Super-tough corrosion-resistant long-life ceramic chopper and preparation method thereof
By preparing ultra-tough corrosion-resistant long-life ceramic splitters, the problem of short service life of traditional ceramic splitters is solved, and efficient application in semiconductor packaging bonding processes is achieved.
Patent Information
- Application Number
- CN202510513078.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-23
- Publication Date
- 2025-07-25
AI Technical Summary
Traditional ceramic splitting knife materials have a short service life in the bonding process of semiconductor packaging, which limits production efficiency and cost control.
The crystal tough phase composition, corrosion-resistant and stable structure composition, strong and tough temperature-guiding composition are mixed with a specific ratio of alumina and flux, and the ultra-tough corrosion-resistant long-life ceramic chopper is prepared through high temperature and high pressure and sintering processes to form a stable microstructure.
It significantly improves the service life of the ceramic splitter, can effectively resist wear, fatigue and high temperature impact during the bonding process, and meets the requirements of semiconductor packaging bonding.
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of ceramic capillary knives, and particularly relates to a super-tough, corrosion-resistant and long-life ceramic capillary knife and a preparation method thereof. Background Art
[0002] In the bonding process of semiconductor packaging, the ceramic capillary knife, as the core execution component of the wire bonding process, its material properties directly determine the bonding quality, production yield and equipment operation rate. Traditional ceramic capillary knife materials such as Al2O3-ZrO2-based ceramic capillary knives, etc., gradually expose the problem of short service life during long-term use, which limits the production efficiency and cost control of semiconductor packaging. In order to meet the growing demands of the semiconductor industry, it is urgent to develop a new material formula that can significantly improve the service life of ceramic capillary knives. Summary of the Invention
[0003] In order to solve the technical problems existing in the prior art, the purpose of the present invention is to provide a super-tough, corrosion-resistant and long-life ceramic capillary knife and a preparation method thereof.
[0004] In order to achieve the above purpose and reach the above technical effects, the technical solution adopted by the present invention is as follows:
[0005] A super-tough, corrosion-resistant and long-life ceramic capillary knife, the preparation raw materials of the super-tough, corrosion-resistant and long-life ceramic capillary knife include the following components in molar ratio:
[0006] Crystal toughness composite phase composition 10%-15%
[0007] Corrosion-resistant stable structure composition 5%-15%
[0008] Tough and heat-conducting composition 10%-15%
[0009] Aluminum oxide 60%-70%
[0010] Flux 1%-5%.
[0011] Further, the crystal toughness composite phase composition includes the following components in molar ratio:
[0012] Yttrium oxide 20%-30%
[0013] Zirconium oxide 25%-35%
[0014] Silicon nitride 10%-20%
[0015] Silicon carbide 10%-20%
[0016] Ytterbium oxide 2%-8%
[0017] Silicon carbide titanium MAX phase nanosheets 8%-12%.
[0018] Further, the corrosion-resistant and structure-stabilizing composition comprises the following components in molar ratio:
[0019] Cerium oxide 15% - 25%
[0020] Lanthanum oxide 15% - 25%
[0021] Zirconium silicate 15% - 25%
[0022] Calcium phosphate 10% - 20%
[0023] Calcium fluorophosphate 5% - 15%
[0024] Molybdenum silicide nanowires 10% - 20%.
[0025] Further, the toughening and heat-conducting composition comprises the following components in molar ratio:
[0026] Aluminum oxide 30% - 40%
[0027] Aluminum nitride 25% - 35%
[0028] Titanium boride 10% - 20%
[0029] Zirconium boride 5% - 15%
[0030] Barium titanate 5% - 15%.
[0031] Further, the flux is titanium dioxide.
[0032] The present invention also discloses a preparation method of a super-tough, corrosion-resistant and long-life ceramic splitting knife, comprising the following steps:
[0033] 1) Prepare a crystal-tough composite phase composition, a corrosion-resistant and structure-stabilizing composition, and a toughening and heat-conducting composition;
[0034] 2) Mix the crystal-tough composite phase composition, the corrosion-resistant and structure-stabilizing composition, and the toughening and heat-conducting composition obtained in step 1) evenly according to a molar ratio of 4:3:3 to obtain a mixture A;
[0035] 3) Mix the mixture A obtained in step 2) with aluminum oxide and the flux evenly according to a molar ratio of 12:85:3 to obtain a mixture B;
[0036] 4) Make the mixture B obtained in step 3) into a green body of a ceramic splitting knife, and then carry out degreasing and sintering to finally obtain the required super-tough, corrosion-resistant and long-life ceramic splitting knife.
[0037] Further, in step 1), the crystal-tough composite phase composition is prepared by the following steps:
[0038] According to the molar ratio, 20%-30% of yttrium oxide, 25%-35% of zirconium oxide, 10%-20% of silicon nitride, 10%-20% of silicon carbide, 2%-8% of ytterbium oxide, and 8%-12% of MAX-phase titanium silicon carbide nanosheets are placed into a high-temperature and high-pressure reactor. Argon is introduced until the pressure reaches 15-20 MPa, and the temperature is raised at a rate of 8-12 °C / min to 1650 °C-1800 °C and held for 6-8 h to obtain the desired crystal-tough composite phase composition.
[0039] Further, in step 1), the corrosion-resistant and structure-stable composition is prepared by the following steps:
[0040] According to the molar ratio, 15%-25% of cerium oxide, 15%-25% of lanthanum oxide, 15%-25% of zirconium silicate, 10%-20% of calcium phosphate, 5%-15% of calcium fluorophosphate, and 10%-20% of molybdenum silicide nanowires are placed into a high-temperature furnace, and the temperature is raised at a rate of 8-12 °C / min to 1600 °C-1800 °C and held for 6-8 h to obtain the desired corrosion-resistant and structure-stable composition.
[0041] Further, in step 1), the tough and heat-conducting composition is prepared by the following steps:
[0042] According to the molar ratio, 30%-40% of aluminum oxide, 25%-35% of aluminum nitride, 10%-20% of titanium boride, 5%-15% of zirconium boride, and 5%-15% of barium titanate are placed into a high-temperature and high-pressure reactor. Argon is introduced until the pressure reaches 15-20 MPa, and the temperature is raised at a rate of 8-12 °C / min to 1700 °C-1800 °C and held for 6-8 h to obtain the desired tough and heat-conducting composition.
[0043] Further, in step 4), the debinding temperature is 500-700 °C, the debinding time is 8-12 h; the sintering temperature is 1400-1500 °C, the sintering time is 8-12 h, the sintering atmosphere is argon protection, and the heating rate is 10-15 °C / min.
[0044] Compared with the prior art, the beneficial effects of the present invention are:
[0045] First, the crystal-tough composite phase composition JRC, the corrosion-resistant and structure-stable composition ESC, and the tough and heat-conducting composition STTC are synthesized separately, and then the crystal-tough composite phase composition JRC, the corrosion-resistant and structure-stable composition ESC, and the tough and heat-conducting composition STTC are added to aluminum oxide. In this way, a super-tough, corrosion-resistant, and long-life ceramic bonding tool is made. It has a more stable microstructure inside, and its properties such as hardness, elastic modulus, and thermal conductivity are excellent. The service life is increased by more than 10% compared with traditional ceramic bonding tools. When used in semiconductor packaging bonding applications, it can meet the requirements of various bonding processes and effectively resist the damage to the ceramic bonding tool caused by factors such as wear, fatigue, and high-temperature impact during the bonding process. Detailed Embodiments
[0046] The present invention will be elaborated in detail below so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby making a clearer and more definite definition of the protection scope of the present invention.
[0047] A brief overview of one or more aspects is given below to provide a basic understanding of these aspects. This overview is not an exhaustive survey of all contemplated aspects, and is neither intended to identify key or decisive elements of all aspects nor to define the scope of any or all aspects. Its sole purpose is to present some concepts of one or more aspects in a simplified form as a prelude to the more detailed description that follows.
[0048] On the one hand, the present invention discloses a super-tough, corrosion-resistant and long-life ceramic capillary, and its preparation raw materials include the following components in molar ratio:
[0049] Crystal toughness composite composition 10%-15%
[0050] Corrosion-resistant stable structure composition 5%-15%
[0051] Tough and heat-conducting composition 10%-15%
[0052] Aluminum oxide 60%-70%
[0053] Flux 1%-5%.
[0054] In some embodiments, the crystal toughness composite composition includes the following components in molar ratio:
[0055] Yttrium oxide 20%-30%
[0056] Zirconium oxide 25%-35%
[0057] Silicon nitride 10%-20%
[0058] Silicon carbide 10%-20%
[0059] Ytterbium oxide 2%-8%
[0060] Titanium carbide MAX phase nanosheets 8%-12%.
[0061] In some embodiments, the corrosion-resistant stable structure composition includes the following components in molar ratio:
[0062] Cerium oxide 15%-25%
[0063] Lanthanum oxide 15%-25%
[0064] Zirconium silicate 15%-25%
[0065] Calcium phosphate 10%-20%
[0066] Calcium fluorophosphate 5%-15%
[0067] Molybdenum silicide nanowires 10%-20%.
[0068] In some embodiments, the tough and heat-conducting composition comprises the following components in molar ratio:
[0069] Aluminum oxide 30%-40%
[0070] Aluminum nitride 25%-35%
[0071] Titanium boride 10%-20%
[0072] Zirconium boride 5%-15%
[0073] Barium titanate 5%-15%.
[0074] In some embodiments, the flux is titanium dioxide.
[0075] On the other hand, the present invention also discloses a preparation method of a super-tough, corrosion-resistant and long-life ceramic splitting tool, comprising the following steps:
[0076] 1) Prepare a crystal-tough combined phase composition, a corrosion-resistant stable structure composition, and a tough and heat-conducting composition;
[0077] 2) Mix the crystal-tough combined phase composition, the corrosion-resistant stable structure composition, and the tough and heat-conducting composition obtained in step 1) evenly according to a molar ratio of 4:3:3 to obtain a mixture A;
[0078] 3) Uniformly mix the mixture A obtained in step 2) with aluminum oxide and the flux according to a molar ratio of 12:85:3 to obtain a mixture B;
[0079] 4) Make the mixture B obtained in step 3) into a green body of the ceramic splitting tool, and then carry out debinding and sintering to finally obtain the required super-tough, corrosion-resistant and long-life ceramic splitting tool.
[0080] In step 1), the crystal-tough combined phase composition is prepared by the following steps:
[0081] According to the molar ratio, put 20%-30% of yttrium oxide, 25%-35% of zirconium oxide, 10%-20% of silicon nitride, 10%-20% of silicon carbide, 2%-8% of ytterbium oxide, and 8%-12% of MAX phase nanosheets of titanium silicon carbide into a high-temperature and high-pressure reactor, introduce argon until the pressure reaches 15-20 MPa, heat up at a heating rate of 8-12 °C / min to 1650 °C - 1800 °C, and keep warm for 6-8 h to obtain the required crystal-tough combined phase composition.
[0082] In step 1), the corrosion-resistant stable structure composition is prepared by the following steps:
[0083] According to the molar ratio, 15%-25% of cerium oxide, 15%-25% of lanthanum oxide, 15%-25% of zirconium silicate, 10%-20% of calcium phosphate, 5%-15% of calcium fluorophosphate and 10%-20% of molybdenum silicide nanowires are put into a high-temperature furnace, and the temperature is increased to 1600°C-1800°C at a heating rate of 8-12°C / min, and the temperature is kept for 6-8h to obtain the desired corrosion-resistant and structurally stable composition.
[0084] In step 1), the strong and tough thermal conductive composition is prepared by the following steps:
[0085] According to the molar ratio, 30%-40% of aluminum oxide, 25%-35% of aluminum nitride, 10%-20% of titanium boride, 5%-15% of zirconium boride and 5%-15% of barium titanate are placed in a high-temperature and high-pressure reactor, argon is introduced until the pressure reaches 15-20MPa, the temperature is increased to 1700℃-1800℃ at a heating rate of 8-12℃ / min, and the temperature is kept for 6-8h to obtain the required strong and tough thermal conductive composition.
[0086] In step 4), the degreasing temperature is 500-700°C, and the degreasing time is 8-12h; the sintering temperature is 1400-1500°C, and the sintering time is 8-12h. The sintering atmosphere is argon protection, and the heating rate is 10-15°C / min.
[0087] Example 1
[0088] A super-tough, corrosion-resistant and long-life ceramic splitter, the raw materials for preparing the same include the following components in molar ratio:
[0089] Crystal toughness composite JRC 12%
[0090] ESC 10% corrosion resistant structural composition
[0091] Strong and tough thermal conductive composition STTC 13%
[0092] Alumina 62%
[0093] Titanium dioxide flux 3%.
[0094] In this embodiment, the crystal-tough composite composition JRC includes the following components in molar ratio:
[0095] Yttrium oxide 25%
[0096] Zirconia 30%
[0097] Silicon Nitride 15%
[0098] Silicon carbide 15%
[0099] Ytterbium oxide 5%
[0100] Silicon Carbide Titanium MAX Phase Nanosheets 10%.
[0101] The crystal-tough composite JRC is prepared by the following steps:
[0102] According to the molar ratio, 25% yttrium oxide, 30% zirconium oxide, 15% silicon nitride, 15% silicon carbide, 5% ytterbium oxide and 10% silicon carbide titanium MAX phase nanosheets are mixed evenly and put into a high-temperature and high-pressure reactor. Argon is introduced until the pressure reaches 18 MPa. The temperature is increased to 1650°C at a heating rate of 10°C / min and kept warm for 6 hours to obtain the desired crystalline-tough composite phase composition.
[0103] Under high temperature, high pressure and argon protection conditions, yttrium oxide and zirconium oxide undergo partial solid solution reaction to form a yttrium oxide-zirconia solid solution phase with a certain toughness. At the same time, silicon nitride and silicon carbide react to form a covalent bond network structure between silicon atoms and nitrogen atoms and carbon atoms, in which the nitrogen atoms in silicon nitride partially replace the silicon atoms in silicon carbide and combine with the surrounding carbon atoms to form a special Si-CN ternary structural unit, which is intertwined with the yttrium oxide-zirconia solid solution.
[0104] Yb in Ytterbium Oxide (Yb2O3) 3+ Partially replace Y in yttrium oxide (Y2O3) 3+ , due to Yb 3+ The ion radius is large (0.102nm), which will cause lattice distortion and thus increase the hardness of the product.
[0105] By introducing silicon carbide titanium (Ti3SiC2) MAX phase nanosheets, the layered structure is inserted at the grain boundary, absorbing the crack propagation energy through the interlayer slip mechanism, thereby improving the fracture toughness of the product. This structure gives the product higher hardness and toughness. During the use of the ceramic splitter, it can effectively resist the impact and friction during bonding, reduce product wear and microcracks, and thus increase the product life.
[0106] The corrosion-resistant and structurally stable composition ESC comprises the following components in molar ratio:
[0107] Cerium oxide 20%
[0108] Lanthanum oxide 20%
[0109] Zirconium silicate 20%
[0110] Calcium phosphate 15%
[0111] Calcium fluorophosphate 10%
[0112] Molybdenum silicide nanowires 15%.
[0113] The corrosion-resistant and structure-stabilizing composition ESC is prepared by the following steps:
[0114] According to the molar ratio, 20% cerium oxide, 20% lanthanum oxide, 20% zirconium silicate, 15% calcium phosphate, 10% calcium fluorophosphate and 15% molybdenum silicide nanowires are put into a high-temperature furnace, heated to 1600°C at a heating rate of 8°C / min, and kept warm for 8 hours to obtain the desired corrosion-resistant and structurally stable composition.
[0115] Under high temperature, cerium oxide and lanthanum oxide react with zirconium silicate, and rare earth elements (cerium and lanthanum) partially replace zirconium atoms in zirconium silicate to form a rare earth-doped zirconium silicate structure, which can stabilize the crystal structure of the material and improve its chemical stability. Calcium phosphate and calcium fluorophosphate decompose at high temperature and react with other components to form complex compounds containing phosphorus and calcium that fill the gaps in the crystal structure, enhancing the material's resistance to corrosive substances (such as moisture, chemical reagents, etc.) that may exist in the bonding environment, preventing ceramic splitters from being damaged by corrosion and extending their service life. Molybdenum silicide (MoSi2) nanowires are interspersed in the Ca-PF glass phase, increasing the number of thermal shock cycles through mechanical interlocking, while their high melting point can maintain high-temperature structural stability.
[0116] The tough thermal conductive composition STTC comprises the following components in molar ratio:
[0117] Alumina 35%
[0118] Aluminum Nitride 30%
[0119] Titanium boride 15%
[0120] Zirconium boride 10%
[0121] Barium titanate 10%.
[0122] The tough thermal conductive composition STTC is prepared by the following steps:
[0123] According to the molar ratio, 35% aluminum oxide, 30% aluminum nitride, 15% titanium boride, 10% zirconium boride and 10% barium titanate are placed in a high-temperature and high-pressure reactor, argon gas is introduced until the pressure reaches 16 MPa, the temperature is increased to 1700°C at a heating rate of 12°C / min, and the temperature is kept for 7 hours to obtain the required strong and tough thermal conductive composition.
[0124] Under high temperature and high pressure, aluminum oxide reacts with aluminum nitride to form an aluminum oxide and nitrogen compound phase, which improves the toughness of the material. Solid solution and diffusion reactions occur between titanium boride and zirconium boride to form a titanium boride-zirconium boride composite phase, which enhances the hardness and thermal conductivity of the material. Barium titanate undergoes a crystal transformation at high temperatures and interacts with other components to form special polarized micro-regions inside the material, which helps to evenly disperse and conduct heat and reduce the degradation of material properties caused by local overheating. This material, which has both strong toughness and good thermal conductivity, can cope with the dual effects of thermal stress and mechanical stress during the bonding process, avoiding reduced service life due to thermal fatigue and mechanical damage.
[0125] A preparation method of a super-tough, corrosion-resistant and long-life ceramic splitting tool includes the following steps:
[0126] 1) Prepare a crystal-tough composite phase composition JRC, a corrosion-resistant stable structure composition ESC, and a strong-tough heat-conducting composition STTC;
[0127] 2) Mix the crystal-tough composite phase composition JRC, the corrosion-resistant stable structure composition ESC, and the strong-tough heat-conducting composition STTC obtained in step 1) in a three-dimensional mixer for 5 h according to a molar ratio of 4:3:3 to ensure uniform mixing and obtain a mixture A;
[0128] 3) Mix the mixture A obtained in step 2) with alumina and a flux in a planetary ball mill using zirconia balls as the grinding medium, with a ball-to-material ratio of 4:1 and a rotation speed of 250 rpm, and grind for 6 h to ensure uniform mixing and obtain a mixture B;
[0129] 4) Use an injection molding process to form the mixture B obtained in step 3) into a green body of the ceramic splitting tool, with an injection pressure of 120 MPa and an injection temperature of 180 °C. Subsequently, place the green body in a debinding furnace for debinding treatment, with a debinding temperature of 600 °C and a debinding time of 10 h to remove the organic matter in the green body. Then, place the debound body in a high-temperature sintering furnace for sintering, with a sintering temperature of 1500 °C, a sintering time of 8 h, an argon protection sintering atmosphere, and a heating rate of 15 °C / min. After sintering, the final ceramic splitting tool product can be obtained.
[0130] Example 2
[0131] A super-tough, corrosion-resistant and long-life ceramic splitting tool, the preparation raw materials of which include the following components in molar ratios:
[0132] Crystal-tough composite phase composition 15%
[0133] Corrosion-resistant stable structure composition 5%
[0134] Strong-tough heat-conducting composition 10%
[0135] Alumina 69%
[0136] Titanium dioxide flux 1%.
[0137] The crystal-tough composite phase composition includes the following components in molar ratios:
[0138] Yttrium oxide 30%
[0139] Zirconia 25%
[0140] Silicon nitride 20%
[0141] Silicon carbide 10%
[0142] 3% ytterbium oxide
[0143] 12% titanium carbide MAX-phase nanosheets
[0144] The corrosion-resistant and structure-stabilizing composition comprises the following components in molar ratio:
[0145] 15% cerium oxide
[0146] 25% lanthanum oxide
[0147] 25% zirconium silicate
[0148] 10% calcium phosphate
[0149] 5% calcium fluorophosphate
[0150] 20% molybdenum silicide nanowires
[0151] The toughening and heat-conducting composition comprises the following components in molar ratio:
[0152] 40% aluminum oxide
[0153] 25% aluminum nitride
[0154] 10% titanium boride
[0155] 10% zirconium boride
[0156] 15% barium titanate
[0157] A preparation method of a super-tough, corrosion-resistant and long-life ceramic splitting tool, comprising the following steps:
[0158] 1) Prepare a crystal-tough composite phase composition, a corrosion-resistant and structure-stabilizing composition, and a toughening and heat-conducting composition;
[0159] 2) Mix the crystal-tough composite phase composition, the corrosion-resistant and structure-stabilizing composition, and the toughening and heat-conducting composition obtained in step 1) evenly according to a molar ratio of 4:3:3 to obtain mixture A;
[0160] 3) Mix the mixture A obtained in step 2) with aluminum oxide and a flux evenly according to a molar ratio of 12:85:3 to obtain mixture B;
[0161] 4) Make the mixture B obtained in step 3) into a green body of the ceramic splitting tool, and then carry out debinding and sintering. The debinding temperature is 500 °C, the debinding time is 12 h, the sintering temperature is 1400 °C, the sintering time is 12 h, the sintering atmosphere is argon protection, and the heating rate is 10 °C / min, finally obtaining the required super-tough, corrosion-resistant and long-life ceramic splitting tool.
[0162] In step 1), the crystal-tough composite phase composition is prepared by the following steps:
[0163] Yttrium oxide 30%, zirconium oxide 25%, silicon nitride 20%, silicon carbide 10%, ytterbium oxide 3% and MAX phase nanosheets of titanium silicon carbide 12% are put into a high-temperature and high-pressure reactor according to the molar ratio. Argon is introduced until the pressure reaches 15 MPa, and the temperature is raised to 1650 °C at a heating rate of 8 °C / min and kept for 6 h to obtain the required crystal-tough composite phase composition.
[0164] In step 1), the corrosion-resistant and structure-stabilizing composition is prepared by the following steps:
[0165] Cerium oxide 15%, lanthanum oxide 25%, zirconium silicate 25%, calcium phosphate 10%, calcium fluorophosphate 5% and molybdenum silicide nanowires 20% are put into a high-temperature furnace according to the molar ratio, and the temperature is raised to 1600 °C at a heating rate of 8 °C / min and kept for 6 h to obtain the required corrosion-resistant and structure-stabilizing composition.
[0166] In step 1), the tough and heat-conducting composition is prepared by the following steps:
[0167] Aluminum oxide 40%, aluminum nitride 25%, titanium boride 10%, zirconium boride 10% and barium titanate 15% are put into a high-temperature and high-pressure reactor according to the molar ratio. Argon is introduced until the pressure reaches 15 MPa, and the temperature is raised to 1700 °C at a heating rate of 8 °C / min and kept for 6 h to obtain the required tough and heat-conducting composition.
[0168] The rest is the same as in Example 1.
[0169] Comparative Example 1
[0170] The difference between this comparative example and Example 1 is that this comparative example has no mixture A, only aluminum oxide and flux, that is, the weight ratio of mixture A, aluminum oxide, and flux is 0:95:5.
[0171] The rest is the same as in Example 1.
[0172] Comparative Example 2
[0173] The difference between this comparative example and Example 1 is that the weight ratio of the crystal-tough composite phase composition JRC, the corrosion-resistant and structure-stabilizing composition ESC, and the tough and heat-conducting composition STTC in this comparative example is 3:4:3.
[0174] The rest is the same as in Example 1.
[0175] Comparative Example 3
[0176] The difference between this comparative example and Example 1 is that the weight ratio of the crystal-tough composite phase composition JRC, the corrosion-resistant and structure-stabilizing composition ESC, and the tough and heat-conducting composition STTC in this comparative example is 3:3:4.
[0177] The rest is the same as in Example 1.
[0178] Comparative Example 4
[0179] The difference between this comparative example and Example 1 is that the weight ratio of the crystal-tough combined phase composition JRC, the corrosion-resistant stable structure composition ESC, and the tough and heat-conducting composition STTC in this comparative example is 2:4:4.
[0180] The rest is the same as in Example 1.
[0181] Comparative Example 5
[0182] The difference between this comparative example and Example 1 is that the weight ratio of the crystal-tough combined phase composition JRC, the corrosion-resistant stable structure composition ESC, and the tough and heat-conducting composition STTC in this comparative example is 4:2:4.
[0183] The rest is the same as in Example 1.
[0184] Experimental instruments:
[0185] Hardness testing instrument: Nano Indenter G200, with a maximum loading load of 50 mN, a loading rate of 0.5 mN / s, and a holding time of 10 s.
[0186] Elastic modulus testing instrument: Ultrasonic pulse echo tester (UPK-300), with a frequency range of 1 - 10 MHz, capable of measuring longitudinal and transverse wave velocities, and then calculating the elastic modulus.
[0187] Thermal conductivity testing instrument: Thermal Constants Analyzer (TPS2500S), using the transient plane heat source method, with the test sample size being a square with a side length of 10 mm and a thickness of 3 mm.
[0188] Bonding life testing equipment: High-precision semiconductor bonder (Kulicke & Soffa 4526), with the bonding pressure accurately controllable within 30 - 200 g, the bonding temperature range being 120 - 350 °C, the bonding time being 5 - 100 ms, using aluminum wire bonding with an aluminum wire diameter of 30 μm, and taking the number of bondings when obvious wear, fracture, or bonding failure (such as insufficient bonding strength, short circuit, etc.) occurs on the bonding tool as the bonding life index.
[0189] Performance testing:
[0190] Hardness testing: Take the ceramic bonding tool samples of Example 1 and Comparative Examples 1 - 5, and conduct hardness testing on a nano indenter. Each sample is tested at 6 points, and the average value is taken.
[0191] Elastic modulus testing: Use an ultrasonic pulse echo tester to conduct elastic modulus testing on the samples. Each sample is tested 4 times, and the average value is taken.
[0192] Thermal conductivity test: After processing the samples into appropriate sizes, place them in a thermal constant analyzer and conduct thermal conductivity tests at room temperature. Each sample is tested 3 times and the average value is taken.
[0193] Bonding life test: Install the ceramic capillary knives of Example 1 and Comparative Examples 1-5 on a high-precision semiconductor bonder respectively. Set the bonding pressure to 80 g, the bonding temperature to 200 °C, and the bonding time to 30 ms. Conduct aluminum wire bonding experiments and record the number of bondings until bonding failure occurs. Test 12 samples for each formulation and take the average value.
[0194] The test results are shown in Table 1.
[0195] Table 1
[0196] Average hardness / GPa Average elastic modulus / GPa Average thermal conductivity / W / (m·K) Average bonding life / times Example 1 23.8 388 34 680000 Comparative Example 1 16.4 365 25.1 600000 Comparative Example 2 20.5 372 26.3 620000 Comparative Example 3 21.8 370 28.8 630000 Comparative Example 4 19.3 378 27.2 600000 Comparative Example 5 22.1 366 30.6 610000
[0197] As can be seen from Table 1, the hardness, elastic modulus, thermal conductivity, and service life of the super-tough and corrosion-resistant ceramic capillary knife prepared in Example 1 are all higher than those of Comparative Examples 1-5. This shows that only by using the formulation of the present invention can a super-tough and corrosion-resistant ceramic capillary knife be made. Without mixture A, or if the weight ratios of the crystal-tough composite phase composition JRC, corrosion-resistant stable structure composition ESC, and tough and heat-conducting composition STTC are not within the scope disclosed in the present invention, the required super-tough and corrosion-resistant ceramic capillary knife cannot be made. At the same time, it shows that the super-tough and corrosion-resistant ceramic capillary knife of the present invention can significantly improve the service life of the ceramic capillary knife while ensuring good properties such as hardness, elastic modulus, and thermal conductivity. When applied in semiconductor packaging bonding, it can better meet the requirements of various bonding processes and effectively resist the damage to the ceramic capillary knife caused by factors such as wear, fatigue, and high-temperature impact during the bonding process.
[0198] For the parts or structures not specifically described in the present invention, existing technologies or existing products can be adopted and will not be elaborated here.
[0199] The above are only the embodiments of the present invention, and do not limit the patent scope of the present invention accordingly. Any equivalent structure or equivalent process transformation made by using the content of the specification of the present invention, or directly or indirectly applied in other related technical fields, shall be similarly included in the patent protection scope of the present invention.
Claims
1. A super-tough, corrosion-resistant and long-life ceramic bonding tool, characterized in that, The preparation raw materials of the super-tough, corrosion-resistant and long-life ceramic splitting tool include the following components in molar ratio: Crystalline toughness composite composition 10%-15% Corrosion-resistant stable structure composition 5%-15% Toughness and heat conduction composite composition 10%-15% Aluminum oxide 60%-70% Flux 1%-5%.
2. The super-tough, corrosion-resistant and long-life ceramic splitting tool according to claim 1, characterized in that, The crystalline toughness composite composition includes the following components in molar ratio: Yttrium oxide 20%-30% Zirconium oxide 25%-35% Silicon nitride 10%-20% Silicon carbide 10%-20% Ytterbium oxide 2%-8% Titanium silicon carbide MAX phase nanosheets 8%-12%.
3. The super-tough, corrosion-resistant and long-life ceramic splitting knife according to claim 1, characterized in that, The corrosion-resistant stable structure composition includes the following components in molar ratio: Cerium oxide 15%-25% Lanthanum oxide 15%-25% Zirconium silicate 15%-25% Calcium phosphate 10%-20% Calcium fluorophosphate 5%-15% Molybdenum silicide nanowires 10%-20%.
4. The super-tough, corrosion-resistant and long-life ceramic cleaving tool according to claim 1, wherein The toughness and heat conduction composite composition includes the following components in molar ratio: Aluminum oxide 30%-40% Aluminum nitride 25%-35% Titanium boride 10%-20% Zirconium boride 5%-15% Barium titanate 5%-15%.
5. A super-tough, corrosion-resistant and long-life ceramic splitting tool according to claim 1, characterized in that, The flux is titanium dioxide.
6. The preparation method of a super-tough, corrosion-resistant and long-life ceramic bonding tool according to any one of claims 1-5, characterized in that It includes the following steps: 1) Prepare the crystalline toughness composite composition, the corrosion-resistant stable structure composition, and the toughness and heat conduction composite composition; 2) Mix the crystalline toughness composite composition, the corrosion-resistant stable structure composition, and the toughness and heat conduction composite composition obtained in step 1) evenly according to a molar ratio of 4:3:3 to obtain mixture A; 3) Uniformly mix the mixture A obtained in step 2) with aluminum oxide and the flux according to a molar ratio of 12:85:3 to obtain mixture B; 4) Make the mixture B obtained in step 3) into a green body of the ceramic splitting tool, and then carry out degreasing and sintering to finally obtain the required super-tough, corrosion-resistant and long-life ceramic splitting tool.
7. The preparation method of a super-tough, corrosion-resistant and long-life ceramic splitting tool according to claim 6, characterized in that, In step 1), the crystalline toughness composite composition is prepared by the following steps: According to the molar ratio, put 20%-30% of yttrium oxide, 25%-35% of zirconium oxide, 10%-20% of silicon nitride, 10%-20% of silicon carbide, 2%-8% of ytterbium oxide, and 8%-12% of titanium silicon carbide MAX phase nanosheets into a high-temperature and high-pressure reactor, introduce argon until the pressure reaches 15-20 MPa, heat up at a heating rate of 8-12 °C / min to 1650 °C - 1800 °C, and keep the temperature for 6-8 h to obtain the required crystalline toughness composite composition.
8. The method for preparing a super-tough, corrosion-resistant and long-life ceramic splitter according to claim 6, characterized in that: In step 1), the corrosion-resistant stable structure composition is prepared by the following steps: According to the molar ratio, put 15%-25% of cerium oxide, 15%-25% of lanthanum oxide, 15%-25% of zirconium silicate, 10%-20% of calcium phosphate, 5%-15% of calcium fluorophosphate, and 10%-20% of molybdenum silicide nanowires into a high-temperature furnace, heat up at a heating rate of 8-12 °C / min to 1600 °C - 1800 °C, and keep the temperature for 6-8 h to obtain the required corrosion-resistant stable structure composition.
9. The preparation method of a super-tough, corrosion-resistant and long-life ceramic splitting tool according to claim 6, characterized in that, In step 1), the toughness and heat conduction composite composition is prepared by the following steps: According to the molar ratio, 30%-40% of alumina, 25%-35% of aluminum nitride, 10%-20% of titanium boride, 5%-15% of zirconium boride and 5%-15% of barium titanate are put into a high-temperature and high-pressure reactor, and argon is introduced until the pressure reaches 15-20 MPa. Then, the temperature is raised to 1700℃-1800℃ at a heating rate of 8-12℃ / min and kept warm for 6-8 h to obtain the required tough and heat-conducting composition.
10. The preparation method of a super-tough, corrosion-resistant and long-life ceramic splitting tool according to claim 6, characterized in that, In step 4), the debinding temperature is 500-700℃, and the debinding time is 8-12 h; the sintering temperature is 1400-1500℃, the sintering time is 8-12 h, the sintering atmosphere is argon protection, and the heating rate is 10-15℃ / min.