CN113233903A - 一种氮化硅陶瓷基板及其制备方法 - Google Patents
一种氮化硅陶瓷基板及其制备方法 Download PDFInfo
- Publication number
- CN113233903A CN113233903A CN202110053149.6A CN202110053149A CN113233903A CN 113233903 A CN113233903 A CN 113233903A CN 202110053149 A CN202110053149 A CN 202110053149A CN 113233903 A CN113233903 A CN 113233903A
- Authority
- CN
- China
- Prior art keywords
- silicon nitride
- ceramic substrate
- nitride ceramic
- ball milling
- weight ratio
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 66
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000000758 substrate Substances 0.000 title claims abstract description 49
- 239000000919 ceramic Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 239000004615 ingredient Substances 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000000748 compression moulding Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 abstract description 6
- 238000005452 bending Methods 0.000 abstract description 5
- 238000010292 electrical insulation Methods 0.000 abstract description 5
- 241001391944 Commicarpus scandens Species 0.000 abstract description 3
- 230000017525 heat dissipation Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
- C04B35/587—Fine ceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3229—Cerium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/3865—Aluminium nitrides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/95—Products characterised by their size, e.g. microceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
本发明公开了一种氮化硅陶瓷基板及其制备方法，包括步骤：S1、在氮化硅底料中按照第一预设重量的比例加入配料及助烧剂形成混合底料；S2、按照第二预设重量的比例加溶剂并同时进行球磨混合；S3、将球磨后的材料在模具中进行压制成型；S4、将压制成型后的材料进行烧结得到氮化硅陶瓷基板。具有热导率高，与单晶Si相近的热膨胀系数、电绝缘及机械性能良好。较突出特点是氮化硅基板的厚度可以做到0.28‑0.34mm，并且弯曲强度较高，机械性能好，不易折断变形，基板尺寸边长32‑200mm。
Description
技术领域
本发明涉及新材料技术领域，尤其涉及一种氮化硅陶瓷基板及其制备方法。
背景技术
随着电子信息技术的飞速发展，散热问题严重制约了电子器件向高密度、多 功能、高速化和大功率的发展。Si3N4陶瓷因具有与A1N相近的理论热导率、与 单晶Si相近的热胀系数、电绝缘以及机械性能良好、无毒等特点，被认为是一 种很有潜力的高速电路和大功率器件的散热和封装材料。
现有的陶瓷存在着强度较低，散热性能也较差的问题；物理、化学性能，其 他的比如高韧性、低膨胀系数、耐热冲击性、良好的绝缘性、耐磨损和耐腐蚀等 均有待提高；且制造过程中的环境污染问题亟待解决。
发明内容
本发明旨在提出一种氮化硅陶瓷基板及其制备方法，用于解决现有技术中强 度较低，散热性能也较差；物理、化学性能，其他的比如高韧性、低膨胀系数、 耐热冲击性、良好的绝缘性、耐磨损和耐腐蚀等均有待提高；且制造过程中存在 环境污的问题。
本发明提出了一种氮化硅陶瓷基板的制备方法，包括步骤：S1、在氮化硅底 料中按照第一预设重量的比例加入配料及助烧剂形成混合底料；S2、按照第二预 设重量的比例加溶剂并同时进行球磨混合；S3、将球磨后的材料在模具中进行压 制成型；S4、将压制成型后的材料进行烧结得到氮化硅陶瓷基板。
于本发明的一实施例中，所述氮化硅底料为α-Si3N4和β-Si3N4中的至少 一种；所述氮化硅底料的纯度≥92，D50的范围为0.32-0.45μm。
于本发明的一实施例中，所述配料为AlN；所述AlN的纯度大于98％，比表 面积为0.85-0.92m2，O含量＜0.8％。
于本发明的一实施例中，所述第二预设重量配比为：底料100份；配料1-10 份；助烧剂0-1份。
于本发明的一实施例中，所述助烧剂包括按照第三预设重量配比进行混合的Y2O3、CeO2和La2O3；所述第三预设重量配比为：Y2O3 1份；CeO2 0.5-1份；La2O3 0.5-1 份。
于本发明的一实施例中，所述第一预设重量配比为：混合底料1份；球磨介 质0.5-1.5份；溶剂1.5-3份；所述溶剂为无水乙醇；所述球磨介质为氮化硅球； 球磨转速为340-350r/min；球磨时间为2-4H。
于本发明的一实施例中，压制成型的加载压力为75-150Mpa，模具为金属模 具，模具尺寸为50-200mm边长的正方形模具，保压时间为2-3min；烧结温度为 1800-2000℃，烧结压力40-70MPa，保温时间为30-45min。
于本发明的一实施例中，所述步骤S2和S3之间还包括步骤：将球磨后的混 合溶液过100目筛后放入恒温干燥箱中干燥，干燥至水分率在1.5-2％之间后进 入步骤S3。
于本发明的一实施例中，所述步骤S4后还包括步骤：将烧制好的氮化硅陶 瓷基板加工切割制样，加工成品的边长尺寸为32-200mm，厚度0.28-6mm。
本发明还提供了一种氮化硅陶瓷基板，采用上述的氮化硅陶瓷基板的制备方 法制备而成。
本发明的氮化硅陶瓷基板及其制备方法，具有以下优点：
具有热导率高，与单晶Si相近的热膨胀系数、电绝缘及机械性能良好。较 突出特点是氮化硅基板的厚度可以做到0.28-0.34mm，并且弯曲强度较高，机械 性能好，不易折断变形，基板尺寸边长32-200mm。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例 仅仅是本发明一部分实施例，而不是全部的实施例。
本发明提供了一种氮化硅陶瓷基板的制备方法，包括步骤：S1、在氮化硅底 料中按照第一预设重量的比例加入配料及助烧剂形成混合底料；S2、按照第二预 设重量的比例加溶剂并同时进行球磨混合；S3、将球磨后的材料在模具中进行压 制成型；S4、将压制成型后的材料进行烧结得到氮化硅陶瓷基板。
在一实施例中，所述氮化硅底料为α-Si3N4和β-Si3N4中的至少一种；所 述氮化硅底料的纯度≥92，D50的范围为0.32-0.45μm。通常，采用其中一种 即可，也可以根据需要两种同时使用。进一步地，所述配料为AlN；所述AlN的 纯度大于98％，比表面积为0.85-0.92m2，O含量＜0.8％。
在另一实施例中，所述第二预设重量配比为：底料100份；配料1-10份； 助烧剂0-1份。优选地，采用底料100份，配料5份，助燃剂0.5份；当然，助 烧剂的种类和加入量对烧结体的致密度和热导率有强烈的影响。助烧剂的引入会 在晶界中形成低热导率的玻璃相，在保证致密的前提下，应尽量减少烧结助剂的 用量。因此，在一实施例中，所述第二预设重量配比为底料100份，配料8份， 助燃剂0份。
进一步地，所述助烧剂包括按照第三预设重量配比进行混合的Y2O3、CeO2和 La2O3；所述第三预设重量配比为：Y2O3 1份；CeO2 0.5-1份；La2O3 0.5-1份。其 中，所述第一预设重量配比为：混合底料1份；球磨介质0.5-1.5份；溶剂1.5-3 份；优选地，混合底料1份；球磨介质1份；溶剂1份；所述溶剂为无水乙醇； 所述球磨介质为氮化硅球；球磨转速为340-350r/min；球磨时间为2-4H。
进一步地，压制成型的加载压力为75-150Mpa，模具为金属模具，模具尺寸 为50-200mm边长的正方形模具，保压时间为2-3min；烧结温度为1800-2000℃， 烧结压力40-70MPa，保温时间为30-45min。
为了进一步提升加工效果，所述步骤S2和S3之间还包括步骤：将球磨后的 混合溶液过100目筛后放入恒温干燥箱中干燥，干燥至水分率在1.5-2％之间后 进入步骤S3。此外，所述步骤S4后还包括步骤：将烧制好的氮化硅陶瓷基板加 工切割制样，加工成品的边长尺寸为32-200mm，厚度0.28-6mm。在氮气保护下， 制备出热导率为80-85W·m-1·K-1，制备出的氮化硅陶瓷基板具有热导率高， 与单晶Si相近的热膨胀系数、电绝缘及机械性能良好。
具体地生产时，选用O，Al，Fe，Ca杂质含量低的Si3N4原料，利用热压烧 结方式在高温条件下加压制备出氮化硅陶瓷片；助烧剂的种类和加入量对烧结体 的致密度和热导率有强烈的影响。烧结助剂的引入会在晶界中形成低热导率的玻 璃相，在保证致密的前提下，应尽量减少烧结助剂的用量。球磨转速为 340～350r/min，球磨时间为2～4h；原料通过球磨混料，将混合溶液放入恒温干 燥箱中干燥，干燥温度为50℃。球磨后的浆料采用100目筛过筛，以获取颗粒 尺寸均匀的混合粉，同时为了防止氮化硅粉发潮或被污染，需将过筛好的煤粉封 存备用。氮化硅粉体水分率保证在1.5％～2％，使圆片表面颗粒间形成毛细管力， 从而避免毛刺的产生，减少掉粉现象的发生。预压成型压力为75-150MPa，保压 时间为2-3min；排出坯体内的孔隙，使得坯体更加致密。还包括将压片放入石 墨模具中，在高温下有氮气气保护下加压烧结，可对其起到保护作用，避免O 杂质的引入，有利于高热导率的氮化硅陶瓷基板的制备。烧结温度为 1800～2000℃，室温到600℃之前及600℃之后的升温速率分别为10℃/min和5℃ /min，高温保温30～45min，随后随炉冷却，真空度保持在1Pa以内。
将按照上述方法制备好的氮化硅陶瓷基板进行测试，得到了表1的数据：
| 序号 | 项目 | 单位 | 指标数 |
| 1 | 维氏硬度 | Kgf/mm<sup>2</sup> | 1635 |
| 2 | 密度 | g/cm<sup>3</sup> | 3.2 |
| 3 | 粗糙度 | μm | "0.4" |
| 4 | 断裂韧性 | MPa.m1/2 | 5.7-8 |
| 5 | 热导率 | W/m.k | 60～81.3 |
| 6 | 抗弯强度 | MPa | 550 |
| 7 | 热膨胀系数 | ×10-6℃ | 3.2 |
| 8 | 最高使用温度 | ℃ | 1300(空气中) |
表1：氮化硅陶瓷基板测试数据表
由此可见，通过本发明方法制备的氮化硅陶瓷基板，具有热导率高，与单晶 Si相近的热膨胀系数、电绝缘及机械性能良好。较突出特点是氮化硅基板的厚 度很薄，并且弯曲强度较高，机械性能好，不易折断变形。
本发明还提供了一种氮化硅陶瓷基板，采用上述的氮化硅陶瓷基板的制备方 法制备而成。
本发明提供的氮化硅陶瓷基板及其制备方法，具有热导率高，与单晶Si相 近的热膨胀系数、电绝缘及机械性能良好。较突出特点是氮化硅基板的厚度可以 做到0.28-0.34mm，并且弯曲强度较高，机械性能好，不易折断变形，基板尺寸 边长32-200mm。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限 于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明 的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之 内。
Claims (10)
1.一种氮化硅陶瓷基板的制备方法，其特征在于，包括步骤：
S1、在氮化硅底料中按照第一预设重量的比例加入配料及助烧剂形成混合底料；
S2、按照第二预设重量的比例加溶剂并同时进行球磨混合；
S3、将球磨后的材料在模具中进行压制成型；
S4、将压制成型后的材料进行烧结得到氮化硅陶瓷基板。
2.根据权利要求1所述的氮化硅陶瓷基板的制备方法，其特征在于，所述氮化硅底料为α-Si3N4和β-Si3N4中的至少一种；所述氮化硅底料的纯度≥92，D50的范围为0.32-0.45μm。
3.根据权利要求2所述的氮化硅陶瓷基板的制备方法，其特征在于，所述配料为AlN；所述AlN的纯度大于98％，比表面积为0.85-0.92m2，O含量＜0.8％。
4.根据权利要求3所述的氮化硅陶瓷基板的制备方法，其特征在于，所述第二预设重量配比为：底料100份；配料1-10份；助烧剂0-1份。
5.根据权利要求4所述的氮化硅陶瓷基板的制备方法，其特征在于，所述助烧剂包括按照第三预设重量配比进行混合的Y2O3、CeO2和La2O3；所述第三预设重量配比为：Y2O3 1份；CeO2 0.5-1份；La2O3 0.5-1份。
6.根据权利要求5所述的氮化硅陶瓷基板的制备方法，其特征在于，所述第一预设重量配比为：
混合底料1份；球磨介质0.5-1.5份；溶剂1.5-3份；
所述溶剂为无水乙醇；
所述球磨介质为氮化硅球；球磨转速为340-350r/min；球磨时间为2-4H。
7.根据权利要求6所述的氮化硅陶瓷基板的制备方法，其特征在于，压制成型的加载压力为75-150Mpa，模具为金属模具，模具尺寸为50-200mm边长的正方形模具，保压时间为2-3min；
烧结温度为1800-2000℃，烧结压力40-70MPa，保温时间为30-45min。
8.根据权利要求7所述的氮化硅陶瓷基板的制备方法，其特征在于，所述步骤S2和S3之间还包括步骤：
将球磨后的混合溶液过100目筛后放入恒温干燥箱中干燥，干燥至水分率在1.5-2％之间后进入步骤S3。
9.根据权利要求8所述的氮化硅陶瓷基板的制备方法，其特征在于，所述步骤S4后还包括步骤：
将烧制好的氮化硅陶瓷基板加工切割制样，加工成品的边长尺寸为32-200mm，厚度0.28-6mm。
10.一种氮化硅陶瓷基板，其特征在于，采用权利要求1至9所述的氮化硅陶瓷基板的制备方法制备而成。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110053149.6A CN113233903A (zh) | 2021-01-15 | 2021-01-15 | 一种氮化硅陶瓷基板及其制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110053149.6A CN113233903A (zh) | 2021-01-15 | 2021-01-15 | 一种氮化硅陶瓷基板及其制备方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113233903A true CN113233903A (zh) | 2021-08-10 |
Family
ID=77130034
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110053149.6A Pending CN113233903A (zh) | 2021-01-15 | 2021-01-15 | 一种氮化硅陶瓷基板及其制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113233903A (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115246741A (zh) * | 2022-08-30 | 2022-10-28 | 辽宁伊菲科技股份有限公司 | 一种传热速度快高绝缘的氮化硅陶瓷电极及制备方法 |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020084103A1 (en) * | 2000-10-27 | 2002-07-04 | Kabushiki Kaisha Toshiba | Silicon nitride ceramic substrate, silicon nitride ceramic circuit board using the substrate, and method of manufacturing the substrate |
| CN1842506A (zh) * | 2004-05-20 | 2006-10-04 | 株式会社东芝 | 具有高导热性的氮化硅烧结体及氮化硅结构部件 |
| CN105503199A (zh) * | 2015-12-30 | 2016-04-20 | 山东大学 | 一种高热导率氮化硅-氮化铝复合材料及其制备方法 |
| CN106957176A (zh) * | 2016-01-12 | 2017-07-18 | 河北高富氮化硅材料有限公司 | 一种高导热性能氮化硅陶瓷的制备方法 |
| CN111484335A (zh) * | 2020-04-22 | 2020-08-04 | 衡阳凯新特种材料科技有限公司 | 氮化硅陶瓷浆料用烧结助剂复合添加剂、氮化硅陶瓷浆料及其制备方法和应用 |
| CN112142476A (zh) * | 2020-09-28 | 2020-12-29 | 中国科学院上海硅酸盐研究所 | 一种提高氮化硅陶瓷基板材料热导率和力学性能的硅热还原方法 |
| CN112159236A (zh) * | 2020-10-19 | 2021-01-01 | 江苏贝色新材料有限公司 | 高导热氮化硅陶瓷基板及其制备方法 |
-
2021
- 2021-01-15 CN CN202110053149.6A patent/CN113233903A/zh active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020084103A1 (en) * | 2000-10-27 | 2002-07-04 | Kabushiki Kaisha Toshiba | Silicon nitride ceramic substrate, silicon nitride ceramic circuit board using the substrate, and method of manufacturing the substrate |
| CN1842506A (zh) * | 2004-05-20 | 2006-10-04 | 株式会社东芝 | 具有高导热性的氮化硅烧结体及氮化硅结构部件 |
| CN105503199A (zh) * | 2015-12-30 | 2016-04-20 | 山东大学 | 一种高热导率氮化硅-氮化铝复合材料及其制备方法 |
| CN106957176A (zh) * | 2016-01-12 | 2017-07-18 | 河北高富氮化硅材料有限公司 | 一种高导热性能氮化硅陶瓷的制备方法 |
| CN111484335A (zh) * | 2020-04-22 | 2020-08-04 | 衡阳凯新特种材料科技有限公司 | 氮化硅陶瓷浆料用烧结助剂复合添加剂、氮化硅陶瓷浆料及其制备方法和应用 |
| CN112142476A (zh) * | 2020-09-28 | 2020-12-29 | 中国科学院上海硅酸盐研究所 | 一种提高氮化硅陶瓷基板材料热导率和力学性能的硅热还原方法 |
| CN112159236A (zh) * | 2020-10-19 | 2021-01-01 | 江苏贝色新材料有限公司 | 高导热氮化硅陶瓷基板及其制备方法 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115246741A (zh) * | 2022-08-30 | 2022-10-28 | 辽宁伊菲科技股份有限公司 | 一种传热速度快高绝缘的氮化硅陶瓷电极及制备方法 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111484335A (zh) | 氮化硅陶瓷浆料用烧结助剂复合添加剂、氮化硅陶瓷浆料及其制备方法和应用 | |
| US5767028A (en) | Aluminum nitride sintered body and method for manufacturing the same | |
| CN102030538A (zh) | 氮化铝陶瓷的制备方法及采用该方法制备的氮化铝陶瓷 | |
| CN110818428B (zh) | 一种共晶增强增韧氮化硅陶瓷的制备方法 | |
| CN113943162B (zh) | 一种α-SiAlON高熵透明陶瓷材料及其制备方法 | |
| CN115028460A (zh) | 一种高导热氮化硅陶瓷基片的制备方法 | |
| CN101734920B (zh) | 一种氮化钛多孔陶瓷及其制备方法 | |
| CN113233903A (zh) | 一种氮化硅陶瓷基板及其制备方法 | |
| CN113563085B (zh) | 一种高介电性能的AlN电子陶瓷材料 | |
| KR101567311B1 (ko) | 세라믹 소재 및 그의 제조방법 | |
| CN107935576B (zh) | 氮化硅结合莫来石-碳化硅陶瓷复合材料及其制备方法 | |
| CN108503370A (zh) | 一种单相氮化硅陶瓷及其sps制备工艺 | |
| CN111484333A (zh) | 一种兼具高热导率和高强度的氮化铝陶瓷及其制备方法 | |
| CN115073186A (zh) | 一种氮化硅陶瓷烧结体及其制备方法 | |
| CN112239363B (zh) | 氮化硅镁粉体及其制备方法、陶瓷材料及导热基板 | |
| CN115010499A (zh) | 一种稀土氟化物与氧化钪双掺制备高性能氮化铝陶瓷基板的方法 | |
| CN108424133B (zh) | 一种堇青石/氮化铝电子封装陶瓷基片及制备方法 | |
| CN113929463A (zh) | 一种烧结法制备钛副族碳氮化物固溶体复相陶瓷材料的方法 | |
| CN113149658A (zh) | 一种氮化钛基复合陶瓷材料及其制备方法 | |
| JPH02192467A (ja) | 窒化アルミニウム―六方晶窒化ほう素系焼結体の製造方法 | |
| JP3177650B2 (ja) | 高強度アルミナ質焼結体およびその製造方法 | |
| JPH06329474A (ja) | 窒化アルミニウム焼結体およびその製造方法 | |
| CN117228952A (zh) | 高强度高硬度钆铝硅基板材料及其制备方法 | |
| JP2003201179A (ja) | 窒化アルミニウム焼結体およびその製造方法 | |
| JPH1112039A (ja) | 高放熱リッド用の窒化アルミニウム系焼結体の製造方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210810 |