CN116390839A - 生片的制造方法 - Google Patents
生片的制造方法 Download PDFInfo
- Publication number
- CN116390839A CN116390839A CN202180067605.0A CN202180067605A CN116390839A CN 116390839 A CN116390839 A CN 116390839A CN 202180067605 A CN202180067605 A CN 202180067605A CN 116390839 A CN116390839 A CN 116390839A
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- Prior art keywords
- silicon nitride
- green sheet
- slurry
- parts
- water
- Prior art date
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 35
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 144
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 143
- 239000002002 slurry Substances 0.000 claims abstract description 99
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 56
- 238000000465 moulding Methods 0.000 claims abstract description 35
- 239000011230 binding agent Substances 0.000 claims abstract description 21
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012778 molding material Substances 0.000 claims abstract description 7
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- 238000000034 method Methods 0.000 claims description 12
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- 150000001875 compounds Chemical class 0.000 description 22
- 239000000843 powder Substances 0.000 description 20
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- 239000002904 solvent Substances 0.000 description 20
- 238000005245 sintering Methods 0.000 description 18
- 239000007789 gas Substances 0.000 description 17
- 238000010304 firing Methods 0.000 description 15
- 239000000693 micelle Substances 0.000 description 12
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- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
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- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
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- LXOFYPKXCSULTL-UHFFFAOYSA-N 2,4,7,9-tetramethyldec-5-yne-4,7-diol Chemical compound CC(C)CC(C)(O)C#CC(C)(O)CC(C)C LXOFYPKXCSULTL-UHFFFAOYSA-N 0.000 description 1
- IHJUECRFYCQBMW-UHFFFAOYSA-N 2,5-dimethylhex-3-yne-2,5-diol Chemical compound CC(C)(O)C#CC(C)(C)O IHJUECRFYCQBMW-UHFFFAOYSA-N 0.000 description 1
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- WGIMXKDCVCTHGW-UHFFFAOYSA-N 2-(2-hydroxyethoxy)ethyl dodecanoate Chemical compound CCCCCCCCCCCC(=O)OCCOCCO WGIMXKDCVCTHGW-UHFFFAOYSA-N 0.000 description 1
- CEBKHWWANWSNTI-UHFFFAOYSA-N 2-methylbut-3-yn-2-ol Chemical compound CC(C)(O)C#C CEBKHWWANWSNTI-UHFFFAOYSA-N 0.000 description 1
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- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 description 1
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- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
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- 239000001257 hydrogen Substances 0.000 description 1
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- 230000001771 impaired effect Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
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- 229910052746 lanthanum Inorganic materials 0.000 description 1
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- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
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- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
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- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
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- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
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- 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
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- 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
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- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
本发明的一实施方式涉及生片的制造方法、氮化硅烧结体的制造方法或生片成型材料，其中，该生片的制造方法包括如下工序：得到氮化硅水浆料的工序，所述氮化硅水浆料至少包含氮化硅、水和粘结剂，水的配混量相对于每100质量份氮化硅为10～70质量份；减压处理工序，对前述氮化硅水浆料进行减压处理，得到生片成型用浆料；以及，片成型工序，将前述生片成型用浆料成型，得到片成型体。
Description
技术领域
本发明的一实施方式涉及生片的制造方法、氮化硅烧结体的制造方法或生片成型材料。
背景技术
在各种陶瓷烧结体中，使氮化硅粉末在高温下烧结得到的氮化硅烧结体的重量轻且从常温至高温的机械强度强、存在耐化学药品性、导热性、电绝缘性优异等特征，可用作散热基板、耐磨耗用构件、高温结构用构件等。
作为制造氮化硅烧结体的方法的一例，可以举出将被称为生片的片状成型体进行烧成的方法。可以通过利用刮刀法等，将溶剂中分散有氮化硅粉末、粘结剂等原料的氮化硅浆料成型为片状，从而制造生片。
基于现有的刮刀法制造生片时，从成型的容易性、干燥的容易性等观点出发，使用甲苯、醇等有机溶剂作为浆料的溶剂(例如专利文献1、2)。例如专利文献1中，使用浆料制造生片，所述浆料使用了相对于氮化硅与烧结助剂的混合粉末100重量份为总计70重量份的甲苯与乙醇的混合溶液。另外，专利文献2中，使用固体成分浓度60％的浆料制造生片，作为溶剂示例了乙醇。
现有技术文献
专利文献
专利文献1：日本特开2019-052072号公报
专利文献2：日本特开2020-093978号公报
发明内容
发明要解决的问题
如上所述，以往作为生片制造用的浆料的溶剂陆续使用了有机溶剂，但近年来，要求环境负荷少的制造方法。因此，本发明人等尝试了使用环境负荷小于有机溶剂的水作为浆料的溶剂来制造生片。然而，使用水作为前述溶剂的情况下，表明会有得到的生片中产生大量气泡的问题。而且，如果将产生了大量气泡的生片烧成，则在得到的烧结体的表面会产生凹陷、空隙等缺陷，例如，表明在机械特性、电特性方面有得不到良好的烧结体的问题。
本发明的一实施方式制造使用水作为浆料的溶剂来减轻环境负荷、且抑制了气泡的发生的生片。
用于解决问题的方案
本发明人等进行了深入研究，结果表明：使用水作为浆料的溶剂时，由于浆料中的氮化硅的一部分与水发生反应而产生气体，因此，生片中产生大量气泡。而且，进一步推进了研究，结果表明：如果使用水作为浆料的溶剂，则在浆料原料混合时粘结剂会形成胶束，给得到的烧结体的性状造成不良影响，因此，为了破坏该胶束，需要在减压条件下对氮化硅水浆料进行处理的减压处理工序。另一方面，还发现前述氮化硅与水的反应主要发生在前述减压处理工序中。
基于这些见解，本发明人等为了抑制前述减压处理工序中气体的产生，对能在短时间的减压处理工序中制造生片的氮化硅水浆料的组成进行了研究，结果发现：通过使用将浆料中的水的配混量限制在特定范围的氮化硅水浆料，可以有效地抑制生片的气泡，至此完成了本发明。
本发明的构成例如以下所述。
本发明的一实施方式为一种生片的制造方法，其包括如下工序：
得到氮化硅水浆料的工序，所述氮化硅水浆料至少包含氮化硅、水和粘结剂，水的配混量相对于每100质量份氮化硅为10～70质量份；
减压处理工序，对前述氮化硅水浆料进行减压处理，得到生片成型用浆料；以及，
片成型工序，将前述生片成型用浆料成型，得到片成型体。
前述氮化硅水浆料优选还包含消泡剂，前述消泡剂优选为聚醚系消泡剂，前述消泡剂的配混量优选相对于每100质量份氮化硅为0.25～5.0质量份。
前述减压处理优选以15℃以上且55℃以下进行。
另外，作为本发明的一实施方式，可以举出氮化硅烧结体的制造方法，所述制造方法包括将通过前述生片的制造方法得到的生片在1500～2000℃的条件下进行烧成的工序。
进一步，作为本发明的一实施方式，可以举出生片成型材料，所述生片成型材料是由氮化硅水浆料得到的，所述氮化硅水浆料包含氮化硅、水和粘结剂，水的配混量相对于每100质量份氮化硅为10～70质量份。
优选的是，该氮化硅水浆料包含聚醚系消泡剂，前述聚醚系消泡剂的配混量相对于每100质量份氮化硅为0.25～5.0质量份。
发明的效果
根据本发明的一实施方式，使用水作为浆料的溶剂制造生片时，可以制造抑制了气泡的生片。与使用有机溶剂作为浆料的溶剂的以往氮化硅烧结体的制造方法相比，通过使用该生片，可以在环境负荷少的制造条件下制造氮化硅烧结体，而且，可以得到具有良好物性的氮化硅烧结体。
另外，通过使用水作为浆料的溶剂，在接下来的烧成工序中，不会因残留的溶剂的挥发而引起***等危险，因此，在简化氮化硅烧结体的制造设备的方面也具有优势。
具体实施方式
《生片的制造方法》
本发明的一实施方式为一种生片的制造方法，其包括如下工序：得到氮化硅水浆料的工序，所述氮化硅水浆料至少包含氮化硅、水和粘结剂，水的配混量相对于每100质量份氮化硅为10～70质量份；减压处理工序，对前述氮化硅水浆料进行减压处理，得到生片成型用浆料；以及，片成型工序，将前述生片成型用浆料成型，得到片成型体。
＜得到氮化硅水浆料的工序＞
得到氮化硅水浆料的工序为得到如下氮化硅水浆料的工序：至少包含氮化硅、水、和粘结剂，水的配混量相对于每100质量份氮化硅为10～70质量份。
〔氮化硅〕
氮化硅水浆料包含氮化硅。作为这种包含氮化硅的氮化硅水浆料，作为其原料，优选使用氮化硅粉末。
氮化硅水浆料中配混的氮化硅粉末只要为化学式Si3N4所示的粉末状的物质就没有特别限定，可以使用公知的粉末。例如，氮化硅粉末可以为含有α-Si3N4颗粒的粉末，也可以为含有β-Si3N4颗粒的粉末，还可以含有这些两者。特别优选使用含有β-Si3N4颗粒80％以上、特别是90％以上的氮化硅粉末。
氮化硅水浆料中配混的氮化硅粉末可以为1种，也可以为2种以上。
氮化硅水浆料中配混的氮化硅粉末的比表面积优选5m2/g以上且优选20m2/g以下。
氮化硅粉末的比表面积低于5m2/g的情况下，有烧结性降低的倾向。另一方面，比表面积如果超过20m2/g，则制备后述的浆料时，容易引起与水的反应，另外，得到的浆料中容易掺入气泡，脱泡需要大量的时间，因此，结果，有得到的生片中的气泡量会增加的倾向。
前述氮化硅粉末的比表面积更优选7m2/g以上、更优选15m2/g以下。需要说明的是，本说明书中的比表面积是指，使用基于氮气吸附的BET1点法测得的BET比表面积。
〔水〕
氮化硅水浆料使用水作为溶剂。通过使用水作为氮化硅水浆料的溶剂，与使用有机溶剂的情况相比，可以减少环境负荷。
作为该水，没有特别限制，可以使用自来水等，但优选使用纯水、离子交换水等。
氮化硅水浆料中的水的配混量相对于每100质量份氮化硅为10质量份以上、优选30质量份以上且为70质量份以下、优选50质量份以下。通过将水的配混量限制为70质量份以下，可以有效地抑制气泡残留在生片中。
如前所述，通过将氮化硅水浆料中的水的配混量设为10～70质量份，可以抑制气泡残留在生片中的理由尚不清楚，但本发明人等如以下考虑。
即，认为如果将包含粘结剂的氮化硅水浆料的水的配混量限制为10～70质量份，则存在于氮化硅表面、氮化硅间的粘结剂的浓度变高，可以抑制氮化硅与水的接触机会。而且，其结果，推测可以抑制由氮化硅与水的反应而产生的氨气等气体的产生，并且还可以抑制因气体的产生而产生的气泡。
另外，推测在前述浆料中，由于粘结剂的分子分散于水中，容易形成包含气泡的胶束，需要减压处理工序将其去除，但通过限制前述水的配混量，可以抑制该胶束的产生量。通过抑制胶束的产生量，可以在更短时间内结束减压处理工序，其结果，推测可以抑制减压处理工序中的气体的产生。
〔粘结剂〕
氮化硅水浆料中配混粘结剂。通过配混粘结剂，可以容易地将由氮化硅水浆料得到的片成型体维持为期望的形状。
作为粘结剂，优选使用有机高分子，例如可以举出聚乙烯醇、聚乙烯醇缩丁醛、甲基纤维素、藻酸、聚乙二醇、羧甲基纤维素、乙基纤维素、丙烯酸类树脂。
氮化硅水浆料中配混的粘结剂可以为1种，也可以为2种以上。
氮化硅水浆料中的粘结剂的配混量相对于每100质量份氮化硅优选为1～30质量份，前述配混量可以根据成型条件等而适宜确定。
〔添加剂〕
氮化硅水浆料中，在不妨碍本发明的效果的范围内，也可以配混公知的添加剂。
氮化硅水浆料中能配混的添加剂可以分别为1种，也可以为2种以上。
[烧结助剂]
氮化硅水浆料中，优选配混烧结助剂。
作为烧结助剂，只要用于氮化硅粉末的烧结就没有特别限制，从可以抑制得到的氮化硅烧结体的导热率的降低等方面出发，特别适合使用不含氧原子的化合物。
作为前述不含氧原子的化合物，优选包含稀土元素或镁元素的碳氮化物系的化合物(以下也称为“特定的碳氮化物系的化合物”)、和包含镁元素的氮化物系的化合物(以下也称为“特定的氮化物系的化合物”)。通过使用这种选自由特定的碳氮化物系的化合物和特定的氮化物系的化合物组成的组中的1种以上的化合物作为烧结助剂，从而可以更有效地容易得到导热率高的氮化硅烧结体。认为前述特定的碳氮化物系的化合物作为吸附氮化硅水浆料中配混的氮化硅粉末中有可能包含的氧的吸气剂发挥功能，认为前述特定的氮化物系的化合物可以降低氮化硅烧结体的总氧量。作为结果，认为通过使用选自由特定的碳氮化物系的化合物和特定的氮化物系的化合物组成的组中的1种以上的化合物，从而可以得到导热率更高的氮化硅烧结体。
特定的碳氮化物系的化合物和特定的氮化物系的化合物可以分别使用1种，也可以使用2种以上。
作为前述稀土元素，优选Y(钇)、La(镧)、Sm(钐)、Ce(铈)、Yb(镱)等。
作为包含稀土元素的碳氮化物系的化合物，例如可以举出Y2Si4N6C、Yb2Si4N6C、Ce2Si4N6C，这些之中，从可以容易得到导热率高的氮化硅烧结体等方面出发，优选Y2Si4N6C、Yb2Si4N6C。
作为包含镁元素的碳氮化物系的化合物，例如可以举出MgSi4N6C。
另外，作为包含镁元素的氮化物系的化合物，例如可以举出MgSiN2。
前述特定的碳氮化物系的化合物和特定的氮化物系的化合物中，特别优选的化合物为Y2Si4N6C、MgSi4N6C、MgSiN2。
另外，烧结助剂优选与前述不含氧原子的化合物同时使用金属氧化物。通过使用金属氧化物作为烧结助剂，从而氮化硅的烧结变得容易进行，可以容易得到更致密且强度高的烧结体。
作为金属氧化物，例如可以举出氧化钇(Y2O3)、氧化镁(MgO)、氧化铈(CeO2)。这些之中，优选氧化钇。
金属氧化物可以使用1种，也可以使用2种以上。
在并用不含氧原子的化合物与金属氧化物作为烧结助剂的情况下，前述不含氧原子的化合物与金属氧化物的质量比(不含氧原子的化合物/金属氧化物)优选0.2以上、更优选0.4以上、进一步优选0.6以上且优选4以下、更优选2以下。
前述质量比如果在这种范围内，则可以容易得到致密且导热率高的氮化硅烧结体。
氮化硅水浆料中配混烧结助剂的情况下，氮化硅水浆料中的烧结助剂的配混量相对于每100质量份氮化硅，优选5质量份以上、更优选7质量份以上且优选20质量份以下、更优选10质量份以下。
[消泡剂]
氮化硅水浆料中，可以配混消泡剂。
通过配混消泡剂，容易破坏由于氮化硅与水的反应所产生的气体带来的气泡，可以更高度地抑制生片中产生气泡的情况。此外，也可以通过消泡剂破坏由于在搅拌、成型等生片制造操作时掺入外部空气所产生的气泡，因此，容易更高度地抑制生片中产生气泡的情况。
可以使用公知的消泡剂作为消泡剂，但适合使用聚醚系消泡剂。
作为聚醚系消泡剂，例如可以举出：(聚)氧乙烯、(聚)氧丙烯等聚氧化烯类；二乙二醇庚醚、聚氧乙烯油醚、聚氧丙烯丁醚、聚氧乙烯聚氧丙烯2-乙基己醚等(聚)氧化烯烷基醚类；聚氧丙烯苯醚、聚氧乙烯壬基苯醚等(聚)氧化烯(烷基)芳醚类；2,4,7,9-四甲基-5-癸炔-4,7-二醇、2,5-二甲基-3-己炔-2,5-二醇、3-甲基-1-丁炔-3-醇等乙炔醚类；二乙二醇油酸酯、二乙二醇月桂酸酯、乙二醇二硬脂酸酯等(聚)氧化烯脂肪酸酯类；聚氧乙烯山梨糖醇酐单月桂酸酯、聚氧乙烯山梨糖醇酐三油酸酯等(聚)氧化烯山梨糖醇酐脂肪酸酯类；聚氧丙烯甲醚硫酸钠、聚氧乙烯十二烷基苯酚醚硫酸钠等(聚)氧化烯烷基(芳基)醚硫酸酯盐类；(聚)氧乙烯磷酸硬脂酯等(聚)氧化烯磷酸烷基酯类；聚氧乙烯月桂胺等(聚)氧化烯烷基胺类。
氮化硅水浆料中配混消泡剂的情况下，消泡剂的配混量没有特别限定，相对于每100质量份氮化硅，优选0.25质量份以上、更优选0.5质量份以上且优选5.0质量份以下、更优选2.0质量份以下。
[有机溶剂]
氮化硅水浆料中，也可以并用水以外的有机溶剂、例如醇等作为溶剂，但从环境负荷的观点出发，有机溶剂的配混量优选尽量少，优选为前述溶剂的配混量的50％以下、更优选为20％以下、进一步优选为1％以下。
〔氮化硅水浆料的制造方法〕
氮化硅水浆料的制造方法没有特别限定，例如可以以规定的配混量量取各成分，以氮化硅粉末分散于溶剂的方式进行搅拌混合。作为进行搅拌混合的分散装置，例如可以举出超声波分散装置、珠磨机、辊磨机、均质混合器、Ultra Mixer、分散混合器、贯通型高压分散装置、碰撞型高压分散装置、多孔型高压分散装置、捣碎型高压分散装置、(碰撞+贯通)型高压分散装置、超高压均化器。另外，搅拌混合后，根据需要，可以进行过滤器过滤等操作，将浆料中的粗大颗粒去除的工序等。
＜减压处理工序＞
减压处理工序中，对前述氮化硅水浆料进行减压处理，得到生片成型用浆料。
减压处理工序通过在低于大气压的减压条件下(例如-0.20MPa·G以上、例如-0.08MPa·G以下)使氮化硅水浆料存在而进行。
通过减压处理工序，可以将胶束化后的粘结剂的胶束破坏，可以抑制烧成生片而得到的烧结体的表面处的缺陷的发生。而且，如前所述，通过使氮化硅水浆料中配混的水的配混量为10～70质量份，从而氮化硅与水的接触机会变少，且浆料中的胶束的发生量变少，因此推测：可以在短时间内结束减压处理工序，可以抑制成为生片的气泡原因的氮化硅与水的反应所导致的气体的产生。
减压处理工序的压力优选-0.15MPa·G以上、优选-0.09MPa·G以下。
如果压力过低，则有会由于突然沸腾等而产生新气泡的担心。如果压力过高，则有在短时间内难以充分破坏胶束的倾向。
减压处理工序的温度只要是氮化硅水浆料确保流动性就没有特别限制，优选15℃以上、更优选20℃以上、进一步优选25℃以上且优选55℃以下、更优选45℃以下。
减压处理工序的温度越低，胶束的破坏效率越变差，因此，必须长时间进行减压处理工序，但氮化硅与水的反应性也变低，可以减少每单位时间的气体产生量。另一方面，减压处理工序的温度越高，氮化硅与水的反应性越变高，每单位时间的气体产生量变多，但可以缩短减压处理工序的时间。出于这些的均衡性，通过在前述温度范围内进行减压处理工序，从而变得容易有效地抑制生片中产生气泡的情况。
减压处理工序的优选时间根据减压处理的温度而不同，从充分破坏胶束、且抑制氮化硅与水的反应所导致的气体的产生的观点出发，优选1小时以上、优选5小时以下。使减压处理时的温度为25℃以上的情况下，减压处理工序的时间特别优选3小时以下。
减压处理工序中，根据条件而去除作为溶剂的水，减压处理工序后的浆料(生片成型用浆料)的粘度有时不同于氮化硅水浆料。该情况下，通过减压处理工序，可以破坏前述胶束，且将生片成型用浆料的粘度调整为适于成型者。
从成型性的观点出发，生片成型用浆料的23℃下的粘度优选1000mPa·s以上、更优选3000mPa·s以上且优选10000mPa·s以下、更优选7000mPa·s以下。
需要说明的是，该粘度是由旋转粘度计测得的值。
从成型性和容易进行后述的干燥工序的观点出发，生片成型用浆料的固体成分浓度优选65～75％。
《生片成型材料》
本发明的一实施方式的生片成型材料只要是由前述氮化硅水浆料得到的材料就没有特别限制。
该生片成型材料的适合的具体例为前述氮化硅水浆料、或为前述生片成型用浆料。
＜片成型工序＞
将生片成型用浆料成型得到片成型体的片成型工序没有特别限定，可以使用公知的成型方法，但从得到的片成型体的厚度的均匀性良好等的观点出发，优选通过刮刀法进行成型。
可以将如前述成型而成的片成型体作为生片，但优选经过使如前述成型而成的片成型体干燥的干燥工序而形成生片。
前述干燥工序是从如前述成型而成的片成型体中去除水的工序，通过进行该干燥工序，从而变得容易进行后述的脱脂工序、烧成工序。
干燥工序例如可以通过将片成型体静置在30～150℃左右的温度下而进行。
干燥工序中，优选以得到的生片的含水率成为10％以下的方式使片干燥。
得到的生片根据需要可以加工成适当的大小、任意的形状等。作为这种大小、形状，例如通常加工成一边为100～2000mm、厚度为0.3～1.2mm的大致长方体的形状。
另外，优选在后述的烧成工序之前，根据需要对得到的生片进行脱脂工序。
作为脱脂工序的一例，出于从生片中去除粘结剂等有机物的目的，可以举出将片成型体加热的工序。
脱脂工序时的加热温度通常为300℃以上、优选400℃以上且通常为1200℃以下、优选1000℃以下。
另外，脱脂工序中的生片的加热时间可以根据粘结剂的种类、脱脂气氛而适宜选择，通常为30分钟以上、优选2小时以上且通常为140小时以下、优选120小时以下。
脱脂工序通常在氧气、空气等氧化性气体、氢气等还原性气体、氩气、氮气等非活性气体、二氧化碳、或它们的混合气体气氛下、或混合有这些气体与水蒸气的加湿气体气氛下进行。
《氮化硅烧结体》
本发明的一实施方式的氮化硅烧结体可以通过将通过前述生片的制造方法得到的生片进行烧成(烧成工序)而得到。
烧成条件没有特别限定，只要在得到氮化硅烧结体的公知的烧成条件下进行实施即可。
前述烧成通常在非活性气体气氛下进行。非活性气体气氛下例如是指，氮气气氛下、或氩气气氛下等。
前述烧成优选在控制了压力的气氛下进行。
作为此时的压力，没有特别限定，低压下，烧成时氮化硅有时发生分解，高压下，耗费设备等成本，因此，例如为0MPa·G以上、例如10MPa·G以下、优选3MPa·G以下、进一步优选0.1MPa·G以下。
烧成温度只要期望的烧结反应进行就没有特别限定，通常为1200℃以上、优选1500℃以上、通常为2000℃以下、优选1800℃以下。
烧成时间只要期望的烧结反应进行就没有特别限定，通常设为3～20小时左右。
如前述制造的氮化硅烧结体是使用水作为生片的制造中使用的浆料的溶剂而得到的烧结体，生片的制造时产生的气泡所导致的表面的凹陷、内部的空隙等缺陷的发生得到抑制。而且，这种抑制了表面凹陷、空隙等缺陷的氮化硅烧结体的机械特性/电特性等物性良好。
作为氮化硅烧结体的机械强度的指标的3点弯曲强度(依据JIS R 1601而测定)优选500MPa以上、更优选550MPa以上。
抑制了表面的凹陷、内部的空隙等缺陷的氮化硅烧结体容易成为3点弯曲强度处于前述范围的烧结体，因此，作为制品的可靠性优异。
氮化硅烧结体的绝缘击穿电压优选11kV以上、更优选13kV以上。
这种绝缘击穿电压的氮化硅烧结体不易产生绝缘击穿，作为制品的可靠性优异。
氮化硅烧结体的导热率优选60W/m·K以上、更优选75W/m·K以上。
该导热率可以通过激光闪光法而测定。
氮化硅烧结体的用途没有特别限定，例如可以举出各种散热基板、功率模块基板(车载用、电气铁路用、大功率半导体用)、高频电路基板、LED用封装体、光学拾波器用底座(DVD、CD用)、发动机或气体涡轮用材料、涡轮增压器转子、柴油发动机的电热塞、热型火花塞、加热器管、低压铸造用杆、电偶保护管、废气用吹入管、耐热和/或耐冲击性构件、研磨布校正平台、高频淬火治具、车体组装和/或发动机制造用治具、加压工序用治具、绝缘部件、绝缘性医疗器具和/或手术器具、塑性加工用辊。
实施例
以下，根据实施例对本发明的一实施方式具体地进行说明，但本发明不限定于这些实施例。各试验方法如以下所述。
＜生片的气泡的评价＞
以目视观察制造条件相同且形状相同的10张生片(300mm×2000mm×0.4mm)的表面，算出每1张的凹陷的数量(凹陷的数量的平均值)，根据下述评价基准进行评价。
(评价基准)
A：每1张生片的凹陷的数量低于10个
B：每1张生片的凹陷的数量为10个以上且低于20个
C：每1张生片的凹陷的数量为20个以上且低于30个
D：每1张生片的凹陷的数量为30个以上且低于40个
E：每1张生片的凹陷的数量为40个以上
＜烧结体表面性状的评价＞
以目视观察制造条件相同且形状相同的10张烧结体(300mm×2000mm×0.4mm)的表面，算出每1张的凹陷的数量(凹陷的数量的平均值)，根据下述评价基准进行评价。
(评价基准)
A：每1张烧结体的凹陷的数量低于10个
B：每1张烧结体的凹陷的数量为10个以上且低于20个
C：每1张烧结体的凹陷的数量为20个以上且低于30个
D：每1张烧结体的凹陷的数量为30个以上且低于40个
E：每1张烧结体的凹陷的数量为40个以上
试验中使用的原料和其缩写如以下所示。
＜氮化硅粉末＞
·C1：比表面积12m2/g的β-Si3N4粉末
＜烧结助剂＞
·S1：氧化钇(比表面积20m2/g)
·S2：氮化硅镁(比表面积12m2/g)
＜粘结剂＞
·B1：丙烯酸类树脂乳剂(藤仓化成株式会社制：Acrybase EMK-02)
＜消泡剂＞
(聚醚系消泡剂)
·D1：聚氧化烯(SAN NOPCO LIMITED制：SN Defoamer 485)
＜实施例1＞
将氮化硅粉末C1 100g、烧结助剂S1 5.6g、烧结助剂S2 3.4g、粘结剂B124g、消泡剂D1 0.5g、水47g混合，搅拌48小时，得到氮化硅水浆料。将得到的氮化硅水浆料投入至容器，使容器内形成-0.1MPa·G的减压状态，在30℃下静置2.5小时，从而进行减压处理工序，得到生片成型用浆料。使得到的生片成型用浆料通过聚乙烯网(孔径229μm)去除粗大颗粒后，使用得到的浆料，以刮刀法制作300mm×2000mm×0.4mm的片成型体。使得到的片成型体载置于设定为50℃的板状加热器上，静置3小时并干燥，得到生片。对于得到的生片，进行气泡的评价后，在500℃下脱脂60小时，然后，在氮气气氛下、在1800℃、0.1MPa·G的条件下，烧成16小时，得到氮化硅烧结体。之后，对于得到的氮化硅烧结体，进行表面性状的评价。将氮化硅水浆料的组成和减压处理工序条件示于表1、得到的生片和氮化硅烧结体的评价结果示于表2。
＜实施例2～5、比较例1～3＞
如表1所示变更氮化硅水浆料的组成和减压处理工序条件，除此之外，与实施例1同样地进行评价。需要说明的是，比较例3中，对氮化硅水浆料未进行减压处理工序。
将氮化硅水浆料的组成和减压处理工序条件示于表1、得到的生片和氮化硅烧结体的评价结果示于表2。
[表1]
[表2]
前述实施例中，通过实施例1～5的制造方法得到的生片成型用浆料的固体成分浓度为65～75％、23℃中的粘度为4000～6000mPa·s。需要说明的是，粘度是由旋转粘度计测得的值。
与水的配混量多的比较例1、2相比，本发明的一实施方式的实施例1～5得到了气泡少的生片，其结果，可以得到良好的烧结体。需要说明的是，水的配混量少的比较例3无法成型为生片本身。
Claims (8)
1.一种生片的制造方法，其包括如下工序：
得到氮化硅水浆料的工序，所述氮化硅水浆料至少包含氮化硅、水和粘结剂，水的配混量相对于每100质量份氮化硅为10～70质量份；
减压处理工序，对所述氮化硅水浆料进行减压处理，得到生片成型用浆料；以及，
片成型工序，将所述生片成型用浆料成型，得到片成型体。
2.根据权利要求1所述的生片的制造方法，其中，所述氮化硅水浆料还包含消泡剂。
3.根据权利要求2所述的生片的制造方法，其中，所述消泡剂为聚醚系消泡剂。
4.根据权利要求2或3所述的生片的制造方法，其中，所述消泡剂的配混量相对于每100质量份氮化硅为0.25～5.0质量份。
5.根据权利要求1～4中任一项所述的生片的制造方法，其中，以15℃以上且55℃以下进行所述减压处理。
6.一种氮化硅烧结体的制造方法，其包括如下工序：
将通过权利要求1～5中任一项所述的生片的制造方法得到的生片以1500～2000℃进行烧成。
7.一种生片成型材料，其是由氮化硅水浆料得到的，所述氮化硅水浆料包含氮化硅、水和粘结剂，水的配混量相对于每100质量份氮化硅为10～70质量份。
8.根据权利要求7所述的生片成型材料，其中，所述氮化硅水浆料包含聚醚系消泡剂，
所述聚醚系消泡剂的配混量相对于每100质量份氮化硅为0.25～5.0质量份。
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| EP4067302A4 (en) * | 2019-11-28 | 2024-05-15 | Tokuyama Corporation | METHOD FOR MANUFACTURING A SINTERED SILICON NITRIDE TABLET |
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- 2021-09-29 EP EP21877457.8A patent/EP4227283A1/en active Pending
- 2021-09-29 CN CN202180067605.0A patent/CN116390839A/zh active Pending
- 2021-09-29 WO PCT/JP2021/035968 patent/WO2022075156A1/ja active Application Filing
- 2021-09-29 JP JP2022555403A patent/JPWO2022075156A1/ja active Pending
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