Aln ceramic material for semiconductor heater component and manufacturing method thereof

Abstract

The present invention relates to an AlN ceramic material for a semiconductor heater component and a manufacturing method thereof. The AlN ceramic material for a semiconductor heater component according to the present invention includes titanium nitride (TiN), magnesium aluminate (MgAl2O4), and aluminum nitride (AlN).

Description

ALN ceramic material for semiconductor heater components and its manufacturing method

[0001] The present invention relates to an AlN ceramic material for a semiconductor heater component and a method for manufacturing the same.

[0002] Today, with the advancement of semiconductor components and advancements in semiconductor processing technology, manufacturing temperatures are rising and various chemicals are being introduced, making manufacturing conditions increasingly harsh. In semiconductor manufacturing, aluminum nitride (AlN) ceramic is typically used as a heater component. It boasts a similar coefficient of thermal expansion to Si wafers, excellent thermal conductivity and insulation, plasma resistance, and high volume resistivity.

[0003] Despite the excellent properties of AlN ceramic materials, it is difficult to sinter AlN as a single raw material due to its difficult sintering characteristics. Therefore, additives are added to improve the sintering density and thermal conductivity properties. Leading companies manufacturing AlN ceramic heaters are introducing various additives to achieve densification, porosity reduction, increased thermal conductivity, and improved bonding properties in order to produce materials with excellent sintering density / thermal conductivity when manufacturing ceramic heaters. Among these, products are manufactured by adding yttria, and the amount of yttria added is managed by each manufacturer when commercializing the product. Without the addition of yttria, it is difficult to achieve densification, porosity reduction, increased thermal conductivity, and improved bonding properties. However, the addition of these additive elements can increase the volume resistivity of the gas within a certain range of input amounts. However, by forming oxygen defects and secondary yttria oxides such as YAG and YAM within the gas, the volume resistivity can be reduced at high temperatures and the leakage current can increase.

[0004] Leakage current generated during semiconductor processing due to reduced high-temperature volume resistivity can affect semiconductor wafers during the semiconductor manufacturing process, resulting in reduced yield. This phenomenon is a common characteristic of ceramic materials, where volume resistivity decreases with increasing temperature. In AlN materials, the reduced volume resistivity and increased leakage current at high temperatures weaken the electrostatic force (wafer chucking force) of Si wafers, leading to defects such as wafer detachment.

[0005] Recently, as the semiconductor manufacturing process temperature has risen to over 500℃, the high-temperature process application area of ​​ceramic heaters has expanded, and there is a need to develop ceramic heaters with high resistance characteristics that can minimize leakage current at high temperatures.

[0006] The background technology described above is technology that the inventor possessed or acquired in the process of deriving the disclosure of the present application, and cannot necessarily be said to be publicly known technology disclosed to the general public prior to the present application.

[0007] In order to solve the above-described problem, the present invention aims to provide an AlN ceramic material for a semiconductor heater component having excellent volume resistance even at high temperatures and a method for manufacturing the same.

[0008] However, the problems to be solved by the present invention are not limited to the problems mentioned above, and other problems not mentioned can be clearly understood by a person having ordinary skill in the relevant technical field from the description below.

[0009] The AlN ceramic material for a semiconductor heater component according to the present invention includes titanium nitride (TiN), magnesium aluminate (MgAl2O4), and aluminum nitride (AlN).

[0010] According to one embodiment, the AlN ceramic material for the semiconductor heater component may be yttria-free.

[0011] According to one embodiment, the semiconductor heater component may be a plate of a semiconductor heater, a shaft of a semiconductor heater, or a combination thereof.

[0012] According to one embodiment, the magnesium aluminate (MgAl2O4) may exist as a secondary phase of the Mg-Al-O series.

[0013] According to one embodiment, the composition comprises two or more Mg-Al-O series secondary phase XRD peaks, wherein the XRD peaks may have a 2θ value of 44° to 46°.

[0014] In one embodiment, the XRD peak may be an yttria series XRD peak-free having a 2θ value of 28° to 30° or 33° to 35°.

[0015] In one embodiment, the crystal grain size may be from 1.5 μm to 2.5 μm.

[0016] According to one embodiment, the high temperature resistance value of 500°C or higher may be 1.0E+8 Ω·cm to 1.0E+10 Ω·cm.

[0017] According to one embodiment, the room temperature resistance value may be 1.0E+10 Ω·cm to 1.0E+12 Ω·cm.

[0018] In one embodiment, the relative density may be between 99.5% and 100.5%.

[0019] In one embodiment, the porosity may be from 0.02% to 0.2%.

[0020] According to one embodiment, the thermal conductivity may be 80 W / mK to 95 W / mK at room temperature and 40 W / mK to 50 W / mK at a high temperature of 500°C or higher.

[0021] A method for manufacturing an AlN ceramic material for a semiconductor heater component according to the present invention includes a step of forming a composite powder by mixing titanium dioxide (TiO2), magnesium oxide (MgO), and aluminum nitride (AlN); and a step of sintering the composite powder.

[0022] According to one embodiment, the titanium dioxide (TiO2) may be present in an amount of 0.2 to 0.5 parts by weight based on 100 parts by weight of the composite powder, and the magnesium oxide (MgO) may be present in an amount of 0.2 to 1.5 parts by weight based on 100 parts by weight of the composite powder.

[0023] According to one embodiment, the sintering step may be performed at a temperature of 1500°C to 2000°C.

[0024] According to one embodiment, the sintering step may be pressure sintering at a pressure of 5 MPa to 25 MPa per unit area.

[0025] The present invention can provide an AlN ceramic material for a semiconductor heater component having excellent volume resistance even at high temperatures and a method for manufacturing the same.

[0026] Specifically, the AlN ceramic material according to the present invention can solve the problem of performance and yield degradation due to leakage current while exhibiting excellent volume resistivity at high temperatures of 500°C or higher. Furthermore, it can exhibit excellent bonding and thermal conductivity even without additives such as yttria.

[0027] Figure 1 shows the results of XRD analysis of an example according to the present invention.

[0028] Figures 2a and 2b are the results of XRD analysis of examples and comparative examples of the present invention.

[0029] Figure 3 is a graph showing the relative density, porosity, and crystal grain size of examples and comparative examples of the present invention.

[0030] Figure 4 is a graph showing the volume resistance of examples and comparative examples of the present invention.

[0031] Figures 5a and 5b are graphs comparing the crystal grain size and volume resistivity of examples and comparative examples of the present invention.

[0032] Hereinafter, embodiments are described in detail with reference to the attached drawings. However, the embodiments may be modified in various ways, and the scope of the patent application is not limited or restricted by these embodiments. It should be understood that all modifications, equivalents, or alternatives to the embodiments are included within the scope of the patent application.

[0033] The terms used in the examples are for illustrative purposes only and should not be construed as limiting. Singular expressions include plural expressions unless the context clearly dictates otherwise. In this specification, terms such as "comprise" or "have" are intended to specify the presence of a feature, number, step, operation, component, part, or combination thereof described in the specification, but should be understood to not preclude the presence or addition of one or more other features, numbers, steps, operations, components, parts, or combinations thereof.

[0034] Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by a person of ordinary skill in the art to which the embodiments pertain. Terms defined in commonly used dictionaries should be interpreted as having a meaning consistent with their meaning in the context of the relevant technology, and shall not be interpreted in an idealized or overly formal sense unless explicitly defined herein.

[0035] In addition, when describing with reference to the attached drawings, the same components will be given the same reference numerals regardless of the drawing numbers, and redundant descriptions thereof will be omitted. When describing an embodiment, if it is determined that a detailed description of a related known technology may unnecessarily obscure the gist of the embodiment, the detailed description thereof will be omitted. In addition, when describing a component of an embodiment, terms such as first, second, A, B, (a), (b), etc. may be used. These terms are only to distinguish the component from other components, and the nature, order, or sequence of the component is not limited by the terms. When a component is described as being "connected," "coupled," or "connected" to another component, it should be understood that the component may be directly connected or connected to the other component, but another component may also be "connected," "coupled," or "connected" between each component.

[0036] Components included in one embodiment and components with common functions will be described using the same names in other embodiments. Unless otherwise stated, the descriptions given in one embodiment can be applied to other embodiments, and detailed descriptions will be omitted to the extent of overlap.

[0037]

[0038] The AlN ceramic material for a semiconductor heater component according to the present invention includes titanium nitride (TiN), magnesium aluminate (MgAl2O4), and aluminum nitride (AlN).

[0039] Semiconductor heaters, among the components used in semiconductor manufacturing equipment, secure and simultaneously heat wafers during the semiconductor manufacturing process. These heaters utilize ceramic materials and consist of a ceramic substrate and a heating element for generating heat. To maintain stable production during the wafer deposition process, ceramic substrates must possess plasma resistance and high volume resistivity at both low and high temperatures. Therefore, they require excellent electrical insulation and thermal conductivity. Therefore, ceramic materials, including aluminum nitride (AlN), which are stable at high temperatures and possess excellent physical properties such as electrical insulation and thermal conductivity, can be used as the main component of ceramic substrates. However, aluminum nitride has a volume resistivity that decreases with increasing temperature. Consequently, in ceramic heaters using aluminum nitride, the volume resistivity of the ceramic body decreases as temperature increases, which can result in leakage current. Meanwhile, recent semiconductor process temperatures have been increasing, leading to a sharp decrease in the volume resistivity of aluminum nitride ceramic heaters, resulting in leakage current. Therefore, a method for overcoming this problem of maintaining the volume resistivity of the ceramic material at high temperatures is required.

[0040] The AlN ceramic material for a semiconductor heater component according to the present invention includes titanium nitride and magnesium aluminate, thereby exhibiting excellent volume resistivity at high temperatures and having high-temperature region high-resistance characteristics, and can solve the problem of performance and yield degradation due to leakage current.

[0041] The above titanium nitride may be a secondary phase formed from titanium dioxide (TiO2), and the above magnesium aluminate may be a secondary phase formed from magnesium oxide (MgO).

[0042]

[0043] According to one embodiment, the AlN ceramic material for the semiconductor heater component may be yttria-free.

[0044] Conventional AlN ceramic materials for semiconductor heater components were manufactured by adding yttria to achieve densification, reduce porosity, increase thermal conductivity, and improve bonding characteristics. However, the addition of yttria has resulted in the generation of oxygen defects and yttria secondary phases such as YAG and YAM, which increase leakage current at high temperatures. The present invention provides an yttria-free ceramic material that exhibits excellent volume resistivity at high temperatures, while also providing an AlN ceramic material free from bonding problems.

[0045]

[0046] According to one embodiment, the semiconductor heater component may be a plate of a semiconductor heater, a shaft of a semiconductor heater, or a combination thereof.

[0047] The AlN material of the present invention may be applied only to the plate, only to the shaft, or to both in a semiconductor heater composed of a plate and a shaft.

[0048]

[0049] According to one embodiment, the magnesium aluminate (MgAl2O4) may exist as a secondary phase of the Mg-Al-O series.

[0050] The above secondary phase may be identified as a peak in an XRD profile measured at 40kv / 40mA using CuKα rays.

[0051]

[0052] According to one embodiment, the composition comprises two or more Mg-Al-O series secondary phase XRD peaks, wherein the XRD peaks may have a 2θ value of 44° to 46°.

[0053] There may be two or more XRD peaks indicating a secondary phase of the Mg-Al-O series. This may be because MgO is uniformly distributed and reacts within the material to form a certain amount or more of the Mg-Al-O phase. Preferably, two XRD peaks may be confirmed, and at least one of the XRD peaks may have a 2θ value of 44° to 46°.

[0054] Figure 1 is the result of analyzing XRD of an example according to the present invention. Referring to Figure 1, two peaks of Mg-O-Al series secondary phases and a TiN secondary phase can be confirmed.

[0055] In one embodiment, the TiN secondary phase XRD peak may have a 2θ value of 42° to 44°.

[0056]

[0057] The ratio of the diffraction peak intensity of titanium nitride to the diffraction peak intensity of aluminum nitride (TiN / AlN) may be 0.05% to 1%, and the ratio of the diffraction peak intensity of the secondary phase of Mg-Al-O series to the diffraction peak intensity of aluminum nitride (MgAl2O4 / AlN) may be 0.05% to 6%.

[0058] Compared to the main peak of aluminum nitride, when the secondary phases of titanium nitride and Mg-Al-O series exhibit diffraction peak intensities in the above range, an increase in intensity due to TiN and an increase in resistance due to Mg-Al-O can be exhibited, while a decrease in volume resistivity due to TiN and a decrease in thermal conductivity due to Mg-Al-O can be prevented.

[0059]

[0060] In one embodiment, the XRD peak may be an yttria series XRD peak-free having a 2θ value of 28° to 30° or 33° to 35°.

[0061] The AlN ceramic material according to the present invention is yttria-series XRD peak-free in the XRD profile, and peaks of yttria-series secondary phases do not appear. That is, since no yttria additive is added when manufacturing the AlN ceramic material, yttria-series secondary phases are not formed, and it may be yttria-series XRD peak-free. Since no XRD peaks are detected at all in the range of the 2θ value of 28° to 30° or 33° to 35°, it can be confirmed that it is yttria-free, and it can be confirmed that it does not contain a Y-Al-O secondary phase.

[0062] The above XRD measurement conditions may preferably be performed using an acceleration voltage / current of 40 kV / 40 mA, CuK α ray (wavelength 1.54060), a scan speed of 1° / min, and a range of 2θ of 10° to 80°.

[0063]

[0064] In one embodiment, the crystal grain size may be from 1.5 μm to 2.5 μm.

[0065] The above grain size, measured by EBSD, may be correlated with the density of grain boundaries (boundaries between crystals). As grains become smaller, the number of grain boundaries increases, which increases the potential barrier, which can hinder charge transfer. Furthermore, grain size is linked to thermal conductivity, and a certain level of thermal conductivity may be required to reduce temperature distribution deviations in the heater.

[0066] The size of the above crystal grains may preferably be 1.5 μm to 2.0 μm, or 2.0 μm to 2.5 μm. If the size of the crystal grains exceeds the above range, there may be a problem of reduced high-temperature volume resistance.

[0067] The measurement conditions for the above crystal grains may preferably be to photograph a mapped image at a magnification of 2,000x and an acceleration voltage of 20kV after mirror polishing so that the specimen roughness is at the level of Ra 0.09 to 0.03. The size of the crystal grains may be obtained by obtaining the median crystal grain based on the grain boundary of the photographed image.

[0068]

[0069] According to one embodiment, the high temperature resistance value of 500°C or higher may be 1.0E+8 Ω·cm to 1.0E+10 Ω·cm.

[0070] Preferably, it may be a resistance value measured with an AC resistor at a high temperature of 500°C to 650°C. Specifically, the analysis specimen for resistance measurement may be manufactured in a disk shape and measured by forming platinum (Pt) coated electrodes on both upper and lower ends. The measurement range may be 10 kHz to 10 mHz, the E range may be -10 V to 10 V, and the temperature may be increased from room temperature to 500°C in 100°C increments. The temperature may be measured 5 minutes after reaching and stabilizing the measurement temperature, thereby minimizing an error in electrical resistance characteristics due to temperature change.

[0071] If the high temperature resistance value is below the above range, the leakage current between the mesh and the molybdenum (Mo) heating wire cannot be blocked, making stable heater operation impossible, which may cause problems in stable production in the CVD process. That is, the resistance value of conventional AlN ceramic materials decreases at high temperatures, which causes leakage current to flow between the mesh and the Mo heating wire, which forms an electrostatic force. If the leakage current moves in the direction of the RF mesh, the RF mesh cannot perform its functions, such as wafer chucking and serving as a ground in the plasma process. The AlN ceramic material according to the present invention exhibits a high high temperature resistance value within the above range compared to conventional AlN materials, thereby blocking the leakage current between the mesh and the Mo heating wire, enabling stable heater operation and thus enabling stable production in the CVD process, thereby solving the problem of reduced performance and yield due to leakage current.

[0072]

[0073] According to one embodiment, the room temperature resistance value may be 1.0E+10 Ω·cm to 1.0E+12 Ω·cm.

[0074] The above room temperature may be 15°C to 25°C.

[0075] When the room temperature resistance value is within the above range, the heater can be operated. If it is below the above range, there may be a problem in which the heater cannot be used due to a number of impurities.

[0076]

[0077] In one embodiment, the relative density may be between 99.5% and 100.5%.

[0078] The above relative density is AlN 100% (3.26 g / cm 3) is based on the theoretical density of AlN ceramic material according to the present invention, and refers to a density that is compared to the density measured by the Archimedes method. If the relative density is below the above range, there may be problems such as a decrease in mechanical properties due to a decrease in sinterability and a decrease in thermal conductivity. If the relative density is within the above range, the heater can be operated without any problems in the use of the product.

[0079]

[0080] In one embodiment, the porosity may be from 0.02% to 0.2%.

[0081] The porosity is formed through a sintering process that fills empty spaces through movement and diffusion between powders in a sintering temperature range, and a state in which the porosity is close to 0 may indicate a single crystal state. The porosity may preferably be 0.02% to 0.15%; 0.02% to 0.1%; 0.02% to 0.05%; 0.05% to 0.2%; 0.05% to 0.15%; 0.05% to 0.1%; 0.1% to 0.2%; 0.1% to 0.15%; or 0.15% to 0.2%.

[0082] If the porosity is below the above range, there may be a problem of reduced volume resistivity due to the absence of potential walls in the absence of grain boundaries. If the porosity exceeds the above range, there may be a problem of reduced structural ceramic properties due to pores due to a significant increase in porosity. When the porosity is within the above range, the heater can be operated without any problems in the use of the product.

[0083]

[0084] According to one embodiment, the thermal conductivity may be 80 W / mK to 95 W / mK at room temperature and 40 W / mK to 50 W / mK at a high temperature of 500°C or higher.

[0085] If the thermal conductivity is below the above range, problems such as poor sinterability, decreased relative density, increased porosity, and deterioration of mechanical properties may occur. If it exceeds the above range, problems such as increased grain size and decreased grain boundary density may occur, resulting in decreased volume resistance. In particular, in order to minimize the temperature distribution deviation of the heater (below 10°C at 500°C), a certain level of thermal conductivity is required even at high temperatures, and therefore, a thermal conductivity within the above range may be desirable.

[0086]

[0087] A method for manufacturing an AlN ceramic material for a semiconductor heater component according to the present invention includes a step of forming a composite powder by mixing titanium dioxide (TiO2), magnesium oxide (MgO), and aluminum nitride (AlN); and a step of sintering the composite powder.

[0088] The step of forming the above composite powder may be to add titanium dioxide powder and magnesium oxide powder to aluminum nitride powder and mix them in a dry or wet manner.

[0089] In order to maintain the volume resistivity of a ceramic material at high temperatures, a metal-based additive may be added to aluminum nitride. However, the metal-based additive may lower the thermal conductivity of the ceramic heater, thereby worsening the temperature uniformity of the ceramic heater. The method for manufacturing an AlN ceramic material of the present invention can solve the above problem by forming a composite powder and granules to which titanium dioxide and magnesium oxide are added in appropriate amounts, thereby manufacturing the AlN ceramic material. Titanium dioxide can play a role in increasing the resistance when added in a small amount, and magnesium oxide can play a role in increasing the volume resistivity by forming a composite material. In addition, by not including yttria, it is possible to eliminate factors that may cause changes in resistance and thermal conductivity due to the formation of secondary phases such as YAG and YAM due to the formation of secondary phases with Mg and Ti, thereby enabling the stable manufacture of the material.

[0090]

[0091] According to one embodiment, the titanium dioxide (TiO2) may be present in an amount of 0.2 to 0.5 parts by weight based on 100 parts by weight of the composite powder, and the magnesium oxide (MgO) may be present in an amount of 0.2 to 1.5 parts by weight based on 100 parts by weight of the composite powder.

[0092] As the content of titanium dioxide increases, the high-temperature resistance of the AlN ceramic material decreases, and as the content of magnesium oxide increases, the crystal grain size may decrease, the high-temperature resistance may increase, or the porosity may increase. Therefore, it is necessary to form a composite powder that allows a reaction with AlN to occur in an appropriate range of amounts.

[0093] If the titanium dioxide content is below the above range, it exists as Ti within the material and does not affect the material itself, so the phase may not be confirmed. If it exceeds the above range, the low resistance characteristics of TiN may have the effect of reducing the resistance of the entire material, which may cause a problem of reduced volume resistance at high temperatures.

[0094] If the magnesium oxide content is outside the above range, it may cause volatilization during sintering, which may result in the formation of a large number of small pores, which may result in problems such as a decrease in material properties such as density, an increase in pores, and a decrease in structural characteristics and thermal conductivity characteristics. The content of magnesium oxide may preferably be 0.2 parts by weight to 1.0 parts by weight; 0.2 parts by weight to 0.5 parts by weight; 0.5 parts by weight to 1.5 parts by weight; 0.5 parts by weight to 1.0 parts by weight; or 1.0 parts by weight to 1.5 parts by weight.

[0095]

[0096] According to one embodiment, the sintering step may be performed at a temperature of 1500°C to 2000°C.

[0097] Through the above sintering, an AlN ceramic material for a semiconductor heater component including a secondary phase of TiN and Mg-Al-O series can be manufactured.

[0098] Preferably, it may be performed at a temperature of 1600°C to 2000°C, 1600°C to 1900°C, or 1700°C to 1900°C.

[0099] If the sintering temperature is below the above range, densification does not occur during sintering, and thus problems such as a decrease in density, an increase in porosity, a decrease in the physical properties of the structure, and a decrease in thermal conductivity may occur. If the sintering temperature is above the above range, problems such as an increase in the crystal grain size, a decrease in the crystal grain boundary, and a decrease in the volume resistivity may occur.

[0100]

[0101] According to one embodiment, the sintering step may be pressure sintering at a pressure of 5 MPa to 25 MPa per unit area.

[0102] The above pressure sintering may be a sintering process condition for densification under yttria-free conditions.

[0103] Preferably, it may be pressurized and sintered at a pressure of 5 MPa to 20 MPa; 5 MPa to 15 MPa; 5 MPa to 10 MPa; 10 MPa to 25 MPa; 10 MPa to 20 MPa; 10 MPa to 15 MPa; 15 MPa to 25 MPa; 15 MPa to 20 MPa; or 20 MPa to 25 MPa.

[0104] If the pressure is below the above range, problems such as a decrease in density, an increase in porosity, and a decrease in thermal conductivity may occur, and if the pressure exceeds the above range, problems such as a change in the distance between the heater and mesh (getting closer), an increase in leakage current, and a change in heat distribution may occur in the heater performance.

[0105]

[0106] Hereinafter, the present invention will be described in more detail by way of examples and comparative examples.

[0107] However, the following examples are only intended to illustrate the present invention, and the content of the present invention is not limited to the following examples.

[0108]

[0109] Example

[0110] An AlN ceramic material for semiconductor heater components was manufactured by sintering a composite powder mixed with titanium dioxide (TiO2), magnesium oxide (MgO), and aluminum nitride (AlN). The compositions of the examples and comparative examples are as shown in Table 1 below. The results of analyzing the secondary phases of the examples and comparative examples in which a TiN secondary phase and a Mg-Al-O secondary phase were confirmed are shown in Table 2 below.

[0111] First component (AlN, mass%) Second component (TiO2, mass%) Third component (MgO, mass%) Fourth component (Y2O3, mass%) Crystal phase Columnar phase Secondary phase Example 199.250.250.50AlNTiN,Mg-Al-O Example 298.750.2510AlNTiN,Mg-Al-O Example 398.250.251.50AlNTiN,Mg-Al-O Comparative example 198.750.750.50AlNTiN,Mg-Al-O Comparative example 298.250.7510AlNTiN,Mg-Al-O Comparative example 3100000AlN-Comparative example 495005AlNY-Al-O Comparative example 599.60.100.3AlNAl-O

[0112]

[0113] Item Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 XRD Secondary Phase (Phase Fraction) TiNO (0.10) O (0.11) O (0.09) O (0.8) O (0.77) Spinel (MgAl2O) O (2.0) O (2.3) O (5.7) O (2.6) O (5.0) Diffraction Peak Intensity Ratio (%) MgAl2O4 / AlN 1.5 5 1.7 8 5.9 9 2.8 0 3.15 Diffraction Peak Intensity Ratio (%) TiN / AlN 0.08 0.3 6 0.2 6 1.5 4 1.32

[0114] As shown in Table 1 above, the secondary phases of the examples and comparative examples were confirmed, and in the case of the comparative example to which yttria was added, Y-Al-O was confirmed as the secondary phase.

[0115]

[0116] Figures 2a and 2b show the results of XRD analysis of examples and comparative examples of the present invention. When XRD peak measurements are performed to confirm the crystallographic characteristics of AlN ceramic materials, it can be confirmed that secondary phases of the TiN and Mg-Al-O series are formed.

[0117] Referring to Figs. 2a, 2b and Table 2, the XRD peaks of Mg-Al-O were confirmed in the sections where the MgO content was 0.5 / 1 / 1.5 wt% in the composite powder phase, and were generated between 2-theta (2θ) 36° ~ 38° and 44° ~ 46°. In particular, the part where the 2nd peak of Mg-Al-O is generated between 44° ~ 46° in the XRD phase can be regarded as a characteristic of the high-temperature composition of the AlN ceramic material according to the present invention. That is, the appearance of only one main peak means that it was formed only at the seed level, and the appearance of multiple peaks of the Mg-Al-O phase means that the phase was formed with a certain or higher distribution. Consequently, the presence of multiple peaks for the Mg-Al-O phase means that a larger amount of the Mg-Al-O phase was formed, which may be affected by the process conditions such as the amount added and the dispersion of MgO. In addition, it can be confirmed that as the content of MgO increases, the intensity of the peak increases (intensity ratio compared to the AlN main peak), and that it shows a desirable range of 6% or less compared to the AlN main peak.

[0118] In the composite powder, the XRD peak of TiN was confirmed in the range of 0.25 / 0.75 wt% of TiO2 content, and was generated between 2-theta (2θ) 42° and 44°. In addition, as the content of TiO2 increases, the intensity of the peak increases (intensity ratio compared to the AlN main peak), and it can be confirmed that it shows a desirable range of 1% or less compared to the AlN main peak.

[0119]

[0120] The characteristics of the above examples and comparative examples, such as relative density, porosity, grain size, and volume resistivity, were analyzed and shown in Table 3, Figures 3, 4, 5a, and 5b below.

[0121]

[0122] Relative density (%)Porosity (%)Grain (μm)Volume resistivity (Ω cm)25℃500℃Example 199.8660.032.281.5E+114.8E+8Example 2100.1980.041.831.5E+111.1E+9Example 3100.450.181.894.0E+108.4E+8Comparative example 1100.4160.062.246.1E+109.4E+7Comparative example 2100.5190.101.745.5E+109.0E+7Comparative example 399.9810.094.962.1E+101.2E+6Comparative example 4101.5330.385.638.1E+101.4E+7Comparison example 599.0790.37.374.8E+112.4E+7

[0123] The relative density and porosity of the sintered body must satisfy the relative density of 99% or more and the porosity of 0.2% or less, which are possible for manufacturing structural ceramics. Referring to Table 3 and Fig. 3, it can be confirmed that the compositions of Examples 1 to 3 satisfy the target relative density and porosity. In particular, the grain growth control effect according to the increase in Mg is confirmed, and the grain growth control effect is clearly confirmed up to 0.5 to 1 wt%, but the limits of 1 wt% and 1.5 wt% were confirmed to have similar grain sizes. The porosity tends to increase according to the increase in Mg, and in the case of 1.5 wt%, due to the clear increase in porosity, a deterioration in the structural ceramic properties due to pores is expected at a higher increase, and therefore, it can be confirmed that the limit range of the Mg content is appropriate to be 1.5 wt% or less.

[0124]

[0125] For the measurement of volume resistivity, a sample with a thickness of 2 mm and a diameter of 12 mm was prepared as a specimen for measurement, and electrodes were formed on the upper and lower parts with a diameter of 12 mm and made of platinum. Bio-Logig's HTF-1100 and SP-300 equipment were used, and the measurement voltage was applied at 2.5 V and the measurement frequency was 10 mHz to 10 kHz, and the measurement was performed with an AC resistor.

[0126] Referring to Table 3 and Fig. 4 above, in the case of TiN, the case where the high temperature volume resistivity satisfies 1.0E+8 Ω·cm or more is satisfied when the amount of TiO2 introduced in the composite powder is 0.25 wt%, and this shows the characteristic of lowering the volume resistivity as the amount of TiN produced increases. The composition range that satisfies the high temperature volume resistivity of 1.0E+8 Ω·cm is the range of TiO2 0.2~0.5 wt% and MgO 0.2~1.5 wt% in the composite powder, which shows high temperature and high resistance characteristics. That is, in the step of forming a composite powder, the section that satisfies 1.0E+8 Ω·cm or more among the volume resistivity measured in the 500 ℃ range of the material sintered by adding TiO2 and MgO is the section with 0.25 wt% TiO2 input, and it can be expected that the volume resistivity will satisfy 1.0E+8 Ω·cm or more in the range of 0.2 to 0.5 wt%. In addition, the section that satisfies 1.0E+8 Ω·cm or more among the volume resistivity measured in the 500 ℃ range of the AlN ceramic material sintered by adding Ti and Mg oxides is the section with 0.5 / 1 / 1.5 wt% MgO input in TiO2 0.25 wt%, and it can be expected that the volume resistivity will satisfy 1.0E+8 Ω·cm or more in the range of 0.2 to 1.5 wt% MgO.

[0127] The high temperature volume resistance at 500 ℃ shows the maximum characteristic when the MgO content is 1 wt%, and the high temperature volume resistance decreases from 1.5 wt%, so the high temperature resistance characteristic is expected to deteriorate with further increase. In addition, since the composition of Example 3 has a tendency for pores to increase, it is judged that it is difficult to expect an effective effect from an increase of MgO of 1.5 wt% or more.

[0128]

[0129] Referring to Figures 5a and 5b, it can be confirmed that the high-temperature volume resistance according to the grain size increases as the grain size decreases. In particular, when MgO is 1 wt%, the grain size is the smallest and the high-temperature volume resistance is also the largest. As the TiO2 content increases, the grain size tends to decrease, but the high-temperature volume resistance decreases. This is thought to be due to the increased TiN production factor rather than the grain size reduction effect due to TiO2.

[0130]

[0131] Although the embodiments have been described above, those skilled in the art will appreciate that various technical modifications and variations can be applied based on the above. For example, appropriate results can still be achieved even if the described techniques are performed in a different order than described, and / or components of the described systems, structures, devices, circuits, etc. are combined or combined in a different manner than described, or are replaced or substituted with other components or equivalents.

[0132] Therefore, other implementations, other embodiments, and equivalents to the claims also fall within the scope of the claims described below.

Claims

1. Containing titanium nitride (TiN), magnesium aluminate (MgAl2O4) and aluminum nitride (AlN). AlN ceramic material for semiconductor heater components.

2. In paragraph 1, The AlN ceramic material for the semiconductor heater component is yttria-free. AlN ceramic material for semiconductor heater components.

3. In paragraph 1, The above semiconductor heater component is a plate of a semiconductor heater, a shaft of a semiconductor heater, or includes both. AlN ceramic material for semiconductor heater components.

4. In paragraph 1, The above magnesium aluminate (MgAl2O4) exists as a secondary phase of the Mg-Al-O series. AlN ceramic material for semiconductor heater components.

5. In paragraph 1, Contains two or more secondary XRD peaks of the Mg-Al-O series, The above XRD peak has a 2θ value of 44° to 46°. AlN ceramic material for semiconductor heater components.

6. In paragraph 5, The above XRD peak is an yttria series XRD peak-free with a 2θ value of 28° to 30° or 33° to 35°. AlN ceramic material for semiconductor heater components.

7. In paragraph 1, The crystal grain size is 1.5 ㎛ to 2.5 ㎛, AlN ceramic material for semiconductor heater components.

8. In paragraph 1, The high temperature resistance value of 500 ℃ or higher is 1.0E+8 Ω·cm to 1.0E+10 Ω·cm, AlN ceramic material for semiconductor heater components.

9. In paragraph 1, The room temperature resistance value is 1.0E+10 Ω·cm to 1.0E+12 Ω·cm, AlN ceramic material for semiconductor heater components.

10. In paragraph 1, The relative density is 99.5% to 100.5%, AlN ceramic material for semiconductor heater components.

11. In paragraph 1, The porosity is 0.02% to 0.2%, AlN ceramic material for semiconductor heater components.

12. In paragraph 1, The thermal conductivity at room temperature is 80 W / mK to 95 W / mK, A thermal conductivity of 40 W / mK to 50 W / mK at a high temperature of 500 ℃ or higher, AlN ceramic material for semiconductor heater components.

13. A step of forming a composite powder by mixing titanium dioxide (TiO2), magnesium oxide (MgO), and aluminum nitride (AlN); and A step of sintering the above composite powder; including; Method for manufacturing AlN ceramic material for semiconductor heater components.

14. In paragraph 13, The above titanium dioxide (TiO2) is 0.2 to 0.5 parts by weight based on 100 parts by weight of the composite powder, The above magnesium oxide (MgO) is 0.2 to 1.5 parts by weight based on 100 parts by weight of the composite powder. Method for manufacturing AlN ceramic material for semiconductor heater components.

15. In paragraph 13, The above sintering step is performed at a temperature of 1500 ℃ to 2000 ℃. Method for manufacturing AlN ceramic material for semiconductor heater components.

16. In paragraph 13, The above sintering step is a pressure sintering step at a pressure of 5 MPa to 25 MPa per unit area. Method for manufacturing AlN ceramic material for semiconductor heater components.

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