WO2019088203A1 - 半導体製造装置用部材、その製法及び成形型 - Google Patents

半導体製造装置用部材、その製法及び成形型 Download PDF

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Publication number
WO2019088203A1
WO2019088203A1 PCT/JP2018/040588 JP2018040588W WO2019088203A1 WO 2019088203 A1 WO2019088203 A1 WO 2019088203A1 JP 2018040588 W JP2018040588 W JP 2018040588W WO 2019088203 A1 WO2019088203 A1 WO 2019088203A1
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Prior art keywords
disc
shaft
electrode
unbaked
semiconductor manufacturing
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PCT/JP2018/040588
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English (en)
French (fr)
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和宏 ▲のぼり▼
拓二 木村
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日本碍子株式会社
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Priority to CN201880070786.0A priority Critical patent/CN111316418B/zh
Priority to KR1020207012611A priority patent/KR102373076B1/ko
Priority to JP2019550475A priority patent/JP6911140B2/ja
Publication of WO2019088203A1 publication Critical patent/WO2019088203A1/ja
Priority to US16/864,282 priority patent/US20200258769A1/en

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    • C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
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    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
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    • C04B2237/70—Forming laminates or joined articles comprising layers of a specific, unusual thickness
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    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/76—Forming laminates or joined articles comprising at least one member in the form other than a sheet or disc, e.g. two tubes or a tube and a sheet or disc
    • C04B2237/765—Forming laminates or joined articles comprising at least one member in the form other than a sheet or disc, e.g. two tubes or a tube and a sheet or disc at least one member being a tube
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    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/80—Joining the largest surface of one substrate with a smaller surface of the other substrate, e.g. butt joining or forming a T-joint

Definitions

  • the present invention relates to a member for a semiconductor manufacturing apparatus, a method of manufacturing the same, and a mold.
  • the member for semiconductor manufacturing apparatuses such as a ceramic heater provided with the ceramic-made disc which incorporates an electrode, and the ceramic-made shaft which supports the disc, is known.
  • a disc and a shaft are separately fired and manufactured, and then heat treatment is performed in a state in which the both are in contact with each other. What is joined is known.
  • the present invention has been made to solve such problems, and its main object is to increase the strength of a member for a semiconductor manufacturing apparatus and to prevent the disc from peeling off the shaft.
  • the member for semiconductor manufacturing apparatus of the present invention is A member for a semiconductor manufacturing apparatus, comprising: a ceramic disc containing an electrode; and a ceramic shaft supporting the disc, The disc and the shaft are integrated without a bonding interface, It is a thing.
  • the member for a semiconductor manufacturing apparatus since the disc and the shaft are integrated without the bonding interface, peeling of the bonding interface does not occur.
  • the heat history of the disk and the shaft may be twice. In this case, the growth of the sintered particles can be suppressed as compared with the case where the stress is applied, and hence the strength can be increased.
  • the electrode may be at least one of a heater electrode, an RF electrode, and an electrostatic electrode. Such electrodes are preferably parallel to the plate surface of the disc.
  • the disc has a gas passage opened in the side surface of the disc and provided along the plate surface direction of the disc, and the shaft extends in the vertical direction
  • a gas supply passage may be provided to supply the gas to the gas passage.
  • the boundary between the outer surface of the shaft and the surface of the disc on which the shaft is integrated may be an R surface or a tapered surface. In this way, the stress applied to the boundary can be relaxed.
  • the shaft is a cylindrical member, and a boundary between the outer surface of the shaft and the surface of the disc on which the shaft is integrated is an R surface or a tapered surface. May be Also in this case, the stress applied to the boundary can be relaxed.
  • the mold of the present invention is A mold used to manufacture the above-described member for a semiconductor manufacturing apparatus, A disc forming portion which is a space for forming a disc lower layer on the shaft side in the disc; A shaft forming portion which is a space communicating with the disc forming portion to form the shaft; Is provided.
  • the disc-shaped portion and the shaft-shaped portion communicate with each other. Therefore, when the ceramic slurry containing the ceramic raw material powder and the molding agent is injected into the mold, the ceramic slurry is filled in both the disc forming portion and the shaft forming portion. After that, when the molding agent is chemically reacted in the mold to mold the ceramic slurry, the unbaked disc lower layer formed by the circular forming portion and the unsintered shaft formed by the shaft forming portion are joined. It is possible to obtain an integrated base molding without using it. If this basic molded body is fired, a member for a semiconductor manufacturing apparatus can be obtained by firing once. In addition, although it may bake after laminating an electrode (or electrode precursor) and a disk compact in the unbaked disc lower layer of a basic compact also in some cases, also in that case, a member for semiconductor manufacturing equipment by firing once. Is obtained.
  • the boundary between the disc-shaped portion and the shaft-shaped portion may be an R surface or a tapered surface.
  • the disc molding portion is a space surrounded by a pair of circular surfaces and an outer peripheral surface connected to the pair of circular surfaces, and of the pair of circular surfaces on the shaft molding portion side.
  • the circular surface may be a concave surface recessed toward the shaft molding portion, and the circular surface of the pair of circular surfaces on the opposite side to the shaft molding portion may be a convex surface expanded toward the shaft molding portion .
  • the fired disc lower layer becomes a substantially flat plane.
  • the concave and convex surfaces have a height difference d of 0.7 mm or more and 2.6 mm or less between the central position and a position 150 mm apart from the central position in the radial direction, or the inclination angle of the concave and convex surfaces It is preferable that ⁇ be 0.25 ° ⁇ ⁇ ⁇ 1 °. In this way, the lower layer of the disc after firing becomes flatter.
  • the concave surface is a conically or frustoconically recessed surface on the shaft molding portion side, and the convex surface is conical or frustoconical on the side opposite to the shaft molding portion. It may be a bulging surface. Alternatively, the concave surface and the convex surface may be curved surfaces.
  • the manufacturing method of the member for semiconductor manufacturing apparatus of the present invention is (A) Basic forming in which the unbaked disc lower layer formed by the circular forming portion and the unsintered shaft formed by the shaft forming portion are integrated without a joint using the forming die described above Manufacturing the body by mold casting method; (B) On the upper surface of the above-mentioned unbaked disc lower layer of the above-mentioned base compact, the unbaked disc upper layer in which the electrode parallel to the above-mentioned unbaked disc lower layer or its precursor was formed is laminated Process, (C) After the final compact is calcined, the disc and the shaft are fired by being placed on a horizontal support surface with the unbaked disc upper layer down and the unbaked shaft up. Obtaining a member for a semiconductor manufacturing apparatus integrated in a state in which there is no bonding interface, Is included.
  • a member for a semiconductor manufacturing device in which a disc and a shaft are integrated without a bonding interface.
  • Such a member for a semiconductor manufacturing apparatus can be produced by firing the final molded body only once (in one heat history), and therefore, compared to the case where the disc or shaft is fired twice, Growth can be suppressed and thus the strength can be increased.
  • a ceramic slurry containing ceramic raw material powder and a molding agent is injected into a molding die, and the molding agent is chemically reacted in the molding die to mold the ceramic slurry.
  • a molding agent for example, an isocyanate and a polyol may be included and molded by a urethane reaction.
  • the “precursor of the electrode” refers to one that becomes an electrode by firing, and refers to, for example, a layer in which an electrode paste is applied or printed in the shape of the electrode.
  • the unbaked disc lower layer and the unbaked shaft are When the unbaked shaft is downward and the unbaked disc lower layer is supported with the unbent shaft and the unbaked disc lower side facing upward, the outer lower rim of the lower disc is warped compared to the central part. become.
  • the firing step when the final compact is supported with the unfired shaft facing up and fired, the fired disc becomes a substantially flat flat surface.
  • gas may be generated when the molding agent chemically reacts in the mold, but the gas is likely to be discharged to the outside along the concave surface. Therefore, almost no air bubbles remain in the base compact.
  • the height difference d of each of the concave surface and the convex surface is 0.7 mm or more and 2.6 mm or less, or when the inclination angle ⁇ is 0.25 ° ⁇ ⁇ ⁇ 1 °, the disc lower layer after firing is It is preferable because it has a flatter surface.
  • step (a) when the basic molded body is manufactured by a mold casting method, a gas passage is opened on the upper surface of the unbaked disc lower layer.
  • step (b) the upper layer of the non-sintered disk may be bonded onto the gas passage to obtain a final molded product. In this way, it is possible to obtain a member for a semiconductor manufacturing apparatus having a gas passage which is opened on the side surface of the disc and provided along the surface direction of the disc.
  • the final compact after calcination may be fired in a state where a weight is placed on the unbaked disc lower layer. In this way, the disk of the ceramic heater obtained after firing becomes flatter and deformation is more suppressed.
  • FIG. 2 is a perspective view of a ceramic heater 10; AA sectional drawing (longitudinal sectional view) of FIG. The longitudinal cross-sectional view of the base molding 30.
  • FIG. FIG. 10 is a molding process diagram until the final molded body 50 is produced.
  • FIG. 7 is a firing process diagram for firing the calcined body 60 to obtain the ceramic heater 10;
  • FIG. 2 is a perspective view of a ceramic heater 110. 7.
  • FIG. FIG. 7 is a firing process diagram for firing the calcined body 160 to obtain a ceramic heater 110.
  • FIG. 7 is a longitudinal sectional view of a modification of the ceramic heater 10;
  • FIG. 7 is a longitudinal sectional view of a modification of the ceramic heater 10;
  • FIG. 1 is a perspective view of a ceramic heater 10
  • FIG. 2 is a cross-sectional view taken along the line AA of FIG.
  • the ceramic heater 10 is a kind of member for a semiconductor manufacturing apparatus, and a disk 12 made of the same ceramic material and a shaft 20 are integrated in a state where there is no bonding interface.
  • the disk 12 incorporates the heater electrode 14 and the RF electrode 16 as shown in FIG.
  • the upper surface of the disk 12 is a wafer mounting surface 12a, on which a silicon wafer to be subjected to plasma processing is mounted.
  • the heater electrode 14 and the RF electrode 16 are substantially parallel to the wafer mounting surface 12 a.
  • the heater electrode 14 is, for example, one in which a conductive coil is wired over the entire surface of the disk in a single-stroke manner.
  • a heater terminal rod (not shown) is connected to the heater electrode 14 and generates heat when a voltage is applied through the heater terminal rod.
  • the RF electrode 16 is a circular thin layer electrode having a diameter slightly smaller than that of the disk 12, and is formed of, for example, a sheet of thin metal wires woven into a mesh.
  • the RF electrode 16 is embedded in the disc 12 between the heater electrode 14 and the wafer mounting surface 12 a.
  • a feed rod (not shown) is connected to the RF electrode 16, and an AC high frequency voltage is applied through the feed rod.
  • the material of the heater electrode 14 and the RF electrode 16 preferably has a thermal expansion coefficient close to that of the ceramic material used for the disc 12 in consideration of preventing the occurrence of a crack in the disc 12 at the time of manufacture.
  • the shaft 20 is integrated with the lower surface of the disc 12 without a bonding interface, and supports the disc 12.
  • the ceramic heater 10 is placed in a chamber (not shown), and the wafer is placed on the wafer placement surface 12a. Then, by applying an alternating high frequency voltage to the RF electrode 16, plasma is generated between the parallel flat plate electrode composed of an opposing horizontal electrode (not shown) installed above the chamber and the RF electrode 16 embedded in the disk 12. The plasma is used to deposit or etch a CVD film on the wafer. Further, the temperature of the wafer is obtained based on a detection signal of a thermocouple (not shown), and the voltage applied to the heater electrode 14 is controlled so that the temperature becomes a set temperature (for example, 350 ° C. or 300 ° C.).
  • a set temperature for example, 350 ° C. or 300 ° C.
  • FIG. 3 is a longitudinal sectional view of the base formed body 30
  • FIG. 4 is a longitudinal sectional view of the forming die 40
  • FIG. 5 is a forming process diagram until the final formed body 50 is produced
  • FIG. FIG. 2 is a firing process diagram for obtaining a ceramic heater 10;
  • a base formed body 30 used to manufacture the ceramic heater 10 is manufactured.
  • the base molded body 30 is one in which the unbaked disc lower layer 32 and the unbaked shaft 34 are integrally molded in a seamless state.
  • the unbaked disc lower layer 32 is a molded body corresponding to the disc lower layer 12 b (see FIG. 2) closer to the shaft than the upper surface of the heater electrode 14 in the disc 12.
  • the unbaked shaft 34 corresponds to the shaft 20. Molding.
  • a heater electrode groove 33 for inserting the heater electrode 14 is formed on the upper surface of the unbaked disc lower layer 32.
  • the unbaked disc lower layer 32 has a shape in which the outer peripheral edge is warped as compared with the central portion.
  • the upper surface of the unbaked disc lower layer 32 is a concave surface conically recessed toward the unsintered shaft 34, and the lower surface is a convex surface bulging conically toward the unsintered shaft 34. ing.
  • the height difference d between the center position and the position 150 mm away from the center position in the radially outward direction is 0.7 mm or more and 2.6 mm or less, or It is preferable that an inclination angle ⁇ formed by a line segment connecting the outer peripheral edge with the horizontal surface be a predetermined angle in a range of 0.25 ° or more and 1 ° or less.
  • the forming die 40 is configured of a die main body 41, a first lid 42, a bottom plate 43 and a cylindrical body 44.
  • the internal space of the forming die 40 is formed of a disc forming portion 45 and a shaft forming portion 46.
  • the mold main body 41 is a portion for shaping the outer peripheral surface of the base molding 30
  • the first lid 42 is a portion for molding the upper surface of the unbaked disc lower layer 32 of the base molding
  • the bottom plate 43 is a base
  • the cylindrical body 44 is a portion for shaping the lower surface of the green shaft 34 of the molded body 30, and the cylindrical portion 44 is a portion for molding the hollow portion of the green shaft 34.
  • the disc molding portion 45 is a space for molding the unbaked disc lower layer 32, it can be said to be a space for forming the disc lower layer 12b.
  • the disc-shaped portion 45 is a space surrounded by a pair of circular surfaces 45a and 45b and an outer peripheral surface 45c connected to the pair of circular surfaces 45a and 45b.
  • the circular surface 45a on the shaft molding portion 46 side is a concave surface recessed toward the shaft molding portion 46 side.
  • the circular surface 45b opposite to the shaft molding portion 46 is a convex surface that bulges toward the shaft molding portion 46 side.
  • the height difference d between the center position and the position 150 mm apart from the center position in the radially outer direction is 0.7 mm or more and 2.6 mm or less.
  • the inclination angle ⁇ of the circular surface 45a and the circular surface 45b is preferably 0.25 ° ⁇ ⁇ ⁇ 1 °. Table 1 below shows an example of the relationship between the inclination angle ⁇ and the height difference d.
  • the circular surface 45 b has a shape capable of forming the heater electrode groove 33 of the unbaked disc lower layer 32 of the base compact 30.
  • the injection port 40 a of the slurry is provided on the outer peripheral surface 45 c of the disc forming portion 45, and the discharge port 40 b is provided on the bottom plate 43 of the shaft forming portion 46.
  • the concave circular surface 45a may be a surface which is recessed in a conical shape or a truncated cone shape, or may be a surface which is curved in a concave shape.
  • the convex circular surface 45 b may be a conically or frustoconically expanded surface or a convexly curved surface.
  • this forming die 40 is disposed so that the disc forming portion 45 is on the bottom and the shaft forming portion 46 is on the top, and ceramic slurry is injected from the injection port 40a to form the disc. The whole of the portion 45 and the shaft forming portion 46 is filled, and the slurry is cured to obtain the base formed body 30.
  • the specific procedure is as follows.
  • a solvent and a dispersant are added to the ceramic powder and mixed to make a ceramic slurry precursor.
  • the ceramic material used as the ceramic powder may be an oxide-based ceramic or a non-oxide-based ceramic.
  • alumina, yttria, aluminum nitride, silicon nitride, silicon carbide, samaria, magnesia, magnesium fluoride, ytterbium oxide and the like may be used. These materials may be used alone or in combination of two or more.
  • the particle diameter of the ceramic material is not particularly limited as long as the slurry can be prepared and prepared.
  • the solvent is not particularly limited as long as it dissolves the dispersant, isocyanate, polyol and catalyst.
  • hydrocarbon solvents toluene, xylene, solvent naphtha etc.
  • ether solvents ethylene glycol monoethyl ether, butyl carbitol, butyl carbitol acetate etc.
  • alcohol solvents isopropanol, 1-butanol, ethanol, 2-ethyl hexanol And terpineol, ethylene glycol, glycerin and the like
  • ketone solvents acetone, methyl ethyl ketone and the like
  • esters butyl acetate, dimethyl glutarate, triacetin and the like
  • polybasic acid solvents glutaric acid and the like
  • a solvent having two or more ester bonds such as polybasic acid ester (eg, dimethyl glutarate etc.), acid ester of polyhydric alcohol (eg, triacetin etc.) and the like.
  • the dispersing agent is not particularly limited as long as, for example, the ceramic powder is uniformly dispersed in a solvent.
  • polycarboxylic acid type copolymers, polycarboxylic acid salts, sorbitan fatty acid esters, polyglycerin fatty acid esters, phosphoric acid ester salt type copolymers, sulfonic acid type copolymers, polyurethane polyester type copolyesters having tertiary amines A polymer etc. can be illustrated.
  • polycarboxylic acid copolymers polycarboxylic acid salts and the like are preferably used.
  • the slurry before molding can be made to have a low viscosity and high fluidity.
  • a solvent and a dispersing agent are added to the ceramic powder at a predetermined ratio, and these are mixed and crushed for a predetermined time to produce a ceramic slurry precursor.
  • the isocyanate is not particularly limited as long as it is a substance having an isocyanate group as a functional group, but, for example, hexamethylene diisocyanate (HDI), tolylene diisocyanate (TDI), diphenylmethane diisocyanate (MDI), or modified products thereof, etc. It can be used.
  • a reactive functional group other than an isocyanate group may be contained, and furthermore, as in the case of polyisocyanate, a large number of reactive functional groups may be contained.
  • the polyol is not particularly limited as long as it is a substance having a functional group capable of reacting with an isocyanate group, for example, a hydroxyl group, an amino group, etc.
  • Polypropylene glycol (PPG), polytetramethylene glycol (PTMG), polyhexamethylene glycol (PHMG), polyvinyl butyral (PVB) and the like may be used.
  • the catalyst is not particularly limited as long as it promotes the urethane reaction, and examples thereof include triethylenediamine, hexanediamine, 6-dimethylamino-1-hexanol, 1,5-diazacyclo (4.3.0) nonene-5, 1,8-Diazabicyclo [5.4.0] -7-undecene, (dimethylbenzylamine), hexamethyltetraethylenetetramine and the like may be used.
  • the ceramic slurry is poured from the injection port 40 a of the forming die 40 to fill the disc forming portion 45 and the shaft forming portion 46.
  • a urethane resin as an organic binder is generated by a chemical reaction (urethane reaction) with an isocyanate and a polyol, and further urethane groups (-O-CO- generated in the same molecule between adjacent urethane resin molecules)
  • the ceramic slurry is cured by crosslinking so as to connect NH-).
  • the urethane resin functions as an organic binder.
  • the mixing method at the time of producing a ceramic slurry precursor or a ceramic slurry is not specifically limited, For example, a ball mill, self-revolution type stirring, vibration type stirring, propeller type stirring, a static mixer etc. can be illustrated.
  • the size of the base compact 30 is determined in consideration of the size of the ceramic heater 10 and the shrinkage rate at the time of firing.
  • gas may be generated when the molding agent chemically reacts in the mold 40, but the gas is likely to be discharged to the outside along the circular surface 45a (concave surface) of the inclination angle ⁇ . Therefore, no air bubbles remain in the base compact 30.
  • the mold 40 is turned over, and the first lid 42 is removed to expose the upper surface of the unbaked disc lower layer 32 of the base molded body 30 (see FIG. 5B).
  • the heater electrode 14 of the shape of a circle is inserted (refer FIG.5 (c)).
  • a second lid 47 whose lower surface is convex downward is attached, and a space is formed above the unbaked disc lower layer 32 (see FIG. 5D). This space is filled with the same ceramic slurry as described above, and cured by a chemical reaction to form the non-fired disc middle layer 35 (see FIG. 5E).
  • An RF electrode groove 35 a is formed on the upper surface of the unbaked disc middle layer 35.
  • the second lid 47 is removed to expose the upper surface of the unbaked disc middle layer 35 (see FIG. 5F), and the mesh-like RF electrode 16 is disposed in the RF electrode groove 35a (FIG. 5 (g )reference).
  • a third lid 48 whose lower surface is convex downward is attached, and a space is formed above the RF electrode 16 (see FIG. 5H). This space is filled with the same ceramic slurry as described above, and cured by a chemical reaction to form an unbaked disk upper layer 36 (see FIG. 5 (i)).
  • the final molded body 50 is one in which the disc portion including the heater electrode 14 and the RF electrode 16 and the hollow shaft portion are integrally formed without a joint, and the upper and lower surfaces of the disc portion are at the central portion.
  • the outer peripheral edge has a curved shape.
  • the height difference d between the center position of the circular surface and the position 150 mm away from the center position in the radially outward direction is preferably 0.7 mm or more and 2.6 mm or less.
  • the inclination angle ⁇ is preferably 0.25 ° or more and 1 ° or less.
  • the decomposition temperature may be, for example, 400 to 600 ° C.
  • the atmosphere may be any of air, inert atmosphere, vacuum and hydrogen atmosphere, but in the case of embedding an electrode or using non-oxide ceramic, inert atmosphere or vacuum
  • the final compact 50 after degreasing is heat-treated (calcined) at 750 to 1300 ° C. to obtain a calcined body 60 (see FIG. 6A).
  • the purpose of calcination is to increase the strength and facilitate handling.
  • the atmosphere may be any of air, inert atmosphere, vacuum and hydrogen atmosphere, but when the electrode is embedded or non-oxide ceramic is used, either inert atmosphere or vacuum is used.
  • the calcined body 60 is, as with the final molded body 50, integrally formed with the disc portion including the heater electrode 14 and the RF electrode 16 and the hollow shaft portion without a joint, and the disc portion is The outer peripheral edge is curved as compared with the central portion, and the inclination angle ⁇ is 0.25 ° or more and 1 ° or less. After drying, degreasing and calcination may be performed at once.
  • the calcined body 60 is fired to obtain the ceramic heater 10 in a state where the calcined body 60 is disposed so that the disc portion is on the bottom and the shaft portion is on the top.
  • the maximum temperature at the time of firing is appropriately set according to the type of powder and the particle diameter of the powder, but is preferably set in the range of 1000 to 2000.degree.
  • the disc portion of the shape of the outer peripheral edge warped as compared with the central portion of the calcined body 60 becomes substantially flat by firing.
  • the atmosphere may be air, inert atmosphere or vacuum. Also, in order to further suppress deformation during firing and make the disc portion flatter, as shown in FIG.
  • the flat horizontal support plate 70 (for example, a plate made of BN material) It is preferable that the disc portion be placed on the lower side and the shaft portion be on the upper side, and the doughnut-shaped weight 72 be placed on the disc portion and fired under normal pressure with a load applied. By doing this, the ceramic heater 10 shown in FIG. 6 (b) is obtained. If the weight of the weight 72 is too heavy, a difference in contraction may occur between the disc portion being loaded and the free shaft portion, resulting in breakage. Therefore, it is preferable to set appropriately in the range of 5 to 10 kg. It is preferable that the weight 72 has a shape that can be divided into two or more along the diameter in consideration of attachment and detachment.
  • the ceramic heater 10 of the present embodiment since the disc 12 and the shaft 20 are integrated without a bonding interface, peeling of the bonding interface does not occur. Further, since the ceramic heater 10 can be manufactured by firing the calcined body 60 only once (in one heat history), compared to the case where the disk 12 and the shaft 20 are subjected to heat history twice. The growth of sintered particles can be suppressed, and thus the strength can be increased.
  • the disc molding portion 45 and the shaft molding portion 46 are in communication. Therefore, the ceramic slurry is injected into the mold 40, and the molding agent is chemically reacted in the mold 40 to mold the slurry, whereby the unbaked disc lower layer 32 and the unbaked shaft 34 have no joint.
  • the base molding 30 integrated in the state can be obtained.
  • the heater electrode 14, the non-sintered disk middle layer 35, the RF electrode 16, and the non-sintered disk upper layer 36 are stacked on the non-sintered disk lower layer 32 of the basic molded body 30 and calcined and fired as the final molded body 50.
  • the ceramic heater 10 is obtained by firing once.
  • the ceramic heater 10 in which the disc 12 and the shaft 20 are integrated without the bonding interface.
  • the pair of circular surfaces 45a and 45b forming the disc molding portion 45 are the concave and convex surfaces described above as the forming die 40, the unbaked disc lower layer 32 and the unbaked shaft 34 are integrated in a seamless state.
  • the unbaked shaft 34 is down and the unbaked disc lower layer 32 is facing up, the outer base of the unbent disc lower layer 32 is warped as compared with the central portion. become.
  • the firing step when the calcined body 60 is supported with the unfired shaft 34 facing up and fired, the disc 12 after firing becomes a substantially flat surface.
  • gas may be generated when the molding agent chemically reacts in the mold 40, but the gas is easily discharged to the outside along the concave surface. Therefore, almost no air bubbles remain in the final molded body 50.
  • the height difference d of each of the concave surface and the convex surface is 0.7 mm or more and 2.6 mm or less, or when the inclination angle ⁇ is 0.25 ° ⁇ ⁇ ⁇ 1 °, the disc lower layer after firing is It becomes a flatter plane.
  • a gas passage 18 may be provided under the heater electrode 14 of the ceramic heater 10 of the embodiment described above.
  • the ceramic heater 10 having the gas passage 18 is referred to as a ceramic heater 110.
  • FIG. 7 is a perspective view of the ceramic heater 110
  • FIG. 8 is a cross-sectional view taken along the line BB in FIG.
  • the gas passage 18 is a passage extending in the vertical and horizontal directions in parallel with the wafer mounting surface 12 a of the disk 12, and both ends are open on the side surface of the ceramic heater 110.
  • a gas supply passage 22 which extends in the vertical direction and supplies the gas to the gas passage 18 is provided on the peripheral wall of the shaft 20.
  • a gas is discharged from the opening of the gas passage 18 through the gas supply passage 22 to a disk By spouting to the side surface 12, it is possible to prevent deposits from adhering to the lower surface of the disk 12.
  • a base molded body 130 shown in FIG. 9B is manufactured.
  • the base molded body 130 is a base molded body except that the gas passage 18 is provided on the upper surface of the unbaked disc lower layer 132 instead of the heater electrode groove 33 and the gas feed passage 22 is provided on the unbaked shaft 134.
  • the configuration is the same as that of 30.
  • the height difference d between the center position and the position 150 mm away from the center position on the upper and lower surfaces of the unbaked disc lower layer 132 is 0.7 mm or more and 2.6 mm or less, or the inclination angle It is preferable that ⁇ be 0.25 ° or more and 1 ° or less.
  • This base molded body 130 is molded using a mold 140 shown in FIG. 9 (a).
  • the mold 140 has a shape similar to that of the mold 40 except that the circular surface 45 b of the mold 40 has a shape capable of forming the gas passage 18 and that the core bar member 142 for forming the gas supply passage 22 is added. It is the same composition.
  • the forming die 140 is disposed so that the disc forming portion 45 is down and the shaft forming portion 46 is up, and the ceramic slurry is injected from the injection port to fill the entire disc forming portion 45 and the shaft forming portion 46 Then, the base compact 130 is obtained by curing the slurry.
  • a disc compact 136 (see FIG. 9C) in which the heater electrode 14 and the RF electrode 16 are embedded is manufactured.
  • the production of the unfired shaft 34 of the calcined body 60 may be omitted in FIG. 5, and only the disk portion may be produced.
  • the upper and lower surfaces of the disk compact 136 also have the height difference d in the above-described numerical range or the inclination angle ⁇ in the above-described numerical range.
  • the adhesive 132a is printed on the upper surface of the base molding 130 except for the gas passage 18, and the printing surface of the adhesive 132a and the heater electrode of the disk molding 136 14) Overlay and bond to the surface on the 14 side. Thereby, the final molded object 150 shown in FIG. 9D is obtained.
  • the adhesive for example, a paste-like adhesive containing the same ceramic material as the disc 12 and the shaft 20, a binder, and a dispersion medium may be used.
  • the final formed body 150 is dried, degreased, and calcined into the calcined body 160 in the same manner as the embodiment described above, and then the calcined body 160 is fired to obtain the ceramic heater 110.
  • a flat horizontal support plate 70 for example, a plate made of BN material
  • the ceramic heater 110 may be fired at atmospheric pressure in a state in which the load is applied to a disc. Since the ceramic heater 110 is integrated with the disc 12 and the shaft 20 without the bonding interface, peeling of the bonding interface does not occur.
  • the ceramic heater 110 can be manufactured by firing the calcined body 160 only once (in one heat history), compared to the case where the disk 12 and the shaft 20 are subjected to heat history twice.
  • the growth of sintered particles can be suppressed, and thus the strength can be increased.
  • both the heater electrode 14 and the RF electrode 16 are incorporated in the disc 12, but only one of them may be incorporated in the disc 12.
  • an electrostatic electrode may be incorporated in the disk 12. The same applies to the ceramic heater 110 in this respect.
  • the circular surface 45a of the mold 40 is a concave surface which is conically recessed, and the circular surface 45b is a convex surface which is conically expanded.
  • the circular surface 45a is a concave surface which is concaved in a conical shape.
  • the surface 45b may be a truncated cone.
  • the circular surface 45 a may be a concave surface recessed in a curved surface, and the circular surface 45 b may be a convex surface recessed in a curved surface.
  • the mold 140 in this respect.
  • the coil-shaped heater electrode 14 is fitted in the heater electrode groove 33 and the mesh-shaped RF electrode 16 is fitted in the RF electrode groove 35a, but such grooves 33 and 35a are not provided.
  • the paste may be used to form an electrode pattern by screen printing or the like.
  • the electrode pattern may be formed on the surface of the molded body, or may be provided in advance on the inner surface of the mold before manufacturing the molded body and be attached to the molded body when the molded body is manufactured.
  • the electrode paste is prepared to include, for example, a conductive material, a ceramic material, a binder, and a dispersion medium.
  • tungsten, tungsten carbide, platinum, silver, palladium, nickel, molybdenum, ruthenium, aluminum, and compounds of these substances can be exemplified.
  • binder polyethylene glycol (PEG), propylene glycol (PG), polypropylene glycol (PPG), polytetramethylene glycol (PTMG), polyhexamethylene glycol (PHMG), polyvinyl butyral (PVB), acrylic resin, etc.
  • dispersant and the dispersion medium the same ones as the molding agent can be used. The same applies to the ceramic heater 110 in this respect.
  • the inclination angle ⁇ of the upper and lower surfaces of the unbaked disc 32 of the base molded body 30 is 0.25 ° or more and 1 ° or less, but the inclination angle ⁇ is an angle outside this range (for example, 0 ° 2 °).
  • the wafer mounting surface 12a of the ceramic heater 10 obtained is not as flat as the embodiment described above, since the disc 12 and the shaft 20 are integrated without a bonding interface, peeling of the bonding interface Does not happen.
  • the calcined body can be manufactured with one heat history, the growth of sintered particles can be suppressed compared to the case where the disk 12 and the shaft 20 are subjected to the heat history twice. As a result, the strength can be increased. The same applies to the ceramic heater 110 in this respect.
  • the stage of the base compact 30 (see FIG. 5B), the stage of attaching the heater electrode 14 to the base compact 30 (see FIG. 5C), the heater electrode 14 on the base compact 30.
  • the step of laminating the unbaked disc middle layer 35 (see FIG. 5F), and the step of laminating the heater electrode 14, the unbaked disc middle layer 35 and the RF electrode 16 on the base compact 30 (see FIG. 5G)
  • the fired body may be produced by firing in the same manner as the above-mentioned firing step, and the remaining portion may be separately produced and joined to the fired body.
  • the shaft 20 is a cylindrical member, but a solid cylindrical member may be used.
  • the boundary portion 10b with the back surface 12c of 12 may be an R surface (a curved surface having a predetermined radius of curvature).
  • the boundary portions 10a and 10b may be tapered surfaces. In this way, the stress applied to the boundaries 10a and 10b can be relaxed.
  • the portions corresponding to the boundary portions 10a and 10b in the molding die 40 of FIG. 4 may be R surfaces or tapered surfaces.
  • one of the boundaries 10a and 10b may be an R surface and the other may be perpendicular, or one of the boundaries 10a and 10b may be a tapered surface, and the other may be orthogonal, or one of the boundaries 10a and 10b may be The R surface and the other may be tapered surfaces.
  • the ceramic heater 10 was produced, and in Experimental Example A11, a ceramic heater similar to the ceramic heater 10 was produced. Further, the ceramic heater 110 was manufactured in the experimental examples B1 to B4, and the ceramic heater similar to the ceramic heater 110 was manufactured in the experimental example B4.
  • Example A1 Forming step First, 100 parts by mass of aluminum nitride powder (purity 99.7%), 5 parts by mass of yttrium oxide, 2 parts by mass of dispersant (polycarboxylic acid copolymer), and dispersion medium (polybasic acid ester) A ceramic slurry precursor was obtained by mixing 30 parts by mass with a ball mill (Trommel) for 14 hours. To this ceramic slurry precursor, 4.5 parts by mass of isocyanate (4,4'-diphenylmethane diisocyanate), 0.1 parts by mass of water, and 0.4 parts by mass of catalyst (6-dimethylamino-1-hexanol) are added. A ceramic slurry was obtained by mixing and mixing.
  • a final compact 50 was produced in accordance with the procedure shown in FIG.
  • the inclination angle ⁇ of the mold 40 was 0.5 °.
  • the height difference d between the center position of the circular surface of the mold 40 and the position 150 mm away from the center position in the radially outward direction was 1.3 mm.
  • the heater electrode 14 used Mo coil, and the RF electrode 16 used Mo mesh.
  • the obtained final molded body 50 is dried at 100 ° C. for 10 hours, subsequently degreased at a maximum temperature of 500 ° C., and further calcined at a maximum temperature of 820 ° C. in a nitrogen atmosphere. I got a body 60.
  • the disc portion of the calcined body 60 is placed on the flat horizontal support plate 70 made of BN with the shaft portion up, and the doughnut-shaped weight 72 (10 kg) is a disc In a state where it was placed on a part and load was applied, it was fired at 1860 ° C. for 6 hours by firing under atmospheric pressure in nitrogen gas. Thereby, ceramic heater 10 (diameter of disk 12 is 300 mm) was obtained.
  • the ceramic heater 10 of Example 1 had a strength of 330 MPa, an average particle diameter of 4.2 ⁇ m, and a warp of 0.05 mm after firing. In addition, no bubbles were observed in the final molded body 50. In addition, strength measurement conformed to JIS: 1601, and a test piece was cut out so as to include a connecting portion between the disc 12 and the shaft 20.
  • the test piece was a rectangular solid having a width W of 4.0 mm, a thickness t of 3.0 mm, and a length of 40 mm.
  • This test piece was placed on two fulcrums arranged at a fixed distance so that the connecting part was at the center between the fulcrums, divided into two points at equal distances from the center between the fulcrums to the right and left and broken
  • the maximum bending stress was measured.
  • the average particle size is defined as the average of the major and minor axes of the particles observed by SEM as the particle size, and the average of the particle sizes of 40 particles observed as the average particle size.
  • the warpage was a difference between the maximum value and the minimum value of the height on the wafer mounting surface 12a.
  • the presence or absence of air bubbles was judged by visually observing the cross section of the final molded body 50. Further, as shown in the SEM image (magnification of 500, reflection electron image) of FIG. 13, the ceramic heater 10 of Experimental Example A1 is integrated in a state where the bonding interface between the disc-like sintered body and the tubular sintered body can not be distinguished. It had been.
  • the SEM image may use a
  • Example A2 to A7 In Experimental Examples A2 to A7, a ceramic heater 10 was produced in the same manner as in Experimental Example A1, except that the inclination angle ⁇ and the height difference d of Experimental Example A1 were changed.
  • the ceramic heater 10 of the experimental examples A2 to A7 is also integrated in the state where the disc 12 and the shaft 20 do not have a bonding interface, as in the experimental example A1.
  • the inclination angle ⁇ , elevation difference d, firing method, strength, average particle diameter, warpage after firing and presence of air bubbles in experimental examples A2 to A7 are summarized in Table 2.
  • Example A8 Forming Step A ceramic slurry precursor was prepared in the same manner as in Experimental Example A1. To this ceramic slurry precursor, 4.5 parts by mass of isocyanate (hexamethylene diisocyanate), 0.1 parts by mass of water, and 0.4 parts by mass of catalyst (6-dimethylamino-1-hexanol) are added and mixed. Thus, a ceramic slurry was obtained. Using this ceramic slurry, a final compact 50 was produced in accordance with the procedure shown in FIG. The inclination angle ⁇ of the mold 40 was 0.5 °, and the height difference d was 1.3 mm. The heater electrode 14 and the RF electrode 16 were formed by screen printing Mo paste (containing aluminum nitride powder (purity 99.7%)). Therefore, the heater electrode groove 33 and the RF electrode groove 35a are omitted.
  • isocyanate hexamethylene diisocyanate
  • catalyst 6-dimethylamino-1-hexanol
  • Example A9 Forming Step 5% by mass of yttrium oxide as a sintering aid was added to 95% by mass of aluminum nitride powder, and mixed using a ball mill. A binder was added to the obtained mixed powder and granulated by a spray granulation method. The obtained granulated powder was degreased, and a disc-shaped compact and a tubular compact were molded by die molding and CIP. An Mo mesh as an RF electrode and an Mo coil as a heater electrode were embedded in the inside of the disk-shaped compact.
  • the disc-shaped compact was fired at 1860 ° C. for 6 hours in a nitrogen gas by a hot press method to obtain a disc-shaped fired body.
  • the tubular formed body was fired at 1860 ° C. for 6 hours by normal pressure firing in nitrogen gas to obtain a tubular fired body.
  • Example B1 After the final compact 150 was produced according to FIG. 9 and the final compact 150 was calcined into a calcined mass 160, the ceramic heater 110 of Experimental Example B1 was produced according to FIG.
  • the ceramic slurry in the forming step was prepared in the same manner as in Experimental Example A1.
  • the conditions of the drying, degreasing, and calcination steps and the firing step were also the same as in Experimental Example A1.
  • As the adhesive a paste was used in which aluminum nitride powder, an acrylic resin as a binder, and terbineol as a dispersion medium were mixed. The characteristics are shown in Table 3. Incidentally, no bonding interface was observed in this ceramic heater 110 either.
  • Example B2 After the final compact 150 was produced according to FIG. 9 and the final compact 150 was calcined into a calcined mass 160, the ceramic heater 110 of Experimental Example B2 was produced according to FIG.
  • the ceramic slurry of the forming step was prepared in the same manner as Example A8.
  • the conditions of the drying, degreasing, and calcination steps and the firing step were the same as those of Experimental Example A8.
  • As the adhesive a paste was used in which aluminum nitride powder, an acrylic resin as a binder, and terbineol as a dispersion medium were mixed. The characteristics are shown in Table 3. Incidentally, no bonding interface was observed in this ceramic heater 110 either.
  • Example B3 Forming Step 5% by weight of yttrium oxide was added as a sintering aid to 95% by weight of aluminum nitride powder, and mixed using a ball mill. A binder was added to the obtained mixed powder and granulated by a spray granulation method. The obtained granulated powder was degreased, and a disc-shaped compact and a tubular compact were molded by die molding and CIP. As a disk-shaped compact, a first disk-shaped compact in which a heater electrode (Mo coil) was embedded inside, and a second disk-shaped compact in which an RF electrode (mesh electrode) was embedded inside were produced.
  • a heater electrode Mo coil
  • RF electrode meh electrode
  • the first disc-shaped sintered body and the second disc-shaped molded body are separately separately fired in a nitrogen gas by a hot press method at 1860 ° C. for 6 hours, thereby the first disc-shaped sintered body and the second disc-shaped molded body. It was set as a disk-shaped sintered body. Further, the tubular formed body was fired at 1860 ° C. for 6 hours by firing in a normal pressure in nitrogen gas to obtain a tubular fired body.
  • experimental examples A1 to A8 and experimental examples B1 to B2 correspond to examples of the present invention
  • experimental examples A9 and B3 correspond to comparative examples.
  • the above-described experimental examples do not limit the present invention.
  • the present invention is applicable to members used in a semiconductor manufacturing apparatus, such as a ceramic heater, an electrostatic chuck heater, and an electrostatic chuck.

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Abstract

本発明の半導体製造装置用部材は、電極を内蔵するセラミック製の円板と前記円板を支持するセラミック製のシャフトとを備えており、円板とシャフトとは、接合界面のない状態で一体化されている。

Description

半導体製造装置用部材、その製法及び成形型
　本発明は、半導体製造装置用部材、その製法及び成形型に関する。
　従来より、電極を内蔵するセラミック製の円板と、その円板を支持するセラミック製のシャフトとを備えたセラミックヒータなどの半導体製造装置用部材が知られている。こうした半導体製造装置用部材を製造するにあたっては、例えば特許文献１に記載されているように、円板とシャフトとをそれぞれ別々に焼成して作製したあと、両者を接触させた状態で熱処理を行い接合したものが知られている。
特開２００６－２３２５７６号公報
　しかしながら、一旦焼成した円板やシャフトを接合のため熱処理すると、熱履歴が２回掛かるため、焼結粒子が成長してしまい、円板やシャフトの強度が弱くなったり、まれに接合界面の剥離が起きたりするという問題があった。
　本発明はこのような課題を解決するためになされたものであり、半導体製造装置用部材の強度を高くすると共に円板とシャフトとの剥離が起こらないようにすることを主目的とする。
　本発明の半導体製造装置用部材は、
　電極を内蔵するセラミック製の円板と前記円板を支持するセラミック製のシャフトとを備えた半導体製造装置用部材であって、
　前記円板と前記シャフトとは、接合界面のない状態で一体化されている、
　ものである。
　この半導体製造装置用部材では、円板とシャフトとは、接合界面のない状態で一体化されているため、接合界面の剥離が起きることはない。また、こうした半導体製造装置用部材は、円板とシャフトとの一体成形体を１度だけの焼成で（１回の熱履歴で）作製することができるため、円板やシャフトに２回熱履歴が掛かる場合に比べて焼結粒子の成長を抑えることができ、ひいては強度を高くすることができる。
　本発明の半導体製造装置用部材において、前記電極は、ヒータ電極、ＲＦ電極及び静電電極の少なくとも１つとしてもよい。こうした電極は、円板の板面と平行になっていることが好ましい。
　本発明の半導体製造装置用部材において、前記円板は、前記円板の側面に開口し前記円板の板面方向に沿って設けられたガス通路を有し、前記シャフトは、上下方向に延びて前記ガス通路にガスを供給するガス供給路を有していてもよい。ガス供給路を介してガス通路の開口から円板の側面にガスを噴出させることにより、円板の下面に堆積物が付着するのを防止することができる。
　本発明の半導体製造装置用部材において、前記シャフトの外面と前記円板のうち前記シャフトが一体化されている面との境界部は、Ｒ面又はテーパ面であってもよい。こうすれば、境界部に加わる応力を緩和することができる。
　本発明の半導体製造装置用部材において、前記シャフトは円筒部材であり、前記シャフトの外面と前記円板のうち前記シャフトが一体化されている面との境界部は、Ｒ面又はテーパ面であってもよい。このようにしても、境界部に加わる応力を緩和することができる。
　本発明の成形型は、
　上述した半導体製造装置用部材を製造するのに用いられる成形型であって、
　前記円板のうちシャフト側の円板下層を形成するための空間である円板成形部と、
　前記円板成形部に連通し前記シャフトを形成するための空間であるシャフト成形部と、
　を備えたものである。
　この成形型では、円板成形部とシャフト成形部とが連通している。そのため、セラミック原料粉末とモールド化剤とを含むセラミックスラリーを成形型内に注入すると、セラミックスラリーは円板成形部とシャフト成形部の両方に充填される。その後、成形型内でモールド化剤を化学反応させてセラミックスラリーをモールド化させると、円形成形部によって成形される未焼成円板下層とシャフト成形部によって成形される未焼成シャフトとがつなぎ目のない状態で一体化された基礎成形体を得ることができる。この基礎成形体を焼成すれば、１度の焼成により半導体製造装置用部材が得られる。なお、基礎成形体の未焼成円板下層に更に電極（あるいは電極前駆体）や円板成形体を積層してから焼成する場合もあるが、その場合も１度の焼成により半導体製造装置用部材が得られる。
　本発明の成形型において、円板成形部とシャフト成形部との境界部は、Ｒ面又はテーパ面であってもよい。
　本発明の成形型において、前記円板成形部は、一対の円形面と該一対の円形面に連なる外周面とで囲まれた空間であり、前記一対の円形面のうち前記シャフト成形部側の円形面は、前記シャフト成形部側に窪んだ凹面であり、前記一対の円形面のうち前記シャフト成形部とは反対側の円形面は、前記シャフト成形部側に膨らんだ凸面であってもよい。こうすれば、未焼成円板下層と未焼成シャフトがつなぎ目のない状態で一体化された基礎成形体を未焼成シャフトが下、未焼成円板下層が上を向く姿勢で支持したとき、未焼成円板下層は中心部に比べて外周縁が反り上がった形状になる。この基礎成形体を焼成する場合、未焼成シャフトが上、未焼成円板下層が下を向く姿勢で支持して焼成すれば、焼成後の円板下層はほぼフラットな平面になる。前記凹面及び前記凸面は、中心位置とその中心位置から半径外方向に１５０ｍｍ離れた位置との高低差ｄが０．７ｍｍ以上２．６ｍｍ以下であること、あるいは、前記凹面及び前記凸面の傾斜角度θは０．２５°≦θ≦１°であることが好ましい。こうすれば、焼成後の円板下層はよりフラットな平面になる。なお、基礎成形体の未焼成円板下層に更に電極（あるいは電極前駆体）や円板成形体を積層してから焼成する場合もあるが、その場合、焼成後の円板下層、電極及び円板がフラットな平面になる。
　本発明の成形型において、前記凹面は、前記シャフト成形部側に円錐状又は円錐台状に窪んだ面であり、前記凸面は、前記シャフト成形部とは反対側に円錐状又は円錐台状に膨らんだ面であってもよい。あるいは、前記凹面及び前記凸面は、湾曲面であってもよい。
　本発明の半導体製造装置用部材の製法は、
（ａ）上述した成形型を用いて、前記円形成形部によって成形される未焼成円板下層と前記シャフト成形部によって成形される未焼成シャフトとがつなぎ目のない状態で一体化された基礎成形体を、モールドキャスト法により作製する工程と、
（ｂ）前記基礎成形体の前記未焼成円板下層の上面に、前記未焼成円板下層と平行な電極又はその前駆体が形成された未焼成円板上層を積層して最終成形体を得る工程と、
（ｃ）前記最終成形体を仮焼したあと、前記未焼成円板上層が下、前記未焼成シャフトが上になるように水平支持面に載置した状態で焼成することにより、円板とシャフトとが接合界面のない状態で一体化された半導体製造装置用部材を得る工程と、
　を含むものである。
　この半導体製造装置用部材の製法によれば、円板とシャフトとが接合界面のない状態で一体化された半導体製造装置用部材を得ることができる。こうした半導体製造装置用部材は、最終成形体を１度だけ焼成して（１回の熱履歴で）作製することができるため、円板やシャフトを２度焼成する場合に比べて焼結粒子の成長を抑えることができ、ひいては強度を高くすることができる。
　ここで、「モールドキャスト法」とは、セラミック原料粉末とモールド化剤とを含むセラミックスラリーを成形型内に注入し、その成形型内でモールド化剤を化学反応させてセラミックスラリーをモールド化させることにより成形体を得る方法をいう。モールド化剤としては、例えば、イソシアネート及びポリオールを含み、ウレタン反応によりモールド化するものとしてもよい。「電極の前駆体」とは、焼成することにより電極となるものをいい、例えば電極ペーストを電極の形状に塗布又は印刷した層などをいう。
　本発明の半導体製造装置用部材の製法において、成形型として、円板成形部をなす一対の円形面が上述した凹面と凸面のものを用いた場合、未焼成円板下層と未焼成シャフトとがつなぎ目のない状態で一体化された基礎成形体を未焼成シャフトが下、未焼成円板下層が上を向く姿勢で支持したとき、円板下層は中心部に比べて外周縁が反り上がった形状になる。焼成工程で、最終成形体を未焼成シャフトが上になるように支持して焼成すれば、焼成後の円板はほぼフラットな平面になる。また、モールドキャスト法では、成形型内でモールド化剤が化学反応したときにガスが発生することがあるが、そのガスは凹面に沿って外部へ排出されやすい。そのため、基礎成形体に気泡はほとんど残らない。特に、凹面及び凸面のそれぞれの高低差ｄを０．７ｍｍ以上２．６ｍｍ以下にした場合、あるいは、傾斜角度θを０．２５°≦θ≦１°にした場合、焼成後の円板下層はよりフラットな平面になるため好ましい。
　本発明の半導体製造装置用部材の製法において、前記工程（ａ）では、前記基礎成形体をモールドキャスト法により作製する際に、前記未焼成円板下層の上面にガス通路を側面に開口するように形成しておき、前記工程（ｂ）では、前記ガス通路の上に、前記未焼成円板上層を接着して最終成形体を得るようにしてもよい。こうすれば、円板の側面に開口し円板の板面方向に沿って設けられたガス通路を有する半導体製造装置用部材を得ることができる。
　本発明の半導体製造装置用部材の製法において、前記工程（ｃ）では、仮焼したあとの前記最終成形体の前記未焼成円板下層に錘を載せた状態で焼成してもよい。こうすれば、焼成後に得られるセラミックヒータの円板はよりフラットになると共に変形がより抑制される。
セラミックヒータ１０の斜視図。 図１のＡ－Ａ断面図（縦断面図）。 基礎成形体３０の縦断面図。 成形型４０の縦断面図。 最終成形体５０を作製するまでの成形工程図。 仮焼体６０を焼成してセラミックヒータ１０を得る焼成工程図。 セラミックヒータ１１０の斜視図。 図７のＢ－Ｂ断面図。 最終成形体１５０を作製するまでの成形工程図。 仮焼体１６０を焼成してセラミックヒータ１１０を得る焼成工程図。 セラミックヒータ１０の変形例の縦断面図。 セラミックヒータ１０の変形例の縦断面図。 実験例Ａ１のセラミックヒータ１０のＳＥＭ写真。 実験例Ａ１１のセラミックヒータのＳＥＭ写真。
　本発明の好適な実施形態を、図面を参照しながら以下に説明する。図１はセラミックヒータ１０の斜視図、図２は図１のＡ－Ａ断面図である。
　セラミックヒータ１０は、図１に示すように、半導体製造装置用部材の一種であり、同じセラミック材料からなる円板１２とシャフト２０とが接合界面のない状態で一体化されたものである。
　円板１２は、図２に示すように、ヒータ電極１４及びＲＦ電極１６を内蔵している。円板１２の上面はウエハ載置面１２ａであり、プラズマ処理を施すシリコン製のウエハが載置される。ヒータ電極１４及びＲＦ電極１６は、ウエハ載置面１２ａとほぼ平行になっている。ヒータ電極１４は、例えば導電性のコイルを円板の全面にわたって一筆書きの要領で配線したものである。このヒータ電極１４には、それぞれヒータ端子棒（図示せず）が接続されており、そのヒータ端子棒を介して電圧が印加されることにより発熱する。ＲＦ電極１６は、円板１２よりもやや小径の円形の薄層電極であり、例えば細い金属線を網状に編み込んでシート状にしたメッシュで形成されている。このＲＦ電極１６は、円板１２のうちヒータ電極１４とウエハ載置面１２ａとの間に埋設されている。ＲＦ電極１６には、給電棒（図示せず）が接続されており、その給電棒を介して交流高周波電圧が印加されるようになっている。なお、ヒータ電極１４やＲＦ電極１６の材質は、製造時に円板１２にクラックが発生するのを防止することを考慮すると、円板１２に用いるセラミック材料と熱膨張係数が近いものが好ましい。
　シャフト２０は、円板１２の下面に接合界面のない状態で一体化されており、円板１２を支持している。
　次に、セラミックヒータ１０の使用例について説明する。図示しないチャンバ内にセラミックヒータ１０を配置し、ウエハ載置面１２ａにウエハを載置する。そして、ＲＦ電極１６に交流高周波電圧を印加することにより、チャンバ内の上方に設置された図示しない対向水平電極と円板１２に埋設されたＲＦ電極１６とからなる平行平板電極間にプラズマを発生させ、そのプラズマを利用してウエハにＣＶＤ成膜を施したりエッチングを施したりする。また、図示しない熱電対の検出信号に基づいてウエハの温度を求め、その温度が設定温度（例えば３５０℃とか３００℃）になるようにヒータ電極１４へ印加する電圧を制御する。
　次に、セラミックヒータ１０の製造例について説明する。図３は基礎成形体３０の縦断面図、図４は成形型４０の縦断面図、図５は最終成形体５０を作製するまでの成形工程図、図６は仮焼体６０を焼成してセラミックヒータ１０を得る焼成工程図である。
１．成形工程
　まず、セラミックヒータ１０を製造するのに用いられる基礎成形体３０を作製する。基礎成形体３０は、図３に示すように、未焼成円板下層３２と未焼成シャフト３４とがつなぎ目のない状態で一体に成形されたものである。未焼成円板下層３２は、円板１２のうちヒータ電極１４の上面よりもシャフト側の円板下層１２ｂ（図２参照）に相当する成形体であり、未焼成シャフト３４は、シャフト２０に相当する成形体である。未焼成円板下層３２の上面には、ヒータ電極１４を嵌め込むためのヒータ電極用溝３３が形成されている。未焼成円板下層３２は、中心部に比べて外周縁が反り上がった形状になっている。具体的には、未焼成円板下層３２の上面は未焼成シャフト３４に向かって円錐状に窪んだ凹面となっており、下面は未焼成シャフト３４に向かって円錐状に膨出した凸面となっている。未焼成円板下層３２の上下面のそれぞれにおいて、中心位置とその中心位置から半径外方向に１５０ｍｍ離れた位置との高低差ｄが０．７ｍｍ以上２．６ｍｍ以下であること、あるいは、中心部と外周縁とを結んだ線分が水平面となす傾斜角度θが０．２５°以上１°以下の範囲内の所定角度となっていることが好ましい。
　基礎成形体３０を作製するには、基礎成形体３０を成形するための成形型４０を用意する。成形型４０は、図４に示すように、型本体４１と第１蓋４２と底板４３と円柱体４４とで構成されている。成形型４０の内部空間は、円板成形部４５とシャフト成形部４６とで構成されている。型本体４１は、基礎成形体３０の外周面を形取る部分であり、第１蓋４２は、基礎成形体３０の未焼成円板下層３２の上面を形取る部分であり、底板４３は、基礎成形体３０の未焼成シャフト３４の下面を形取る部分であり、円柱体４４は、未焼成シャフト３４の中空部分を形取る部分である。また、円板成形部４５は、未焼成円板下層３２を成形するための空間であるため、円板下層１２ｂを形成するための空間ともいえる。この円板成形部４５は、一対の円形面４５ａ，４５ｂと該一対の円形面４５ａ，４５ｂに連なる外周面４５ｃとで囲まれた空間である。一対の円形面４５ａ，４５ｂのうち、シャフト成形部４６側の円形面４５ａは、シャフト成形部４６側に窪んだ凹面である。また、シャフト成形部４６とは反対側の円形面４５ｂは、シャフト成形部４６側に膨らんだ凸面である。凹面である円形面４５ａ及び凸面である円形面４５ｂは、その中心位置とその中心位置から半径外方向に１５０ｍｍ離れた位置との高低差ｄが０．７ｍｍ以上２．６ｍｍ以下であることが好ましい。また、円形面４５ａ及び円形面４５ｂの傾斜角度θは０．２５°≦θ≦１°であることが好ましい。以下の表１に傾斜角度θと高低差ｄとの関係の一例を示す。円形面４５ｂは、基礎成形体３０の未焼成円板下層３２のヒータ電極用溝３３を形成可能な形状となっている。成形型４０において、スラリーの注入口４０ａは円板成形部４５の外周面４５ｃに設けられ、排出口４０ｂはシャフト成形部４６の底板４３に設けられている。なお、凹面である円形面４５ａは、円錐状又は円錐台状に窪んだ面でもよいし、凹状に湾曲した面でもよい。また、凸面である円形面４５ｂは、円錐状又は円錐台状に膨らんだ面でもよいし、凸状に湾曲した面でもよい。
Figure JPOXMLDOC01-appb-T000001
　この成形型４０を、図５（ａ）に示すように、円板成形部４５が下、シャフト成形部４６が上になるように配置し、セラミックスラリーを注入口４０ａから注入して円板成形部４５及びシャフト成形部４６の全体に充填し、そのスラリーを硬化させることにより基礎成形体３０を得る。具体的な手順は以下の通りである。
　セラミック粉体に、溶媒及び分散剤を加えて混合して、セラミックスラリー前駆体を作製する。セラミック粉体として使用されるセラミック材料は、酸化物系セラミックでもよいし、非酸化物系セラミックでもよい。例えば、アルミナ、イットリア、チッ化アルミ、チッ化ケイ素、炭化ケイ素、サマリア、マグネシア、フッ化マグネシウム、酸化イッテルビウム等が使用され得る。これらの材料は、１種類単独で、或いは２種以上を組み合わせて使用され得る。また、スラリーを調整・作製可能な限りにおいて、セラミック材料の粒子径は特に限定されない。溶媒としては、分散剤、イソシアネート、ポリオール及び触媒を溶解するものであれば、特に限定されない。例えば、炭化水素溶媒（トルエン、キシレン、ソルベントナフサ等）、エーテル溶媒（エチレングリコールモノエチルエーテル、ブチルカルビトール、ブチルカルビトールアセテート等）、アルコール溶媒（イソプロパノール、１－ブタノール、エタノール、２－エチルヘキサノール、テルピネオール、エチレングリコール、グリセリン等）、ケトン溶媒（アセトン、メチルエチルケトン等）、エステル（酢酸ブチル、グルタル酸ジメチル、トリアセチン等）、多塩基酸溶媒（グルタル酸等）を例示することができる。特に、多塩基酸エステル（例えば、グルタル酸ジメチル等）、多価アルコールの酸エステル（例えば、トリアセチン等）等の、２以上のエステル結合を有する溶剤を使用することが好ましい。分散剤としては、例えば、セラミック粉体を溶媒中に均一に分散するものであれば、特に限定されない。例えば、ポリカルボン酸系共重合体、ポリカルボン酸塩、ソルビタン脂肪酸エステル、ポリグリセリン脂肪酸エステル、リン酸エステル塩系共重合体、スルホン酸塩系共重合体、３級アミンを有するポリウレタンポリエステル系共重合体等を例示することができる。特に、ポリカルボン酸系共重合体、ポリカルボン酸塩等を使用することが好ましい。この分散剤を添加することで、成形前のスラリーを、低粘度とし、且つ高い流動性を有するものとすることができる。このように、セラミック粉体に、溶媒、及び分散剤が所定の割合で添加され、所定時間に亘ってこれらを混合・解砕して、セラミックスラリー前駆体が作製される。
　続いて、セラミックスラリー前駆体に、モールド化剤（イソシアネート及びポリオール）と、触媒とが添加され、これらを混合・真空脱泡して、セラミックスラリーを作製する。イソシアネートとしては、イソシアネート基を官能基として有する物質であれば特に限定されないが、例えば、ヘキサメチレンジイソシアネート（ＨＤＩ）、トリレンジイソシアネート（ＴＤＩ）、ジフェニルメタンジイソシアネート（ＭＤＩ）、或いは、これらの変性体等が使用され得る。なお、分子内おいて、イソシアネート基以外の反応性官能基が含有されていてもよく、更には、ポリイソシアネートのように、反応官能基が多数含有されていてもよい。ポリオールとしては、イソシアネート基と反応し得る官能基、例えば、水酸基、アミノ基等を有する物質であれば特に限定されないが、例えば、エチレングリコール（ＥＧ）、ポリエチレングリコール（ＰＥＧ）、プロピレングリコール（ＰＧ）、ポリプロピレングリコール（ＰＰＧ）、ポリテトラメチレングリコール（ＰＴＭＧ）、ポリヘキサメチレングリコール（ＰＨＭＧ）、ポリビニルブチラール（ＰＶＢ）等が使用され得る。触媒としては、ウレタン反応を促進させる物質であれば特に限定されないが、例えば、トリエチレンジアミン、ヘキサンジアミン、６－ジメチルアミノ－１－ヘキサノール、１，５－ジアザシクロ（４．３．０）ノネンー５、１，８－ジアザビシクロ［５．４．０］－７－ウンデセン、（ジメチルベンジルアミン）、ヘキサメチルテトラエチレンテトラミン等が使用され得る。セラミックスラリーを成形型４０の注入口４０ａから流し込んで円板成形部４５とシャフト成形部４６に充填する。その後、イソシアネート及びポリオールによる化学反応（ウレタン反応）により有機バインダとしてのウレタン樹脂を生成させ、さらに隣接するウレタン樹脂の分子間において、同分子中にそれぞれ生成されているウレタン基（－Ｏ－ＣＯ－ＮＨ－）同士を連結するように架橋させることにより、セラミックスラリーを硬化させる。ウレタン樹脂は有機バインダとして機能する。これにより、成形型４０の内部に基礎成形体３０が作製される。
　なお、セラミックスラリー前駆体やセラミックスラリーを作製する際の混合方法は、特に限定されるものではなく、例えばボールミル、自公転式撹拌、振動式撹拌、プロペラ式撹拌、スタティックミキサー等を例示できる。基礎成形体３０の大きさは、セラミックヒータ１０の大きさと焼成時の収縮率とを考慮して決定する。また、成形型４０内でモールド化剤が化学反応したときにガスが発生することがあるが、そのガスは傾斜角度θの円形面４５ａ（凹面）に沿って外部へ排出されやすい。そのため、基礎成形体３０に気泡は残らない。
　続いて、成形型４０をひっくり返したあと第１蓋４２を取り外し、基礎成形体３０の未焼成円板下層３２の上面を露出させ（図５（ｂ）参照）、ヒータ電極用溝３３にコイル状のヒータ電極１４を嵌め込む（図５（ｃ）参照）。続いて、下面が下に向かって凸になっている第２蓋４７を取り付け、未焼成円板下層３２の上方に空間を形成する（図５（ｄ）参照）。この空間に先ほどと同様のセラミックスラリーを充填し、化学反応により硬化させることにより未焼成円板中層３５を成形する（図５（ｅ）参照）。未焼成円板中層３５の上面には、ＲＦ電極用溝３５ａが形成される。続いて、第２蓋４７を取り外し、未焼成円板中層３５の上面を露出させ（図５（ｆ）参照）、ＲＦ電極用溝３５ａにメッシュ状のＲＦ電極１６を配置する（図５（ｇ）参照）。続いて、下面が下に向かって凸になっている第３蓋４８を取り付け、ＲＦ電極１６の上方に空間を形成する（図５（ｈ）参照）。この空間に先ほどと同様のセラミックスラリーを充填し、化学反応により硬化させることにより未焼成円板上層３６を成形する（図５（ｉ）参照）。続いて、第３蓋４８、底板４３及び円柱体４４を取り外し、型本体４１を分解し、最終成形体５０を取り出す（図５（ｊ）参照）。最終成形体５０は、ヒータ電極１４及びＲＦ電極１６を含む円板部分と中空のシャフト部分とがつなぎ目のない状態で一体に成形されたものであり、円板部分の上面及び下面は中心部に比べて外周縁が反り上がった形状である。円形面の中心位置とその中心位置から半径外方向に１５０ｍｍ離れた位置との高低差ｄは０．７ｍｍ以上２．６ｍｍ以下であることが好ましい。また、傾斜角度θは０．２５°以上１°以下であることが好ましい。
２．乾燥・脱脂・仮焼工程
（１）乾燥
　最終成形体５０に含まれる分散媒を蒸発させる。使用する分散媒種により乾燥温度や乾燥時間は適宜設定すればよい。ただし、乾燥温度が高すぎるとクラックの原因となるため好ましくない。また、雰囲気は大気、不活性雰囲気、真空、水素雰囲気のいずれでもよい。
（２）脱脂
　分散媒を蒸発させたあとの最終成形体５０に含まれるバインダ、分散剤及び触媒を分解させる。分解温度としては、例えば４００～６００℃、雰囲気は大気、不活性雰囲気、真空、水素雰囲気のいずれでもよいが、電極を埋設する場合や非酸化物系セラミックを使用する場合は不活性雰囲気か真空のいずれかとする。
（３）仮焼
　脱脂したあとの最終成形体５０を７５０～１３００℃で熱処理（仮焼）を行うことにより仮焼体６０（図６（ａ）参照）を得る。仮焼するのは、強度を高くしてハンドリングしやすくするためである。雰囲気は大気、不活性雰囲気、真空、水素雰囲気のいずれでもよいが、電極を埋設する場合や非酸化物系セラミックを使用する場合は不活性雰囲気か真空のいずれかとする。仮焼体６０は、最終成形体５０と同様、ヒータ電極１４及びＲＦ電極１６を含む円板部分と中空のシャフト部分とがつなぎ目のない状態で一体に成形されたものであり、円板部分は中心部に比べて外周縁が反り上がった形状であり、傾斜角度θは０．２５°以上１°以下になっている。なお、乾燥後、脱脂と仮焼を一度に行ってもよい。
３．焼成工程
　仮焼体６０を円板部分が下、シャフト部分が上になるように配置した状態で、仮焼体６０を焼成してセラミックヒータ１０を得る。焼成時の最高温度は粉末の種類、粉末の粒子径により適宜設定するが、１０００～２０００℃の範囲に設定することが好ましい。仮焼体６０のうち中心部に比べて外周縁が反り上がった形状の円板部分は焼成によってほぼフラットになる。雰囲気は大気、不活性雰囲気、真空のいずれでもよい。また、焼成時の変形をより抑制し円板部分をよりフラットにするため、図６（ａ）のように、フラットな水平支持板７０（例えばＢＮ材からなる板）に、仮焼体６０の円板部分を下、シャフト部分を上にして載せ、ドーナツ状の錘７２を円板部分に載せて荷重を加えた状態で常圧焼成するのが好ましい。こうすることにより、図６（ｂ）に示すセラミックヒータ１０が得られる。錘７２の重さが重すぎると、加重されている円板部分とフリーのシャフト部分との間に収縮差が生じて割れるおそれがある。そのため、５～１０ｋｇの範囲で適宜設定するのが好ましい。錘７２は、装着や脱着を考慮すると、直径に沿って２つ以上に分割可能な形状になっていることが好ましい。
　以上詳述した本実施形態のセラミックヒータ１０では、円板１２とシャフト２０とは接合界面のない状態で一体化されているため、接合界面の剥離が起きることはない。また、セラミックヒータ１０は、仮焼体６０を１度だけ焼成して（１回の熱履歴で）作製することができるため、円板１２やシャフト２０を２回熱履歴を掛ける場合に比べて焼結粒子の成長を抑えることができ、ひいては強度を高くすることができる。
　また、成形型４０は、円板成形部４５とシャフト成形部４６とが連通している。そのため、セラミックスラリーを成形型４０内に注入し、成形型４０内でモールド化剤を化学反応させてスラリーをモールド化させることにより、未焼成円板下層３２と未焼成シャフト３４とがつなぎ目のない状態で一体化された基礎成形体３０を得ることができる。この基礎成形体３０の未焼成円板下層３２にヒータ電極１４、未焼成円板中層３５、ＲＦ電極１６及び未焼成円板上層３６を積層して最終成形体５０としてから仮焼、焼成するため、１度の焼成によりセラミックヒータ１０が得られる。
　更に、上述したセラミックヒータ１０の製法によれば、円板１２とシャフト２０とが接合界面のない状態で一体化されたセラミックヒータ１０を容易に得ることができる。特に、成形型４０として、円板成形部４５をなす一対の円形面４５ａ，４５ｂが上述した凹面と凸面であるため、未焼成円板下層３２と未焼成シャフト３４とがつなぎ目のない状態で一体化された基礎成形体３０を未焼成シャフト３４が下、未焼成円板下層３２が上を向く姿勢で支持したとき、未焼成円板下層３２は中心部に比べて外周縁が反り上がった形状になる。焼成工程で、仮焼体６０を未焼成シャフト３４が上になるように支持して焼成すれば、焼成後の円板１２はほぼフラットな平面になる。また、モールドキャスト法では、成形型４０内でモールド化剤が化学反応したときにガスが発生することがあるが、そのガスは凹面に沿って外部へ排出されやすい。そのため、最終成形体５０に気泡はほとんど残らない。特に、凹面及び凸面のそれぞれの高低差ｄを０．７ｍｍ以上２．６ｍｍ以下にした場合、あるいは、傾斜角度θを０．２５°≦θ≦１°にした場合、焼成後の円板下層はよりフラットな平面になる。
　更にまた、焼成工程では、仮焼体６０の円板部分に錘７２を載せた状態で常圧焼成するため、円板１２はよりフラットになると共により変形が抑制される。
　なお、本発明は上述した実施形態に何ら限定されることはなく、本発明の技術的範囲に属する限り種々の態様で実施し得ることはいうまでもない。
　例えば、上述した実施形態のセラミックヒータ１０のヒータ電極１４の下に、図７及び図８に示すようにガス通路１８を設けてもよい。ガス通路１８を有するセラミックヒータ１０をセラミックヒータ１１０と称する。図７はセラミックヒータ１１０の斜視図、図８は図７のＢ－Ｂ断面図である。ガス通路１８は、円板１２のウエハ載置面１２ａと平行に縦横に延びる通路であり、両端はセラミックヒータ１１０の側面に開口している。シャフト２０の周壁には、上下方向に延びてガス通路１８にガスを供給するガス供給路２２が設けられている。セラミックヒータ１１０のウエハ載置面１２ａに載置したウエハにプラズマを利用してＣＶＤ成膜を施したりエッチングを施したりする際、ガス供給路２２を介してガスをガス通路１８の開口から円板１２の側面に噴出させることにより、円板１２の下面に堆積物が付着するのを防止することができる。セラミックヒータ１１０を製造するには、まず、図９（ｂ）に示す基礎成形体１３０を作製する。基礎成形体１３０は、未焼成円板下層１３２の上面にヒータ電極用溝３３ではなくガス通路１８を設けたことと、未焼成シャフト１３４にガス供給路２２を設けたこと以外は、基礎成形体３０と同様の構成である。未焼成円板下層１３２の上下両面は、それぞれ、中心位置とその中心位置から半径外方向に１５０ｍｍ離れた位置との高低差ｄは０．７ｍｍ以上２．６ｍｍ以下であること、あるいは、傾斜角度θが０．２５°以上１°以下であることが好ましい。この基礎成形体１３０は、図９（ａ）に示す成形型１４０を用いて成形する。成形型１４０は、成形型４０の円形面４５ｂをガス通路１８を形成可能な形状にしたことと、ガス供給路２２を形成するための芯棒部材１４２を加えたこと以外は、成形型４０と同様の構成である。この成形型１４０を、円板成形部４５が下、シャフト成形部４６が上になるように配置し、セラミックスラリーを注入口から注入して円板成形部４５及びシャフト成形部４６の全体に充填し、そのスラリーを硬化させることにより基礎成形体１３０を得る。一方、基礎成形体１３０とは別に、ヒータ電極１４とＲＦ電極１６とを埋設した円板成形体１３６（図９（ｃ）参照）を作製する。円板成形体１３６を作製するには、例えば、図５において仮焼体６０の未焼成シャフト３４の作製を省略して円板部分のみを作製すればよい。この円板成形体１３６の上下両面も上述した数値範囲の高低差ｄあるいは上述した数値範囲の傾斜角度θを有していることが好ましい。そして、図９（ｃ）に示すように、基礎成形体１３０の上面のうちガス通路１８を除く部分に接着剤１３２ａを印刷し、その接着剤１３２ａの印刷面と円板成形体１３６のヒータ電極１４側の表面とを重ね合わせて接着する。これにより、図９（ｄ）に示す最終成形体１５０が得られる。接着剤としては、例えば、円板１２やシャフト２０と同じセラミック材料とバインダと分散媒とを含むペースト状の接着剤を用いればよい。最終成形体１５０を、上述した実施形態と同様にして、乾燥、脱脂、仮焼して仮焼体１６０としたあとこの仮焼体１６０を焼成することにより、セラミックヒータ１１０を得る。例えば、図１０に示すように、フラットな水平支持板７０（例えばＢＮ材からなる板）に、仮焼体１６０の円板部分を下、シャフト部分を上にして載せ、ドーナツ状の錘７２を円板に載せて荷重を加えた状態で常圧焼成してセラミックヒータ１１０としてもよい。このセラミックヒータ１１０は、円板１２とシャフト２０とは接合界面のない状態で一体化されているため、接合界面の剥離が起きることはない。また、セラミックヒータ１１０は、仮焼体１６０を１度だけ焼成して（１回の熱履歴で）作製することができるため、円板１２やシャフト２０を２回熱履歴を掛ける場合に比べて焼結粒子の成長を抑えることができ、ひいては強度を高くすることができる。
　上述した実施形態では、ヒータ電極１４及びＲＦ電極１６の両方を円板１２に内蔵した例を示したが、いずれか一方のみを円板１２に内蔵してもよい。また、これらの電極１４，１６に代えて又は加えて静電電極を円板１２に内蔵してもよい。この点はセラミックヒータ１１０も同様である。
　上述した実施形態では、成形型４０の円形面４５ａを円錐状に窪んだ凹面とし、円形面４５ｂを円錐状に膨らんだ凸面としたが、円形面４５ａを円錐台状に窪んだ凹面とし、円形面４５ｂを円錐台状に窪んだ凸面としてもよい。あるいは、円形面４５ａを曲面状に窪んだ凹面とし、円形面４５ｂを曲面状に窪んだ凸面としてもよい。この点は成形型１４０も同様である。
　上述した実施形態では、ヒータ電極用溝３３にコイル状のヒータ電極１４を嵌め込み、ＲＦ電極用溝３５ａにメッシュ状のＲＦ電極１６を嵌め込んだが、このような溝３３，３５ａを設けず、電極ペーストを用いてスクリーン印刷等により電極パターンを形成してもよい。電極パターンは、成形体の表面に形成してもよいし、成形体を作製する前の成形型の内面に予め設けておき成形体を作製する際にその成形体に付着させてもよい。電極ペーストは、例えば、導電材料とセラミック材料とバインダーと分散媒とを含むように調製する。導電材料としては、タングステン、タングステンカーバイト、白金、銀、パラジウム、ニッケル、モリブデン、ルテニウム、アルミニウム及びこれらの物質の化合物等を例示することができる。バインダーとしては、ポリエチレングリコール（ＰＥＧ）、プロピレングリコール（ＰＧ）、ポリプロピレングリコール（ＰＰＧ）、ポリテトラメチレングリコール（ＰＴＭＧ）、ポリヘキサメチレングリコール（ＰＨＭＧ）、ポリビニルブチラール（ＰＶＢ）、アクリル樹脂等を使用できる。また、分散剤、分散媒はモールド化剤と同様のものを使用できる。この点はセラミックヒータ１１０も同様である。
　上述した実施形態では、基礎成形体３０の未焼成円板３２の上下両面の傾斜角度θを０．２５°以上１°以下としたが、傾斜角度θがこの範囲外の角度（例えば０°とか２°）であってもよい。その場合、得られるセラミックヒータ１０のウエハ載置面１２ａは上述した実施形態ほどフラットにならないものの、円板１２とシャフト２０とは接合界面のない状態で一体化されているため、接合界面の剥離が起きることはない。また、その場合も、仮焼体を１回の熱履歴で作製することができるため、円板１２やシャフト２０を２回熱履歴を掛ける場合に比べて焼結粒子の成長を抑えることができ、ひいては強度を高くすることができる。この点はセラミックヒータ１１０も同様である。
　上述した実施形態において、基礎成形体３０の段階（図５（ｂ）参照）、基礎成形体３０にヒータ電極１４を取り付けた段階（図５（ｃ）参照）、基礎成形体３０にヒータ電極１４及び未焼成円板中層３５を積層した段階（図５（ｆ）参照）、基礎成形体３０にヒータ電極１４、未焼成円板中層３５及びＲＦ電極１６を積層した段階（図５（ｇ）参照）のいずれかの段階で、上述した焼成工程と同様の手法で焼成して焼成体を作製し、残りの部分は個別に製作してその焼成体と接合してもよい。
　上述した実施形態では、シャフト２０は円筒部材を用いたが、中実の円柱部材を用いてもよい。
　上述した実施形態のセラミックヒータ１０において、図１１に示すように、シャフト２０の外面と円板１２のうちシャフト２０が一体化されている裏面１２ｃとの境界部１０ａやシャフト２０の内面と円板１２の裏面１２ｃとの境界部１０ｂをＲ面（所定の曲率半径を持つ曲面）としてもよい。あるいは、図１２に示すように、境界部１０ａ，１０ｂをテーパ面としてもよい。こうすれば、境界部１０ａ，１０ｂに加わる応力を緩和することができる。境界部１０ａ，１０ｂがＲ面やテーパ面であるセラミックヒータ１０を製造する場合、図４の成形型４０のうち境界部１０ａ，１０ｂに対応する部分をＲ面やテーパ面にすればよい。なお、境界部１０ａ，１０ｂの一方をＲ面、もう一方を直角としてもよいし、境界部１０ａ，１０ｂの一方をテーパ面、もう一方を直角としてもよいし、境界部１０ａ，１０ｂの一方をＲ面、もう一方をテーパ面としてもよい。この点はセラミックヒータ１１０も同様である。
　以下に説明する実験例Ａ１～Ａ１０ではセラミックヒータ１０を作製し、実験例Ａ１１ではセラミックヒータ１０と同様のセラミックヒータを作製した。また、実験例Ｂ１～Ｂ４ではセラミックヒータ１１０を作製し、実験例Ｂ４ではセラミックヒータ１１０と同様のセラミックヒータを作製した。
［実験例Ａ１］
１．成形工程
　まず、窒化アルミニウム粉末（純度９９．７％）１００質量部と、酸化イットリウム５質量部と、分散剤（ポリカルボン酸系共重合体）２質量部と、分散媒（多塩基酸エステル）３０質量部とを、ボールミル（トロンメル）を用いて１４時間混合することにより、セラミックスラリー前駆体を得た。このセラミックスラリー前駆体に対して、イソシアネート（４，４’－ジフェニルメタンジイソシアネート）４．５質量部、水０．１質量部、触媒（６－ジメチルアミノ－１－ヘキサノール）０．４質量部を加えて混合することにより、セラミックスラリーを得た。このセラミックスラリーを用いて、図５に示した手順にしたがって最終成形体５０を作製した。成形型４０の傾斜角度θは０．５°とした。成形型４０の円形面の中心位置とその中心位置から半径外方向に１５０ｍｍ離れた位置との高低差ｄは１．３ｍｍであった。また、ヒータ電極１４はＭｏコイルを使用し、ＲＦ電極１６はＭｏメッシュを使用した。
２．乾燥・脱脂・仮焼工程
　得られた最終成形体５０を１００℃で１０時間乾燥し、続いて最高温度５００℃で脱脂し、更に最高温度８２０℃、窒素雰囲気で仮焼することにより、仮焼体６０を得た。
３．焼成工程
　図６に示すように、ＢＮ製のフラットな水平支持板７０に、仮焼体６０の円板部分を下、シャフト部分を上にして載せ、ドーナツ状の錘７２（１０ｋｇ）を円板部分に載せて荷重を加えた状態で、窒素ガス中で常圧焼成により１８６０℃で６時間焼成した。これにより、セラミックヒータ１０（円板１２の直径は３００ｍｍ）を得た。
　実施例１のセラミックヒータ１０は、表２に示すように、強度３３０ＭＰａ、平均粒子径４．２μｍ、焼成後の反り０．０５ｍｍであった。また、最終成形体５０に気泡は見られなかった。なお、強度測定はＪＩＳ：１６０１に準じており、円板１２とシャフト２０との連結部を含むように試験片を切り出した。試験片は、幅Ｗが４．０ｍｍ、厚さｔが３．０ｍｍ、長さが４０ｍｍの直方体とした。この試験片を、一定距離に配置された２支点上に連結部が支点間の中央になるように置き、支点間の中央から左右に等しい距離にある２点に分けて荷重を加えて折れたときの最大曲げ応力を測定した。平均粒子径は、ＳＥＭにて観察した粒子の長軸と短軸の平均を粒子径とし、観察した粒子４０個の粒子径の平均を平均粒子径とした。反りは、ウエハ載置面１２ａにおける高さの最大値と最小値との差とした。気泡の有無は、最終成形体５０の断面を目視により観察して判断した。また、実験例Ａ１のセラミックヒータ１０は、図１３のＳＥＭ像（倍率５００倍、反射電子像）に示すように、円板状焼成体と管状焼成体との接合界面が判別できない状態で一体化されていた。なお、ＳＥＭ像は２次電子像を利用してもよい。
［実験例Ａ２～Ａ７］
　実験例Ａ２～Ａ７では、実験例Ａ１の傾斜角度θ及び高低差ｄを変更した以外は、実験例Ａ１と同様にしてセラミックヒータ１０を作製した。実験例Ａ２～Ａ７のセラミックヒータ１０も、実験例Ａ１と同様、円板１２とシャフト２０とが接合界面のない状態で一体化されていた。実験例Ａ２～Ａ７の傾斜角度θ、高低差ｄ、焼成方法、強度、平均粒子径、焼成後の反り及び気泡の有無を表２にまとめた。
［実験例Ａ８］
１．成形工程
　実験例Ａ１と同様にしてセラミックスラリー前駆体を調製した。このセラミックスラリー前駆体に対して、イソシアネート（ヘキサメチレンジイソシアネート）４．５質量部、水０．１質量部、触媒（６－ジメチルアミノ－１－ヘキサノール）０．４質量部を加えて混合することにより、セラミックスラリーを得た。このセラミックスラリーを用いて、図５に示した手順にしたがって最終成形体５０を作製した。成形型４０の傾斜角度θは０．５°、高低差ｄは１．３ｍｍとした。ヒータ電極１４及びＲＦ電極１６はＭｏペースト（窒化アルミニウム粉末（純度９９．７％）を含む）をスクリーン印刷して形成した。そのため、ヒータ電極用溝３３やＲＦ電極用溝３５ａは省略した。
２．乾燥・脱脂・仮焼工程
　得られた最終成形体５０を１００℃で１０時間乾燥し、続いて最高温度１３００℃、水素雰囲気で脱脂・仮焼することにより、仮焼体６０を得た。
３．焼成工程
　実験例Ａ１と同様にして焼成することにより、実験例Ａ８のセラミックヒータ１０を得た。その特性を表２に示す。なお、このセラミックヒータ１０も実験例Ａ１と同様、接合界面が見られなかった。
［実験例Ａ９］
１．成形工程
　窒化アルミニウム粉末９５質量％に、焼結助剤として酸化イットリウム５質量％を加え、ボールミルを用いて混合した。得られた混合粉末に、バインダを添加し、噴霧造粒法により造粒した。得られた造粒粉を脱脂し、金型成形及びＣＩＰにより円板状成形体と管状成形体とを成形した。円板状成形体の内部にはＲＦ電極としてＭｏメッシュ、ヒータ電極としてＭｏコイルを埋設した。
２．焼成工程
　円板状成形体を窒素ガス中でホットプレス法により１８６０℃で６時間焼成し、円板状焼成体とした。これとは別に、管状成形体を窒素ガス中で常圧焼成により１８６０℃で６時間焼成し、管状焼成体とした。
３．接合工程
　円板状焼成体と管状焼成体との接合界面に硝酸イットリウムを塗布し、１００℃で１時間乾燥した。そして、特開２００６－２３２５７６号公報の実施例１に記載されている接合方法により、円板状焼成体と管状焼成体とを熱処理して接合し、実験例Ａ９のセラミックヒータを得た。その特性を表２に示す。なお、実験例Ａ９のセラミックヒータは、図１４のＳＥＭ像に示すように、円板状焼成体と管状焼成体との接合界面が判別できる状態で一体化されていた。
Figure JPOXMLDOC01-appb-T000002
　表２の実験例Ａ１～Ａ７の結果から明らかなように、傾斜角度θが０．２５°以上１°以下（高低差ｄが０．７ｍｍ以上２．６ｍｍ以下）であれば傾斜角度θが０°（高低差ｄが０ｍｍ）の場合に比べて反りが軽減されることがわかった。また、実験例Ａ１，Ａ３～Ａ７のように傾斜角度θ（高低差ｄ）がつけられている場合には、最終成形体５０に気泡は見られなかった。更に、実験例Ａ１，Ａ８は、実験例Ａ９に比べて平均粒子径が小さく、強度が高かった。実験例Ａ９では、円板状焼成体と管状焼成体とを再焼成して接合したため、接合界面が判別でき、焼結粒子の成長も進んで強度が低下したと考えられる。これに対し、実験例Ａ１，Ａ８では、円板部分とシャフト部分とのつなぎ目のない仮焼体６０を１度だけ焼成したため、接合界面がなく、焼結粒子の成長も抑えることができ、ひいては強度を高くすることができたと考えられる。なお、実験例Ａ２～Ａ７のセラミックヒータ１０は、傾斜角度θ及び高低差ｄが異なる以外は実験例Ａ１と同様に作製したため、強度や平均粒子径は実験例Ａ１と同等と考えられる。
［実験例Ｂ１］
　図９にしたがって最終成形体１５０を作製し、その最終成形体１５０を仮焼して仮焼体１６０にしたあと、図１０にしたがって実験例Ｂ１のセラミックヒータ１１０を作製した。成形工程のセラミックスラリーは実験例Ａ１と同様にして調製した。また、乾燥・脱脂・仮焼工程及び焼成工程の条件も実験例Ａ１と同様とした。接着剤には、窒化アルミニウム粉末、バインダとしてアクリル樹脂及び分散媒としてテルビネオールを混合したペーストを用いた。その特性を表３に示す。なお、このセラミックヒータ１１０も接合界面が見られなかった。
［実験例Ｂ２］
　図９にしたがって最終成形体１５０を作製し、その最終成形体１５０を仮焼して仮焼体１６０にしたあと、図１０にしたがって実験例Ｂ２のセラミックヒータ１１０を作製した。成形工程のセラミックスラリーは実験例Ａ８と同様にして調製した。また、乾燥・脱脂・仮焼工程及び焼成工程の条件も実験例Ａ８と同様とした。接着剤には、窒化アルミニウム粉末、バインダとしてアクリル樹脂及び分散媒としてテルビネオールを混合したペーストを用いた。その特性を表３に示す。なお、このセラミックヒータ１１０も接合界面が見られなかった。
［実験例Ｂ３］
１．成形工程
　窒化アルミニウム粉末９５重量％に、焼結助剤として酸化イットリウム５重量％を加え、ボールミルを用いて混合した。得られた混合粉末に、バインダを添加し、噴霧造粒法により造粒した。得られた造粒粉を脱脂し、金型成形及びＣＩＰにより円板状成形体と管状成形体とを成形した。円板状成形体として、内部にヒータ電極（Ｍｏコイル）を埋設した第１円板状成形体と、内部にＲＦ電極（メッシュ電極）を埋設した第２円板状成形体を作製した。
２．焼成工程
　第１円板状成形体と第２円板状成形体を、それぞれ個別に窒素ガス中でホットプレス法により１８６０℃で６時間焼成することにより、第１円板状焼成体と第２円板状焼成体とした。また、管状成形体を窒素ガス中で常圧焼成により１８６０℃で６時間焼成することにより、管状焼成体とした。
３．接合工程
　第１円板状焼成体と第２円板状焼成体と管状焼成体との接合界面に硝酸イットリウムを塗布し、１００℃で１時間乾燥した。そして、特開２００６－２３２５７６号公報の実施例１に記載されている接合方法により、第１円板状焼成体と第２円板状焼成体と管状焼成体とを熱処理して接合し、実験例Ｂ３のセラミックヒータを得た。その特性を表３に示す。なお、実験例Ｂ３のセラミックヒータは、第１円板状焼成体と第２円板状焼成体と管状焼成体との接合界面がＳＥＭで判別できる状態で一体化されていた。
Figure JPOXMLDOC01-appb-T000003
　表３から明らかなように、実験例Ｂ１～Ｂ２では、実験例Ｂ３に比べて反りが軽減されることがわかった。また、実験例Ｂ１～Ｂ２は、実験例Ｂ３に比べて平均粒子径が小さく、強度が高かった。実験例Ｂ３では、第１円板状焼成体と第２円板状焼成体と管状焼成体とを熱処理して接合したため、接合界面が判別でき、焼結粒子の成長も進んで強度が低下したと考えられる。これに対し、実験例Ｂ１～Ｂ２では、円板部分とシャフト部分とのつなぎ目のない仮焼体１６０を１度だけ焼成したため、接合界面がなく、焼結粒子の成長も抑えることができ、ひいては強度を高くすることができたと考えられる。
　以上説明した実験例のうち、実験例Ａ１～Ａ８及び実験例Ｂ１～Ｂ２が本発明の実施例に相当し、実験例Ａ９及び実験例Ｂ３が比較例に相当する。なお、上述した実験例は本発明を何ら限定するものではない。
　本出願は、２０１７年１１月２日に出願された日本国特許出願第２０１７－２１２９３２号を優先権主張の基礎としており、引用によりその内容の全てが本明細書に含まれる。
　本発明は、半導体製造装置に用いられる部材、例えばセラミックヒータ、静電チャックヒータ、静電チャックなどに利用可能である。
１０，１１０　セラミックヒータ、１０ａ，１０ｂ　境界部、１２　円板、１２ａ　ウエハ載置面、１２ｂ　円板下層、１２ｃ　裏面、１４　ヒータ電極、１６　ＲＦ電極、１８　ガス通路、２０　シャフト、２２　ガス供給路、３０　基礎成形体、３２　未焼成円板下層、３３　ヒータ電極用溝、３４　未焼成シャフト、３５　未焼成円板中層、３５ａ　ＲＦ電極用溝、３６　未焼成円板上層、４０　成形型、４０ａ　注入口、４０ｂ　排出口、４１　型本体、４２　第１蓋、４３　底板、４４　円柱体、４５　円板成形部、４５ａ，４５ｂ　円形面、４５ｃ　外周面、４６　シャフト成形部、４７　第２蓋、４８　第３蓋、５０　最終成形体、６０　仮焼体、７０　水平支持板、７２　錘、１３０　基礎成形体、１３２　未焼成円板下層、１３２ａ　接着剤、１３４　未焼成シャフト、１３６　円板成形体、１４０　成形型、１４２　芯棒部材、１５０　最終成形体、１６０　仮焼体。

Claims (12)

  1. 　電極を内蔵するセラミック製の円板と前記円板を支持するセラミック製のシャフトとを備えた半導体製造装置用部材であって、
    　前記円板と前記シャフトとは、接合界面のない状態で一体化されている、
    　半導体製造装置用部材。
  2. 　前記電極は、ヒータ電極、ＲＦ電極及び静電電極の少なくとも１つである、
    　請求項１に記載の半導体製造装置用部材。
  3. 　前記円板は、前記円板の側面に開口し前記円板の板面方向に沿って設けられたガス通路を有し、前記シャフトは、上下方向に延びて前記ガス通路にガスを供給するガス供給路を有する、
    　請求項１又は２に記載の半導体製造装置用部材。
  4. 　前記シャフトの外面と前記円板のうち前記シャフトが一体化されている面との境界部は、Ｒ面又はテーパ面である、
    　請求項１～３のいずれか１項に記載の半導体製造装置用部材。
  5. 　前記シャフトは、円筒部材であり、
    　前記シャフトの内面と前記円板のうち前記シャフトが一体化されている面との境界部は、Ｒ面又はテーパ面である、
    　請求項１～４のいずれか１項に記載の半導体製造装置用部材。
  6. 　請求項１～５のいずれか１項に記載の半導体製造装置用部材を製造するのに用いられる成形型であって、
    　前記円板のうちシャフト側の円板下層を形成するための空間である円板成形部と、
    　前記円板成形部に連通し前記シャフトを形成するための空間であるシャフト成形部と、
    　を備えた成形型。
  7. 　前記円板成形部は、一対の円形面と該一対の円形面に連なる外周面とで囲まれた空間であり、
    　前記一対の円形面のうち前記シャフト成形部側の円形面は、前記シャフト成形部側に窪んだ凹面であり、前記一対の円形面のうち前記シャフト成形部とは反対側の円形面は、前記シャフト成形部側に膨らんだ凸面である、
    　請求項６に記載の成形型。
  8. 　前記凹面及び前記凸面は、中心位置とその中心位置から半径外向きに１５０ｍｍ離れた位置との高低差ｄが０．７ｍｍ以上２．６ｍｍ以下である、
    　請求項７に記載の成形型。
  9. 　前記凹面及び前記凸面の傾斜角度θは、０．２５°≦θ≦１°である、
    　請求項７又は８に記載の成形型。
  10. 　前記凹面は、前記シャフト成形部側に円錐状又は円錐台状に窪んだ面であり、前記凸面は、前記シャフト成形部とは反対側に円錐状又は円錐台状に膨らんだ面である、
    　請求項７～９のいずれか１項に記載の成形型。
  11. （ａ）請求項６～１０のいずれか１項に記載の成形型を用いて、前記円形成形部によって成形される未焼成円板下層と前記シャフト成形部によって成形される未焼成シャフトとがつなぎ目のない状態で一体化された基礎成形体を、モールドキャスト法により作製する工程と、
    （ｂ）前記基礎成形体の前記未焼成円板下層の上面に、前記未焼成円板下層と平行な電極又はその前駆体が形成された未焼成円板上層を積層して最終成形体を得る工程と、
    （ｃ）前記最終成形体を仮焼したあと、前記未焼成円板上層が下、前記未焼成シャフトが上になるように水平支持面に載置した状態で焼成することにより、円板とシャフトとが接合界面のない状態で一体化された半導体製造装置用部材を得る工程と、
    　を含む半導体製造装置用部材の製法。
  12. 　前記工程（ａ）では、前記基礎成形体をモールドキャスト法により作製する際に、前記未焼成円板下層の上面にガス通路を側面に開口するように形成しておき、
    　前記工程（ｂ）では、前記ガス通路の上に、前記未焼成円板上層を接着して最終成形体を得る、
    　請求項１１に記載の半導体製造装置用部材の製法。
PCT/JP2018/040588 2017-11-02 2018-10-31 半導体製造装置用部材、その製法及び成形型 WO2019088203A1 (ja)

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