WO2022195947A1 - Aln ceramic substrate, and heater for semiconductor manufacturing device - Google Patents
Aln ceramic substrate, and heater for semiconductor manufacturing device Download PDFInfo
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- WO2022195947A1 WO2022195947A1 PCT/JP2021/040196 JP2021040196W WO2022195947A1 WO 2022195947 A1 WO2022195947 A1 WO 2022195947A1 JP 2021040196 W JP2021040196 W JP 2021040196W WO 2022195947 A1 WO2022195947 A1 WO 2022195947A1
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- ceramic substrate
- aln
- resistance heating
- aln ceramic
- heating element
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- 239000000919 ceramic Substances 0.000 title claims abstract description 69
- 239000000758 substrate Substances 0.000 title claims abstract description 59
- 238000004519 manufacturing process Methods 0.000 title claims description 35
- 239000004065 semiconductor Substances 0.000 title claims description 34
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims description 59
- 239000002245 particle Substances 0.000 claims description 30
- 238000010304 firing Methods 0.000 description 21
- 239000000843 powder Substances 0.000 description 16
- 230000002093 peripheral effect Effects 0.000 description 13
- 230000036581 peripheral resistance Effects 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 239000011812 mixed powder Substances 0.000 description 9
- 239000002994 raw material Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000004453 electron probe microanalysis Methods 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 238000003991 Rietveld refinement Methods 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 241000519995 Stachys sylvatica Species 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/68—Heating arrangements specially adapted for cooking plates or analogous hot-plates
- H05B3/74—Non-metallic plates, e.g. vitroceramic, ceramic or glassceramic hobs, also including power or control circuits
Definitions
- the present invention relates to AlN ceramic substrates and heaters for semiconductor manufacturing equipment.
- a known heater for a semiconductor manufacturing apparatus includes an AlN ceramic substrate and a resistance heating element embedded inside the AlN ceramic substrate. Such heaters for semiconductor manufacturing equipment are used to heat a wafer mounted on the surface of an AlN ceramic substrate. Further, as a heater for semiconductor manufacturing equipment, as disclosed in Patent Document 2, a heater in which a resistance heating element and an electrostatic electrode are embedded in an AlN ceramic base is also known. In such a heater for a semiconductor manufacturing apparatus, if current leaks from the resistance heating element to the wafer or from the electrostatic electrode to the wafer, the wafer will be damaged. Therefore, it is preferable to control the volume resistivity of the AlN ceramic substrate to a high value.
- Patent Document 3 as an AlN ceramic substrate, a mixed powder obtained by adding yttrium oxide powder as a sintering aid to AlN raw material powder is granulated, and the granules are used to produce a disk-shaped molded body.
- a hot press sintering of the compact at 1850 to 1890° C. is disclosed.
- the volume resistivity of the AlN ceramic substrate at 550° C. is as high as 1 ⁇ 10 9 to 2.6 ⁇ 10 9 ⁇ cm.
- the leakage current flowing through the AlN ceramic substrate may not be sufficiently blocked.
- the present invention has been made to solve such problems, and the main object thereof is to provide an AlN ceramic substrate having a higher volume resistivity at high temperatures than conventional ones.
- the AlN ceramic substrate of the present invention is An AlN ceramic substrate comprising yttrium aluminate, Volume resistivity at 550 ° C. is 3 ⁇ 10 9 ⁇ cm or more, It is.
- This AlN ceramic substrate has a higher volume resistivity at high temperatures than conventional ones. Therefore, when this AlN ceramic substrate is used as an AlN ceramic substrate in which a resistance heating element of a heater for semiconductor manufacturing equipment is embedded, it is possible to sufficiently prevent leakage current from flowing through the AlN ceramic substrate.
- a volume resistivity of 5 ⁇ 10 9 ⁇ cm or more is preferable because leakage current can be further suppressed, and a volume resistivity of 1 ⁇ 10 10 ⁇ cm or more is more preferable because the thickness of the ceramic substrate can be further reduced.
- Examples of yttrium aluminate include Y 4 Al 2 O 9 (YAM) and YAlO 3 (YAL).
- the average particle size of the AlN sintered particles is preferably 1.5 ⁇ m or more and 2.5 ⁇ m or less, and yttrium aluminate exists in a dispersed state at the grain boundaries between the AlN sintered particles. is preferred. In this way, the yttrium aluminate is finely and uniformly dispersed. Therefore, it is possible to prevent a current path from occurring in the yttrium aluminate and increase the volume resistivity of the AlN ceramic substrate at high temperatures.
- a heater for semiconductor manufacturing equipment has a resistance heating element embedded in the AlN ceramic substrate described above.
- the volume resistivity of the AlN ceramic substrate at high temperatures is even higher than before. Therefore, it is possible to sufficiently prevent leakage current from flowing through the AlN ceramic substrate.
- the resistance heating element is preferably made of Mo
- the AlN ceramic base includes a first annular layer surrounding the resistance heating element so as to be in contact with the resistance heating element.
- a second annular layer surrounding the first annular layer and the first annular layer preferably has a higher Y content and a wider layer width than the second annular layer.
- the first annular layer may continuously surround the resistive heating element and the second annular layer may continuously surround the first annular layer.
- the second annular layer may have a shape in which a portion of the annular shape has a discontinuous portion, and a shape that forms a single ring (smooth ring) if the discontinuous portion is virtually connected.
- the average value per unit width of the Y content distributed in the width direction of the first annular layer is larger than the average value per unit width of the Y content distributed in the width direction of the second annular layer good.
- FIG. 2 is a plan view of the heater 10 for semiconductor manufacturing equipment; AA sectional view of FIG. Sectional drawing of the modification of the 2nd annular layer L2.
- 4 is a SEM photograph of a cross section containing Mo of the AlN ceramic sintered body 12 of Example 1.
- FIG. 4 is a schematic diagram of a cross section containing Mo of the AlN ceramic sintered body 12 of Example 1.
- FIG. 4 is a graph showing the results of EPMA analysis of Example 1.
- FIG. 4 is a SEM photograph of a cross section containing Mo of the AlN ceramic sintered body of Comparative Example 1.
- FIG. 4 is a schematic diagram of a cross section containing Mo of the AlN ceramic sintered body of Comparative Example 1.
- FIG. 4 is a graph showing the results of EPMA analysis of Comparative Example 1.
- FIG. 1 is a plan view of a heater 10 for semiconductor manufacturing equipment
- FIG. 2 is a sectional view taken along line AA of FIG. Note that the dashed-dotted lines in FIG. 1 indicate the boundaries of the zones.
- the inner and outer resistance heating elements 30 and 40 are indicated by hidden lines (dotted lines), but the RF electrode 20 is omitted.
- a heater 10 for a semiconductor manufacturing apparatus has an RF electrode 20, an inner circumference side resistance heating element 30, and an outer circumference side resistance heating element 40 embedded in a disk-shaped AlN ceramic substrate 12.
- the AlN ceramic substrate 12 contains yttrium aluminate (for example, YAL or YAM), and has a wafer mounting surface 12a on its upper surface.
- the volume resistivity of the AlN ceramic substrate 12 at 550° C. is 3 ⁇ 10 9 ⁇ cm or higher, preferably 5 ⁇ 10 9 ⁇ cm or higher, more preferably 1 ⁇ 10 10 ⁇ cm or higher.
- the AlN ceramic substrate 12 is divided into an inner zone Zin and an outer zone Zout when viewed from above.
- the inner peripheral zone Zin is a circular zone with a diameter smaller than the diameter of the AlN ceramic substrate 12 .
- the outer zone Zout is an annular zone surrounding the inner zone Zin.
- the RF electrode 20 is a circular metal mesh (eg, Mo coil) and is provided substantially parallel to the wafer mounting surface 12a.
- the RF electrode 20 is buried closer to the wafer mounting surface 12 a than the inner resistance heating element 30 and the outer resistance heating element 40 .
- the diameter of RF electrode 20 is slightly smaller than the diameter of AlN ceramic substrate 12 .
- a high-frequency voltage is applied between the RF electrode 20 and a parallel plate electrode (not shown) spaced apart from the wafer mounting surface 12a.
- the RF electrode 20 is connected to the RF connecting member 22 .
- the RF connection member 22 has an upper end connected to the lower surface of the RF electrode 20 and a lower end exposed from the lower surface 12 b of the AlN ceramic substrate 12 .
- the RF connection member 22 is provided so as to pass through the gaps in the wiring pattern of the inner resistance heating element 30 .
- An RF connecting member 22 is used to apply a high frequency voltage between the RF electrode 20 and the parallel plate electrodes.
- the inner circumference side resistance heating element 30 is a metal coil (eg, Mo coil) and is provided substantially parallel to the wafer mounting surface 12a.
- the inner peripheral resistance heating element 30 is wired from one of a pair of terminals 32 and 34 provided near the center of the AlN ceramic substrate 12 to the entire inner peripheral zone Zin in a unicursal manner without crossing. It is provided so as to reach the other of the pair of terminals 32 and 34 .
- a pair of terminals 32 and 34 are connected to a pair of inner peripheral side connecting members 36 and 38 .
- the lower ends of the pair of inner peripheral side connecting members 36 and 38 are exposed from the lower surface 12b of the AlN ceramic substrate 12. As shown in FIG.
- a voltage is applied between the pair of terminals 32 and 34 using the pair of inner peripheral connecting members 36 and 38 .
- the outer-peripheral-side resistance heating element 40 is a metal coil (for example, a Mo coil) and is provided substantially parallel to the wafer mounting surface 12a.
- the outer resistance heating element 40 passes through the inner zone Zin from one of a pair of terminals 42 and 44 provided near the center of the AlN ceramic substrate 12 and is led out to the outer zone Zout. , and then pulled back to the inner peripheral zone Zin to reach the other of the pair of terminals 42 and 44 .
- a pair of terminals 42 and 44 are connected to a pair of outer peripheral side connection members 46 and 48 .
- the lower ends of the pair of outer peripheral side connecting members 46 and 48 are exposed from the lower surface 12b of the AlN ceramic substrate 12.
- a voltage is applied between the pair of terminals 42 and 44 using the pair of outer connection members 46 and 48 .
- the outer resistance heating element 40 is provided on the same plane as the inner resistance heating element 30 .
- the heater 10 for semiconductor manufacturing equipment is installed in a chamber (not shown).
- a wafer W is mounted on the wafer mounting surface 12a of the heater 10 for a semiconductor manufacturing apparatus, and an external power source is connected to the connection members 36 and 38 of the inner peripheral resistance heating element 30, so that an electric current is generated between the pair of terminals 32 and 34.
- an external power source is connected to the connection members 36 and 38 of the inner peripheral resistance heating element 30, so that an electric current is generated between the pair of terminals 32 and 34.
- another external power supply is connected to the connection members 46 and 48 of the outer resistance heating element 40 to apply a voltage between the pair of terminals 42 and 44 .
- the inner peripheral resistance heating element 30 and the outer peripheral resistance heating element 40 generate heat to heat the wafer W to a predetermined temperature.
- the temperature of the inner zone Zin and the outer zone Zout can be individually controlled.
- a high-frequency voltage is applied between a parallel plate electrode (not shown) and the RF electrode 20 spaced apart above the wafer W, and the wafer W is subjected to various processes necessary for fabricating semiconductor chips.
- the application of the high frequency voltage to the RF electrode 20 and the application of voltage to the inner and outer resistance heating elements 30 and 40 are terminated, and the wafer W is removed from the wafer mounting surface 12a.
- AlN raw material powder is prepared.
- the AlN raw material powder may contain a small amount of O, C, Ti, and Ca.
- the AlN raw material powder preferably contains 0.65 to 0.90 mass % of O, 220 to 380 mass ppm of C, 95 mass ppm or less of Ti, and 250 mass ppm or less of Ca.
- the average particle diameter of the AlN raw material powder is preferably set so that the average particle diameter of the AlN sintered particles after firing is 1.5 ⁇ m or more and 2.5 ⁇ m or less, for example, 1.5 ⁇ m or more and 2.0 ⁇ m or less. .
- Y 2 O 3 powder is added as a sintering aid to the prepared AlN raw material powder and mixed to obtain a mixed powder, which is granulated by spray drying.
- Y 2 O 3 is added so as to be 4 to 6% by mass with respect to the entire mixed powder.
- the average particle size of the Y 2 O 3 powder is preferably of submicron order.
- a mixing method wet mixing using an organic solvent may be employed, or dry mixing such as a ball mill, vibration mill, and dry bag mixing may be employed.
- the RF electrode 20 and the inner and outer peripheral resistance heating elements 30 and 40 are embedded in the granules and molded to produce a compact.
- the formed body is fired to obtain an AlN sintered body.
- the heater 10 for semiconductor manufacturing equipment is obtained.
- a firing method for example, hot press firing can be used.
- the maximum temperature (firing temperature) during hot press firing is preferably set in the range of 1650°C or higher and 1750°C or lower, preferably 1670°C or higher and 1730°C or lower.
- the firing temperature is maintained for 0.5 to 100 hours
- the press pressure is 5 to 50 MPa
- the atmosphere is a nitrogen atmosphere or a vacuum atmosphere (for example, 0.13 to 133.3 Pa).
- the average particle size of the AlN sintered particles is preferably 1.5 ⁇ m or more and 2.5 ⁇ m or less. It is preferable that yttrium aluminate, which is finer than the AlN sintered particles, is present in a dispersed state at grain boundaries between the AlN sintered particles. If the average particle size of the AlN sintered particles is larger than this, the yttrium aluminate exists in a wet state at the grain boundary between the AlN sintered particles, making it easier to form a current path. not high enough.
- the average particle size of the AlN sintered particles is 1.5 ⁇ m or more and 2.5 ⁇ m or less, yttrium aluminate exists in a state of being dispersed in the grain boundaries between the AlN sintered particles, so a current path is formed. and the volume resistivity at high temperatures is sufficiently high.
- the AlN ceramic substrate 12 has an inner surface so as to be in contact with the inner resistance heating element 30 as shown in the enlarged view of FIG.
- a first annular layer L1 continuously (that is, without interruption) surrounding the circumferential resistance heating element 30 and a second annular layer L2 continuously surrounding the first annular layer L1 appear.
- the first annular layer L1 has a higher Y content and a wider layer width than the second annular layer L2. That is, the first annular layer L1 is a Y-rich layer, and the second annular layer L2 is a Y-poor layer.
- Such a microstructure is also seen around the outer resistance heating element 40 .
- the reason why the first annular layer L1 becomes the Y-rich layer is considered as follows.
- the Y concentration in the region in contact with the Mo inner peripheral resistance heating element 30 decreases.
- Mo has a high affinity for oxygen and tries to take oxygen from the yttrium aluminate around Mo, whereas the yttrium aluminate around Mo does not want to take oxygen. Therefore, it is considered to move to a position away from Mo.
- the Y concentration in the region of the AlN ceramic substrate 12 in contact with the Mo inner resistance heating element 30 is considered to decrease. This may be one of the reasons why the volume resistivity at high temperatures is not sufficiently high.
- the firing temperature when the firing temperature is 1650° C. or higher and 1750° C. or lower, the Y concentration in the region (first annular layer L1) in contact with the Mo inner circumference side resistance heating element 30 becomes relatively high. If the firing temperature is 1750° C. or lower, it is difficult for Mo to deprive the surrounding yttrium aluminate of oxygen. As a result, when the firing temperature is 1650° C. or higher and 1750° C. or lower, the Y concentration in the region (first annular layer L1) of the AlN ceramic substrate 12 that is in contact with the Mo inner peripheral side resistance heating element 30 does not decrease. It is thought that it will become a rich layer. This may be one of the reasons why the volume resistivity at high temperatures is sufficiently high.
- the volume resistivity of the AlN ceramic substrate 12 at a high temperature (550° C.) is 3 ⁇ 10 9 ⁇ cm or more, which is higher than that of the conventional heater. Therefore, it is possible to sufficiently prevent leakage current from flowing through the AlN ceramic substrate 12 .
- a volume resistivity of 5 ⁇ 10 9 ⁇ cm or more is preferable because leakage current can be further suppressed, and a volume resistivity of 1 ⁇ 10 10 ⁇ cm or more is more preferable because the thickness of the ceramic substrate can be further reduced.
- the average particle size of the AlN sintered particles in the AlN ceramic substrate 12 is preferably 1.5 ⁇ m or more and 2.5 ⁇ m or less, and yttrium aluminate exists in a dispersed state at the grain boundary between the AlN sintered particles. is preferred. In this way, the yttrium aluminate is finely and uniformly dispersed. Therefore, it is possible to prevent the occurrence of a current path of yttrium aluminate and increase the volume resistivity of the AlN ceramic substrate 12 at high temperatures.
- the inner and outer peripheral resistance heating elements 30 and 40 are preferably made of Mo. and a second annular layer L2 that continuously surrounds the first annular layer L2.
- the first annular layer L1 has a higher Y content than the second annular layer L2 A wide width is preferred.
- Such structures are believed to contribute in some way to the high volume resistivity at high temperatures. Such a structure is obtained by performing the operation of keeping for at least one hour or more until the maximum temperature is reached (between 1500 ° C. and 10 ° C. below the maximum temperature) when performing hot press firing. , is likely to occur.
- the heater 10 for a semiconductor manufacturing apparatus includes a mixed powder of AlN powder and Y 2 O 3 powder (the Y 2 O 3 powder is 4% by mass or more and 6% by mass or less of the entire mixed powder), the RF electrode 20 and the inner circumference.
- the molded body is hot-press fired at a maximum firing temperature of 1650° C. or higher and 1750° C. or lower. It is obtained. Therefore, it is possible to relatively easily manufacture the heater 10 for semiconductor manufacturing equipment, which can sufficiently prevent the leak current from flowing through the AlN ceramic substrate 12 .
- the RF electrode 20 is embedded in the AlN ceramic substrate 12, but the RF electrode 20 may be omitted, the RF electrode 20 may be replaced with an electrostatic electrode, or the RF electrode 20 may be replaced with an electrostatic electrode. It may also be used as an electrostatic electrode.
- an electrostatic electrode is provided, the wafer W can be attracted and held on the wafer mounting surface 12a by applying a voltage to the electrostatic electrode.
- a metal mesh is exemplified as the RF electrode 20, but a metal plate may be employed.
- the metal coils have been exemplified as the inner and outer peripheral resistance heating elements 30 and 40, metal ribbons and metal meshes may also be employed.
- the RF electrode 20 and the inner and outer resistance heating elements 30 and 40 may be formed by printing a conductive paste in a predetermined shape or pattern.
- the inner resistance heating element 30 is embedded in the inner zone Zin and the outer resistance heating element 40 is embedded in the outer zone Zout.
- a resistance heating element may be embedded in each zone by dividing it. Alternatively, a single resistance heating element may be wired throughout the AlN ceramic substrate 12 without dividing it into a plurality of zones.
- the inner peripheral side resistance heating element 30 and the outer peripheral side resistance heating element 40 are embedded on the same plane, but they may be embedded on different surfaces.
- the heater 10 for a semiconductor manufacturing apparatus is illustrated, but the AlN ceramic substrate 12 can be used alone without embedding the RF electrode 20 and the inner and outer peripheral resistance heating elements 30 and 40 in the AlN ceramic substrate 12. can be made with
- the second annular layer L2 has a shape that continuously surrounds the first annular layer L1, but it is not particularly limited to this.
- the second annular layer L2 may have a shape that is not continuous but has an annular portion L2a that is interrupted.
- the second annular layer L2 forms one ring (smooth ring) if the discontinuous portions L2a are virtually connected.
- Example 1 AlN raw material powder was prepared. 5% by mass of Y 2 O 3 powder was added as a sintering aid to this AlN raw material powder and mixed by a ball mill to obtain a mixed powder, which was granulated by spray drying. Y 2 O 3 was added so as to be 5% by mass with respect to the entire mixed powder. Subsequently, using the granules of the mixed powder, a disk-shaped compact was produced. An RF electrode 20 and inner and outer resistance heating elements 30 and 40 were embedded in the compact. Then, the heater 10 for a semiconductor manufacturing apparatus was produced by hot-press firing the compact.
- the maximum temperature (firing temperature) during firing was 1720° C.
- the time to keep the firing temperature was 2 hours
- the press pressure was 20 MPa
- the atmosphere was nitrogen atmosphere.
- the operation of keeping for 1 hour was performed twice or more until the maximum temperature was reached (from 1500° C. to a temperature 10° C. lower than the maximum temperature).
- the crystal phase contained in the AlN ceramic substrate 12 was identified by X-ray diffraction. About 0.5 g of powder was measured for X-ray diffraction with a Bruker AXS D8 ADVANCE. The measurement conditions were a CuK ⁇ ray source, a tube voltage of 40 kV, and a tube current of 40 mA. Rietveld analysis was performed on the measurement results to identify and quantify the crystal phase. Crystal phases identified from the XRD profile were AlN, YAM, and YAL, and TiN was not confirmed.
- Comparative Example 1 A heater for a semiconductor manufacturing apparatus was manufactured in the same manner as in Example 1, except that the maximum temperature was set to 1850° C. and the operation to keep the temperature was not performed until the maximum temperature was reached. Also in Comparative Example 1, the crystal phases identified from the XRD profile were AlN, YAM, and YAL, and TiN was not confirmed.
- the volume resistivity of the AlN ceramic substrate 12 of the heater 10 for semiconductor manufacturing equipment of Example 1 was measured at 550°C. Measurement was performed as follows. A leak current (current flowing between the wafer W and the RF electrode 20) is obtained when a Si wafer W is placed on the wafer mounting surface 12a and a voltage is applied between the wafer W and the RF electrode 20 (metal mesh) at 550°C. ) was measured. The diameter of the RF electrode 20 was ⁇ 355.6 mm, the film thickness of the dielectric layer (the layer between the wafer mounting surface 12a and the RF electrode 20) was 1.02 mm, and the applied voltage was 660V.
- a plurality of heaters 10 for a semiconductor manufacturing apparatus of Example 1 were produced, and the leak current was measured to be on the order of 40 mA.
- the volume resistivity of the AlN ceramic substrate 12 at 550° C. was indirectly calculated from the leak current, the average value was 1.2 ⁇ 10 10 ⁇ cm.
- the leakage current was measured in Comparative Example 1 in the same manner as in Example 1, it was on the order of 280 mA, and the average volume resistivity of the AlN ceramic substrate at 550° C. was 2.4 ⁇ 10 9 ⁇ cm. .
- Example 1 When the average particle size of the AlN sintered particles was determined from the SEM photograph of the cross section containing Mo of the AlN ceramic sintered body 12 of Example 1, it was 1.9 ⁇ m. Therefore, in Example 1, it was determined that the yttrium aluminate was uniformly dispersed in the grain boundaries between fine AlN sintered particles. When the average particle size of Comparative Example 1 was determined in the same manner, the average particle size was 4.5 ⁇ m, which is larger than that of Example 1. The average particle size is obtained by obtaining a secondary electron image (magnification: 3000), drawing a straight line on the image, measuring the length of each line segment that crosses 40 particles, and calculating the average value thereof. did.
- a secondary electron image magnification: 3000
- FIG. 4 is a SEM photograph of a cross section of the AlN ceramic sintered body 12 of Example 1 including Mo (the inner peripheral resistance heating element 30), and FIG. 5 is a schematic diagram thereof.
- the first annular layer L1 continuously (without interruption) surrounds Mo so as to be in contact with Mo
- the second annular layer L2 continuously surrounds the first annular layer L1.
- the first annular layer L1 had a large number of fine white spots (Y derived from yttrium aluminate) dispersed therein, but the second annular layer L2 had almost no such spots and was almost black.
- FIG. 6 is a graph showing the results of EPMA analysis for Mo and Y along the arrow directions in FIG. In FIG.
- the portions where the Mo concentration rises sharply and the portions where it falls steeply are regarded as boundaries between the resistance heating element (Mo) and the AlN ceramic sintered body.
- the Y concentration in the first annular layer L1 was relatively high, but the Y concentration in the second annular layer L2 was almost zero. From this, it was found that the first annular layer L1 was a Y-rich layer and the second annular layer L2 was a Y-poor layer. Also, the layer width of the first annular layer L1 was wider than the layer width of the second annular layer L2.
- FIG. 7 is a SEM photograph of a cross section containing Mo of the AlN ceramic sintered body of Comparative Example 1
- FIG. 8 is a schematic diagram thereof.
- a first layer surrounding Mo so as to be in contact with Mo and a second layer surrounding the first layer were observed.
- the first layer was almost black with almost no spots, and the second layer had relatively many spots.
- the second layer was non-continuous and discontinuous.
- FIG. 9 shows the results of EPMA analysis of Mo and Y along the arrow directions in FIG. In FIG. 9, the portions where the Mo concentration steeply rises and falls are regarded as boundaries between the resistance heating element (Mo) and the AlN sintered body.
- Mo resistance heating element
- the Y concentration of the first layer was almost zero and the Y concentration of the second layer was relatively high. From this, it was found that the first layer in Comparative Example 1 was a Y-poor layer and the second layer was a Y-rich layer, that is, contrary to Example 1.
- the present invention can be used for heaters for semiconductor manufacturing equipment.
- Heater for semiconductor manufacturing equipment 12 AlN ceramic substrate, 12a Wafer mounting surface, 12b Lower surface, 20 RF electrode, 22 RF connection member, 30 Inner peripheral side resistance heating element, 32, 34 Terminal, 36, 38 Inner peripheral side connection Member, 40 outer resistance heating element, 42, 44 terminals, 46, 48 outer connecting member, L1 first annular layer, L2 second annular layer, W wafer, Zin inner zone, Zout outer zone.
Abstract
Description
イットリウムアルミネートを含むAlNセラミック基体であって、
550℃での体積抵抗率が3×109Ωcm以上である、
ものである。 The AlN ceramic substrate of the present invention is
An AlN ceramic substrate comprising yttrium aluminate,
Volume resistivity at 550 ° C. is 3 × 10 9 Ωcm or more,
It is.
まず、AlN原料粉末を用意した。このAlN原料粉末に焼結助剤としてY2O3粉末を5質量%添加してボールミルにより混合して混合粉末とし、これをスプレードライにて顆粒化した。Y2O3は混合粉末全体に対して5質量%となるように添加した。続いて、混合粉末の顆粒を用いて、円盤形状の成形体を作製した。成形体には、RF電極20と内周側及び外周側抵抗発熱体30,40を埋設した。そして、この成形体をホットプレス焼成することにより半導体製造装置用ヒータ10を作製した。ホットプレス焼成では、焼成時の最高温度(焼成温度)を1720℃、焼成温度でのキープ時間を2時間、プレス圧力を20MPa、雰囲気を窒素雰囲気とした。なお、ホットプレス焼成では、最高温度に到達するまでの間(1500℃から最高温度より10℃低い温度までの間)で、1時間キープする操作を2回以上行った。 [Example 1]
First, AlN raw material powder was prepared. 5% by mass of Y 2 O 3 powder was added as a sintering aid to this AlN raw material powder and mixed by a ball mill to obtain a mixed powder, which was granulated by spray drying. Y 2 O 3 was added so as to be 5% by mass with respect to the entire mixed powder. Subsequently, using the granules of the mixed powder, a disk-shaped compact was produced. An
最高温度を1850℃としたこと及び最高温度に到達するまでの間でキープする操作を行わなかったこと以外は、実施例1と同様にして半導体製造装置用ヒータを作製した。比較例1も、XRDプロファイルから同定された結晶相はAlN,YAM,YALであり、TiNは確認されなかった。 [Comparative Example 1]
A heater for a semiconductor manufacturing apparatus was manufactured in the same manner as in Example 1, except that the maximum temperature was set to 1850° C. and the operation to keep the temperature was not performed until the maximum temperature was reached. Also in Comparative Example 1, the crystal phases identified from the XRD profile were AlN, YAM, and YAL, and TiN was not confirmed.
実施例1の半導体製造装置用ヒータ10につき、AlNセラミック基体12の550℃での体積抵抗率を測定した。測定は、次のようにして行った。ウエハ載置面12aにSiウエハWを載せ、550℃でウエハWとRF電極20(金属メッシュ)との間に電圧を印加したときのリーク電流(ウエハWとRF電極20との間を流れる電流)を測定した。RF電極20の直径はφ355.6mm、誘電層(ウエハ載置面12aとRF電極20との間の層)の膜厚は1.02mm、印加電圧は660Vとした。実施例1の半導体製造装置用ヒータ10を複数作製し、リーク電流を測定したところ、40mA台であった。AlNセラミック基体12の550℃での体積抵抗率を、リーク電流から間接的に計算したところ、平均値は1.2×1010Ωcmであった。一方、比較例1も実施例1と同様にしてリーク電流を測定したところ、280mA台であり、AlNセラミック基体の550℃での体積抵抗率の平均値は2.4×109Ωcmであった。 [Volume resistivity]
The volume resistivity of the AlN
実施例1のAlNセラミック焼結体12のMoを含む断面を撮影したSEM写真からAlN焼結粒子の平均粒径を求めたところ、1.9μmであった。そのため、実施例1では、微細なAlN焼結粒子同士の粒界にイットリウムアルミネートが均一に分散していると判断した。比較例1についても同様にして平均粒径を求めたところ、4.5μmであり、実施例1と比べて大きな粒子であった。なお、平均粒径は、二次電子像(倍率3000倍)を取得し、その画像上に直線を引き、40個の粒子を横切る線分の長さをそれぞれ測定し、それらの平均値として算出した。 [Microstructure]
When the average particle size of the AlN sintered particles was determined from the SEM photograph of the cross section containing Mo of the AlN ceramic
Claims (5)
- イットリウムアルミネートを含むAlNセラミック基体であって、
550℃での体積抵抗率が3×109Ωcm以上である、
AlNセラミック基体。 An AlN ceramic substrate comprising yttrium aluminate,
Volume resistivity at 550 ° C. is 3 × 10 9 Ωcm or more,
AlN ceramic substrate. - AlN焼結粒子の平均粒径が1.5μm以上2.5μm以下であり、
AlN焼結粒子同士の粒界にイットリウムアルミネートが分散した状態で存在する、
請求項1に記載のAlNセラミック基体。 The average particle diameter of the AlN sintered particles is 1.5 μm or more and 2.5 μm or less,
Yttrium aluminate exists in a dispersed state at the grain boundary between AlN sintered particles,
The AlN ceramic substrate of claim 1. - 請求項1又は2に記載のAlNセラミック基体に抵抗発熱体が埋設された、
半導体製造装置用ヒータ。 A resistance heating element is embedded in the AlN ceramic substrate according to claim 1 or 2,
Heater for semiconductor manufacturing equipment. - 前記抵抗発熱体は、Mo製であり、
前記AlNセラミック基体には、前記抵抗発熱体に接するように前記抵抗発熱体を取り囲む第1環状層と、前記第1環状層を取り囲む第2環状層とが存在し、前記第1環状層は、前記第2環状層に比べてY含有量が多くて層幅が広い、
請求項3に記載の半導体製造装置用ヒータ。 The resistance heating element is made of Mo,
The AlN ceramic substrate includes a first annular layer surrounding the resistance heating element so as to be in contact with the resistance heating element, and a second annular layer surrounding the first annular layer, wherein the first annular layer comprises: The Y content is larger and the layer width is wider than that of the second annular layer,
4. The heater for semiconductor manufacturing equipment according to claim 3. - 前記第1環状層は、前記抵抗発熱体を連続的に取り囲み、
前記第2環状層は、前記第1環状層を連続的に取り囲む、
請求項4に記載の半導体製造装置用ヒータ。 the first annular layer continuously surrounds the resistive heating element;
the second annular layer continuously surrounds the first annular layer;
5. The heater for semiconductor manufacturing equipment according to claim 4.
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CN202180010171.0A CN115606318A (en) | 2021-03-18 | 2021-11-01 | AlN ceramic base and heater for semiconductor manufacturing apparatus |
US18/046,614 US20230138000A1 (en) | 2021-03-18 | 2022-10-14 | AlN CERAMIC SUBSTRATE AND HEATER FOR SEMICONDUCTOR MANUFACTURING APPARATUS |
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JP2003313078A (en) * | 2002-04-18 | 2003-11-06 | Taiheiyo Cement Corp | Aluminum nitride sintered compact and electrostatic chuck using the same |
JP2015514661A (en) * | 2012-02-29 | 2015-05-21 | ハリス,ジョナサン・エイチ | Transient liquid phase, normal pressure bonding of aluminum nitride parts |
US10403535B2 (en) * | 2014-08-15 | 2019-09-03 | Applied Materials, Inc. | Method and apparatus of processing wafers with compressive or tensile stress at elevated temperatures in a plasma enhanced chemical vapor deposition system |
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JP2015514661A (en) * | 2012-02-29 | 2015-05-21 | ハリス,ジョナサン・エイチ | Transient liquid phase, normal pressure bonding of aluminum nitride parts |
US10403535B2 (en) * | 2014-08-15 | 2019-09-03 | Applied Materials, Inc. | Method and apparatus of processing wafers with compressive or tensile stress at elevated temperatures in a plasma enhanced chemical vapor deposition system |
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