WO2022156636A1 - 一种高热导、净尺寸氮化硅陶瓷基片的制备方法 - Google Patents
一种高热导、净尺寸氮化硅陶瓷基片的制备方法 Download PDFInfo
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- WO2022156636A1 WO2022156636A1 PCT/CN2022/072352 CN2022072352W WO2022156636A1 WO 2022156636 A1 WO2022156636 A1 WO 2022156636A1 CN 2022072352 W CN2022072352 W CN 2022072352W WO 2022156636 A1 WO2022156636 A1 WO 2022156636A1
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- silicon nitride
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- ceramic substrate
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 87
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000000758 substrate Substances 0.000 title claims abstract description 87
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- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 238000005245 sintering Methods 0.000 claims abstract description 59
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 50
- 239000000843 powder Substances 0.000 claims abstract description 37
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 27
- 239000012298 atmosphere Substances 0.000 claims abstract description 25
- 238000007493 shaping process Methods 0.000 claims abstract description 23
- 238000009849 vacuum degassing Methods 0.000 claims abstract description 18
- 230000001681 protective effect Effects 0.000 claims abstract description 13
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- 238000002156 mixing Methods 0.000 claims abstract description 10
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- 239000011268 mixed slurry Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 51
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 25
- 238000010345 tape casting Methods 0.000 claims description 23
- 239000007789 gas Substances 0.000 claims description 19
- 238000005121 nitriding Methods 0.000 claims description 13
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims description 10
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- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 230000003746 surface roughness Effects 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 8
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims description 7
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 7
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 6
- -1 sintering aid Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- 238000002955 isolation Methods 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 4
- 239000013530 defoamer Substances 0.000 claims description 3
- 239000007767 bonding agent Substances 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 1
- 238000000465 moulding Methods 0.000 abstract description 5
- 239000002002 slurry Substances 0.000 description 25
- 239000000463 material Substances 0.000 description 13
- 239000002994 raw material Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 238000005253 cladding Methods 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 7
- 238000005266 casting Methods 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
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- 238000003754 machining Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 235000021384 green leafy vegetables Nutrition 0.000 description 2
- 238000000462 isostatic pressing Methods 0.000 description 2
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- 229920001778 nylon Polymers 0.000 description 2
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- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- DEXFNLNNUZKHNO-UHFFFAOYSA-N 6-[3-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-3-oxopropyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)C(CCC1=CC2=C(NC(O2)=O)C=C1)=O DEXFNLNNUZKHNO-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000009916 joint effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
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Definitions
- the invention relates to a preparation method of a silicon nitride ceramic substrate with high thermal conductivity and net size, and belongs to the field of ceramic material preparation.
- semiconductor devices have developed rapidly along the direction of high power, high frequency and integration.
- the heat generated by the operation of the semiconductor device is a key factor that causes the failure of the semiconductor device, and the thermal conductivity of the insulating substrate is the key to affecting the heat dissipation of the overall semiconductor device.
- semiconductor devices often face complex mechanical environments such as bumps and vibrations during use, which imposes strict requirements on the mechanical reliability of the materials used.
- Silicon nitride (Si 3 N 4 ) ceramics with high thermal conductivity have excellent mechanical and thermal properties.
- the excellent mechanical properties and good high thermal conductivity make silicon nitride ceramics promising to make up for the deficiencies of existing substrate materials such as alumina and aluminum nitride. , it has great market prospects in the application of high-end semiconductor devices, especially high-power semiconductor devices.
- the thickness requirements of silicon nitride ceramic substrates for commercial applications are concentrated at about 0.2 to 0.8 mm. For such thin samples, it is very difficult to form. Therefore, the molding of substrates is the core technology to realize its mass production and subsequent application.
- the forming methods of ceramic substrates mainly include tape casting, dry pressing, and rolling. Among them, the dry-pressed substrates often have problems such as difficulty in directly preparing ceramic substrates with a thickness of less than 0.5 mm, inability to accurately control the thickness, and uneven thickness due to the non-uniformity of powder flow and the technological characteristics of mechanical pressure. Therefore, subsequent machining is required.
- the rolling film forming process is complex, and it is necessary to repeatedly roll the film to eliminate the uneven thickness caused by the limitations of the process itself and the lumps caused by the agglomeration of the raw materials, resulting in the prepared substrates prone to blistering and surface unevenness.
- Only mechanical processing can meet the requirements of the subsequent copper cladding process.
- the tape casting process has high production efficiency, low cost, can be fully automated, and is convenient for continuous batch production. It is the most promising and potential process technology for ceramic substrate molding, but there are also prepared tape casting.
- the film is prone to blistering, cracking, deformation, uneven thickness, etc., resulting in problems such as low yield, low flatness, uneven thickness, and the need for subsequent machining.
- the ceramic substrate has the characteristics of high flatness, uniform thickness and smooth surface, which are the technological requirements for its subsequent copper cladding.
- the present invention provides a method for preparing a high thermal conductivity, clean size silicon nitride ceramic substrate, comprising:
- ( 2 ) tape casting and drying are carried out in a nitrogen atmosphere to obtain a first green body; the drying is to use a flowing heat N atmosphere with increasing temperature for drying;
- the crucible used for the gas pressure sintering is a high-purity BN crucible Or a graphite crucible with a high-purity BN isolation layer attached to the surface.
- the problem of the ease of casting substrates is solved. Blistering, cracking, deformation, uneven thickness and other problems, realize the net size forming of high thermal conductivity silicon nitride ceramic substrate.
- the purpose of reducing or eliminating air bubbles in the slurry and reducing the agglomeration in the slurry is achieved by fully ball-milling and mixing under a protective atmosphere during the preparation of the casting slurry, combined with low-vacuum and long-term degassing treatment.
- the preparation of high-quality, defect-free cast films and their uniform thickness are achieved by the precise control of the cylindrical doctor blade and its height during the casting process, and the continuous hot N2 atmosphere with increasing temperature to dry the cast film blanks. precise control of sex.
- the secondary oxidation of the silicon nitride powder raw material is suppressed by measures such as ball-milling mixing and N 2 protective atmosphere in the process of tape casting, so as to ensure that the prepared silicon nitride ceramic substrate has the characteristics of high thermal conductivity.
- the density, thickness uniformity and flatness of the prepared cast film are further improved.
- the micro-positive pressure debonding process is adopted, and by precisely controlling the escape rate of the gas generated by the decomposition of organic matter during the debonding process, the cracking, surface peeling and bubble generation during the debonding process of the green body are prevented, and the surface of the green body on the substrate is avoided. defect.
- high nitrogen pressure sintering in the sintering process the deformation of the substrate blank during the sintering process is controlled, the decomposition of silicon nitride is suppressed, and the surface roughness of the silicon nitride substrate is precisely adjusted.
- the sintering aids are rare earth oxides and alkaline earth metal oxides, and the amount added is the total mass of silicon nitride powder, silicon nitride formed by nitriding silicon powder, and sintering aids of 4.0 to 5.0 wt%.
- the rare earth oxide contains Y 2 O 3 and the alkaline earth metal oxide contains MgO.
- the dispersing agent is selected from at least one of polyethylene glycol (PEG) and triethyl phosphate (TEP), and the amount added is silicon nitride powder, silicon powder completely nitrided.
- the defoaming agent may be oleic acid, and the amount added is 0.2-1.0 wt% of the total mass of silicon nitride powder, silicon nitride formed by complete nitridation of silicon powder, and sintering aids .
- the binder may be polyvinyl butyral (PVB), and the amount added is the total of silicon nitride powder, silicon nitride formed by complete nitridation of silicon powder, and sintering aids. 5-9wt% of the mass.
- the plasticizer is selected from at least one of diethyl phthalate (DEP), dibutyl phthalate (DBP) and polyethylene glycol (PEG).
- DEP diethyl phthalate
- DBP dibutyl phthalate
- PEG polyethylene glycol
- the amount added is 2-6 wt% of the total mass of silicon nitride powder, silicon nitride formed by complete nitridation of silicon powder and sintering aid.
- the protective atmosphere is a nitrogen atmosphere or an inert atmosphere, and the pressure of the protective atmosphere is 0.1 MPa.
- the mixing method is ball milling mixing, the rotation speed of the ball milling mixing is 30-100 rpm, and the total time is 6-24 hours; the vacuum degree of the vacuum degassing is -0.1 ⁇ -10kPa, the time is 6 ⁇ 24 hours.
- at least one of silicon nitride powder and silicon powder, sintering aid, dispersant and defoaming agent are ball-milled and mixed for 3 to 12 hours, and then the binder and The plasticizer is continuously ball-milled and mixed for 3 to 12 hours to obtain the mixed slurry.
- the pressure of the nitrogen atmosphere is 0.1-0.2 MPa.
- the pressure is 0.1-0.2MPa
- the temperature is 40-85°C
- the total drying time is 15-60 minutes; preferably , the drying is carried out in at least two stages, and the nitrogen temperature in the latter stage is greater than the nitrogen temperature in the previous stage; more preferably, the number of stages is 3, including: the temperature of the first stage is 40-60 ° C, the drying time 5 to 20 minutes, the temperature range of the second stage is 55 to 70 ° C, the drying time is 5 to 20 minutes, the temperature range of the third stage is 65 to 85 ° C, and the drying time is 5 to 20 minutes, and the first stage The temperature of ⁇ the temperature of the second stage ⁇ the temperature of the third stage.
- the shaping pretreatment is to treat the first green body by cold isostatic pressing; the pressure of the cold isostatic pressing is 40-200 MPa, and the time is 2-10 minutes.
- the atmospheric pressure of the slightly positive nitrogen atmosphere is 0.1-0.2 MPa; the debonding time is 1-3 hours.
- the quality of the silicon powder is not less than 75% of the mass of the original powder, wherein the quality of the original powder is the nitrogen generated after the silicon nitride powder and the silicon powder are completely nitrided.
- the pressure of the nitrogen atmosphere in the gas pressure sintering is 0.5-10 MPa; the holding time of the gas pressure sintering is 4-12 hours.
- the crucible used for the gas pressure sintering is a high-purity BN crucible or a graphite crucible with a high-purity BN isolation layer attached to the surface.
- the purity of the high-purity BN crucible is greater than 99%.
- the purity of the high-purity BN isolation layer is >99%.
- the present invention provides a high thermal conductivity, net size silicon nitride ceramic substrate prepared according to the above preparation method, wherein the high thermal conductivity, net size silicon nitride ceramic substrate has a thickness of 0.2-1.0 mm and a uniform thickness.
- the property is ⁇ 0.04mm, the flatness is 0-0.002mm/mm, and the surface roughness is 0.3-0.8 ⁇ m; the thermal conductivity of the silicon nitride ceramic substrate is greater than 80W ⁇ m -1 ⁇ K -1 .
- the flatness, thickness uniformity and surface roughness of the substrate are respectively controlled in the range of 0.002mm/mm, ⁇ 0.04mm and 0.3-0.8 ⁇ m, it can be directly used in the subsequent copper cladding process without machining.
- the size of the silicon nitride ceramic substrate is at least 90 mm ⁇ 90 mm, preferably (114-140) mm ⁇ (114-190) mm.
- the distinctive feature of the invention is that the prepared silicon nitride ceramic substrate can realize precise control of sintering size and surface quality, can be used directly without subsequent processing, and has the characteristics of simple preparation process, economical and practicality.
- Another notable feature of the present invention is that high thermal conductivity of the silicon nitride ceramic substrate is achieved by controlling oxidation and impurity introduction during the preparation process.
- FIG. 1 is the silicon nitride ceramic substrate prepared in Example 1.
- FIG. 2 is the microstructure of the silicon nitride ceramic substrate prepared in Example 1.
- FIG. 3 is a silicon nitride ceramic substrate prepared in Comparative Example 3.
- FIG. 3 is a silicon nitride ceramic substrate prepared in Comparative Example 3.
- FIG. 4 is a silicon nitride ceramic substrate prepared in Comparative Example 5.
- Table 1 in FIG. 5 is the process parameters of the silicon nitride ceramic substrate prepared by the present invention.
- Table 2 in FIG. 6 is the performance parameters of the silicon nitride ceramic substrate prepared by the present invention.
- the silicon nitride ceramic base is solved.
- the problems of easy blistering, cracking, deformation, and uneven thickness of the sheet are realized, and the preparation of silicon nitride ceramic substrates with uniform thickness, no surface pores and stains, no subsequent machining, and can be directly used in the subsequent copper cladding process .
- the following exemplifies the preparation method of the high thermal conductivity, neat size silicon nitride ceramic substrate.
- Preparation of agglomeration-free, bubble-free slurries At least one of silicon nitride powder and silicon powder, sintering aids, dispersants, defoaming agents, binders and plasticizers are ball-milled and mixed in a protective atmosphere (such as N2 atmosphere, the pressure can be 0.1MPa) After the material is degassed, vacuum degassing is carried out to prepare a mixed slurry without agglomeration and bubbles. In the ball milling process, silicon nitride ceramic grinding balls are used.
- the sintering aids can be rare earth oxides and alkaline earth metal oxides.
- the rare earth oxide contains at least Y 2 O 3
- the alkaline earth metal oxide contains at least MgO.
- the molar ratio between the rare earth oxide and the alkaline earth metal oxide may be (1.0-1.4):(2.5-2.9).
- the content of the silicon powder may be 75-100 wt%.
- the prepared slurry is vacuumed to remove air bubbles, the vacuum degree can be -0.1 ⁇ -10kPa, and the degassing time can be 6 ⁇ 24h.
- Preparation of cast film blanks with uniform thickness and no bubbles on the surface Cast molding under N2 atmosphere (0.1-0.2MPa). Drying is carried out in a flowing hot N 2 atmosphere (the flow rate can be 10-1000 liters/min) to achieve the preparation of a cast film green body with uniform thickness and no bubbles on the surface.
- a cylindrical doctor blade is used for tape casting under N 2 atmosphere, and the thickness of the cast film green body can be adjusted by controlling the height of the doctor blade.
- the casting film green body is dried by using a flowing hot N2 atmosphere with increasing temperature, the temperature range of the hot N2 atmosphere can be 40-85 DEG C, and the atmosphere pressure can be 0.1-0.2MPa.
- the number of passing temperature stages is 2, including: the temperature of the first stage can be 40-65°C, the drying time is 15-30 minutes, the temperature range of the second stage can be 60-85°C, and the drying time is 15- 30 minutes, and the temperature of the first stage ⁇ the temperature of the second stage.
- the number of passing temperature stages is 3, including: the temperature of the first stage can be 40-60°C, the drying time can be 5-20 minutes, the temperature range of the second stage can be 55-70°C, and the drying time can be 5-20 minutes, the temperature range of the third stage can be 65-85°C, the drying time can be 5-20 minutes, and the temperature of the first stage ⁇ the temperature of the second stage ⁇ the temperature of the third stage.
- Shaping pretreatment of cast film green body Under a certain pressure (40-200MPa), cold isostatic pressing pretreatment is performed on the cut cast film blank (substrate blank) to ensure the thickness uniformity and flatness of the cast film.
- the time of shaping pretreatment may be 2-10 minutes.
- the substrate blank is heat-treated.
- a slight positive pressure is generated by passing in an N 2 atmosphere
- the atmospheric pressure may be 0.1-0.2 MPa
- the processing temperature is 500-900° C.
- the processing time is 1-3 h.
- the mass of the silicon powder is not less than 75% of the original powder mass, wherein the original powder mass is the mass of silicon nitride generated after the silicon nitride powder and the silicon powder are completely nitrided sum.
- the substrate blank is nitrided in a hydrogen/nitrogen mixed atmosphere with a hydrogen content not higher than 5 vol% and a certain temperature.
- the atmosphere pressure may be 0.1-0.2 MPa
- the nitriding temperature may be 1350-1450° C.
- the nitriding time may be 3-6 hours.
- Gas pressure sintering was carried out under high pressure N2 atmosphere.
- the sintering of the substrate green body is carried out by placing it in a BN crucible and performing gas pressure sintering under the condition of high-pressure N 2 atmosphere, wherein the N 2 atmosphere pressure is preferably 0.5-10 MPa, which is more conducive to improving the mechanical properties of the material within this range.
- the N 2 atmosphere pressure is preferably 0.5-10 MPa, which is more conducive to improving the mechanical properties of the material within this range.
- Thermal / electrical properties reduce the roughness of the substrate surface.
- the sintering temperature can be 1800-2000°C, and the holding time can be 4-12 hours.
- the preparation process of the high thermal conductivity, clean size silicon nitride ceramic substrate in the present invention is all carried out in a nitrogen atmosphere.
- the thickness uniformity of the silicon nitride ceramic substrate obtained by using a micrometer test is ⁇ 0.04mm.
- the flatness of the silicon nitride ceramic substrate obtained by testing with a profilometer can range from 0 to 0.002 mm/mm.
- the surface roughness of the silicon nitride ceramic substrate obtained by testing with a profiler can be 0.3-0.8 ⁇ m.
- the thermal conductivity of the silicon nitride ceramic substrate obtained by testing the silicon nitride ceramic substrate obtained by using a laser thermal conductivity meter is greater than 80W ⁇ m -1 ⁇ K -1 .
- defoamer oleic acid, 0.5g
- dispersant PEG, 0.5g
- the prepared slurry was vacuumed to remove air bubbles for 12 hours, and the vacuum degree was -0.5kPa.
- a cylindrical scraper was used to cast the above-mentioned slurry after debubbling, and the thickness of the cast film green body was precisely controlled at 0.4 ⁇ 0.04mm by controlling the height of the scraper.
- the casting film green body was dried using a flowing hot N2 atmosphere with increasing temperature (flow rate of 100 L/min), the pressure of the N2 atmosphere was 0.1MPa, and the temperature of the hot N2 atmosphere with increasing temperature was 45 °C (8 min. ), 65°C (8 minutes) and 80°C (8 minutes) are composed of three stages: front, middle and back.
- the green substrate was debonded at 700 °C for 2 h under a N2 atmosphere of 0.15 MPa.
- the debonded substrate blanks were loaded into a high-purity BN crucible (purity > 99%) and then placed in a gas pressure sintering furnace. After sintering at 1900°C for 10h under a 5MPa N2 atmosphere, the furnace was cooled to room temperature.
- the silicon nitride ceramic substrate prepared in Example 1 is shown in Fig. 1, the size is 114.4mm ⁇ 114.4mm, the size deviation is ⁇ 0.1mm, the thickness is 0.32 ⁇ 0.02mm, the flatness is 0.2mm, and the surface roughness is 0.4 ⁇ m.
- the thermal conductivity of the material is 95W/(m ⁇ K) and the bending strength is 780MPa.
- the substrate does not require subsequent mechanical processing, and can be directly used for the subsequent copper cladding process.
- the microstructure of its section is shown in Figure 2, and the microstructure is uniform and dense.
- Example 1 The raw material ratio, composition, and technological process refer to Example 1. Specific parameters such as slurry preparation, vacuum degassing, tape casting, green body shaping, debonding and sintering processes are shown in Table 1 in Figure 5. The prepared substrate The material properties are shown in Table 2 in Figure 6.
- dispersant PEG, 0.3g
- grinding ball silicon nitride ball, 120g
- organic solvent absolute ethanol, 50g
- the casting film green body was dried using a flowing hot N2 atmosphere with increasing temperature (flow rate of 50 L/min), the pressure of the N2 atmosphere was 0.2 MPa, and the temperature of the hot N2 atmosphere with increasing temperature was 45 °C (6 min. ), 65°C (6 minutes) and 80°C (6 minutes) are composed of front, middle and back sections.
- Example 6 The raw material ratio, composition, and technological process refer to Example 6. Specific parameters such as slurry preparation, vacuum degassing, tape casting, green body shaping, debonding, nitriding treatment and sintering process are shown in Table 1. The sheet material properties are shown in Table 2.
- Example 10 The preparation process of the silicon nitride ceramic substrate in Example 10 refers to Example 1, the difference is that: an automatic slicer is used to cut into square pieces of 200mm ⁇ 200mm, and cold isostatic pressing is performed at 100MPa for shaping.
- Example 11 The preparation process of the silicon nitride ceramic substrate in Example 11 refers to Example 6, the difference is that: an automatic slicer is used to cut into square pieces of 200mm ⁇ 200mm, and cold isostatic pressing is performed at 100MPa for shaping.
- the specific parameters of raw material ratio and composition, slurry preparation, vacuum degassing, tape casting, debonding and sintering process are as shown in Table 1, and the process process refers to Example 1, the difference is that no china shaping pretreatment is performed.
- the properties of the prepared substrate materials are shown in Table 2. Because the tape-casting substrate blank is not subjected to isostatic pressing pretreatment, the thickness uniformity and flatness of the prepared substrate are obviously reduced, and the thermal conductivity is also slightly reduced.
- the specific parameters such as raw material ratio and composition, slurry preparation, vacuum degassing, tape casting, green body shaping, debonding and sintering process are as shown in Table 1.
- the technological process refers to Example 1, except that high nitrogen gas is not used.
- High temperature sintering was carried out under pressure, and only 0.1MPa N2 protective atmosphere was used.
- the properties of the prepared substrate materials are shown in Table 2. Because the gas pressure sintering in a high nitrogen atmosphere is not used, the surface roughness of the prepared substrate is obviously increased, which cannot meet the requirements of the subsequent copper cladding process for the surface roughness of the substrate.
- the specific parameters such as raw material ratio and composition, slurry preparation, vacuum degassing, tape casting, green body shaping, debonding and sintering process are as shown in Table 1, and the technological process refers to Example 1, the difference is: no micro-positive Pressure debonding (debonding using vacuum conditions).
- the properties of the prepared substrate materials are shown in Table 2. Due to the use of vacuum debonding, the escape rate of the gas generated by the decomposition of the organic matter during the debonding process is uncontrollable (too fast), and microcrack defects exist locally on the surface of the prepared substrate (see Figure 3).
- the specific parameters such as raw material ratio and composition, slurry preparation, tape casting, green body shaping, debonding and sintering process are shown in Table 1, and the process refers to Example 1, except that vacuum degassing measures are not taken.
- the properties of the prepared substrate materials are shown in Table 2. Because the vacuum degassing measure is not adopted, there are a small amount of air bubbles in the slurry, and there are small air bubble defects on the surface of the prepared substrate.
- the specific parameters such as raw material ratio and composition, slurry preparation, vacuum degassing, tape casting, green body shaping, debonding and sintering process are as shown in Table 1.
- the technological process refers to Example 1, the difference is that high purity is not used.
- the BN crucible is used as a container for high-temperature sintering of silicon nitride substrate blanks, but is directly placed in the graphite crucible.
- the properties of the prepared substrate materials are shown in Table 2. Because the high-purity BN crucible is not used, the graphite crucible is easy to contaminate the substrate, the surface uniformity of the prepared substrate is poor, and there are local color spot defects (see Figure 4).
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Abstract
Description
Claims (15)
- 一种高热导、净尺寸氮化硅陶瓷基片的制备方法,其特征在于,包括:(1)将选自氮化硅粉和硅粉中至少一种的原始粉体、烧结助剂、分散剂、消泡剂、粘结剂和增塑剂在保护气氛中混合后,再经真空脱气,得到混合浆料;所述真空脱气的真空度为-0.1~-10kPa,时间为6~24小时;(2)在氮气气氛中进行流延成型和干燥,得到第一素坯;所述干燥为采用温度递增的流动热N 2气氛进行干燥;(3)将所得第一素坯进行整形预处理,得到第二素坯,所述整形预处理为采用冷等静压的方式处理第一素坯;(4)将所得第二素坯在微正压的氮气气氛中、500~900℃下进行脱粘,得到第三素坯,所述微正压的氮气气氛的气氛压力为0.12~0.2MPa;所述脱粘的时间为1~3小时;(5)将所得第三素坯置于氮气气氛中、1800~2000℃下进行气压烧结,得到所述高热导、净尺寸氮化硅陶瓷基片;所述气压烧结所用坩埚为高纯BN坩埚或表面附着有高纯BN隔离层的石墨坩埚。
- 根据权利要求1所述的制备方法,其特征在于,步骤(1)中,所述烧结助剂为稀土氧化物和碱土金属氧化物,加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂的总质量的4.0~5.0wt%;所述分散剂选自聚乙二醇(PEG)、磷酸三乙酯(TEP)中的至少一种,加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂总质量的0.2~1.0wt%;所述消泡剂为油酸,加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂总质量的0.2~1.0wt%;所述粘结剂为聚乙烯醇缩丁醛(PVB),加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂总质量的5~9wt%;所述增塑剂选自邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)和聚乙二醇(PEG)中的至少一种,加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂总质量的2~6wt%。
- 根据权利要求2所述的制备方法,其特征在于,所述稀土氧化物含有Y 2O 3,所述碱土金属氧化物含有MgO。
- 根据权利要求1或2所述的制备方法,其特征在于,步骤(1)中,所述保护气氛为氮气气氛或惰性气氛,保护气氛的压力为0.1MPa;所述混合的方式为球磨混合,所述球磨混合的转速为30~100转/分钟,总时间为6~24小时。
- 根据权利要求4所述的制备方法,其特征在于,先将氮化硅粉和硅粉中至少一种、烧结助剂、分散剂和消泡剂球磨混合3~12小时后,再加入粘结剂和增塑剂继续球磨混合3~12小时,得到所述混合浆料。
- 根据权利要求1所述的制备方法,其特征在于,步骤(2)中,当流延成型时,所述氮气气氛的压力为0.1~0.2MPa;当进行干燥时,所述氮气气氛为流动的氮气,压力为0.1~0.2MPa,温度为40~85℃,干燥的总时间为15~60分钟。
- 根据权利要求6所述的制备方法,其特征在于,采用至少两个阶段的方式进行干燥,且后一个阶段的氮气温度>前一个阶段的氮气温度。
- 根据权利要求7所述的制备方法,其特征在于,阶段数为3个,包括:第一阶段的温度为40~60℃、干燥时间为5~20分钟,第二阶段的温度范围为55~70℃、干燥时间为5~20分钟,第三阶段的温度范围为65~85℃、干燥时间为5~20分钟,且第一阶段的温度<第二阶段的温度<第三阶段的温度。
- 根据权利要求1所述的制备方法,其特征在于,步骤(3)中,所述冷等静压的压力为40~200MPa,时间为2~10分钟。
- 根据权利要求1所述的制备方法,其特征在于,当原始粉体中含有硅粉时,硅粉的质量不低于原始粉体质量的75%,其中原始粉体质量为氮化硅粉体和硅粉完全氮化之后所生成氮化硅的质量总和。
- 根据权利要求10所述的制备方法,其特征在于,在气压烧结之前,将第三素坯进行氮化处理,所述氮化处理的参数包括:氮气气氛为氢气含量不高于5vol%的氢气/氮气混合气氛,气体的压力为0.1~0.2MPa,氮化处理温度为1350~1450℃,氮化处理时间为3~6小时。
- 根据权利要求1所述的制备方法,其特征在于,步骤(5)中,所述气压烧结中氮气气氛的压力为0.5~10MPa;所述气压烧结的保温时间为4~12小时。
- 一种根据权利要求1-12中任一项所述的制备方法制备的高热导、净尺寸氮化硅陶瓷基片,其特征在于,所述高热导、净尺寸氮化硅陶瓷基片厚度为0.2~1.0mm,厚度均匀性为±0.04mm,平面度为0~0.002mm/mm,表面粗糙度为0.3~0.8μm;所述氮化硅陶瓷基片的热导率大于80W·m -1·K -1。
- 根据权利要求13所述的高热导、净尺寸氮化硅陶瓷基片,其特征在于,所述氮化硅陶瓷基片的尺寸至少为90mm×90mm。
- 根据权利要求14所述的高热导、净尺寸氮化硅陶瓷基片,其特征在于,所述氮化硅陶瓷基片的尺寸至少为(114~140)mm×(114~190)mm。
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CN116608647A (zh) * | 2023-05-24 | 2023-08-18 | 江苏富乐华功率半导体研究院有限公司 | 一种氮化硅生坯的干燥方法 |
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CN115028461A (zh) * | 2022-05-31 | 2022-09-09 | 浙江多面体新材料有限公司 | 一种硅粉流延成型制备高导热氮化硅陶瓷基片的方法 |
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