JP3417457B2 - Target containing MgO as main component and method for producing the same - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a target suitable for forming a MgO film for protecting a dielectric layer of an AC type plasma display panel by a sputtering method and a method for manufacturing the target.

[0002]

2. Description of the Related Art In recent years, liquid crystal (Liquid Crystal Display:
Research and development and practical application of various flat displays such as LCD) are remarkable, and the production thereof is also rapidly increasing. The development and commercialization of color plasma display panels (PDPs) have also become active recently. PDPs tend to be large in size and are at the shortest distance from large-screen wall-mounted TVs for high-definition televisions, and trial production of PDPs with a diagonal size of 40 inches is already underway. PDPs are classified into an AC type in which a metal electrode is covered with a glass dielectric material and a DC type in which a metal electrode is exposed in a discharge space in terms of an electrode structure.

At the beginning of the development of this AC type PDP, since the glass dielectric layer was exposed in the discharge space, it was directly exposed to a discharge, and the surface of the dielectric layer was changed by the sputtering of ion bombardment, so that the discharge starting voltage was increased. It was rising. Therefore, attempts have been made to use various oxides having high heat of sublimation as protective films for this dielectric layer. This protective film plays an important role because it is in direct contact with the discharge gas. That is, the characteristics required for the protective film are low discharge voltage, sputtering resistance during discharge, fast discharge response, and insulation. As a material satisfying these conditions, M
gO is used for the protective film. This protective film made of MgO protects the surface of the dielectric layer from sputtering during discharge and plays an important role in extending the life of the PDP.

Currently, as the protective film of the AC type PDP,
An MgO film formed by an electron beam evaporation method using a crushed single crystal MgO as an evaporation material is known. The MgO film formed by this electron beam evaporation method can be formed at a high speed of 1000 angstroms / minute or more. Regarding the crystal orientation of the formed MgO film, the film oriented to the (111) plane can be driven with the lowest sustaining voltage, and further exists in the film (11
1) As the amount of surface increases, the emission ratio of secondary electrons increases,
It is said that the driving voltage will also decrease. The above single crystal M
The crushed product of gO is obtained by melting MgO clinker having a purity of 98% or more and light-burning MgO (MgO sintered at 1000 ° C. or less) in an electric arc furnace (arc furnace), that is, after forming an ingot by electric melting, It is manufactured by taking out a single crystal part from this ingot and crushing it.

[0005]

However, in the electron beam evaporation method using the above-mentioned conventional crushed single crystal MgO as an evaporation material, there is an advantage that the film formation speed is high, but on the other hand, splash or a film formation occurs. When the area is large, there is a problem that it is difficult to make the film thickness uniform. In order to solve this point, a method of forming a MgO film by a sputtering method can be considered. However, in this method, a MgO sintered body having a high insulating property is required as a target material, and in order to further increase the film forming speed, A dense MgO sintered body is required. In addition, the above MgO
The density of the MgO sintered body, the purity,
The crystal grain boundaries and the texture structure within the crystal grains influence.

Generally, the MgO sintered body has excellent heat resistance, corrosion resistance and electric insulation, but it is poor in strength, fracture toughness and thermal shock resistance, and it was difficult to use it as it is as a target material for the sputtering method. In order to eliminate this point, various sintering aids can be added to increase the density of the MgO sintered body, but this method also systematically improves the MgO crystal grain boundaries of the MgO sintered body. Due to the presence of defects, there is a problem that the orientation of the MgO film is inferior and the film formation rate cannot be increased.

An object of the present invention is to improve strength, fracture toughness value and thermal shock resistance, and to form a Mg film formed by a sputtering method.
It is an object of the present invention to provide a target containing MgO as a main component and a method for producing the same, which can improve the orientation of the O film and the film formation rate. Another object of the present invention is to provide a MgO film that can be formed by a sputtering method to obtain a MgO film having a low discharge voltage, a sputtering resistance during discharge, a fast discharge response, and a high insulating property. It is to provide a target containing a main component and a method for manufacturing the target.

[0008]

The invention according to claim 1 is
As shown in FIG. 1, the average crystal grain size is 0.5 to 100 μm.
LaB _{6 in} MgO matrix with crystalline particles 1 of
This is a target whose main component is MgO in which particles 2 are dispersed in an amount of 1 to 25% by volume. MgO described in claim 1
In the target containing Mg as the main component, there is no anisotropy, that is, in the MgO matrix crystal grain or in the crystal grain boundary 3 where the physical properties such as the coefficient of thermal expansion in the predetermined biaxial (a-axis and c-axis) directions are the same. By performing the compounding in which the LaB ₆ particles 2 are dispersed, it is possible to improve the physical properties of the target of the MgO composite material that is the ceramic sintered body. For example, when SiC particles are dispersed in an Al ₂ O ₃ matrix, the coefficient of thermal expansion of the dispersed particles is not more than 1/2 of the coefficient of thermal expansion of the matrix. The stress generated around and inside the dispersed particles during the sintering process is 1000 to 1
Reach 800 MPa. If this stress increases, cracks may run at the interface between the matrix and the dispersed particles, and in order to prevent this, only very fine SiC particles can be dispersed.

On the other hand, the coefficient of thermal expansion of the LaB ₆ particles 2 of the present invention becomes soft at a high temperature, so at 1300 ° C., the coefficient of thermal expansion of MgO (about 12 × 10 ⁻⁶ / ° C.) is about 0.
8 times. Due to the thermal behavior of the dispersed particles with respect to the MgO matrix at high temperature, the matrix and the dispersed particles are strongly bonded to each other at the three crystal grain boundaries of the matrix during sintering. When used as a target due to the strong bonding at the three crystal grain boundaries, sputtering does not cause cracking or abnormal discharge of the target even if sputtering is performed at a high voltage that can achieve a film formation rate of 600 Å / min or more. The formed MgO film has a low discharge voltage, sputtering resistance during discharge, fast discharge response, and high insulation. As a result, it becomes suitable as a protective film for the dielectric layer of the AC type PDP. On the other hand, as described above, the LaB ₆ particles 2 which are dispersed particles become soft at high temperature, and therefore the difference in the coefficient of thermal expansion between the matrix and the dispersed particles becomes small at high temperature. As a result, the LaB ₆ particles 2 having a relatively large particle size can be dispersed in a range that does not cause cracks in the crystal grain boundaries 3 of the matrix, so that the total area for tightening the crystal grain boundaries 3 becomes large, and The number of defects of 3 is small and the strength is improved.

The invention according to claim 2 relates to MgO powder and La.
A step of wet mixing the B ₆ powder, a step of dry crushing the mixture after drying with heating under reduced pressure, and the step of forming the mixed powder were dry-pulverized, the molded body 1300-1
And a step of sintering at a temperature of 650 ° C. for manufacturing a target containing MgO as a main component. When the target is manufactured by the manufacturing method according to the second aspect, the dispersed particles are uniformly dispersed in the MgO matrix, the matching of the crystal grain interfaces is good, and the defects of the crystal grain boundaries are small, that is, the structure is good. A controlled target is obtained.

The invention according to claim 3 is the invention according to claim 2, characterized in that the molded body is further heated to 1400 to 1650 ° C in a vacuum or in an inert gas atmosphere and sintered. To do. The invention according to claim 4 is the invention according to claim 2, further comprising heating the molded body to 1300 to 1350 ° C. in vacuum or in an inert gas atmosphere at normal pressure to perform primary sintering,
Further, in vacuum or in an inert gas atmosphere at normal pressure, 1450 to
It is characterized in that the temperature is raised to 1650 ° C. and secondary sintering is performed.
The invention according to claim 5 is the invention according to claim 3 or 4, characterized in that the temperature is raised to 700 to 900 ° C. in a reducing gas atmosphere for reduction treatment before the compact is further sintered. And When the target is manufactured by the manufacturing method described in any one of claims 3 to 5, a target having a better controlled texture can be obtained.

According to the invention of claim 6, MgO powder and La
A step of wet mixing the B ₆ powder, a step of dry crushing the mixture after drying with heating under reduced pressure, the mixed powder was dry pulverized in an inert gas atmosphere from 1450 to 1,650 ° C.
The method of manufacturing a target containing MgO as a main component, the method including the step of raising the temperature to sinter and sintering. When the target is manufactured by the manufacturing method according to the sixth aspect, the target can be made more precise and the number of manufacturing steps can be reduced.

[0013]

BEST MODE FOR CARRYING OUT THE INVENTION Next, embodiments of the present invention will be described. The target containing MgO as a main component of the present invention is a ceramic sintered body, MgO is used as a matrix, and LaB ₆ particles are used as dispersed particles. The average crystal grain size of MgO is 0.5 to 100 μm, preferably 2 to 50 μm, and the average grain size of dispersed particles is 2.0 μm.
m or less, preferably 1.0 μm or less, and the content ratio of the dispersed particles to the matrix is 1 to 25% by volume,
It is preferably 5 to 20% by volume. Here, the content ratio of the dispersed particles is a ratio of the inner content to the total of MgO and the dispersed particles.

The average crystal grain size of MgO is 0.5 to 100 μm.
The reason why it is limited to m is that the tissue can be controlled in this range. Further, the reason why the average particle size of the dispersed particles is limited to 2.0 μm or less is to facilitate the control of the MgO structure,
This is because microcracks do not occur even when the residual stress exceeds the predetermined limit. On the other hand, if the average particle size of the dispersed particles exceeds 2.0 μm, microcracks are likely to occur. Further, the addition amount of the dispersed particles is limited to 1 to 25% by volume, because if it exceeds 25% by volume, the control of the material structure becomes difficult, the spatter resistance and the insulating property vary, and the reliability of the material is lost. is there. Further, when the amount of the dispersed particles added is within the above range, the structure can be controlled so that the dispersed particles are uniformly taken into the matrix, and the characteristics of the formed film are improved.

A method of manufacturing the target of the present invention having the above structure will be described. First, the average particle size is 0.1-5μ
1 to 20% by volume of LaB ₆ powder having an average particle diameter of 0.2 to 2 μm is mixed with MgO powder of m, preferably 0.2 to 1 μm, and further wet mixed using ethanol or the like as a dispersion medium. The reason why the average particle size of the MgO powder is limited to 0.1 to 5 μm is to facilitate sintering. In addition, the wet mixing is
It is performed by a stirring mill or a wet ball mill. In the stirring mill, a ZrO ₂ ball having a diameter of 1 to 3 mm was used.
Wet mix for 5 to 1 hour. The reason why the diameter of the ZrO ₂ balls is limited to 1 to 3 mm is that mixing is insufficient when the diameter is less than 1 mm, and impurities increase when the diameter exceeds 3 mm. The reason why the mixing time is as short as 1 hour at the longest is that if it exceeds 1 hour, not only the mixing of the raw materials but also the work of crushing is performed, which causes the generation of impurities, and the mixing time of 1 hour is sufficient. .

In the wet ball mill, when ZrO ₂ balls are used, a large number of ZrO ₂ balls having a diameter of 5 to 10 mm are used and wet mixed for 8 to 24 hours, preferably 20 to 24 hours. The diameter of the ZrO ₂ ball is 5-10
The reason why it is limited to mm is that mixing is insufficient if it is less than 5 mm, and there is a problem that impurities increase if it exceeds 10 mm. Further, the reason that the mixing time is as long as 24 hours at the longest is that the generation of impurities is small even after continuous mixing for a long time.

Next, the above mixture is heated under reduced pressure to dry and then dry crushed. The mixture is dried under reduced pressure using a rotary evaporator for 4 to 12 hours, and then dry crushed for 12 to 24 hours using a dry ball mill. Further, the inside of this ball mill is preferably replaced with argon gas in order to prevent the oxidation of the LaB ₆ powder.

Next, the dry-crushed mixed powder is molded. As a method for molding the mixed powder, it is preferable to use both a uniaxial pressure molding device and a cold isostatic pressing device (CIP (Cold Isostatic Press) molding device). First, the mixed powder pulverized by dry crushing was filled in a mold of a uniaxial pressure molding device,
After uniaxial pressure molding at a pressure of MPa to perform temporary molding, this temporary molded body is filled in a rubber mold of a CIP molding machine to 140 to 2
CIP molding is performed at a pressure of 00 MPa.

Further, by sintering the above-mentioned compact, M
A target containing gO as a main component is obtained. The sintering method includes a one-step sintering method and a two-step sintering method. For the one-step sintering method, the molded body is subjected to a vacuum in a vacuum of 1 × 10 ⁻² to 1 × 10 ⁻⁴ Torr, preferably 1 × 10 ⁻³ to 1 × 10 ⁻⁴ Torr.
There is a method of sintering by raising the temperature to 0 to 1650 ° C. and holding at this temperature for 2 to 3 hours. Sintering temperature 1400
The reason why the temperature is limited to ˜1650 ° C. is that a dense sintered body cannot be obtained at a temperature lower than 1400 ° C., and grain growth is caused at a temperature higher than 1650 ° C. to deteriorate the characteristics.

Further, in the one-step sintering method, 0.02-0.5M
There is a method of sintering by raising the temperature to 1400 to 1650 ° C. in an inert gas atmosphere having a pressure of Pa, preferably 0.1 to 0.5 MPa, and holding at this temperature for 2 to 3 hours. As the inert gas, it is preferable to use argon gas, nitrogen gas or the like, and the gas pressure is 0.02 to 0.5 MP.
The reason for limiting the value to a is that if the pressure is less than 0.02 MPa, the inside of the furnace cannot be made into a positive atmosphere, and if the pressure exceeds 0.5 MPa, the characteristics do not change and it is not necessary to raise the gas pressure.

On the other hand, in the two-stage sintering method, the temperature is raised to 1300 to 1350 ° C. in a vacuum or an inert gas atmosphere at normal pressure, and this temperature is maintained for 1 to 2 hours for primary sintering. 1450 to 1650 in a vacuum or an inert gas atmosphere at normal pressure
This is a method in which the temperature is raised to ° C and the temperature is maintained for 2 to 3 hours to carry out secondary sintering. As the inert gas, it is preferable to use argon gas, nitrogen gas or the like. Further, the primary sintering temperature is limited to 1300 to 1350 ° C. The primary sintering in this temperature range eliminates uneven sintering (difference in structure) between the surface and the inside even if the grain size is large. Therefore, the reason why the secondary sintering temperature is limited to 1450 to 1650 ° C. is that a dense sintered body cannot be obtained below 1450 ° C.
This is because if the temperature exceeds 50 ° C., the grains grow and the characteristics deteriorate. In both cases of single-stage sintering and two-stage sintering, 700 to 900 in a reducing gas atmosphere before sintering the molded body.
It is preferable to raise the temperature to 750 ° C., preferably 750 to 850 ° C., for reduction treatment. Hydrogen gas or the like is preferably used as the reducing gas, and the reducing treatment is performed to prevent the dispersed particles from being oxidized.

Another method of manufacturing the target of the present invention will be described. In this manufacturing method, the mixed powder obtained by dry crushing in the same manner as in the above manufacturing method is heated to 1450 to 1650 ° C., preferably 1500 to 1600 ° C. under a press pressure of 15 to 30 MPa in an inert gas atmosphere. At this temperature
Hold for 2 hours for sintering (hereinafter referred to as hot press sintering)
By doing so, a target is manufactured. Since this hot press sintering can perform molding and sintering at the same time, it has the advantages that the target can be made more precise and the number of manufacturing steps can be reduced. As the inert gas, it is preferable to use argon gas, nitrogen gas or the like, and the gas pressure is 0.02 to 0.5 MPa, preferably 0.1 to 0.5.
It is set to MPa. In addition, the mixed powder is 15 to 30 MPa.
To pressurize, it is preferable to use a pressing device having a graphite die with excellent heat resistance. Further, the pressure of the mixed powder was limited to 15 to 30 MPa because a dense sintered body could not be obtained at less than 15 MPa, and a wall thickness of the die became thicker than 30 MPa to obtain only a small sintered body. Because it is not the target. Furthermore, the sintering temperature is 1450 to 1650.
The reason for limiting the temperature to 1 ° C is that a dense sintered body cannot be obtained at a temperature lower than 1450 ° C, and the characteristics deteriorate due to grain growth at a temperature higher than 1650 ° C.

[0023]

EXAMPLES The present invention will be described in more detail with reference to Examples and Comparative Examples below, but the present invention is not limited to the following Examples unless it exceeds the gist. <Example 1> First, 1% by volume of LaB ₆ powder (manufactured by Shin Nippon Metal Co., Ltd., average particle size 1.4 μm) was mixed with MgO powder (3N manufactured by Ako Kasei Co., Ltd., average particle size 0.2 μm), and ethanol was added. As a dispersion medium, wet mixing was performed for 1 hour with a stirring mill. The mixture was heated under reduced pressure for 8 hours using a rotary evaporator to dry it, and then dry crushed in a dry ball mill for 4 hours.
The inside of the ball mill was replaced with argon gas to prevent the dispersed particles from being oxidized. Next, the dry crushed mixed powder was filled in a graphite die (inner diameter 130 mm), and the mixed powder was placed in a sintering furnace (manufactured by Fuji Denpa Kogyo Co., Ltd.) with a pressing pressure of 15 MPa applied thereto. The inside of the sintering furnace was set to 1450 with an argon gas atmosphere having a gas pressure of 0.05 MPa.
The temperature was raised to 0 ° C. and the temperature was maintained for 1 hour for sintering. The target manufactured in this manner was referred to as Example 1.

Example 2 First, 10% by volume of LaB ₆ powder was mixed with MgO powder and wet-mixed for 1 hour with a stirring mill using ethanol as a dispersion medium. This mixture was dry-crushed in the same manner as in Example 1. Next, the dry crushed mixed powder was filled in a mold (inner diameter 160 mm) of a uniaxial pressing device, uniaxially pressure molded at 7.35 MPa, and then 147 MPa.
CIP molding was carried out to obtain a molded body. This compact was placed in a sintering furnace (manufactured by Fuji Denpa Kogyo Co., Ltd.), subjected to reduction treatment in a hydrogen atmosphere at 800 ° C. for 2 hours, then held in an argon atmosphere at 1350 ° C. for 1 hour, and further heated to 1600 ° C. for 2 hours. Hold for time and sinter. The target produced in this manner was referred to as Example 2.

Example 3 A target was prepared in the same manner as in Example 1 except that 10% by volume of LaB ₆ powder was mixed with MgO powder. Example 4 A target was prepared in the same manner as in Example 1 except that 5% by volume of LaB ₆ powder was mixed with MgO powder. <Example 5> A target produced under exactly the same conditions as in Example 2 was referred to as Example 5. To <Example 6> MgO powder, except that mixed with 20 vol% of LaB ₆ powder, a target was prepared in the same manner as in Example 2.

Comparative Example 1 A compact was prepared in the same manner as in Example 2 except that the MgB powder was not mixed with LaB ₆ powder at all, and the compact was placed in a sintering furnace and subjected to a reduction treatment. Without carrying out, it was held at 1600 ° C. for 2 hours in an argon atmosphere and sintered. The target manufactured in this manner was used as Comparative Example 1. Comparative Example 2 A target was produced in the same manner as in Example 1 except that 40% by volume of LaB ₆ powder was mixed with MgO powder. Comparative Example 3 A target was prepared in the same manner as in Example 2 except that 35% by volume of LaB ₆ powder was mixed with MgO powder. Comparative Example 4 A target of a commercially available MgO sintered body was set as Comparative Example 4.

<Comparison Test and Evaluation> (a) Relative Density and Fracture Strength Test The targets obtained in Examples 1 to 6 and Comparative Examples 1 to 3 were cut out, ground and polished to obtain JIS R1.
The size of a 3 mm × 4 mm × 40 mm 3-point bending test piece according to 601 was used, and the relative density and breaking strength were measured.
The results are shown in Table 1. The relative density was measured by the Archimedes method in toluene, and the breaking strength was measured by a 3-point bending test.

[0028]

[Table 1]

As is clear from Table 1, the relative densities of the targets of Comparative Examples 1 to 3 are in the order of 96%, whereas the relative densities of the targets of Examples 1 to 6 are 99% or more and are dense. . The bending strength of the targets of Examples 1 to 6 was twice as high as that of Comparative Examples 1 to 3. In Examples 1 to 6, this is L within a range that does not cause a crack at the crystal grain interface.
Now that you uniformly dispersed aB ₆ particles, even less strength defects of the grain boundaries and because could be improved, because defects in the grain boundaries is caused by excessive mixing ratio of LaB ₆ powder in Comparative Examples 2 and 3 It is believed that there is.

(B) MgO film formation rate, formed MgO film
Film characteristic test and its discharge property test The targets of Examples 2, 5 and 6 and the targets of Comparative Examples 3 and 4 were processed into a disk shape having an outer diameter of 127 mm, and then bonded to a copper back plate, Five types of substrates were produced by forming a film on a glass substrate by a sputtering method. The film-forming conditions are as follows: the distance from the target to the substrate (T / S) is 5 cm, the substrate temperature is 300 ° C., and the gas pressure is 1.
Each was set to 0 mTorr and the high frequency output (RF) was set to 1500W. The film pressure of the formed MgO film is He-
With a Ne laser (wavelength 6238 angstrom),
Ellipso measurement of 1 wavelength and 2 incident angles (55 °, 70 °) was performed on the film, and it was determined using analysis software.
The film forming rate of the MgO film was obtained by dividing the film thickness of O by the film forming time. At the same time, the refractive index and absorption coefficient of the MgO film were obtained.

The discharge start voltage of the MgO film was measured by using the targets of Examples 2, 5 and 6 and the targets of Comparative Examples 3 and 4 as shown in FIG.
up) Substrate 10 was prepared and measured. The TEG substrate 10 is a glass substrate having a thickness of 1 mm (Corning # 7059
InSn by photolithography on 11)
After forming the base electrode 12 made of a composite oxide film with a thickness of 1 μm and a width of 100 μm at intervals of 100 μm, a glass layer 13 having a thickness of 3 μm was formed by reactive DC sputtering of Si so as to cover these base electrodes 12. The MgO film 14 having a thickness of 0.7 μm formed under the same film forming conditions by the above-described sputtering method.
It was made by forming a film.

The discharge start voltage is 50 for each of the above 5 types of TEG substrates with Ne-5% Xe of the device shown in FIG.
The sample is placed on a heating sample table 16 arranged in a vacuum bell jar 15 of 0 Torr, the base electrode 12 (FIG. 2) is connected to a pulse power source 17, and the TEG substrate 10 is controlled at a constant temperature while being measured by a thermocouple 18. Increase the power supply voltage,
The voltage at which discharge started was measured. The pulse power supply 17 is 0
The voltage is variable in the range of 300 V and the frequency is 66 kHz.
The pulse width is 10 μsec. Table 2 shows the film forming rate, the refractive index, the absorption coefficient, and the discharge starting voltage of the MgO film.

[0033]

[Table 2]

As is clear from Table 2, when the targets of Examples 2, 5 and 6 were used to form a film by sputtering,
It was possible to form a film at a speed 9 times or more that of the target of Comparative Example 4 (commercial MgO sintered body) and 2.5 to 3.5 times that of Comparative Example 3. This is because in Examples 2, 5 and 6, the MgO matrix and the dispersed particles were strongly bonded at the crystal grain interface of the matrix, so that the target did not crack even when the film was formed at a high speed, and abnormal discharge did not occur. by. The refractive indexes were 1.68 and 1.67 in Comparative Examples 3 and 4, while 1.78 to 1.
The absorption coefficient was slightly improved to 80 in Comparative Examples 3 and 4.
012 and 0.011 while Examples 2, 5
In Nos. 6 and 6, it was significantly improved to 0.001 or less. Further, the discharge start voltage of Examples 2, 5 and 6 was lower by 10 to 24 V than that of Comparative Examples 3 and 4. The substrate on which the MgO film was formed using the targets of Examples 2, 5 and 6 was used as a PD.
The resistance to spatter when incorporated into P was good, and the drive voltage was lower than before.

[0035]

As described above, according to the present invention, M having crystal grains having an average crystal grain size of 0.5 to 100 μm is used.
The LaB ₆ particles were dispersed in the gO matrix in an amount of 1 to 25% by volume to form a target.
The fracture toughness value and thermal shock resistance can be improved. In addition, when a film is formed by a sputtering method using the target of the present invention, two-phase coexistence, that is, since the MgO matrix and the dispersed particles are sputter evaporated without forming a solid solution or a reactant, a high-speed stable film formation becomes possible, The obtained film is completely solid-solved in the substrate and the orientation of the film is improved. Further, when a substrate on which an MgO film is formed using the target of the present invention is incorporated into a PDP, the discharge voltage can be lowered, the spatter resistance during discharge can be improved, and the discharge responsiveness can be increased. This MgO film has high insulation.

Further, the MgO powder and the LaB ₆ powder are wet-mixed, the mixture is heated under reduced pressure and dried, and then dry-crushed to form a dry-crushed mixed powder, and the molded body is further cooled to 1300 to 1650 ° C. When the target is manufactured by sintering at the temperature of, the dispersed particles are uniformly dispersed in the MgO matrix, the matching of the grain boundaries is good, and the defects of the grain boundaries are small, that is, the structure is well controlled. You get the target. In addition, the molded body is heated to 1400 to 1650 ° C. in a vacuum or in an inert gas atmosphere for sintering,
1300 to 13 in an inert gas atmosphere of vacuum or normal pressure
Before raising the temperature to 50 ° C. to perform primary sintering, and further raising the temperature to 1450 to 1650 ° C. in vacuum or in an inert gas atmosphere at normal pressure to perform secondary sintering, or before sintering the compact. If the temperature is raised to 700 to 900 ° C. in a reducing gas atmosphere to carry out the reduction treatment, a target having a well-structured structure can be obtained.

Further, the MgO powder and the LaB ₆ powder are wet-mixed, the mixture is heated under reduced pressure to dry and then dry crushed, and the dry crushed mixed powder is pressed under an inert gas atmosphere at a pressing pressure of 15 to 30 MPa. If the temperature is raised to 1450 to 1650 ° C. and then sintered, the target can be made more precise and the number of manufacturing steps can be reduced.

[Brief description of drawings]

FIG. 1 is a diagram illustrating a strengthening mechanism of a target containing MgO as a main component of the present invention.

FIG. 2 is a cross-sectional view of a TEG substrate having a MgO film formed by a sputtering method using a target containing MgO as a main component of the present invention.

FIG. 3 is a configuration diagram of an apparatus for measuring a discharge start voltage of the TEG substrate shown in FIG.

[Explanation of symbols]

1 MgO matrix crystal particles 2 LaB ₆ particles

─────────────────────────────────────────────────── ─── Continuation of the front page (56) Reference JP-A-10-237636 (JP, A) (58) Fields investigated (Int.Cl. ⁷ , DB name) C23C 14/00-14/58 C04B 35 / 04

Claims (6)

(57) [Claims] 1. LaB ₆ particles in a MgO matrix having crystal particles (1) having an average crystal grain size of 0.5 to 100 μm.
A target whose main component is MgO in which 1 to 25% by volume of (2) is dispersed. 2. A step of wet mixing MgO powder and LaB ₆ powder, a step of heating the mixture under reduced pressure to dry and then dry crushing, a step of molding the dry crushed mixed powder, A method of manufacturing a target containing MgO as a main component, which comprises a step of sintering a compact at a temperature of 1300 to 1650 ° C. 3. The method for producing a target containing MgO as a main component according to claim 2, wherein the compact is heated to 1400 to 1650 ° C. in a vacuum or in an inert gas atmosphere and sintered. 4. The molded body is heated to 1300 to 1350 ° C. in vacuum or in an inert gas atmosphere at normal pressure to perform primary sintering,
Further, in vacuum or in an inert gas atmosphere at normal pressure, 1450 to
The Mg according to claim 2, wherein the temperature is raised to 1650 ° C and the secondary sintering is performed.
A method of manufacturing a target containing O as a main component. 5. The reduction treatment by raising the temperature to 700 to 900 ° C. in a reducing gas atmosphere before sintering the molded body.
Alternatively, the method for producing a target containing MgO as a main component according to 4 above. 6. A step of wet mixing MgO powder and LaB ₆ powder, a step of heating the mixture under reduced pressure to dry and then dry crushing, and a step of dry crushing the mixed powder in an inert gas atmosphere. 14
Mg including a step of raising the temperature to 50 to 1650 ° C. and sintering.
A method of manufacturing a target containing O as a main component.