WO2014141974A1 - 冷却板、その製法及び半導体製造装置用部材 - Google Patents
冷却板、その製法及び半導体製造装置用部材 Download PDFInfo
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- WO2014141974A1 WO2014141974A1 PCT/JP2014/055665 JP2014055665W WO2014141974A1 WO 2014141974 A1 WO2014141974 A1 WO 2014141974A1 JP 2014055665 W JP2014055665 W JP 2014055665W WO 2014141974 A1 WO2014141974 A1 WO 2014141974A1
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- cooling plate
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- F28F3/00—Plate-like or laminated elements; Assemblies of plate-like or laminated elements
- F28F3/12—Elements constructed in the shape of a hollow panel, e.g. with channels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
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- B23K1/00—Soldering, e.g. brazing, or unsoldering
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Definitions
- the present invention relates to a cooling plate, a manufacturing method thereof, and a member for a semiconductor manufacturing apparatus.
- ⁇ Cooling plates are joined to the electrostatic chuck, which is heated during the semiconductor process, for heat dissipation.
- alumina may be used as the material of the electrostatic chuck
- aluminum may be used as the material of the cooling plate
- resin may be used as the bonding material.
- Alumina and aluminum have a very large difference in coefficient of linear thermal expansion.
- the coefficient of linear thermal expansion of alumina is 7.9 ppm / K (RT-800 ° C: Uchida Otsukuru, “Ceramic Physics”).
- the coefficient is 31.1 ppm / K (RT-800 ° C., edited by the Japan Society of Thermophysical Properties, “New Thermophysical Handbook”).
- the cooling plate When metal bonding is used for bonding between the electrostatic chuck and the cooling plate, the cooling plate must have characteristics that the linear thermal expansion coefficient difference from the electrostatic chuck is small and that the thermal conductivity is low in order to maintain heat dissipation. Examples thereof include high density, high density for passing a coolant or a cooling gas, and high strength for enduring processing and installation.
- a composite material disclosed in Patent Document 1 can be given.
- This composite material is a TiC-based Ti—Si—C based composite material having a phase composed of Ti 3 SiC 2 : 1.0 to 20.0 vol%, SiC: 0.5 to 8.0 vol%, and residual TiC. .
- the difference in linear thermal expansion coefficient between TiC and alumina is small, it is considered that the difference in thermal expansion coefficient between Ti—Si—C composite material having TiC group as a main phase and alumina in Patent Document 1 is also small.
- this TiC-based Ti—Si—C based composite material is said to be able to fully utilize the high thermal conductivity of TiC, but in the first place the thermal conductivity of TiC is 31.8 W / mK (Nippon Heat This is only the edition of the Physical Society of Japan, “New Edition Thermophysical Handbook”, Yokendo, March 2008, p.291-294) and is not at a level that can be called high thermal conductivity. Therefore, it cannot be said that the TiC-based Ti—Si—C based composite material also has high thermal conductivity.
- the present invention has been made to solve such problems, and in the cooling plate used for cooling the alumina ceramic member having a refrigerant passage inside, the difference in linear thermal expansion coefficient from alumina is extremely small.
- the main purpose is to provide a material having sufficiently high thermal conductivity, denseness and strength.
- the cooling plate of the present invention is A cooling plate having a refrigerant passage inside and used for cooling an alumina ceramic member, A dense composite material containing 37 to 60% by mass of silicon carbide particles, each containing titanium silicide, titanium silicon carbide and titanium carbide in a smaller amount than the mass% of the silicon carbide particles and having an open porosity of 1% or less.
- each substrate bonded by a metal bonding layer is made of the dense composite material described above.
- This dense composite material has a very small difference in linear thermal expansion coefficient from alumina, and has a sufficiently high thermal conductivity, denseness and strength. For this reason, such a member for a semiconductor manufacturing apparatus in which a cooling plate and an alumina ceramic member are joined does not peel off the cooling plate and the alumina ceramic member even when used repeatedly between a low temperature and a high temperature. While maintaining, the service life is extended.
- TCB Thermal Compression Bonding
- the metal bonding layer employs an aluminum alloy bonding material containing Mg or Si and Mg as the metal bonding material, and at a temperature lower than the solidus temperature of the bonding material. It is preferably formed by hot press bonding. In this way, better cooling performance can be obtained.
- the dense composite material preferably has a mass% of titanium carbide smaller than a mass% of the titanium silicide and a mass% of the titanium silicon carbide.
- the mass% of the titanium silicide is preferably larger than the mass% of the titanium silicon carbide.
- the dense composite material is preferably present in the gap between the silicon carbide particles so that at least one of the titanium silicide, the titanium silicon carbide, and the titanium carbide covers the surface of the silicon carbide particles.
- the titanium carbide is preferably dispersed inside the titanium silicide.
- the titanium silicide is preferably a TiSi 2.
- the dense composite material preferably has a difference in average linear thermal expansion coefficient of 40 to 570 ° C.
- the dense composite material preferably has an average linear thermal expansion coefficient of 40 to 570 ° C. of 7.2 to 8.2 ppm / K.
- the dense composite material preferably has a thermal conductivity of 75 W / mK or more.
- the dense composite material preferably has a four-point bending strength of 200 MPa or more.
- the dense composite material preferably has 16 or more silicon carbide particles having a major axis of 10 ⁇ m or more in an SEM image (reflection electron image) obtained by enlarging a region of 90 ⁇ m in length ⁇ 120 ⁇ m in width by 1000 times.
- the manufacturing method of the cooling plate of the present invention is as follows: A method of manufacturing a cooling plate having a refrigerant passage therein and used for cooling an alumina ceramic member, (A) Dense material containing 37 to 60% by mass of silicon carbide particles, and containing titanium silicide, titanium silicon carbide and titanium carbide in a smaller amount than the mass% of the silicon carbide particles and having an open porosity of 1% or less.
- the above-described cooling plate can be easily manufactured.
- a bonding material of an aluminum alloy containing Mg or containing Si and Mg is adopted as the metal bonding material, and the solidus temperature or lower of the bonding material. It is preferable to perform hot-pressure bonding at a temperature of In this way, a cooling plate with better cooling performance can be obtained.
- the semiconductor manufacturing apparatus member of the present invention is An alumina electrostatic chuck with a built-in electrostatic electrode and heater electrode; Any of the cooling plates described above; A cooling plate-chuck bonding layer formed by hot-pressure bonding a metal bonding material between the surface of the first substrate of the cooling plate and the electrostatic chuck; It is equipped with.
- the cooling plate and the alumina ceramic member are not peeled off, and the service life is extended while maintaining high heat dissipation performance. Further, the heat of the electrostatic chuck can be efficiently released to the cooling plate.
- the cooling plate-chuck bonding layer employs an aluminum alloy bonding material containing Mg or Si and Mg as the metal bonding material, and a solid phase of the bonding material. It is preferably formed by hot-pressure bonding at a temperature below the line temperature.
- FIG. 2 is a cross-sectional view taken along line AA in FIG. 1.
- the two-component phase diagram of Si-Ti. 3 is an SEM image (reflection electron image) of the dense composite material obtained in Experimental Example 2.
- SEM image reflection electron image
- FIG. 1 is a plan view of a member 10 for a semiconductor manufacturing apparatus
- FIG. 2 is a cross-sectional view taken along the line AA in FIG.
- the semiconductor manufacturing apparatus member 10 includes an alumina electrostatic chuck 20 capable of adsorbing a silicon wafer W subjected to plasma processing, and a cooling plate made of a dense composite material having a linear thermal expansion coefficient similar to that of alumina. 30 and a cooling plate-chuck bonding layer 40 for bonding the electrostatic chuck 20 and the cooling plate 30 to each other.
- the electrostatic chuck 20 is a disc-shaped alumina plate whose outer diameter is smaller than the outer diameter of the wafer W, and includes an electrostatic electrode 22 and a heater electrode 24.
- the electrostatic electrode 22 is a planar electrode to which a DC voltage can be applied by an external power source (not shown) via a rod-shaped power supply terminal 23.
- a DC voltage is applied to the electrostatic electrode 22
- the wafer W is attracted and fixed to the wafer mounting surface 20a by a Coulomb force, and when the application of the DC voltage is canceled, the wafer W is released from being fixed to the wafer mounting surface 20a. Is done.
- the heater electrode 24 is patterned, for example, in the manner of a single stroke so as to be wired over the entire surface of the electrostatic chuck 20, and generates heat when a voltage is applied to heat the wafer W.
- a voltage can be applied to the heater electrode 24 by a bar-shaped power supply terminal 25 that reaches one end and the other end of the heater electrode 24 from the back surface of the cooling plate 30.
- the cooling plate 30 is a disk-like plate whose outer diameter is the same as or slightly larger than that of the electrostatic chuck 20, and includes a first substrate 31, a second substrate 32, a third substrate 33, a first substrate 31 and a second substrate. 32, a first metal bonding layer 34 formed between the second substrate 32 and the third metal bonding layer 35 formed between the second substrate 32 and the third substrate 33, a refrigerant passage 36 through which a refrigerant can flow, It has.
- the first to third substrates 31, 32, and 33 are formed of a dense composite material.
- the dense composite material contains 37 to 60% by mass of silicon carbide particles, and contains titanium silicide, titanium silicon carbide and titanium carbide in a smaller amount than the mass% of the silicon carbide particles, respectively, and the open porosity is 1% or less. However, details will be described later.
- the second substrate 32 is formed with a punched portion 32a.
- the punched portion 32 a is formed by punching from one surface of the second substrate 32 to the other surface so as to have the same shape as the coolant passage 36.
- the first and second metal bonding layers 34, 35 are formed between the first substrate 31 and one surface of the second substrate 32, and between the other surface of the second substrate 32 and the third substrate 33.
- Each of the substrates 31 to 33 is formed by hot-pressure bonding with a —Si—Mg-based or Al—Mg-based metal bonding material interposed therebetween.
- the cooling plate 30 has a refrigerant supply hole 46a that extends from a surface opposite to the surface on which the electrostatic chuck 20 is bonded to the inlet 36a and the outlet 36b of the refrigerant passage 36 and extends in a direction orthogonal to the wafer mounting surface 20a.
- a refrigerant discharge hole 46b is formed.
- terminal insertion holes 43 and 45 are formed in the cooling plate 30 so as to penetrate the surface to which the electrostatic chuck 20 is bonded and the opposite surface.
- the terminal insertion hole 43 is a hole for inserting the power supply terminal 23 of the electrostatic electrode 22, and the terminal insertion hole 45 is a hole for inserting the power supply terminal 25 of the heater electrode 24.
- the cooling plate-chuck bonding layer 40 is hot-pressure bonded by sandwiching an Al—Si—Mg-based or Al—Mg-based metal bonding material between the first substrate 31 of the cooling plate 30 and the electrostatic chuck 20. It is formed by.
- the power supply terminals 23 and 25 are configured not to directly contact the cooling plate 30, the first and second metal bonding layers 34 and 35, and the cooling plate-chuck bonding layer 40.
- the semiconductor manufacturing apparatus member 10 has a gas supply hole for supplying He gas to the back surface of the wafer W and a lift pin insertion hole for inserting a lift pin for lifting the wafer W from the wafer mounting surface 20a. You may provide so that the member 10 for semiconductor manufacturing apparatuses may be penetrated in the direction orthogonal to the mounting surface 20a.
- the wafer W is mounted on the wafer mounting surface 20a with the semiconductor manufacturing apparatus member 10 installed in a vacuum chamber (not shown). Then, the inside of the vacuum chamber is reduced by a vacuum pump so as to obtain a predetermined degree of vacuum, a DC voltage is applied to the electrostatic electrode 22 to generate a Coulomb force, and the wafer W is attracted and fixed to the wafer mounting surface 20a. To do. Next, the inside of the vacuum chamber is set to a reactive gas atmosphere at a predetermined pressure (for example, several tens to several hundreds Pa), and plasma is generated in this state. Then, the surface of the wafer W is etched by the generated plasma. A controller (not shown) controls the power supplied to the heater electrode 24 so that the temperature of the wafer W becomes a preset target temperature.
- a predetermined pressure for example, several tens to several hundreds Pa
- FIG. 5A and 5B are explanatory views of the second substrate 32, where FIG. 5A is a plan view and FIG. 5B is a cross-sectional view taken along line BB of FIG.
- the first to third substrates 31 to 33 which are disk-shaped thin plates, are manufactured using the dense composite material described above (see FIG. 3A).
- punching is performed from one surface of the second substrate 32 to the other surface so as to have the same shape as the coolant passage 36, and a punching portion 32a is formed in the second substrate 32 (see FIGS. 3B and 5).
- the punched portion 32a can be formed by a machining center, a water jet, electric discharge machining, or the like.
- the metal bonding material 51 is sandwiched between one surface of the first substrate 31 and the second substrate 32, and the metal bonding material 52 is interposed between the other surface of the second substrate 32 and the third substrate 33.
- the first to third substrates 31 to 32 are hot-press bonded (see FIG. 3D). Thereby, the punched portion 32 a becomes the coolant passage 36, the first metal bonding layer 34 is formed between the first substrate 31 and the second substrate 32, and the first metal bonding layer 34 is formed between the second substrate 32 and the third substrate 33. The two-metal bonding layer 35 is formed, and the cooling plate 30 is completed. At this time, as the metal bonding materials 51 and 52, it is preferable to use an Al—Si—Mg-based or Al—Mg-based bonding material.
- Thermocompression bonding (TCB) using these bonding materials takes 1 to 5 hours at a pressure of 0.5 to 2.0 kg / mm 2 with each substrate heated to a temperature below the solidus temperature in a vacuum atmosphere. And pressurizing. Thereafter, a coolant supply hole 46a extending from the back surface side of the cooling plate 30 to the inlet 36a of the coolant passage 36 and a coolant discharge hole 46b extending from the back surface side of the cooling plate 30 to the outlet 36b of the coolant passage 36 are formed. Terminal insertion holes 43 and 45 penetrating the front and back surfaces of 30 are formed (see FIG. 3E). In FIG. 3E, the inlet 36a and outlet 36b of the refrigerant passage 36, the refrigerant supply hole 46a, and the refrigerant discharge hole 46b are formed. (See Figure 1 for these).
- the electrostatic chuck 20 in which the electrostatic electrode 22 and the heater electrode 24 are embedded and the power supply terminals 23 and 25 are attached is manufactured (see FIG. 4A).
- Such an electrostatic chuck 20 can be prepared in accordance with, for example, the description of JP-A-2006-196864.
- a metal bonding material 28 is sandwiched between the surface of the electrostatic chuck 20 opposite to the wafer mounting surface 20a and the surface of the first substrate 31 of the cooling plate 30, and the power supply terminals 23 and 25 are respectively inserted into the terminal insertion holes.
- the electrostatic chuck 20 and the cooling plate 30 are hot-pressure bonded (see FIG. 4A).
- a cooling plate-chuck bonding layer 40 is formed between the electrostatic chuck 20 and the cooling plate 30 to complete the semiconductor manufacturing apparatus member 10 (see FIG. 4B).
- the metal bonding material 28 it is preferable to perform TCB using an Al—Si—Mg-based or Al—Mg-based bonding material as described above.
- the cooling plate 30 is made of the above-mentioned dense composite material in which the first to third substrates 31 to 33 bonded by the first and second metal bonding layers 34 and 35 are formed.
- This dense composite material has a very small difference in linear thermal expansion coefficient from that of alumina, and has a sufficiently high thermal conductivity, denseness and strength. Therefore, the semiconductor manufacturing apparatus member 10 in which the cooling plate 30 and the electrostatic chuck 20 which is an alumina ceramic member are joined can be used even when the cooling plate 30 and the electrostatic chuck 20 are repeatedly used between a low temperature and a high temperature. As a result, the service life is extended while maintaining high heat dissipation performance.
- first to third substrates 31 to 33 made of the above-mentioned dense composite material are difficult to be joined by electron beam welding or the like, and cooling performance is lowered when joined by a resin adhesive, Since the bonding is performed by TCB using a metal bonding material, bonding can be performed relatively easily, and good cooling performance can be obtained.
- the first to third substrates 31 to 33 are sufficiently dense, the cooling liquid and the cooling gas can be passed through the cooling plate 30, and the cooling efficiency is further improved. Furthermore, since the first to third substrates 31 to 33 have sufficiently high strength, they can withstand processing and bonding when manufacturing the semiconductor manufacturing apparatus member 10, and are resistant to stress caused by temperature changes during use. Can withstand enough.
- FIG. 6 is a cross-sectional view of the semiconductor manufacturing apparatus member 110.
- the semiconductor manufacturing apparatus member 110 includes an electrostatic chuck 20 made of alumina capable of adsorbing a silicon wafer W subjected to plasma processing, and a cooling plate made of a dense composite material having a linear thermal expansion coefficient similar to that of alumina. 130, and a cooling plate-chuck bonding layer 40 for bonding the cooling plate 130 and the electrostatic chuck 20 to each other.
- the cooling plate 130 is a disk-like plate whose outer diameter is the same as or slightly larger than that of the electrostatic chuck 20, and is formed between the first substrate 131, the second substrate 132, and the first substrate 131 and the second substrate 132. And a coolant passage 136 through which the coolant can flow.
- the first and second substrates 131 and 132 are made of the same material as the dense composite material used in the first embodiment.
- the second substrate 132 has a groove serving as a coolant passage 136 on the surface facing the first substrate 131.
- the metal bonding layer 134 is formed by sandwiching an Al—Si—Mg-based or Al—Mg-based metal bonding material between the first substrate 131 and the surface of the second substrate 132 where the groove 132a is provided. , 132 are formed by hot-pressure bonding.
- the cooling plate 130 is formed with a refrigerant supply hole and a refrigerant discharge hole that are connected to the inlet and the outlet of the refrigerant passage 136, respectively. Further, terminal insertion holes 43 and 45 are formed in the cooling plate 130 as in the first embodiment. Since the cooling plate-chuck bonding layer 40 is the same as that of the first embodiment, the description thereof is omitted.
- the usage example of the member 110 for a semiconductor manufacturing apparatus is the same as that of the first embodiment, and thus the description thereof is omitted.
- FIG. 7 is a manufacturing process diagram of the member 110 for a semiconductor manufacturing apparatus
- FIG. 8 is an explanatory view of the second substrate 132
- (a) is a plan view
- (b) is a CC cross-sectional view.
- the first and second substrates 131 and 132 which are disk-shaped thin plates, are manufactured using the dense composite material described above (see FIG. 7A).
- channel 132a used as the refrigerant path 36 is formed in the surface facing the 1st board
- the groove 132a can be formed by a machining center, a water jet, electric discharge machining, or the like.
- the metal bonding material 61 is sandwiched between the first substrate 131 and the surface of the second substrate 132 where the groove 132a is formed (see FIG. 7C), and the first and second substrates 131 and 132 are heated. Pressure bonding is performed (see FIG. 7D).
- the groove 132a becomes the coolant passage 136
- the metal bonding layer 134 is formed between the first substrate 131 and the second substrate 132, and the cooling plate 130 is completed.
- the first and second substrates 131 and 132 joined by the metal joining layer 134 are made of the dense composite material described above.
- the composite material has a very small difference in linear thermal expansion coefficient from alumina, and has sufficiently high thermal conductivity, denseness and strength. Therefore, the semiconductor manufacturing apparatus member 110 in which the cooling plate 130 and the electrostatic chuck 20 which is an alumina ceramic member are joined can be used even when the cooling plate 130 and the electrostatic chuck 20 are repeatedly used between a low temperature and a high temperature. As a result, the service life is extended while maintaining high heat dissipation performance.
- first and second substrates 131 and 132 made of the above-described dense composite material are difficult to be joined by electron beam welding or the like, and if they are joined with a resin adhesive, the cooling performance is lowered. Since the bonding is performed by TCB using a metal bonding material, bonding can be performed relatively easily, and good cooling performance can be obtained.
- first and second substrates 131 and 132 are sufficiently dense, the cooling liquid and the cooling gas can be passed through the cooling plate 130, and the cooling efficiency is further improved. Furthermore, since the first and second substrates 131 and 132 have sufficiently high strength, they can withstand the processing and joining when manufacturing the semiconductor manufacturing apparatus member 110, and are resistant to stress caused by temperature changes during use. Can withstand enough.
- the dense composite material used in the above-described embodiment contains 37 to 60% by mass of silicon carbide particles, and contains titanium silicide, titanium silicon carbide and titanium carbide in amounts less than the mass% of the silicon carbide particles, respectively.
- the porosity is 1% or less.
- the open porosity is a value measured by the Archimedes method using pure water as a medium.
- Silicon carbide particles are contained in an amount of 37 to 60% by mass.
- the X-ray diffraction pattern of the composite material was obtained and the content was determined by simple quantification using data analysis software.
- silicon carbide particles are contained in an amount of less than 37% by mass, it is not preferable because the thermal conductivity cannot be sufficiently increased.
- the open porosity is increased and the strength is not sufficiently increased.
- the silicon carbide particles preferably have 16 or more silicon carbide particles having a major axis of 10 ⁇ m or more in an SEM image (reflected electron image) obtained by enlarging a dense 90 ⁇ m ⁇ 120 ⁇ m region 1000 times. . This is because the composite material is sufficiently sintered and sufficiently densified.
- Titanium silicide, titanium silicon carbide, and titanium carbide are contained in a smaller amount than the mass% of the silicon carbide particles.
- titanium silicide include TiSi 2 , TiSi, Ti 5 Si 4 , and Ti 5 Si 3, and among these, TiSi 2 is preferable.
- the titanium silicon carbide is preferably Ti 3 SiC 2 (TSC), and the titanium carbide is preferably TiC.
- TSC Ti 3 SiC 2
- the mass% of titanium carbide is preferably smaller than the mass% of titanium silicide and the mass% of titanium silicon carbide.
- the mass% of titanium silicide is preferably larger than the mass% of titanium silicon carbide.
- the mass% is the largest for silicon carbide, and decreases in the order of titanium silicide, titanium silicon carbide, and titanium carbide.
- the mass% is the largest for silicon carbide, and decreases in the order of titanium silicide, titanium silicon carbide, and titanium carbide.
- 37 to 60% by mass of silicon carbide, 31 to 41% by mass of titanium silicide, 5 to 25% by mass of titanium silicon carbide, and 1 to 4% by mass of titanium carbide may be used.
- At least one of titanium silicide, titanium silicon carbide, and titanium carbide exists in the gap between the silicon carbide particles so as to cover the surface of the silicon carbide particles.
- the silicon carbide particles are dispersed at a high frequency, pores are likely to remain between the silicon carbide particles. However, if the silicon carbide particle surface is covered with other particles as described above, the pores are easily filled. It is preferable because it tends to be a dense and high-strength material.
- the titanium carbide is preferably present so as to be dispersed inside the titanium silicide phase. In the structure of the composite material shown in the SEM image of FIG.
- titanium carbide is dispersed inside the large titanium silicide domain.
- the titanium silicide domain is large, the domain itself becomes a source of destruction and there is a concern about the strength reduction of the composite material, but by dispersing titanium carbide inside the titanium silicide, the effect of supplementing the strength of the titanium silicide phase is achieved, It is considered that high strength is maintained as a composite material.
- the dense composite material used in the above-described embodiment has a linear thermal expansion coefficient comparable to that of alumina. Therefore, when a member made of the dense composite material of the present invention and a member made of alumina are joined (for example, metal joining), even if they are repeatedly used between a low temperature and a high temperature, they are hardly peeled off.
- the dense composite material of the present invention preferably has a difference in average linear thermal expansion coefficient of 40 to 570 ° C. from that of alumina of 0.5 ppm / K or less. More specifically, the average linear thermal expansion coefficient at 40 to 570 ° C. of the dense composite material of the present invention is preferably 7.2 to 8.2 ppm / K.
- the average linear thermal expansion coefficient at 40 to 570 ° C. of a dense alumina sintered body obtained by hot press firing an alumina raw material with a purity of 99.99% or higher was measured under the same conditions as those for the dense composite material of the present invention. 0.7 ppm / K.
- the dense composite material used in the above-described embodiment is excellent in thermal conductivity, but specifically, the thermal conductivity is preferably 75 W / mK or more.
- the dense composite material used in the above-described embodiment is excellent in strength, but specifically, the four-point bending strength is preferably 200 MPa or more. If it carries out like this, it will become easy to apply the member produced with this dense composite material to a cooling plate etc.
- the manufacturing method of the dense composite material used in the above-described embodiment is selected so that (a) 39 to 51% by mass of silicon carbide raw material particles having an average particle diameter of 10 ⁇ m to 25 ⁇ m are contained, and Ti and Si are included. Producing a powder mixture having a mass ratio of Si / (Si + Ti) of 0.26 to 0.54 with respect to Si and Ti derived from the raw material excluding silicon carbide, comprising at least one raw material formed; (B) sintering the powder mixture at 1370 to 1460 ° C. by hot pressing under an inert atmosphere.
- the average particle diameter of the SiC raw material when the average particle diameter of the SiC raw material is less than 10 ⁇ m, the surface area of the SiC particles becomes too large, resulting in insufficient densification, and the open porosity may not be 1% or less. Therefore, it is not preferable.
- the average particle size of the SiC raw material when the average particle size of the SiC raw material is increased, the surface area of the SiC particles is decreased, so that the density is improved.
- the average particle size is excessively increased, the strength may be insufficient. Since the particle size of the SiC particles shown in the SEM image of FIG. 10 to be described later is about 25 ⁇ m at the maximum, it is not necessary to use raw material particles having an average particle size exceeding 25 ⁇ m.
- the silicon carbide raw material particles in the powder mixture are less than 39% by mass, the resulting composite material may not be sufficiently high in thermal conductivity, which is not preferable. Moreover, when it exceeds 51 mass%, since the obtained composite material becomes insufficiently densified and there exists a possibility that an open porosity may exceed 1%, it is not preferable.
- the one or more raw materials selected to include Ti and Si include, for example, a combination of metal Ti and metal Si, a combination of metal Ti, metal Si, and titanium disilicide, and metal Ti and titanium disilicide. And titanium disilicide alone.
- the mass ratio of Si / (Si + Ti) is less than 0.26, the amount of liquid phase components generated at 1330 ° C.
- the mass ratio of Si / (Si + Ti) exceeds 0.54, the amount of the liquid phase component increases, so that the same problem is likely to occur.
- the mass ratio of Si / (Si + Ti) is more preferably 0.29 to 0.47.
- examples of the inert atmosphere include a vacuum atmosphere, an argon gas atmosphere, a helium atmosphere, and a nitrogen atmosphere.
- the press pressure at the time of hot press firing is not particularly limited, but is preferably set to 50 to 300 kgf / cm 2 .
- the temperature during the hot press firing is 1370 to 1460 ° C. When fired at a temperature lower than 1370 ° C., the resulting composite material is insufficiently densified, and the open porosity may exceed 1%, which is not preferable. Baking at a temperature exceeding 1460 ° C. is not preferable because the liquid phase component oozes out and it is difficult to obtain a dense composite material having an open porosity of 1% or less.
- the firing time may be appropriately set according to the firing conditions, but may be appropriately set, for example, between 1 and 10 hours.
- the semiconductor manufacturing apparatus member 10 of the embodiment is an alumina coulomb type as the electrostatic chuck 20, and has a diameter of 297 mm, a thickness of 5 mm, and a dielectric film thickness (from the electrostatic electrode 22 to the wafer mounting surface 20a). Thickness) is 0.35 mm, and the heater electrode 24 is an Nb coil. Further, as the cooling plate 30, first to third substrates 31 to 33 made of dense materials of Experimental Example 10 to be described later are made of Al—Si—Mg based bonding material (88.5 wt% Al, 10 wt%). Of Si, 1.5 wt% Mg, and the solidus temperature was about 560 ° C.).
- TCB was performed by pressurizing each substrate at a pressure of 1.5 kg / mm 2 over 5 hours in a vacuum atmosphere while being heated to 540 to 560 ° C.
- the obtained cooling plate 30 had a diameter of 340 mm and a thickness of 32 mm.
- the electrostatic chuck 20 and the cooling plate 30 were also joined by TCB using the same joining material.
- the thickness of the cooling plate-chuck bonding layer 40 was 0.12 mm.
- the member for the semiconductor manufacturing apparatus of the comparative example is the same as the above-described example except that a cooling plate in which the first to third substrates made of aluminum are joined by acrylic resin (thermal conductivity 0.2 W / mK) is used. It produced similarly.
- pure water (refrigerant) having a temperature of 25 ° C. is flowed through the refrigerant passage 36 of the cooling plate 30 of the semiconductor manufacturing apparatus member 10 of the embodiment at a flow rate of 13 L / min, and predetermined power is supplied to the heater electrode 24 to thereby form the heater electrode.
- the temperature of the wafer mounting surface 20a when 24 was heated was monitored with a surface thermometer.
- the semiconductor manufacturing apparatus member of the comparative example was monitored in the same manner. The results are shown in Table 1. From Table 1, it can be seen that the cooling performance of the example is superior to that of the comparative example regardless of the input power.
- the suitable application example of the dense composite material used by embodiment mentioned above is demonstrated.
- SiC raw material a commercial product having a purity of 97% or more and an average particle diameter of 15.5 ⁇ m or 6.9 ⁇ m was used.
- the metal Si raw material a commercial product having a purity of 97% or more and an average particle diameter of 9.0 ⁇ m was used.
- metal Ti raw material a commercial product having a purity of 99.5% or more and an average particle diameter of 31.1 ⁇ m was used.
- titanium disilicide a commercially available product having a purity of 99% or more and an average particle diameter of 6.9 ⁇ m was used.
- the blended powder was uniaxially pressed at a pressure of 200 kgf / cm 2 to produce a disk-shaped molded body having a diameter of about 50 mm and a thickness of about 17 mm, and stored in a firing graphite mold.
- -Firing A dense sintered material was obtained by subjecting the disk-shaped compact to hot press firing.
- the press pressure was 200 kgf / cm 2
- firing was performed at the firing temperature (maximum temperature) shown in Tables 2 and 3, and a vacuum atmosphere was maintained until the end of firing.
- the holding time at the firing temperature was 4 hours.
- the simple profile fitting function (FPM Eval.) Of the powder diffraction data analysis software “EVA” manufactured by Bruker AXS was used. This function calculates the component phase quantity ratio using I / Icor (intensity ratio to corundum diffraction intensity) of the qualitative crystalline phase ICDD PDF card.
- the PDF card number of each crystal phase is SiC: 00-049-1428, TiSi2: 01-071-0187, TSC: 01-070-6297, TiC: 01-070-9258 (TiC0.62), Si: 00- 027-1402 was used.
- an alumina standard sample (purity 99.7%, bulk density 3.9 g / cm 3 , length 20 mm) attached to the apparatus was used.
- Another alumina standard sample was prepared, and the value obtained by measuring the linear thermal expansion coefficient under the same conditions was 7.7 ppm / K.
- SEM observation SEM observation of the dense composite material was performed. In the SEM observation, a cross section of the dense composite material was observed with a reflected electron image by an electron microscope (SEM; XL30 manufactured by Philips). The reflected electron image was observed under the conditions of an acceleration voltage of 20 kV and a spot size of 4.
- Experimental examples 8 to 14 the powder mixture in which the raw materials were mixed so that the value of Si / (Si + Ti) was 0.342 was hot-press fired at the temperature shown in Table 2.
- a SiC raw material having an average particle diameter of 15.5 ⁇ m was used.
- the firing temperature is 1370 to 1460 ° C.
- the open porosity is 1% or less
- the 4-point bending strength and the thermal conductivity are sufficiently high
- the difference in linear thermal expansion coefficient from alumina is 0.
- a dense composite material of 5 ppm / K or less was obtained (Experimental Examples 9 to 12, 14).
- Example 16 Dense composite materials within 5 ppm / K were obtained (Experimental Examples 16-19, 22-25, 27). However, when the firing temperature was 1480 ° C., bleeding occurred during hot press firing, and the resulting composite material had an open porosity exceeding 1% and lacked denseness (Experimental Example 15, 21). Further, even when the firing temperature was 1350 ° C., a non-dense composite material having an open porosity exceeding 1% was obtained (Experimental Examples 20 and 26). In Example 27, different raw materials were used, but good dense composite materials equivalent to those in Examples 22 to 25 were obtained.
- Experimental examples 30 to 35 In Experimental Examples 30 to 35, the powder mixture in which the raw materials were mixed so that the value of Si / (Si + Ti) was 0.468 was hot-press fired at the temperature shown in Table 3. A SiC raw material having an average particle diameter of 15.5 ⁇ m was used. As a result, when the firing temperature is 1370 to 1460 ° C., the open porosity is 1% or less, the 4-point bending strength and the thermal conductivity are sufficiently high, and the difference in linear thermal expansion coefficient from alumina is 0. A dense composite material within 5 ppm / K was obtained (Experimental Examples 31 to 34).
- the average particle diameter of a SiC raw material is 10 micrometers or more and 25 micrometers or less in order to obtain a dense composite material.
- the average particle size of the SiC raw material is less than 10 ⁇ m, the ratio of SiC particles having a small particle size increases, so that the surface area of the SiC particles becomes too large, resulting in insufficient densification, and the open porosity is reduced to 1% or less.
- the average particle size of the SiC particles after firing is slightly smaller than the average particle size of the SiC raw material.
- the average particle size of the SiC raw material When the average particle size of the SiC raw material is increased, the surface area of the SiC particles is decreased and the denseness is improved. However, when the average particle size is excessively increased, the strength may be insufficient. Since the particle size of the SiC particles shown in the SEM image of FIG. 10 to be described later is about 25 ⁇ m at the maximum, it is not necessary to use raw material particles having an average particle size exceeding 25 ⁇ m.
- FIG. 9 shows a two-component phase diagram of Si—Ti with respect to the mass ratio of b shown in Tables 2 and 3, that is, Si / (Si + Ti).
- Si / (Si + Ti) coincides with the horizontal axis on the upper side of the state diagram.
- the value of Si / (Si + Ti) is preferably in the appropriate range of 0.26 to 0.54 (26 wt% to 54 wt% on the upper horizontal axis in FIG. 9).
- titanium silicide represented by chemical formulas of TiSi 2 , TiSi, Ti 5 Si 4 , and Ti 5 Si 3 is formed at an arbitrary ratio during firing. Therefore, titanium disilicide, titanium silicon carbide, and titanium carbide (TiCx) are generated by the reaction between the titanium silicide and the surface of the SiC particles.
- FIG. 10 is a photograph of the reflection electron image of Experimental Example 2. This photograph is an SEM image (reflected electron image) obtained by enlarging an area of 90 ⁇ m in length and 120 ⁇ m in width by 1000 times after the cross-section polishing of the dense composite material.
- the dark gray particles are SiC particles
- the gray structure between the SiC particles is TiSi 2
- the light gray structure between the SiC particles is TSC
- the columnar structure dispersed in TiSi 2 is TiC (the brightness is TSC).
- FIG. 10 shows that the surface of the SiC particle is covered with at least one of TSC, TiSi 2 , and TiC. From FIG.
- the major axis (the maximum diameter of the particles) was determined for each SiC particle whose entire shape was within the range of the visual field.
- the number of SiC particles having a major axis of 10 ⁇ m or more was 34.
- a photograph of a backscattered electron image was taken for a dense composite material suitable for use in the above-described embodiment, and the number of SiC particles having a major axis of 10 ⁇ m or more was determined. Tables 2 and 3 As shown in FIG.
- the cooling plate of the present invention is used, for example, as a cooling plate that is metal-bonded to an electrostatic chuck or susceptor made of alumina.
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Abstract
Description
内部に冷媒通路を有し、アルミナセラミック部材の冷却に用いられる冷却板であって、
炭化珪素粒子を37~60質量%含有すると共に、珪化チタン、チタンシリコンカーバイド及び炭化チタンをそれぞれ前記炭化珪素粒子の質量%より少量含有し、開気孔率が1%以下である緻密質複合材料で作製された第1基板と、
前記緻密質複合材料で作製され、前記冷媒通路と同じ形状となるように打ち抜かれた打ち抜き部を有する第2基板と、
前記緻密質複合材料で作製された第3基板と、
前記第1基板と前記第2基板との間に金属接合材を挟んで両基板を熱圧接合することにより両基板間に形成された第1金属接合層と、
前記第2基板と前記第3基板との間に金属接合材を挟んで両基板を熱圧接合することにより両基板間に形成された第2金属接合層と、
を備えたものであるか、
又は、
炭化珪素粒子を37~60質量%含有すると共に、珪化チタン、チタンシリコンカーバイド及び炭化チタンをそれぞれ前記炭化珪素粒子の質量%より少量含有し、開気孔率が1%以下である緻密質複合材料で作製された第1基板と、
前記緻密質複合材料で作製され、前記第1基板と向かい合う面に前記冷媒通路となる溝を有する第2基板と、
前記第1基板と前記第2基板のうち前記溝が設けられた面との間に金属接合材を挟んで両基板を熱圧接合することにより形成された金属接合層と、
を備えたものである。
内部に冷媒通路を有し、アルミナセラミック部材の冷却に用いられる冷却板を製造する方法であって、
(a)炭化珪素粒子を37~60質量%含有すると共に、珪化チタン、チタンシリコンカーバイド及び炭化チタンをそれぞれ前記炭化珪素粒子の質量%より少量含有し、開気孔率が1%以下である緻密質複合材料を用いて、第1~第3基板を作製する工程と、
(b)前記第2基板の一方の面から他方の面まで前記冷媒通路と同じ形状となるように打ち抜いて前記第2基板に打ち抜き部を形成する工程と、
(c)前記第1基板と前記第2基板の一方の面との間および前記第3基板と前記第2基板の他方の面との間にそれぞれ金属接合材を挟んで前記第1~第3基板を熱圧接合する工程と、
を含むものであるか、
又は、
(a)炭化珪素粒子を37~60質量%含有すると共に、珪化チタン、チタンシリコンカーバイド及び炭化チタンをそれぞれ前記炭化珪素粒子の質量%より少量含有し、開気孔率が1%以下である緻密質複合材料を用いて、第1基板及び第2基板を作製する工程と、
(b)前記第2基板の一方の面に前記冷媒通路となる溝を形成する工程と、
(c)前記第1基板と前記第2基板のうち前記溝が設けられた面との間に金属接合材を挟んで両基板を熱圧接合する工程と、
を含むものである。
静電電極及びヒータ電極を内蔵したアルミナ製の静電チャックと、
上述したいずれかの冷却板と、
前記冷却板の前記第1基板の表面と前記静電チャックとの間に金属接合材を挟んで両者を熱圧接合することにより形成された冷却板-チャック接合層と、
を備えたものである。
以下に、第1実施形態の半導体製造装置用部材10について説明する。図1は半導体製造装置用部材10の平面図、図2は図1のA-A断面図である。
以下に、第2実施形態の半導体製造装置用部材110について説明する。図6は半導体製造装置用部材110の断面図である。
上述した実施形態で使用する緻密質複合材料は、炭化珪素粒子を37~60質量%含有すると共に、珪化チタン、チタンシリコンカーバイド及び炭化チタンをそれぞれ前記炭化珪素粒子の質量%より少量含有し、開気孔率が1%以下のものである。ここでは、開気孔率は、純水を媒体としたアルキメデス法により測定した値とする。
実施例の半導体製造装置用部材10は、静電チャック20として、アルミナ製のクーロンタイプで、直径が297mm、厚み5がmm、誘電体膜厚(静電電極22からウエハ載置面20aまでの厚み)が0.35mm、ヒータ電極24がNbコイルのものを用いた。また、冷却板30として、後述する実験例10の緻密質材料で作製した第1~第3基板31~33を、Al-Si-Mg系接合材(88.5重量%のAl、10重量%のSi、1.5重量%のMgを含有し、固相線温度が約560℃)を用いてTCBにより接合した。TCBは、真空雰囲気下、540~560℃に加熱した状態で各基板を1.5kg/mm2 の圧力で5時間かけて加圧することにより行った。得られた冷却板30は、直径が340mm、厚みが32mmであった。静電チャック20と冷却板30との接合も、同じ接合材を用いてTCBにより行った。冷却板-チャック接合層40の厚みは0.12mmであった。一方、比較例の半導体製造装置用部材は、アルミニウム製の第1~第3基板をアクリル樹脂(熱伝導率0.2W/mK)により接合した冷却板を用いた以外は、上述した実施例と同様にして作製した。
以下に、上述した実施形態で使用する緻密質複合材料の好適な適用例について説明する。SiC原料は、純度97%以上、平均粒径15.5μm或いは、6.9μmの市販品を使用した。平均粒径10.1μmのSiC原料(実験例28)は、平均粒径15.5μmと6.9μmのSiC原料を1:1で混合することにより調整した。金属Si原料は、純度97%以上、平均粒径9.0μmの市販品を使用した。金属Ti原料は、純度99.5%以上、平均粒径31.1μmの市販品を使用した。二珪化チタンは、純度99%以上、平均粒径6.9μmの市販品を使用した。
・調合
SiC原料、金属Si原料、金属Ti原料及び二珪化チタン原料を、表2及び表3に示す質量%となるように秤量し、イソプロピルアルコールを溶媒とし、ナイロン製のポット、直径10mmの鉄芯入りナイロンボールを用いて4時間湿式混合した。混合後スラリーを取り出し、窒素気流中110℃で乾燥した。その後、30メッシュの篩に通し、調合粉末とした。尚、秤量した原料約500gを高速流動混合機(粉体投入部の容量1.8L)に投入し、攪拌羽根の回転数1500rpmで混合した場合にも湿式混合と同様の材料特性が得られることを確認した。
・成形
調合粉末を、200kgf/cm2の圧力で一軸加圧成形し、直径50mm、厚さ17mm程度の円盤状成形体を作製し、焼成用黒鉛モールドに収納した。
・焼成
円盤状成形体をホットプレス焼成することにより緻密質焼結材料を得た。ホットプレス焼成では、プレス圧力を200kgf/cm2とし、表2及び表3に示す焼成温度(最高温度)で焼成し、焼成終了まで真空雰囲気とした。焼成温度での保持時間は4時間とした。
表2及び表3には、a:各実験例の出発原料組成(質量比)、b:原料中、SiCを除いたSi,Ti,TiSi2に由来する、Si,Tiの総量に対するSiの質量比(Si/(Si+Ti))、c:原料SiCの平均粒径、d:ホットプレス焼成温度、e:焼成時の液相の染み出しの有無、f:緻密質複合材料の縦90μm×横120μmの領域を1000倍に拡大したSEM像(反射電子像)における長径10μm以上のSiC粒子の数、g:XRD測定結果から求めた複合材料の構成相とその量比(簡易定量結果)、h:複合材料の基本特性(開気孔率、嵩密度、4点曲げ強度、線熱膨張係数、熱伝導率)を示した。なお、実験例1~44のうち、実験例2~5,7,9~12,14,16~19,22~25,27,28,31~34,43が上述した実施形態で使用するのに適した緻密質複合材料であり、残りは適さない材料である。
複合材料を乳鉢で粉砕し、X線回折装置により結晶相を同定した。測定条件はCuKα,40kV,40mA,2θ=5~70°とし、封入管式X線回折装置(ブルカー・エイエックスエス製 D8 ADVANCE)を使用した。また、構成相の簡易定量を行った。この簡易定量は、複合材料に含まれる結晶相の含有量をX線回折のピークに基づいて求めた。ここでは、SiC、TiSi2、TSC(Ti3SiC2)、TiCおよびSiに分けて簡易定量を行い含有量を求めた。簡易定量には、ブルカー・エイエックスエス社の粉末回折データ解析用ソフトウェア「EVA」の簡易プロファイルフィッティング機能(FPM Eval.)を利用した。本機能は定性した結晶相のICDD PDFカードのI/Icor(コランダムの回折強度に 対する強度比)を用いて構成相の量比を算出するものである。各結晶相のPDFカード番号は、SiC:00-049-1428、TiSi2:01-071-0187、TSC: 01-070-6397、TiC:01-070-9258(TiC0.62)、Si:00-027-1402を用いた。
(1)平均粒径
日機装株式会社製、マイクロトラックMT3300EXを使用し、純水を分散媒として測定した。
(2)開気孔率及び嵩密度
純水を媒体としたアルキメデス法により測定した。
(3)4点曲げ強度
JIS-R1601に従って求めた。
(4)線熱膨張係数(40~570℃の平均線熱膨張係数)
ブルカーエイエックスエス(株)製、TD5020S(横型示差膨張測定方式)を使用し、アルゴン雰囲気中、昇温速度20℃/分の条件で650℃まで2回昇温し、2回目の測定データから40~570℃の平均線熱膨張計数を算出した。標準試料には装置付属のアルミナ標準試料(純度99.7%、嵩密度3.9g/cm3、長さ20mm)を使用した。このアルミナ標準試料をもう1本用意し、同一条件で線熱膨張係数を測定した値は7.7ppm/Kであった。
(5)熱伝導率
レーザーフラッシュ法により測定した。
(6)SEM観察
緻密質複合材料のSEM観察を行った。SEM観察では、緻密質複合材料の断面を電子顕微鏡(SEM;フィリップス社製XL30)により反射電子像で観察した。反射電子像の観察は、加速電圧20kV、スポットサイズ4の条件で行った。
(1)実験例1~7
実験例1~7では、Si/(Si+Ti)の値が0.298となるように原料を混合した粉体混合物を、表2に記載の温度でホットプレス焼成した。SiC原料は平均粒径15.5μmのものを用いた。その結果、焼成温度を1370~1460℃とした場合には、開気孔率が1%以下であり、4点曲げ強度や熱伝導率が十分高く、アルミナとの線熱膨張係数の差が0.5ppm/K以内の緻密質複合材料が得られた(実験例2~5,7)。しかし、焼成温度を1480℃とした場合には、ホットプレス焼成時に染み出しが発生し、得られた複合材料は開気孔率が1%を超え、緻密性に欠けるものだった(実験例1)。また、焼成温度を1350℃とした場合にも、開気孔率が1%を超える非緻密性の複合材料が得られた(実験例6)。なお、染み出しとは、高温下で生じる液相又は気相成分が焼成治具の隙間からはみ出した状態で焼結することである。染み出しの発生は、焼成した材料の組成ずれや緻密化不足の原因となる他、焼成治具の腐食、磨耗に繋がるため好ましくない。
実験例8~14では、Si/(Si+Ti)の値が0.342となるように原料を混合した粉体混合物を、表2に記載の温度でホットプレス焼成した。SiC原料は平均粒径15.5μmのものを用いた。その結果、焼成温度を1370~1460℃とした場合には、開気孔率が1%以下であり、4点曲げ強度や熱伝導率が十分高く、アルミナとの線熱膨張係数の差が0.5ppm/K以内の緻密質複合材料が得られた(実験例9~12,14)。しかし、焼成温度を1480℃とした場合には、ホットプレス焼成時に染み出しが発生し、得られた複合材料は開気孔率が1%を超え、緻密性に欠けるものだった(実験例8)。また、焼成温度を1350℃とした場合にも、開気孔率が1%を超える非緻密性の複合材料が得られた(実験例13)。
実験例15~27では、Si/(Si+Ti)の値が0.396となるように原料を混合した粉体混合物を、表2に記載の温度でホットプレス焼成した。SiC原料は平均粒径15.5μmのものを用いた。なお、実験例15~26では原料としてSiC,金属Si及び金属Tiを用いたが、実験例27では原料としてSiC,金属Ti及びTiSi2を用いた。その結果、焼成温度を1370~1460℃とした場合には、開気孔率が1%以下であり、4点曲げ強度や熱伝導率が十分高く、アルミナとの線熱膨張係数の差が0.5ppm/K以内の緻密質複合材料が得られた(実験例16~19、22~25、27)。しかし、焼成温度を1480℃とした場合には、ホットプレス焼成時に染み出しが発生し、得られた複合材料は開気孔率が1%を超え、緻密性に欠けるものだった(実験例15,21)。また、焼成温度を1350℃とした場合にも、開気孔率が1%を超える非緻密性の複合材料が得られた(実験例20,26)。なお、実験例27では、異なる原料を用いたが、実験例22~25と同等の良好な緻密質複合材料が得られた。
実験例28では、表3に示すように、平均粒径15.5μmと6.9μmのSiC原料を1:1で混合し、平均粒径10.1μmとしたSiC原料を用い、Si/(Si+Ti)の値が0.396となるように原料を混合した粉体混合物を、1430℃でホットプレス焼成した。その結果、開気孔率が1%以下であり、4点曲げ強度や熱伝導率が十分高く、アルミナとの線熱膨張係数の差が0.5ppm/K以内の緻密質複合材料が得られた。一方、実験例29では、表3に示すように、平均粒径6.9μmのSiCを用い、Si/(Si+Ti)の値が0.396となるように原料を混合した粉体混合物を、1430℃でホットプレス焼成した。その結果、開気孔率が1%を超える非緻密性の複合材料が得られた。こうしたことから、緻密質複合材料を得るには、SiC原料の平均粒径を10μm以上とすべきことがわかった。
実験例30~35では、Si/(Si+Ti)の値が0.468となるように原料を混合した粉体混合物を、表3に記載の温度でホットプレス焼成した。SiC原料は平均粒径15.5μmのものを用いた。その結果、焼成温度を1370~1460℃とした場合には、開気孔率が1%以下であり、4点曲げ強度や熱伝導率が十分高く、アルミナとの線熱膨張係数の差が0.5ppm/K以内の緻密質複合材料が得られた(実験例31~34)。しかし、焼成温度を1480℃とした場合には、ホットプレス焼成時に染み出しが発生し、得られた複合材料は開気孔率が1%を超え、緻密性に欠けるものだった(実験例30)。また、焼成温度を1350℃とした場合にも、得られた複合材料は開気孔率が1%を超える非緻密性のものだった(実験例35)。
実験例36~41では、表3に示すように、Si/(Si+Ti)の値が0.54を超えるように原料を混合した粉体混合物を、それぞれ異なる温度でホットプレス焼成した。SiC原料は平均粒径15.5μmのものを用いた。その結果、1350℃以上でホットプレス焼成した場合には、焼成時に染み出しが発生した。また、実験例38を除き、開気孔率が1%を超える非緻密性の複合材料が得られた。これらの複合材料は、構成相としてTiCを含んでおらず、代わりにSiを含むものがあった。更に、4点曲げ強度も概して低かった。また、実験例37と上記の実験例35を比較すると、いずれも高気孔率であったが、構成相としてTiCを含む実験例35の方が曲げ強度が高かった。これは、TiCが珪化チタン内部に分散する為に高強度化しているものと考えられた。
実験例42~44及び実験例17,23では、表3に示すように、Si/(Si+Ti)の値が0.396となるように原料を混合した粉体混合物を、1430℃でホットプレス焼成した。但し、原料として用いたSiC、金属Si及び金属Tiの質量%はそれぞれ異なる値になるようにした。その結果、SiC原料が59質量%を超えた場合には、複合材料中のSiC粒子が60質量%を超え、4点曲げ強度や熱伝導率は十分高い複合材料が得られたが、開気孔率が1%を超える非緻密性の材料となり、アルミナとの線熱膨張係数差が0.5ppm/Kを超えた(実験例42)。一方、SiC原料が30質量%未満の場合には、複合材料中のSiC粒子が37質量%未満となり、熱伝導率が十分高い値にならなかった(実験例44)。これに対して、SiC原料の質量%が適正な範囲の場合には、開気孔率が1%以下であり、4点曲げ強度や熱伝導率が十分高く、アルミナとの線熱膨張係数の差が0.5ppm/K以内の緻密質複合材料が得られた(実験例43,17,23)。
実験例2~5,7,9~12,14,16~19,22~25,27,28,31~34,43で得られた緻密質複合材料は、アルミナとの線熱膨張係数の差が0.5ppm/K以内であり、熱伝導率、緻密性及び強度が十分高かった。このため、こうした緻密質複合材料からなる第1材と、アルミナからなる第2材とを金属接合した半導体製造装置用部材は、低温と高温との間で繰り返し使用されたとしても、第1材と第2材とが剥がれることがないため、耐用期間が長くなる。なお、これらの実験例をみると、緻密質複合材料を得るための原料組成のSiCは39~51質量%の範囲に入り、緻密質複合材料中のSiC粒子は37~60質量%の範囲に入る。
(1)SiC原料の平均粒径について
緻密質複合材料を得るうえで、SiC原料の平均粒径が10μm以上25μm以下であることが好ましいことがわかった。SiC原料の平均粒径が10μm未満の場合には、粒径の小さなSiC粒子の比率が高まるために、SiC粒子の表面積が大きくなりすぎて緻密化不足になり、開気孔率を1%以下にすることができないおそれがある(実験例29)。なお、SiCは骨材であり、SiCの表面において他の成分と反応するため、焼成後のSiC粒子の平均粒径はSiC原料の平均粒径よりわずかに小さくなる。SiC原料の平均粒径が大きくなる場合、SiC粒子の表面積は小さくなるので緻密性は向上するが、大きくなり過ぎる場合には強度が不足する恐れがある。後出の図10のSEM像に示されるSiC粒子の粒径は、最大でも25μm程度であるから、あえて平均粒径25μmを超える原料粒子を用いる必要はない。
緻密質複合材料を得るうえで、構成相としてSiC粒子を37~60質量%含有すると共に、TiSi2、TSC及びTiCをそれぞれSiCの質量%より少量含有していることが必須であった。SiC粒子が60質量%を超えた場合には、開気孔率が1%を超える非緻密性の材料となり、アルミナとの線熱膨張係数差が0.5ppm/K以上の複合材料が得られた(実験例42)。また、SiC粒子が37質量%未満の場合には、熱伝導率が十分高い値にならなかった(実験例44)。
表2,3に示したbの質量比つまりSi/(Si+Ti)に関して、Si-Tiの2成分状態図を図9に示す。Si/(Si+Ti)は状態図の上側の横軸と一致する。Si/(Si+Ti)の値は適正範囲0.26~0.54(図9の上側の横軸で26wt%~54wt%)に入ることが好ましい。この適正範囲に入る場合、焼成中にTiSi2,TiSi,Ti5Si4,Ti5Si3の化学式で表される珪化チタンが任意の比率で生成する。そのため、これらの珪化チタンとSiC粒子の表面とが反応することで二珪化チタン、チタンシリコンカーバイド、チタンカーバイド(TiCx)が生成する。
焼成温度が1460℃を超えた場合には、原料組成が適正であっても、開気孔率が1%を超えてしまい、緻密化しなかった(実験例1,8,15,21,30)。これは、ホットプレス焼成時に染み出しが発生したためと思われる。一方、焼成温度が1370℃未満だった場合には、原料組成が適正であっても、やはり開気孔率が1%を超えてしまい、緻密化しなかった((実験例6,13,20,26,35)。このため、焼成温度は1370~1460℃が好適であることがわかった。
図10は、実験例2の反射電子像の写真である。この写真は、緻密質複合材料の断面研磨後、縦90μm×横120μmの領域を1000倍に拡大したSEM像(反射電子像)である。図10では、濃灰色の粒子がSiC粒子、SiC粒子間の灰色の組織がTiSi2、SiC粒子間の明灰色の組織がTSC、TiSi2中に分散する柱状組織がTiC(明るさはTSCと同レベル)である。図10から、SiC粒子の表面はTSC、TiSi2、TiCの少なくとも1つによって覆われていることがわかる。図10から、全形が視野の範囲内に収まる各SiC粒子について、長径(粒子の最大径)を求めた。そうしたところ、長径10μm以上のSiC粒子の数は、34個であった。その他の実験例で、上述した実施形態で使用するのに適した緻密質複合材料についても反射電子像の写真を撮影し、長径10μm以上のSiC粒子の数を求めたところ、表2及び表3に示すように16個以上であった。
Claims (18)
- 内部に冷媒通路が形成され、アルミナセラミック部材の冷却に用いられる冷却板であって、
炭化珪素粒子を37~60質量%含有すると共に、珪化チタン、チタンシリコンカーバイド及び炭化チタンをそれぞれ前記炭化珪素粒子の質量%より少量含有し、開気孔率が1%以下である緻密質複合材料で作製された第1基板と、
前記緻密質複合材料で作製され、前記冷媒通路と同じ形状となるように打ち抜かれた打ち抜き部を有する第2基板と、
前記緻密質複合材料で作製された第3基板と、
前記第1基板と前記第2基板との間に金属接合材を挟んで両基板を熱圧接合することにより両基板間に形成された第1金属接合層と、
前記第2基板と前記第3基板との間に金属接合材を挟んで両基板を熱圧接合することにより両基板間に形成された第2金属接合層と、
を備えた冷却板。 - 内部に冷媒通路を有し、アルミナセラミック部材の冷却に用いられる冷却板であって、
炭化珪素粒子を37~60質量%含有すると共に、珪化チタン、チタンシリコンカーバイド及び炭化チタンをそれぞれ前記炭化珪素粒子の質量%より少量含有し、開気孔率が1%以下である緻密質複合材料で作製された第1基板と、
前記緻密質複合材料で作製され、前記第1基板と向かい合う面に前記冷媒通路となる溝を有する第2基板と、
前記第1基板と前記第2基板のうち前記溝が設けられた面との間に金属接合材を挟んで両基板を熱圧接合することにより形成された金属接合層と、
を備えた冷却板。 - 前記金属接合層は、前記金属接合材としてMgを含有するかSi及びMgを含有するアルミニウム合金の接合材を採用し、該接合材の固相線温度以下の温度で熱圧接合することにより形成されたものである、
請求項1又は2に記載の冷却板。 - 前記緻密質複合材料は、炭化チタンの質量%が前記珪化チタンの質量%及び前記チタンシリコンカーバイドの質量%より小さい、
請求項1~3のいずれか1項に記載の冷却板。 - 前記緻密質複合材料は、前記珪化チタンの質量%が前記チタンシリコンカーバイドの質量%より大きい、
請求項1~4のいずれか1項に記載の冷却板。 - 前記緻密質複合材料は、前記炭化珪素粒子同士の間隙に、前記珪化チタン、前記チタンシリコンカーバイド及び前記炭化チタンの少なくとも1つが前記炭化珪素粒子表面を覆うように存在している、
請求項1~5のいずれか1項に記載の冷却板。 - 前記緻密質複合材料は、前記炭化チタンが前記珪化チタンの内部に分散している、
請求項1~6のいずれか1項に記載の冷却板。 - 前記珪化チタンは、TiSi2である、
請求項1~7のいずれか1項に記載の冷却板。 - 前記緻密質複合材料は、アルミナとの40℃~570℃の平均線熱膨張係数の差が0.5ppm/K以下である、
請求項1~8のいずれか1項に記載の冷却板。 - 前記緻密質複合材料は、40℃~570℃の平均線熱膨張係数が7.2~8.2ppm/Kである、
請求項1~9のいずれか1項に記載の冷却板。 - 前記緻密質複合材料は、熱伝導率が75W/mK以上である、
請求項1~10のいずれか1項に記載の冷却板。 - 前記緻密質複合材料は、4点曲げ強度が200MPa以上である、
請求項1~11のいずれか1項に記載の冷却板。 - 前記緻密質複合材料は、縦90μm×横120μmの領域を1000倍に拡大したSEM像(反射電子像)において長径10μm以上の炭化珪素粒子の数が16個以上である、
請求項1~12のいずれか1項に記載の冷却板。 - 内部に冷媒通路が形成され、アルミナセラミック部材の冷却に用いられる冷却板を製造する方法であって、
(a)炭化珪素粒子を37~60質量%含有すると共に、珪化チタン、チタンシリコンカーバイド及び炭化チタンをそれぞれ前記炭化珪素粒子の質量%より少量含有し、開気孔率が1%以下である緻密質複合材料を用いて、第1~第3基板を作製する工程と、
(b)前記第2基板の一方の面から他方の面まで前記冷媒通路と同じ形状となるように打ち抜いて前記第2基板に打ち抜き部を形成する工程と、
(c)前記第1基板と前記第2基板の一方の面との間および前記第3基板と前記第2基板の他方の面との間にそれぞれ金属接合材を挟んで前記第1~第3基板を熱圧接合する工程と、
を含む冷却板の製法。 - 内部に冷媒通路を有し、アルミナセラミック部材の冷却に用いられる冷却板を製造する方法であって、
(a)炭化珪素粒子を37~60質量%含有すると共に、珪化チタン、チタンシリコンカーバイド及び炭化チタンをそれぞれ前記炭化珪素粒子の質量%より少量含有し、開気孔率が1%以下である緻密質複合材料を用いて、第1基板及び第2基板を作製する工程と、
(b)前記第2基板の一方の面に前記冷媒通路となる溝を形成する工程と、
(c)前記第1基板と前記第2基板のうち前記溝が設けられた面との間に金属接合材を挟んで両基板を熱圧接合する工程と、
を含む冷却板の製法。 - 前記工程(c)では、前記金属接合材としてMgを含有するかSi及びMgを含有するアルミニウム合金の接合材を採用し、該接合材の固相線温度以下の温度で熱圧接合する、
請求項14又は15に記載の冷却板の製法。 - 静電電極及びヒータ電極を内蔵したアルミナ製の静電チャックと、
請求項1~13のいずれか1項に記載の冷却板と、
前記冷却板の前記第1基板の表面と前記静電チャックとの間に金属接合材を挟んで両者を熱圧接合することにより形成された冷却板-チャック接合層と、
を備えた半導体製造装置用部材。 - 前記冷却板-チャック接合層は、前記金属接合材としてMgを含有するかSi及びMgを含有するアルミニウム合金の接合材を採用し、該接合材の固相線温度以下の温度で熱圧接合することにより形成されたものである、
請求項17に記載の半導体製造装置用部材。
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CN104045347A (zh) | 2014-09-17 |
KR20140140112A (ko) | 2014-12-08 |
TWI600613B (zh) | 2017-10-01 |
TWI599553B (zh) | 2017-09-21 |
US20140272378A1 (en) | 2014-09-18 |
CN104285290A (zh) | 2015-01-14 |
JP6182082B2 (ja) | 2017-08-16 |
JPWO2014141974A1 (ja) | 2017-02-16 |
KR20140113364A (ko) | 2014-09-24 |
US9188397B2 (en) | 2015-11-17 |
KR101499409B1 (ko) | 2015-03-05 |
TW201504192A (zh) | 2015-02-01 |
TW201446647A (zh) | 2014-12-16 |
CN104045347B (zh) | 2017-09-05 |
JP2014198662A (ja) | 2014-10-23 |
CN104285290B (zh) | 2016-03-23 |
JP5666748B1 (ja) | 2015-02-12 |
KR102084033B1 (ko) | 2020-03-03 |
US9255747B2 (en) | 2016-02-09 |
US20150077895A1 (en) | 2015-03-19 |
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