CN116283308B - 一种氮化硅陶瓷加热棒的制备方法 - Google Patents
一种氮化硅陶瓷加热棒的制备方法 Download PDFInfo
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 149
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 149
- 238000010438 heat treatment Methods 0.000 title claims abstract description 35
- 239000000919 ceramic Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 44
- 238000005266 casting Methods 0.000 claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 79
- 238000002156 mixing Methods 0.000 claims description 31
- 239000002002 slurry Substances 0.000 claims description 26
- 239000011230 binding agent Substances 0.000 claims description 21
- 239000002270 dispersing agent Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 17
- 238000005303 weighing Methods 0.000 claims description 16
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- 229920001684 low density polyethylene Polymers 0.000 claims description 15
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 14
- 238000000465 moulding Methods 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 13
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 13
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 13
- 239000005642 Oleic acid Substances 0.000 claims description 13
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 13
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 13
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 13
- 239000012188 paraffin wax Substances 0.000 claims description 13
- 239000004014 plasticizer Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000007767 bonding agent Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000004512 die casting Methods 0.000 claims description 8
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 8
- 229940090181 propyl acetate Drugs 0.000 claims description 8
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 6
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 6
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims description 3
- OWCYYNSBGXMRQN-UHFFFAOYSA-N holmium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ho+3].[Ho+3] OWCYYNSBGXMRQN-UHFFFAOYSA-N 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 3
- -1 sintering aid Substances 0.000 claims description 3
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 3
- 229940075624 ytterbium oxide Drugs 0.000 claims description 3
- 238000004814 ceramic processing Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 238000001746 injection moulding Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供一种氮化硅陶瓷加热棒的制备方法,涉及氮化硅陶瓷加工技术领域;该氮化硅陶瓷加热棒的制备方法包括以下步骤:S1、制备氮化硅层;S2、在氮化硅层上粘结电路;S3、制备内芯棒体;S4、通过热压铸工艺将步骤S2制备的氮化硅层和步骤S3制备的内芯棒体组装成型,用氮化硅层包裹内芯棒体,得到氮化硅加热棒坯体;S5、将步骤S4制备的氮化硅加热棒坯体在真空气压炉中进行压力烧结。本发明的氮化硅陶瓷加热棒的制备方法生产效率高,成品强度较高。
Description
技术领域
本发明涉及氮化硅陶瓷加工技术领域,具体的,涉及一种氮化硅陶瓷加热棒的制备方法。
背景技术
氮化硅陶瓷加热棒与传统的金属加热棒相比,具有更高的强度、更优的高温性能、更快的升温速度,以及优秀的耐腐蚀性能等。
氮化硅陶瓷加热棒通常包括芯棒,以及包裹在芯棒外侧并设有电路的料片;例如申请号为202111467856 .6的中国发明专利申请提供了一种陶瓷加热棒,包括芯棒和料片,其中,芯棒通过注塑成型或模塑成型。
与注塑成型或模塑成型相比,热压铸成型具有更高的生产效率,且能够使产物具有更高的强度;目前已广泛应用于氧化铝、氧化锆陶瓷领域,但在氮化硅陶瓷领域的应用却极为少见,这主要是因为热压铸成型时要求陶瓷粉料均匀地分散开,不能出现团聚或不均匀现象,所以一般热压铸成型时粉体的粒度多为0.9-1.1μm。而氮化硅作为一种强共价键化合物,烧结时要求粉体颗粒尽量小(多为0.4-0.6μm)才能在较低温度下烧结致密,而0.4-0.6μm的超细粉体颗粒因其比表面积较大,表面能较高,极易发生团聚现象,容易造成浆料中氮化硅粉体的不均匀分布,容易发生致密度不均匀,烧结变形或烧结缺陷的问题。另外较细颗粒的粉体在溶液中溶解时无法形成高固含量浆料,从而出现坯体致密度低、易烧结变形问题。
总之,现有的氮化硅陶瓷难以通过成本更低且加工效率更高的热压铸方式成型。
发明内容
为此,本发明提出一种氮化硅陶瓷加热棒的制备方法,以至少部分解决现有的氮化硅陶瓷难以通过成本更低且加工效率更高的热压铸方式成型的技术问题。
本发明的技术方案如下:
一种氮化硅陶瓷加热棒的制备方法,包括以下步骤:
S1、制备氮化硅层;
S2、在氮化硅层上粘结电路;
S3、制备内芯棒体,其包括以下工序:
S31、称取氮化硅粉、烧结助剂和结合剂;其中,烧结助剂为氧化镁、氧化铝及氧化钇中的至少一种;结合剂为PP、LDPE、石蜡和油酸的混合物;
S32、将PP、LDPE和石蜡进行混合;
S33、向工序S32得到的混合物内加入油酸并混合;
S34、向工序S33得到的混合物内加入烧结助剂并混合;
S35、向工序S34得到的混合物内加入氮化硅粉得到合格的氮化硅浆料;其中,氮化硅粉经过以下前处理:
将氮化硅粉在pH在2~3之间的酸性水溶液下洗涤;
将洗涤后的氮化硅粉用去离子水清洗,直至溶液呈中性;
将清洗后的氮化硅粉在高纯氮气且温度为800~1000℃的环境下烘烤;
S36、将氮化硅浆料经热压铸成型,得到内芯棒体;
S4、通过热压铸工艺将步骤S2制备的氮化硅层和步骤S3制备的内芯棒体组装成型,用氮化硅层包裹内芯棒体,得到氮化硅加热棒坯体;
S5、将步骤S4制备的氮化硅加热棒坯体在真空环境中烧结。
进一步的,步骤S1包括以下工序:
S11、称取氮化硅粉、烧结助剂、分散剂和溶剂,混合并进行球磨;
S12、向工序S11的产物中加入粘结剂和增塑剂,进行球磨,得到浆料;
S13、将工序S12所得到的浆料流延成型,得到氮化硅层。
进一步的,工序S11中,氮化硅粉满足:α相≥94%、纯度≥99.9%、粒度D50:0.5-0.6μm,D90:1.2-1.3μm;烧结助剂为氧化铝、氧化钇、氧化钬和氧化镱中的至少一种;分散剂为nk2300;溶剂由无水乙醇和乙酸丙酯混合形成。
进一步的,工序S11中,氮化硅粉、烧结助剂、分散剂和溶剂的混合物中固形物含量为48-55% ;其中,氮化硅粉、烧结助剂、分散剂的重量比为:(90-94):(6-10):(2-3),溶剂包括体积比为1:(0.8-1.5)的无水乙醇与乙酸丙酯。
进一步的,工序S12中,粘结剂的添加量为氮化硅粉重量的9-15%,且粘结剂包括重量比为1:(3-4)的PVB72与PVB98。
进一步的,工序S12中,增塑剂的添加量为氮化硅粉重量的6-10%,且增塑剂包括重量比为1:(4-5)的PEG400与OE400。
进一步的,工序S31中,烧结助剂、氮化硅粉与结合剂的重量比为(7-15):(85-93):(20-35);且氮化硅粉满足:α相≥94%,比表面积为12-15m2/g。
进一步的,所述结合剂中,PP、LDPE、石蜡与油酸的重量比为(15-20):(15-20):(50-60):(3-10)。
本发明的工作原理及有益效果为:
本发明提供的氮化硅陶瓷加热棒的制备方法,通过对氮化硅粉进行表面改性处理,降低表面能,提高了氮化硅粉的分散性和在溶液中的固含量,进而能够采用热压铸的方式制备芯棒;与注塑或模塑成型的方式制备芯棒相比;由于热压铸成型机的压射速度数倍于注塑成型机,且对物料所实施的动能更大,因而能够提高成型后坯体密度,使胚体具有更大强度,且具有更高的生产效率。
具体实施方式
下面将结合本发明实施例,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。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都涉及本发明保护的范围。
原料说明:
PP:聚丙烯;厂家:北京燕山化工;
LDPE:低密度聚乙烯;厂家:北京燕山化工;
nk2300: 分散剂(含高分子量硅烷共聚物);厂家:佛山千佑化工;
PVB72:聚乙烯醇缩丁醛B72规格;厂家:美国伊士曼;
PVB72:聚乙烯醇缩丁醛B98规格;厂家:美国伊士曼;
PEG400:聚乙三醇;厂家:美国伊士曼;
OE400:三甘醇二异辛酸酯;厂家:美国伊士曼。
本实施例提供一种氮化硅陶瓷加热棒的制备方法,包括以下步骤:
S1、制备氮化硅层;
S2、在氮化硅层上粘结电路;
S3、制备内芯棒体,其包括以下工序:
S31、称取氮化硅粉、烧结助剂和结合剂;其中,烧结助剂为氧化镁、氧化铝及氧化钇中的至少一种;结合剂为PP、LDPE、石蜡和油酸的混合物;
S32、将PP、LDPE和石蜡进行混合;
S33、向工序S32得到的混合物内加入油酸并混合;
S34、向工序S33得到的混合物内加入烧结助剂并混合;
S35、向工序S34得到的混合物内加入氮化硅粉得到合格的氮化硅浆料;其中,氮化硅粉经过以下前处理:
将氮化硅粉在pH在2~3之间的酸性水溶液下洗涤;
将洗涤后的氮化硅粉用去离子水清洗,直至溶液呈中性;
将清洗后的氮化硅粉在高纯氮气且温度为800~1000℃的环境下烘烤;
S36、将氮化硅浆料经热压铸成型,得到内芯棒体;
S4、通过热压铸工艺将步骤S2制备的氮化硅层和步骤S3制备的内芯棒体组装成型,用氮化硅层包裹内芯棒体,得到氮化硅加热棒坯体;
S5、将步骤S4制备的氮化硅加热棒坯体在真空环境中烧结。
本实施例中,通过将氮化硅粉在PH在2~3之间的酸性水溶液下洗涤,然后将洗涤后的氮化硅粉用去离子水清洗,直至溶液呈中性;能够有效的对粉体进行表现改性,调节PH,降低粉体表面的氧化程度,从而升高等电点,提高电位,改善浆料的流动性;而通过将清洗后的氮化硅粉在高纯氮气且温度在800~1000℃的环境下高温烘烤,能够降低氮化硅粉表面能,提高氮化硅粉在溶液的分散性。
通过对氮化硅粉进行上述处理,使工序S35得到的氮化硅浆料能够通过热压铸成型机成型,得到内芯棒体。通过采用热压铸成型机生产内芯棒体,能够提高内芯棒体的生产效率,并提高内芯棒体的强度。
本实施例中,在工序S31中,烧结助剂、氮化硅粉与结合剂为20-35的重量比为(7-15):(85-93):(20-35);且氮化硅粉满足:α相≥94%,比表面积为12-15m2/g。
本实施例中,所述结合剂中,PP、LDPE、石蜡与油酸的重量比为(15-20):(15-20):(50-60):(3-10)。
本实施例中,步骤S1包括以下工序:
S11、称取氮化硅粉、烧结助剂、分散剂和溶剂,混合并进行球磨;
S12、向工序S11的产物中加入粘结剂和增塑剂,进行球磨,得到浆料;
S13、将工序S12所得到的浆料在流延成型机上进行流延,得到氮化硅层。
其中,工序S11中,氮化硅粉满足:α相≥94%、纯度≥99.9%、粒度D50:0.5-0.6μm,D90:1.2-1.3μm;烧结助剂为氧化铝、氧化钇、氧化钬和氧化镱中的至少一种;分散剂为nk2300;溶剂由无水乙醇和乙酸丙酯混合形成。
工序S11中,工序S11中,氮化硅粉、烧结助剂、分散剂和溶剂的混合物中固形物含量为48-55% ;其中,氮化硅粉、烧结助剂、分散剂的重量比为:(90-94):(6-10):(2-3),溶剂包括体积比为1:(0.8-1.5)的无水乙醇与乙酸丙酯。
工序S12中,粘结剂的添加量为氮化硅粉重量的9-15%,且粘结剂包括重量比为1:(3-4)的PVB72与PVB98。
工序S12中,增塑剂的添加量为氮化硅粉重量的6-10%,且增塑剂包括重量比为1:(4-5)的PEG400与OE400。
本实施例中,通过采用上述的方式制备氮化硅层,在步骤S4中,通过热压铸将氮化硅层与内芯棒体组装成型时,能够在工序S12所添加的粘结剂的作用下,使氮化硅层与内芯棒体直接组装成型,而无需在氮化硅层和内芯棒体之间单独添加粘合剂,能够简化该氮化硅陶瓷加热棒的制备方法。
实施例一
S11、称取6份烧结助剂、94份氮化硅粉、2份分散剂;并量取1份无水乙醇和0.8份乙酸丙酯进行混合;
将上述原料混合,其中,烧结助剂、氮化硅粉和分散剂与溶剂的比例满足:混合后,固形物的含量为48%。
对混合后的原料进行第一次球磨得到浆料,球磨时长为10h;
S12、称取1份PVB72和3份PVB98混合后得到粘结剂,称取工序S11中氮化硅粉重量的9%的粘结剂投入工序S11所得到的浆料内;
称取1份PEG400和4份OE400混合后得到增塑剂,称取工序S11中氮化硅粉重量的6%的增塑剂投入工序S11所得到的浆料内;
进行第二次球磨,得到浆料。
S13、在流延成型机上进行流延,得到厚度0.3mm的氮化硅层。
S2、在由工序S13成型好的氮化硅层上粘结电路,粘结电路后的氮化硅层必须在干燥、无尘的真空环境中保存。
S32和S33、称取15份PP、20份LDPE、50份石蜡及3份油酸;先将PP、LDPE和石蜡进行混合,再加入油酸后混合得到结合剂;
S31、S34和S35、称取7份烧结助剂、93份氮化硅粉和20份混合剂;先向结合剂内加入烧结助剂并混合,再加入氮化硅粉混合。
其中氮化硅粉满足,α相为94%以上,比表面积为12m2/g;且经过以下前处理:将氮化硅粉在pH为2的酸性水溶液下洗涤;将洗涤后的氮化硅粉用去离子水清洗,直至溶液呈中性;将清洗后的氮化硅粉在高纯氮气且温度在800℃的环境下高温烘烤。
S36、将工序S35所得到得氮化硅浆料在热压铸成型机上进行成型,得到内芯棒体。
S4、通过热压铸工艺将步骤S2制备的氮化硅层和步骤S3制备的内芯棒体组装成型,用氮化硅层包裹内芯棒体,得到氮化硅加热棒坯体;其中热压铸温度为60℃。
S5、将步骤S4制备的氮化硅加热棒坯体在真空气压炉中进行压力烧结。其中烧结温度为1700℃,压力为0.5MPa,最终得到致密加热棒。
实施例二
S11、称取10份烧结助剂、90份氮化硅粉、3份分散剂;并量取1份无水乙醇和1.5份乙酸丙酯进行混合;
将上述原料混合,其中,烧结助剂、氮化硅粉和分散剂与溶剂的比例满足:混合后,固形物的含量为55%。
对混合后的原料进行第一次球磨得到浆料,球磨时长为15h;
S12、称取1份PVB72和4份PVB98混合后得到粘结剂,称取工序S11中氮化硅粉重量的15%的粘结剂投入工序S11所得到的浆料内;
称取1份PEG400和5份OE400混合后得到增塑剂,称取工序S11中氮化硅粉重量的10%的增塑剂投入工序S11所得到的浆料内;
进行第二次球磨,得到浆料。
S13、在流延成型机上进行流延,得到厚度0.5mm的氮化硅层。
S2、在由工序S13成型好的氮化硅层上粘结电路,粘结电路后的氮化硅层必须在干燥、无尘的真空环境中保存。
S32和S33、称取20份PP、15份LDPE、60份石蜡及10份油酸;先将PP、LDPE和石蜡进行混合,再加入油酸后混合得到结合剂;
S31、S34和S35、称取15份烧结助剂、85份氮化硅粉和35份混合剂;先向结合剂内加入烧结助剂并混合,再加入氮化硅粉混合。
其中氮化硅粉满足,α相为94%以上,比表面积为15m2/g;且经过以下前处理:将氮化硅粉在PH在3之间的酸性水溶液下洗涤;将洗涤后的氮化硅粉用去离子水清洗,直至溶液呈中性;将清洗后的氮化硅粉在高纯氮气且温度在1000℃的环境下高温烘烤。
S36、将工序S35所得到得氮化硅浆料在热压铸成型机上进行成型,得到内芯棒体。
S4、通过热压铸工艺将步骤S2制备的氮化硅层和步骤S3制备的内芯棒体组装成型,用氮化硅层包裹内芯棒体,得到氮化硅加热棒坯体;其中热压铸温度为60-110℃。
S5、将步骤S4制备的氮化硅加热棒坯体在真空气压炉中进行压力烧结。其中烧结温度为1900℃,压力为2MPa,最终得到致密加热棒。
以上仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (5)
1.一种氮化硅陶瓷加热棒的制备方法,其特征在于,包括以下步骤:
S1、制备氮化硅层;
S2、在氮化硅层上粘结电路;
S3、制备内芯棒体,其包括以下工序:
S31、称取氮化硅粉、烧结助剂和结合剂;其中,烧结助剂为氧化镁、氧化铝及氧化钇中的至少一种;结合剂为PP、LDPE、石蜡和油酸的混合物;
S32、将PP、LDPE和石蜡进行混合;
S33、向工序S32得到的混合物内加入油酸并混合;
S34、向工序S33得到的混合物内加入烧结助剂并混合;
S35、向工序S34得到的混合物内加入氮化硅粉得到合格的氮化硅浆料;其中,氮化硅粉经过以下前处理:
将氮化硅粉在pH在2~3之间的酸性水溶液下洗涤;
将洗涤后的氮化硅粉用去离子水清洗,直至溶液呈中性;
将清洗后的氮化硅粉在高纯氮气且温度为800~1000℃的环境下烘烤;
S36、将氮化硅浆料经热压铸成型,得到内芯棒体;
S4、通过热压铸工艺将步骤S2制备的氮化硅层和步骤S3制备的内芯棒体组装成型,用氮化硅层包裹内芯棒体,得到氮化硅加热棒坯体;
S5、将步骤S4制备的氮化硅加热棒坯体在真空环境中烧结;
其中,步骤S1包括以下工序:
S11、称取氮化硅粉、烧结助剂、分散剂和溶剂,混合并进行球磨;
S12、向工序S11的产物中加入粘结剂和增塑剂,进行球磨,得到浆料;
S13、将工序S12所得到的浆料流延成型,得到氮化硅层;
且工序S12中,粘结剂的添加量为氮化硅粉重量的9-15%,且粘结剂包括重量比为1:(3-4)的PVB72与PVB98;
工序S11中,氮化硅粉满足:α相≥94%、纯度≥99.9%、粒度D50:0.5-0.6μm,D90:1.2-1.3μm;烧结助剂为氧化铝、氧化钇、氧化钬和氧化镱中的至少一种;分散剂为nk2300;溶剂由无水乙醇和乙酸丙酯混合形成。
2.根据权利要求1所述的氮化硅陶瓷加热棒的制备方法,其特征在于,工序S11中,氮化硅粉、烧结助剂、分散剂和溶剂的混合物中固形物含量为48-55% ;其中,氮化硅粉、烧结助剂、分散剂的重量比为:(90-94):(6-10):(2-3),溶剂包括体积比为1:(0.8-1.5)的无水乙醇与乙酸丙酯。
3.根据权利要求1所述的氮化硅陶瓷加热棒的制备方法,其特征在于,工序S12中,增塑剂的添加量为氮化硅粉重量的6-10%,且增塑剂包括重量比为1:(4-5)的PEG400与OE400。
4.根据权利要求1所述的氮化硅陶瓷加热棒的制备方法,其特征在于,工序S31中,烧结助剂、氮化硅粉与结合剂的重量比为(7-15):(85-93):(20-35);且氮化硅粉满足:α相≥94%,比表面积为12-15m2/g。
5.根据权利要求4所述的氮化硅陶瓷加热棒的制备方法,其特征在于,所述结合剂中,PP、LDPE、石蜡与油酸的重量比为(15-20):(15-20):(50-60):(3-10)。
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CN111405694A (zh) * | 2020-03-31 | 2020-07-10 | 宝应县荣泰电子有限公司 | 一种陶瓷点火器所用加热棒及其制作工艺 |
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