KR20180111581A - Method for cleaning a sputtering target, apparatus for cleaning a sputtering target, method for manufacturing a sputtering target, sputtering target, method for manufacturing a recycled ingot and a recycled ingot - Google Patents

Abstract

Provided is a method for cleaning a target, comprising: a process of separating a target from a sputtering target where a target mainly composed of metal and a support member are coupled by using a bonding material; and a process of injecting water to a surface of the target where the bonding material is attached in order to remove the bonding material from the target material. The target can be reused as an ingot.

Description

FIELD OF THE INVENTION [0001] The present invention relates to a method of cleaning a target material, an apparatus therefor, a method of manufacturing a target material, a target material, and a method of manufacturing a reclaim ingot and a recycling ingot. , METHOD FOR MANUFACTURING A RECYCLED INGOT AND A RECYCLED INGOT}

The present invention relates to a method of cleaning a target material, an apparatus therefor, a method of manufacturing a target material, a target material, a method of manufacturing a reclaim ingot, and a reclaim ingot.

The sputtering target is generally formed by bonding (bonding) a target material composed of a metal, an alloy or a ceramic and a supporting member with a bonding material. The target material is recovered after its use, and the metal can be reused (recycled) as an ingot (slab, ingot) by dissolving and casting again.

Regarding the recycling of the sputtering target, for example, Japanese Patent Application Laid-Open Nos. 2005-23350, 2005-23349, and 2015/151498 disclose mechanical recycling such as acid treatment or blast treatment The removal of the surface adherend of the sputtering target is disclosed.

As a result of intensive studies, the inventors of the present invention have found that, in a sputtering target in which a target material mainly composed of metal and a support member are joined by a bonding material, the target material is separated from the sputtering target after use, It has been found that the attached bonding material can be easily removed from the target material by cleaning the target material by spraying water onto the remaining surface attached thereto.

The present invention relates to the following invention.

[1] A process for producing a target material, comprising the steps of: separating the target material from a target material mainly composed of metal; and a sputtering target having a support member joined with a bonding material; spraying water on the surface of the target material on which the bonding material is adhered And a step of removing the bonding material from the target material.

[2] The method of cleaning a target material according to [1], wherein the pressure of the water is 90 MPa or more.

[3] A method for cleaning a target material described in [1] or [2], wherein the metal is aluminum or copper.

[4] A method for producing a target material, which comprises the step of carrying out the cleaning method according to any one of [1] to [3].

[5] A target material mainly composed of a metal and a target material separated from a sputtering target in which a support member is joined with a bonding material,

And the elements derived from the bonding material and the support member are not detected by energy-dispersive X-ray fluorescence analysis.

[6] A process for producing a recycled ingot comprising the step of casting a target material obtained by performing the cleaning method according to any one of [1] to [3] to obtain a reclaim ingot containing the metal.

[7] A reclaim ingot derived from a target material mainly composed of metal and a target material of a sputtering target having a support member joined with a bonding material,

Wherein a total amount of the elements derived from the bonding material and the support member is less than 10 ppm by weight.

[8] A recycled ingot as described in [7], wherein the metal as the main component of the recycled ingot is aluminum or copper.

[9] The recycled ingot according to [7], wherein the metal as the main component of the recycled ingot is aluminum and the total amount of the elements is less than 5 ppm by weight.

[10] A sputtering target comprising a target material mainly composed of a metal and a target material separated from a sputtering target in which a support member is joined by a bonding material, water is sprayed from the target material onto the surface to which the bonding material is adhered, , The apparatus comprising:

At least one nozzle head having at least one jetting port for jetting water to the target material,

An actuator for operating the nozzle head,

And a processing chamber in which the actuator is disposed and for receiving and processing the target material.

[11] The apparatus according to [10], further comprising a clamp for fixing the target material in the treatment chamber.

[12] The apparatus according to [10] or [11], further comprising an inversion mechanism for inverting the target material.

[13] The apparatus according to any one of [10] to [12], further comprising a drain mechanism for collecting and discharging the water jetted from the jetting port and separating the processed material including the bonding material removed from the target material. .

1 is a schematic diagram showing an outline of the present invention.
Fig. 2 is a schematic view showing the coupling of the target material and the support member of the sputtering target. Fig.
Fig. 3 is a schematic view showing the coupling of the target material and the support member of another sputtering target. Fig.
4 is a schematic view showing the coupling of a target material and a support member of another sputtering target.
5 is a schematic perspective view schematically showing an embodiment of an apparatus that can be used in the present invention.
Fig. 6 is a schematic top view schematically showing an embodiment of an apparatus usable in the present invention. Fig.
7 is a schematic view showing a cross section taken along the line AA of the apparatus shown in Fig.
Fig. 8 is a schematic view showing a section in BB of the apparatus shown in Fig. 6; Fig.
9 is a schematic view schematically showing the relationship between the actuator 103 shown in Figs. 5 to 8 and the nozzle head 102. Fig.
10 is a schematic view schematically showing a membrane separation type solid-liquid separation device as an example of a drainage mechanism.
11 is a schematic view schematically showing a multistage sedimentation tank as an example of a drainage mechanism.

In the present invention, as shown in the schematic diagram of Fig. 1, for example, in the present invention, an ingot obtained by melting a metal and casting the ingot is generally processed (for example, the obtained ingot is subjected to a sintering process such as rolling or extrusion After machining such as cutting and polishing, a target material having a shape such as a flat plate shape or a cylindrical shape is manufactured, and the target material and a backing plate or backing tube, which are separately formed support members, Or by bonding.

According to one embodiment of the present invention, the sputtering target used for sputtering is separated into a target material and a support member. Further, by spraying water onto the separated target material, the bonding material can be removed from the target material. In addition, the ingot material from which the bonding material has been removed is melted and cast to obtain ingot (hereinafter referred to as "recycled ingot"). By processing the recycled ingot, the target material can be produced.

How to clean the target material

In the present invention, the " sputtering target " is not particularly limited as long as it is composed of a target material composed mainly of a metal (element) and a support member joined together by a bonding material and can be used for sputtering.

When the sputtering target is a flat plate type, a flat plate-like backing plate may be used as a supporting member. Further, when the sputtering target is cylindrical, a cylindrical backing tube may be used as the supporting member. Here, a cylindrical backing tube can be inserted into the cylindrical target member, so that the inner peripheral portion of the cylindrical target member and the outer peripheral portion of the backing tube can be joined by the bonding material.

The " target material " is mainly composed of a metal (element), for example, aluminum (Al), copper (Cu), chromium (Cr), iron (Fe), tantalum (Ta) Ti, Zr, W, Mo, Nb, Ag, Co, Ru, Pt, Pd, (Element) selected from the group consisting of gold (Au), rhodium (Rh), iridium (Ir) and nickel (Ni). The target material is preferably a metal or an alloy having a Vickers hardness of usually 200 or less, preferably 100 or less, more preferably 50 or less. Among them, it is preferable to mainly consist of aluminum (purity of 99.99% (4N) or more, preferably purity of 99.999% (5N) or more) or copper (purity of 99.99% (4N) or more). Vickers hardness can be confirmed by Vickers hardness test (JIS Z 2244: 2003). The dimensions, shape, and structure of the target material are not particularly limited. As the target material, it is preferable to use a plate-like material.

When the target material has a plate shape, the dimension of the target material in the longitudinal direction is, for example, 500 mm to 4000 mm, preferably 1000 mm to 3200 mm, and more preferably 1200 mm to 2700 mm.

The dimension in the width direction (direction perpendicular to the longitudinal direction) is, for example, 50 mm to 1200 mm, preferably 150 mm to 750 mm, and more preferably 170 mm to 300 mm.

The thickness is, for example, 5 mm to 35 mm, preferably 10 mm to 30 mm, and more preferably 12 mm to 25 mm.

In the present invention, for example, even a target material for a large flat panel display can be easily processed.

When the support member is a " backing plate ", it is mainly composed of at least one of copper (Cu), chromium (Cr), aluminum (Al), titanium (Ti), tungsten (W), molybdenum (Mo), tantalum (Element) selected from the group consisting of iron (Nb), iron (Fe), cobalt (Co) and nickel (Ni). In the case of the "backing plate", the supporting member is preferably copper (oxygen-free copper), chrome copper alloy, aluminum alloy, or the like. The size, shape, and structure of the backing plate are not particularly limited as long as it is plate-like in which the target material can be disposed.

Even when the supporting member is a " backing tube ", the constituent metal is the same as that of the backing plate. In the case of the "backing tube", the supporting member is preferably stainless steel (SUS), titanium, titanium alloy, or the like. It is preferable that the dimensions of the backing tube are longer than the cylindrical target material in order to be inserted into the cylindrical target material to join them, and the outer diameter of the backing tube is slightly smaller than the inner diameter of the cylindrical target material.

The "bonding material" is not particularly limited as long as it can be used for forming a sputtering target by contributing to the bonding of the target material and the supporting member (FIG. 2). The bonding material includes a brazing material, a hard material and the like.

The "solder material" is a material containing a metal or an alloy having a low melting point (for example, 723K or less) and is made of indium (In), tin (Sn), zinc (Zn), lead (Pb) A material containing a metal selected from the group consisting of copper (Cu), bismuth (Bi), cadmium (Cd) and antimony (Sb), or an alloy thereof. More specifically, it is preferable to use a metal such as In, In-Sn, Sn-Zn, Sn-Zn-In, In-Ag, Sn-Pb-Ag, Sn- Cd, Pb-Sn-Sb, Pb-Sn-Cd, Pb-Sn-In and Bi-Sn-Sb.

As the " hard material ", a target material and a support member can be combined, and a metal or an alloy having a melting point lower than that of the target material and the support member can be used without particular limitation.

As the bonding material, a solder material such as In or In alloy, Sn or Sn alloy generally having a low melting point is preferable.

For example, the solder material can be bonded by forming a diffusion layer (alloy layer) and a metal (element) included in the target material on the bonding surface with the target material by heating. The solder material can also be bonded to the surface of the support member by forming a diffusion layer (alloy layer) and a metal (element) included in the support member. Therefore, a solder layer can be formed of such a brazing material to bond the target material and the support member (Fig. 3).

In general, sufficient bonding strength may not be obtained due to the influence of the oxide film which may exist on the surface of the target material or the support member by merely placing the above-described solder material on the target material or the support member. For this reason, a metallization layer may first be provided to improve the wettability of the solder material to their surface.

The term " metallization " is a treatment method that can be generally used to metalize the surface of a base metal. In the present invention, for example, when a target material or a support member has an oxide film, Is used to form a metallization layer by bonding with a target material or a support member.

The metallization layer can be formed by heating, for example, using an ultrasonic soldering iron to destroy the oxide film of the target material or the support member by the vibration energy (cavitation effect) of the ultrasonic wave, Can be formed by chemically bonding metal atoms contained in the solder material of the support member and the metal atoms contained in the support member. The above-mentioned bonding material can be used for forming the metallization layer.

The metallization layers 5 and 5 '(see FIG. 4) can also be bonded to the solder layer 4 and can be bonded between the support material 2 and the solder layer 4, The solder layer 4 and the support member 2 and the solder layer 4 can be firmly bonded to each other.

The thickness of the solder layer is, for example, 10 mu m to 1000 mu m, preferably 50 mu m to 500 mu m in the case of a flat plate type and 100 mu m to 2000 mu m, preferably 250 mu m to 1500 mu m Within the range.

The thickness of the metallized layer is usually in the range of 1 탆 to 100 탆, preferably 10 탆 to 100 탆, and more preferably 5 탆 to 50 탆 in both the flat plate type and the cylindrical type.

The solder material that can be used for the metallization can be selected from the group consisting of indium (In), tin (Sn), zinc (Zn), lead (Pb), silver (Ag), copper (Cu), bismuth Cd) and antimony (Sb), or a material containing an alloy thereof. More specifically, the material may be In, In-Sn, Sn-Zn, Sn-Zn- Pb-Sn-Sb, Pb-Sn-In, Bi-Sn-Sb, Pb-Ag, Sn-Bi, Sn-Ag-Cu, Pb-Sn, And the like. A material having high affinity with the target material or the support member may be appropriately selected.

In the present invention, as shown in the schematic diagram of Fig. 1, after the sputtering target is used in sputtering, the target material is separated (peeled) from the sputtering target.

The method of separating the target material from the support member is not particularly limited. For example, heat (for example, 180 占 폚 to 300 占 폚) is applied to the bonding layer (or bonding layer) which may be formed of the bonding material, and the bonding layer is softened or melted, So that the target material can be separated from the sputtering target.

When the target material is in the form of a flat plate, it is preferable that the target material after separation has a bonding material adhered to the side (hereinafter also referred to as "bonding surface" or "bonding surface" In many cases. Even if the attached bonding material is peeled off with a spatula (for example, a spatula made of silicone) or the like, it is difficult to completely remove the bonding material. In particular, it is difficult to remove the metallized layer combined with the target material, and usually a metallization layer with a thickness of several micrometers and a solder layer with a thickness of about 50 to 200 m remain. The bonding material may adhere and remain on the sputtering surface of the target material. The reason for this is that, for example, when the target material is separated, the molten bonding material adheres to the sputtering surface. As another principle, since the separated target materials are stacked and stored, the bonding surface and the sputtering surface are in contact with each other, and the bonding material of the bonding surface is attached to the sputtering surface.

When the target material is cylindrical, the cylindrical target material can be bonded to the outer peripheral portion of the cylindrical backing tube by using a bonding material. Therefore, similarly to the case of the plate target described above, And it is not possible to completely remove the bonding material, including the metallization layer. The bonding material may remain on the sputtering surface of the target material. The components derived from the backing tube may also be incorporated as impurities. Therefore, the cleaning method may also be applied to the outer peripheral portion or the inner peripheral portion, which is the sputtering surface, of the cylindrical target material.

The existence of adhesion of the bonding material in the target material after separation can be confirmed by, for example, energy dispersive X-ray fluorescence analysis (EDXRF).

In addition, the metal element may diffuse from the support member to the target material (particularly, in the vicinity of the bonding surface). These metal elements can also be confirmed by EDXRF. In addition, wavelength dispersive X-ray fluorescence analysis (WDXRF), electron probe microanalysis (EPMA), Auger electron spectroscopy (AES), X- ICP-MS, X-ray photoelectron spectroscopy (XPS), Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS), and Laser Induced Coupled Plasma Mass Spectrometry : Laser Ablation Inductively Coupled Plasma Mass Spectrometry (XRD), and X-ray Diffraction Analysis (XRD). Although the impurities derived from the bonding material and the supporting member can be identified, It is preferable to confirm from EDXRF and WDXRF from the width.

Here, when an ingot (hereinafter sometimes referred to as "slab" or "ingot") is produced by using the target material after the separation with the bonding material attached thereto as it is and manufacturing the target material from the ingot, Impurities are mixed. Further, the metal element may diffuse from the support member to the target material and may be mixed as an impurity. Such a metal element may also be incorporated into the ingot as an impurity.

In the present invention, after the target material is separated from the sputtering target, the target material may be cleaned by spraying water on at least the remaining surface of the target material with the bonding material attached thereto to remove the attached bonding material from the target material 1). Further, the metalization layer bonded to the target material can also be removed by the cleaning.

The method of spraying water is not particularly limited, but it is preferable to spray water under the following conditions.

The injection of water can be performed, for example, by using a pump, and it is preferable to spray water at a high pressure (hereinafter sometimes referred to as " water jet "). The pressure for spraying water is, for example, 90 MPa or more, preferably 90 MPa to 350 MPa, more preferably 100 MPa to 300 MPa, more preferably 150 MPa to 280 MPa, and particularly preferably 180 MPa to 250 MPa. By increasing the injection pressure, the bonding material, particularly the metallization layer, can be removed, and a sufficient cleaning effect can be obtained. By lowering the injection pressure to some extent, it is possible to prevent the target material itself from being excessively shaved beyond the metallization layer. If the target material itself is shaved deeply, for example, by 1.5 mm or more, the yield may be deteriorated or the equipment cost may increase.

The injection of water is preferably carried out using a rotary (or rotatable) nozzle head having a plurality of nozzles (or nozzles). The shape of the nozzle head is not particularly limited and the shape of the side of the nozzle head facing the target material (or the side on which the nozzle is provided) may be a polygonal shape such as a triangular shape or a rectangular shape, However, in order to rotate and spray water, regular polygonal shapes such as circular and square shapes are preferable, and a true circular shape is more preferable. It is preferable to use a nozzle head capable of mounting the jetting port so that water is jetted in a direction substantially parallel to the rotational axis of the nozzle head. It is preferable to use a nozzle head capable of mounting the jetting port so that water is jetted in a direction substantially perpendicular to the rotational axis of the nozzle head when treating the joint surface (inner peripheral portion) of the cylindrical target material.

The number of ejection openings (or the number of nozzles) provided in one nozzle head is not particularly limited, and is, for example, one or more, preferably one to fifteen, more preferably three to ten. The number of nozzles may be appropriately determined in accordance with the size of the nozzle head. By making the number of nozzles larger, it is possible to prevent a residue of a bonding material or the like from being generated or a processing time to be long. If the number of nozzles is large, the total discharge amount increases, so that a larger and more expensive pump is required, which may increase the equipment cost. When a plurality of ejection openings are provided in the nozzle head, the ejection openings may be arranged at the same diameter position or at different diameter positions of the nozzle head. Further, it may be a combination of a long-diameter arrangement and a short-diameter arrangement.

The dimension of the jetting port (nozzle diameter) is, for example, 0.1 mm or more, preferably 0.15 mm to 0.50 mm, and more preferably 0.2 mm to 0.35 mm. The ejection openings having the same diameter may be mounted on the nozzle head, or the ejection openings having different diameters may be combined and mounted on the nozzle head.

The amount of water discharged (or the amount of water) changes depending on the pressure of the water to be sprayed and the dimension of the jetting port, and the cleaning effect becomes higher as the size of the jetting port increases. The total discharge amount of water jetted from the total jetting ports of one nozzle head is, for example, 2.0 L / min or more, preferably 2.0 L / min to 42 L / min, more preferably 5.0 L / min to 30 L / min , More preferably 5.0 L / min to 20 L / min.

It is preferable that the jetting of water is performed in the form of a belt (line) in the horizontal direction at a constant speed while maintaining a constant distance from the treated surface of the target material. The injection of water may be repeated several times, preferably once to three times, at the same place. Alternatively, in the case where the processing width in one injection of water is smaller than the target width, water may be injected partially overlapping (overlapping) in a line shape.

The moving speed of the nozzle head is, for example, 100 mm / min or more, preferably 500 mm / min to 7000 mm / min, and more preferably 900 mm / min to 5000 mm / min. By increasing the moving speed, the processing time can be shortened. If the moving speed is reduced, a sufficient cleaning effect can be obtained.

The rotational speed of the nozzle head is, for example, 500min ^-1 or more, preferably 500min ^-1 ~ 4000min ^-1, more preferably 900min ^-1 ~ 2500min ^-1. By increasing the rotation speed, depending on the number of the nozzles, the water touches the entire surface of the target material, and the residue of the bonding material or the like can be prevented. When the rotational speed is reduced, the impact when the target material is touched is increased, so that a sufficient cleaning effect can be obtained.

The distance (or nozzle distance) between the nozzle head and the target material is, for example, 10 mm or more, preferably 15 mm to 100 mm, and more preferably 20 mm to 70 mm. By increasing the distance to some extent, it is possible to prevent the influence of the protruding water from reaching the target material, and as a result, a sufficient cleaning effect can be obtained. By reducing the distance to some extent, the impact at the time of contact with the target material becomes large, so that a sufficient cleaning effect can be obtained.

The water to be sprayed is not particularly limited as long as it does not contain particle-like impurities or dust that may block the nozzle, for example, use of tap water or pure water. Further, a filter may be provided between the pump and the nozzle, and water may be injected through the filter.

The spraying direction of water is not particularly limited as long as the target material is in contact with water, and it may be perpendicular or inclined with respect to the target material. For example, the angle of the jetting port (the angle between the central axis of the jetting port and the perpendicular to the target material) is 0 ° to 60 °, preferably 0 ° to 45 °, more preferably 5 ° to 45 °, More preferably 5 ° to 30 °, even more preferably 8 ° to 30 °, particularly preferably 10 ° to 25 °. When water is injected obliquely to the target material, since the nozzle head rotates, the processing width becomes larger than when the nozzle is vertically jetted. The water contacted to the target material does not stay on the treatment surface and is avoided to the outside, so that the cleaning effect is also expected to be improved. When water is sprayed obliquely from the nozzle head, cleaning of the side surface can be performed while the nozzle head is positioned above the target material.

By setting the direction of spraying of the water within the above-described range, it is possible to prevent a decrease in impact when it touches the target material, and a sufficient cleaning effect can be obtained. Further, with respect to the treatment of the bonding surface of the target material, the treatment of the sputtering surface, and the treatment of the side surface, it is not necessary to set the target material again or change the position of the nozzle head. When a plurality of jetting ports are provided in the nozzle head, the angles of the respective nozzles may be the same or different. The angle of each jetting port may be appropriately determined so as not to produce a desired processing width or a residual due to the non-contact of water.

The nozzle head may simultaneously scan a plurality of nozzle heads to shorten the processing time per target material.

In the above description, the rotary nozzle head is used. However, in the case where the target material can be rotated or the flat nozzle nozzle in which water is linearly sprayed is used, a fixed nozzle head is used The target material can be efficiently cleaned.

When the joining material and the metalized layer are sufficiently removed by cleaning from the joint surface of the used target material, the surface of the target material itself is also cut away. In this case, the surface of the target material itself is preferably 5 占 퐉 or more, preferably 10 占 퐉 or more and 1000 占 퐉 or less, preferably 20 占 퐉 or more and 750 占 퐉 or less, more preferably 50 占 퐉 or more and 500 占 퐉 Or less, and the cleaned surface can be an irregular surface. (Scales, spirals, etc.) may be formed in accordance with the movement of the nozzle head at the time of cleaning. In the case of an easy-to-see shape, the specular reflectance at a wavelength of 300 nm to 1500 nm of the cleaned surface is usually 1.0% or less. To confirm that the impurities derived from the bonding material and the supporting member are sufficiently removed, to be.

The rate of change of the reflectance (wavelength of the cleaned surface / reflectance of the surface before cleaning) relative to the wavelength of each incident light at a wavelength of 300 nm to 1500 nm is usually 0.025 or more and 0.85 or less, preferably 0.05 or more and 0.75 or less, More preferably not less than 0.08 and not more than 0.60, and more preferably not less than 0.10 but not more than 0.40, it is possible to confirm that the impurities derived from the bonding material and the supporting member are sufficiently removed, and that the target material is excessively removed Can be prevented.

The arithmetic mean roughness (Ra) at the bonding surface of the target material after cleaning is not less than 5 占 퐉 and preferably not less than 10 占 퐉, more preferably not less than 15 占 퐉 in order to confirm that impurities derived from the bonding material and the support member are sufficiently removed. Mu m or more. (Arithmetic mean roughness (Ra) of the cleaned surface / arithmetic mean roughness (Ra) of the surface before cleaning) of the arithmetic mean roughness (Ra) before and after cleaning is preferably 4 or more and 80 or less, More preferably 7.5 or more and 20 or less, and still more preferably 10 or more and 15 or less. The arithmetic mean roughness (Ra) at the bonding surface of the target material after cleaning is usually 100 占 퐉 or less, preferably 50 占 퐉 or less. If the arithmetic mean roughness (Ra) is too large, foreign matter such as dust or sand tends to adhere, or the thickness of the oxide film becomes thick, and the impurities in the recycled ingot may increase.

According to the cleaning method of the present invention, the lower detection limit of EDXRF (usually, the lower detection limit varies depending on the element, for example, the detection limit of the impurity derived from the bonding material is about 0.01 wt% The amount of the element derived from the bonding material and the supporting member can be reduced to a value lower than that of the bonding material and the supporting member. That is, according to the present invention, in the target material after cleaning, the bonding material and the element derived from the supporting member are substantially not detected (or the target material after cleaning does not substantially contain elements derived from the bonding material and the supporting member) .

In the present invention, " substantially no element derived from the bonding material and the supporting member is detected " (or " substantially not including the element derived from the bonding material and the supporting member " Means that the amount of elements derived from the bonding material and the support member is reduced to a level that is smaller than the lower limit and can not be detected in EDXRF. Here, the " impurity " derived from the bonding material or the supporting member indicates only the main elements constituting the bonding material and the supporting member. &Quot; Element derived from bonding material and supporting member " means the main element constituting the bonding material and supporting member. The content of the element is usually 0.1 parts by mass, preferably 0.5 parts by mass or more, and more preferably 1 part by mass or more based on 100 parts by mass of the bonding material and the supporting member.

The cleaning method of the present invention is different from the method of machining a flat surface at a predetermined height, such as a cutting process by a flat, and is a method of efficiently carving out only the surface of a target material (or a work) . Therefore, the cleaning method of the present invention is capable of processing at a high yield even if there is irregularity or deformation in the target material, and can be applied not only to the joining surface of the target material but also to the sputtering surface of the target material having irregularities formed by sputtering, And the like.

Further, since the cleaning method of the present invention can set the work without paying attention to the height of the processing surface, it is possible to easily perform the setting without requiring time for setting and cleaning. Therefore, the conventional method such as blasting and cutting There are many advantages compared to.

Device

The present invention also relates to a device usable in the cleaning method described above. More specifically, at least a target material composed of metal described above and a target material (or a used target material) separated from a sputtering target in which a support member is joined with a bonding material are provided on at least a surface to which the bonding material is attached (Hereinafter sometimes referred to simply as a " cleaning apparatus ").

The cleaning apparatus may include at least the following constitutions (a) to (c).

(a) at least one nozzle head having at least one jetting orifice for jetting water to a target material

(b) an actuator for manipulating or moving the nozzle head

(c) an actuator is disposed, and a processing chamber for containing and treating the target material

For example, as shown in FIGS. 5 to 8, the apparatus 100 includes, at least,

At least one nozzle head 102 having at least one jetting port (not shown) capable of jetting water to the used target material (or workpiece) 101,

An X-axis slider 103Y, a Y-axis slider 103Y and a Z-axis slider 103Z capable of operating (or moving) the nozzle head 102. The nozzle head 102 ) Can be moved in any direction of the X, Y and Z axes,

And a treatment chamber 104 capable of disposing an actuator and capable of receiving (treating) the target material 101 (or cleaning).

In the illustrated embodiment, the target material 101 is described as a flat plate, but the target material 101 usable in the apparatus 100 is not limited to a flat plate.

· Nozzle head

The nozzle head can be used without particular limitation as long as it has at least one jetting orifice (or nozzle) capable of jetting water. There is no particular limitation on the number of nozzle heads to be used. When a plurality of nozzle heads are used, it is preferable that the nozzles are arranged at appropriate intervals so that the water sprayed from the nozzles does not interfere with each other.

Further, the apparatus of the present invention may further include a nozzle head (or a side nozzle head) for spraying water on the side surface of the workpiece for cleaning. There are no particular restrictions on the number of nozzle heads used to process the sides of the workpiece (X-Z surface and / or Y-Z surface) and the location of the placement.

As the nozzle head, those described in detail in the above-mentioned " method for cleaning the target material " can be appropriately used without limitation.

And a rotary unit for rotating the nozzle head.

· Actuator

As the actuator, any actuator capable of operating or moving the nozzle head may be used by using driving force by electric, hydraulic, air pressure or the like. Preferably, at least one of the X-axis, the Y-axis, and the Z-axis, and more preferably, the nozzle head can arbitrarily and suitably move in all directions of the X-axis, the Y-axis, and the Z-

More specifically, as shown in Figs. 5 to 9 (particularly, Fig. 9), in order to move the nozzle head in all directions of the X axis, Y axis and Z axis, the X axis slider 103X, A Y-axis slider 103Y, and a Z-axis slider 103Z can be used.

The nozzle head 102 is configured to be able to directly or indirectly be coupled to the Z-axis slider 103Z via a rod 106 or the like as required, for example. The Z-axis slider 103Z , The nozzle head 102 can be moved in the Z-axis direction (the up-down direction or the direction in which the target material 101 approaches or moves away from the target surface) (Fig. 9). In another embodiment, the Z-axis slider 103Z may be configured so that the rod 106 passes through the Z-axis slider 103Z.

The Z-axis slider 103Z is configured to be physically or mechanically coupled to the Y-axis slider 103Y so that the nozzle head 102 can be moved along with the slider 103Z to the Y- (The direction in which the target material 101 advances or the direction perpendicular to the device 100 or the longitudinal direction of the target material 101 shown in Fig. 9).

The Y axis slider 103Y is configured so as to be physically or mechanically coupled to the X axis slider 103X so that the X axis slider 103X moves the nozzle head 102 along with the sliders 103Y and 103Z (The direction of travel of the target material 101 or the longitudinal direction of the device 100 or the target material 101 shown in Fig. 9) (Fig. 9). The end of the Y-axis slider 103Y on the opposite side to the end engaged with the X-axis slider 103X is engaged with a support guide (or guide rail) that can be disposed in parallel with the X- ).

By using the actuator 103 (Fig. 9) including the sliders 103X, 103Y and 103Z, the nozzle head 102 can be appropriately moved in three directions of the X axis, Y axis and Z axis.

As long as the sliders 103X, 103Y, and 103Z can be slidably moved relative to each other using a driving force by electricity, hydraulic pressure, air pressure, or the like, there is no particular limitation on the driving style and the combining style.

The movement of the nozzle head by the actuator and the injection of water may be controlled by an electronic program. In this case, each slider may be suitably connected by an electric cable or the like. The moving speed of the nozzle head and the jetting of water are preferably controlled as defined in the above-described " cleaning method of the target material ".

The actuator may be waterproof and waterproof, thereby preventing the problem of rust and oil falling caused by contact of the sprayed water or the target material with the generated water. In the case of connecting each slider of the actuator with an electric cable, it is preferable that the electric cable is also waterproof.

Although water may be injected vertically downward from the nozzle head as in the illustrated embodiment, a mechanism capable of changing the angle of the nozzle head may be further arranged as required. In this case, the angle of the nozzle head can also be controlled by an electronic program. With such a mechanism, the cylindrical target material can be more efficiently cleaned.

As the actuator, for example, a three-axis combination type industrial robot made by IAI Co., Ltd. may be used.

Further, the actuators usable in the apparatus of the present invention are not limited to those described above.

· Treatment room

The main purpose of the treatment chamber is to dispose the actuator described above together with the nozzle head, to receive the target material, and to treat the target material according to the above-described " target material cleaning method ".

By treating the target material in the treatment chamber, water sprayed from the nozzle head due to contact with the target material, or solid treated material (or dust) containing the bonding material removed from the target material scattered around, Can be prevented.

For example, as shown in Figs. 5 to 8, the processing chamber 104 has a rectangular main body and its upper portion is opened, and the actuator (concretely, the sliders 103X, 103Y, (The actuator 103 including the actuator 103).

The size of the treatment chamber 104 is not particularly limited, and it is preferable that the target material for a large sputtering target can be treated.

In the case of transporting the target material 101 along the longitudinal direction thereof as in the illustrated embodiment, the ratio (X / Y) of the dimension in the X-axis direction to the dimension in the Y-axis direction of the treatment chamber 104 is, for example, 3/16 to 10/1, preferably 1/2 to 10/3, and more preferably 6/7 to 7/3.

The ratio (X / Z) of the dimension in the X-axis direction to the dimension in the Z-axis direction is, for example, 1/3 to 10/1, preferably 1/2 to 4/1, more preferably 5/6 ~ 35/12.

The ratio (Y / Z) of the dimension in the Y-axis direction to the dimension in the Z-axis direction is, for example, 1/5 to 8/1, preferably 3/5 to 2/1, more preferably 5/6 ~ 35/24.

In this case, the dimension in the X-axis direction is, for example, 750 mm to 5000 mm, preferably 1000 mm to 4000 mm, and more preferably 1500 mm to 3500 mm.

The dimension in the Y-axis direction is, for example, 500 mm to 4000 mm, preferably 1200 mm to 2000 mm, and more preferably 1500 mm to 1750 mm.

Specifically, the dimension in the Z-axis direction is, for example, 500 mm to 2500 mm, preferably 1000 mm to 2000 mm, and more preferably 1200 mm to 1750 mm.

In the illustrated embodiment, the target material 101 is conveyed along the longitudinal direction thereof by using the conveying means 105 such as a belt conveyor or a roller, which will be described in detail below, The target material 101 may be transported along the width direction (direction perpendicular to the longitudinal direction) of the target material 101 (for example, along the Y axis) The ashes 101 may be processed.

The ratio (X / Y) of the dimension in the X-axis direction to the dimension in the Y-axis direction of the treatment chamber 104 in the case of transporting the target material 101 along the width direction (direction perpendicular to the longitudinal direction) For example, from 3/16 to 10/1, preferably from 1/2 to 10/3, and more preferably from 6/7 to 7/3.

The ratio (X / Z) of the dimension in the X-axis direction to the dimension in the Z-axis direction is, for example, 1/3 to 10/1, preferably 1/2 to 4/1, more preferably 5/6 ~ 35/12.

The ratio (Y / Z) of the dimension in the Y-axis direction to the dimension in the Z-axis direction is, for example, 1/5 to 8/1, preferably 3/5 to 2/1, more preferably 5/6 ~ 35/24.

In this case, the dimension in the X-axis direction is, for example, 750 mm to 5000 mm, preferably 1000 mm to 4000 mm, and more preferably 1500 mm to 3500 mm.

The dimension in the Y-axis direction is, for example, 500 mm to 4000 mm, preferably 1200 mm to 2000 mm, and more preferably 1500 mm to 1750 mm.

The dimension in the Z-axis direction is, for example, 500 mm to 2500 mm, preferably 1000 mm to 2000 mm, and more preferably 1200 mm to 1800 mm.

When the conveying means 105 is used, the processing chamber 104 may have a pair of openings (inlet and outlet) through which the conveying means 105 and the target material 101 pass. The size of the opening is not particularly limited as long as it is possible to pass the target material 101 through.

When the target material 101 is transported along its longitudinal direction as shown in the illustrated embodiment, the dimension of the opening in the Y-axis direction is, for example, 100 mm or more, preferably 150 mm to 1500 mm, The dimension in the Z-axis direction is, for example, 10 mm or more, preferably 12 mm to 300 mm, more preferably 20 mm to 200 mm, and even more preferably 45 mm to 150 mm .

When the target material 101 is transported along its width direction (direction perpendicular to the longitudinal direction), the dimension of the opening in the X-axis direction is, for example, 500 mm or more, preferably 750 mm to 4000 mm, The dimension in the Z-axis direction is, for example, 10 mm or more, preferably 12 mm to 300 mm, more preferably 20 mm to 200 mm, still more preferably 45 mm to 300 mm, 150 mm.

In the above embodiment, the apparatus capable of transporting the target material 101 has been described. However, the cleaning apparatus of the present invention does not need to include the conveying means 105. [

In the embodiment shown in Fig. 5, the opening is also shown on the side surface (X-Z plane) so that the inside of the processing chamber 104 can be seen clearly. However, such opening may or may not exist. When such openings are present, opening and closing doors (for example, right and left door) may be provided in these openings to prevent splashing of water or dust. By providing such a door, maintenance in the processing chamber 104 can be simplified.

The bottom of the inside of the treatment chamber 104 is filled with water (including solid matter (or dust) including the bonding material removed from the target material) (hereinafter referred to as " , And a pool (not shown) for temporarily storing the water (hereinafter referred to as " treated water ").

In the inside of the treatment chamber 104, a discharge port (not shown) for discharging treated water may be provided. The discharge port may be disposed on the bottom surface of the process chamber 104. However, since the process material may accumulate to block the discharge port, the discharge port may be spaced from the bottom surface by an interval of, for example, 1 mm to 50 mm, preferably 10 mm to 25 mm It can also be placed on the side. There is no particular limitation on the shape, dimension and structure of the discharge port as long as it can discharge the treated water.

In addition, a shower mechanism may be optionally provided in the processing chamber 104 to wash the processing material attached to the inner wall surface of the processing chamber 104.

The treatment chamber usable in the apparatus of the present invention is not limited to the above.

Other configurations

In addition to the above configuration, the apparatus may include other configurations.

·clamp

The apparatus of the present invention may further comprise a clamp for fixing the target material in the treatment chamber. By fixing the target material with a clamp, the target material can be fixed so as not to move during the cleaning process. There is no particular limitation on the position of the clamp in the treatment chamber. It is preferable to fix the side surface of the target material from both sides thereof. By so fixing, the target surface of the target material is not covered with the clamp, and water can be sprayed over the entire surface of the target surface.

In the case where the target material is deformed and bent in an arcuate shape, when the water is sprayed from above the target material, the target material may vibrate and the performance of the cleaning treatment may be lowered. However, The vibration of the target material can be suppressed.

In the case where there is little warpage of the target material or when there is a base under the target material, it is only necessary to fix the target material so that the target material does not move from a predetermined predetermined position because the water is sprayed from above the vertical direction of the target material.

There is an advantage that it is not necessary to perform zero point adjustment (designation of a processing range) at the time of operating the nozzle head by fixing the target material with a clamp at a predetermined predetermined position (positioning of the target material).

There is no limitation on the shape and dimensions of the clamp, but it is preferable to use a clamp capable of fixing the side surface of the target material from both sides thereof as described above. For example, Imao Corporation, a side clamp manufactured by Tsudakoma Kogyo Co., Ltd., and the like can be used. The number of clamps and the position at which the clamps are arranged are not particularly limited and may be appropriately determined in accordance with the target material.

The mechanism of the clamp may be automatic or manual. However, in order to simplify the task of fixing the large target member, it is necessary to provide a mechanism for automatically setting the target member such that the side surface of the target member is sandwiched from both sides thereof . When the clamp is of the manual type, it is preferable to provide an opening, preferably an opening and closing door, on the side surface (X-Z surface) of the processing chamber 104 from the viewpoint of workability.

· Carrier

The apparatus of the present invention may include a transport mechanism capable of transporting a target material into the treatment chamber and carrying out the target material from the treatment chamber (for example, the transport means 105 shown in Figs. 5 to 8).

The conveying mechanism may be any type of conveying mechanism capable of conveying the target material such as a belt conveyor, a roller conveyor, a conveyor such as a caterpillar, a shuttle conveying, a pallet conveying, a vacuum chuck conveying, .

The conveying speed of the target material by the conveying mechanism is not particularly limited, but is, for example, 15 m / min to 60 m / min, preferably 20 m / min to 50 m / min, more preferably 25 m / min to 40 m / min.

The transport mechanism may form a continuous loop so that the target material can be carried into the processing chamber again after the target material is taken out from the processing chamber.

The transport mechanism may be one which can be arbitrarily divided depending on the purpose of carrying, carrying out, processing chamber contents, loop, and the like.

The transport mechanism may be provided with a target material supply mechanism on the inlet side of the treatment chamber and a reversing mechanism of the target material may be provided on the outlet side of the treatment chamber.

· The supply mechanism of the target material

The apparatus of the present invention may include a supply mechanism of the target material so that the target material can be appropriately supplied to the above-described transport mechanism. The supply mechanism of the target material is not particularly limited as long as it can appropriately supply the target material. The supply mechanism of the target material may include a cassette for storing a plurality of target materials, and if necessary, the target material may be appropriately supplied. As a supply mechanism of the target material, a commercially available automatic feeder may be used.

· Reversing mechanism of target material

The apparatus of the present invention may further include an inversion mechanism for inverting the target material, preferably a mechanism capable of reversing the target material in a state in which the target material is fixed (for example, clamped). By including such an inversion mechanism, the target surface of the target material can be reversed arbitrarily. The dimensions of the reversing mechanism are not particularly limited.

A commercially available automatic inversion device may be used, for example, an automatic inversion device of Advex Co., Ltd. may be used.

· Drainage

The treated water after the target material has been washed contains the solid treated material (or dust) containing the bonding material removed from the target material, and the apparatus of the present invention can remove the desired A drainage mechanism capable of collecting and discharging only water and discharging a solid treated material such as a bonding material may be included.

The drainage mechanism can be used without particular limitation as long as it can separate the solid and the liquid. In this field, commonly known solid-liquid separators can be suitably used as needed.

Preferably, the drainage mechanism is connected to an outlet that can be provided inside the treatment chamber.

For example, a membrane separation type solid-liquid separation device which can be generally used for water treatment can be used. In the membrane separation type solid-liquid separation apparatus, at least one membrane cartridge including a membrane capable of solid-liquid separation is used, and the collected water is sucked and filtered by a pump through a collecting pipe connected to such a membrane cartridge, (Fig. 10). At this time, the treated material can be settled in the bottom of the tank, so it can be recovered separately and reused.

As the drainage mechanism, a sedimentation tank capable of separating solid and liquid by sedimentation may be used. For example, a hopper-type sedimentation tank generally used for water treatment, a circular sedimentation tank equipped with a central drive scraper, a transverse sedimentation tank, and the like can be given. By using such a settling tank, it is possible to separately recover the solid treated material including the bonding material removed from the target material.

Alternatively, the solid and the liquid may be separated using a multistage sedimentation tank as shown in Fig. The multistage settling tank can be drained from the upper side of the settling tank to the lower settling tank sequentially from the settling tank having a high water level to the settling tank having a low water level with a plurality of settling tanks. The treated material is settled in the bottom of each settling tank and can be recovered separately and reused.

There is no particular limitation on the number of stages of the sedimentation tank and the capacity of each sedimentation tank. The drainage from the settling tank to the next settling tank may be performed using a pump.

· Side nozzle head

The apparatus of the present invention may include at least one side nozzle head having at least one nozzle for spraying water on the side surface of the target material in the treatment chamber. As the side nozzle head, the nozzle head described in the above-described " method for cleaning the target material " can be used as described above. The side nozzle heads may be fixed or movable. When the side nozzle head is movable, it is preferable to move the side nozzle head along the X axis or the Y axis.

There are no particular limitations on the position and the number of the side nozzle heads.

By using such a side nozzle head as needed, it is possible to perform the cleaning treatment three-dimensionally including not only the main surface of the target material but also the side surface thereof.

·Pump

The apparatus of the present invention may include a pump capable of supplying water to the above described nozzle head and / or side nozzle head. As the pump, for example, the pump described in the above-described " method for cleaning the target material "

The pump can be connected to the nozzle head and / or the side nozzle head through a fluid-connectable line, preferably a pressure-resistant line. These lines may be arranged arbitrarily and may be arranged along the rod 106 shown in FIGS. 5 to 8 or through the interior of the rod 106, for example. Such a pump may be disposed either inside or outside the treatment chamber, but is preferably disposed outside the treatment chamber. There is no particular limitation on the number of pumps to be used, and a plurality of pumps may be used.

· Control means

The configuration described above can be appropriately controlled by using the control means. Examples of the control means include a CPU, a ROM, a RAM, and the like. The configuration described above can be arbitrarily selected and electrically connected, and the configuration can be controlled by such control means using an electronic program as required.

· Drying equipment

The apparatus of the present invention may include a drying mechanism for rapidly removing water adhered to the used target material after cleaning, both inside and outside the treatment chamber. By removing the water, it is possible to prevent problems such as contamination of foreign matters caused by the water adhering to the raw material when the used target after washing is melted and cast as a raw material.

Examples of the drying mechanism include a drying mechanism by blowing air such as dry air or nitrogen gas to the used target material after cleaning and blowing water adhering to the target material, A drying mechanism by heating can be employed. In the case where the processing chamber 104 has an opening (exit) through which the conveying means 105 and the target material 101 pass, it is preferable to provide a drying mechanism by blowing air to any of adjacencies of inside and outside of the opening.

[Preferred Embodiment of Cleaning Apparatus]

The apparatus, in a preferred embodiment,

A nozzle head,

An actuator,

A processing chamber,

At least one component selected from the group consisting of a clamp, a side nozzle head, a reversing mechanism, a drainage mechanism, a drying mechanism, and a transport mechanism.

The device of the present invention should not be construed to be limited to the configuration including the above configuration.

Manufacturing method of recycled ingot

The reclaim ingot can be produced by dissolving and casting the target material obtained by the manufacturing method including the step of carrying out the cleaning method of the present invention, for example, as shown in Fig.

As a method for producing the recycled ingot, the target material washed in accordance with the present invention can be manufactured through a process of melting or casting. The melting and casting can be performed in a known order. As the recycling ingot, the melting method may be dissolving in the air or in a vacuum by an electric furnace or a burning furnace. As the casting method, a continuous casting method, a semi-continuous casting method, a metal casting method, a precision casting method, a hot- Can be adopted. Further, degassing treatment and inclusion removing treatment may be performed during the dissolution and casting steps.

The production conditions (temperature, etc.) of the recycled ingot may be appropriately determined according to the metal (element) mainly included in the target material.

When the metal contained as the main component in the target material is aluminum, the target material after being cleaned may be carbon or alumina at a temperature of 670 to 1200 占 폚, preferably 750 to 850 占 폚 in a vacuum state (e.g., 0.03 Torr) Or the like, and if necessary, stirring is carried out in the air to remove the dross, and then the mixture is cooled in the atmosphere, whereby recycled ingot can be produced.

When the metal contained as the main component in the target material is copper, the target material after being cleaned may be carbon, alumina or the like at a temperature of 1100 to 1500 占 폚, preferably 1150 to 1200 占 폚 under vacuum (for example, 0.03 Torr) And then the dross is removed by stirring in an atmosphere if necessary, followed by cooling in the atmosphere, whereby a recycled ingot can be produced.

The recycled ingot may be produced only from a target material after cleaning, or may be a mixture of a conventional raw material metal and a target material after cleaning.

When the raw material metal and the target after cleaning are mixed, the mixing ratio of the target material after the cleaning is usually 20 wt% or more, and it is preferable that the mixing ratio is 50 wt% or more in order to suppress the ratio of the raw material cost in the production cost.

Recycled ingot

The recycled ingot of the present invention is a reclaim ingot derived from a target material of a sputtering target in which a target material mainly composed of metal and a supporting member are joined together by a bonding material. As described above, , And may have substantially the same composition as the original (unused) target material. Therefore, a target material having substantially the same composition as the original target material can be manufactured from the recycled ingot.

Here, "having substantially the same composition as the original target material" means that the main metal (element) is the same and can contain the same amount of impurities as those of the original target material.

The recycled ingot generally has a total amount of impurities derived from the bonding material and the supporting member of usually less than 10 ppm, preferably 0.1 ppm to 8 ppm, more preferably 5 ppm or less (or less), more preferably 0.1 ppm to 5 ppm, and even more preferably 0.1 ppm to 2 ppm. The total amount of impurities in the recycled ingot is, for example, less than 50 ppm, preferably 0.1 ppm to 20 ppm, more preferably 0.1 ppm to 10 ppm, more preferably 5 ppm or less (or less) And is in the range of 0.1 ppm to 5 ppm. The impurities contained in the original target material and the amount thereof may depend on the kind of the metal contained as the main component in the target material and the method of producing the original target material.

The recycled ingot may be used for purposes other than the target material, and may also be used as a raw material for products requiring high purity such as aluminum electrolytic capacitors, hard disk substrates, corrosion-resistant materials, and high-purity alumina.

When the metal contained as the main component in the target material is aluminum, the total amount of the elements derived from the bonding material and the support member contained in the recycled ingot is, for example, less than 10 ppm, preferably 0.1 ppm to 8 ppm, Preferably 5 ppm or less (or less), more preferably 0.1 ppm to 5 ppm, and even more preferably 0.1 ppm to 2 ppm. For example, a target material made of aluminum for flat display usually has a content of 50 ppm or less, preferably 0.1 ppm to 20 ppm, more preferably 0.1 ppm to 10 ppm, and even more preferably 5 ppm (or less) , There is no particular problem in sputtering.

When the metal contained as the main component in the target material is copper, the total amount of the elements derived from the bonding material and the support member contained in the recycled ingot is usually less than 10 ppm, preferably 0.05 ppm to 9 ppm, 0.05 ppm to 8 ppm. It is known that the target material made of oxygen-free copper for flat display, for example, may contain impurities of usually 100 ppm or less, preferably 0.1 ppm to 75 ppm, more preferably 0.1 ppm to 50 ppm, The sputtering is not particularly affected.

Since the amount of impurities contained in the recycled ingot is very small, the amount of such impurities can be measured using Glow Discharge Mass Spectrometry (GDMS). The quantitative lower limit of the GDMS varies depending on the principal element of the target material and the element to be detected. For example, when the metal containing the target material as the main component is aluminum, it is usually 0.001 ppm to 0.1 ppm, to be.

As described above, according to the present invention, the used target material can be easily cleaned, and the target material after cleaning does not substantially contain elements derived from the bonding material and the supporting member. Therefore, by recycling (or recycling) the target material treated by this cleaning method, it is possible to obtain a recycled ingot substantially containing no elements derived from the bonding material and the supporting member. That is, according to the present invention, a target material having substantially the same composition as the original target material can be easily reproduced.

According to the present invention, it is possible to efficiently remove a bonding material (solder material, hard material, etc.) present in the surface layer of a target material mainly composed of metal.

It is necessary to increase the water pressure of the water jet (for example, increase to 90 MPa or more) in accordance with the bonding state of the bonding material in the surface layer of the target material, particularly the formation state of the metallization layer. However, , It is possible to remove the bonding material without damaging the target material itself even if water of high water pressure is exposed.

Hereinafter, the present invention will be described in detail with reference to examples of the present invention, but the present invention is not limited to the following examples.

[Example]

Example 1

The target material was separated from the backing plate by heating (280 DEG C) the bonding layer of the used sputtering target.

The sputtering target was prepared in the same manner as in Example 1 except that a flat plate type target material (purity: 99.999%, Vickers hardness: 15-17, dimensions: 2000 mm x 200 mm x 15 mm) made of aluminum and a backing plate made of oxygen- (Solder material of Sn-Zn-In is used for the metallization of the target material) with a solder material (thickness of solder layer: 350 mu m) of In.

Further, the solder material attached to the bonded surfaces of the separated target materials was scraped with a spatula made of silicon, and the solder material was recovered as much as possible. After separating from the backing plate, the target material was cut to a size of about 300 mm x 200 mm x 15 mm.

Three nozzles of a nozzle diameter of 0.25 mm (manufactured by Sugino Machine Co., Ltd., model number: DN-0825) and 0.30 mm (model number: DN-0830 manufactured by Sugino Machine Co., Ltd., , A neodymium nozzle head (model number: MNH-2506CH, manufactured by Sugino Machine Co., Ltd.) equipped with a nozzle head of 0.30 mm on the outside of the nozzle head and a 0.25 mm nozzle on the inside side of the nozzle head) Water was sprayed onto the bonded surface and the sputtering surface of the ashes to clean the entire surface (water pressure: 245 MPa, quantity: 11.6 L / min, distance between the target material and the nozzle head: 55 mm, injection: twice, overlap: Rotation speed of the nozzle head: 1500 min ^-1 , moving speed of the nozzle head: 3000 mm / min). At this time, the nozzle head and the used target material were arranged so that the center axis of the nozzle head and the used surface of the used target material were vertical, and the nozzle head was scanned in the direction of the long side of the used target material The nozzle faces the oblique direction with respect to the abutment surface, and the water abuts the abutment surface obliquely). The bonding material and the metallized layer were removed from the surface of the target material after the cleaning, and it was formed into an easy shape. The retroreflectivity at the wavelength of 300-1,500 nm of the joint surface in the form of an ejaculate was measured with an ultraviolet visible near infrared spectrophotometer (Hitachi High Technologies, U-4100 type). The specimen was irradiated with incident light at an incident angle of 5 ° using a 5 ° specular reflection attachment and the reflectance of the reflected light reflected at a reflection angle of 5 ° with respect to the incident light was obtained in terms of the wavelength of the incident light in 100 nm units. The maximum was 0.4% when the wavelength of the incident light was 1300 nm, 0.3% when the wavelength was 500 nm, and 0.2% when the wavelength was 1000 nm. When the wavelength of the incident light is 1300 nm, the maximum reflectance is about 2 to 3%. When the wavelength is 500 nm, the reflectance is 1 to 2% and the wavelength is 1000 nm It was 1 to 2%. In addition, the arithmetic mean roughness (Ra) was measured using a contact surface roughness meter (Surf Test SJ-301 manufactured by Mitsutoyo Co., Ltd.) in accordance with JIS B 0601 (2001) Three points were measured, and the average value of Ra was 19 占 퐉. In addition, the arithmetic mean roughness (Ra) of the bonding surfaces to which the bonding material was bonded before treatment was 1.7 mu m on average.

Using the EDXRF analyzer (EDX-700L, detection limit: about 0.01 wt% in In) manufactured by Shimadzu Corporation, the bonded surfaces of the used target after cleaning under the following conditions were analyzed (semi-quantitative analysis). As a result, Sn, Zn, In derived from the brazing material, and Cu derived from the backing plate could not be detected at all at the joint surface of the used target after cleaning. At that time, the presence or absence of detection of the X-ray peak was also confirmed with respect to the elements of the components of the bonding material and the backing plate.

When the bonded surfaces of the used target materials before cleaning are analyzed by EDXRF as described above, Sn, Zn, and In derived from the brazing material are 10 wt% or less, 10 wt% or less, 1 wt% And Cu derived from the backing plate is present in an amount of 1 wt% to 50 wt%. By using the cleaning method of the present invention, after the used target material after cleaning, impurities derived from the solder material and the backing plate It was found that it does not substantially contain the contained elements.

<Analysis condition>

X-ray irradiation diameter: 10 mm?

Excitation voltage: 10 kV (Na ~ Sc), 50 kV (Ti ~ U)

Current: 100 ㎂

Measurement time: 200 sec (100 sec measurement at each excitation voltage)

Atmosphere: He

Duct: Rh target

Filter: None

Measurement method: Fundamental parameter method

Detector: Si (Li) semiconductor detector

The used target material after washing was dissolved in a vacuum state (about 0.03 Torr) at 850 캜, stirred in the air to remove dross, and then cooled in the atmosphere to produce recycled ingots.

The amount of impurities contained in the recycled ingot was analyzed using a GDMS (VG Elemental, VG9000) for trace amounts of Sn, Zn, In and Cu. The results of the analysis of the ingot produced by the same method from the used target material (before washing) and the unused target material (before bonding) are shown in Table 1 below.

Example 2

The target material was separated from the backing plate by heating (280 DEG C) the bonding layer of the used sputtering target.

The sputtering target was a plate-like target material (purity: 99.99%, Vickers hardness: 90, dimension: 2000 mm x 200 mm x 15 mm) made of oxygen-oxygen copper and a backing plate made of oxygen- (Solder material of Sn-Zn-In is used for metallization of the target material) with a solder material (thickness of solder layer: 350 mu m) of In.

Further, the solder material attached to the bonded surfaces of the separated target materials was scraped with a spatula made of silicon, and the solder material was recovered as much as possible. After separating from the backing plate, the target material was cut to a size of about 300 mm x 200 mm x 15 mm.

A circular circular nozzle head (model number: MNH-2506CH manufactured by Sugino Machine Co., Ltd.) equipped with six nozzles of a nozzle diameter of 0.30 mm (manufactured by Sugino Machine Co., model number: DN-0830) (Water pressure: 245 MPa, water: 13.7 L / min, distance between the target material and the nozzle head: 25 mm, injection: 3 times, overlap: 5 mm The rotation speed of the nozzle head is 1500 min ^-1 , and the moving speed of the nozzle head is 100 mm / min). At this time, the nozzle head and the used target material were arranged so that the central axis of the nozzle head and the joining surface were vertical, and the nozzle head was scanned in the direction of the long side of the used target material Since the surface has a convex mountain-like structure in the downward direction, the nozzle faces the oblique direction with respect to the abutting surface, and the water is obliquely fitted to the abutting surface. The bonding material and the metallized layer were removed from the surface of the target material after the cleaning, and it was formed into an easy shape. When the wavelength of the incident light was 0.5% at a wavelength of 1300 nm and 0.1% at a wavelength of 500 nm, the maximum reflectance at a wavelength of 300 nm to 1500 nm was measured under the same conditions as in Example 1, When it was 1000 nm, it was 0.3%. When the wavelength of the incident light is 1300 nm, the maximum reflectance is about 2 to 3%, and when the wavelength is 500 nm, the reflectance of the bonded surface having the bonded body before treatment is 1 to 2% And when the wavelength was 1000 nm, it was 1 to 2%. The arithmetic mean roughness (Ra) was measured in the same manner as in Example 1, and the average value of Ra was 17 占 퐉. In addition, the arithmetic mean roughness (Ra) of the bonding surfaces to which the bonded bodies were bonded before treatment was 2.1 mu m on average.

Using the EDXRF analyzer (EDX-700L) manufactured by Shimadzu Corporation, the bonded surfaces of the used target after cleaning were analyzed under the same conditions as in Example 1. [ As a result, no Sn, Zn, or In derived from the solder material could be detected on the joint surface of the used target after cleaning.

When the bonded surfaces of the used target materials before cleaning are analyzed by EDXRF as described above, Sn, Zn, and In derived from the brazing material are respectively 1 wt% to 20 wt%, 1 wt% to 20 wt%, and 2 wt% By weight to 60% by weight.

The used target after cleaning was dissolved in a vacuum state (about 0.03 Torr) at 1200 占 폚, stirred in air to remove dross, and then cooled in the atmosphere to produce recycled ingots.

The amount of impurities contained in the recycled ingot was analyzed using a GDMS (VG Elemental, VG9000) for trace amounts of Sn, Zn and In. Table 2 shows the results of the analysis of the ingot produced from the unused target material (before joining) by the same method.

From the results shown in Table 2, it can be seen that the amount of impurities (In, Sn, and Zn derived from the solder material) contained in the recycled ingot produced by using the used target material after cleaning is smaller than that of the unused target material A slight increase is known, but the sum of the increase is about 1.4 ppm (by weight).

Example 3

The target material was separated from the backing plate by heating (280 DEG C) the bonding layer of the used sputtering target.

The sputtering target was prepared in the same manner as in Example 1 except that a flat plate type target material (purity: 99.999%, Vickers hardness: 15-17, dimensions: 2000 mm x 200 mm x 15 mm) made of aluminum and a backing plate made of oxygen- : 99.99%, dimension: 2300 mm x 250 mm x 15 mm) with the following brazing material (solder layer thickness: 350 m).

Further, the solder material attached to the bonded surfaces of the separated target materials was scraped with a spatula made of silicon, and the solder material was recovered as much as possible. After separating from the backing plate, the target material was cut to a size of about 300 mm x 200 mm x 15 mm.

The bonded surfaces of the target materials were cleaned under the following conditions 1 to 10. Under both conditions, the bonding material and the metallized layer were removed from the surface of the target material after cleaning, and the result was an easy-to-shape. Using the EDXRF analyzer (EDX-700L, detection limit: about 0.01 wt% in In) manufactured by Shimadzu Corporation, the target material after washing was subjected to the same conditions as in Example 1 to measure the contact surface of the used target after cleaning I analyzed it. As a result, none of In, Sn, Zn derived from the brazing material, and Cu derived from the backing plate could be detected on the joint surface of the used target after cleaning. Particularly, the target material after being cleaned obtained under the following conditions 1 to 8 is dissolved in a vacuum state (for example, 0.03 Torr) at 850 ° C and stirred in the atmosphere to remove the dross , And then cooled in the atmosphere to produce a recycled ingot.

The amount of impurities contained in the ingot produced from the unused target material (before joining), the recycled ingot, and the used target material (before washing) in the same manner was measured using GDMS (VG Elemental Co., VG9000) did. The results are shown in Tables 3 and 4 below.

Condition 1

Solder material for bonding: In

Metallization Solder material: Sn-Zn-In

Water pressure: 200MPa

Quantity: 8.5L / min

Number of nozzles: 6 (nozzle head is manufactured by Sugino Machine Co., Ltd., type number: MNH-2506CH)

Nozzle diameter: 0.25 mm (manufactured by Sugino Machine Co., Ltd., model number: DN-0825)

Nozzle distance: 25mm

Rotation speed: 1500 min ^-1

Moving speed: 1000mm / min

Line processing: 1 time

Overlap: 5mm

Cleaning process:

Condition 2

Solder material for bonding: In

Metallization Solder material: Sn-Zn-In

Water pressure: 200MPa

Quantity: 8.5L / min

Number of nozzles: 6 (nozzle head is manufactured by Sugino Machine Co., Ltd., type number: MNH-2506CH)

Nozzle diameter: 0.25 mm (manufactured by Sugino Machine Co., Ltd., model number: DN-0825)

Nozzle distance: 25mm

Rotation speed: 1500 min ^-1

Moving speed: 1000mm / min

Line processing: 1 time

Overlap: 22mm

Cleaning process: bonding surface and sputtering surface

Condition 3

Solder material for bonding: In

Metallization Solder material: Sn-Zn-In

Water pressure: 200MPa

Quantity: 8.5L / min

Number of nozzles: 6 nozzle heads, manufactured by Sugino Machine Co., Ltd., type number: MNH-2506CH)

Nozzle diameter: 0.30 mm (manufactured by Sugino Machine Co., Ltd., model number: DN-0830)

Nozzle distance: 25mm

Rotation speed: 1500 min ^-1

Moving speed: 1000mm / min

Line processing: 1 time

Overlap: 22mm

Cleaning process: bonding surface and sputtering surface

Condition 4

Solder material for bonding: In

Metallization Solder material: Sn-Zn-In

Water pressure: 200MPa

Quantity: 8.5L / min

Number of nozzles: 6 (nozzle head is manufactured by Sugino Machine Co., Ltd., type number: MNH-2506CH)

Nozzle diameter: 0.25 mm (manufactured by Sugino Machine Co., Ltd., model number: DN-0825)

Nozzle distance: 25mm

Rotation speed: 1500 min ^-1

Moving speed: 2000 mm / min

Line processing: 2 times

Overlap: 22mm

Cleaning process: bonding surface and sputtering surface

Condition 5

Solder material for bonding: In

Metallization Solder material: Sn-Zn-In

Water pressure: 200MPa

Quantity: 8.5L / min

Number of nozzles: 6 (nozzle head is manufactured by Sugino Machine Co., Ltd., type number: MNH-2506CH)

Nozzle diameter: 0.25 mm (manufactured by Sugino Machine Co., Ltd., model number: DN-0825)

Nozzle distance: 25mm

Rotation speed: 1500 min ^-1

Moving speed: 2000 mm / min

Line processing: 2 times

Overlap: 5mm

Cleaning process: bonding surface and sputtering surface

Condition 6

Solder material for bonding: Sn-Zn

Metallization Solder material: Sn-Zn-In

Water pressure: 200MPa

Quantity: 8.5L / min

Number of nozzles: 6 (nozzle head is manufactured by Sugino Machine Co., Ltd., type number: MNH-2506CH)

Nozzle diameter: 0.25 mm (manufactured by Sugino Machine Co., Ltd., model number: DN-0825)

Nozzle distance: 25mm

Rotation speed: 1500 min ^-1

Moving speed: 1000mm / min

Line processing: 2 times

Overlap: 5mm

Cleaning process: bonding surface and sputtering surface

Condition 7

Solder material for bonding: In

Metallization Solder material: Sn-Zn-In

Water pressure: 245MPa

Quantity: 11.6L / min

Number of nozzles: 6 (nozzle head is manufactured by Sugino Machine Co., Ltd., type number: MNH-2506CH)

Nozzle diameter: 0.25 mm, 0.30 mm (each of three nozzles manufactured by Sugino Machine Co., Ltd., model number: DN-0825, DN-0830, 0.30 mm nozzle at three outer sides of the nozzle head, 0.25 mm at three inner sides Nozzle)

Nozzle distance: 55mm

Rotation speed: 1500 min ^-1

Moving speed: 4000mm / min

Line processing: 2 times

Overlap: 5mm

Cleaning process: bonding surface and sputtering surface

Condition 8

Solder material for bonding: Sn-Zn

Metallization Solder material: Sn-Zn-In

Water pressure: 245MPa

Quantity: 11.6L / min

Number of nozzles: 6 (nozzle head is manufactured by Sugino Machine Co., Ltd., type number: MNH-2506CH)

Nozzle diameter: 0.25 mm, 0.30 mm (each of three nozzles manufactured by Sugino Machine Co., Ltd., model number: DN-0825, DN-0830, 0.30 mm nozzle at three outer sides of the nozzle head, 0.25 mm at three inner sides Nozzle)

Nozzle distance: 55mm

Rotation speed: 1500 min ^-1

Moving speed: 3000mm / min

Line processing: 2 times

Overlap: 5mm

Cleaning process: bonding surface and sputtering surface

Condition 9

Solder material for bonding: In

Metallization Solder material: Sn-Zn-In

Water pressure: 150MPa

Quantity: 7.3L / min

Number of nozzles: 3 (Nozzle head is placed on a machine made by Sugino Machine Co., Ltd., pitch circle diameter (P.C.D.) 20 mm, water is sprayed in the vertical direction)

Nozzle diameter: 0.35 mm (manufactured by Sugino Machine Co., Ltd., model number: DN-0835)

Nozzle distance: 25mm

Rotation speed: 1000 min ^-1

Moving speed: 1000mm / min

Line processing: 1 time

Overlap: 5mm

Cleaning process:

Condition 10

Solder material for bonding: In

Metallization Solder material: Sn-Zn-In

Water pressure: 245MPa

Quantity: 3.4L / min

Number of nozzles: 6 (nozzle head is manufactured by Sugino Machine Co., Ltd., type number: MNH-2506CH)

Nozzle diameter: 0.15 mm (manufactured by Sugino Machine Co., Ltd., model number: DN-0815)

Nozzle distance: 25mm

Rotation speed: 1500 min ^-1

Moving speed: 1000mm / min

Line processing: 1 time

Overlap: 5mm

Cleaning process:

Comparative Example 1

The used flat plate type target material as in Example 1 was cut to a size of about 100 mm x 200 mm x 15 mm and immersed in a nitric acid aqueous solution of 4.4 wt% at room temperature for 20 hours to remove the solder material by chemical treatment. When the wavelength of the incident light was 1300 nm, the maximum reflectance was 13%. When the wavelength was 500 nm, the reflectance was 6.0% and the wavelength was 1000 nm. , It was 8.0%. Further, the arithmetic average roughness (Ra) was measured in the same manner as in Example 1, and the average value of Ra was 1.1 탆. When the wavelength of the incident light is 1300 nm, the maximum reflectance is about 2 to 3%, and when the wavelength is 500 nm, the reflectance is 1 to 2% at a wavelength of incident light of 300 to 1500 nm, And when the wavelength was 1000 nm, it was 1 to 2%, and the arithmetic mean roughness (Ra) of the bonding surfaces before the treatment was 1.7 탆 on average. Using the EDXRF analyzer (EDX-700L, detection limit: about 0.01 wt% in In) manufactured by Shimadzu Corporation, the bonded surfaces of the used targets after the chemical treatment were analyzed under the same conditions as in Example 1. As a result, it was found that Cu derived from the backing plate was detected at 0.6 wt% on the joint surface of the used target material after the chemical treatment, and the impurities were not removed.

Further, after the chemical treatment, the used target material was dissolved in a vacuum state (about 0.03 Torr) at 850 캜, stirred in the air to remove dross, and then cooled in the air to produce recycled ingots.

The amount of the impurities contained in the ingot produced by dissolving the unused target material (before joining), the recycled ingot of Comparative Example 1, and the used target material (before chemical treatment) was measured by GDMS (VG 9000 manufactured by VG Elemental Co., Ltd.) . The results are shown in Table 5 below.

The total amount of the impurities (i.e., In, Sn, Zn, Cu) derived from the bonding material contained in the recycled ingot and the backing plate, on the basis of weight, A recycled ingot having substantially the same composition as that of the original target material could not be obtained at about 19 ppm.

Example 4

The target material was separated from the backing plate by heating (280 DEG C) the bonding layer of the used sputtering target.

The sputtering target was made of an aluminum plate-shaped target material (purity: 99.999%, Vickers hardness: 14 to 17, dimensions: 2000 mm x 200 mm x 15 mm) and a backing plate made of oxygen- : 2300 mm x 250 mm x 15 mm) with the following brazing material (solder layer thickness: 350 m).

Further, the solder material attached to the bonded surfaces of the separated target materials was scraped with a spatula made of silicon, and the solder material was recovered as much as possible. After the target material was separated from the backing plate, the target material was cut to a size of about 300 mm x 200 mm x 15 mm.

The joining surface, sputtering surface and side surface of the 55 target materials were cleaned under the following condition 11. In either case, the bonding material and the metallized layer were removed from the surface of the target material after cleaning, and the result was an easy shape. 10 out of 55 cleaned sheets were randomly selected to measure the reflectance of the joint surface in the form of an ejaculate in the entire wavelength range of 300 to 1500 nm under the same conditions as in Example 1. [ In any of the target materials, the specular reflectance was about 0.4% at the maximum, and an average of about 0.2% when the wavelength was 500 nm and an average of 0.2% when the wavelength was 1000 nm. The arithmetic average roughness (Ra) of 10 randomly selected samples was measured in the same manner as in Example 1, and the average value of Ra was 20 占 퐉. When the wavelength of the incident light is 1300 nm, the maximum reflectance is about 2 to 3%, and when the wavelength is 500 nm, the reflectance of the bonded surface having the bonded body before treatment is 1 to 2% And when the wavelength was 1000 nm, it was 1 to 2%, and the arithmetic average roughness (Ra) of the bonding surfaces before the treatment was 1.8 탆 on average. Using the EDXRF analyzer (EDX-700L, detection limit: about 0.01 wt% in In) manufactured by Shimazu Seisakusho, the target material after washing was subjected to the same conditions as in Example 1, Cotton. As a result, none of In, Sn, Zn derived from the brazing material, and Cu derived from the backing plate could be detected on the joint surface of the used target after cleaning. The yield was calculated from the weight difference between the 55 target materials before and after cleaning, and the average yield was 98%.

Subsequently, 25 pieces (about 50 kg) of the treated target cleaned material were dissolved in a vacuum at 800 ° C to remove the dross, and then a molten metal was poured into a mold made of carbon in the atmosphere, And then cooled in the atmosphere to produce a recycled ingot. The amount of the impurities contained in the recycled ingot was measured using GDMS (VG 9000, VG9000 (model number)). The results are shown in Table 4.

Condition 11

Solder material for bonding: In

Metallization Solder material: Sn-Zn-In

Water pressure: 245MPa

Quantity: 18.6L / min

Number of nozzles: 6 (nozzle head is manufactured by Sugino Machine Co., Ltd., type number: MNH-2506-15C (nozzles are disposed at a position of P.C.D. 36 mm))

Nozzle diameter: 0.35 mm (manufactured by Sugino Machine Co., Ltd., model number: DN-0835)

Nozzle distance: 60mm

Rotation speed: 2000 min ^-1

Moving speed: 4000mm / min

Line processing: 2 times

Overlap: 5mm

Cleaning process: bonding surface, sputtering surface and side surface

According to the present invention, for example, by using the apparatus described above, the used target material is cleaned as described above, whereby the used target material substantially not containing the elements derived from the bonding material and the supporting member Can be obtained. By producing the ingot using the used target material as a raw material, a recycled ingot having substantially the same composition as that of the original target material can be obtained. According to the present invention, a target material having substantially the same composition as the original target material can be regenerated from such recycled ingot, which is useful for recycling the target material.

1 target material
2 supporting member
3 bonding material (or bonding layer)
4 solder layer
5, 5 'metallization layer
10, 20, 30 Sputtering target
100 device
101 target material (or workpiece)
102 nozzle head
103 Actuator
103X X axis slider
103Y Y-axis slider
103Z Z-axis slider
104 treatment room
105 conveying means
106 load

Claims (13)

A step of separating the target material from a target material mainly composed of metal and a sputtering target in which a support member is joined with a bonding material; and a step of spraying water on the surface of the target material on which the bonding material is adhered, And removing the bonding material from the ash. The method according to claim 1,
Wherein the pressure of the water is 90 MPa or more. 3. The method according to claim 1 or 2,
Wherein the metal is aluminum or copper. A method for producing a target material comprising the step of carrying out the cleaning method according to any one of claims 1 to 3. A target member separated from a sputtering target in which a support member is joined with a bonding material,
And the elements derived from the bonding material and the support member are not detected by energy dispersive X-ray fluorescence analysis. A method for producing a recycled ingot comprising the step of casting a target material subjected to the cleaning method according to any one of claims 1 to 3 to obtain a recycled ingot containing the metal. A reclaim ingot derived from a target material mainly composed of metal and a target material of a sputtering target having a support member joined with a bonding material,
Wherein the total amount of the elements derived from the bonding material and the supporting member is less than 10 ppm by weight. 8. The method of claim 7,
A recycled ingot in which the metal as the main component of the recycled ingot is aluminum or copper. 8. The method of claim 7,
Wherein the metal as a main component of the recycled ingot is aluminum and the total amount of the elements is less than 5 ppm by weight. The bonding material is removed from the target material by spraying water on a surface of the target material on which the bonding material is adhered, the target material being mainly composed of metal and the target material separated from the sputtering target in which the supporting member is joined with the bonding material &Lt; / RTI &gt;
At least one nozzle head having at least one jetting port for jetting water to the target material,
An actuator for operating the nozzle head,
And a processing chamber in which the actuator is disposed and for receiving and processing the target material. 11. The method of claim 10,
And a clamp for fixing the target material in the treatment chamber. The method according to claim 10 or 11,
And a reversing mechanism for reversing the target material. 13. The method according to any one of claims 10 to 12,
And a drain mechanism for collecting and discharging the water jetted from the jetting port and separating the processed material including the bonding material removed from the target material.

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