CN101740183A - Ceramics member with embedded electric conductor and manufacturing method thereof - Google Patents
Ceramics member with embedded electric conductor and manufacturing method thereof Download PDFInfo
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- CN101740183A CN101740183A CN200910179080A CN200910179080A CN101740183A CN 101740183 A CN101740183 A CN 101740183A CN 200910179080 A CN200910179080 A CN 200910179080A CN 200910179080 A CN200910179080 A CN 200910179080A CN 101740183 A CN101740183 A CN 101740183A
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/22—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
- H05B3/28—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material
- H05B3/283—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material the insulating material being an inorganic material, e.g. ceramic
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/683—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping
- H01L21/687—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using mechanical means, e.g. chucks, clamps or pinches
- H01L21/68714—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using mechanical means, e.g. chucks, clamps or pinches the wafers being placed on a susceptor, stage or support
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/02—Details
- H05B3/03—Electrodes
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/02—Details
- H05B3/06—Heater elements structurally combined with coupling elements or holders
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/017—Manufacturing methods or apparatus for heaters
Abstract
The invention provides a ceramics base material with an embedded electric conductor. In the previous ceramics base made of ceramics base materials with a refractory metal electrode layer, a joint part of the embedded electrode layer and a Ni electrode rod is easy to be broken and damaged and the like, and the broken or damaged joint part can not be restored, thus the expensive base is rejected. According to the inventive ceramics base material, A Si alloy layer containing B is used for filling the gaps among the exposing surface of the joint part of electrode terminals of the refractory metal conductor in the ceramics base material and the electrode terminals and the ceramics base material, thus the structure has the oxidation resistance and air tightness, and the broken or damaged problem is solved. Or a Si alloy layer containing more than 2% of Mn is used. In addition, a carburizing processing layer or boronising processing layer is formed on the exposing surface of the conductor, the Si alloy layer is used for filling the gaps among the exposing surface of the electrode terminals and the electrode terminals and the ceramics base material.
Description
Technical field
The present invention relates to a kind of built-in in the nitride ceramics base material be the ceramic component and the manufacture method thereof of the electric conductors that refractory metal constituted such as metal by Mo, W.
In the present invention, " electric conductor " is meant refractory metal heater and electrode class and its peripheral metalwork classes such as Mo, W that flows through electric current or be used for applying voltage.For example, in ceramic base material, be meant the refractory metal heater of the ceramic heater of built-in refractory metal heater itself, engage with this heater and same by the metalwork class that refractory metal constituted, the electrostatic chuck electrode and the RF electrode of refractory metal, or the electrode class identical with the application target of these members.
So-called refractory metal heater is meant the linear heating element of using refractory metal itself to make, or refractory metal powder cream is printed the sintering heater that burns till and make.In addition, so-called refractory metal electrode is meant the electrode film that uses refractory metal itself, or the refractory metal line is processed into the electrode of mesh-like, or refractory metal powder cream is printed the sintered electrode class of burning till and making etc.
In the present invention, the heater of these refractory metals, electrode class, with and the metalwork class of refractory metal of periphery, all be called " being built in the electric conductor in the ceramic base material ".
Electric conductor of the present invention is a built-in in advance electric conductor in the ceramic base material that does not burn till, and when ceramic base material is burnt till, is built in by the while sintering in the ceramic base material of sintering.
" refractory metal " of the present invention even if be meant under ceramic firing temperature, for example is to carry out sintering under 1700～1900 ℃ in the AlN pottery, can fusion, rotten all refractory metals yet, and for example Mo, W etc. are representative metals wherein.
In the present invention, be built-in with heater heater, electrostatic chuck electrode, RF electrode, and the base of ceramic class and the identical member of application target of other refractory metal electrode class etc., all be called " ceramic component of built-in electric conductor ".
Background technology
Semiconductor substrates such as silicon wafer can carry out processing such as etching, film forming usually by mounting on the treatment bench that is called pedestal.
In recent years, develop a kind of ceramic pedestal that in the aluminium nitride base material, is built-in with heater heater, electrostatic chuck electrode, RF electrode etc., and be extensive use of.
These heater heaters, electrostatic chuck electrode, RF electrode etc. when burning till substrate ceramic, together by built-in, burnt till simultaneously to one and are made.
Because firing temperature reaches the high temperature near 2,000 degree, so refractory metals such as use Mo, W such as heater heater, electrostatic chuck electrode, RF electrodes.For example, shown in the disclosure of patent documentation 1 (spy opens the 2003-272805 communique), patent documentation 2 (spy opens the 2003-288975 communique), patent documentation 3 (spy opens the 2000-286038 communique), in the pedestal of built-in ceramic heater, the linear heating element of using Mo, W, Mo-W alloy is as heater wire, these heater wires are connected with the intermetallic metal spare that is made of materials such as Mo, W, Mo-W alloys equally by mechanical mechanisms such as ca(u)lk portions, with ceramic base material one sintering, be built in the ceramic base material.The resulting metal level of powder paste that maybe will print, burn till W, Mo etc. is as heater, and these metal levels and base material are sintered into one, and are built in the ceramic base material.
In the pedestal of built-in RF electrode, with mesh-like electrode that materials such as Mo, W, Mo-W alloy constituted or the metal level that the powder paste of W, Mo etc. is printed, burnt till and obtains is used as electrode uses, these members are embedded in the ceramic base material, by integral sintering, and be built in the ceramic base material.
Substrate ceramic mainly uses aluminium nitride, silicon nitride.
With regard to intermetallic metal spare, in patent documentation 1 (spy opens the 2003-272805 communique), be illustrated as spherical, ellipsoid of revolution, columned combination member, in patent documentation 2 (spy opens the 2003-288975 communique), be illustrated as cylindric terminal.
On intermetallic metal spare, electrode layer and mesh-like electrode that the powder paste of W, Mo etc. is printed, burnt till and makes, soldering has long Ni electrode bar.
About these solderings the pedestal of the structure in the past of long Ni electrode bar is arranged, have following problem points.
That is, as shown in Figure 8, in structure in the past, the recess bottom being formed on the ceramic base material 2 exposes the intermetallic metal spare 4 that engages with linear heating element 3, or the RF electrode 9 of mesh-like, or with printing, the made electrode layer (not shown) of firing mode.
Ni electrode bar 14 inserts the recess of ceramic base materials, and is brazed in this intermetallic metal spare, RF electrode or exposing on the face with the made electrode layer of printing, firing mode.
When soldering, also the Ni electrode bar being brazed in the encirclement electrode layer exposes on the ceramic base face of face, there is not the space if can allow between Ni electrode bar and the ceramic base material, just fully the enclosed electrode layer expose face and make it and outside atmosphere isolated, what can prevent electrode layer exposes face generation high-temperature oxydation.In addition, in processing procedure, even the Ni rod is subjected to the effect of transverse curvature external force, because the root cadre firmly is brazed on the ceramic base material, so can prevent junction surface with electrode layer is affected and unfavorable conditions such as deterioration, fracture takes place, but the explanation of following reason is surrounding on the ceramic base face that electrode layer exposes face with the soldering of Ni electrode bar what difficulty is arranged.
The coefficient of linear expansion of Ni is 13 * 10
-6If the ceramic base material aluminium nitride then is 4.5 * 10
-6If silicon nitride then is 3.5 * 10
-6, the coefficient of linear expansion of Ni and ceramic base material is widely different, and Ni is the hard material that possesses rigidity, so the thermal stress that takes place at the junction surface because of the difference of coefficient of linear expansion is not relaxed.Thermal stress can be destroyed the junction surface of ceramic base material.
The scolder of high-temperature use must use high melting point solder, the high melting point solder of Shi Yonging in the past, and coefficient of linear expansion is all very big, and all is hard material, and scolder itself can become the generation source of thermal stress.Solder layer can't absorb thermal stress.
Reason as previously discussed, using high-temperature solder soldering Ni rod and ceramic base material is difficulty very.
Reason as previously discussed, in structure in the past with ceramic base material and Ni electrode bar securely airtight joint be very difficult, so adopt the structure that the Ni rod is mechanically screwed in ceramic base material, saying so is not more in order to reduce the effort of doing in the gap.Promptly as shown in Figure 8, on the recess side of ceramic base material 2, form screw thread, in this screwed hole, insert metal tube 13.The hole portion that Ni rod 14 inserts this metal tube inner face allows side and metal tube soldering fix.The front end end face that become the Ni rod this moment also with the structure of intermetallic metal spare 4,9 solderings simultaneously of mesh-like RF electrode.
Because the coefficient of linear expansion of metal tube self is bigger than ceramic base material, rigidity is also bigger, so if very close to each other between ceramic base material and the metal tube, then differential expansion can destroy ceramic base material, therefore allow the gap of leaving the differential expansion degree between ceramic base material and the metal tube be the present situation of present technology.
Therefore, repeat heat and can cause the oxidation of metal tube, and then cause intermetallic metal spare, the linear heating element that combines with intermetallic metal spare, mesh-like electrode, or print the oxidation of burning till electrode layer etc.Refractory metal such as Mo, W is very fragile to oxidation, can consume because of oxidation.And repeat to heat the gap enlargement that also can make between metal tube and the ceramic base material.
The intermetallic metal spare, the mesh-like RF electrode that engage with the bottom end face of Ni electrode bar, or with printing, burn till made electrode layer, all can with ceramic base material simultaneously during sintering, be heated to embrittlement, so original intensity is just not enough near the high temperature of 2,000 degree.
Because between Ni rod and ceramic base material, leave the space, so if the Ni rod is subjected to the effect of crooked power, the effect that electrode interior also can directly be subjected to crooked power is burnt till in soldering part and intermetallic metal spare, the printing of mesh-like electrode.
The overlap action of the above reason, intermetallic metal spare, mesh-like electrode, printing are burnt till in the electrode layer and are ruptured easily.In addition, the Ni rod partly also ruptures because of deterioration easily with the soldering that electrode layer is burnt till in intermetallic metal spare, mesh-like electrode, printing.The problem that intermetallic metal spare, linear heating element, mesh-like electrode consume because of oxidation perhaps also can take place, and causes then and can't use.
If because of such fracture or oxidation consumption can't use, pedestal just can't be repaired, even expensive pedestal also have to abandon need not, this is the common occurrence feelings.
Summary of the invention
The invention that the present invention finishes in view of relevant issues just, its first purpose is, provides a kind of and can prevent that in the ceramic component that is built-in with the electric conductor that is made of refractory metal this electric conductor from exposing the new-type structure and the manufacture method thereof of the high-temperature oxydation of face.In addition, second purpose is, providing a kind of does not have the space between electrode terminal section that is engaged in electric conductor and ceramic base material, can prevent the new-type structure and the manufacture method thereof of electric conductor and electrode terminal junction surface and oxidation, strength deterioration and fracture around it.
Can solve in order to method down about the problems referred to above of the ceramic component that is built-in with electric conductor.
Solve the mode of high-temperature oxydation problem
In being built-in with the ceramic component of electric conductor, expose on the face fusion Si alloy-layer and it is covered at electric conductor, expose the high-temperature oxydation of face to prevent electric conductor.
The Si alloy possesses excellent thermal endurance and oxidative resistance, making its coefficient of linear expansion and refractory metal coupling is easily, though can possess the coverlay of thermal endurance and oxidative resistance in the electric conductor surface coverage of refractory metal, but when fusing the fused mass of Si alloy on the refractory metal surface, fierce corrosion (erosion) can take place on the refractory metal surface.Corrosion is the conversion zone (alloy-layer) of Si and refractory metal.
At the position that is etched, can too much produce the coefficient of linear expansion silicide bigger and very crisp than the refractory metal of base material, if repeat heat, can chap, perhaps the problem peeled off from base material of the position that can be etched.
The present invention forms the coverlay of oxidative resistance, anti-fissility, crack resistance excellence by making the coverlay fusion that can not suffer erosion or corrode the repressed Si alloy of energy on the electric conductor surface of refractory metal.
In the present invention, when deposited covering Si alloy on the surface of refractory metal electric conductor, the 1st mode about " erosion " that be used for preventing that Si alloy molten thing from causing, contain B as Si alloy that should deposited covering, on refractory metal electric conductor and the Si alloy interface that is used for covering, to form the enriched layer of B or the compound layer of B.
When the Si alloy that will contain B deposited on refractory metal electric conductors such as Mo, W the time, if have the enriched layer of B or the boride layer of refractory metals such as Mo, W on electric conductor and Si alloy interface, the Si alloy of fusion obviously reduces " erosion " situation that member caused.Perhaps do not corrode fully.
In addition, no matter be nitride ceramics, oxide ceramics, or other pottery, no matter be any kind, as long as the Si alloy is through the composition adjustment, just can make its coefficient of linear expansion and substrate ceramic coupling, utilize this advantage, just can prevent peeling off, chapping of Si alloy fused layers that the difference because of coefficient of linear expansion causes.
The existence of the boride layer of the enriched layer of this B or the Mo of member or W is to exist when Si alloy middle of fusion added the B more than 0.1%.Promptly, using the B in Si alloy as follows, added 0.1% or more alloy the time have an above-mentioned layer, the element of one or two or more kinds that described Si alloy is selected by Si and in the middle of the element set of Fe, Ni, Co, Cr, Mo, W, Re, Cu, Mn, precious metal, Ti, Zr, Hf, V, Nb, Ta, Ge, Al, Ca, Mg, rare earth element, P constitutes.
Adding B in the Si alloy can reduce electric conductor and be subjected to " erosion ", think this be because, B among the Si alloy becomes branch preferentially to be diffused on the refractory metal electric conductor, and conducting electricity the concentrated diffusion layer of interface, side generation B, it can constrain the erosion process of base material, and suppresses the generation of silicide.Confirmed in the concentrated diffusion layer of B, to form the boride of refractory metals such as Mo, W, and thought that boride can become the barrier layer, prevented corrosion function.
Because the B addition is in the generation that just can begin to suppress silicide more than 0.1%, thus in the Si alloy addition of B preferably more than 0.1%.Further preferably more than 0.3%.The most further, so just can not corrode more than 0.8%.Though the upper limit to the B amount is not particularly limited, if surpass 15%, the powder manufacturing cost of the Si alloy that uses as the powder paste raw material when fusion can uprise, and is not preferred economically.
In the 1st settling mode of the present invention, the Si alloy is following composition range probably.Need to prove, be not limited to following ranges certainly.
The composition of the 1st mode
By main component Si, one or two or more kinds the element, one or two or more kinds element, the element of C group and the alloy of from the B group, selecting that residual impurity becomes branch to constitute from A group, selected.
The element of A group: Fe, Ni, Co, Zr, Ti, Cr, Mo, W
The element of B group: Hf, Nb, Ta, V, Mn, Cu, Al, Ge
The element of C group: B
The composition range of A group element: 3～65 weight %
The composition range of B group element: 0～20 weight %
The composition range of C group element: 0.1～15 weight %
The composition of the 2nd mode
In addition, about the 2nd mode of the present invention,, use the Si alloy that contains the above Mn of 2 weight % at least as the Si alloy.That is,, just can significantly suppress the erosion that Si alloy molten thing is caused the refractory metal electric conductor by using the Si alloy that contains the Mn more than the 2 weight % at least.
Its optimum range is 2～15 weight %.
If do not reach lower limit then can not take place deposited, if surpass the upper limit then erosion condition can become serious.
In the 2nd settling mode of the present invention, the Si alloy is following composition range probably.Need to prove, be not limited to following ranges certainly.
The alloy that becomes branch to constitute by main component Si, one or two or more kinds element, Mn and the residual impurity from A group, selected.
The element of A group:
Fe、Ni、Co、Ti、Zr、Hf、Cr、Mo、W、Nb、Ta、V、Cu、Al、Ge
The composition range of A group element: 3～65 weight %
Mn:2～15 weight %
About Si alloy that contains B and the Si alloy that contains Mn, the composition blending will be carried out in advance so that the powder paste of these alloys of coefficient of linear expansion and ceramic base material coupling, be coated on surface, electrode terminal surface or the ceramic base face of refractory metal electric conductor, be placed on heating under vacuum or the inert atmosphere again, be heated to more than the solidus temperature of alloy, can make its fusion thus.
In addition, the 3rd mode is to form one deck at least of selecting from carburized layer, boride layer in advance on the high-melting-point electric conductor surface of Mo, W etc.Promptly form the individual processing layer of carburizing, boronising, also form the Combined Processing layer of carburizing boronising, nicarbing, boronising nitrogenize, carburizing boronising nitrogenize.Preferred especially carburized layer, boride layer, carburizing boride layer, as the composition of Si alloy, with the above-mentioned Si alloy that contains the B 0.1% or more, reach when containing the Si alloy combination of the Mn more than the 2 weight % at least, can bring into play preventing the effect that corrodes.With regard to Carburization Treatment, can directly use normally used pack carburizing, liquid carburizing, gas carburizing, gas carburizing nitridation treatment method.With regard to boronising is handled, normally used processing methods such as directly applying solid boronising, electrolytic boriding, molten bath boronising, gas boriding.
For from outside supply capability, must expose bonding electrodes terminal on the face at electric conductor.
Joint about electrode terminal, can use and fuse in advance the jointing metal or the different types of jointing metal that expose the Si alloy-layer surface identical type on the face at electric conductor, perhaps fusing the Si alloy-layer that exposes on the face at electric conductor itself is to engage the knitting layer that electric conductor exposes face and electrode terminal.In other words, also can be to have the layer that engages with anti-oxidation function concurrently.
From preventing that electric conductor from exposing the viewpoint of face oxidation, fusion is exposed Si alloy-layer on the face at electric conductor, be not limited in electric conductor and expose face, also cover continuously and surround the ceramic base face that electric conductor exposes face, so that electric conductor exposes in the clearance portion of face and ceramic base material is included in.At this moment, the Si alloy-layer preferably also fuses at the encirclement electric conductor and exposes on the ceramic base face of face.
Eliminate the mode in the gap between electrode terminal and the ceramic base material
When by be built in the electric conductor that refractory metal constituted among the ceramic base material expose among the recess that face is positioned at ceramic component the time, intercalation electrode terminal among this recess, allowing this terminal and electric conductor expose face metallurgy engages, and with the gap between this electrode terminal of Si alloy-layer landfill and the ceramic base material, allow this Si alloy-layer and electrode terminal and ceramic base material the two the fusion, eliminate the gap between electrode terminal and the ceramic base material thus.
At electrode terminal is under the situation of refractory metal, and when fusion Si alloy on electrode terminal and ceramic base material, electrode terminal also above-mentioned erosion problem can take place.
When electrode terminal is refractory metal, in order to prevent Si alloy molten thing the electrode terminal of refractory metal is caused erosion, can use the 1st mode, the 2nd mode, the 3rd mode that prevent above-mentioned erosion.In addition, at this moment, because electrode terminal and electric conductor are refractory metal, so jointing metal can not be the Si alloy.For example can be Co system, Ni system, Au system, other high-melting-point brazing metal.
When electrode terminal was ceramic material, for example ceramic base material was an aluminium nitride, and was under the situation of aluminium nitride at electrode terminal, allowed the two jointing metal that fuses together of ceramic base material and ceramic electrode terminal, just must use the Si alloy.
The structure of electrode terminal
In the present invention, the electrode terminal that engages with electric conductor need not whole be made by same material.For example electrode terminal is embedded into the part and the part of outwards giving prominence to from recess in the ceramic base material recess, need not be same material.
In the present invention, be the material of electrode terminal that is embedded into the part of recess at least, be necessary for and possess fusing point and the coefficient of linear expansion and the ceramic base material matched materials that under the fusion temperature of Si alloy, can not melt.In addition, to expose that face engages by metallurgical modes such as soldering, diffusion bond be necessary condition for electrode terminal and electric conductor.
Terminal material can be the refractory metal with energising member identical type, or with the material that can not be subjected to the ceramic base material identical type that melt of si alloy corrodes, or can not be subjected to the ceramic material that the Si alloy corrodes and the composite material of Si alloy.For example, can be to make the porous body of the ceramic material that can not be subjected to the erosion of Si alloy flood the material that Si alloy molten thing obtains, or can not be subjected to the ceramic material that the Si alloy corrodes and the duplexer of Si alloy, or make the ceramic packing fusion that can not be subjected to the erosion of Si alloy be scattered in the material that obtains among the Si alloy base material, or Si alloy itself.
When ceramic base material was aluminium nitride, terminal material was preferably the refractory metal that fusing points such as Mo, W surpass the Si alloy melting point, or the ceramic material identical with ceramic base material itself, or the close ceramic material of coefficient of linear expansion.In addition, when ceramic base material is the silicon nitride series pottery, can suitably use W, carborundum, silicon nitride itself.
Need to prove that the material of electrode terminal can not be a conductive material.This is because the metal that surrounds the knitting layer of terminal possesses conductivity, so can guarantee conductive path with knitting layer.In addition, from the outwards outstanding part of recess, can be after the landfill recess, use material different or identical materials soldering and engage with the electrode terminal section that is filled into recess.
With of the covering of Si alloy to electrode terminal
When electrode terminal is refractory metal, has the more weak shortcoming of non-oxidizability to the electrode terminal part that exposes outside from recess.At this moment, cover the part of exposing outside, just can improve the oxidative resistance of exposed portions serve with the fusion of Si alloy.At this moment, for the erosion that prevents that the Si alloy from causing, can use the 1st mode, the 2nd mode, the 3rd mode that prevent above-mentioned erosion.
Description of drawings
Fig. 1 is the photo of the characteristic X-ray picture (reflection) of B and Mo.
Fig. 2 is the figure of explanation structure of the present invention.
Fig. 3 is the figure of explanation another structure of the present invention.
Fig. 4 is the figure of explanation another structure of the present invention.
Fig. 5 is the structure chart of the pedestal of the expression electrode terminal section structure in the past that stays recess after extracting.
Fig. 6 be landfill Fig. 5 recess and through the key diagram of the structure of repairing.
Fig. 7 is the key diagram of embodiment.
Fig. 8 is the key diagram of conventional art.
Symbol description: 1-ceramic component, 2-ceramic base material, 3-electric conductor (heater), 4-electric conductor (intermetallic metal spare), 5-electrode terminal, 6-Si alloy molten thing layer, the 7-brazing layer, the coverlay of 8-Si alloy, 9-electric conductor (RF electrode), 10-recess, the 11-composite material, the 12-packing material, 13-metal tube, 14-Ni rod.
Embodiment
Following test example is used to confirm that " erosion " of the present invention prevents the effect of mode.
Make sample
On the plate surface of the Mo of 20 * 40 * thickness 1mm and W, coating 10 * 10 * thickness 1mm and one-tenth are grouped into the powder paste of different Si alloys, in a vacuum heating make its deposited after, cut off overlay, measure the degree of depth that Mo, W plate suffer erosion.
In addition, measure the degree of depth that the Mo surface without the Mo plate of any processing suffers erosion, and the degree of depth that suffers erosion after handling through over carburizing, boronising.
About carburizing, be that to be immersed in the carbon dust be to form carburized layer among the pack carburizing material of main component and 1200 ℃ of heating 3 hours.
About boronising, be to be immersed in the pack boronizing medium (boron powder+boron carbide) and to heat 5 hours to form the boronising coverlay at 1000 ℃.
The result
The measurement result of depth of erosion is shown in table 1.
Table 1
| Numbering | The one-tenth of Si base alloy is grouped into % | The kind of plate | Depth of erosion μ m | Deposited temperature ℃ |
| ??1 | ??Si-25Cr | ??Mo | ??120 | ??1320 |
| ??2 | ??Si-25Cr-0.12B | ??Mo | ??21 | ??1320 |
| ??3 | ??Si-25Cr-0.32B | ??Mo | ??14 | ??1320 |
| ??4 | ??Si-18Cr-5Ni-0.2??0B | ??Mo | ??18 | ??1320 |
| ??5 | ??Si-20Cr-0.65B | ??Mo | ??8 | ??1320 |
| ??6 | ??Si-9Ni | ??Mo | ??150 | ??1300 |
| ??7 | ??Si-9Ni-0.09B | ??Mo | ??32 | ??1300 |
| ??8 | ??Si-9Ni-0.38B | ??Mo | ??12 | ??1300 |
| ??9 | ??Si-21Co | ??Mo | ??98 | ??1280 |
| ??10 | ??Si-21Co-0.39B | ??Mo | ??10 | ??1280 |
| ??11 | ??Si-7Fe | ??Mo | ??139 | ??1300 |
| ??12 | ??Si-7Fe-0.11B | ??Mo | ??29 | ??1300 |
| ??13 | ??Si-40Co-2.9Mn | ??Mo | ??31 | ??1250 |
| ??14 | ??Si-30Co-15Cr-3.??2Mn | ??Mo | ??28 | ??1250 |
| ??15 | ??Si-30Co-3.5Mn-5.??1Cu | ??Mo | ??21 | ??1200 |
| ??16 | ??Si-20Ni-3.0B | ??Mo | Do not have | ??1280 |
| Numbering | The one-tenth of Si base alloy is grouped into % | The kind of plate | Depth of erosion μ m | Deposited temperature ℃ |
| ??17 | ??Si-25Cr-0.12B | Carburizing Mo | Do not have | ??1320 |
| ??18 | ??Si-25Cr-0.12B | Boronising Mo | Do not have | ??1320 |
| ??19 | ??Si-25Cr | Boronising Mo | ??18 | ??1320 |
| ??20 | ??Si-25Cr | Carburizing Mo | ??10 | ??1320 |
| ??21 | ??Si-40Co-2.9Mn | Boronising Mo | Do not have | ??1250 |
| ??22 | ??Si-40Co-2.9Mn | Carburizing Mo | Do not have | ??1250 |
| ??23 | ??Si-20Cr-0.65B | ??W | Do not have | ??1320 |
| ??24 | ??Si-10％Ni-0.8％??B | ??Mo | Do not have | ??1300 |
| ??25 | ??Si-20Cr-1.5B | ??Mo | Do not have | ??1320 |
Si-25Cr is meant Si-25%Cr.The % omission is not put down in writing
According to the result of table 1, as can be known if Mn and the 0.1 weight % above B of interpolation more than 2% can prevent very effectively that just Mo, W from suffering erosion.
In addition, as can be known when B 0.8% when above, just can not suffer erosion.In addition, the anti-erosion effect of carburizing, boronising also clearly if also use the alloy that adds B, the alloy that adds Mn, just can suffer erosion hardly.
To the experiment slice of numbering 10 in the sample, with the B of characteristic X-ray picture research section, the distribution of Mo element.In addition, the composition of numbering 10 consists of Si-21Co-0.39B.
Fig. 1 represents the photo of the characteristic X-ray picture (reflection) of B and Mo.According to the result of photo, on the interface of Mo, B is from the Si alloy diffusion and be condensed into high concentration as can be known.
The present invention is described with reference to the accompanying drawings.
Fig. 2, Fig. 3, Fig. 4 are the figure of explanation structure of the present invention.
In Fig. 2, Fig. 3, symbol 1 is a ceramic component.
In Fig. 2, after ceramic base material burns till, be connected with electric conductor 3 in order to make external power source, electrode terminal 5 engages with the face that exposes of electric conductor (intermetallic metal spare) 4, under the situation that is for example RF electrode and so on, can intermetallic metal spare be set as required yet and directly engage with electric conductor.In addition, electric conductor 3, electric conductor 4 all are illustrated as electric conductor in the present invention.
In Fig. 2, the gap of electrode terminal 5 and ceramic base material 2, electric conductor (intermetallic metal spare) 4,6 landfills of the melting layer of the Si alloy that is melted.
In Fig. 3, do not have can the intercalation electrode terminal recess, electric conductor (intermetallic metal spare) 4 exposes on the surface of ceramic base material.
The fused mass layer 6 of Si alloy, from preventing that electric conductor from exposing the viewpoint of the oxidation of face, as shown in Figure 3, be not limited in electric conductor and expose face, preferred covering continuously surrounded the ceramic base face that electric conductor exposes face, so that in the clearance portion that electric conductor is exposed face and ceramic base material is included in.At this moment, Si alloy-layer fused mass layer 6 preferred ceramic base face fusion of also exposing face with the encirclement electric conductor.
The key diagram of Fig. 4, the face that exposes of using electrode terminal 5 that the alloy bond (soldering) different with the Si alloy be made of refractory metal and electric conductor 3 is shown, and in order to give the electrode terminal part that outwards protrudes from recess fuses the Si alloy with oxidative resistance coverlay 8.
The gap of electrode terminal 5 and ceramic base material 2 with melting layer 6 landfills of Si alloy, allows Si alloy and electrode terminal and ceramic base material fuse, and makes between electrode terminal and the ceramic base material very close to each other.
Electrode terminal and electric conductor expose face, can use Ni, Co, Au system or other high melting point solder to carry out soldering.Also can engage with the diffusion bond mode.
The engaging of electrode terminal and ceramic base material, electrode terminal expose engaging of face with electric conductor and can carry out simultaneously, also can carry out individually.
That is,, come bonding electrodes terminal and electric conductor to expose face, then under the temperature lower, use Si alloy bond electrode terminal and ceramic base material than first step by soldering or diffusion bond as first step.
In the present invention, the fusion of Si alloy molten thing layer is meant that the Si alloy with predetermined component is heated to more than the solidus temperature, makes it be transformed into liquid phase and fusion.
Fusion is meant to be transformed into fused mass and the metallurgy joint takes place.
The metallurgy joint is meant at least one phenomenon in partial melting that wetting, diffusion or interface take place at least etc. and engages.
In the present invention; expose the gap of face with gap, electrode terminal and the electric conductor of the fused mass landfill electrode terminal of Si alloy and ceramic base material and make the method for its fusion; can be Si alloy powder, particulate or the sheet material of in this gap, filling predetermined component; in a vacuum or in the inert atmosphere; be heated to more than the solidus temperature of this Si alloy, make it be transformed into fused mass and fuse.The fused mass of Si alloy has the character that can both fuse with electrode terminal, ceramic base material and these materials of electric conductor.
Under the situation of Fig. 2～4,, can use the 1st method, the 2nd method, the 3rd method that can prevent above-mentioned erosion for the electrode terminal that prevents electric conductor and refractory metal is subjected to the erosion of Si alloy molten thing.
Applying in a flexible way of obsolete structural articles in the past
The electrode terminal of pedestal class that is built-in with the structure in the past of electric conductor can go out of use because damage, and the present invention can go out of use these because damage members be finished goods of the present invention as material.
That is, in the pedestal of structure in the past, can leave recess after extracting the Ni electrode bar, the electrode terminal of volume structure of the present invention is embedded into this recess, the landfill gap also engages, and just can produce the very excellent pedestal of oxidative resistance, durability.
Fig. 5 is the structure chart of pedestal that leaves the structure in the past of recess after electrode terminal section is pulled out.
Electric conductor (heater wire) 3 is made of the Mo line, and the form to engage with the electric conductor (intermetallic metal spare) 4 that is all the Mo system is embedded among the ceramic base material.Heater wire, intermetallic metal spare are all burnt till simultaneously when the Low fire ceramic base material and are built among the ceramic base material.
Electric conductor (RF electrode) 9 Mo by mesh-like constitute, and are identical with Mo line, Mo intermetallic metal spare, burnt till simultaneously when Low fire ceramic base material 2 and are built among the ceramic base material.
On the inner face of the recess 10 of intermetallic metal spare and the recess 10 of RF electrode, cut internal thread to screw in the Ni electrode bar, after the Ni electrode bar was extracted, screw thread can stay like this.
Key diagram when Fig. 6 is the recess of landfill Fig. 5 and then the ceramic component of finishing structure of the present invention.
Promptly, the recess of the ceramic base material after the Ni electrode bar is extracted is embedded in electrode terminal, gap with the gap of the melting layer landfill electrode terminal of Si alloy and ceramic base material and electrode terminal and intermetallic metal spare, RF electrode, allow melting layer and ceramic base material, electrode terminal and intermetallic metal spare, the RF electrode of this Si alloy fuse, finish the ceramic component of structure of the present invention thus.In other words, surround the gap of electrode terminal and all fill up with the melting layer of Si alloy, allow the face of contact electrode terminal all fuse, the former pedestal in the past that should discard just can be regenerated and be become goods of the present invention.
In the structure of Fig. 6, with regard to electrode terminal, as long as can coefficient of linear expansion and the ceramic base material coupling, just be not limited to refractory metal.The ceramic material of coefficient of linear expansion and ceramic base material coupling, or other above-mentioned electrode terminal material can be brought use all.
Need to prove,, can use above-mentioned the 1st method, the 2nd method, the 3rd method that corrode of being used for preventing for the fused mass that prevents the Si alloy corrodes refractory metal electrode terminal, intermetallic metal spare, RF electrode.
(embodiment)
According to embodiment the present invention is described.
This embodiment uses the pedestal of the structure in the past that leaves recess after the Ni electrode bar is extracted as shown in Figure 5 and go out of use, the ceramic component of the present invention of the structure of shop drawings 6.
Ceramic base material uses aluminium nitride.
Replace the Ni electrode bar of structure in the past, to be inserted into the Ni electrode bar through the Mo system novel electrode terminal of screw thread processing and extract the left recess in back, gap between the gap between electrode terminal and the ceramic base material, electrode terminal and intermetallic metal spare, and electrode terminal and RF gaps between electrodes, filling contains the Si-10%Ni-0.8%B alloy powder cream of the B of 0.8 weight %, in a vacuum, be heated to 1300 ℃ to produce fused mass, respectively with electrode terminal, ceramic base material, electrode intermetallic metal spare and the fusion of RF electrode.In addition, at this moment, also at the Mo system electrode terminal part that outwards protrudes from the cavity, coating contains the powder paste of the Si-10%Ni-0.8%B alloy of 0.8% B, the coverlay of fusion Si alloy on Mo electrode terminal surface simultaneously equally.
Gap between gap between electrode terminal and the ceramic base material, electrode terminal and the intermetallic metal spare, and electrode terminal and RF gaps between electrodes, with this Si alloy landfill, the Si alloy can suitably fuse with ceramic base material, intermetallic metal spare, RF electrode and electrode terminal, allows the junction surface obtain good air-tightness.In addition, also can on the Mo surface, fuse flawless Si alloy coverlay.
Energising heating test
Can apply the alternating voltage of 200V to the electrode terminal 5 of the side that engages with the intermetallic metal spare 4 of Fig. 6, repeat to be warmed up to 500 ℃.
The measurement of corroding
Cut off electrode terminal and the ceramic base material around it, measure the erosion that the Si alloy is caused Mo terminal, Mo intermetallic metal spare, Mo line, Mo screen cloth (RF electrode).
The situation that does not have discovery to suffer erosion fully.
Fig. 7 is expression landfill recess and another embodiment of repairing.
The recess part that lacks intermetallic metal spare shown in Figure 6 of embodiment 1 is formerly filled the mixed-powder of Si alloy and carborundum, and heating and melting in a vacuum allows the composite material fused mass filling recess of Si alloy and carborundum, after solidifying with the recess reparation.
About silicon carbide powder, use particle mean size to be lower than the powder of 45 μ m, mix 20 weight % with respect to the Si alloy.
In the present embodiment, fill the Si alloy of recess and the composite material of carborundum, become the electrode terminal material of the recess part that lacks intermetallic metal spare.
Ceramic base material is all aluminium nitride mutually with embodiment 1.
Before filling fused mass, suffer erosion in order to prevent the Mo line, in advance the exposed division that residues in Mo heater wire 3 in the recess and MoRF electrode wires 9 is implemented boronising and handle.The Si alloy composition of being filled is the Si-25%Cr-5%Mn alloy that contains 5 weight %Mn.
In the recess part of exposing Mo line RF electrode 9, insert with ceramic base material and be all the packing material 12 of nitrogenize aluminum and landfill, gap between the gap between RF electrode 9 and the packing material 12 and ceramic base material and packing material 12, filling contains the powder paste of Si-25%Cr-5%Mn alloy of the Mn of 5 weight %, heating, fusion, fill up the gap with fused mass, with whole clearance plane fusion.In addition, because the packing material 12 of nitrogenize aluminum is an insulator, do not have conductivity, so in order to ensure conductive path, fuse the Si alloy-layer too on the surface of packing material, encase packing material is whole with the Si alloy-layer, outer surface just possesses conductivity.
The result
The junction surface of Si alloy and ceramic base material obtains good air-tightness.In addition, Mo line, RF electrode wires, heater wire all do not break because of erosion, and be deposited all right with the Si alloy.
Soldering Mo electrode terminal on the composite layer of Si alloy and carborundum, and apply alternating voltage, just can be used as heater and heat once more.
[industrial utilizability]
As above detailed description the in detail, the present invention has the excellent effect of exposing the face oxidation of the refractory metal electric conductor that prevents from being built in ceramic base material. And, owing to can eliminate gap between electrode terminal and the ceramic base material, prevent that the refractory metal electric conductor from exposing the excellent effect that the mechanical strength of face and electrode terminal junction surface and periphery thereof is deteriorated, rupture so have. In addition, when the electrode terminal section of the ceramic component of the built-in electric conductor of structure (pedestal class) in the past has when damaged, also the present invention can be used for it is repaired, the recovery of high priced line is used, have very large contribution.
In addition, as the aluminium nitride heater that uses in semiconductor CVD device, can expect has a lot of demands. In addition, the regeneration of obsolete aluminium nitride heater is repaired becomes possibility, and expection can extensive use in the semiconductor industry technical field.
Claims (14)
1. the ceramic component of a built-in electric conductor, described electric conductor are the electric conductors that is made of refractory metal that burns till simultaneously with ceramic base material, and described ceramic component is characterised in that,
Expose on the face at electrode terminal junction surface at this electric conductor, and fusion Si alloy-layer forms.
2. the ceramic component of a built-in electric conductor, the electric conductor that constitutes by refractory metal that its built-in and ceramic base material burn till simultaneously, expose among the recess that face is positioned at this ceramic base material at the electrode terminal junction surface of this electric conductor, and in this recess, insert electrode terminal, gap between the face is exposed at the electrode terminal junction surface of this electrode terminal and this electric conductor and the gap between this electrode terminal and this ceramic base material is formed by Si alloy-layer landfill, described ceramic component is characterised in that
The layer fusion of this Si alloy exposed on the face of face and this ceramic base material at the face of this electrode terminal that contacts with this layer, the electrode terminal junction surface of this electric conductor.
3. the ceramic component of a built-in electric conductor; The electric conductor that is consisted of by refractory metal that its built-in and ceramic base material burn till simultaneously; Expose among the recess that face is positioned at this ceramic base material at the electrode terminal junction surface of this electric conductor; And in this recess, insert the electrode terminal that is consisted of by refractory metal; The electrode terminal junction surface of this electrode terminal and this electric conductor is exposed the layer landfill that gap between the face and the gap between this electrode terminal and this ceramic base material be engaged metal and is formed; Described ceramic component is characterised in that
At least the jointing metal of this electrode terminal and this ceramic base material is the Si alloy, and this Si alloy-layer fusion forms on this electrode terminal and this ceramic base material.
4. according to the ceramic component of any described built-in electric conductor in the claim 1～3, it is characterized in that, at least be that the coverlay of fusion Si alloy forms on the face of the electrode terminal that is made of refractory metal to the material of the part that described ceramic base material exposes outside.
5. according to the ceramic component of any described built-in electric conductor in the claim 1～4, it is characterized in that, described Si alloy is the Si alloy that contains B, expose face or/and on the fused interface of described electrode terminal that constitutes by refractory metal and Si alloy, form the enriched layer of B or the compound layer of B at the electrode terminal junction surface of described electric conductor.
6. according to the ceramic component of any described built-in electric conductor in the claim 1～4, it is characterized in that described Si alloy contains the above Mn of at least 2 weight %.
7. according to the ceramic component of any described built-in electric conductor in the claim 1～6, it is characterized in that, expose face or/and on the face of the described electrode terminal that constitutes by refractory metal, form arbitrary layer in Carburization Treatment layer and the boronising processing layer at the electrode terminal junction surface of described electric conductor.
8. the manufacture method of the ceramic component of a built-in electric conductor, described electric conductor are the conductors that is made of refractory metal that burns till simultaneously with ceramic base material, and described manufacture method is characterised in that,
Expose on the face at electrode terminal junction surface at this electric conductor, the melting layer of fusion Si alloy.
9. the manufacture method of the ceramic component of a built-in electric conductor; The built-in electric conductor that is consisted of by refractory metal that burns till simultaneously with ceramic base material of described ceramic component; Expose among the recess that face is positioned at this ceramic base material at the electrode terminal junction surface of this electric conductor; And in this recess, insert electrode terminal; Gap between the face is exposed at the electrode terminal junction surface of this electrode terminal and this electric conductor and the gap between this electrode terminal and this ceramic base material is formed by Si alloy-layer landfill; Described manufacture method is characterised in that
When making described ceramic component, this Si alloy-layer fusion is exposed on the face of face and this ceramic base material at the face of this electrode terminal that contacts with this layer, the electrode terminal junction surface of this electric conductor.
10. the manufacture method of the ceramic component of a built-in electric conductor; The built-in electric conductor that is consisted of by refractory metal that burns till simultaneously with ceramic base material of described ceramic component; Expose among the recess that face is positioned at this ceramic base material at the electrode terminal junction surface of this electric conductor; And in this recess, insert the electrode terminal that is consisted of by refractory metal; The electrode terminal junction surface of this electrode terminal and this electric conductor is exposed the layer landfill that gap between the face and the gap between this electrode terminal and this ceramic base material be engaged metal and is formed; Described manufacture method is characterised in that
When making described ceramic component, use the jointing metal of Si alloy at least, and allow this Si alloy-layer and this electrode terminal and this ceramic base material fuse as this electrode terminal and this ceramic base material.
11. the manufacture method of the ceramic component of any described built-in electric conductor according to Claim 8～10, it is characterized in that, described electrode terminal be on the electrode terminal face that constitutes by refractory metal to the material of the part that described ceramic base material exposes outside at least, the coverlay of fusion Si alloy.
12. the manufacture method of the ceramic component of any described built-in electric conductor according to Claim 8～10, it is characterized in that, described Si alloy is the Si alloy that contains B, expose face or/and on the fused interface of described electrode terminal that constitutes by refractory metal and Si alloy, form the enriched layer of B or the compound layer of B at the electrode terminal junction surface of described electric conductor.
13. the manufacture method of the ceramic component of any described built-in electric conductor is characterized in that according to Claim 8～10, as described Si alloy, uses the Si alloy that contains the above Mn of 2 weight % at least.
14. the manufacture method of the ceramic component of any described built-in electric conductor according to Claim 8～10, it is characterized in that, expose face or/and on the face of the described electrode terminal that constitutes by refractory metal at the electrode terminal junction surface of described electric conductor, at least form arbitrary layer in Carburization Treatment layer and the boronising processing layer, make the melting layer fusion of Si alloy then.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008-283827 | 2008-11-05 | ||
| JP2008283827A JP2010111523A (en) | 2008-11-05 | 2008-11-05 | Ceramic member having conductor built-in, and method for manufacturing the same |
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| Publication Number | Publication Date |
|---|---|
| CN101740183A true CN101740183A (en) | 2010-06-16 |
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| CN200910179080A Pending CN101740183A (en) | 2008-11-05 | 2009-10-12 | Ceramics member with embedded electric conductor and manufacturing method thereof |
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| Country | Link |
|---|---|
| JP (1) | JP2010111523A (en) |
| KR (1) | KR20100050388A (en) |
| CN (1) | CN101740183A (en) |
| TW (1) | TW201019783A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107564792A (en) * | 2017-08-17 | 2018-01-09 | 沈阳拓荆科技有限公司 | A kind of RF signal transmitting devices for apparatus for processing plasma |
| CN114346523A (en) * | 2022-01-11 | 2022-04-15 | 成都成维精密机械制造有限公司 | Welding flux for connecting silicon carbide ceramics and preparation method thereof |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9543184B2 (en) * | 2012-01-26 | 2017-01-10 | Kyocera Corporation | Electrostatic chuck |
| JP6356598B2 (en) * | 2014-12-25 | 2018-07-11 | 京セラ株式会社 | Parts for semiconductor manufacturing equipment |
| JP6497248B2 (en) * | 2015-07-13 | 2019-04-10 | 住友電気工業株式会社 | Wafer holder |
| JP7143256B2 (en) * | 2019-07-01 | 2022-09-28 | 日本碍子株式会社 | Wafer mounting table and its manufacturing method |
-
2008
- 2008-11-05 JP JP2008283827A patent/JP2010111523A/en active Pending
-
2009
- 2009-09-22 KR KR1020090089573A patent/KR20100050388A/en active IP Right Grant
- 2009-10-12 CN CN200910179080A patent/CN101740183A/en active Pending
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107564792A (en) * | 2017-08-17 | 2018-01-09 | 沈阳拓荆科技有限公司 | A kind of RF signal transmitting devices for apparatus for processing plasma |
| CN107564792B (en) * | 2017-08-17 | 2019-12-13 | 沈阳拓荆科技有限公司 | RF signal transmission device for plasma processing equipment |
| CN114346523A (en) * | 2022-01-11 | 2022-04-15 | 成都成维精密机械制造有限公司 | Welding flux for connecting silicon carbide ceramics and preparation method thereof |
Also Published As
| Publication number | Publication date |
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| TW201019783A (en) | 2010-05-16 |
| KR20100050388A (en) | 2010-05-13 |
| JP2010111523A (en) | 2010-05-20 |
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