WO2021012448A1 - 一种氧化锆复合氧化铝陶瓷烧结体、其制备方法及应用 - Google Patents

一种氧化锆复合氧化铝陶瓷烧结体、其制备方法及应用 Download PDF

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WO2021012448A1
WO2021012448A1 PCT/CN2019/115243 CN2019115243W WO2021012448A1 WO 2021012448 A1 WO2021012448 A1 WO 2021012448A1 CN 2019115243 W CN2019115243 W CN 2019115243W WO 2021012448 A1 WO2021012448 A1 WO 2021012448A1
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alumina
content
zirconia
calculated
sintered body
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PCT/CN2019/115243
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English (en)
French (fr)
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黄雪云
江楠
童文欣
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南充三环电子有限公司
潮州三环（集团）股份有限公司
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Priority to JP2021537059A priority Critical patent/JP7199543B2/ja
Priority to EP19938792.9A priority patent/EP3845507B1/en
Publication of WO2021012448A1 publication Critical patent/WO2021012448A1/zh

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Definitions

  • the invention relates to an alumina ceramic sintered body, in particular to a zirconia composite alumina ceramic sintered body, its preparation method and application.
  • the invention relates to a high-temperature ceramic sintered body and a substrate using the ceramic sintered body.
  • the ceramic sintered body can be applied to substrates for power device packaging, such as high-reflectivity LED ceramic substrates and power module substrates; and can also be applied to the use of DCB and AMB Process metal-ceramic bonding metalized substrate belongs to the technical field of alumina composite ceramic performance improvement.
  • Patent Document 1 with application number CN201080015347.3 discloses that the upper limit of the weight of zirconia powder contained in the sintered body is 30wt%, and the proportion of zirconia in the tetragonal phase is more than 80%, and the content of magnesium oxide is 0.05-0.5wt According to this, compared with the previous ceramic substrates containing only alumina, the mechanical strength of the substrate and the heat dissipation effect can be significantly improved; Patent Document 2 with the application number CN201380056024.2, by adding 2- 15wt% zirconia and 0.01-1wt% yttrium oxide, and the alumina particle size is controlled to 2-8um to achieve the purpose of improving the mechanical strength of the ceramic, thereby reducing the thickness of the metal layer and the ceramic body layer and further improving the metal-ceramic-substrate
  • Patent Document 3 discloses that by adding 2-9wt% zirconia and 0.04-1wt% yttrium oxide and 0.04
  • Patent Documents 1 and 3 add SiO 2 and MgO as flux phases to promote the densification of ceramic sintered bodies.
  • the flux phase especially SiO 2
  • the grain boundary phases of alumina and zirconia are between the grain boundary phases of alumina and zirconia. Enrichment reduces the strength between the grain boundaries, resulting in the mechanical strength of the sintered body not reaching the optimal value.
  • the heterogeneity between the crystal grains of the ceramic sintered body is further increased, and the decline of the phonon transfer rate eventually leads to a decline in the thermal conductivity.
  • the particle size of alumina is controlled at 2-8um. Under this crystal size, the particle size of zirconia is distributed between 0.7-2.5um.
  • the larger alumina grain size results in a decrease in the number of grain boundaries and bulk pores. As the size of defects increases, the strength of the ceramic matrix will eventually be low. At the same time, due to the large alumina grain size, the large grain size of zirconia between grain boundaries or the serious degree of grain agglomeration, the stability of tetragonal zirconia is insufficient. Eventually, the toughening effect of the zirconia phase transformation during the fracture of the ceramic matrix decreases, and the mechanical strength of the matrix cannot reach the optimal value.
  • the purpose of the present invention is to overcome the shortcomings of the prior art and provide a sintered body of zirconia composite alumina ceramics.
  • the sintered body has higher mechanical strength and thermal conductivity performance.
  • a zirconia composite alumina ceramic sintered body which contains the following components by mass percentage: a zirconium-containing compound (calculated in the form of zirconia) 0.01-20%, Yttrium-containing compounds (content calculated in the form of yttrium oxide) 0-1.75%, silicon-containing compounds (content calculated in the form of silicon oxide) 0.01-0.8%, calcium-containing compounds (content calculated in the form of calcium oxide) 0-0.035%, magnesium The compound (content calculated in the form of magnesium oxide) is 0-0.05%, and the balance is alumina.
  • tetragonal zirconia exists in the alumina crystal grains. During the fracture of the sintered body, the crack extends to the zirconia grain boundary and the zirconia undergoes a phase change (the tetragonal phase is transformed into a monoclinic phase), which changes the potential energy of the crack Absorption prevents crack propagation.
  • the degree of phase change prevents crack propagation increases, resulting in a further increase in mechanical strength; in the solution of the present invention, under the same zirconia content, by reducing SiO 2 , MgO, CaO With the addition of zirconia, the concentration of flux at the grain boundary decreases, thereby further enhancing the strength of the grain boundary, resulting in the same zirconia addition, the mechanical strength of the ceramic sintered body is further improved.
  • thermal conductivity of the composite ceramic sintered body shows a downward trend.
  • the reason is that the thermal conductivity of non-metallic materials is conducted by phonons (ie lattice resonance), and the lattice spacing is consistent. The better the performance, the higher the phonon transfer rate. Due to the inconsistent lattice spacing between zirconia and alumina, the addition of zirconia leads to a decrease in the phonon transfer rate, which leads to a decrease in thermal conductivity. Under the same amount of zirconia, with the addition of MgO and CaO , The amount of SiO 2 added decreases, and the thermal conductivity of the composite ceramic sintered body shows an upward trend.
  • the flux in the sintered body is almost all enriched between the alumina or zirconia grain boundaries, and the lattice spacing of the enriched phase
  • the difference from the main crystalline phase is obvious, which causes the phonon transfer rate to decrease. Therefore, the thermal conductivity of the sintered body is improved by reducing the content of the enriched phase.
  • the bonding mechanism of the copper clad laminate is mainly that the metal copper reacts with the Al-OH bond on the surface of the substrate at a temperature near the melting point to form an Al-O-Cu bond to achieve the bonding effect.
  • the Zr-OH bond can also interact with the metal Copper bonding, a small amount of Zr-O-Cu bonds play a complementary role in bonding strength, but as the content of ZrO 2 further increases, the bonding strength of Al-O-Cu and Zr-O-Cu is different, resulting in bonding The intensity shows a downward trend.
  • the definition of dielectric strength is the threshold voltage for breakdown (conduction) on both sides of the substrate divided by the thickness of the substrate; for metals, there are free moving electrons in the bulk phase to form currents.
  • dielectric strength For alumina crystals, there is no internal Freely moving electrons can only migrate by cations as carriers, and the smaller the cation radius, the faster the migration speed (for example, the presence of Na particles in the sample will cause the insulation strength to decrease).
  • the oxygen vacancies between the crystals are mainly used as carriers to move (Al 3+ migration) to form a current.
  • the factor that determines the speed of the oxygen vacancies is mainly the grain size (the number of grain boundaries, Al 3+ is in It is more difficult to migrate between grain boundaries), the content of flux impurities (if the magnesium and calcium atom radius is small, the migration speed is faster, and the silica-lime glass phase has no grain boundaries to limit the migration speed) and the content of zirconia (the zirconium atom radius is larger) (Move slower than Al 3+ ) will affect the dielectric strength.
  • the zirconia composite alumina ceramic sintered body contains the following components by mass percentage: zirconium-containing compound (content is calculated as zirconia) 5-15%, yttrium-containing compound (content is calculated as yttrium oxide) ) 0.3-1%, silicon-containing compounds (content calculated in the form of silicon oxide) 0.04-0.8%, calcium-containing compounds (content calculated in the form of calcium oxide) 0.01-0.03%, magnesium-containing compounds (content calculated in the form of magnesium oxide) 0 -0.03%, the balance is alumina.
  • the zirconia composite alumina ceramic sintered body contains the following components by mass percentage: zirconium-containing compound (content is calculated as zirconia) 5-10%, yttrium-containing compound (content is in yttrium oxide form) Calculated) 0.3-0.8%, silicon-containing compounds (content calculated in the form of silicon oxide) 0.4-0.6%, calcium-containing compounds (content calculated in the form of calcium oxide) 0.01-0.03%, magnesium-containing compounds (content calculated in the form of magnesium oxide) 0-0.03%, the balance is alumina.
  • the present invention can better improve the consistency of Al 2 O 3 grain boundaries, and improve the strength and thermal conductivity of alumina grain boundaries.
  • the grain boundaries of alumina and zirconia are staggeredly distributed, achieving a good effect of mutually restricting the grain size.
  • the magnesium-containing compound is magnesium aluminum spinel.
  • the average particle size D50 of the zirconium-containing compound is (0.1-1.5) times the average particle size D50 of alumina.
  • the difference between the average particle size of zirconia and alumina is too large, which will cause large gaps in the crystal phases of different substances in the sintered body and reduce the mechanical strength of the product.
  • the average particle size D50 of the alumina is 0.8-3um, and the maximum particle size range is 4-10um.
  • the average particle size D50 of the alumina is 1.3-2.5um, and the maximum particle size range is 4-7um.
  • the average particle size D50 of the zirconia is 0.2-1.5um, and the maximum particle size range is 1.0-2.5um.
  • the average particle size D50 of the zirconia is 0.4-0.8um, and the maximum particle size range is 1.2-1.8um.
  • Sintered body of the present invention by controlling the primary particle size of ZrO 2 and ZrO 2 to achieve uniform dispersion of the flux Al 2 O 3 matrix densified-situ fluxing effect, the technique may further enhance the mechanical strength of the alumina ceramic substrate and Thermal conductivity: By reducing the average particle size and maximum particle size of Al 2 O 3 in the sintered body, increasing the number of Al 2 O 3 grain boundaries in the matrix, reducing the pore size, and further improving the degree of dispersion of ZrO 2 in the matrix, Improve the phase change toughening effect of ZrO 2 in the matrix, and further improve the mechanical strength of the ceramic matrix.
  • the present invention also provides an alumina substrate containing the zirconia composite alumina ceramic sintered body.
  • the present invention provides a ceramic substrate for a copper clad laminate.
  • the present invention provides an alumina substrate used for DBC copper clad.
  • the present invention also provides a method for preparing the alumina substrate, including the following steps:
  • step (1) After the pre-dispersed powder in step (1) is calcined at low temperature, it is crushed, and then the remaining part of the alumina powder is added for further mixing and dispersion to complete the dispersion and mixing of the raw material powder;
  • step (3) Mixing the raw material powder after dispersion and mixing in step (2) with the organic binder and dispersant;
  • a two-step method is used to disperse the raw material powder in the zirconia composite alumina ceramic substrate, that is, the zirconia powder and a part of the alumina
  • the powder is dispersed and calcined at low temperature.
  • a certain bonding force is formed between the ZrO 2 and Al 2 O 3 powders in the ZTA pre-sintered body; then the ZTA pre-sintered body is dispersed into the alumina powder again.
  • This method can It can improve the dispersion effect of ZrO 2 in ZTA, so as to better realize the fluxing effect of ZrO 2 and reduce the addition of SiO 2 , MgO and CaO.
  • the parameters of pre-dispersion and mixing dispersion are: dispersion time: 30-45h, powder particle size control range: D50 ⁇ 0.8um.
  • the parameters for low-temperature calcination are: sintering temperature>1300°C, holding time of 1-3h; parameters for crushing: ball milling time 20-40h, particle size control range: D50 ⁇ 0.6um.
  • the mixing parameters of the raw material powder and the dispersant are: dispersion time: 30-45h, particle size control range: D50 ⁇ 0.6um; the mixing parameters of the raw material powder and the organic binder are : Dispersion time: 5-15h, milling viscosity ⁇ 1000CPs.
  • the process parameters of the slurry defoaming and aging process are as follows: (1) Slurry defoaming: defoaming pressure: -0.05 ⁇ -0.1MPa, stirring speed: 10-30Hz, slurry temperature: 15-35 °C, slurry viscosity: 1000-7000Cps; (2) ZTA powder and binder blending: aging time: 5-24h, stirring speed: 0-3Hz, slurry temperature control 25-30°C, slurry viscosity control: 1000-7000Cps.
  • the casting process parameters are: casting speed: 0.7-3m/s, zone one temperature: 15-50°C, zone two temperature: 40-70°C, zone three temperature: 65-110°C, Zone wind speed: 0.2-1.5m/s, zone two wind speed: 0.8-5m/s, zone three wind speed: 0.5-5m/s.
  • the sintering process parameters are: test piece temperature: 1400-1570°C, holding time: 0.5-4h.
  • the present invention also discloses a copper-clad process of the alumina substrate, which includes the following steps:
  • the copper sheet is placed on the surface of the substrate and passed through a reducing atmosphere furnace (the furnace temperature is controlled near the critical melting point of copper) to bond the metal copper to the surface of the base layer;
  • Copper coating on the second side Place the processed copper foil on the other side of the substrate, and bond the metal copper to the second side of the base layer through a reducing atmosphere furnace (furnace temperature is slightly lower than the first copper coating temperature) .
  • Alumina zirconia composite ceramic sintered body of the present invention the flux by reducing the content of (MgO ⁇ 500ppm, CaO ⁇ 350ppm, SiO 2 ⁇ 8000ppm), to reduce the influence of the grain boundary strength and flux phonon transfer rate, while the control ZrO 2 and the primary particle size to achieve uniform dispersion of the flux ZrO 2 Al 2 O 3 matrix densification, the fluxing action-situ, to further enhance the mechanical strength and thermal conductivity of an alumina ceramic matrix.
  • Figure 1 is an SEM image of the ZTA pre-sintered body of the present invention
  • Fig. 2 is an SEM image of the ZTA sintered body of Example 22 of the present invention.
  • the present invention sets Examples 1-15.
  • the components and contents of the sintered bodies described in Examples 1-15 and Comparative Example 1 (content unit is WT%) are set as shown in Table 1:
  • the specific preparation method includes the following steps:
  • step (1) After the pre-dispersed powder in step (1) is calcined at low temperature, as shown in Figure 2, it is broken again, and then the remaining part of the alumina powder is added for further mixing and dispersion to complete the dispersion and mixing of the raw material powder ;
  • Pre-dispersion and mixing and dispersion parameters dispersion time: 30-45h, powder particle size control range: D50 ⁇ 0.8um; low-temperature calcination parameters: sintering temperature range: 1300°C-1400°C, holding time 1-3h ;
  • the crushing parameters are: ball milling time 20-40h, particle size control range: D50 ⁇ 0.6um;
  • step (3) Mix the raw material powder after dispersing and mixing in step (2) with the organic binder and dispersant; the parameters for mixing the raw material powder and dispersant are: dispersion time: 30-45h, particle size control range: D50 ⁇ 0.6um; the mixing parameters of the raw material powder and the organic binder are: dispersion time: 5-15h, grinding viscosity ⁇ 1000CPs;
  • slurry defoaming defoaming pressure: -0.05 ⁇ -0.1MPa, stirring speed: 10-30Hz, slurry temperature: 15-35°C, slurry viscosity: 1000-7000Cps ;
  • ZTA powder and adhesive blending aging time: 5-24h, stirring speed: 0-3Hz, slurry temperature control 25-30°C, slurry viscosity control: 1000-7000Cps;
  • the test method of insulation strength can be in accordance with the test method in the national standard GB/T18791-2002. Put the test sample in the transformer oil, apply DC or AC voltage to it, and gradually increase the test voltage until the test sample is Breakdown loses insulation properties, and the dielectric strength of the sample is obtained.
  • the scribing depth is controlled between 35-50% of the thickness of the sample.
  • the zirconia and alumina in the ZTA pre-sintered body are uniformly dispersed, and the average particle size D50 of the two is reasonably controlled.
  • the two alumina particle sizes marked in the figure are 588nm and 784nm, respectively.
  • the two zirconia particle sizes are 417nm and 708nm.
  • Figure 2 is the SEM image of the alumina sintered body of Example 22. It can be seen from Figure 2 that the zirconia and alumina are evenly dispersed.
  • the specific particle size please refer to the identification of the two alumina particle sizes in the figure, which are 1.35 um and 888nm.
  • the above alumina substrate is coated with copper, the specific method is:
  • the copper sheet is placed on the surface of the substrate and passed through a reducing atmosphere furnace (the furnace temperature is controlled near the critical melting point of copper) to bond the metal copper to the surface of the base layer;
  • Copper coating on the second side Place the processed copper foil on the other side of the substrate, and bond the metal copper to the second side of the base layer through a reducing atmosphere furnace (furnace temperature is slightly lower than the first copper coating temperature) .
  • the bonding strength and temperature reliability of the copper-clad substrate were tested.
  • the test results are shown in Table 3.
  • the specific test methods are as follows:
  • the adhesion between the copper plate and the alumina substrate was evaluated by the peel strength measurement.
  • the measurement method is as follows. Use pliers to peel off the end of a pattern with a width of 5 mm, which is a part of the copper circuit pattern bonded to the alumina substrate, and fix the bonded substrate on the workbench of the tensile tester, and mount the end of the pattern on the peeling The chuck of the testing machine. At this time, it is installed so that the angle between the surface of the alumina substrate and the peeled copper circuit pattern becomes 90° (vertical direction). After that, the tensile tester was operated, and the peeled pattern was stretched and moved upward via a chuck, and the maximum peeling load at this time was measured. The maximum peeling load is divided by the width (0.5 cm) to calculate the bonding strength.
  • Zero-containing compound content is calculated in the form of zirconia 5-10%
  • yttrium-containing compound content is calculated in the form of yttria 0.3-0.8%
  • silicon-containing compound content is in the form of silicon oxide Calculated) 0.4-0.6%
  • calcium-containing compounds calculated in the form of calcium oxide
  • magnesium-containing compounds calculated in the form of magnesium oxide

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Abstract

一种氧化锆复合氧化铝陶瓷烧结体以及包含该烧结体的氧化铝基板及其制备方法。该烧结体包含以下质量百分含量的成分：含锆化合物(含量以氧化锆形式计算)0.01-20％、含钇化合物(含量以氧化钇形式计算)0-1.75％、含硅化合物(含量以氧化硅形式计算)0.01-0.8％、含钙化合物(含量以氧化钙形式计算)0-0.035％、含镁化合物(含量以氧化镁形式计算)0-0.05％，余量为氧化铝。通过降低助熔剂含量，降低助熔剂对晶界强度及声子传递速率的影响，通过控制ZrO2初始粒径及分散均匀性实现ZrO2助熔Al2O3基体致密化，提升氧化铝陶瓷基体的机械强度及热导率。

Description

一种氧化锆复合氧化铝陶瓷烧结体、其制备方法及应用 技术领域
本发明涉及一种氧化铝陶瓷烧结体，尤其是一种氧化锆复合氧化铝陶瓷烧结体、其制备方法及应用。
背景技术
本发明涉及高温陶瓷烧结体以及采用该陶瓷烧结体的基板，该陶瓷烧结体可应用于功率器件封装用基板，比如高反光率LED陶瓷基板，功率模组基板；也可应用于采用DCB、AMB工艺金属-陶瓷键合的金属化基板，属于氧化铝复合陶瓷性能提升技术领域。
申请号为CN201080015347.3的发明专利文献1，公开了烧结体中含有氧化锆粉体重量的上限是30wt％，且四方晶相的氧化锆比例在80％以上，氧化镁含量在0.05-0.5wt％之间，据此与以往单含氧化铝的陶瓷基板相比能够明显提高基板的机械强度并改善散热效果；申请号为CN201380056024.2的专利文献2，通过在氧化铝陶瓷基体中增加2-15wt％氧化锆及0.01-1wt％氧化钇，且控制氧化铝粒径为2-8um，实现提高陶瓷机械强度的目的，从而可以降低金属层与瓷体层的厚度进一步提升金属-陶瓷-基材的导热效率；申请号为DE102004012231专利文献3，公开了通过在氧化铝陶瓷基体中增加2-9wt％氧化锆及0.04-1wt％氧化钇和0.04-1wt％氧化钙或实现提高陶瓷机械强度的目的，从而可以降低金属层与瓷体层的厚度进一步提升金属-陶瓷-基材的导热效率。
专利文献1、3中加入SiO 2、MgO作为助熔剂相促进陶瓷烧结体的致密化程度，但烧结体致密化后，该助熔剂相(尤其是SiO 2)在氧化铝及氧化锆晶界相间富集从而降低晶界间的强度从而导致烧结体的机械强度未能达到最佳值。此外，由于助熔剂的加入导致陶瓷烧结体晶粒间的非均质性进一步增加，声子传递速率下降最终导致热导率反而存在下降趋势。专利文献2中氧化铝粒径控制在2-8um，在该晶粒尺寸下氧化锆粒径分布在0.7-2.5um之间，氧化铝晶粒尺寸较大造成晶界数量下降，同时体相气孔等缺陷尺寸增大，最终导致陶瓷基体强 度偏低，同时因氧化铝晶粒尺寸较大，晶界间氧化锆晶粒尺寸较大或者晶粒团聚程度较严重造成四方相氧化锆稳定性不足，最终导致陶瓷基体断裂过程中氧化锆相变增韧效果下降，基体的机械强度无法达到最佳值。
发明内容
基于此，本发明的目的在于克服上述现有技术的不足之处而提供一种氧化锆复合氧化铝陶瓷烧结体。所述烧结体具有较高的机械强度及热导率性能。
为实现上述目的，本发明所采取的技术方案为：一种氧化锆复合氧化铝陶瓷烧结体，包含以下质量百分含量的成分：含锆化合物(含量以氧化锆形式计算)0.01-20％、含钇化合物(含量以氧化钇形式计算)0-1.75％、含硅化合物(含量以氧化硅形式计算)0.01-0.8％、含钙化合物(含量以氧化钙形式计算)0-0.035％、含镁化合物(含量以氧化镁形式计算)0-0.05％，余量为氧化铝。
关于机械强度：四方相氧化锆存在于氧化铝晶粒中，在烧结体断裂过程中裂纹延伸至氧化锆晶界处氧化锆发生相变(四方相转变为单斜相)，将裂纹处的势能吸收从而阻止裂纹扩散，随着氧化锆加入量的增加，相变阻止裂纹扩散程度增加，导致机械强度进一步上升；在本发明的方案中，相同氧化锆含量下，通过降低SiO 2、MgO、CaO的加入量，晶界处的助熔剂浓度下降，从而进一步提升晶界强度，导致相同氧化锆添加量下，陶瓷烧结体的机械强度得到进一步提升。
关于热导率：随着氧化锆的加入，复合陶瓷烧结体的热导率呈下降趋势，原因为非金属材质的热导率是靠声子(即晶格谐振)传导的，晶格间距一致性越好声子传递速率越高，由于氧化锆与氧化铝晶格间距不一致，氧化锆的加入导致声子传递速率下降从而导致热导率下降；相同氧化锆加入量下，随着MgO、CaO、SiO 2的加入量降低，复合陶瓷烧结体热导率呈上升趋势，原因为烧结体中的助熔剂几乎全部富集在氧化铝或氧化锆晶界之间，该富集相的晶格间距与主晶相差异明显，造成声子传递速率下降，故通过降低富集相含量达到了提升烧结体热导率的效果。
关于键合强度：覆铜板键合机理主要为金属铜在近熔点温度下与基体表面Al-OH键发生反应，形成Al-O-Cu键从而实现键合效果，Zr-OH键同样能够与 金属铜键合，少量的Zr-O-Cu键对键合强度起到互补作用，但随着ZrO 2含量进一步增加，Al-O-Cu与Zr-O-Cu键合强度存在差异，导致键合强度呈现下降趋势。
关于绝缘强度：绝缘强度定义即基板两侧击穿(导通)的临界电压除以基体的厚度；对于金属来说体相内存在自由移动的电子形成电流，对于氧化铝晶体来说，内部无自由移动的电子，只能靠阳离子作为载流子迁移，且阳离子半径越小则迁移速度越快(例如样品中存在Na粒子则会导致绝缘强度下降)。对于氧化铝基体来说，主要依靠晶体间的氧空位作为载流子移动(Al 3+迁移)形成电流，因此决定氧空位移动速度的因素主要为晶粒尺寸(晶界数量，Al 3+在晶界间迁移难度较大)、助熔剂杂质的含量(如果镁、钙原子半径小迁移速度较快，硅钙玻璃相无晶界限制迁移速度增加)及氧化锆含量(锆原子半径更大故较Al 3+移动速度更慢)均会影响绝缘强度。
优选地，所述的氧化锆复合氧化铝陶瓷烧结体，包含以下质量百分含量的成分：含锆化合物(含量以氧化锆形式计算)5-15％、含钇化合物(含量以氧化钇形式计算)0.3-1％、含硅化合物(含量以氧化硅形式计算)0.04-0.8％、含钙化合物(含量以氧化钙形式计算)0.01-0.03％、含镁化合物(含量以氧化镁形式计算)0-0.03％，余量为氧化铝。
更优选地，所述的氧化锆复合氧化铝陶瓷烧结体，包含以下质量百分含量的成分：含锆化合物(含量以氧化锆形式计算)5-10％、含钇化合物(含量以氧化钇形式计算)0.3-0.8％、含硅化合物(含量以氧化硅形式计算)0.4-0.6％、含钙化合物(含量以氧化钙形式计算)0.01-0.03％、含镁化合物(含量以氧化镁形式计算)0-0.03％，余量为氧化铝。
本发明通过降低SiO 2、MgO、CaO的加入量，可以更好的提升Al 2O 3晶界一致性，提升氧化铝晶界强度以及热导率。采用本发明配方得到的ZTA陶瓷烧结体，氧化铝及氧化锆晶界交错分布，达到很好的相互限制晶粒尺寸效果。
优选地，所述含镁化合物为镁铝尖晶石。
优选地，所述含锆化合物的平均粒径D50为氧化铝的平均粒径D50的(0.1-1.5)倍。氧化锆与氧化铝的平均粒径相差过大，将导致烧结体中不同物质 晶相出现较大间隙，降低其产品的机械强度。
优选地，所述氧化铝的平均粒径D50为0.8-3um，最大粒径范围为4-10um。
更优选地，所述氧化铝的平均粒径D50为1.3-2.5um，最大粒径范围为4-7um。
优选地，所述氧化锆的平均粒径D50为0.2-1.5um，最大粒径范围为1.0-2.5um。
更优选地，所述氧化锆的平均粒径D50为0.4-0.8um，最大粒径范围为1.2-1.8um。
本发明烧结体中，通过控制ZrO 2初始粒径及分散均匀性实现ZrO 2助熔Al 2O 3基体致密化，实现原位助熔效果，该技术可进一步提升氧化铝陶瓷基体的机械强度及热导率；通过降低烧结体中Al 2O 3的平均粒径及最大粒径，增加基体中Al 2O 3晶界数量，减小气孔尺寸，同时进一步提升ZrO 2在基体中的分散程度，提升ZrO 2在基体中的相变增韧效果，进一步提升陶瓷基体的机械强度。
同时，本发明还提供一种包含所述氧化锆复合氧化铝陶瓷烧结体的氧化铝基板。
优选地，本发明提供一种用于覆铜板的陶瓷基板。
更优选地，本发明提供一种用于DBC覆铜的氧化铝基板。
此外，本发明还提供一种所述氧化铝基板的制备方法，包括如下步骤：
(1)将原料粉体粉碎，将原料粉体中除氧化铝外的粉体先与一部分氧化铝进行预分散；
(2)将步骤(1)预分散后的粉体低温煅烧后，再破碎，然后加入剩余部分的氧化铝粉体，进行进一步混合分散，完成原料粉体的分散混合；
(3)将步骤(2)分散混合后的原料粉体与有机粘合剂、分散剂进行混合；
(4)浆料脱泡、陈腐工序；
(5)流延成型工序；
(6)烧结，得到所述氧化铝基板。
本发明所述氧化铝基板中，考虑到氧化锆与氧化铝粉体比重存在差异，采用两步法分散氧化锆复合氧化铝陶瓷基板中的原料粉体，即首先将氧化锆粉与一部分氧化铝粉体进行分散，低温煅烧后，此时ZTA预烧结体中ZrO 2与Al 2O 3粉体间形成一定键合力；然后将ZTA预烧结体再次分散至氧化铝粉体中，以该方法可以很好的提高ZrO 2在ZTA中的分散效果，从而更好的实现ZrO 2助熔效果降低SiO 2、MgO、CaO的加入量。
优选地，所述步骤(1)、(2)中，预分散和混合分散的参数为：分散时间：30-45h，粉体粒度控制范围：D50≤0.8um。
优选地，所述步骤(2)中，低温煅烧的参数为：烧结温度＞1300℃，保温时间为1-3h；破碎的参数为：球磨时间20-40h，粒度控制范围：D50≤0.6um。
优选地，所述步骤(3)中，原料粉体与分散剂混合的参数为：分散时间：30-45h，粒度控制范围：D50≤0.6um；原料粉体与有机粘合剂混合的参数为：分散时间：5-15h，出磨粘度≤1000CPs。
优选地，所述浆料脱泡、陈腐工序的工艺参数如下：(1)浆料脱泡：脱泡压力：-0.05～-0.1MPa，搅拌速度：10-30Hz，浆料温度：15-35℃，浆料粘度：1000-7000Cps；(2)ZTA粉体与粘合剂调和：陈腐时间：5-24h，搅拌速度：0-3Hz，浆料温度控制25-30℃，浆料粘度控制：1000-7000Cps。
优选地，所述流延成型工艺参数为：流延速度：0.7-3m/s，一区温度：15-50℃，二区温度：40-70℃，三区温度：65-110℃，一区风速：0.2-1.5m/s，二区风速：0.8-5m/s，三区风速：0.5-5m/s。
优选地，所述烧结工艺参数为：测片温度：1400-1570℃，保温时间：0.5-4h。
再次，本发明还公开一种所述氧化铝基板的覆铜工艺，包括如下步骤：
(1)铜箔裁剪成合适的尺寸；
(2)铜箔表面预氧化，以提高铜箔表面的键合活性；
(3)氧化铝基板表面清洁并化学处理，以提高表面-OH的基团活性；
(4)第一面覆铜：铜片置于基板表面通过还原气氛炉(炉温控在铜的临界熔点附近)，使金属铜与基体层表面键合；
(5)第二面覆铜：将基板另一面上放置处理好的铜箔，通过还原气氛炉(炉温略低于第一次覆铜温度)，使金属铜与基体层第二面键合。
相对于现有技术，本发明的有益效果为：
本发明氧化锆复合氧化铝陶瓷烧结体中，通过降低助熔剂含量(MgO＜500ppm，CaO≤350ppm，SiO 2＜8000ppm)，降低助熔剂对晶界强度及声子传递速率的影响，同时通过控制ZrO 2初始粒径及分散均匀性实现ZrO 2助熔Al 2O 3基体致密化，实现原位助熔效果，进一步提升氧化铝陶瓷基体的机械强度及热导率。
附图说明
图1为本发明ZTA预烧结体的SEM图；
图2为本发明实施例22的ZTA烧结体SEM图。
具体实施方式
为更好的说明本发明的目的、技术方案和优点，下面将结合附图和具体实施例对本发明作进一步说明。
本发明设置实施例1～15，实施例1～15和对比例1中所述烧结体的各成分及含量(含量单位为WT％)设置如表1所示：
表1实施例1～15中所述烧结体中各成分及含量
Figure PCTCN2019115243-appb-000001
Figure PCTCN2019115243-appb-000002
具体制备方法包括如下步骤：
(1)将原料粉体粉碎，将原料粉体中除氧化铝外的粉体先与一部分氧化铝进行预分散，如附图1所示；
(2)将步骤(1)预分散后的粉体低温煅烧后，如附图2所示，再破碎，然后加入剩余部分的氧化铝粉体，进行进一步混合分散，完成原料粉体的分散混合；预分散和混合分散的参数为：分散时间：30-45h，粉体粒度控制范围：D50≤0.8um；低温煅烧的参数为：烧结温度范围：1300℃-1400℃，保温时间为1-3h；破碎的参数为：球磨时间20-40h，粒度控制范围：D50≤0.6um；
(3)将步骤(2)分散混合后的原料粉体与有机粘合剂、分散剂进行混合；原料粉体与分散剂混合的参数为：分散时间：30-45h，粒度控制范围：D50≤0.6um；原料粉体与有机粘合剂混合的参数为：分散时间：5-15h，出磨粘度≤1000CPs；
(4)浆料脱泡、陈腐工序；浆料脱泡：脱泡压力：-0.05～-0.1MPa，搅拌速度：10-30Hz，浆料温度：15-35℃，浆料粘度：1000-7000Cps；ZTA粉体与粘合剂调和：陈腐时间：5-24h，搅拌速度：0-3Hz，浆料温度控制25-30℃，浆料粘度控制：1000-7000Cps；
(5)流延成型工序；流延速度：0.7-3m/s，一区温度：15-50℃，二区温度：40-70℃，三区温度：65-110℃，一区风速：0.2-1.5m/s，二区风速：0.8-5m/s，三区风速：0.5-5m/s；
(6)烧结，得到所述氧化铝基板；测片温度：1400-1570℃，保温时间：0.5-4h。
分别测定陶瓷基板的绝缘强度、热传导系数、抗折强度(取每组测试最小值记录，样品烧结温度1450℃)。
其中，绝缘强度的测试方法，可按照国家标准GB/T 18791-2002中的测试方法，将实验样品放入变压器油中，对其施加直流或交流电压，并逐渐增加测试电压，直至实验样品被击穿丧失绝缘性能，得出样品的绝缘强度。
热传导系数的测试方法，可按照国家标准GB/T 5598-2015中的测试方法，将样品制成直径d＝10mm的圆片，将试样与同厚度标样在短时间间隔内经激光闪烁热扩散系数测试仪测试得到试样热扩散系数α及比热Cp，通过阿基米德法测试得到试样的体积密度，通过导热系数公式λ＝α·Cp·ρ得到试样热导系数。
抗折强度的测试方法，将样品激光划线切割为l＝40mm、b＝24mm的矩形片状体，划线深度控制在样品厚度的35-50％之间，采用螺旋测微器测得各样品厚度h划线面置于电子万能试验机上，跨距L＝30mm，辊棒直径d＝3mm，上辊棒下降速度v＝0.5mm/min，测得试样临界抗弯力F，通过强度计算公式δ＝3FL/2bh 2得到样品强度结果。
测试结果如表2所示：
表2
Figure PCTCN2019115243-appb-000003
Figure PCTCN2019115243-appb-000004
由图1可以看出，ZTA预烧结体中氧化锆和氧化铝分散均匀，且其二者平均粒径D50的控制合理，如图中标识的两处氧化铝粒径分别为588nm和784nm，标识的两处氧化锆粒径分别为417nm和708nm。
从表2可以看出，氧化锆含量的加入/增加，极大程度提高基片的抗折强度，但同时导致其热传导性能的下降。同时，由实施例17-20可以看出，相同氧化锆含量下，通过降低SiO 2、MgO、CaO的加入量，使得晶界处的助熔剂浓度下降，能进一步提升晶界强度，降低声子传递速率。换而言之，相同氧化锆添加量下，减少SiO 2、MgO、CaO的加入量，能同时达到提升陶瓷烧结体的机械强度和热导率。从表2可以进一步看出，氧化锆含量过低时，基板的强度较低，过高时，热传导系数下降，只有当抗折弯强度和热传导系数二者能很好的匹配时，才较能够同时满足覆铜基板的要求。一般而言，如若能同时保证抗折强度在500MPa以上和热传导系数为27W/m·K以上，更能满足多应用场合的要求，比如覆铜陶瓷基板，这也是本申请中配方优选“含锆化合物(含量以氧化锆形式计算)5-10％、含钇化合物(含量以氧化钇形式计算)0.3-0.8％、含硅化合物(含量以氧化硅形式计算)0.4-0.6％、含钙化合物(含量以氧化钙形式计算)0.01-0.03％、含镁化合物(含量以氧化镁形式计算)0-0.03％，余量为氧化铝”的重要原因。
此外，参照实施例16实验过程中的配比组成，通过氧化铝和氧化锆粉体的研磨和分散，控制氧化铝粒径和氧化锆粒径分布，其余参照上述的工艺方法和测试方法。在实验中，较难控制成型后基板的粒径，故此处不包括始值和末值，具体数据可见表3。
表3
Figure PCTCN2019115243-appb-000005
从表3可发现，控制氧化铝的平均粒径在1.40um左右时，氧化锆平均粒径 的控制在0.4-0.7um范围内(氧化锆晶粒尺寸过低和过高都会对抗着强度造成不良影响)，能适当地提升基板的抗折强度。
其中，图2为实施例22的氧化铝烧结体的SEM图，由图2可见，氧化锆和氧化铝分散均匀，其颗粒尺寸具体可参考图中两处氧化铝粒径的标识，分别为1.35um和888nm。
将上述氧化铝基板进行覆铜，具体方法为：
(1)铜箔裁剪成合适的尺寸；
(2)铜箔表面预氧化，以提高铜箔表面的键合活性；
(3)氧化铝基板表面清洁并化学处理，以提高表面-OH的基团活性；
(4)第一面覆铜：铜片置于基板表面通过还原气氛炉(炉温控在铜的临界熔点附近)，使金属铜与基体层表面键合；
(5)第二面覆铜：将基板另一面上放置处理好的铜箔，通过还原气氛炉(炉温略低于第一次覆铜温度)，使金属铜与基体层第二面键合。
测试覆铜后基板的结合强度和温度可靠性，测试结果如表3所示，具体测试方法如下：
(1)铜板与氧化铝复合氧化锆基板的接合性评价
铜板与氧化铝基板的接合性通过剥离强度测定来评价。测定方法如下所述。用钳子将作为与氧化铝基板接合的铜线路图案的一部分的、宽度为5mm的图案的端部剥离，将该接合基板固定于拉伸试验机的工作台，将上述图案的端部安装于剥离试验机的卡盘。此时，以使氧化铝基板的表面与剥离的上述铜线路图案的角度成为90°(垂直方向)的方式进行设置。之后，使拉伸试验机工作，介由卡盘使剥离的上述图案向上方拉伸、移动，测定此时的最大剥离载荷。将该最大剥离载荷除以宽度(0.5cm)，算出接合强度。
(2)氧化铝复合氧化锆DBC基板温度可靠性的评价
对于制作的ZTA线路基板进行数个循环重复的耐热循环试验，其中以-55℃下15分钟、150℃下15分钟、作为1个循环，其中间隔时间＜10s。每间隔5 个循环之后，采用超声波探伤仪检测金属层与陶瓷基体层的结合情况，当结合层边缘出现＞2mm分层时即判定DBC基板可靠性失效。
表3
Figure PCTCN2019115243-appb-000006
从表3可以看出，与对比例相比，本发明中氧化锆的加入能提高覆铜陶瓷基板的接合强度，但随着氧化锆含量的进一步增加，其接合强度又出现一定程度的下降，这也是本申请烧结体中优选“含锆化合物(含量以氧化锆形式计算)5-10％、含钇化合物(含量以氧化钇形式计算)0.3-0.8％、含硅化合物(含量以氧化硅形式计算)0.4-0.6％、含钙化合物(含量以氧化钙形式计算)0.01-0.03％、含镁化合物(含量以氧化镁形式计算)0-0.03％，余量为氧化铝”的重要原因。
最后所应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。

Claims (10)

  1. 一种氧化锆复合氧化铝陶瓷烧结体，其特征在于，包含以下质量百分含量的成分：含锆化合物(含量以氧化锆形式计算)0.01-20％、含钇化合物(含量以氧化钇形式计算)0-1.75％、含硅化合物(含量以氧化硅形式计算)0.01-0.8％、含钙化合物(含量以氧化钙形式计算)0-0.035％、含镁化合物(含量以氧化镁形式计算)0-0.05％，余量为氧化铝。
  2. 如权利要求1所述的氧化锆复合氧化铝陶瓷烧结体，其特征在于，包含以下质量百分含量的成分：含锆化合物(含量以氧化锆形式计算)5-15％、含钇化合物(含量以氧化钇形式计算)0.3-1％、含硅化合物(含量以氧化硅形式计算)0.04-0.8％、含钙化合物(含量以氧化钙形式计算)0.01-0.03％、含镁化合物(含量以氧化镁形式计算)0-0.03％，余量为氧化铝。
  3. 如权利要求2所述的氧化锆复合氧化铝陶瓷烧结体，其特征在于，包含以下质量百分含量的成分：含锆化合物(含量以氧化锆形式计算)5-10％、含钇化合物(含量以氧化钇形式计算)0.3-0.8％、含硅化合物(含量以氧化硅形式计算)0.4-0.6％、含钙化合物(含量以氧化钙形式计算)0.01-0.03％、含镁化合物(含量以氧化镁形式计算)0-0.03％，余量为氧化铝。
  4. 如权利要求1～3任一项所述的氧化锆复合氧化铝陶瓷烧结体，其特征在于，所述含锆化合物的平均粒径D50为氧化铝的平均粒径D50的(0.1-1.5)倍。
  5. 如权利要求1～3任一项所述的氧化锆复合氧化铝陶瓷烧结体，其特征在于，氧化铝的平均粒径D50为0.8-3um，最大粒径范围为4-10um。
  6. 如权利要求5所述的氧化锆复合氧化铝陶瓷烧结体，其特征在于，氧化铝的平均粒径D50为1.3-2.5um，最大粒径范围为4-7um。
  7. 如权利要求1～3任一项所述的氧化锆复合氧化铝陶瓷烧结体，其特征在于，氧化锆的平均粒径D50为0.2-1.5um，最大粒径范围为1.0-2.5um。
  8. 如权利要求7所述的氧化锆复合氧化铝陶瓷烧结体，其特征在于，氧化锆的平均粒径D50为0.4-0.8um，最大粒径范围为1.2-1.8um。
  9. 一种包含权利要求1～3任一项所述氧化锆复合氧化铝陶瓷烧结体的氧化铝基板。
  10. 一种如权利要求9所述氧化铝基板的制备方法，其特征在于，包括如下步骤：
    (1)原料粉体粉碎，将原料粉体中除氧化铝外的粉体先与一部分氧化铝进行预分散；
    (2)将步骤(1)预分散后的粉体低温煅烧后，再破碎，然后加入剩余部分的氧化铝粉体，进行进一步混合分散，完成原料粉体的分散混合；
    (3)将步骤(2)分散混合后的原料粉体与有机粘合剂、分散剂进行混合；
    (4)浆料脱泡、陈腐工序；
    (5)流延成型工序；
    (6)烧结，得到所述氧化铝基板。
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