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Definitions

• the present invention relates to a ceramic substrate, a method for obtaining the same and its use.
• Ceramic compositions or substrates are widely used as substrates for mounting electronic components via a metal layer.
• a ceramic composition acts as an isolating layer on which a metal layer is disposed.
• An electronic component may then be provided on the metal layer.
• Ceramic compositions or substrates used for mounting electronic components are required to have excellent discharge properties, in particular a high coefficient of thermal conductivity.
• the ceramic substrate shall have a good mechanical strength as a mounting substrate. This is in particular necessary, when reducing the thickness of the ceramic substrate due to the ongoing miniaturization of electronic components. Therefore, a ceramic substrate are required that have both a high coefficient of thermal conductivity and a high mechanical strength.
• a known type of ceramic substrate used in such a set-up is an alumina substrate containing zirconium oxide (zirconia toughened alumina substrate-ZTA substrate).
• Such a ceramic substrate is for example described in EP 2 91 1 994 B1 refers to a metal ceramic substrate comprising AI2O3, ZrO 2 and Y2O3, wherein the average grain size of the used AI2O3 is between 2 and 8 pm.
• AI2O3 grain size refers to the grain size of the starting material or the sintered material. There is also no method for determining the grain size provided.
• EP 3786134A1 describes a substrate comprising 70-95 wt% alumina particles in a size between 1 .2 pm to 1 .9 pm and 5-30 wt% zirconia and hafnia.
• the size of the zirconia particles is between 0.4 pm and 0.7 pm.
• US 2021/0261473A1 also concerns ceramic substrates with different AI2O3 and Zr ⁇ 2 particle sizes.
• the size of AI2O3 particles is between 1 .7 and 1 .9 pm and of ZrO 2 particles is between 0.7 and 0.9 pm.
• ceramic substrate are described that comprise aluminum oxide crystals with an average crystal size between 0.9 and 1.6 pm and zirconium oxide crystals with an average crystal size between 0.28 and 0.6 pm.
• the object of the present invention was to provide a ceramic substrate combining a good thermal conductivity and mechanical strength.
• a ceramic substrate that comprises:
• AI2O3 aluminum oxide with an average grain size between 1 .31 and 1 .55 pm;
• Y2O3 - Yttrium oxide
• SiC>2 silicon oxide
• optionally further compounds such as HfO2.
• the ceramic substrate of the invention is characterized by a good thermal stability and a good mechanical strength as illustrated by the data provided below.
• the good mechanical strength was not expected due to the grain size of ZrC>2 determined in the ceramic substrate.
• a ZrO 2 grain size of more than 0.6 pm did not hamper the mechanical strength, on the contrary it was even possible to increase the mechanical strength to a certain extent.
• the present ceramic substrate has a dense crystal arrangement and consists of two phases of ZrC>2 and AI2O3 grains.
• the Zr ⁇ 2 grains are tetragonal or monocline.
• the present ceramic substrate has the following composition:
• wt% preferably 6-1 1 wt%, more preferably 8-10 wt% (based on the overall weight of the ceramic substrate) of zirconium dioxide (ZrO2) with an average grain size between 0.65 and 0.75 pm (measured by planimetric method as described in the method section), 0.2-0.8 wt%, preferably 0.3-0.7 wt%, more preferably 0.4 - 0.6 wt% (based on the overall weight of the ceramic substrate) of yttrium oxide (Y2O3), and
• Yttrium oxide is contained in commercially available zirconium oxide as stabilizer; i.e commercially available yttria stabilized zirconia is used as starting material in the preparation method as described in more detail below.
• commercially available Zirconium oxide also contains hafnium oxide HfO2.
• HfO2 may be present within a range of not less than 1 part by mass and not greater than 3 part by mass per 100 parts of zirconium oxide.
• Yttrium oxide may be present in zirconium oxide in an amount of up to 6 wt%, preferably about 5-5.5 wt%.
• Zirconium oxide also contains further components such as up to 0.55 wt% aluminum oxide AI2O3.
• the ceramic substrate also contains sintering agents, in particular silicon dioxide (SiO2).
• SiO2 silicon dioxide
• a preferred sintering agent is SiO2.
• SiC>2 may be contained in the ceramic substrate in an amount up to 0.5 wt%, preferably up to 0.35 wt%.
• the present ceramic substrate comprises
• Y2O3 yttrium oxide
• SiO2 silicon oxide
• the present ceramic substrate comprises
• ZrO2 zirconium dioxide
• Y2O3 yttrium oxide
• SiO2 silicon oxide
• the present ceramic substrate comprises
• Y2O3 yttrium oxide
• the ceramic substrate has a bending strength (measured according to ASTM C1499-15) of more than 620 MPa, preferably of more than 650 MPa, more preferably of more than 670 MPa, even more preferably of more than 680 MPa, such as 690 MPa.
• the bending strength may be in a range between 620 - 800 MPa, preferably in a range between 630 -760 MPa, even more preferably in a range between 650 - 730 MPa.
• the ceramic substrate has a thermal conductivity (measured at 20°C according to ISO 18755:2005) of more than 20 W/m*K, preferably of more than 22 W/m*K, even more preferably of more than 24 W/m*K.
• the thermal conductivity may be in a range between 20 - 40 W/m*K, preferably between 22- 35 W/m*K, more preferably between 23- 30 W/m*K, even more preferably between 24 - 27 W/m*K.
• the ceramic substrate has a modulus of elasticity or E-module (Young’s Modulus) as determined in a Grindosonic (method described in the experimental section) of more than 310 GPa, preferably of more than 350 GPa, even more preferably of more than 360 GPa.
• the E-module may be in a range between 310 - 400 GPa, preferably in a range between 330 - 390 GPa, more preferably in a range between 350 - 380 GPa.
• the ceramic substrate has a fracture toughness Ki c Niihara (measured according to the IF-method as described in the experimental section) of 3-5 MPa m 1/2 , preferably of 3.5 - 4.5 MPa m 1/2 , more preferably of 3.8-4.2 MPa m 1/2 .
• the Vickers Hardness of the ceramic substrate is between 1500 - 2000 HV, preferably between 1600 - 1900 HV, more preferably between 1700 - 1850 HV, even more preferably between 1750 - 1830 HV.
• the ceramic substrate has a surface roughness Ra (measured according to DIN EN ISO 4288) of less than 0.5 pm, preferably of less than 0.4 pm, more preferably of less than 0.2 pm, such as 0.19 pm.
• the bulk density (measured according to DIN 993-1 / ISO 18754) of the ceramic substrate is more than 3.5 g/cm 3 , preferably of more than 3.95 g/cm3, even more preferably of more than 4 g/cm 3 , such as 4.0-4.1 g/cm 3 .
• the ceramic substrate has an electric breakdown strength (measured at 20°C following DIN EN 60243 ff) of more than 20 kV/mm, preferably of more than 25 kV/mm. more preferably of more than 30 kV/mm.
• the electric breakdown strength may be in a range between 20 - 40 kV/mm, preferably in a range between 25 - 35 kV/mm, more preferably between 28 - 33 kV/mm.
• Specific heat capacity (measured using DSC device as described in the experimental section) of the ceramic substrate is of more than 620 J/gK, preferably of more than 650 J/gK, more preferably more than 670 J/gK.
• the specific heat capacity may be in a range between 620- 750 J/gK, preferably in a range between 650 - 720 J/gK, more preferably between 670-710 J/gK.
• Coefficient of thermal expansion CTE (determined using a dilatometer as described in the experimental section) of the ceramic substrate is at 20-300°C of more than 7 10 -6 /K, at 300- 600°C of more than 810 -6 /K, at 600-900°C of more than 8.6 10 6 /K.
• the present ceramic may have the following properties:
• thermal conductivity may be in a range 22- 35 W/m*K
• E-module may be in a range between 330 - 390 GPa
• electric breakdown strength may be in a range between 25 - 35 kV/mm
• - specific heat capacity may be in a range between 650 - 720 J/gK.
• the present ceramic may have the following properties:
• thermal conductivity may be in a range between 23- 30 W/m*K
• E-module may be in a range between 350 - 380 GPa; electric breakdown strength may be in a range between 28 - 33 kV/mm;
• - specific heat capacity may be in a range between 670-710 J/gK.
• the ceramic substrate may be obtained in a method comprising the following steps:
• a binder such as polyvinylalcohol (PVA) or polyvinylbutyral (PVB)
• PVA polyvinylalcohol
• PVB polyvinylbutyral
• the first grade of AI2O3 may have a particle size d50 of 0.3-0.6 pm and d90 of less than 3.0, preferably less than 2.0 pm and the second grade of AI2O3 may have a particle size d50 of 1 .0-1 .5 pm and d90 of less than 4.0, preferably less than 3.6 pm.
• the first grade of ZrC>2 may have a particle size d50 of 0.25-0.35 pm and d98 less than 2.0 pm and the second grade of ZrO 2 may have a particle size d50 of 0.9-1 .25 pm, and d80 1 .5-2.2 pm.
• the following first mixture is provided as aluminum oxide starting material, said first mixture comprising
• the two types of aluminum oxides having preferably different particle sizes and used as starting material are provided in a weight ratio of about 1 : 1 , i.e. about 50 wt% of each type.
• the following second mixture is provided as zirconium oxide starting material, said second mixture comprising
• the at least one second type of zirconium oxide having a particle size (d50) between 0.8-1 .4 pm, preferably d50 0.9-1 .25 pm.
• At least one first type of zirconium oxide having a particle size between d50 0.2-0.5 pm preferably d50 0.25-0.35 pm and about 30 wt% at least one second type of zirconium oxide having a particle size between d50 0.8-1 .4 pm, preferably d50 0.9-1 .25 pm are used as starting material.
• sintering aids such as SiC>2 and organic compounds such as binder (for example PVA or PVB) are added to the AI2O3 / ZrO 2 mixture.
• the powdery mixture of AI2O3 / ZrO 2 (containing Y2O3) / sintering aids is subsequently added into a mill together with a solvent such as water or organic solvents, preferably containing a dispersing agent to obtain a dispersion.
• a green sheet or film is obtained by a doctor blade method using this slurry.
• a green sheet is obtained by a powder press molding method or a roller compaction method.
• a compact may be obtained by performing profile shape machining with a metal mold or a laser.
• the green sheet may be used directly as a compact and subjected to profile shape machining with a laser after being subject to firing.
• a multipiece compact is preferably used.
• the sintering step is carried out in a furnace.
• the sintering temperature is preferably 1400- 1700°C.
• the ceramic substrate of the invention may be used in an electronic device.
• Such an electronic device may include the ceramic substrate as a support with a metal layer located on one or both surfaces of the ceramic substrate.
• An electronic component may be provided on the metal layer.
• the electronic component provided on the metal layer of the ceramic substrate may be used, for example, in a semiconductor element such as an insulated gate bipolar transistor (IGBT) element, an intelligent power module (IPM) element, a metal oxide semiconductor field effect transistor (MOSFET) element, an LED element, a freewheeling diode (FWD) element, a giant transistor (GTR) element, or a Schottky barrier diode (SBD).
• the electronic component may be used in a heat-generating element for a sublimation type thermal printer head or a thermal inkjet printer head. Further, the electronic component may be used in a Peltier element.
• the starting materials ZrO2, AI2O3 and SiO2 are subjected to an incoming raw material inspection. Two different grades are used for both the AI2O3 and the ZrO 2 to achieve the grain size distributions shown in the final product.
• the mass preparation takes place in a mill.
• the mass preparation contains mixing of the raw materials, meaning the ceramic starting material and the organic compounds.
• the slurry is cast to form a ceramic green film.
• the green film is cut to specified dimensions.
• the ceramic films are sintered at 1400 bis 1700°C.
• Grain size planimetric method applied to the sintered ceramic substrate
• the planimetric method applied for determining the average crystal grain size of alumina and zirconia is now described.
• the surface of the ceramic substrate 1 is subjected to mirror finishing and is heat-treated in a temperature range from 50 to 100°C lower than the firing temperature.
• the heat-treated surface is then used as a measurement surface and is photographed at a multiplication factor of 5000 times using an SEM.
• the photographed image data is analyzed using image analysis software (for example, Win ROOF available from the Mitani Corporation). As a result, the data for the respective crystal grain sizes of alumina and zirconia present in the image data can be obtained.
• the ceramic substrate may contain crystals with a crystal grain size of less than 0.05 mm, only crystals with a crystal grain size of at least 0.05 mm are targeted in the analysis by the image analysis software.
• image analysis software such as that described above is used, separate measurements are possible because there is a difference in color tone between alumina crystal grains and zirconia crystal grains.
• the average value of an equivalent circle diameter of each crystal grain calculated from the area of each crystal grain of alumina is the average crystal grain size of alumina
• the average value of an equivalent circle diameter of each crystal grain calculated from the area of each crystal grain of zirconia is the average crystal grain size of zirconia
• the standard deviation of the crystal grain size of alumina can be determined by the same method as that used to determine the average crystal grain size described above from the data of the crystal grain size of alumina obtained using image analysis software.
• the Klc value was determined using the IF method as described in A. G. Evans, E. A. Charles, J. Am. Ceram. Soc. 1976, 56, 371 -372. Lind G. R. Anstis, P. Chantikul, et al., J. Am. Ceram. Soc. 1981 , 64, 533-538.
• substrates were supplied. A sample was broken out of each substrate, embedded in Clarocit and ground and polished.
• Ki c value was done according to the formula of Niihara as well as Anstis:
• the hardness and Kic values of the measured samples are shown in table 1 below.
• the mean value with standard deviation is given in each case.
• the mean values were formed from at least 5 measured hardness impressions per material.
• the specific heat capacity or heat capacity is a measurable physical quantity that corresponds to the ratio of the heat supplied to an object to the resulting temperature change.
• the specific heat is the amount of heat needed to raise the temperature of one gram of the material by 1 degree Celsius.
• DSC measurements are done according to DIN 51007 and ISO 1 1357-1.
• a DSC measuring cell consists of a furnace and an integrated sensor with corresponding footprints for sample and reference crucibles.
• the sensor surfaces are connected to thermocouples or are even part of the thermocouples themselves. This makes it possible to record both the temperature difference between the sample and reference sides (DSC signal) and the absolute temperature of the sample or reference side.
• DSC signal temperature difference between the sample and reference sides
• the reference side usually heats up faster than the sample side when heating up a DSC measuring cell, i.e. the reference temperature (TR) rises somewhat faster than the sample temperature (TP). Both curves behave parallel to each other during heating with a constant heating speed - until a sample reaction occurs.
• the sample begins to melt at t1.
• the temperature in the sample does not change; however, the temperature of the reference side remains unaffected and continues to rise linearly. After the melting is finished, the sample temperature also increases again and shows a linear slope again from time t2 onwards.
• the difference signal (AT) of the two temperature curves is used.
• a peak is formed by the difference formation, which represents the endothermic melting process.
• the resulting peak points upwards or downwards in the graph.
• the area of the peak is related to the heat content of the conversion (enthalpy in J/g).
• the measurement setup consists of the Grindosonic with connected microphone or piezo sensor, a suitable clapper and a special specimen holder with supports matched to the respective specimen geometry.
• the device is also connected to the PC for recording the measured values.
• Elasticity of a material means that a material deforms under external load, but returns to its original state as soon as the load disappears. This strain is linearly proportional to the applied load (Hooke's Law). The quotient of strain and load results in a propornality factor known as the Young's modulus of the material.
• a measuring device from company Netzsch is used to measure the linear thermal expansion of a sample as a function of temperature. Thermal expansion is a measure of the change in volume of a body in response to changes in temperature. Measuring according to manufacturer's specification DIL 402 Expedis Select & Supreme - NETZSCH Analyzing & T esting (netzsch-thermal-analysis.com)
• the first grade of AI2O3 has a particle size d50 of 0.5 pm and d90 of 2.0 pm and the second grade of AI2O3 has a particle size d50 of 1 .3 pm and d90 of 3.2 pm.
• the first grade of ZrC>2 has a particle size d50 of 0.3-0.32 pm and d90 of 0.60 pm and the second grade of ZrC>2 has a particle size d50 of 1 .17 pm and d80 of 2.06 pm.
• the ceramic substrate obtained contains AI2O3, ZrO2, Y2O3 and SiC>2. Further components in the ceramic substrates can be: Na2O, MgO, K 2 O, CaO, TiO2, Cr 2 O3, Fe20s ,SrO, CeO.
• Table 4 summarizes the mechanical, thermal and electrical properties of the inventive examples of Table 3.

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