JP2022025872A - Long cylindrical ceramic body - Google Patents

Abstract

To provide a long cylindrical ceramic body in which even if a metalized layer is formed on an inner peripheral surface, a discontinuous portion is not likely to be generated on the metalized layer.SOLUTION: A long cylindrical ceramic body according to the present disclosure includes a ceramic main body having a cylindrical shape. An inner peripheral surface in the vicinity of one end of the ceramic main body is a first inner peripheral surface; an inner peripheral surface in the vicinity of the other end of the ceramic main body is a second inner peripheral surface; a portion connecting the first inner peripheral surface and the second inner peripheral surface with each other is a connection part. The second inner peripheral surface has a smaller diameter than that of the first inner peripheral surface. The center of the diameter of the first inner peripheral surface and the center of the diameter of the second inner peripheral surface are present on the same axis. At least part of an inner wall surface of the connection part is inclined with respect to the axis.SELECTED DRAWING: Figure 1

Description

The present disclosure relates to a long tubular ceramic body.

Conventionally, in an electron beam exposure apparatus, a liner tube is provided in an optical lens barrel in order to keep the surroundings including the optical axis in a vacuum. An electromagnetic lens, an electromagnetic deflector, etc. are arranged on the outer peripheral side of the liner tube. Patent Document 1 describes a liner tube in which a titanium metallized layer and a platinum-plated layer are sequentially formed on the inner surface of a ceramic cylinder.

However, in the liner tube described in Patent Document 1, the metallized layer tends to be discontinuous at both ends of the connecting surface connecting the large-diameter inner surface and the small-diameter inner surface. Furthermore, it is difficult to sufficiently control the thickness of the titanium metallized layer. Therefore, it is difficult to control the deflection of the electron beam in the charged particle beam device provided with the liner tube described in Patent Document 1.

Japanese Unexamined Patent Publication No. 2001-6594

An object of the present disclosure is to provide a long cylindrical ceramic body in which a discontinuous portion is unlikely to occur in the metallized layer even if the metallized layer is formed on the inner peripheral surface.

The long tubular ceramic body according to the present disclosure includes a ceramic body having a tubular shape, the inner peripheral surface near one end of the ceramic body is the first inner peripheral portion, and the inner peripheral surface near the other end of the ceramic body is near the other end. The inner peripheral surface is the second inner peripheral portion, the portion connecting the first inner peripheral portion and the second inner peripheral portion is the connecting portion, and the second inner peripheral portion has a diameter smaller than that of the first inner peripheral portion. The center of the diameter of the first inner peripheral portion and the center of the diameter of the second inner peripheral portion are present on the same axis, and at least a part of the inner wall surface of the connecting portion is relative to the axis. It is tilted.

The liner tube according to the present disclosure includes the above-mentioned long cylindrical ceramic body, and has a surface of at least the connection portion side of the first inner peripheral portion, a surface of at least the connection portion side of the second inner peripheral portion, and the inside of the connection portion. A metallized layer is laminated on the wall surface.

The charged particle beam device according to the present disclosure includes the above liner tube and an electromagnetic lens or an electromagnetic deflector on the outer peripheral side of the liner tube.

According to the present disclosure, it is possible to provide a long cylindrical ceramic body in which a discontinuous portion is unlikely to occur in the metallized layer even if the metallized layer is formed on the inner peripheral surface.

(A) is an explanatory view showing a long cylindrical ceramic body according to an embodiment of the present disclosure, and (B) is an explanatory view showing a cross section when cut by XX rays shown in (A). Is. It is explanatory drawing which shows the cross section of the long cylindrical ceramic body which concerns on other embodiment of this disclosure.

As described above, the long tubular ceramic body according to the present disclosure includes a ceramic body having a tubular shape, the inner peripheral surface near one end of the ceramic body is the first inner peripheral portion, and the other of the ceramic bodies. The inner peripheral surface in the vicinity of the end portion is referred to as a second inner peripheral portion, and the portion connecting the first inner peripheral portion and the second inner peripheral portion is referred to as a connecting portion. The long cylindrical ceramic body according to the present disclosure will be described with reference to FIGS. 1 and 2.

As shown in FIG. 1A, the long tubular ceramic body 1 according to the embodiment includes a ceramic body 10 having a tubular shape. As used herein, the term "long" means a length of 100 mm or more.

The ceramic body 10 is not limited as long as it is made of ceramics. Examples of the ceramics include ceramics containing aluminum oxide, silicon carbide, silicon carbide, titanium carbide, titanium carbide and the like as main components. As used herein, the term "main component" refers to a component that accounts for 80% by mass or more in a total of 100% by mass of the components constituting the ceramics. The identification of each component contained in the ceramics is performed by an X-ray diffractometer using CuKα ray, and the content of each component may be determined by, for example, an ICP (Inductively Coupled Plasma) emission spectroscopic analyzer or a fluorescent X-ray analyzer.

In the case of ceramics whose main component is aluminum oxide, for example, magnesium, calcium and silicon may be further contained as oxides.

The length of the ceramic body 10 is not limited as long as it is 100 mm or more, and is appropriately set according to the use of the obtained long cylindrical ceramic body. The length of the ceramic body 10 is, for example, about 100 mm or more and 250 mm or less. The outer diameter of the ceramic body 10 is also not limited, and is appropriately set according to the use of the obtained long cylindrical ceramic body. The outer diameter of the ceramic body 10 is, for example, about 18 mm or more and 40 mm or less. When the ceramic body 10 does not have a single thickness (outer diameter), the outer diameter of the thinnest part and the outer diameter of the thickest part have a length in the above range. You just have to.

The inner peripheral surface of the ceramic body 10 will be described with reference to FIG. 1 (B). As shown in FIG. 1 (B), the first inner peripheral portion 11 is located near one end of the ceramic main body 10, and the second inner peripheral portion 12 is located near the other end of the ceramic main body 10. There is. The first inner peripheral portion 11 has a length from one end surface of the ceramic main body 10 to about 45% of the total length of the ceramic main body 10. The second inner peripheral portion 12 has a length from the other end surface of the ceramic main body 10 to about 35% of the total length of the ceramic main body 10.

The second inner peripheral portion 12 has a diameter smaller than that of the first inner peripheral portion 11. The diameter D2 of the second inner peripheral portion 12 is not limited as long as it is smaller than the diameter D1 of the first inner peripheral portion 11. For example, the diameter D2 of the second inner peripheral portion 12 is preferably about 50% or more and 65% or less of the diameter D1 of the first inner peripheral portion 11. The center of the diameter D1 of the first inner peripheral portion 11 and the center of the diameter D2 of the second inner peripheral portion 12 exist on the same axis.

In the long cylindrical ceramic body 1 according to the embodiment, the first inner peripheral portion 11 and the second inner peripheral portion 12 are connected via a connecting portion 13. Since the diameter D1 of the first inner peripheral portion 11 and the diameter D2 of the second inner peripheral portion 12 are different, the diameters of one end of the connecting portion 13 and the diameter of the other end are different. .. Therefore, at least a part of the inner wall surface of the connecting portion 13 is inclined with respect to the above-mentioned axis passing through the center of the diameter D1 of the first inner peripheral portion 11 and the center of the diameter D2 of the second inner peripheral portion 12. .. As a result, even if a metallized layer is formed on the inner wall surfaces of the first inner peripheral portion 11, the second inner peripheral portion 12, and the connecting portion 13, for example, a discontinuous portion is less likely to occur in the metallized layer. The inclination angle of the inner wall surface of the connecting portion 13 with respect to the axis is not particularly limited, and may be, for example, about 4 ° or more and 18 ° or less.

The inner wall surface of the connecting portion 13'may have a curvature, as in the long cylindrical ceramic body 1'according to the other embodiment shown in FIG. As described above, when the inner wall surface of the connecting portion 13'has a curvature, both end portions of the connecting portion 13' are loosely connected to the first inner peripheral portion 11'and the second inner peripheral portion 12'. As a result, even if a metallized layer is formed on the inner wall surface of the first inner peripheral portion 11', the second inner peripheral portion 12', and the connecting portion 13', a discontinuous portion is less likely to occur in the metallized layer.

On the inner wall surface of the connecting portion 13', at least one end of both ends of the connecting portion 13'should have a greater curvature than the intermediate portion of the connecting portion 13' sandwiched between the both ends. .. In such a configuration, for example, even if a metallized layer is formed on the inner wall surface of the first inner peripheral portion 11', the second inner peripheral portion 12', and the connecting portion 13', both ends of the connecting portion 13'are formed. It becomes difficult for stress to concentrate on the formed metallized layer. As a result, for example, it can be used for a long period of time even in an environment where heating and cooling are repeated.

The radius of curvature of the inner wall surface of the intermediate portion of the connecting portion 13'is not limited. The inner wall surface of the intermediate portion of the connecting portion 13'may have, for example, a radius of curvature of 250 mm or more, and particularly preferably a radius of curvature of about 300 mm or more and 350 mm or less. The radius of curvature of the inner wall surface of the end portion of the connecting portion 13'may be, for example, about 5 mm or more and 15 mm or less.

The method for producing the long tubular ceramic body of the present disclosure is not limited, and for example, it is produced by the following procedure. First, aluminum oxide, silicon carbide, silicon carbide, titanium carbide or titanium carbide powder is prepared. The purity of these powders is not limited. These powders are preferably, for example, having a purity of 99% by mass or more. If necessary, other powders used as raw materials for ceramics may be used.

Hereinafter, a case of obtaining a long cylindrical ceramic body containing aluminum oxide as a main component will be described. First, aluminum oxide powder (purity of 99% by mass or more), which is the main component, and magnesium hydroxide, silicon oxide, and calcium carbonate powders are put into a pulverizing mill together with a solvent (ion-exchanged water) to prepare the powder. After pulverizing until the average particle size (D ₅₀ ) becomes 1.5 μm or less, an organic binder and a dispersant for dispersing aluminum oxide powder are added and mixed to obtain a slurry.

Here, the content of the magnesium hydroxide powder in the total 100% by mass of the powder is 0.3 to 0.42% by mass, the content of the silicon oxide powder is 0.5 to 0.8% by mass, and the content of the calcium carbonate powder is The content is 0.060 to 0.1% by mass, and the balance is aluminum oxide powder and unavoidable impurities.

Examples of the organic binder include acrylic emulsions, polyvinyl alcohols, polyethylene glycols, polyethylene oxides and the like.

Next, after spray-granulating the slurry to obtain granules, a columnar molded body is obtained by pressurizing the slurry with a molding pressure of 78 MPa or more and 128 MPa or less using a cold hydrostatic pressure press molding apparatus. The molded body forms through holes along the axial direction by cutting.

A cylindrical sintered body can be obtained by firing a molded body having through holes in an atmospheric atmosphere, for example, with a firing temperature of 1500 ° C. or higher and 1700 ° C. or lower and a holding time of 4 hours or longer and 6 hours or lower. By subjecting the outer peripheral surface of the obtained cylindrical sintered body to cylindrical grinding and the inner peripheral surface to internal grinding, for example, the long tubular ceramic bodies 1 and 1 having the shapes shown in FIGS. 'You can get.

The long tubular ceramic body of the present disclosure is used, for example, as a member of a liner tube. Hereinafter, the liner tube will be described by taking as an example the case where the long cylindrical ceramic body 1 according to the embodiment is used.

The liner tube according to an embodiment of the present disclosure is a surface of at least the connection portion 13 side of the first inner peripheral portion 11 of the long tubular ceramic body 1 according to the embodiment, and at least the connection portion of the second inner peripheral portion 12. It has a structure in which a metallized layer is laminated on the surface on the 13 side and the inner wall surface of the connecting portion 13.

The metal contained in the metallized layer is not limited, and examples thereof include metals containing molybdenum, tungsten, titanium, silver, and the like as main components. Among these metals, it is preferable that the metal is mainly composed of molybdenum, tungsten or titanium. Molybdenum, tungsten, and titanium are non-magnetic metals, and even if the electron beam passes through the internal space, the electron beam is less likely to be adversely affected. In addition, molybdenum, tungsten and titanium have relatively high resistivity, which makes them less likely to generate eddy currents.

When the metallized layer contains molybdenum or tungsten as a main component, manganese may be 15% by mass or more and 25% by mass or less, and the balance may be a metal as a main component, out of 100% by mass of the metal elements constituting the metallized layer. When the metallized layer contains silver as a main component, copper is 25% by mass or more and 30% by mass or less, titanium is 0.8% by mass or more and 2% by mass or less, and the balance is silver out of 100% by mass of metal elements constituting the metallized layer. May be.

The thickness of the metallized layer is not limited, and may be, for example, about 15 μm or more and 45 μm or less. The coefficient of variation of the thickness of the metallized layer is preferably 0.2 or less, for example. If the coefficient of variation of the thickness of the metallized layer is 0.2 or less, the variation in thickness is small even if the thickness of the metallized layer is reduced. As a result, discontinuous portions of the metallized layer are less likely to occur, and the possibility of poor continuity is reduced.

In the liner tube according to the embodiment, the first plating layer may be further laminated on the metallized layer. The first plating layer is formed of a metal containing gold, platinum or silver as a main component. Gold, platinum or silver contained in such a first plating layer has a high standard potential and is resistant to rust. As a result, the reliability of the liner tube can be further improved.

The thickness of the first plating layer is not limited, and may be, for example, 0.01 μm or more and 0.1 μm or less. The arithmetic mean roughness Ra of the first plating layer is not limited, and may be, for example, about 1.1 μm or more and 1.7 μm or less. On the surface of the first plating layer, the coefficient of variation of the arithmetic mean roughness Ra is preferably 0.2 or less (excluding 0). When the surface of the first plating layer has such a coefficient of variation of the arithmetic mean roughness Ra, it becomes difficult for gas to be adsorbed on the surface of the first plating layer. As a result, the exhaust efficiency for evacuating the internal space of the liner tube is improved.

The root mean square slope RΔq of the first plating layer is not limited, and may be, for example, 0.4 or more and 1.6 or less. Further, on the surface of the first plating layer, the coefficient of variation of the root mean square slope RΔq is preferably 0.25 or less (excluding 0). When the surface of the first plating layer has such a coefficient of variation of the root mean square slope RΔq, it becomes more difficult for gas to be adsorbed on the surface of the first plating layer. As a result, the exhaust efficiency for evacuating the internal space of the liner tube is further improved.

Arithmetic mean roughness Ra and root mean square slope RΔq conform to JIS B 0601: 2001, shape analysis laser microscope (manufactured by KEYENCE CORPORATION, ultra-depth color 3D shape measurement microscope (VK-X1100 or its successor model)). ) Can be used for measurement.

The measurement conditions are coaxial lighting for the illumination method, 120 times the magnification, no cutoff value λs, 0.08 mm for the cutoff value λc, no cutoff value λf, and correction of the termination effect. The measurement range per location from the surface of the first plating layer is set to, for example, 2792 μm × 2093 μm, and one line to be measured is drawn along the longitudinal direction of the measurement range for each measurement range. , Line roughness may be measured. The length per line to be measured is, for example, 2640 μm. The measurement range is set at eight points at substantially equal intervals along the axial direction, and the total number of lines to be measured is eight. The coefficient of variation of the arithmetic mean roughness Ra and the square mean square root slope RΔq may be calculated from the mean value and standard deviation obtained from the eight lines to be measured.

In the liner tube according to one embodiment, a second plating layer containing nickel as a main component may be further laminated between the metallized layer and the first plating layer. By laminating the second plating layer, it is possible to prevent the components forming the first plating layer from diffusing into the metallized layer. The thickness of the second plating layer is not limited, and may be, for example, about 1 μm or more and 3 μm or less.

The coefficient of variation of the total thickness of the metallized layer, the first plating layer and the second plating layer is preferably 0.2 or less, for example. If the coefficient of variation of the total thickness of the metallized layer, the first plating layer, and the second plating layer is 0.2 or less, the variation in thickness is small even if the thickness of these layers is reduced. As a result, the possibility of poor continuity is reduced.

When measuring the thickness of each of the metallized layer, the first plating layer and the second plating layer, first, the liner tube is cut or ground so as to have a semi-cylindrical shape, and then the cross section is polished. A measurement range is set at 10 points along the axial direction, with the polished surface on either side obtained by this polishing as the measurement target.

The measurement range may be set according to the lengths of the first inner peripheral portion, the second inner peripheral portion, and the connecting portion. In the case of the long tubular ceramic body 1', for example, the measurement range is set at 3 points from the 1st inner peripheral portion 11', 5 points from the 2nd inner peripheral portion 12', and 2 points from the connecting portion 13', for a total of 10 points. However, the measurement range may be set to be approximately equal intervals for each part. Then, using a scanning electron microscope, the thickness of the layer to be measured may be measured at a magnification of, for example, 500 times. The coefficient of variation of the thickness of the metallized layer and the coefficient of variation of the total thickness of the metallized layer, the first plating layer and the second plating layer may be calculated from the average value and standard deviation of the thickness obtained for each measurement range. Hereinafter, a method for manufacturing a liner tube will be described.

First, for example, a paste containing molybdenum as a main component and manganese is applied to the inner wall surfaces of the first inner peripheral portion, the second inner peripheral portion, and the connecting portion of the long tubular ceramic body. Here, the viscosity of the paste at room temperature is preferably, for example, 250 p or less, particularly 210 p or less. Next, heat treatment is performed in a forming gas atmosphere having a hydrogen: nitrogen volume ratio of 70 to 80:30 to 20 and a temperature of 1300 ° C to 1400 ° C. By doing this, it is possible to obtain a liner tube in which a metallized layer is laminated. Further, when laminating the first plating layer and the second plating layer, both may be laminated by electroless plating.

The liner tube according to the present disclosure is adopted as a member of a charged particle beam device such as an electron microscope, an ion beam microscope, an electron beam exposure device, an electron beam microanalyzer, an ion beam device, a cyclotron, and an electron beam welder. Such a charged particle beam device includes, for example, a liner tube according to an embodiment of the present disclosure, and an electromagnetic lens or an electromagnetic deflector on the outer peripheral side of the liner tube.

1, 1'Long tubular ceramic body 10 Ceramic body 11, 11'First inner peripheral part 12, 12' Second inner peripheral part 13, 13' Connection part

Claims (13)

Includes a cylindrical ceramic body
The inner peripheral surface near one end of the ceramic body is designated as the first inner peripheral portion, the inner peripheral surface near the other end of the ceramic body is designated as the second inner peripheral portion, and the first inner peripheral portion and the said portion. The part connecting to the second inner peripheral part is used as the connecting part.
The second inner peripheral portion has a diameter smaller than that of the first inner peripheral portion, and the diameter thereof is smaller than that of the first inner peripheral portion.
The center of the diameter of the first inner peripheral portion and the center of the diameter of the second inner peripheral portion are present on the same axis.
A long cylindrical ceramic body in which at least a part of the inner wall surface of the connection portion is inclined with respect to the axis. The long tubular ceramic body according to claim 1, wherein the inner wall surface of the connecting portion has a curvature. The long cylindrical shape according to claim 1 or 2, wherein the inner wall surface of at least one end of both ends of the connection portion has a larger curvature than the inner wall surface of the intermediate portion sandwiched between the both ends. Ceramic body. The long tubular ceramic body according to claim 3, wherein the inner wall surface of the intermediate portion has a radius of curvature of 250 mm or more. The long tubular ceramic body according to any one of claims 1 to 4 is included.
A liner tube in which a metallized layer is laminated on at least the surface of the first inner peripheral portion on the connecting portion side, at least the surface of the second inner peripheral portion on the connecting portion side, and the inner wall surface of the connecting portion. The liner tube according to claim 5, wherein the metallized layer contains molybdenum, tungsten or titanium as a main component. The liner tube according to claim 5 or 6, wherein the metallized layer has a coefficient of variation of 0.2 or less. The liner tube according to any one of claims 5 to 7, wherein a first plating layer containing gold, platinum or silver as a main component is further laminated on the metallized layer. The liner tube according to claim 8, wherein a second plating layer containing nickel as a main component is further laminated between the metallized layer and the first plating layer. The liner tube according to claim 8 or 9, wherein the surface of the first plating layer has a coefficient of variation of arithmetic mean roughness Ra of 0.2 or less (excluding 0). The liner tube according to any one of claims 8 to 10, wherein the surface of the first plating layer has a coefficient of variation of a root mean square slope RΔq of 0.25 or less (excluding 0). The liner tube according to any one of claims 8 to 11, wherein the coefficient of variation of the total thickness of the metallized layer, the first plating layer and the second plating layer is 0.2 or less. A charged particle beam device comprising the liner tube according to any one of claims 5 to 12 and an electromagnetic lens or an electromagnetic deflector on the outer peripheral side of the liner tube.

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