WO2018221504A1 - 窒化アルミニウム質焼結体、および半導体保持装置 - Google Patents

窒化アルミニウム質焼結体、および半導体保持装置 Download PDF

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WO2018221504A1
WO2018221504A1 PCT/JP2018/020519 JP2018020519W WO2018221504A1 WO 2018221504 A1 WO2018221504 A1 WO 2018221504A1 JP 2018020519 W JP2018020519 W JP 2018020519W WO 2018221504 A1 WO2018221504 A1 WO 2018221504A1
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Prior art keywords
aluminum nitride
aln
particles
sintered body
composite
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PCT/JP2018/020519
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English (en)
French (fr)
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王　雨叢
佐藤　政宏
和一 口町
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京セラ株式会社
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Application filed by 京セラ株式会社 filed Critical 京セラ株式会社
Priority to EP18810577.9A priority Critical patent/EP3632877B1/en
Priority to KR1020197034104A priority patent/KR102347643B1/ko
Priority to CN201880033185.2A priority patent/CN110662728A/zh
Priority to US16/615,041 priority patent/US11685695B2/en
Priority to JP2018546571A priority patent/JP6496092B1/ja
Publication of WO2018221504A1 publication Critical patent/WO2018221504A1/ja

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    • H01L21/687—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using mechanical means, e.g. chucks, clamps or pinches
    • H01L21/68714—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using mechanical means, e.g. chucks, clamps or pinches the wafers being placed on a susceptor, stage or support
    • H01L21/68757—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using mechanical means, e.g. chucks, clamps or pinches the wafers being placed on a susceptor, stage or support characterised by a coating or a hardness or a material

Definitions

  • the present disclosure relates to an aluminum nitride sintered body and a semiconductor holding device.
  • Semiconductor manufacturing equipment used in semiconductor manufacturing dry processes uses highly reactive halogen-based plasmas such as F and Cl for film formation, etching, or cleaning. Is done.
  • An aluminum nitride sintered body is used as a material for holding a semiconductor wafer used in such a semiconductor manufacturing apparatus, such as a heater or an electrostatic chuck.
  • the aluminum nitride sintered body has high mechanical strength, high thermal shock resistance, high volume resistivity, high thermal conductivity, and high corrosion resistance to halogen-based gases.
  • the corrosion resistance to the halogen-based gas is high, the corrosion resistance to the halogen-based plasma is also high.
  • the corrosion resistance against plasma may be referred to as plasma resistance.
  • Semiconductor integrated circuits are required to be further miniaturized and densified.
  • As a means for further miniaturizing and increasing the density of a semiconductor integrated circuit it has been attempted to process a semiconductor wafer or the like at a high temperature of, for example, 600 ° C. or higher.
  • a high temperature for example, 600 ° C. or higher.
  • an ordinary aluminum nitride sintered body has an electrical resistivity of 10 6 ⁇ m or less at such a high temperature, and it has been difficult to maintain insulation.
  • Patent Literature 1 discloses a ceramic sintered body of aluminum nitride having a high insulation resistance at 700 ° C. having a grain boundary phase containing magnesium as an insulator of a spark plug.
  • Patent Document 2 discloses an aluminum nitride sintered body containing aluminum nitride, a rare earth compound, and MgAl 2 O 4 as an aluminum nitride sintered body having a high volume resistivity at 800 ° C.
  • An aluminum nitride sintered body of the present disclosure includes aluminum nitride crystal grains containing Mg, a garnet-type crystal structure, a composite oxide containing a rare earth element and Al, and a composite acid containing Mg and Al.
  • the composite oxide in the form of particles and the composite oxynitride are interspersed between the crystal grains of the aluminum nitride.
  • the semiconductor holding device of the present disclosure includes an aluminum nitride sintered body and an electrostatic adsorption electrode, and the aluminum nitride sintered body is the above-described aluminum nitride sintered body.
  • FIG. 3 is a sectional view taken along line iii-iii in FIG. 2. It is a perspective view which shows another example of an electrostatic chuck.
  • FIG. 5 is a sectional view taken along line vv in FIG. 4.
  • the aluminum nitride sintered body 1 of the present embodiment includes aluminum nitride crystal particles 2 containing Mg, a composite oxide containing rare earth elements and Al, and a composite containing Mg and Al. Oxynitride. Between the aluminum nitride crystal particles 2, particulate composite oxide and composite oxynitride, that is, composite oxide particles 3 and composite oxynitride particles 4 are scattered.
  • particulate means, for example, a case where the aspect ratio between the maximum length of the cross section and the minimum length or thickness is 5 or less.
  • Al and N are present in a ratio of 1: 1 to form a crystal lattice.
  • oxygen (O) is dissolved in the aluminum nitride crystal
  • Al vacancies are generated. This is because Al and O become stable at a ratio of 2: 3. Since Al vacancies become conductive carriers at a high temperature, the insulating resistance of an aluminum nitride sintered body having an aluminum nitride crystal in which oxygen is dissolved decreases at a high temperature.
  • the volume resistivity may be used instead of the insulation resistance.
  • the aluminum nitride sintered body 1 of the present embodiment contains a rare earth element, a part of oxygen dissolved in the aluminum nitride crystal particles 2 reacts with the rare earth element. As a result, the amount of oxygen dissolved in the aluminum nitride crystal particles 2 is reduced. The greater the amount of rare earth elements contained in the aluminum nitride sintered body 1, the smaller the amount of oxygen dissolved in the aluminum nitride crystal particles 2.
  • the aluminum nitride crystal particles 2 contain Mg, that is, Mg is dissolved in the aluminum nitride crystal particles 2, oxygen and Mg dissolved in the aluminum nitride crystal particles 2 are combined. As a result, generation of Al vacancies in the aluminum nitride crystal particles 2 is suppressed, and a high insulation resistance can be maintained even at high temperatures.
  • aluminum nitride may be simply referred to as AlN.
  • the aluminum nitride sintered body 1 may be simply referred to as an AlN sintered body 1 and the aluminum nitride crystal particles 2 may be simply referred to as AlN particles 2.
  • the composite oxide particles 3 containing a rare earth element and Al have a garnet-type crystal structure.
  • the complex oxides of rare earth elements and Al include garnet type (R 3 Al 5 O 12 ), perovskite type (RAlO 3 ) and melilite type (R 4 Al 2 O depending on the ratio of rare earth element (R) and Al. 9 ) to form various crystal structures.
  • a complex oxide having a garnet-type crystal structure has a high insulation resistance particularly at a high temperature.
  • the particles 3 contained in the aluminum nitride sintered body 1, that is, the complex oxide of rare earth element and aluminum have a garnet-type crystal structure, so that the aluminum nitride sintered body 1 of the present embodiment is heated at a high temperature. Volume resistivity increases.
  • a composite oxide of a rare earth element and Al may be simply referred to as a composite oxide
  • the composite oxide particle 3 containing a rare earth element and Al may be simply referred to as a composite oxide particle 3.
  • the composite oxide having a crystal structure other than the garnet type may not be substantially present in the aluminum nitride sintered body 1.
  • the crystal phase of the complex oxide other than the garnet structure may not be detected by X-ray diffraction (XRD) measurement.
  • the AlN-based sintered body 1 of the present embodiment further includes composite oxynitride particles 4 containing Mg and Al.
  • a composite oxynitride of Mg and Al (MgAlON) has higher plasma resistance than oxides containing Mg such as MgAl 2 O 4 and MgO. The presence of such a composite oxynitride between the crystal grains 2 of aluminum nitride increases the plasma resistance of the AlN sintered body 1.
  • the thermal expansion coefficient of the composite oxynitride of Mg and Al is smaller than the thermal expansion coefficient of AlN as compared with oxides containing Mg such as MgAl 2 O 4 and MgO. Therefore, compared with the case where MgAl 2 O 4 and MgO exist between the AlN crystal particles 2, there is a composite oxynitride (MgAlON) of Mg and Al between the AlN crystal particles 2 as in this embodiment.
  • the residual stress applied to the vicinity of the grain boundary of the AlN crystal particles 2 can be reduced, and the plasma resistance of the AlN sintered body 1 is increased.
  • the presence of the composite oxynitride particles 4 containing Mg and Al between the aluminum nitride crystal particles 2 increases the plasma resistance of the aluminum nitride sintered body 1. Can be maintained.
  • the composite oxynitride particles 4 containing Mg and Al may be simply referred to as composite oxynitride particles 4.
  • the composite oxide particles 3 and the composite oxynitride particles 4 are interspersed between the AlN particles 2. That is, in the cross section of the AlN-based sintered body 1, the composite oxide particles 3 and the composite oxynitride particles 4 do not cover the surface of the AlN particles 2 as a continuous grain boundary layer, but the grain boundaries between the AlN particles 2. It exists as a grain at the triple point or the boundary between two faces.
  • the AlN particle 2 has a predetermined ratio of a portion in direct contact with another adjacent AlN particle 2 without passing through another phase (a grain boundary layer such as a complex oxide crystal or a complex oxynitride). For example, 30% or more.
  • the ratio of the portions where the AlN particles 2 are in direct contact with each other may be, for example, the average of the ratio of the contour of the AlN particles 2 directly in contact with the contour of the other AlN particles 2 in the cross section of the AlN sintered body 1.
  • AlN has a high thermal conductivity, but the thermal conductivity of the AlN sintered body 1 is affected by the crystal structure of the AlN particles 2 and the structure of the sintered body. For example, if other elements such as oxygen are dissolved in the AlN particles 2 and the crystal structure is disturbed, or if a grain boundary layer having a low thermal conductivity is interposed between the AlN particles 2, the thermal conductivity of the AlN sintered body 1. Will decline.
  • the insulation properties of the AlN particles 2 at a high temperature when the AlN sintered body 1 is fired, Mg is dissolved in the AlN particles 2 or rare earth elements are added to form AlN.
  • Mg is dissolved in the AlN particles 2 or rare earth elements are added to form AlN.
  • an excessive additive component forms a grain boundary phase to cover the surface of the AlN particles 2, and the heat conduction between the adjacent AlN particles 2 decreases.
  • the composite oxide and the composite oxynitride that did not dissolve in the AlN particle 2 do not cover the surface of the AlN particle 2 as a grain boundary layer, and the composite oxide particle 3 and the composite oxynitride respectively.
  • the particles 4 are scattered at the grain boundary triple points between the AlN particles 2 or at the grain boundaries between the two faces. In such a case, since the adjacent AlN particles 2 have a portion in direct contact, the thermal conductivity of the AlN-based sintered body 1 can be maintained high.
  • the composite oxide particles 3 and the composite oxynitride particles 4 are scattered in this way, that is, the AlN particles 2
  • the volume resistivity of the AlN sintered body 1 is kept high by the presence of the particulate composite oxide and the composite oxynitride that are independently spaced apart from each other instead of being continuously present at the grain boundaries. be able to.
  • the average particle diameter of the AlN particles 2 may be 10 ⁇ m or less, for example. Moreover, 1 micrometer or more and 10 micrometers or less may be sufficient, and 3 micrometers or more and 8 micrometers or less may be sufficient.
  • the average particle diameter of the AlN particles 2 By reducing the average particle diameter of the AlN particles 2 to 10 ⁇ m or less, the grain boundaries in the AlN sintered body 1 increase. When the grain boundary increases, the composite oxide and the composite oxynitride become particles and are dispersed in many grain boundaries. As a result, the composite oxide particles 3 and the composite oxynitride particles 4 can be scattered at the grain boundaries between the AlN particles 2.
  • the average particle diameters of the composite oxide particles 3 and the composite oxynitride particles 4 may be 3 ⁇ m or less, respectively.
  • the composite oxide particles 3 and the composite oxynitride particles 4 are interspersed between the AlN particles 2.
  • the structure of the fractured surface or mirror-polished surface of the AlN sintered body 1 is observed using a scanning electron microscope (SEM), a scanning transmission electron microscope (STEM), a transmission electron microscope (TEM) or the like with an element analyzer. The presence of particles and grain boundary layers may be confirmed. In addition, elemental analysis of the observed particles and grain boundary layers may be performed to confirm the components of the particles and grain boundary layers.
  • the content of Mg contained in the AlN particles 2, that is, the solid solution amount of Mg dissolved in the AlN particles 2 is, for example, 0.1 to 100% when the total metal elements contained in the AlN particles 2 are 100 mol%. It may be 1.0 mol%, particularly 0.3 to 0.6 mol%.
  • the resistivity of the AlN particles 2 can be increased.
  • the thermal conductivity of the AlN particles 2 can be maintained high.
  • the content of Mg contained in the AlN particles 2 is determined by using a fractured surface of the AlN-based sintered body 1 or a mirror-polished cross-section, wavelength dispersive X-ray spectroscopy (WDS), energy dispersive X-rays of the AlN particles 2. It is obtained by performing local elemental analysis such as spectroscopy (EDS) and secondary ion mass spectrometry (SIMS).
  • WDS wavelength dispersive X-ray spectroscopy
  • EDS energy dispersive X-rays of the AlN particles 2. It is obtained by performing local elemental analysis such as spectroscopy (EDS) and secondary ion mass spectrometry (SIMS).
  • the kind of rare earth element forming the composite oxide particle 3 is not particularly limited.
  • rare earth elements include Y, La, Ce, Ho, Gd, Nd, Sm, Dy, Yb, Er, and Lu.
  • Y yttrium
  • Y easily forms a garnet-type crystal structure with Al, and has high efficiency in reducing the amount of oxygen dissolved in the AlN crystal.
  • a composite oxide of Y and Al also referred to as Y 3 Al 5 O 12 , YAG
  • a garnet-type crystal structure is higher than a garnet-type composite oxide formed by other rare earth elements with Al.
  • Has volume resistivity. Presence of the garnet-type composite oxide 3 in the AlN sintered body 1 can be confirmed by X-ray diffraction (XRD) measurement of the AlN sintered body 1.
  • the thermal conductivity and plasma resistance of the AlN sintered body 1 are greatly affected by the denseness of the AlN sintered body 1.
  • the open porosity of the AlN sintered body 1 may be 0.2% or less.
  • the aluminum nitride sintered body 1 of the present embodiment may be produced as follows. For example, as a raw material, aluminum nitride powder having a purity of 99% or more, an average particle size of 0.5 ⁇ m to 1.0 ⁇ m, and an oxygen content of 1.2% by weight or less, and a purity of 99% or more and an average particle size of 0.5 ⁇ m to 1.
  • the aluminum nitride powder is sometimes referred to as AlN powder
  • the compound containing magnesium (Mg) is sometimes referred to as Mg-containing compound.
  • R represents shows the rare-earth element
  • Mg-containing compound Add 0.3 mol% to 4.0 mol% (in terms of MgO) and mix to create a mixed powder.
  • the addition amount of the additive is expressed in terms of oxide.
  • An organic binder is appropriately added to the obtained mixed powder and molded into a predetermined shape to obtain a molded body.
  • the obtained molded body is fired at a predetermined maximum temperature and firing profile in a nitrogen atmosphere to obtain the AlN sintered body of the present embodiment.
  • the amount of rare earth oxide powder added is 0.08 mol% or more in terms of oxide with respect to 100 mol% of AlN powder, thereby reducing the oxygen contained in AlN particles 2 and increasing the resistivity of AlN particles 2. Can do.
  • the addition amount of the rare earth oxide powder is 1.2 mol% or less, a garnet-type crystal structure of the rare earth element and Al is easily formed, and other perovskite type (RAlO 3 ), melilite type (R 4 Al 2). Other crystal structures with low resistivity and thermal conductivity at high temperatures such as O 9 ) are less likely to be formed. Thereby, the volume resistivity and thermal conductivity of the AlN-based sintered body 1 can be increased.
  • the addition amount of the rare earth oxide powder may be 0.15 mol% to 0.45 mol% in particular.
  • the rare earth compound added to the AlN powder may be an organic salt, an inorganic salt, or a solution thereof.
  • Al vacancies present in the AlN particles 2 can be reduced by setting the amount of the Mg-containing compound powder to 0.3 mol% or more in terms of oxide with respect to 100 mol% of the AlN powder.
  • the amount of Mg-containing compound powder added may be 0.5 mol% to 1.7 mol% in particular.
  • the Mg-containing compound to be added to the AlN powder in addition to magnesium oxide, magnesium hydroxide, and magnesium carbonate, organic salts, inorganic salts, and solutions thereof may be used. Among these, magnesium hydroxide decomposes during heating, and the surface activity of the decomposed powder is high. Therefore, when used as an Mg-containing compound, Mg is easily dissolved in the AlN particles 2.
  • the addition of 1.0 mol% of the rare earth compound in terms of oxide to 100 mol% of the AlN powder means that the rare earth compound corresponding to 1.0 mol of R 2 O 3 is added to 100 mol of AlN. means. Further, adding 1.0 mol% of the Mg-containing compound in terms of oxide to 100 mol% of the AlN powder means adding an Mg-containing compound corresponding to 1.0 mol of MgO to 100 mol of AlN. To do.
  • the AlN sintered body 1 having a high volume resistivity and thermal conductivity can be obtained efficiently.
  • the raw materials may be mixed by a known method such as a rotary ball mill, a vibration ball mill, a bead mill, or high-speed stirring.
  • a known molding may be used as the molding method. Specific molding methods include, for example, a die press, a cold isostatic press, a sheet molding method such as a doctor blade method and a rolling method, and extrusion molding.
  • Calcination may be performed under predetermined conditions as shown below.
  • the predetermined conditions are conditions relating to a temperature rising rate in the temperature rising process from 1500 ° C. to the maximum temperature, a maximum temperature and holding time, and a cooling rate in the cooling process from the maximum temperature to 1400 ° C.
  • the temperature rising rate is 0.5 ° C./min to 5.0 ° C./min.
  • the rate of temperature rise is 5.0 ° C./min or less, a time for the rare earth element to react with oxygen present in the AlN during the temperature rising process is secured, and a time for Mg to diffuse into the AlN particles 2 is secured. Is done.
  • AlN and MgO react near the surface of the AlN particles 2 to form a solid solution. This solid solution forms MgAlON in the subsequent holding process at the maximum temperature.
  • the heating rate By setting the heating rate to 0.5 ° C./min or more, the grain growth of the AlN particles 2 is suppressed, and a dense AlN-based sintered body 1 is obtained.
  • the phase of a compound other than AlN formed on the surface of the AlN particles 2 during this temperature raising process is generally referred to as a grain boundary phase.
  • the maximum temperature for firing is 1700 ° C to 1900 ° C.
  • the maximum temperature for firing may be in the range of 1750 ° C. to 1850 ° C. from the viewpoint of progress of densification and suppression of grain growth.
  • the holding time at the maximum temperature may be arbitrarily changed according to the average particle diameter of the raw material, the specific surface area, the filling rate of the molded body, and the size of the molded body.
  • the cooling rate may be 0.3 ° C / min to 5.0 ° C / min.
  • the surface tension changes between the AlN particles 2 and the grain boundary phase as the temperature decreases.
  • the cooling rate By setting the cooling rate to 0.3 ° C./min or more, grain growth of the AlN particles 2 is suppressed, and a dense AlN-based sintered body 1 is obtained.
  • the cooling rate By setting the cooling rate to 5.0 ° C./min or less, the time for the grain boundary phase to move is secured according to the change in the surface tension between the AlN particles 2 and the grain boundary phase.
  • the grain boundary phase gathers from the grain boundary between the two faces to the grain boundary triple point, or the grain boundary phase locally aggregates at the grain boundary between the two faces to form particles, and the composite oxide particles between the AlN particles 2 3 and the AlN-based sintered body 1 having a structure interspersed with the composite oxynitride particles 4.
  • Such an AlN sintered body 1 has a portion where the AlN particles 2 are in direct contact with each other at the grain boundary. As a result, the AlN sintered body 1 having a high thermal conductivity and volume resistivity is obtained.
  • a specific temperature in the heating process and a specific temperature in the cooling process are held for a predetermined time.
  • the process may be added to the firing step.
  • the AlN-based sintered body 1 of the present embodiment contains 0.5% by mass or less of Si, Ca, Ti, Mn, Ni, Mo, W, etc. in addition to the above-described Al, Mg, rare earth elements (R) as metal elements. It may contain in the range of. By adding these metal elements, the sinterability and the bondability with the electrode can be improved without deteriorating the desired function.
  • FIG. 2 is a perspective view showing one example of an electrostatic chuck which is a semiconductor holding device
  • FIG. 3 is a sectional view taken along line iii-iii of FIG.
  • the electrostatic chuck 11 includes an electrostatic chucking electrode 13 on the surface of an insulating ceramic base 12.
  • a dielectric layer 14 is provided on the surface of the ceramic substrate 12 so as to cover the electrostatic attraction electrodes 13.
  • the upper surface of the dielectric layer 14 is an adsorption surface 16 that adsorbs an object 15 such as a Si wafer.
  • a power supply terminal 17 electrically connected to the electrostatic attracting electrode 13 is provided.
  • the dielectric layer 14 uses the aluminum nitride sintered body 1 of the present embodiment that is excellent in mechanical strength and thermal shock resistance, has high volume resistivity, high thermal conductivity, and high corrosion resistance to halogen-based gas.
  • the ceramic substrate 12 may be formed of an insulating ceramic such as alumina, silicon nitride, or aluminum nitride.
  • an insulating ceramic such as alumina, silicon nitride, or aluminum nitride.
  • simultaneous firing with the aluminum nitride sintered body 1 constituting the dielectric layer 14 becomes possible.
  • the ceramic base 12 with the aluminum nitride sintered body 1 similarly to the dielectric layer 14, the difference in thermal expansion coefficient between the ceramic base 12 and the dielectric layer 14 is reduced. As a result, deformation such as warpage and distortion is less likely to occur during firing, and the electrostatic chuck 11 with high reliability can be obtained.
  • the electrostatic chucking electrode 13 and the power supply terminal 17 may be formed of a heat-resistant metal such as tungsten, molybdenum, or platinum. These refractory metals have a thermal expansion coefficient similar to that of the aluminum nitride sintered body 1 constituting the ceramic substrate 12. Therefore, when these heat-resistant metals are used for the electrostatic chucking electrode 13 and the power feeding terminal 17, the adhesion between the electrostatic chucking electrode 13 and the power feeding terminal 17 and the ceramic substrate 12 during firing and heating is high. Become. When the power supply terminal 17 is exposed to corrosive gas, the power supply terminal 17 may be formed using an iron-cobalt-chromium alloy.
  • FIGS. 2 and 3 show the electrostatic chuck 11 having only the electrostatic chucking electrode 13 inside the ceramic base 12.
  • the electrostatic chuck 11 has a heater electrode in addition to the electrostatic chucking electrode 13. May be buried. By embedding the heater electrode, the electrostatic chuck 11 can directly generate heat, and heat loss can be greatly reduced as compared with the indirect heating method.
  • FIG. 4 is a perspective view showing another example of an electrostatic chuck which is a semiconductor holding device
  • FIG. 5 is a cross-sectional view taken along the line vv of FIG.
  • the electrostatic chuck 11 includes an insulating base 12 having insulating properties and a disk-shaped dielectric plate 14 made of the aluminum nitride sintered body 1 of the present embodiment.
  • An electrostatic chucking electrode 13 is formed on the lower surface of the dielectric plate 14.
  • the insulating base 12 and the dielectric plate 14 are bonded via a bonding agent 18 such as glass, brazing material, or adhesive.
  • the electrostatic chucking electrode 13 is built in between the insulating substrate 12 and the dielectric plate 14.
  • the upper surface of the dielectric plate 12 is an adsorption surface 16 that adsorbs an object 15 such as a Si wafer.
  • a power supply terminal 17 electrically connected to the electrostatic attracting electrode 13 is provided.
  • the insulating substrate 12 may be formed of an insulating material such as various ceramics such as sapphire, alumina, silicon nitride, and aluminum nitride.
  • the material of the electrostatic chucking electrode 13 may be a metal such as copper or titanium, TiN, TaN, WC, or the like.
  • the electrostatic chucking electrode 13 may be formed on the lower surface of the dielectric plate 14 by a method such as vapor deposition, metallization, plating, PVD, or CD.
  • the electrostatic chuck 11 can be easily manufactured by separately preparing the dielectric plate 14 and the insulating substrate 12 and bonding them with the bonding agent 18.
  • the example of the monopolar electrostatic chuck 11 is shown, but a bipolar electrostatic chuck may be used.
  • the substrate 12 of the semiconductor holding device may include a flow path for flowing a heat medium therein.
  • a heat medium By flowing a heat medium through a flow path provided inside the base body 12, the temperature control of the fixed object 15 fixed to the suction surface 16 can be performed more easily.
  • IPA isopropyl alcohol
  • the produced molded body was heat-treated in vacuum to remove the binder.
  • the molded body from which the binder has been removed is placed in a firing container made of aluminum nitride, and is subjected to nitriding by performing normal pressure firing in a nitrogen atmosphere at the firing conditions shown in Table 1, that is, the heating rate, the holding temperature and time, and the cooling rate.
  • An aluminum (AlN) sintered body was obtained.
  • the open porosity of the obtained AlN sintered body was calculated from density measurement by Archimedes method.
  • Table 2 shows the open porosity of the AlN sintered body.
  • the structure of the obtained AlN sintered material was analyzed by a scanning electron microscope (SEM) and wavelength dispersive X-ray spectroscopy (WDS).
  • SEM scanning electron microscope
  • WDS wavelength dispersive X-ray spectroscopy
  • the Mg content of the AlN particles was confirmed by mirror-polishing the cross section of the aluminum nitride sintered body, discriminating the AlN particles by SEM observation, and elemental analysis of the central portion of the AlN particles. Elemental analysis of AlN particles was performed on 10 AlN particles for each sample, and the average value of Mg content was determined. Table 2 shows the Mg content of the AlN particles.
  • the presence / absence and form of the composite oxide containing rare earth element and Al and the composite oxynitride containing Mg and Al were confirmed by SEM observation of the fracture surface of the AlN sintered body.
  • the presence / absence of composite oxide particles and composite oxynitride particles was judged by confirming elemental analysis of phases other than AlN and the aspect ratio thereof.
  • the composite oxide and composite oxynitride confirmed in the cross section of the AlN sintered body the case where the particulate composite oxide and composite oxynitride are 30% or more in area ratio is marked with ⁇ , and the AlN particles are coated As shown in Table 2, the case where it was composed of continuous grain boundary layers was marked as x. Note that the composite oxide and the composite oxynitride were regarded as particles when the aspect ratio between the maximum length and the minimum length in the cross section was 5 or less.
  • the crystal structure of the complex oxide containing rare earth elements and Al was confirmed by X-ray diffraction (XRD) measurement of the AlN sintered body.
  • the compound containing Mg and Al was confirmed by local elemental analysis of the cross-sectional structure of the AlN sintered body and shown in Table 2. Since MgAl 2 O 4 crystal and MgAlON crystal may overlap with XRD peaks, the particle or grain boundary phase in which only local elemental analysis Mg, Al, O is detected is MgAl 2 O 4, and Mg, Al, The particle or grain boundary phase in which O and N were detected was MgAlON.
  • the volume resistivity of the AlN sintered body was measured based on JIS2141.
  • Table 2 shows the volume resistivity at 700 ° C. of each sample.
  • the thermal conductivity of the AlN sintered body was measured by a laser flash method. The results are shown in Table 2.
  • the plasma resistance of the AlN sintered material was evaluated using a plasma reactor device.
  • a mixed gas of CF 4 , CHF 3 and Ar was used as the fluorine-based gas.
  • the mixing ratio was 20% by volume for CF 4 , 40% by volume for CHF 3, and 40% by volume for Ar.
  • the AlN sintered body was mirror polished surface was placed in a chamber of the plasma reactor apparatus, a mixed gas is introduced into the chamber, with the pressure held in 10Pa in the chamber, power of 0.8 W / cm 2
  • a high-frequency plasma was generated in order to etch the AlN sintered body for 2 hours.
  • Plasma resistance is expressed in terms of etching rate ( ⁇ m / h) and is shown in Table 2.
  • 1 to 12, 14 to 22 and 25 to 29 are AlN particles in which Mg is dissolved, composite oxide particles containing a rare earth element and Al and having a garnet-type crystal structure, and composite oxynitriding containing Mg and Al All of them had high properties such that the volume resistivity at 700 ° C. exceeded 1 ⁇ 10 6 ⁇ m and the thermal conductivity was 120 W / mK or more. Moreover, it had high corrosion resistance against halogen gas plasma.
  • sample no. 1 to 8, 14 to 22, and 25 to 29 are composed of composite oxide particles containing rare earth elements and Al having a garnet type crystal structure, and have a high volume of 1.2 ⁇ 10 7 ⁇ m or more at 700 ° C. Had resistivity.
  • Aluminum nitride sintered body 2 Crystal particles of aluminum nitride 3: Particles of composite oxide containing rare earth element and Al 4: Particles of composite oxynitride containing Mg and Al 11: Electrostatic chuck 12: Substrate 13: Electrostatic chucking electrode 14: Dielectric layer 15: Fixed object 16: Suction surface 17: Feeding terminal 18: Bonding material

Abstract

窒化アルミニウム質焼結体１は、Ｍｇを含む窒化アルミニウムの結晶粒子２と、ガーネット型の結晶構造を有し、希土類元素とＡｌとを含む複合酸化物と、ＭｇとＡｌとを含む複合酸窒化物と、を含む。窒化アルミニウムの結晶粒子２間には、複合酸化物の粒子３および複合酸窒化物の粒子４が点在している。複合酸化物はＹを含んでもよい。窒化アルミニウムの結晶粒子２は、含有する全金属元素を１００ｍｏｌ％としたとき、Ｍｇの含有量が０．１ｍｏｌ％以上１．０ｍｏｌ％以下であってもよい。半導体保持装置は、この窒化アルミニウム質焼結体１と静電吸着用電極１３とを備える。

Description

窒化アルミニウム質焼結体、および半導体保持装置
　本開示は、窒化アルミニウム質焼結体、および半導体保持装置に関する。
　半導体製造のドライプロセス（成膜、洗浄、ドライエッチングなど）に用いられる半導体製造装置には、成膜用、エッチング用、またはクリーニング用として、反応性の高いＦ、Ｃｌ等のハロゲン系プラズマが使用される。このような半導体製造装置に使用される半導体ウェハを保持する部品、たとえばヒータ、静電チャックなどの材料として、窒化アルミニウム質焼結体が用いられている。窒化アルミニウム質焼結体は、高い機械的強度、高い耐熱衝撃性、高い体積抵抗率、高い熱伝導率、及びハロゲン系ガスへの高い耐食性を有している。ハロゲン系ガスへの耐食性が高い場合、ハロゲン系プラズマに対する耐食性も高い。以下、プラズマに対する耐食性を耐プラズマ性という場合もある。
　半導体集積回路には、さらなる微細化および高密度化が要求されている。半導体集積回路をさらに微細化および高密度化する手段の一つとして、半導体ウェハなどを例えば６００℃以上の高温で加工処理することが試みられている。しかしながら、通常の窒化アルミニウム質焼結体は、このような高温では電気抵抗率が１０6Ωｍ以下に低下し、絶縁性を維持することが困難であった。
　高温領域における絶縁性に優れた窒化アルミニウム質焼結体として、マグネシウム、またはマグネシウムを含む化合物を添加した窒化アルミニウム質焼結体が知られている。例えば、特許文献１では、スパークプラグの絶縁碍子として、マグネシウムを含む粒界相を備えた、７００℃での絶縁抵抗が高い窒化アルミニウムのセラミック焼結体が開示されている。特許文献２では、８００℃における体積抵抗率が高い窒化アルミニウム焼結体として、窒化アルミニウムと希土類化合物とＭｇＡｌ2Ｏ4とを含む窒化アルミニウム焼結体が開示されている。
特開平４－１１８８８３号公報 特開２００２－２２０２８２号公報
　本開示の窒化アルミニウム質焼結体は、Ｍｇを含む窒化アルミニウムの結晶粒子と、ガーネット型の結晶構造を有し、希土類元素とＡｌとを含む複合酸化物と、ＭｇとＡｌとを含む複合酸窒化物と、を含み、前記窒化アルミニウムの結晶粒子間に、粒子状の前記複合酸化物および前記複合酸窒化物が点在している。
　本開示の半導体保持装置は、窒化アルミニウム質焼結体と、静電吸着用電極とを備え、前記窒化アルミニウム質焼結体が、上述の窒化アルミニウム質焼結体である。
窒化アルミニウム質焼結体の実施形態の一つにおける組織を模式的に示す断面図である。 静電チャックの例の一つを示す斜視図である。 図２のｉｉｉ－ｉｉｉ線断面図である。 静電チャックの別の例を示す斜視図である。 図４のｖ－ｖ線断面図である。
　本実施形態の窒化アルミニウム質焼結体１は、図１に示すように、Ｍｇを含む窒化アルミニウムの結晶粒子２と、希土類元素とＡｌとを含む複合酸化物と、ＭｇとＡｌとを含む複合酸窒化物と、を含む。窒化アルミニウムの結晶粒子２間には、粒子状の複合酸化物および複合酸窒化物、すなわち複合酸化物の粒子３および複合酸窒化物の粒子４が点在している。ここで、粒子状であるとは、たとえば断面の最大長さと、最小長さまたは厚みとのアスペクト比が、５以下の場合とする。
　窒化アルミニウム結晶は、ＡｌとＮとが１：１の割合で存在し結晶格子を形成している。窒化アルミニウム結晶に酸素（Ｏ）が固溶すると、Ａｌの空孔が生成される。これは、ＡｌとＯとが２：３の割合で安定となるためである。Ａｌの空孔は高温で導電キャリアとなるため、酸素が固溶した窒化アルミニウム結晶を有する窒化アルミニウム焼結体は高温で絶縁抵抗が低下する。以下、絶縁抵抗に替えて体積抵抗率で説明する場合もある。
　本実施形態の窒化アルミニウム質焼結体１は希土類元素を含むため、窒化アルミニウムの結晶粒子２に固溶した酸素の一部が希土類元素と反応する。その結果、窒化アルミニウムの結晶粒子２の酸素の固溶量が少なくなる。窒化アルミニウム質焼結体１に含まれる希土類元素の量が多いほど、窒化アルミニウムの結晶粒子２に固溶した酸素の固溶量は少なくなる。
　また、窒化アルミニウムの結晶粒子２がＭｇを含む、すなわち窒化アルミニウムの結晶粒子２にＭｇが固溶していることで、窒化アルミニウムの結晶粒子２中に固溶した酸素とＭｇとが結合する。その結果、窒化アルミニウムの結晶粒子２中におけるＡｌ空孔の生成が抑制され、高温でも高い絶縁抵抗を維持できる。以下、窒化アルミニウムを単にＡｌＮという場合もある。たとえば、窒化アルミニウム質焼結体１を単にＡｌＮ質焼結体１といい、窒化アルミニウムの結晶粒子２を単にＡｌＮ粒子２という場合もある。
　さらに、本実施形態では、希土類元素とＡｌとを含む複合酸化物の粒子３がガーネット型の結晶構造を有している。希土類元素とＡｌとの複合酸化物は、希土類元素（Ｒ）とＡｌとの比率に応じてガーネット型（Ｒ3Ａｌ5Ｏ12）、ペロブスカイト型（ＲＡｌＯ3）、メリライト型（Ｒ4Ａｌ2Ｏ9）など種々の結晶構造を形成する。その中で、ガーネット型の結晶構造を有する複合酸化物は、特に高温での絶縁抵抗が高い。したがって、窒化アルミニウム質焼結体１に含まれる粒子３、すなわち希土類元素とアルミニウムの複合酸化物が、ガーネット型の結晶構造を有することにより、本実施形態の窒化アルミニウム質焼結体１の高温における体積抵抗率が高くなる。以下、希土類元素とＡｌとの複合酸化物を単に複合酸化物といい、希土類元素とＡｌとを含む複合酸化物の粒子３を単に複合酸化物粒子３という場合もある。
　ガーネット型以外の結晶構造を有する複合酸化物は、窒化アルミニウム質焼結体１中に実質的に存在しなくてもよい。換言すれば、本実施形態の窒化アルミニウム質焼結体１では、Ｘ線回折（ＸＲＤ）測定により、ガーネット構造以外の複合酸化物の結晶相が検出されなくてもよい。
　本実施形態のＡｌＮ質焼結体１は、さらに、ＭｇとＡｌとを含む複合酸窒化物の粒子４を含んでいる。ＭｇとＡｌとの複合酸窒化物（ＭｇＡｌＯＮ）は、ＭｇＡｌ2Ｏ4、ＭｇＯなどのＭｇを含む酸化物よりも耐プラズマ性が高い。このような複合酸窒化物が窒化アルミニウムの結晶粒子２間に存在することで、ＡｌＮ質焼結体１の耐プラズマ性が高くなる。
　また、ＭｇＡｌ2Ｏ4、ＭｇＯなどのＭｇを含む酸化物と比べて、ＭｇとＡｌとの複合酸窒化物（ＭｇＡｌＯＮ）の熱膨張係数は、ＡｌＮの熱膨張係数との差が小さい。したがって、ＡｌＮの結晶粒子２間にＭｇＡｌ2Ｏ4およびＭｇＯが存在する場合と比べ、本実施形態のようにＡｌＮの結晶粒子２間にＭｇとＡｌとの複合酸窒化物（ＭｇＡｌＯＮ）が存在する方が、ＡｌＮの結晶粒子２の粒界付近にかかる残留応力を小さくすることができ、ＡｌＮ質焼結体１の耐プラズマ性が高くなる。このように、本実施形態では、窒化アルミニウムの結晶粒子２間に、ＭｇとＡｌとを含む複合酸窒化物の粒子４が存在することにより、窒化アルミニウム質焼結体１の耐プラズマ性を高く維持することができる。以下、ＭｇとＡｌとを含む複合酸窒化物の粒子４を単に複合酸窒化物粒子４という場合もある。
　本実施形態において、複合酸化物粒子３、および複合酸窒化物粒子４は、ＡｌＮ粒子２間に点在している。すなわち、ＡｌＮ質焼結体１の断面において、複合酸化物粒子３および複合酸窒化物粒子４は、連続した粒界層としてＡｌＮ粒子２の表面を覆うのではなく、ＡｌＮ粒子２間の粒界三重点または二面間粒界に粒子として存在する。換言すれば、ＡｌＮ粒子２は、隣接する他のＡｌＮ粒子２と、他の相（複合酸化物結晶、複合酸窒化物などの粒界層）を介さず直接接している部分を所定の割合、たとえば３０％以上有する。ＡｌＮ粒子２同士が直接接している部分の割合は、たとえばＡｌＮ質焼結体１の断面において、ＡｌＮ粒子２の輪郭が他のＡｌＮ粒子２の輪郭と直接接している割合の平均としてもよい。
　ＡｌＮは高い熱伝導率を有するが、ＡｌＮ質焼結体１の熱伝導率は、ＡｌＮ粒子２の結晶構造や焼結体の組織により影響を受ける。たとえば、ＡｌＮ粒子２に酸素などの他の元素が固溶して結晶構造が乱れたり、ＡｌＮ粒子２間に熱伝導率の低い粒界層が介在すると、ＡｌＮ質焼結体１の熱伝導率は低下する。
　熱伝導率以外の特性、たとえばＡｌＮ粒子２の高温における絶縁性を高めるために、ＡｌＮ質焼結体１を焼成する際にＡｌＮ粒子２にＭｇを固溶させたり、希土類元素を添加してＡｌＮ粒子２に固溶した酸素の固溶量を少なくしようとした場合、余剰の添加成分が粒界相を形成してＡｌＮ粒子２の表面を覆い、隣接するＡｌＮ粒子２間の熱伝導が低下することがある。本実施形態では、ＡｌＮ粒子２に固溶しなかった複合酸化物および複合酸窒化物が、粒界層としてＡｌＮ粒子２の表面を覆うことなく、それぞれが複合酸化物粒子３、複合酸窒化物粒子４として、ＡｌＮ粒子２間の粒界三重点または二面間粒界に点在している。このような場合、隣接するＡｌＮ粒子２同士が直接接する部分を有するため、ＡｌＮ質焼結体１の熱伝導率を高く維持することができる。
　また、たとえば、複合酸化物または複合酸窒化物が低い体積抵抗率を有していても、このように複合酸化物粒子３、複合酸窒化物粒子４が点在している、すなわちＡｌＮ粒子２の粒界に連続して存在するのではなく、粒子状の複合酸化物および複合酸窒化物がそれぞれ独立に離間して存在することにより、ＡｌＮ質焼結体１の体積抵抗率を高く保持することができる。
　ＡｌＮ粒子２の平均粒径は、たとえば１０μｍ以下でもよい。また、１μｍ以上１０μｍ以下、さらに３μｍ以上８μｍ以下でもよい。ＡｌＮ粒子２の平均粒径を１０μｍ以下と小さくすることで、ＡｌＮ質焼結体１中の粒界が多くなる。粒界が多くなると、複合酸化物および複合酸窒化物が粒子状になって多くの粒界に分散する。その結果、複合酸化物粒子３および複合酸窒化物粒子４をＡｌＮ粒子２間の粒界に点在させることができる。また、複合酸化物粒子３および複合酸窒化物粒子４の平均粒径は、それぞれ３μｍ以下でもよい。ＡｌＮ粒子２、複合酸化物粒子３および複合酸窒化物粒子４の平均粒径をこのような範囲とすることでＡｌＮ質焼結体１の熱伝導率及び体積抵抗率を高く維持することができる。
　ＡｌＮ粒子２間に、複合酸化物粒子３および複合酸窒化物粒子４が点在していることは、たとえば、以下のようにして確認すればよい。ＡｌＮ質焼結体１の破断面、または鏡面研磨した断面を、元素分析装置付きの走査電子顕微鏡（ＳＥＭ）、走査透過電子顕微鏡（ＳＴＥＭ）、透過電子顕微鏡（ＴＥＭ）などを用いて組織観察し、粒子や粒界層の存在を確認すればよい。あわせて、観察された粒子や粒界層の元素分析を行い、粒子や粒界層の成分を確認すればよい。
　ＡｌＮ粒子２に含まれるＭｇの含有量、すなわちＡｌＮ粒子２に固溶しているＭｇの固溶量は、たとえば、ＡｌＮ粒子２に含まれる全金属元素を１００ｍｏｌ％としたとき、０．１～１．０ｍｏｌ％、特には０．３～０．６ｍｏｌ％としてもよい。ＡｌＮ粒子２に含まれるＭｇの含有量を０．１ｍｏｌ％以上とすることで、ＡｌＮ粒子２の抵抗率を高めることができる。ＡｌＮ粒子２に含まれるＭｇの含有量を１．０ｍｏｌ％以下とすることで、ＡｌＮ粒子２の熱伝導率を高く維持することができる。ＡｌＮ粒子２に含まれるＭｇの含有量は、ＡｌＮ質焼結体１の破断面、または鏡面研磨した断面を用いて、ＡｌＮ粒子２の波長分散型Ｘ線分光（ＷＤＳ）、エネルギー分散型Ｘ線分光（ＥＤＳ）、二次イオン質量分析（ＳＩＭＳ）などの局所元素分析を行うことにより得られる。
　複合酸化物粒子３を形成する希土類元素の種類は、特に限定されない。希土類元素としては、例えば、Ｙ、Ｌａ、Ｃｅ、Ｈｏ、Ｇｄ、Ｎｄ，Ｓｍ，Ｄｙ、Ｙｂ、Ｅｒ、Ｌｕなどが挙げられる。このうち、特にＹ（イットリウム）を用いてもよい。Ｙは、Ａｌとガーネット型の結晶構造を形成しやすく、ＡｌＮ結晶の酸素の固溶量を低減する効率が高い。また、ガーネット型の結晶構造を有するＹとＡｌとの複合酸化物（Ｙ3Ａｌ5Ｏ12、ＹＡＧともいう）は、他の希土類元素がＡｌと形成するガーネット型の複合酸化物に比べて高い体積抵抗率を有している。ＡｌＮ質焼結体１中におけるガーネット型の複合酸化物３の存在は、ＡｌＮ質焼結体１のＸ線回折（ＸＲＤ）測定により確認できる。
　なお、ＡｌＮ質焼結体１の熱伝導率および耐プラズマ性は、ＡｌＮ質焼結体１の緻密性にも大きく影響される。高い熱伝導率および耐プラズマ性を実現するため、ＡｌＮ質焼結体１の開気孔率は、０．２％以下でもよい。
　本実施形態の窒化アルミニウム質焼結体１は、以下のように作製してもよい。たとえば、原料として、純度９９％以上、平均粒径０．５μｍ～１．０μｍ、酸素含有量１．２質量％以下の窒化アルミニウム粉末と、純度９９％以上、平均粒径０．５μｍ～１．２μｍで比表面積ＢＥＴが３ｍ2／ｇ～１０ｍ2／ｇの希土類化合物粉末と、純度９９％以上、平均粒径０．５μｍ～１．２μｍのマグネシウム（Ｍｇ）を含む化合物の粉末、たとえば水酸化マグネシウム（Ｍｇ（ＯＨ）2）粉末、炭酸マグネシウム（ＭｇＣＯ3）粉末または酸化マグネシウム（ＭｇＯ）粉末と、を準備する。以下、窒化アルミニウム粉末をＡｌＮ粉末といい、マグネシウム（Ｍｇ）を含む化合物をＭｇ含有化合物という場合もある。
　ＡｌＮ粉末１００ｍｏｌ％に対し、希土類酸化物粉末を酸化物換算（Ｒ2Ｏ3換算、Ｒは希土類元素を示す）で０．０８ｍｏｌ％～１．２ｍｏｌ％、Ｍｇ含有化合物の粉末を酸化物換算（ＭｇＯ換算）で０．３ｍｏｌ％～４．０ｍｏｌ％添加して混合し、混合粉末を作成する。以下、特に明記しない限り、添加物の添加量は酸化物換算量で示す。得られた混合粉末に、適宜有機バインダを加え、所定の形状に成形して成形体を得る。
　得られた成形体を、窒素雰囲気中で、所定の最高温度および焼成プロファイルで焼成することにより、本実施形態のＡｌＮ質焼結体が得られる。
　希土類酸化物粉末の添加量を、ＡｌＮ粉末１００ｍｏｌ％に対し、酸化物換算で０．０８ｍｏｌ％以上とすることで、ＡｌＮ粒子２に含まれる酸素を低減してＡｌＮ粒子２の抵抗率を高めることができる。希土類酸化物粉末の添加量を１．２ｍｏｌ％以下とすることで、希土類元素とＡｌとのガーネット型結晶構造が形成されやすくなり、他のペロブスカイト型（ＲＡｌＯ3）、メリライト型（Ｒ4Ａｌ2Ｏ9）等、高温における抵抗率と熱伝導率が低い他の結晶構造が形成されにくくなる。これにより、ＡｌＮ質焼結体１の体積抵抗率と熱伝導率を高めることができる。希土類酸化物粉末の添加量は、特に０．１５ｍｏｌ％～０．４５ｍｏｌ％としてもよい。なお、ＡｌＮ粉末に添加する希土類化合物は、酸化物粉末のほか、有機塩類、無機塩類及びその溶液を用いてもよい。
　Ｍｇ含有化合物の粉末の添加量を、ＡｌＮ粉末１００ｍｏｌ％に対し、酸化物換算で０．３ｍｏｌ％以上とすることで、ＡｌＮ粒子２中に存在するＡｌ空孔を低減することができる。Ｍｇ含有化合物の粉末の添加量を、４．０ｍｏｌ％以下とすることで、Ｍｇの過剰な固溶を抑制し、ＡｌＮ粒子２の熱伝導率を維持することができる。Ｍｇ含有化合物の粉末の添加量は、特に０．５ｍｏｌ％～１．７ｍｏｌ％としてもよい。なお、ＡｌＮ粉末に添加するＭｇ含有化合物は、酸化マグネシウム、水酸化マグネシウム、炭酸マグネシウムのほか、有機塩類、無機塩類およびその溶液を用いてもよい。このうち、水酸化マグネシウムは加熱中に分解し、分解した粉末の表面活性が高いため、Ｍｇ含有化合物として用いるとＭｇがＡｌＮ粒子２に固溶しやすくなる。
　なお、ＡｌＮ粉末１００ｍｏｌ％に対し、希土類化合物を酸化物換算で１．０ｍｏｌ％添加するというのは、１００ｍｏｌのＡｌＮに対し、１．０ｍｏｌのＲ2Ｏ3に相当する希土類化合物を添加することを意味する。また、ＡｌＮ粉末１００ｍｏｌ％に対し、Ｍｇ含有化合物を酸化物換算で１．０ｍｏｌ％添加するというのは、１００ｍｏｌのＡｌＮに対し、１．０ｍｏｌのＭｇＯに相当するＭｇ含有化合物を添加することを意味する。
　また、ＡｌＮ粉末に含まれる酸素量を１．２質量％以下とすることで、高い体積抵抗率および熱伝導率を有するＡｌＮ質焼結体１を効率的に得られる。
　原料の混合は、公知の方法、例えば回転型ボールミル、振動型ボールミル、ビーズミル、高速撹拌などの方法を用いてもよい。成形方法は、周知の成形を用いてもよい。具体的な成形方法としては、たとえば、金型プレス、冷間静水圧プレス、ドクターブレード法や圧延法等のシート成形法、押出成形などが挙げられる。
　焼成は、下記に示すような所定の条件で行ってもよい。所定の条件とは、先ず、１５００℃から最高温度までの昇温過程における昇温速度、最高温度と保持時間、最高温度から１４００℃までの冷却過程における冷却速度に関する条件である。
　１５００℃から最高温度までの昇温過程では、昇温速度を０．５℃／ｍｉｎ～５．０℃／ｍｉｎとする。昇温速度を５．０℃／ｍｉｎ以下にすると、昇温過程で希土類元素がＡｌＮ中に存在する酸素と反応する時間が確保されるとともに、ＭｇがＡｌＮ粒子２の内部に拡散する時間が確保される。また、この昇温過程では、ＡｌＮ粒子２の表面付近でＡｌＮとＭｇＯとが反応して固溶体が形成される。この固溶体は、後の最高温度での保持過程で、ＭｇＡｌＯＮを形成する。昇温速度を０．５℃／ｍｉｎ以上とすることで、ＡｌＮ粒子２の粒成長が抑制され、緻密なＡｌＮ質焼結体１が得られる。なお、この昇温過程で、ＡｌＮ粒子２の表面に形成されるＡｌＮ以外の化合物の相を、総じて粒界相と称する。
　焼成の最高温度は、１７００℃～１９００℃とする。最高温度を１７００℃以上とすることで、前述の諸反応が十分に進行するとともに、緻密化が進行する。最高温度を１９００℃以下とすることで、ＡｌＮ粒子２の粒成長が抑制される。焼成の最高温度は、緻密化の進行と、粒成長の抑制という点から、１７５０℃～１８５０℃の範囲としてもよい。最高温度での保持時間は、原料の平均粒径、比表面積、成形体の充填率および成形体のサイズに応じて任意に変更してもよい。
　最高温度から１４００℃まで冷却する冷却過程では、冷却速度は０．３℃／ｍｉｎ～５．０℃／ｍｉｎとしてもよい。冷却過程では、温度の低下に伴いＡｌＮ粒子２と粒界相との間で表面張力が変化する。冷却速度を０．３℃／ｍｉｎ以上とすることで、ＡｌＮ粒子２の粒成長が抑制され、緻密なＡｌＮ質焼結体１が得られる。冷却速度を５．０℃／ｍｉｎ以下とすることで、ＡｌＮ粒子２と粒界相との表面張力の変化に応じて、粒界相が移動する時間が確保される。その結果、粒界相が二面間粒界から粒界三重点へ集まり、または二面間粒界において粒界相が局所的に凝集して粒子状となり、ＡｌＮ粒子２間に複合酸化物粒子３および複合酸窒化物粒子４が点在した組織を有するＡｌＮ質焼結体１となる。このようなＡｌＮ質焼結体１では、ＡｌＮ粒子２同士が粒界で直接接触している部分を有する。その結果、高い熱伝導率と体積抵抗率とを有するＡｌＮ質焼結体１となる。
　冷却過程において冷却速度が５．０℃／ｍｉｎを超えると、粒界相が移動する時間が確保し難くなる。したがって粒界相がＡｌＮ粒子２の表面を覆い、隣接するＡｌＮ粒子２間の熱伝導が低下する懸念がある。
　なお、上述のように昇温過程の昇温速度の制御、および冷却過程の冷却速度の制御に替えて、例えば昇温過程の特定の温度、および冷却過程の特定の温度で、所定時間保持する過程を焼成工程に加えてもよい。
　本実施形態のＡｌＮ質焼結体１は、金属元素として上述のＡｌ、Ｍｇ、希土類元素（Ｒ）のほか、Ｓｉ、Ｃａ、Ｔｉ、Ｍｎ、Ｎｉ、Ｍｏ、Ｗなどを０．５質量％以下の範囲で含有していてもよい。これらの金属元素を添加することにより、所望の機能を低下させることなく、焼結性、および電極との接合性を高めることができる。
　図２は、半導体保持装置である静電チャックの例の一つを示す斜視図であり、図３は、図２のｉｉｉ－ｉｉｉ線断面図である。静電チャック１１は、図３に示すように絶縁性を有するセラミック基体１２の表面に静電吸着用電極１３を備えている。セラミック基体１２の表面には、静電吸着用電極１３を覆うように誘電体層１４が設けられている。誘電体層１４の上面はＳｉウェハなどの被固定物１５を吸着する吸着面１６である。静電チャック１１の吸着面１６とは反対の面には、静電吸着用電極１３と電気的に接続された給電端子１７が設けられている。
　誘電体層１４は、機械的強度及び耐熱衝撃性に優れ、体積抵抗率が高く、熱伝導率が高く、ハロゲン系ガスへの耐食性が高い本実施形態の窒化アルミニウム質焼結体１を用いる。
　セラミック基体１２は、アルミナ、窒化珪素、窒化アルミニウム等の絶縁性を有するセラミックスで形成されてもよい。セラミック基体１２を、特に窒化アルミニウム質焼結体１で形成することにより、誘電体層１４を構成する窒化アルミニウム質焼結体１との同時焼成が可能となる。また、セラミック基体１２を、誘電体層１４と同様に窒化アルミニウム質焼結体１で形成することで、セラミック基体１２と誘電体層１４との間の熱膨張係数の差が低減される。その結果、焼成時に反りや歪み等の変形を生じにくくなり、信頼性の高い静電チャック１１を得ることができる。
　静電吸着用電極１３および給電端子１７は、タングステン、モリブデン、白金等の耐熱性金属により形成されてもよい。これらの耐熱性金属は、セラミック基体１２を構成する窒化アルミニウム質焼結体１に類似した熱膨張係数を有している。そのため、静電吸着用電極１３および給電端子１７にこれらの耐熱性金属を用いると、焼成時及び加熱時における、静電吸着用電極１３および給電端子１７と、セラミック基体１２との密着性が高くなる。また、給電端子１７が腐食性ガスに曝されるような場合、給電端子１７は鉄－コバルト－クロム合金を用いて形成されてもよい。
　図２、図３には、セラミック基体１２の内部に静電吸着用電極１３のみを備えた静電チャック１１を示したが、例えば、静電チャック１１に静電吸着用電極１３以外にヒータ電極を埋設してもよい。ヒータ電極を埋設することで、静電チャック１１を直接発熱させることができ、間接加熱方式の場合に比べて熱損失を大幅に押さえることができる。
　図４は半導体保持装置である静電チャックの他の例を示す斜視図であり、図５は図４のｖ－ｖ線断面図である。静電チャック１１は、絶縁性を有する絶縁性基体１２と、本実施形態の窒化アルミニウム質焼結体１からなる円盤状の誘電体板１４とを備えている。誘電体板１４の下面には静電吸着用電極１３が形成されている。絶縁性基体１２と誘電体板１４とは、ガラス、ロウ材、あるいは接着剤などの接合剤１８を介して接合されている。静電吸着用電極１３は、絶縁性基体１２と誘電体板１４との間に内蔵されている。誘電体板１２の上面はＳｉウェハなどの被固定物１５を吸着する吸着面１６である。静電チャック１１の吸着面１６とは反対の面には、静電吸着用電極１３と電気的に接続された給電端子１７が設けられている。
　絶縁性基体１２は、サファイア、アルミナ、窒化珪素、窒化アルミニウムなどの各種セラミックスなどの絶縁材料により形成されてもよい。静電吸着用電極１３の材質は、銅、チタンなどの金属やＴｉＮ、ＴａＮ、ＷＣなどであってもよい。静電吸着用電極１３は、誘電体板１４の下面に蒸着、メタライズ、メッキ、ＰＶＤ、ＣＤ等の方法により形成されてもよい。
　静電チャック１１は、誘電体板１４及び絶縁性基体１２をそれぞれ別々に作製しておき、接合剤１８により接合することで容易に製造できる。
　なお、上記の各例では単極型の静電チャック１１の例を示したが、双極型の静電チャックとしてもよい。
　図２、図３、図４、および図５に示したような、半導体保持装置の基体１２は、その内部に熱媒体を流す流路を備えていてもよい。基体１２の内部に設けた流路に熱媒体を流すことにより、吸着面１６に固定した被固定物１５の温度制御をより容易に行うことができる。
　原料として、純度９９％、平均粒径０．７μｍ、酸素含有量１．０質量％の窒化アルミニウム粉末、純度９９％以上、比表面積（ＢＥＴ）７ｍ2／ｇ以上の各種希土類酸化物粉末、および純度９９．５％、および平均粒径５μｍの水酸化マグネシウム（Ｍｇ（ＯＨ）2）粉末を、表１に示す比率で配合した。配合した原料に、溶媒としてイソプロピルアルコール（ＩＰＡ）を加え、ボールミルにより混合し、乾燥することで混合粉末を得た。
　得られた混合粉末１００質量部に対し、バインダとして８質量部のパラフィンワックスを添加した後、１００ＭＰａの圧力でプレス成形し、更に３００ＭＰａの静水圧処理を行い、直径６０ｍｍ、厚さ４ｍｍの円盤状の成形体を作成した。
　作製した成形体を真空中で熱処理し、バインダを除去した。バインダを除去した成形体を、窒化アルミニウム製の焼成容器に入れ、窒素雰囲気中、表１に示す焼成条件すなわち昇温速度、保持温度と時間、および降温速度で常圧焼成を行うことで、窒化アルミニウム（ＡｌＮ）質焼結体を得た。
　得られたＡｌＮ質焼結体の開気孔率は、アルキメデス法による密度測定から算出した。表２にＡｌＮ質焼結体の開気孔率を示す。
　得られたＡｌＮ質焼結体の組織を、走査型電子顕微鏡（ＳＥＭ）および波長分散型Ｘ線分光（ＷＤＳ）により分析した。ＡｌＮ粒子のＭｇ含有量は、窒化アルミニウム質焼結体の断面を鏡面研磨し、ＳＥＭ観察によりＡｌＮ粒子を判別して、ＡｌＮ粒子の中心部を元素分析することにより確認した。ＡｌＮ粒子の元素分析は、各試料１０個ずつのＡｌＮ粒子について行い、Ｍｇ含有量の平均値を求めた。ＡｌＮ粒子のＭｇ含有量を表２に示す。
　希土類元素とＡｌと含む複合酸化物と、ＭｇとＡｌとを含む複合酸窒化物の有無、およびその形態は、ＡｌＮ質焼結体の破断面をＳＥＭ観察することで確認した。複合酸化物粒子および複合酸窒化物粒子の有無は、ＡｌＮ以外の相の元素分析およびそのアスペクト比を確認して判断した。ＡｌＮ質焼結体の断面に確認された複合酸化物および複合酸窒化物のうち、粒子状の複合酸化物および複合酸窒化物が面積比で３０％以上の場合を○とし、ＡｌＮ粒子を被覆するように連続した粒界層で構成されていた場合を×として、表２に記載した。なお、複合酸化物および複合酸窒化物は、断面における最大長さと最小長さとのアスペクト比が５以下の場合を粒子状とみなした。
　希土類元素とＡｌと含む複合酸化物の結晶構造は、ＡｌＮ質焼結体のＸ線回折（ＸＲＤ）測定により確認した。ＭｇとＡｌとを含む化合物は、ＡｌＮ質焼結体の断面組織の局所元素分析により確認し、表２に示した。ＭｇＡｌ2Ｏ4結晶とＭｇＡｌＯＮ結晶とは、ＸＲＤのピークが重なる場合があるため、局所元素分析Ｍｇ、Ａｌ、Ｏのみが検出された粒子または粒界相をＭｇＡｌ2Ｏ4とし、Ｍｇ、Ａｌ、ＯおよびＮが検出された粒子または粒界相をＭｇＡｌＯＮとした。
　ＡｌＮ質焼結体の体積抵抗率は、ＪＩＳ２１４１に基づいて測定した。各試料の７００℃における体積抵抗率を表２に示す。ＡｌＮ質焼結体の熱伝導率は、レーザーフラッシュ法により測定した。結果を表２に示す。
　ＡｌＮ質焼結体の耐プラズマ性の評価は、プラズマリアクター装置を使用して行った。フッ素系のガスとして、ＣＦ4、ＣＨＦ3およびＡｒの混合ガスを用いた。混合比率は、ＣＦ4を２０体積％、ＣＨＦ3を４０体積％、Ａｒを４０体積％とした。表面を鏡面研磨したＡｌＮ質焼結体をプラズマリアクター装置のチャンバー内に設置し、混合ガスをチャンバー内に導入し、チャンバー内の圧力を１０Ｐａに保持した状態で、０．８Ｗ／ｃｍ2の電力で高周波プラズマを発生させ、ＡｌＮ質焼結体を２時間エッチングした。耐プラズマ性はエッチングレート（μｍ／ｈ）で表し、表２に示した。
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000002
　ＡｌＮ粒子を被覆する連続した粒界層が構成されていた試料Ｎｏ．３０、ＡｌＮ粒子にＭｇが固溶していない試料Ｎｏ．１３、２３および２４では、体積抵抗率、熱伝導率、耐プラズマ性のいずれかが低かったのに対し、試料Ｎｏ．１～１２、１４～２２、２５～２９は、Ｍｇが固溶したＡｌＮ粒子、希土類元素とＡｌとを含みガーネット型の結晶構造を有する複合酸化物粒子、およびＭｇとＡｌとを含む複合酸窒化物の粒子を含み、いずれも７００℃での体積抵抗率が１×１０6Ωｍを超え、熱伝導率が１２０Ｗ／ｍＫ以上と高い特性を有していた。また、ハロゲンガスのプラズマに対して高い耐食性を有していた。特に、試料Ｎｏ．１～８、１４～２２、２５～２９は、希土類元素とＡｌとを含む複合酸化物粒子がガーネット型の結晶構造を有するものからなり、７００℃で１．２×１０7Ωｍ以上という高い体積抵抗率を有していた。
　１：窒化アルミニウム質焼結体
　２：窒化アルミニウムの結晶粒子
　３：希土類元素とＡｌとを含む複合酸化物の粒子
　４：ＭｇとＡｌとを含む複合酸窒化物の粒子
１１：静電チャック
１２：基体
１３：静電吸着用電極
１４：誘電体層
１５：被固定物
１６：吸着面
１７：給電端子
１８：接合材

Claims (4)

  1. 　Ｍｇを含む窒化アルミニウムの結晶粒子と、
    　ガーネット型の結晶構造を有し、希土類元素とＡｌとを含む複合酸化物と、
    　ＭｇとＡｌとを含む複合酸窒化物と、を含み、
    　前記窒化アルミニウムの結晶粒子間に、粒子状の前記複合酸化物および前記複合酸窒化物が点在している、窒化アルミニウム質焼結体。
  2. 　前記複合酸化物がＹを含む、請求項１に記載の窒化アルミニウム質焼結体。
  3. 　前記窒化アルミニウムの結晶粒子に含まれる全金属元素を１００ｍｏｌ％としたとき、前記窒化アルミニウムの結晶粒子に含まれるＭｇが、０．１ｍｏｌ％以上１．０ｍｏｌ％以下である、請求項１または２に記載の窒化アルミニウム質焼結体。
  4. 　窒化アルミニウム質焼結体と、静電吸着用電極とを備え、
    前記窒化アルミニウム質焼結体が、請求項１～３のいずれかに記載の窒化アルミニウム質焼結体である、半導体保持装置。
PCT/JP2018/020519 2017-05-30 2018-05-29 窒化アルミニウム質焼結体、および半導体保持装置 WO2018221504A1 (ja)

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