5 at%, and the magnetic properties are H
C is uniform at 9.7 to 10.5 KOe, and exhibits magnetic properties consistent with the film composition. A nearly uniform film is deposited inside the substrate holder. Naturally, this target is made using the sintering method (the master alloy is not a powder but a bulk, and since it is an infiltration target that is completely melted, the oxygen content is low at 350 ppm.Also, since it is not poured into a mold as described above, there are no cavities. The occurrence is extremely low, and the packing density is 99.
A very high value of 5% was obtained.

With this target, the discharge is very stable from the beginning of sputtering, and DC sputtering is possible at an Ar pressure of 2.5 m'' orr.Even after being left in the atmosphere for 24 hours, it remains stable immediately after sputtering. Indicates membrane properties.

[Example 3-2] Next, the effect of the method of the present invention on PrTbArFeCo was confirmed. The manufacturing method is the same as in Example 3-1, and first, as a mother alloy (P r o, zT, bo, s)
go (F eo, a COo, z) zoa t% ingot is made. The melting point of this master alloy is about 810'C, and the bulk shape is 4"φX2,5t. Next, Fes.

Cozoat% powder with a particle size of 200 μm is prepared, and this powder is placed in a mold made of alumina with an inner diameter of 4#φ. Then, place the master alloy on top of it (no pressure) and apply 1050
The mixture was heated in an atmosphere furnace at . After the master alloy was melted, it was cooled, the molded body was taken out from the mold, the outer periphery was processed, and the sputtering targets of 4"φX3t were created.The target compositions were RE, RE-TM, and TM.
The overall composition is Prs, 5Tbz
□,. Fe511, oc Oz, 5at%.

Then, as a result of evaluating the composition distribution and magnetic property distribution in the substrate holder using the same film forming apparatus and film forming method as in Example 3-1, the RE was 28.0 to 28.5 at% and the Hc was 18.0 to 28.5 at%.
It was uniform at 19.0 KOe. Also, the amount of oxygen is 380p
pm, and sputtering was stable from the beginning even after being left in the air for 24 hours, and the film magnetic properties were similarly stable from the beginning.

The production method of the present invention is also applicable to the PrTbFeCo composition, and similar effects were confirmed.

[Example 3-3] Next, the effect of the method of the present invention on SmGdFeCo was confirmed. The manufacturing method is the same as Example 3-1.3-2, and first, as a mother alloy (S mo, z G(!, o, *
) + z, z (F eo, e COo, z) zt, sa
Make L% ingot. The melting point of this master alloy is about 808°C.

And then Few. CO□. At% powder with a particle size of 200 μm is prepared, and this powder is placed in a mold made of mullite with an inner diameter of 4 #φ. Then place the master alloy on top of it (no pressure applied),
The atmosphere was heated to 1040°C under vacuum. After the master alloy was melted, the molded body was cooled, taken out from the mold, processed on its outer periphery, and polished to create a sputtering target of 4#φX3t. As expected, the target composition is RE, RE-
TM.

It has three phases of TM, and the overall composition is Sms and 5Gd.
zz, oFese, ocO+4. It was sat%.

Then, as a result of evaluating the composition distribution and magnetic property distribution in the substrate holder using the same film forming apparatus and film forming method as in Example 3-1.3-2, the RE was 28. 0-28. Hc at 5at%
was uniform at 5 to 5.5 KOe.

In addition, the amount of oxygen was as low as 390 ppm (sputtering was stable from the beginning even after 24 hours of being left in the atmosphere, and the film magnetic properties were similarly stable from the beginning.

The manufacturing method of the present invention is also applicable to the SmGdFeCo composition, and similar effects were confirmed.

[Example 3-4] Next, the effect of the method of the present invention on NdSmDyTbFeCo was confirmed. The manufacturing method is Example 3-1.3-2.3
-3, first, CNdo as the mother alloy, +
Smo, +D yO, 4T bo, 4) 72.2
(F eo, e COo, z) zt, Ila Make an ingot of L%. The melting point of this ingot is about 830'C,
The shape is also a bulk of 4"φ x 2.5t."And next is Fes.

Co2. At% powder with a particle size of 200 μm is prepared, and this powder is placed in a mold made of isolite with an inner diameter of 4″φ.Then, a master alloy is placed on top of it (no pressure applied), and 1 (13
The atmosphere was heated to 0°C. After the mother alloy is melted, it is cooled and the formed body is taken out from the mold and the outer periphery is processed and polished.
A sputtering target of φX3t was prepared. Again, as in the previous example, the target compositions are RE, R.
It has three phases: E-TM and TM, and the overall composition is Nd.
z, tssmz, tsD)' eyes, oTbz, oF
esa,ocO+4. It was sat%. Then, as a result of evaluating the composition distribution and magnetic property distribution in the substrate holder using the same film forming apparatus and film forming method as in Example 3-1.3-2゜3-3, the RE was 28.0 to 28.5 at%. is uniform,
Hc is also 17-17. It was uniform at 5 KOe. or,
The amount of oxygen was as low as 375 ppm, and sputtering was stable from the beginning even after being left in the atmosphere for 24 hours.

The manufacturing method of the present invention is also applicable to the NdSmDyTbFeCo composition, and similar effects were confirmed.

These Example 3-1. 3-2. 3-3. In addition to the composition system shown in 3-4, NdGdNdCo, NdTbFeCo
, NdPrDyNdCo, NdPrDyTbNdCo,
PrDyFeCo, NdSmGdFeCo, CeNdD
Sm, N of yFeCo, CeNdPrDyFeCo, etc.
at least one light rare earth metal selected from Cd, Pr, and Ce; and Cd.

The manufacturing method of the present invention is possible for all composition systems containing at least one heavy rare earth metal among Tb and Dy and at least one transition metal among Fe and Co, and similar effects can be achieved. It was also confirmed that there were.

It was also confirmed that it is possible to obtain a desired CO composition in the target by using Fe powder as the transition metal powder and adjusting the amount of Ce in the master alloy.

Next, an example will be described in which the target composition does not contain a light rare earth metal, that is, it contains a heavy rare earth metal and a transition metal.

[Example 3-5] First, as raw materials Tt) + z (F eo, q Coo,
+) Make an ingot of 2eaL% (Hereinafter, this ingot will be referred to as R+ R
+ T is called the master alloy). The melting point of this master alloy is 847
The temperature is as low as about ℃, and the shape is 4#φX2.5t. Next, a powder of FeqoCOloa L% with a particle size of 200 am was prepared. This powder has a high melting point of about 1500° C., and the porosity of this powder is 43.3, which is the mother alloy.

This powder was placed in a mold made of alumina with an inner diameter of 4", a master alloy was placed on top of it (no pressure applied), and heated in an Ar pressure gas atmosphere. After the master alloy was melted, it was cooled and formed in the mold. The molded body was taken out, and its outer periphery was processed and polished to create a sputtering target of 4″φ x 3t. As expected, the target composition has three phases: RE, RE-TM, and TM, and the overall composition is T bzzF eto, zC07, 11a.
t%.

Then, as a result of evaluating the composition distribution and magnetic property distribution in the substrate holder using the same film forming apparatus and film forming method as in Example 3-1.3-2, it was found that the RE was uniform at 22.0 to 22°5 at%. The magnetic properties were uniform with He ranging from 14°7 to 15.5 KOe. Base) An almost uniform film was formed inside the anti-holder. Also, the amount of oxygen is 350 p
pm, and sputtering was stable from the beginning even after 24 hours of being left in the air, and the film magnetic properties were similarly stable from the beginning.

[Example 3-6] Next, the effect of the method of the present invention on DyFeCo was confirmed. The manufacturing method is the same as Example 3-1.3-2, etc.
First, as a raw material, D>'? +, s(F e o, qCo
o, +)ze, s a t% ingot is made. The melting point of this ingot is about 890°C. And then Feq. C
o.

A powder having a particle size of 200 μm at % was prepared. The melting point of this powder is as high as 1500°C, and the porosity of this powder is 43.2.
%.

Spread this powder in a mold made of mullite with an inner diameter of 4″φ,
An ingot was placed on top of it (no pressure applied), the temperature was raised to 1050℃ in a vacuum, the ingot was melted, and then cooled.The formed body was taken out of the mold and the outer periphery was processed and polished to 4"φ x 3t.
A sputtering target was created. As expected, the target composition has three phases: RE, RE-TM, and TM, and the overall composition is D 3'zzF eto, zc Oq
, *at%. And Example 3-1.3-2
As a result of evaluating the composition distribution and magnetic property distribution in the substrate holder using the same film forming apparatus and film forming method as the above, the RE was 21.5.
It is uniform at ~22.0at%, and the magnetic property Hc is 1
It is uniform at 3.5 to 13.0 KOe. A nearly uniform film was formed inside the substrate holder. Also, the amount of oxygen in this target is as low as 350 ppm.
Sputtering was stable from the beginning even after being left in the air for 24 hours, and the magnetic properties of the film were also stable from the beginning.

Example 3-7 Next, the effect of the method of the present invention on TbGdFeCo was confirmed. The manufacturing method is the same as in Example 3-1.3-2, etc., and first, (Tbo, 5Gdo, s)7+,
s (F eo, q COo, +) [, Sat%
Make an ingot. The melting point of this master alloy is about 838"C. Next, we prepared a powder of Fe, Cot.at% with a particle size of 20Qμm. This melting point is as high as about 1500℃, and the porosity of this powder is It is 43.7%.

Spread this powder in a mold made of isolite with an inner diameter of 4#φ,
Place the mother alloy on top of it. Afterwards, the atmosphere is heated to 1050℃ in a vacuum, and after the master alloy has melted, it is cooled, and the formed body is taken out from the mold and the outer periphery is processed and polished.
A 3t sputtering target was created. As expected, the target composition has three phases: RE, RE-TM, and TM, and the overall composition is Gd++F eto, zcO7,
It was sat%. Then, as a result of evaluating the composition distribution and magnetic property distribution in the substrate holder using the same film forming apparatus and film forming method as in Example 3-1.3-2, the RE was 22.0~
It has a uniform Hc of 22.3 at%, and its magnetic properties are 15.
It was uniformly dusty at 5 to 16.0 KOe. A nearly uniform film was formed inside the substrate holder.

In addition, the amount of oxygen is as low as 300 ppm, so it cannot be left in the atmosphere2.
Even after 4 hours, sputtering remained stable from the beginning, and the film magnetic properties were similarly stable from the beginning.

These Examples 3-5. 3-6. TbFe, TbCo, and GdFeCo in addition to the grouped acid series shown in 3-7.

GdD)'FeCo, GdDyTbFeCo, DyTb
FeCo, GdTbFe, DyCo, TbGd
At least one heavy rare earth metal selected from Gd, Tb, and Dy such as Co, TbD)'Co, and Fe.

It was confirmed that the production method of the present invention is possible for all composition systems containing at least one transition metal among Co, and that similar effects also exist.

It was also confirmed that it is possible to obtain a desired CO composition in the target by using Fe powder as the transition metal powder and adjusting the amount of Co in the master alloy. , shows another method for manufacturing the target of the present invention. This manufacturing method is basically the same as the impregnation method described above, but instead of using 7M powder, foamed TM is used. Foamed TM is a metal porous body with a spongy skeleton and high porosity, as seen in, for example, "Kogyo Materials, October 1987 issue."

A foamed 7M sheet is placed in the mold, and the RE-TM master alloy ingot is placed on top of it. This mother alloy composition is near the eutectic composition on the rare earth metal side in the phase diagram, and is a low melting point alloy with a melting point of 1200'C or less. It is produced by heating this powder and the master alloy to melt the master alloy and infiltrating the molten master alloy into the pores of the powder. When the molten master alloy solidifies, it separates into RE, RE, and TM phases, so the metal structure of the resulting target is inevitably the TM phase.

There are three phases: the RE phase and the RE-7M alloy phase.

Since the foamed TM is not a powder, the continuous TM forms the skeleton. Therefore, the resulting target has increased strength and toughness due to the TM skeleton, making it an extremely strong target.

[Example 4-1] First, as raw materials, the composition was TbtzFezi, zcO+, s
A master alloy ingot of at% is made. Also Feqy, bC.

A foamed FeCo sheet having a composition of , , at% is prepared. This foam sheet has a very high porosity of 91%.
Since it cannot be used as it is, we press the foam sheet,
The porosity was set to 43.5%.

This foamed FeCo sheet is placed in a mold made of alumina with an inner diameter of 4 #φ, and the master alloy is placed on top of it (no pressure applied).
, the atmosphere was heated to 1000° C. under vacuum. The mother alloy has a low melting point of about 850℃, and the molten mother alloy ingot has a foamed F shape.
It dissolves into the eCo sheet. After that, it is cooled and the formed body is taken out from the mold and the outer periphery is processed and polished to 4"φX3t.
A sputtering target was created. A schematic diagram of the metal structure of this target is shown in FIG. In the structure, there is a single phase of transition metals (F eqz, bcob, g)17
1. Single phase of rare earth metal (T b ) 172. An alloy phase (TbFeCo) 173 of transition metals and rare earth metals coexists. The overall composition of the target is TbzzFe,5c
It was osa t%.

This target of the present invention was installed in a sputtering apparatus similar to that shown in FIG. 2, and a film was formed to examine its magnetic properties and composition distribution. The film formation conditions were an Ar pressure of 2.5 mTorr, an initial vacuum level of 3 x 10-7 Torr, and an input power of 1.0 A and 340 V using a DC power supply. FIG. 18 is a diagram showing the composition distribution and magnetic property distribution in the substrate holder using the target of the present invention. As shown in this figure, the composition is uniform with an RE of 22.0 to 22.5 at%, and an Hc of 14.
It is uniform at 7 to 15.5 KOe. (An almost uniform film is formed inside the anti-holder.Of course, this target is not a sintering method, and the master alloy is not a TM receipt powder, but an infiltration target by total melting.) The amount of oxygen was also low, at 500 ppm.Furthermore, the packing density was 99.8%, indicating complete filling.

With this target, the discharge is also very stable from the beginning of sputtering, and DC sputtering is possible at an Ar pressure of 2.5 mTorr. Even after being left in the atmosphere for 24 hours, it exhibits stable film properties immediately after sputtering.

[Example 4-2] Next, as a raw material, the composition is D)'72F ezb, zc
A mother alloy ingot of O+, sat% is made. Also, Feqx,
bC.

A foamed FeCo sheet having a composition of 6.4 at% is prepared. After pressing and adjusting the porosity of the foamed FeCo sheet to 43.1%, the foamed FeCo sheet was placed in a mold made of zirconia with an inner diameter of 4", and the master alloy was placed on top of it. The sample was placed (no pressure applied) and heated in an atmosphere of 1050° C. under vacuum.

After the master alloy was melted, it was cooled, and the molded body formed in the mold was taken out, and the outer periphery was processed and polished to create sputtering targets of 4″φ×3.The target compositions were RE, RE-TM, and TM. The overall composition was D y z□Fe=, Co, at%.

As a result of evaluating the composition distribution and magnetic property distribution in the substrate holder using the same film forming apparatus and film forming method as in Example 4-1, the RE was uniform at 21°5 to 22.0 at%, and the magnetic properties were also HC is uniform at 13.5 to 13.0 KOe.

An almost uniform film was formed inside the substrate holder. Also, the amount of oxygen in this target is 430p
pm, and sputtering was stable from the beginning even after 24 hours of being left in the air, and the BtJ magnetic properties were similarly stable from the beginning.

[Example 4-3] Next, the effect of the method of the present invention on TbGdFeCo was confirmed. The manufacturing method is the same as Example 4-1.4-2, and first, Tb3bGdzbFezb, zCO +
, e a t%, a master alloy ingot is prepared. Also F eq3.
A foamed FeC0 sheet having a composition of bc Ob, a at % was prepared and pressed until the porosity was 43.5%. Then, this foamed FeC0 sheet was 4″φ
It was placed in a mold made of mullite with an inner diameter, and the master alloy was placed on top of it (no pressure applied), and the atmosphere was heated to 120'C under vacuum. After the master alloy was melted, it was cooled and completed in the mold. Take out the molded body, process the outer periphery, and polish it to 4″φx3
A sputtering target of t was prepared. As expected, the target composition has three phases: RE, RE-TM, and TM, and the overall composition is TbzGdzFet3cO2at%
Met. Then, as a result of evaluating the composition distribution and magnetic property distribution in the substrate holder using the same film forming apparatus and film forming method as in Example 4-1.4-2, the RE was 21.5 to 22.0 at%.
The magnetic properties are uniform and Hc is 14 to 15.0 KOe.
It is uniform.

A nearly uniform film was formed inside the substrate holder. Also, the amount of oxygen in this target is 480p
pm, and sputtering was stable from the beginning even after 24 hours of being left in the air, and the film magnetic properties were similarly stable from the beginning.

These Examples 4-1 and 4-2. In addition to the composition system shown in 4-3, TbFe, TbCo, and GdFeCo.

GdDyTbFeCo, DyTbFeCo, CdTbF
Gd such as e, DyCo, TbGdCo, TbDyC0, etc.
, Tb, Dy, and at least one transition metal among Fe, Co. The manufacturing method of the present invention is applicable to the foam metal, It was also confirmed that a similar effect also exists.

Then, the foamed transition metal is changed to Fe, and the mother alloy is C0f.
Target C by adjusting f1.

It was confirmed that it is also possible to create a desired composition.

Next, an example of the manufacturing method of the present invention using a foamed metal will be described where the target composition includes a light rare earth metal, that is, a light rare earth metal, a heavy rare earth metal, and a transition metal.

[Example 4-4] The effect of the method of the present invention on NdDyFeCo was confirmed. The manufacturing method is the same as Example 4-1.4-2, etc.
First, as raw materials (r"Jdo, zD3'o, a) tz,
z (F eo, ll COo, z) zw, aa t%
Make a mother alloy ingot. Also Fe. CO□. A foamed FeCo sheet having a composition of at% is prepared, and the porosity is 62.
．． It was pressed and adjusted until it became 6%. Then, this foamed FeCo sheet was placed in a mold made of isolite with an inner diameter of 4". Then, a master alloy was placed on top of it (no pressure applied), and the atmosphere was heated to 130° C. under vacuum.

After the master alloy was melted, the molded body was cooled and removed from the mold, processed and polished to create a sputtering target of 4″φ x 3t.The target composition was also three phases: RE, RE-TM, and TM. The overall composition is Nds, 5Dyz□.

Fess, oCOz, and sat%. Then, as a result of evaluating the composition distribution and magnetic property distribution in the substrate holder using the same film forming apparatus and film forming method as in Example 4-1.4-2, it was found that the RE was uniform at 28.0 to 28.5 at%. The magnetic properties are uniform with Hc ranging from 9.7 to 10.5 K Oe. A nearly uniform film was formed inside the substrate holder. Also, the amount of oxygen in this target is 475
ppm, and sputtering was stable from the beginning even after 24 hours of being left in the atmosphere, and the film magnetic properties were similarly stable from the beginning.

[Example 4-5] Next, the effect of the method of the present invention on PrTbDyFeCo was confirmed. The manufacturing method is the same as in Examples 4-1 and 4-2, and first, as a mother alloy (Pro, z Tbo, a
D)'0.4)80 (F eo, a COo, 2)
Make a 20at% ingot. The melting point of this master alloy is 820"
It is about C. Also Fes. CO□. A foamed FeCo sheet having a composition of at% is prepared, and the porosity is 62.8%.
Press and adjust until it becomes . And this foamed FeC
The o-sheet was placed on a mold made of alumina with an inner diameter of 4", the master alloy was placed on top of it without pressure, and the atmosphere was heated to 130°C under vacuum. After the master alloy was melted, it was cooled and molded. The completed molded body is taken out, processed and polished to a diameter of 4″φ.
An X3t sputtering target was created. As expected, the target composition has three phases: RE, RE-TM, and TM, and the overall composition is P r s, s T b zD
V1□Fe5ecOz, sat%. Then, as a result of evaluating the composition distribution and magnetic property distribution in the substrate holder using the same film forming apparatus and film forming method as in Example 4-1.4-2, it was found that the RE was uniform at 28.0 to 27.8 at%. can be,
The magnetic properties were also uniform with Hc ranging from 15.5 to 15°8KOe. A nearly uniform film was formed inside the substrate holder.

Furthermore, the oxygen content of this target was as low as 420 ppm, and sputtering was stable from the beginning even after 24 hours of being left in the atmosphere, and the film magnetic properties were similarly stable from the beginning.

[Example 4-6] Next, the effect of the method of the present invention on PrSmDyGdFeCo was confirmed. The manufacturing method is the same as in Example 4-1.4-2, etc., and first, as a master alloy (Pro, + Sm
o, + Dyo, 4Gdo, 4) vz, z (F
e. ,8CO0,2) 2°, Ilat% ingot is made. The melting point of this ingot is about 880°C. Also Fes. C
oz. A foamed FeCo sheet having a composition of aL% was prepared, and the porosity was pressed and adjusted to 63.1%. Then, this foamed FeCo sheet was placed in a mold made of alumina with an inner diameter of 4", and the master alloy was placed on top of it without pressure, and the atmosphere was heated to 1040'C under vacuum. After the master alloy was melted, After cooling, the molded body formed in the mold was taken out, processed and polished to form a sputtering target of 4″φ×3t. After all, the target composition is RE
, RE-TM, and TM, and the overall composition is Pr t, 7ssmz, rsD Y xG d zCO
+4.5at%. And Example 4-1.4-
As a result of evaluating the composition distribution and magnetic property distribution inside the substrate holder using the same film forming apparatus and film forming method as No. 2, the RE was 28.
It is uniform at 0 to 28.1 at%, and the magnetic properties are Hc of 7.
．． It was uniform between 2 and 7.5 KOe. A nearly uniform film was formed inside the substrate holder.

Furthermore, the oxygen content of this target was as low as 490 ppm, and sputtering was stable from the beginning even after being left in the atmosphere for 24 hours, and the film magnetic properties were similarly stable from the beginning.

These Example 4-4. 4-5. In addition to the composition system shown in 4-6, NdGdFeCo and NdTbFeCo.

NdPrDyFeCo, NdPrDyTbFeCo, P
rDyFeCo, NdSmGdFeCo.

PrTbFeCo, CeNdDyFeCo, CeNdP
Sm, Nd, Pr such as rDyFeCo.

At least one light rare earth metal of Ce and Gd
, Dy, and Tb; and at least one of Fe and Co.
It was confirmed that the production method of the present invention is possible for all composition systems containing transfer metals, and that similar effects also exist.

It was also confirmed that it is possible to obtain a desired CO composition in the target by using Fe as the foamed transition metal and adjusting the amount of Co in the master alloy.

In the impregnation method or infiltration method, which is one of the methods of the present invention, the porosity of the powder or foam sheet is important. This is because the target is created by infiltrating the molten ingot into the pores of the powder or foam sheet, so the target composition is determined by the porosity. In other words, a target with a desired composition must be provided by controlling the porosity.

Since the composition of the medium is required to have a rare earth metal content of about 15 at % to 35 at %, the composition of the target must be adjusted accordingly. In order to satisfy this requirement, attempts are being made to match the target composition by varying the porosity of the powder or metal foam.

A concrete and brief explanation will be provided. Prepare powder with a porosity of about 30%, and place an ingot on top of it. This is shown in FIG. 19(a). The state in which the ingot is melted and impregnated into powder is shown in FIG. 19(b). It can be seen that the molten ingot only enters the pores in the powder.

Next, powder with a porosity of 80% was prepared, and an ingot was placed on top of it, as shown in FIG. 20(a). Similarly, the state in which the ingot is melted and impregnated into powder is shown in FIG. 20 (G).

By doing this, the porosity of the powder can be controlled and the composition can be determined.

[Example 5-1] Regarding NdDyFeCo, powders and foamed 7M sheets with various porosity were prepared, and sputtering targets were created by the impregnation method, which is the manufacturing method of the present invention.

As a master alloy (N d o, zD YO, II) 7
2.2 (F e o, aCo o, z) zt, v
+ a t% ingot is made. And then Fe8゜Coz
. A powder having a particle size of 200 μm at % was prepared. The porosity of the powder is 30%, 40%, and 50%.

We prepared 62%, 70%, and 80%. The porosity can be controlled by preparing grains ranging from spherical to irregularly shaped grains. Also, the same (Feg.

Coz. At% foamed metal sheets are prepared, and the porosity is 30%, 40%, 50%, and 62% by pressing.

We prepared 70% and 80%. Previous Example 3-1.
Using the same manufacturing method as 4-4, FeC with various porosity
A sputtering target was prepared using o powder or foamed FeCo sheet.

The table below shows the porosity of the powder used and the target composition.
The porosity of the foam sheet and the composition of the resulting target are shown.

Table 3 30 Ndz, w Dyz, aF 66g, +co+
7.440 Nd3. b D)'+4. zF eb5
．． ecO+b, <50 N da, a D y17.
11F ebz, ac O+5. b62 Nds,
s D Yzz F es++ COIa, s70
Nd6. z D y24.7F ess, 3c O+
z, e80 Ndv, + Dyze, 3F es+,
acO+z, sTable 4 30 N dz, 7D YIl, bF ebs, sc
o+t140'N d3. b D )' +4.
ZF e6s, ec OIb, 450 N da, a
D V Iq, bF ebz, ac O+5. b62
N ds, s D >'zz, oF ess, oc
O+a, s70 N d6. z D yz4.7F
ess, 3c O11880Nd7. + D)'zs
, zF es+, ecO+z, i Using targets with different FeCo powder porosity or FeCo foam sheet with different porosity, films were formed using the same sputtering equipment as shown in Figure 2, and the composition distribution inside the substrate holder was measured. I saw it. Second
Figure 1 is a composition distribution diagram of targets using various porosity powders, and Figure 22 is a composition distribution diagram of targets using various porosity foam sheets.
FIG.

211 is the composition distribution when a film is formed using a powder target with a porosity of 30%, 212 is a composition distribution when the film is formed using a target with a porosity of 40% powder, and 213 is a composition distribution when a film is formed using a target with a porosity of 50% powder. , 214 is the composition distribution when the film is formed using a 62% porosity powder target, 215 is the composition distribution when the film is formed using a 70% porosity powder target, and 216 is the composition when the film is formed using a porosity 80% powder target. distribution. Also, 221 has a porosity of 3
Composition distribution of film formed using 0% foam sheet target, 22
2 is a composition distribution formed using a foam sheet target with a porosity of 40%, 223 is a composition distribution formed using a foam sheet target with a porosity of 50%, and 224 is a film formed using a foam sheet target with a porosity of 62%. composition distribution, 225 has a porosity of 70
% composition distribution of film formed with foam sheet target, 226
is the composition distribution of a film formed using a foam sheet target with a porosity of 80%. In all of these targets, the composition distribution of the film formed using the target produced by the production method of the present invention is extremely small and shows good uniformity, and the film composition can be varied in various ways by controlling the porosity. be.

Other composition systems, PrTbFeCo, SmGdFeCo, S
mDyTbFeCo, NdTbFeCo.

NdGdFeCo, NdPrDyFeCo, N
dPrDyTbFeCo, PrDyFeCo,
NdSmGdTbFeCo, CeNdDyFt=C
o.

Sm, Nd, Pr such as CeNdPrDyFeCo.

at least one light rare earth metal of Ce, and G
It was confirmed that the method of the present invention is effective for all composition systems containing at least one heavy rare earth metal of d, Dy, and 'rb and at least one transition metal of Fe and Co. did.

[Example 5-2] Next, TbFeCo powders and foamed 7M sheets with various porosity were prepared, and sputtering targets were created by the impregnation method, which is the manufacturing method of the present invention.

T b7z (F eo, q COo, +
) Make an ingot of z8a t%. And then Few. Co
,. A powder having a particle size of 200 μm at % was prepared. The porosity of the powder is 30%, 43%, 50%, 60%, and 70%.

80% was used, and the porosity was controlled by preparing grains ranging from spherical to irregularly shaped.

In addition, foamed metal sheets of the same (Fe, .Co, .at%) were prepared, and the porosity was 30% and 43% by pressing.

50%, 60%, 70%, and 80% were prepared. Sputtering targets were prepared using FeCo powder or foamed FeCo sheets having various porosity using the same manufacturing method as in Example 3-5.4-1. In the table below,
The porosity of the powder used and the composition of the resulting target are shown, as well as the porosity of the foam sheet and the composition of the created target.

Table 5 30 Tbzs Few6゜5coa, s43
T bzz F e7o,zCoi150 T
bzs,,Febt,oc 07.560 T
bio, sF ehz, bc 06.970 T
b3s,, F e ss, oCO6,580T bno
,tF es:+1c 05.9Table 6 30 T bus F e,b,sc Oa,s4
3 T bzz F e7o,zc o1850
T bzs, sF ebt, oc 07.560
T bio, sF ebz, bc Ob, q70
T bzs, sF ess, oCOb, 580
T b4o,yF es3゜4CO5,9
These FeCo powder targets with different porosity or F
Using targets with different eCo foam sheet porosity,
A film was formed using a sputtering apparatus similar to that shown in FIG. 2, and the composition distribution inside the substrate holder was observed. FIG. 23 is a composition distribution diagram of Targetera (*) using powders with various porosity, and FIG. 24 is a composition distribution diagram of targets using foamed sheets with various porosity.

231 is the composition distribution when a film is formed using a powder target with a porosity of 30%, 232 is a composition distribution when a film is formed using a target with a porosity of 43% powder, and 233 is a composition distribution when a film is formed using a target with a porosity of 50% powder. , 234 is a composition distribution formed with a target of 60% porosity powder, 235 is a composition distribution of a film formed with a target of 70% porosity powder, and 236 is a composition formed with a target of 80% porosity powder. distribution. Also, 241 has a porosity of 3
Composition distribution of film formed using 0% foam sheet target, 24
2 is a composition distribution formed using a foam sheet target with a porosity of 43%, 243 is a composition distribution formed using a foam sheet target with a porosity of 50%, and 244 is a film formed using a foam sheet target with a porosity of 60%. composition distribution, 245 has a porosity of 70
% composition distribution of a film formed using a foamed sheet target.

246 is the composition distribution obtained by forming a film using a foam sheet target with a porosity of 80%. In all of these targets, the composition distribution of the film formed using the target produced by the manufacturing method of the present invention is extremely small and shows good uniformity, and the film composition can be varied in various ways by controlling the porosity. It is.

Other composition systems, DyFeCo, TbGdFeCo.

TbFe, GdFeCo, GdDVFeCo, GdDy
TbFeCo, DyTbFeCo, GdTbF
e, at least one heavy rare earth metal selected from Gd, Tb, D)' such as TbDyCo, and Fe.

It was confirmed that the method of the present invention is applicable to all composition systems containing at least one transition metal among Co.

Next, in creating targets using the present invention method using transition metal powder, targets were created using powders with various particle sizes.

[Example 6-1] The basic preparation method is the same as Example 3-1, and the raw materials are (N do, z D yo, 5) vz, z (F e
o, a COo, z) z,, e a t% master alloy ingot 4#φx4t), then Fefi. C.O.
□. A variety of powders having different particle sizes at % were prepared, and using these powders, a master alloy was placed on the powder and heated in a vacuum atmosphere at 1000° C. to create a sputtering target.

The result is a target of 4"φX and 6t.

The average particle diameters of the powders used were 5 μm, 8 μm, and 10 μm.
m, 24 μm, 38 μm, 53 μm, 120 μm, 23
0μITI, 570μm, 730μm, 1mm,
1. 5mm, 2mm, 3mm, 3.
2mm.

It is 4mm.

The table below shows the finished targets for the powders used.

Table 7 5μm, 64% Impregnated to 3% from the top of powder 8μm, 6
4% Impregnated to 5% from top of powder 10 μm, 64% Impregnated 100% from top of powder 24 μm, 62% 10
0% impregnation 38μm, 58% 100% impregnation 53μm
m, 55% 100% impregnated 120μm, 51%
100% impregnation 230μm, 48% 100
% impregnation 570μm, 44% 100% impregnation 730
μm, 64% 100% impregnation 1, Omm, 62%
100% impregnation 1.5mm, 58% 10
0% impregnation 2.5mm, 55% 100% impregnation 3,
Omm, 53% 100% impregnation 3.2mm, 51
% 100% impregnated 4, Omm, 48% 1
00% impregnation From the results in the table above, it can be seen that when powder with an average particle diameter of 5 μm or 8 μm is used, the target cannot be manufactured because the master alloy does not penetrate. This is because the particle size of the powder is too small and the pores themselves are too small, which has a relationship with the viscosity of the dissolved mother alloy solution, and does not penetrate. Powder having an average particle size of lo/7m or more can be used to create a target with 100% penetration.

A target using powder having an average particle size of 10 μm or more as shown in the above table was attached to a sputtering apparatus shown in FIG. 2, and film formation was attempted. For all targets, the discharge was stable from the initial stage of sputtering, and there were no problems. Each target was sputtered for a long time and the relationship with the film magnetic properties was examined. Figures 25 and 26
The figure is a sputtering time dependence diagram of film magnetic properties. 251 is a target using 10 μm particle size powder, 252
The target has a particle size of 24 μm, and the target has a particle size of 253 and 38 μm.
Target using m particle size powder, 254 target using 53 μm particle size powder, 255 target using 120 μm particle size powder, 256 target using 230 μm particle size powder, 257 using 570 μm particle size powder It was a target.

It was confirmed that the target using particle size powder of 10 μm to 570 μm had constant film magnetic properties at all sputtering times and was sufficiently usable. The reason why the film magnetic properties are different for each target is because the porosity of the powder is different, and therefore the target composition is different, and this is not directly related to the gist of this example. 26
1 is a target using 730 μm particle size powder, 262 is 1
Target using ゜0mmmm particle size, 263 is l.

Target using 5mmmm particle size, 264 is 2°5mm
265 is a target using 3°0mmmm particle size, 266 is a target using 3°2mmmm particle size, and 267 is a target using 4°0mmmm particle size. It was confirmed that the target using powder with a particle size of 730 μm to 2.5 mm had constant film magnetic properties at all spuck times and was sufficiently usable. 3
When using a target with a grain size of 0 mm mm, the film magnetic properties slightly fluctuate depending on the sputtering time. This is because the particle size has increased, so the RE on the target surface
, RE-TM, and TM vary depending on the spuck time.

However, if the particle size is about 3.0 mm, it is not too large and can be used even during fluctuations. However, the target used for 3.2m and m particle size inspection was 4.0mm.
It was found that the target used for the m particle size was unusable because the fluctuations in the film magnetic properties were too large. From this, in order to manufacture the target of the present invention, the TM powder must have an average particle size of 10 pm or more.3. It is necessary that it is less than Ornm.

Other composition systems, PrTbFeCo, SmGdFeCo, S
mDyTbFeCo, NdTbFeCo.

NdGdFeCo, NdPrDyFeCo, NdPrD
yTbFeCo, PrDyFeCo, NdSmGd
TbFeCo, CeNdDyFeCo.

Sm, Nd, Pr such as CeNdPrDyFeCo.

at least one light rare earth metal of Ce, and G
It is also necessary to use particle sizes in the same range for all composition systems containing at least one heavy rare earth metal among d, Dy, and Tb and at least one transition metal among Fe and Co. I confirmed that there is.

[Example 6-2] Next, regarding TbFeCo, TM powders having different particle sizes were prepared, and the same manufacturing method as in Example 3-5 was attempted.

T 11) + z (F eo, q COo,
I) Prepare a 211a t% master alloy ingot with a diameter of 4”φX.
4t), then Feq. A variety of Co, at% powders with different particle sizes were prepared, and using them, a master alloy was placed on the powder and heated in a vacuum atmosphere at 110°C to create a sputtering target.The finished target was 4
“φX6t.

The average particle diameters of the powders used were 5 μm, 8 μm, and 10 μm.
m, 24 μm, 38 μm, 53 μm, 120 am, 23
0μm, 570μm, 130am, 1mm, 1.5mm
, 2mm, 3mm, 3.2mm.

It is 4mm. The table below shows the finished targets for the powders used.

Table 8 5μm, 44% Impregnated to 3% from the top of powder 8μm, 4
4% Impregnation from top of powder to 5% 10 μm, 44% Impregnation from top of powder to 100% 24 μm, 42% 10
0% impregnation 38μm, 39% 100% impregnation 53μm
m, 37% 100% impregnation 120μm, 35%
100% impregnation 230μm, 32% 100
% impregnation 570μm, 30% 100% impregnation 730
μm, 44% 100% impregnation 1, Omm, 42%
100% impregnation 1.5mm, 39% 10
0% impregnation 2.5mm, 37% 100% impregnation 3,
Omm, 35% 100% impregnation 3.2mm, 32
% 10 (1% impregnation 4, Omm, 30%
100% impregnation From the results in the table above, the average particle size is 5 μm and 8 μm.
It can be seen that if powder of This is because the particle size of the powder is too small and the pores themselves are too small, which has a relationship with the viscosity of the dissolved mother alloy solution, and does not penetrate. Powder having an average particle size of 10 μm or more can be used to create a target with 100% penetration.

A target using powder having an average particle size of 10 μm or more as shown in the above table was attached to a sputtering apparatus shown in FIG. 2, and film formation was attempted. The discharge of all targets was stable from the beginning of the spuck, and there were no problems. Each target was sputtered for a long time and the relationship with the film magnetic properties was examined. Figures 27 and 28
The figure is a sputtering time dependence diagram of film magnetic properties. 271 is a target using 10 μm particle size powder, 272
is a target using 24μm particle size powder, 273 is 38u
Target using m particle size powder, 274 target using 53 μm particle size powder, 275 target using 120 μm particle size powder, 276 target using 230 μm particle size powder, 277 using 570 μm particle size powder It was a target.

It was confirmed that the target using particle size powder of 10 μm to 570 μm had constant film magnetic properties at all sputtering times and was sufficiently usable. The reason why the film magnetic properties are different for each target is because the porosity of the powder is different, and therefore the target composition is different, and this is not directly related to the gist of this example. 28
1 is a target using 730 μm particle size powder, 282 is 1
, target using Ommmm particle size, 283 is 1°5m
Target using mm particle size, 284 is 2゜5mmmm
285 is a target using a particle size of 3°0 mmmm, 286 is a target using a particle size of 3°2 mmmm, and 287 is a target using a particle size of 4°0 mmmm. It was confirmed that the target using powder with a particle size of 730 μm to 2.5 mm had constant film magnetic properties at all sputtering times and was sufficiently usable. 3゜O
When using a target for mmmm grain size, the film magnetic properties vary slightly depending on the sputtering time. This is because the size of the particles has increased, so the RE and R of the target surface
This is because the ratio of E-TM and TM varies depending on the sputtering time.

However, if the particle size is about 3.0 mm, it is possible to use it without making it too thick even during fluctuations. However, the target used for the 3.2 mm particle size, 0 mm
It was found that the target used for grain size had too large a fluctuation in film magnetic properties to be usable. From this, in order to manufacture the target of the present invention, the 7M powder needs to have an average particle size of 10 μm or more and 3.0 mm or less.

Other composition systems DyFeCo, TbGdFeCo.

TbFe, GdFeCo, GdDyFeCo, GdDy
TbFeCo, DyTbFeCo, TbCo, GdTb
Gd, Tb such as Fe, TbDyCo.

At least one heavy rare earth metal among Dy and Fe
It was recognized in 1111 that it is necessary to use particle sizes in the same range for all composition systems containing at least one transition metal among , Co, and Co.

Next, in creating targets using the present invention method using foamed transition metal sheets, targets were created using foamed metals with various pore sizes.

[Example 7-1] Regarding FeDyFeCo, foamed transition metals having various pore diameters were prepared, and the same manufacturing method as in Example 4-4 was attempted.

Raw material Toshite (N d O, 2D yo, s) 72.2
Prepare a master alloy ingot of (F e o, aCoo, z) zt, iamu% 4″φX4t), then Fe5oCOz
Various foam sheets with different pore diameters of oa t% were prepared, and using them, a master alloy was placed on the foam sheets at 100%
A sputtering target was prepared by heating in a vacuum atmosphere at 0°C. The completed target is 4″φ x 6t.

The average particle size of the metal foam used was 5 μm and 8 μm.

10μm, 24μm, 38μm, 53μm, 120pm
, 230 μm, 570 μm, 730 μm.

1mm, 1.5mm, 2mm, 3mm, 3.2mm, 4
It is mm.

The table below shows the completed targets for the foamed metals used.

Table 9 5 μm, 64% foamed FeCo0 impregnated from above to 3% 8
μm, 64% Foamed FeCo0 from top to 5% impregnated 10
μm, 64% 100% impregnation from above foamed FeCo0 24
μm, 62% 100% impregnated 38μm, 58
% 100% impregnation 53μm, 55%
100% impregnation 120μm, 51% 10
0% impregnation 230μm, 48% 100% impregnation 570μm, 44% 100% impregnation 730μm
m, 64% 100% impregnation 1, Omm, 62
% 100% impregnation 1.5mm, 58%
100% impregnated 2.5mm, 55% 1
00% impregnation 3, Omm, 53% 100% impregnation 3.2mm, 51% 100% impregnation 4,
Omm, 48% 100% impregnation From the results in the table above, it can be seen that when metal foams with average pore diameters of 5 μm and 8 μm are used, the target cannot be manufactured because the master alloy does not penetrate. This is related to the viscosity of the dissolved mother alloy solution because the pore diameter of the foamed metal is too small, and it does not penetrate. Foamed metal having an average pore diameter of 10 μm or more can be 100% penetrated to create a target.

A target made of foamed metal having an average pore diameter of 10 μm or more as shown in the above table was attached to the sputtering apparatus shown in FIG. 2, and film formation was attempted. For all targets, the discharge was stable from the initial stage of sputtering, and there were no problems.

Each target was sputtered for a long time and the relationship with the film magnetic properties was examined. FIGS. 29 and 30 are sputtering time dependence diagrams of film magnetic properties.

291 is a target using foam metal with a pore size of 10 μm,
292 is a target using foamed metal with a pore size of 24 μm,
293 is a target using foam metal with a pore diameter of 388 m,
294 is a target using foamed metal with a pore size of 53 μm,
295 is a target using a foamed metal with a pore size of 120 μm, 296 is a target using a foamed metal with a pore size of 230 μm, and 297 is a target using a foamed metal with a pore size of 570 μm.

It was confirmed that a target using foamed metal with a pore diameter of 10 μm to 570 μm had constant film magnetic properties at all sputtering times and was sufficiently usable. The reason why the film magnetic properties are different for each target is because the porosity of the powder is different, and therefore the target composition is different, and this is not directly related to the gist of this example. 3 (11 is a target using foamed metal with 730 μm pore size, 3 (12 is a target using foamed metal with 1.0 mm pore size), 3 (13 is a target using foamed metal with 1.5 mm pore size, 304 is 2. A target using a foamed metal with a pore diameter of 5 mm, 305 a target using a foamed metal with a pore diameter of 3.0 mm, a target 306 using a foamed metal with a pore diameter of 3.2 mm, and a target 307 using a foamed metal with a pore diameter of 4.0 mm. Target: 7308m ~ 2.5m
It was confirmed that the target using foamed metal with m pore diameter had constant film magnetic properties during all sputtering times and was sufficiently usable. 3. In a target using a foamed metal with a pore diameter of 0 mm, the film magnetic properties slightly fluctuate depending on the sputtering time. This is because the size of the pores has become larger, so RE, RE-TM, TM on the target surface
This is because the ratio varies depending on the sputtering time.

However, if the porosity diameter is about 3.0 mm, it is not too large and can be used even during fluctuations. However, the target using foam metal with a pore size of 4.
．． It was found that a target using a foamed metal with a pore diameter of 0 mm was unusable because the film magnetic properties fluctuated too much. From this, in order to manufacture the target of the present invention, the TM foam metal has an average pore diameter of 1.
It is necessary that the thickness is 0 μm or more and 3.0 mm or less.

Other composition systems PrTbFeCo, SmGdFeCo, Sm
DyTbFeCo, NdTbFeCo.

NdGdFeCo, NdPrDyFeCo, NdPrD
yTbFeCo, PrDyFeCo, NdSmGdTb
FeC0, CeNdDyFeCo.

Sm, Nd, Pr such as CeNdPrDyFeCo.

At least one light rare earth metal among Ce and Gd
It is necessary to use pore diameters in the same range for all composition systems containing at least one heavy rare earth metal of , Dy, and 'rb and at least one transition metal of Fe and Go. It was confirmed that there is.

[Example 7-2] Next, for T b Fe C,o, foamed transition metals with different pore diameters were prepared, and the same manufacturing method as in Example 4-1 was attempted.

T byz (F eo, q COo, +
) Prepare a master alloy ingot of z, aa t% 4"φ×4
t), then Fee. Co. We prepared various foamed metals with different pore diameters at %, and using them, we placed a master alloy on the foamed metal and heated it in a vacuum atmosphere at 110°C to create a sputtering target.The completed target was 4 “φX6t.

The average pore diameters of the metal foam used were 5 μm, 8 μm, and 10 μm.
μm, 24 μm, 38 μm, 53 μm.

120μm, 230μm, 570μm, 730μm, 1
mm, 1.5mm, 2mm, 3mm, 3゜2mm, 4m
It is m. The table below shows the completed targets for the foamed metals used.

Table 10 5 μm, 44% foamed FeCo0 impregnated from above to 3% 8
μm, 44% impregnated from above foamed FeCo0 to 5% 10
μm, 44% 100% impregnation from above foamed FeCo0 24
μm, 42% 100% impregnated 38μm, 39
% 100% impregnation 53μm, 37%
100% impregnation 120μm, 35% 10
0% impregnation 230μm, 32% 100% impregnation 570μm, 30% 100% impregnation 730
μm, 44% 100% impregnation 1, Omm, 4
2% 100% impregnation 1.5mm, 39%
100% impregnated 2.5mm, 37%
100% impregnation 3, Omm, 35% ioo%
Impregnation 3.2mm, 32% 100% impregnation 4,
Omm, 30% 100% impregnation From the results in the table above, it can be seen that when using foamed metals with average pore diameters of 5 μm and 8 μm, the master alloy does not penetrate and the target cannot be manufactured. This is related to the viscosity of the dissolved mother alloy solution because the pore diameter of the foamed metal is too small, and it does not penetrate. Foamed metal having an average pore diameter of 10 μm or more can be 100% penetrated to create a target.

A target made of foamed metal having an average pore diameter of 10 μm or more as shown in the above table was attached to the sputtering apparatus shown in FIG. 2, and film formation was attempted. For all targets, the discharge was stable from the initial stage of sputtering, and there were no problems.

Each target was sputtered for a long time and the relationship with the film magnetic properties was examined. FIGS. 31 and 32 are diagrams showing the spuck time dependence of the film magnetic properties.

311 is a target using foamed metal with a pore size of 10 μm,
312 is a target using foam metal with a pore size of 24 μm,
313 is a target using foam metal with a pore size of 38 μm,
314 is a target using foamed metal with a pore size of 53 μm,
315 is a target using a foamed metal with a pore diameter of 120 μm, 316 is a target using a foamed metal with a pore diameter of 2308m, and 317 is a target using a foamed metal with a pore diameter of 5708m.

In the glue get using foamed metal with a pore diameter of 10 μm to 570 μm, the magnetic properties of the film were constant over all sputtering times, and it was found that the film could be used satisfactorily. The reason why the film magnetic properties are different for each target is
This is because the porosity of the powder is different, and therefore the target formation is different, and is not directly related to the gist of this example. 321 is a target using foamed metal with a pore diameter of 7308 m, and 322 is a target using 1. 323 is a target using foamed metal with pore size of 1.5mm, 324 is a target using foamed metal with 2.5mm pore size, 325 is a target using foamed metal with 3.0mm pore size. The target 326 is a target using a foamed metal with a pore size of 3.2 mm, and the target 327 is a target using a foamed metal with a pore size of 4.0 mm. 730μm~2
．． G11L'2 found that the target using a foamed metal with a pore diameter of 5 mm had constant film magnetic properties during all sputtering times and was sufficiently usable. 3. In a target using foamed metal with a pore diameter of 0 mm, the film magnetic properties slightly fluctuate depending on the sputtering time. This is because the size of the pores has become larger, so the RE and R of the target surface
This is because the ratio of E-TM and TM varies depending on the sputtering time.

However, 3. If the porosity diameter is approximately 0 mm, it can be used without being too large even during fluctuations. However, the target using foam metal with a pore size of 4.
．． It was found that a target using a foamed metal with a pore diameter of 0 mm was unusable because the film magnetic properties fluctuated too much. From this, in order to manufacture the target of the present invention, the TM foam metal has an average pore diameter of 1.
It is necessary that the thickness is 0 μm or more and 3.0 mm or less.

Other composition systems, DyFeCo, TbGdFeCo.

TbFe, GdFeCo, GdDyFeCo, GdDy
TbFeCo, DyTbFeCo, TbCo, GdTb
It is necessary to use pore diameters in the same range for all composition systems containing at least one heavy rare earth metal such as Fe, TbDyCo, etc., and at least one transition metal among Fe and Co. It was confirmed that there is.

As mentioned above, in the impregnation method or infiltration method, which is one of the methods of the present invention, the porosity, particle size, and pore size of the powder or metal foam are important, and it is necessary to use a material within a specific range. It turns out that there is.

On the other hand, the composition of the mother alloy is also important, and the balance between the mother alloy financial point for impregnation and the metal structure of the mother alloy, that is, the ratio of rare earth single phase to rare earth and transition metal 2 alloy phase, is important.
The master alloy composition is determined. This will be specifically explained in the following examples.

[Example 8-1] The method of the present invention when creating NdDyFeCo by an impregnation method is as follows:
This is as described in Example 3-1.4-4, etc., and (Ndo, z D)'o, 5) tz, z (Feo
, e COo, z) zy, eat % composition. This total acid has a eutectic composition near the rare earth metal (RE) side in the phase diagram, has a low melting point (about 830° C.), and is convenient for preparation by the impregnation method. In this example, the range of the master alloy composition was examined to see if it was possible to create a target by the impregnation method.

Same Fe7-Co powder as Example 3-1 (porosity 62.4
%), various master alloy compositions were prepared, and targets were created by the impregnation method. The following table shows the composition of the master alloy used, the melting point of the composition, and the finished state of the impregnated target heated at the melting point.

Table 11 Master alloy composition (at%) Melting point r:c) Target finished state (NdD)') 4. (FeCo)s+
Partial force decomposition of 1220 FeCo powder (NdDy
) so (FeCo) so 1200 completely impregnated with powder (NdDy) ss (FeCo) ns 11.
50 Impregnated in complete powder state (NdD)') 6s (F
eCO)+s 980 Impregnated in complete powder state (
NdD)')7z(FeCo)zs 850
Impregnated in powder complete state (NdDy) we (FeCo)zz
1000 Completely impregnated with powder (NdDy)e
z (FeCo) + a 1100 Impregnated in complete powder state (NdD3') to (FeCO) + o 1200
Impregnated in complete powder state (NdD)')q+(FeC
O) v 1230 18. Compounding of Fe-Co powder According to the results in the above table, if a master alloy with a melting point exceeding 1200°C is used, a part of the Fe-Co powder will begin to melt and the impregnation method will not work. I understand. A target using a master alloy with a melting point below 1200°C will not melt FeCo powder,
The target was successfully created using the impregnation method. In other words, it is necessary to use a master alloy composition having a melting point of 1200° C. or lower.

Other composition systems, PrTbFeCo, SmGdFeCo, S
mDyTbFeCo, NdTbFeCo.

NdGdFeCo, NdPrDyFeCo, NdPrD
yTbFeCo, PrDyFeCo, NdSmGdTb
FeCo, CeNdDyFeCo.

Sm, Nd, Pr such as CeNdPrDyFeCo.

At least one light rare earth metal among Ce and Gd
For all composition systems containing at least one heavy rare earth metal among , Dy, and Tb and at least one transition metal among Fe and Co, it is necessary to use a master alloy with a melting point in the same range. I'm ill-advised that there is.

[Example 8-2] Various master alloy compositions of TbFeCo were prepared, and targets were created by an impregnation method. The manufacturing method is the same as the method shown in Example 3-5. Feq. C (11°at% powder with a porosity of 43%) was prepared, and impregnation method targets were created using various mother alloy compositions.The table below shows the mother alloy compositions used, their melting points, and their This figure shows the finished state of an impregnated target created by heating to the melting point.

Table 12 Master alloy composition (a, t%) Nine hanging points (°C) Target finished state Tb5q (FeCO)i, + 12
10 Partial force melting of FeCo powder Tbao (Fe
Co),, o 1200 Impregnated Tb in a complete powder state, (FeCo powder 1100 Impregnated Tb in a complete powder state, t(FeCo)t 1000
Impregnated Tb7□(FeCo)ill in powder state
850 Impregnated Tb7s (Fe
Co)zz 1000 Impregnated in complete powder state Tb*a (F e Co)+v 1100
Impregnated Tbiw(FeCO)u in powder complete state
1200 Impregnated in powder complete state Tbqo (
FeCo) + z 1220 = of FeCo powder
According to the results in the table above, NdDyFeCo
Similarly, it can be seen that when a master alloy with a melting point exceeding 1200° C. is used, a part of the Fe-Co powder begins to dissolve and the impregnation method cannot be used. In a target using a master alloy with a melting point of 1200° C. or lower, even the FeCo powder did not dissolve, and the target was successfully formed by the impregnation method. In other words, it is necessary to use a master alloy composition having a melting point of 1300''C or less.

Other composition systems, DyFeCo, TbGdFeCo.

TbFe, GdFeCo, GdDyFeCo, GdDy
TbFeCo, DyTbFeCo, TbCo, CdTb
Gd, Tb such as Fe, TbDyCo.

Minor amounts of Dy (including one or more heavy rare earth metals and Fe)
It was confirmed that it is necessary to use a master alloy having a melting point in the same range for all composition systems containing at least one transition metal among , Co, and at least one transition metal.

NdDyFeCo shown in these Example 8-1.8-2
, by various mother alloy compositions used in TbFeCo system, etc.
The metal structure of the finished target will be different. In other words, the amounts of the intermetallic compound phases of RE and -TM2 are different. If a master alloy composition with less RE is used, for example RE, 7M6°, the number of intermetallic compounds will increase, and conversely, if a master alloy composition with more RE, for example RE, TM, is used, the number of intermetallic compounds will increase. The compound phase is reduced. The optimum mother alloy composition is selected depending on the sputtering apparatus or film forming method used.

When the amount of intermetallic compound phase cannot be controlled solely by the mother alloy composition, the following method may be used. In other words, by heat-treating the completed target again at a temperature below its melting point, the intermetallic and compound phases can be controlled.

[Example 9-1] Various heat treatments were performed using the NdDyFeCo-impregnated target prepared in Example 3-1 (NdD y) +
We looked at the amount of the intermetallic compound phase of (F e CO) 2. The heat treatment conditions and the amount of intermetallic compound phase are shown in the table below. The heat treatment was performed in a vacuum with no pressure applied.

Table 13 Heat treatment conditions Amount of intermetallic compound phase <area%) Untreated 10 400°C 2hr 11 400°C 10hr 15 400°C 20hr 20 600"C2hr 12 600'C10hr 20 600"C20hr 30 700'C2hr 14 700°C 10hr 30 700 ℃20hr 50 700℃25hr 60 As shown in the table above, it can be seen that the higher the temperature and the longer the time, the greater the amount of intermetallic compounds.

Since this is a phenomenon caused by solid phase diffusion, it is natural that it is related to temperature and time.

The optimum amount of these intermetallic compounds is determined by the sputtering device and sputtering method. A few specific examples are described below.

In the case of a sputtering device as shown in Fig. 2,
If the substrate holder 22 is rotating and the attached substrate rotates on its own axis (that is, the substrate rotates around itself),
Any amount of intermetallic compound may be used. However, if the substrate does not rotate (in other words, only revolves),
The amount of intermetallic compounds is preferably about 10 to 30 area%. Among these, which amount is optimal depends on the distance between the target substrates,
It is determined by the distance between the target center and the substrate holder center and the sputtering conditions (Ar pressure, power).

In the case of a sputtering apparatus as shown in FIG.
The target 31 and the substrate 332 are facing each other, and the substrate is also stationary without moving. In this case, the amount of intermetallic compounds is 1
Approximately 5 to 40 area% is good.

Which of these amounts is optimal depends on the distance between the target boards,
It is determined by the sputtering conditions (Ar pressure, power).6 In the case of a sputtering apparatus as shown in Fig. 34, in which the substrate passes over the target, the amount of intermetallic compounds is 20 to 6.
About 0 area% is good (341 is the target, 342
is the board). Which of these amounts is optimal depends on the distance between target substrates, sputtering conditions (A, r pressure, Power
), determined by the presence or absence of an anti-adhesion plate.

Other composition systems PrTbFeCo, SmGdFeCo, Sm
DyTbFeCo, NdTbFeCo.

NdGdFeCo, NdPrDyFeCo, NdPrD
yTbFeCo, PrDy, FeCo, NdSmGdT
bFeCo, CeNdDyFeCo.

Sm, Nd, Pr such as CeNdPrDyFeCo.

At least one light rare earth metal among Ce and Gd,
Results similar to those of this example were obtained for all composition systems containing at least one heavy rare earth metal among Dy and Tb and at least one transition metal among Fe and Co. .

[Example 9-2] Various heat treatments were performed using the TbFeCo-impregnated target prepared in Example 3-5 to obtain T b I (FeCo).
We looked at the amount of intermetallic compound phase in . The heat treatment conditions and the amount of intermetallic compound phase are shown in the table below. The heat treatment was performed in a vacuum with no pressure applied.

Table 13 Heat treatment conditions ffi (area) of intermetallic compound phase
%) Untreated 7% 400℃ 3hr 8% 400℃ 15hr 12% 400℃ 30hr 17% 400℃ 60hr 27% 650℃ 3hr 10% 650℃ 15hr 22% 650℃ 30hr 37% 750℃ 2hr
11% 750° C. 15 hr 37% 750° C. 30 hr 67% As in the case of Example 9-1, the higher the heat treatment temperature and the longer the heat treatment time, the greater the amount of intermetallic compounds.

The optimum amount of these intermetallic compounds is determined by the sputtering device and sputtering method.

Other composition systems, DyFeCo, TbGdFeCo.

TbFe, GdFeCo, GdDyFeCo, GdDy
TbFeCo, DyTbFeCo, TbCo, GdTb
Gd, Tb such as Fe, TbDyCo.

At least one heavy rare earth metal among Dy and Fe
, Co, and at least one type of transition metal, results similar to those of this example were obtained.

In the method of the present invention described so far, when a powder or foam metal is used and a master alloy ingot is placed on top of it and manufactured by the impregnation method, it is necessary to control the composition of the powder or foam metal. Porosity needs to be controlled. The method described below uses powder, but the composition can be controlled without controlling the porosity.
This is a method that allows rJ.

Briefly, a transition metal powder and a powder obtained by pulverizing a rare earth transition metal master alloy ingot having a near eutectic composition are appropriately mixed, and the mixture is sufficiently mixed until the mixture becomes uniform. After that, in the mold,
Add this mixed powder and heat to around 000°C (no pressure)
After cooling, the molded body is processed to create a target.

[Example 1O-1] NdD)'FeCo will be described. First, as a raw material (
N do,z D )'o,++)tz,z (F e
o, s COo, z) Create a mother alloy ingot with zt, aat%. This ingot is roughly crushed using a show crusher, and then crushed using a ball mill or the like until it has an average particle size of 2008 m. And 200um of Fe so COzoa tz
Prepare a powder with a certain particle size and thoroughly mix it with the mother alloy powder.

The amounts of this FeCo powder and NdDyFeCo master alloy powder are:
In total N ds, s D )'zz, oF es*, o
They are mixed in such a quantitative ratio that c Ox and oa tz are obtained. Then, put this mixed powder into a crucible with an inner diameter of 4'φ,
After vacuuming, heat to 1050"C without applying pressure. At this time, the mother alloy powder is melted, but the FeCo powder is not. Therefore, the unmelted FeCo powder is surrounded by the molten mother alloy, and cooled. When this happens, the molten master alloy is separated into two phases, NdDy and (NdDy)+(FeCo)z, resulting in a three-phase mixed target.

Since the composition of the finished target is determined by the ratio of the initially mixed master alloy powder to the FeCo powder, there is no need to control the porosity of the powder, making it easier to control.

The target thus prepared was mounted on a sputtering apparatus similar to that shown in Fig. 2, a film was formed, and its magnetic properties and composition distribution were evaluated. As a result, the RE was 28 to 28.5 at%.
Hc was uniform at 9.7 to 10.5 KOe. Furthermore, the amount of oxygen was as low as 490 ppm, and sputtering was stable from the beginning even after being left in the atmosphere for 24 hours, and the film magnetic properties were similarly stable from the beginning.

This manufacturing method uses powder, but since it is not a sintering method and one of the mother alloy powders is completely dissolved, the packing density is 99.3%, and surface oxidation will progress to the inside even if left in the air. Never.

Other composition systems, PrTbFeCo, SmGdFeCo, S
mDyTbFeCo, NdTbFeCo.

NdGdFeCo, NdPrDyFeCo, NdPrD
yTbFeCo, PrDyFeCo, NdSmGd
TbFeCo, CeNdDyFeCo.

CeNdPrDyFeCo, etc. Sm, Nd, Pr, C
at least one heavy rare earth metal of e, and Fe
The same manufacturing method is possible for all composition systems containing at least one transition metal among Co,
It was also confirmed that similar effects existed.

(Example 1O-2) Next, TbFeCo will be described. First, Tb as a raw material
Master alloy ingots of ttFezh, zcO+, and Ila tz are made. This ingot is roughly crushed using a show crusher, and then crushed using a ball mill or the like until it has an average particle size of 200 am. And F eq3. bc O6, 2 of 48t%
A powder having a particle size of 00 μm is prepared and thoroughly mixed with the above-mentioned mother alloy powder. The FeCo powder and the TbFeCo master alloy powder are mixed in such a ratio that the total amount of Tt)zzFe is 5 cOsat%. This mixed powder was then put into an alumina mold with an inner diameter of 4'' and heated in an atmosphere of 1050'C under vacuum (no pressure applied). After that, it was cooled, and the resulting molded body was processed and used as a sputtering target. This coupe 6. is Tb, Tb+(FeCo)z, FeCo
It consists of three phases.

Then, it was installed in a film forming apparatus similar to that shown in Fig. 2, and film formation was attempted.
As a result of evaluating the composition distribution and magnetic property distribution inside the substrate holder, the RE was 21. 5-22. The magnetic properties were uniform at 0 at%, and the magnetic properties were also uniform at Hc of 14.5 to 15.2 KOe. Further, the target oxygen amount was 440 ppm, and the packing density was 99.5%, which was good. Sputtering remained stable from the beginning even after being left in the atmosphere for 24 hours.
The film magnetic properties were similarly stable from the beginning.

Other composition systems, DyFeCo, TbGclFeC.

, TbFe, GdFeCo, GdDyFeCo.

GdDyTbFeCo, DyTbFeCo, TbCo,
The same manufacturing method can be used for all composition systems containing a small amount of Gd, Tb, and Dy, such as GdTbFe and TbDyCo (all containing one or more heavy rare earth metals and at least one or more transition metals among Fe and Co). It was also confirmed that similar effects exist.

It goes without saying that in the case of the method of the present invention (Examples 10-1, 10-2), the entire composition must have a melting point of 1200°C or less, as in Example 8-1.8-2. That's a good thing.

The transition metal powder or foamed transition metal used in the present invention (Example 1-1) to (Example 1O-2) described above is based on an FeCo alloy. The alloy is RE-FeC.

It was also confirmed that it is possible to create a target using RE-Co, and a similar target of the present invention can be created. It has also been confirmed that similar effects can be achieved. Further F
eCo alloy base, or C.

Using base powder or foam metal, RE-
Even when Fe alloy was used, the target of the present invention could be created in the same way, and similar effects could be confirmed. As a matter of course, it was also possible to create the target of the present invention using a mixture of Fe powder and Go powder.

In addition to the rare earth transition metal compositions shown in the present examples, T
Even if additives such as i, Cr, Al, Zr, Pt, Au, Ag, Cu, etc. or unavoidable impurities such as St, Ca, C, etc. are mixed, production by the method of the present invention is possible, and similar It has also been confirmed that there are effects.

〔Effect of the invention〕

In this way, the rare earth transition metal sputtering target made by the method of the present invention can be used in various sputtering devices.
Sputtering with a uniform composition distribution within the film formation surface is possible, the amount of oxygen is low, the packing density is high, and sputtering is stable from the initial stage.

Furthermore, even if the film is left in the atmosphere, sputtering is stable from the beginning, and the magnetic properties of the film are also stable.

[Brief explanation of the drawing]

FIG. 1 is a schematic diagram of the surface structure of a sputtering target produced by the method of the present invention. FIG. 2 is a schematic diagram of a sputtering device. FIG. 3 is a diagram showing the composition distribution and magnetic property distribution in the substrate holder using the NdDyFeCo target of the present invention. FIG. 4 is a schematic diagram of the surface structure of a conventional casting alloy NdDyFeCo target. FIG. 5 is a diagram showing the composition distribution and magnetic property distribution in the substrate holder using a conventional casting alloy NdDyFeCo target. FIG. 6 is a diagram of the composition distribution and magnetic property distribution in the substrate holder using a semi-molten NdDyFeCo target. Figure 7 shows the NdDyFe of the present invention after being left in the atmosphere for 24 hours.
FIG. 3 is a diagram showing the relationship between sputtering time and film magnetic properties for a Co target and a semi-molten NdDyFeCo target. FIG. 8 is a sputtering time dependence diagram of the film magnetic properties of the semi-molten NdDyFeCo target with respect to the exposure time in the atmosphere. FIG. 9 is a diagram of the composition distribution and magnetic property distribution in the substrate holder using the TbFeCo target of the present invention. FIG. 10 is a diagram showing the composition distribution and magnetic property distribution in the substrate holder using a conventional cast alloy TbFeCo target. FIG. 11 is a diagram of the composition distribution and magnetic property distribution in the substrate holder using a semi-molten TbFeCo target. Figure 12 shows the TbFeC of the present invention after being left in the atmosphere for 24 hours.
Figure 2 is a diagram showing the relationship between the sputtering time and film magnetic properties of the o target and the semi-molten TbFeCo target. FIG. 13 is a sputtering time dependence diagram of the film magnetic properties of the semi-molten TbFeCo target with respect to the exposure time in the atmosphere. FIG. 14 is a schematic diagram of the manufacturing method of the present invention using an impregnation method. FIG. 15 is a schematic diagram of the surface structure of the target of the present invention obtained by the impregnation method. FIG. 16 is a diagram of the composition distribution and magnetic property distribution in the substrate holder using the target of the present invention by the impregnation method. FIG. 17 is a schematic diagram of the metal structure of the target of the present invention using a foamed metal sheet. FIG. 18 is a diagram of the composition distribution and magnetic property distribution in the substrate holder using the target of the present invention made of a foamed metal sheet. FIG. 19(a) is a schematic diagram of a master alloy ingot using powder with a porosity of about 30% before melting. FIG. 19(b) is a schematic diagram of a place where a master alloy using powder with a porosity of about 30% is melted and impregnated. FIG. 20(a) is a schematic diagram of a master alloy ingot using powder with a porosity of about 80% before melting. FIG. 20(b) is a schematic diagram of a place where a master alloy using powder with a porosity of about 80% is melted and impregnated. Figure 21 shows NdDyFeCo using various porosity powders.
Composition distribution diagram inside the target substrate holder. Figure 22 shows NdDyF using various porosity foam sheets.
A composition distribution diagram of the eCo target in the substrate holder. FIG. 23 is a composition distribution diagram in the substrate holder of a TbFeCo target using various porosity powders. Figure 24 shows TbFeC using various porosity foam sheets.
o A composition distribution diagram of the target in the substrate holder. Figure 25 shows Nd using powder with a particle size of 10 μm to 570 μm.
A diagram showing the relationship between film magnetic properties and sputtering time of a DyFeCo target. Figure 26 shows the N
dA diagram showing the relationship between film magnetic properties and sputtering time of a DyFeCo target. Figure 27 shows T
b A diagram showing the relationship between film magnetic properties and sputtering time of a FeCo target. Figure 28 shows T
b A diagram showing the relationship between film magnetic properties of a FeCo target and sputtering time. FIG. 29 is a diagram showing the relationship between film magnetic properties and sputtering time of an NdDyFeCo target using a foamed metal with a pore size of 10 μm to 570 μm. Figure 30 shows 730 μm to 4. A diagram showing the relationship between film magnetic properties and sputtering time of a NdDyFeCo target using Qmm pore diameter foam metal. FIG. 31 is a diagram showing the relationship between film magnetic properties and sputtering time of a TbFeCo target using foamed metal with a pore diameter of 10 μm to 570 μm. FIG. 32 shows 730 μm to 4. A diagram showing the relationship between film magnetic properties and sputtering time of a TbFeCo target using a foamed metal with a pore size of 0 mm. FIG. 33 is a schematic diagram of a sputtering apparatus in which a substrate faces a target and is stationary. FIG. 34 is a schematic diagram of a sputtering apparatus in which a substrate passes over a target. FIG. 35 is a structural diagram of a magneto-optical recording medium. 1 ・” (N d D y) + 3 (F e C0) 6
7 a t% composition phase 2...FeCo composition phase 3...FeDy composition phase 21...sputtering target 22...substrate holder 41 ・" (Ndo, +zD)'0.1111)
25 (F eo, ec 00.2) 75 at% composition phase 42- (N do, + D Yo, t) + x,:
+ (F eo, ac Oo, t) bh, 7 at% composition phase 71...Target of the present invention 72...Semi-molten method target 81...Leave in the atmosphere for 10 minutes 82...Leave in the atmosphere for 30 minutes 83...・Leave in the atmosphere for 1 hour 84...Leave in the atmosphere for 5 hours 85...Leave in the atmosphere for 10 hours 121...Target of the present invention 122...Semi-melting method target 131...Leave in the atmosphere for 10 minutes 132...Leave in the atmosphere 30 minutes 133...Leave in the atmosphere for 1 hour 134...Leave in the atmosphere for 3 hours 141...Crucible 142...High frequency induction heating coil 143...R+R+Tz master alloy 144-F esoCozoa t% powder 151-F
e -Co particles 1, 52...Nd-Dy rare earth metal single phase 153-
(Rare earth transition metal alloy phase 171-F eqz of NdDyL (FeCo)z, single phase 172 of bc 06.4 at%...Single phase 173 of rare earth gold Ji (Tb)
...Alloy phase of transition metal and rare earth metal (TbFeCo) 211...30% porosity powder target 212...
Powder target 213 with 40% porosity...50% porosity
Powder target 214...62% porosity powder target 215...70% porosity powder target 216...
・Powder target 221 with porosity of 80%...porosity of 30
% foam sheet target 222...porosity 40% foam sheet target 223...porosity 50% foam sheet target 224...porosity 62% foam sheet target 225...pores Target 226 of foam sheet with 70% porosity...Target 231 of foam sheet with 80% porosity...Target 232 of powder with 30% porosity...
...Powder target 233 with porosity 43%...Porosity 5
0% powder target 234...60% porosity powder target 235...70% porosity powder target 236
...Powder target 241 with porosity 80%...Target 242 of foam sheet with porosity 30%...Porosity 43
% foam sheet target 243...porosity 50% foam sheet target 244...porosity 60% foam sheet target 245...porosity 70% foam sheet target 246...pores 80% foam sheet target 251...Target 252 using 10 μm particle size powder...Target 25 using 24 μm particle size powder
3...Target 254 using 38 μm particle size powder...
・Target 255...12 using 53 μm particle size powder
0μm20μm particle size powder target 256...230μ
m30μm particle size powder target 257...57 (11I
Target 261...730μm3 using m particle size powder
0μm particle size powder target 262...Target 263 using 1.0 mmmm particle size Target 264 using 1.5 mmmm particle size Target 265 using 2.5 mmmm particle size Target 266 used: 3.2 mmmm particle size Target 267: 4.0 mmmm particle size used Target 2
71...Target 272 using 10 μm particle size powder
...Target 273...3 using 24 μm particle size powder
Target 274...53μm using 8μm particle size powder
Target using particle size powder 275...120μm20
μm particle size powder target 276...230μm30μm
Particle size powder target 277...Target using 570 μm particle size powder 281...730 gm30 μm particle size powder target 282...Target using 1.0 mmmm particle size 283...Target 284 using 1.5 mmmm particle size ...Target 28 using 2.5mmmm particle size
5...Target 286 using 3.0mmmm particle size
...Target 287 using 3.2mmmm particle size...
Target 291...10 using 4.0mmmm particle size
μm Target using foamed metal with pore size 292...248m Target using foamed metal with pore size 293...388m Target using foamed metal with pore size 294...538m Target using foamed metal with pore size 295. ...Target 296 using foamed metal with a pore size of 1208m...Target 297 using foamed metal with a pore size of 230μm...Target 3 using foamed metal with a pore size of 570μm (11...using foamed metal with a pore size of 7308m Target 3 (12...using foamed metal with a pore size of 1.0 mm) Target 3 (13...using a foamed metal with a pore size of 1.5 mm) Target 3 (using a foamed metal with a pore size of 2.5 mm) Target 305: Target 305 using foam metal with a pore size of 3.0 mm Target 307 using foam metal with a pore size of 3.2 mm Target 311 using foam metal with a pore size of 4.0 mm ...Target 312 using foamed metal with a pore size of 10μm...Target 313 using foamed metal with a pore size of 248m...Target 314 using foamed metal with a pore size of 38μm...Target using foamed metal with a pore size of 538m Target 315...120 tIm pore size using foamed metal 316...230 μm pore size target using foam metal 317...570 μm pore size target using foam metal 321...730 gm pore size foaming Target using metal 322...Target using foam metal with 1.0 mm pore diameter323...Target using foam metal with 1.5 mm pore diameter324...Target using foam metal with 2.5 mm pore diameter 325...Target using foamed metal with 3.0mm pore diameter 326...Target using foamed metal with 3.2mm pore diameter 327...Target using foamed metal with 4.0mm pore diameter 331...Target 332...Substrate 341...Target 342...Substrate 351...Polycarbonate substrate 352...A/!SiN dielectric film 353=NdDyFeCo magneto-optical recording film 354...
Aj2SiN dielectric film and above Applicant: Seiko Epson Co., Ltd. Representative Patent Attorney Masayoshi Kamiyanagi and one other person Figure 2 667 Female - CR・Kc,'. Large 3-'P8i Otsu1inch r81i'kty>λt 'f
・・t 9 II+fa'J(?=0)
(?-15″e-)1 da 3 7 1st te figure C 卜・') (?'・15
)0"'°") Figure 18 ("'g9 note 1 (1
Figure (α) 19th figure (b) 2/Otsu (Yn 15Q-) 23rd C and -l Dahino Figure 27

Claims (1)

[Scope of Claims] (1) A cast alloy target for manufacturing a magneto-optical recording layer made of a rare earth transition metal alloy by sputtering, wherein the metal structure in the cast alloy target is a rare earth metal elemental phase and a transition metal elemental phase. A sputtering target characterized by comprising a rare earth transition metal alloy phase. (2) The main composition of the sputtering target is at least one light rare earth metal (LR) selected from Sm, Nd, Pr, and Ce, and at least one heavy rare earth metal selected from Gd, Tb, and Dy. (HR),
2. The sputtering target according to item 1, further comprising at least one transition metal (TM) selected from Fe and Co. (3) The main composition of the sputtering target is at least one heavy rare earth metal (HR) selected from Gd, Tb, and Dy, and Fe and Co.
2. The sputtering target according to claim 1, comprising at least one transition metal (TM) among the following. (4) In the sputtering target, a transition metal powder and a rare earth transition metal alloy ingot are placed in a mold, and the inside of the mold is heated at a temperature between the melting point of the transition metal and the melting point of the ingot. The method for producing a sputtering target according to item 1, item 2, or item 3, characterized in that the sputtering target is produced by processing a molded product obtained by cooling. (5) The sputtering target includes a foamed transition metal sheet and a rare earth transition metal alloy ingot placed in the mold at a temperature between the melting point of the transition metal sheet and the melting point of the ingot. The method for producing a sputtering target according to item 1, item 2, or item 3, characterized in that the sputtering target is produced by processing a molded product obtained by heating and then cooling. (6) The sputtering target is placed in a mold as a mixed powder of transition metal powder and rare earth transition metal alloy powder, and the sputtering target is placed in the mold at a melting point between the transition metal and the rare earth transition metal alloy. The first method is characterized in that it is produced by processing a molded product obtained by heating and then cooling.
The method for manufacturing a sputtering target according to item 1 or 2 or 3. (7) The sputtering target has a porosity of 30
5. The method for producing a sputtering target according to item 4, wherein the sputtering target is produced using transition metal powder of % or more and 80% or less. (8) The sputtering target has a porosity of 30
6. The method for producing a sputtering target according to item 5, wherein the sputtering target is produced using a foamed transition metal sheet of % or more and 80% or less. (9) In the method for manufacturing a sputtering target, the average particle size of the transition metal powder is 10 μm or more; 3.
5. The method for manufacturing a sputtering target according to item 4, wherein the sputtering target has a diameter of 0 mm or less. (10) In the method for producing a sputtering target, the average pore diameter of the foamed transition metal sheet is 1.
Fifth, characterized in that it is 0 μm or more and 3.0 mm or less
A method for manufacturing a sputtering target as described in . (11) In the method for producing a sputtering target, the composition of the rare earth transition metal ingot has a melting point of 1.
7. The method for producing a sputtering target according to item 4, item 5, or item 6, characterized in that the ingot having a composition of 200° C. or less is used. (12) In the method for producing a sputtering target, the fourth method is characterized in that the molded body is heat-treated.
6. The method for manufacturing a sputtering target according to item 5. (13) In a magneto-optical recording medium in which at least one dielectric film and at least one magneto-optical recording film are present on a transparent substrate, the sputtering target according to item 1, 2 or 3 is used. A magnetic recording medium characterized in that it is manufactured using the magnetic recording medium.