CN116041061A - 一种钽铌酸钾陶瓷及其制备方法 - Google Patents
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- 239000000919 ceramic Substances 0.000 title claims abstract description 83
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 35
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000011591 potassium Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 84
- 239000011734 sodium Substances 0.000 claims abstract description 50
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 22
- 150000002500 ions Chemical class 0.000 claims abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 5
- 229910052802 copper Inorganic materials 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims description 71
- 238000005245 sintering Methods 0.000 claims description 64
- 238000000227 grinding Methods 0.000 claims description 40
- 239000000843 powder Substances 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 239000000084 colloidal system Substances 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 25
- 239000003292 glue Substances 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 22
- 238000007599 discharging Methods 0.000 claims description 18
- 239000003082 abrasive agent Substances 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 16
- 238000007873 sieving Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000008187 granular material Substances 0.000 claims description 8
- 230000006698 induction Effects 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 229920002994 synthetic fiber Polymers 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 239000010949 copper Substances 0.000 abstract description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 2
- 230000000630 rising effect Effects 0.000 description 12
- 238000001816 cooling Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
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Abstract
本发明属于无机非金属材料领域,尤其涉及一种钽铌酸钾陶瓷及其制备方法。为钠、铁共掺钽铌酸钾晶体,其化学式为Na,Cu:K1+ZTa1‑ xNbxO3,其中,Nb的量为0.36≤X≤0.40,0.15≤Z≤0.3,居里点位于‑241~90℃之间,所述钽铌酸钾陶瓷在居里点以上晶体为立方相,m3m点群;在居里点以下变为四方相,4mm点群;通过引入钠、铜元素作为掺杂离子,通过确定掺杂量,选择优选配比,配合专用的制备方法,制备了高质量陶瓷,均匀性好,陶瓷质量得到大幅度提高;陶瓷漏电性能得到大幅度改善,进一步推动了KTN陶瓷的器件应用;本制备方法操作简单,成本低,大大降低了生产成本。
Description
技术领域
本发明属于无机非金属材料领域,尤其涉及一种钽铌酸钾陶瓷及其制备方法。
背景技术
近年来随着电子信息技术的迅速发展,具备优异的铁电和压电性能的材料已经成为目前研究领域的热点之一。目前来说,铅系材料仍然是应用于这些领域的主体材料,但是铅系材料在制备和使用的过程中会对环境造成严重的污染问题。因此寻找一种无铅且性能优越的材料成为大势所趋。
钽铌酸钾陶瓷(KTN)是一种优良的铁电材料和热释电材料,是一种可以与铅系材料相媲美的无铅铁电环保材料。但现有的钽铌酸钾陶瓷存在漏电流大、抗疲劳差的缺点,阻碍其在器件应用化的发展进程。为了寻求优质的KTN陶瓷,对材料的制备工艺进行深入研究也是一项有意义的工作。
发明内容
本发明针对现有技术中存在的上述技术问题,提出一种能纯度较高、结晶良好、高均匀性,而且具有更优异的铁电性能的钽铌酸钾陶瓷及其制备方法。
为了达到上述目的,本发明采用的技术方案为:
一种钽铌酸钾陶瓷,其特征在于,为钠、铁共掺钽铌酸钾晶体,其化学式为Na,Cu:K1+ZTa1-xNbxO3,其中,Nb的量为0.36≤X≤0.40,0.15≤Z≤0.3,居里点位于-241~90℃之间,所述钽铌酸钾陶瓷在居里点以上晶体为立方相,m3m点群;在居里点以下变为四方相,4mm点群。
作为优选,所述Na+的掺杂浓度为3.2-3.6at%,所述的Cu2+掺杂浓度为2.5-3at%,所述的Na+/Cu2+掺杂浓度比1.06-1.44。
作为优选,当Nb的量0.36≤x<0.38,Z为0.25<Z≤0.3,掺杂浓度比X/Z为1.2-1.52;
当Nb的量0.38≤X≤0.40,Z为0.15≤Z≤0.25,掺杂浓度比X/Z为1.52-2.67。
上述钽铌酸钾陶瓷的制备方法,以高纯K2CO3、Nb2O5、Ta2O5为原料,以高纯Na2O和CuO为掺杂离子,采用提拉法生长,生长装置为感应加热提拉式单晶炉。
优选的,所述钽铌酸钾陶瓷的制备方法,具体包括如下步骤:
S1、制备研磨料A:
根据所需Na,Cu:K1+ZTa1-xNbxO3陶瓷组分,选择原料K2CO3、Nb2O5、Ta2O5原料混合均匀,获得原料A;
将所述原料A放入陶瓷坩埚中,在800℃烧结5小时,得到多晶料A;
取出多晶料A,将其重新研磨成粉末,粒度为170nm-250nm,获得研磨料A;
S2、制备研磨料B:
将掺杂原料Na2O和CuO混合均匀,获得原料B,将原料B放入陶瓷坩埚中,在700℃烧结3小时进,得到多晶料B;
取出所述多晶料B重新研磨成粉末粒度为200nm-300nm,获得研磨料B;
S3、烧结预合成:
将步骤S1所得研磨料A和步骤S2所得研磨料B,混合均匀,进行压实,并置于高温炉中预烧,升温速度为120-150℃/h,650℃-700℃保温2h,获得烧结预合成料C;
S4、研磨与过筛:
将步骤S3获得的预合成料C压碎加入无水酒精作为分散剂置于球墨罐中球墨6h,得到粉末D粒度0.355mm-0.425mm;其中,所述的合成料C与无水酒精的质量体积比为0.2-0.6g/L;
S5、研磨造粒:
将步骤S4获得的粉末D添加PVA胶体,注胶后充分研磨,然后过45目的筛子过筛造粒,以保证粉料颗粒均匀;所述的PVA胶体的质量分数9%;
S6、压片排胶:
将步骤S5造粒完成的颗粒通过液压机压成直径为25mm,厚度为10mm的圆柱片;将该圆柱片置于高温炉中,以10℃/min升温速率,600℃保温1h,排出胶体;
S7、烧结:
将步骤S6所得排胶后的样品进行烧结,烧结温度为1230-1300℃,保温时间3h。
作为优选,在步骤S1制备研磨料A之前,对原料进行预处理:将Nb2O5、Ta2O5在800℃下煅烧30分钟,Na2O和CuO在500℃下煅烧30分钟,K2CO3在100℃下干燥1h。
作为优选,当0.36≤x≤0.38时,步骤S7中,烧结过程的升温速率为15-20℃/min,降温速率为6-8℃/min。
作为优选,当0.38≤x≤0.40时,步骤S7中,烧结过程的升温速率为7-10℃/min,降温速率为3-5℃/min。
与现有技术相比,本发明的优点和积极效果在于:通过引入钠、铜元素作为掺杂离子,通过确定掺杂量,选择优选配比,配合专用的制备方法,制备了高质量陶瓷,均匀性好,陶瓷质量得到大幅度提高;陶瓷漏电性能得到大幅度改善,进一步推动了KTN陶瓷的器件应用;本制备方法操作简单,成本低,大大降低了生产成本。
附图说明
图1为本发明实施例1制备的钽铌酸钾陶瓷的XRD图谱;
图2为本发明实施例2制备的钽铌酸钾陶瓷的XRD图谱;
图3为本发明实施例2制备的钽铌酸钾陶瓷的断面图;
图4为本发明实施例3制备的钽铌酸钾陶瓷的漏电流图。
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。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
一种钽铌酸钾陶瓷,化学式为Na,Cu:K1.27Ta0.64Nb0.36O3,X=0.36,Na+的掺杂浓度为3.3at%,Cu2+掺杂浓度为2.7at%;
上述的Na,Cu:K1.27Ta0.64Nb0.36O3陶瓷的制备方法,以高纯K2CO3、Nb2O5、Ta2O5为原料,以高纯Na2O和CuO为掺杂离子,采用提拉法生长,生长装置为感应加热提拉式单晶炉,陶瓷生长步骤如下:
原料预处理:按化学计量比将Nb2O5、Ta2O5在800℃下煅烧30分钟,Na2O和CuO在500℃下煅烧30分钟,K2CO3在100℃下干燥1h;
烧结预合成:根据所需陶瓷组分,选择原料K2CO3,Nb2O5、Ta2O5混合均匀,获得原料A;将原料A放入陶瓷坩埚中,在800℃烧结5小时,得到多晶料A;取出多晶料A重新研磨成粉末粒度为200nm,获得研磨料A;将掺杂原料Na2O和CuO混合均匀,获得原料B,将原料B放入陶瓷坩埚中,在700℃烧结3小时进,得到多晶料B;取出多晶料B重新研磨成粉末粒度为200nm,获得研磨料B;将研磨料A和研磨料B,混合均匀,进行压实,并置于高温炉中预烧,升温速度为130℃/h,680℃保温2h,获得烧结预合成料C;
研磨与过筛:将上述获得的预合成料C压碎加入无水酒精作为分散剂置于球墨罐中球墨6h,得到粉末D粒度0.355mm;其中所述的合成料C与无水酒精的质量体积比为0.2g/L;
研磨造粒:将上述获得的粉末D添加PVA胶体,注胶后充分研磨,然后过45目的筛子过筛造粒,以保证粉料颗粒均匀;PVA胶体的质量分数9%;
压片排胶:将造粒完成的颗粒通过液压机压成直径为25mm,厚度为10mm的圆柱片:将该圆柱片置于高温炉中,以10℃/min升温速率,600℃保温1h,排出胶体;
烧结:排胶后的样品需要烧结,样品的烧结温度设定为在升温排胶结束后,继续加热;样品的烧结温度设定为1230-1300℃,保温时间3h;其中升温速率为18℃/min,降温速率为6℃/min。
如图1所示,为实施例1制备的Na,Cu:K1.27Ta0.64Nb0.36O3陶瓷的XRD图谱,从图中可以看出陶瓷片纯相无杂质。
实施例2
一种钽铌酸钾陶瓷Na,Cu:K1.17Ta0.62Nb0.38O3,X=0.38,Z=0.17,Na+的掺杂浓度为3.2at%,Cu2+掺杂浓度为2.8at%;
本实施例所述的Na,Cu:K1.17Ta0.62Nb0.38O3陶瓷的制备方法,以高纯K2CO3、Nb2O5、Ta2O5为原料,以高纯Na2O和CuO为掺杂离子,采用提拉法生长,生长装置为感应加热提拉式单晶炉,陶瓷生长步骤如下:
原料预处理:将Nb2O5、Ta2O5在800℃下煅烧30分钟,Na2O和CuO在500℃下煅烧30分钟,K2CO3在100℃下干燥1h。
烧结预合成:根据所需Na,Cu:K1.17Ta0.62Nb0.38O3陶瓷组分,选择原料K2CO3,Nb2O5、Ta2O5原料混合均匀,获得原料A;将原料A放入陶瓷坩埚中,在800℃烧结5小时,得到多晶料A;取出多晶料A重新研磨成粉末粒度为250nm,获得研磨料A;将掺杂原料Na2O和CuO混合均匀,获得原料B,将原料B放入陶瓷坩埚中,在700℃烧结3小时进,得到多晶料B;取出多晶料B重新研磨成粉末粒度为200nm,获得研磨料B;将研磨料A和研磨料B,混合均匀,进行压实,并置于高温炉中预烧,升温速度为150℃/h,650℃保温2h,获得烧结预合成料C排;
研磨与过筛:将上述获得的预合成料C压碎加入无水酒精作为分散剂置于球墨罐中球墨6h,得到粉末D粒度0.405mm;其中所述的合成料C与无水酒精的质量体积比为0.2g/L;
研磨造粒:将上述获得的粉末D添加PVA胶体,注胶后充分研磨,然后过45目的筛子过筛造粒,以保证粉料颗粒均匀;PVA胶体的质量分数9%;
压片排胶:将造粒完成的颗粒通过液压机压成直径为25mm,厚度为10mm的圆柱片:将该圆柱片置于高温炉中,以10℃/min升温速率,600℃保温1h,排出胶体;
烧结:排胶后的样品需要烧结,样品的烧结温度设定为在升温排胶结束后,继续加热;样品的烧结温度设定为1230℃,保温时间3h;其中升温速率为10℃/min,降温速率为3℃/min。
如图2所示为上述制备的Na,Cu:K1.17Ta0.62Nb0.38O3陶瓷的XRD图谱,从图中可以看出陶瓷无杂相;图3为Na,Cu:K1.17Ta0.62Nb0.38O3陶瓷的断面图,从图中可以看出致密度高。
实施例3
一种钽铌酸钾陶瓷Na,Cu:K1.25Ta0.6Nb0.4O3,X=0.4,Z=0.25,Na+的掺杂浓度为3.3at%,Cu2+掺杂浓度为2.5at%;
上述Na,Cu:K1.25Ta0.6Nb0.4O3陶瓷的制备方法,以高纯K2CO3、Nb2O5、Ta2O5为原料,以高纯Na2O和CuO为掺杂离子,采用提拉法生长,生长装置为感应加热提拉式单晶炉,陶瓷生长步骤如下:
原料预处理:将Nb2O5、Ta2O5在800℃下煅烧30分钟,Na2O和CuO在500℃下煅烧30分钟,K2CO3在100℃下干燥1h。
烧结预合成:所需陶瓷组分,选择原料K2CO3,Nb2O5、Ta2O5原料混合均匀,获得原料A;将原料A放入陶瓷坩埚中,在800℃烧结5小时,得到多晶料A;取出多晶料A重新研磨成粉末粒度为170nm,获得研磨料A;将掺杂原料Na2O和CuO混合均匀,获得原料B,将原料B放入陶瓷坩埚中,在700℃烧结3小时进,得到多晶料B;取出多晶料B重新研磨成粉末粒度为200nm,获得研磨料B;将研磨料A和研磨料B,混合均匀,进行压实,并置于高温炉中预烧,升温速度为130℃/h,670℃保温2h,获得烧结预合成料C;
研磨与过筛:将上述获得的预合成料C压碎加入无水酒精作为分散剂置于球墨罐中球墨6h,得到粉末D粒度0.355mm;其中所述的合成料C与无水酒精的质量体积比为0.6g/L;
研磨造粒:将上述获得的粉末D添加PVA胶体,注胶后充分研磨,然后过45目的筛子过筛造粒,以保证粉料颗粒均匀;PVA胶体的质量分数9%;
压片排胶:将造粒完成的颗粒通过液压机压成直径为25mm,厚度为10mm的圆柱片:将该圆柱片置于高温炉中,以10℃/min升温速率,600℃保温1h,排出胶体;
烧结:排胶后的样品需要烧结,样品的烧结温度设定为在升温排胶结束后,继续加热。样品的烧结温度设定为1230-1300℃,保温时间3h;其中升温速率为7℃/min,降温速率为5℃/min。
图4为上述制备的Na,Cu:K1.25Ta0.6Nb0.4O3陶瓷的漏电流图,从图中可以看出漏电流较低,具有较好的电学性能。
实施例4
一种钽铌酸钾陶瓷Na,Cu:K1.3Ta0.63Nb0.37O3,X=0.37,Z=0.3,Na+的掺杂浓度为3.4at%,Cu2+掺杂浓度为3.0at%;
上述Na,Cu:K1.3Ta0.63Nb0.37O3陶瓷的制备方法,以高纯K2CO3、Nb2O5、Ta2O5为原料,以高纯Na2O和CuO为掺杂离子,采用提拉法生长,生长装置为感应加热提拉式单晶炉,陶瓷生长步骤如下:
原料预处理:将Nb2O5、Ta2O5在800℃下煅烧30分钟,Na2O和CuO在500℃下煅烧30分钟,K2CO3在100℃下干燥1h。
烧结预合成:所需陶瓷组分,选择原料K2CO3,Nb2O5、Ta2O5原料混合均匀,获得原料A;将原料A放入陶瓷坩埚中,在800℃烧结5小时,得到多晶料A;取出多晶料A重新研磨成粉末粒度为180nm,获得研磨料A;将掺杂原料Na2O和CuO混合均匀,获得原料B,将原料B放入陶瓷坩埚中,在700℃烧结3小时进,得到多晶料B;取出多晶料B重新研磨成粉末粒度为240nm,获得研磨料B;将研磨料A和研磨料B,混合均匀,进行压实,并置于高温炉中预烧,升温速度为120℃/h,700℃保温2h,获得烧结预合成料C;
研磨与过筛:将上述获得的预合成料C压碎加入无水酒精作为分散剂置于球墨罐中球墨6h,得到粉末D粒度0.385mm;其中所述的合成料C与无水酒精的质量体积比为0.4g/L;
研磨造粒:将上述获得的粉末D添加PVA胶体,注胶后充分研磨,然后过45目的筛子过筛造粒,以保证粉料颗粒均匀;PVA胶体的质量分数9%;
压片排胶:将造粒完成的颗粒通过液压机压成直径为25mm,厚度为10mm的圆柱片:将该圆柱片置于高温炉中,以10℃/min升温速率,600℃保温1h,排出胶体;
烧结:排胶后的样品需要烧结,样品的烧结温度设定为在升温排胶结束后,继续加热。样品的烧结温度设定为1230-1300℃,保温时间3h;其中升温速率为15℃/min,降温速率为8℃/min。
实施例5
一种钽铌酸钾陶瓷Na,Cu:K1.15Ta0.61Nb0.39O3,X=0.39,Z=0.15,Na+的掺杂浓度为3.6at%,Cu2+掺杂浓度为2.9at%;
上述Na,Cu:K1.15Ta0.61Nb0.39O3陶瓷的制备方法,以高纯K2CO3、Nb2O5、Ta2O5为原料,以高纯Na2O和CuO为掺杂离子,采用提拉法生长,生长装置为感应加热提拉式单晶炉,陶瓷生长步骤如下:
原料预处理:将Nb2O5、Ta2O5在800℃下煅烧30分钟,Na2O和CuO在500℃下煅烧30分钟,K2CO3在100℃下干燥1h。
烧结预合成:所需陶瓷组分,选择原料K2CO3,Nb2O5、Ta2O5原料混合均匀,获得原料A;将原料A放入陶瓷坩埚中,在800℃烧结5小时,得到多晶料A;取出多晶料A重新研磨成粉末粒度为220nm,获得研磨料A;将掺杂原料Na2O和CuO混合均匀,获得原料B,将原料B放入陶瓷坩埚中,在700℃烧结3小时进,得到多晶料B;取出多晶料B重新研磨成粉末粒度为280nm,获得研磨料B;将研磨料A和研磨料B,混合均匀,进行压实,并置于高温炉中预烧,升温速度为150℃/h,680℃保温2h,获得烧结预合成料C;
研磨与过筛:将上述获得的预合成料C压碎加入无水酒精作为分散剂置于球墨罐中球墨6h,得到粉末D粒度0.425mm;其中所述的合成料C与无水酒精的质量体积比为0.3g/L;
研磨造粒:将上述获得的粉末D添加PVA胶体,注胶后充分研磨,然后过45目的筛子过筛造粒,以保证粉料颗粒均匀;PVA胶体的质量分数9%;
压片排胶:将造粒完成的颗粒通过液压机压成直径为25mm,厚度为10mm的圆柱片:将该圆柱片置于高温炉中,以10℃/min升温速率,600℃保温1h,排出胶体;
烧结:排胶后的样品需要烧结,样品的烧结温度设定为在升温排胶结束后,继续加热。样品的烧结温度设定为1230-1300℃,保温时间3h;其中升温速率为8℃/min,降温速率为4℃/min。
实施例6
一种钽铌酸钾陶瓷Na,Cu:K1.25Ta0.62Nb0.38O3,X=0.38,Z=0.25,Na+的掺杂浓度为3.5at%,Cu2+掺杂浓度为2.7at%;
上述Na,Cu:K1.25Ta0.62Nb0.38O3陶瓷的制备方法,以高纯K2CO3、Nb2O5、Ta2O5为原料,以高纯Na2O和CuO为掺杂离子,采用提拉法生长,生长装置为感应加热提拉式单晶炉,陶瓷生长步骤如下:
原料预处理:将Nb2O5、Ta2O5在800℃下煅烧30分钟,Na2O和CuO在500℃下煅烧30分钟,K2CO3在100℃下干燥1h。
烧结预合成:所需陶瓷组分,选择原料K2CO3,Nb2O5、Ta2O5原料混合均匀,获得原料A;将原料A放入陶瓷坩埚中,在800℃烧结5小时,得到多晶料A;取出多晶料A重新研磨成粉末粒度为240nm,获得研磨料A;将掺杂原料Na2O和CuO混合均匀,获得原料B,将原料B放入陶瓷坩埚中,在700℃烧结3小时进,得到多晶料B;取出多晶料B重新研磨成粉末粒度为220nm,获得研磨料B;将研磨料A和研磨料B,混合均匀,进行压实,并置于高温炉中预烧,升温速度为130℃/h,650℃保温2h,获得烧结预合成料C;
研磨与过筛:将上述获得的预合成料C压碎加入无水酒精作为分散剂置于球墨罐中球墨6h,得到粉末D粒度0.405mm;其中所述的合成料C与无水酒精的质量体积比为0.5g/L;
研磨造粒:将上述获得的粉末D添加PVA胶体,注胶后充分研磨,然后过45目的筛子过筛造粒,以保证粉料颗粒均匀;PVA胶体的质量分数9%;
压片排胶:将造粒完成的颗粒通过液压机压成直径为25mm,厚度为10mm的圆柱片:将该圆柱片置于高温炉中,以10℃/min升温速率,600℃保温1h,排出胶体;
烧结:排胶后的样品需要烧结,样品的烧结温度设定为在升温排胶结束后,继续加热。样品的烧结温度设定为1230-1300℃,保温时间3h;其中升温速率为20℃/min,降温速率为7℃/min。
Claims (8)
1.一种钽铌酸钾陶瓷,其特征在于,为钠、铁共掺钽铌酸钾晶体,其化学式为Na,Cu:K1+ ZTa1-xNbxO3,其中,Nb的量为0.36≤X≤0.40,0.15≤Z≤0.3,居里点位于-241~90℃之间,所述钽铌酸钾陶瓷在居里点以上晶体为立方相,m3m点群;在居里点以下变为四方相,4mm点群。
2.根据权利要求1所述的钽铌酸钾陶瓷,其特征在于,所述Na+的掺杂浓度为3.2-3.6at%,所述的Cu2+掺杂浓度为2.5-3at%,所述的Na+/Cu2+掺杂浓度比1.06-1.44。
3.根据权利要求2所述的钽铌酸钾陶瓷,其特征在于,当Nb的量0.36≤x<0.38,Z为0.25<Z≤0.3,掺杂浓度比X/Z为1.2-1.52;
当Nb的量0.38≤X≤0.40,Z为0.15≤Z≤0.25,掺杂浓度比X/Z为1.52-2.67。
4.根据权利要求1-3所述的任一项钽铌酸钾陶瓷的制备方法,其特征在于:以高纯K2CO3、Nb2O5、Ta2O5为原料,以高纯Na2O和CuO为掺杂离子,采用提拉法生长,生长装置为感应加热提拉式单晶炉。
5.根据权利要求4所述的钽铌酸钾陶瓷的制备方法,其特征在于,具体包括如下步骤:
S1、制备研磨料A:
根据所需Na,Cu:K1+ZTa1-xNbxO3陶瓷组分,选择原料K2CO3、Nb2O5、Ta2O5原料混合均匀,获得原料A;
将所述原料A放入陶瓷坩埚中,在800℃烧结5小时,得到多晶料A;
取出多晶料A,将其重新研磨成粉末,粒度为170nm-250nm,获得研磨料A;
S2、制备研磨料B:
将掺杂原料Na2O和CuO混合均匀,获得原料B,将原料B放入陶瓷坩埚中,在700℃烧结3小时进,得到多晶料B;
取出所述多晶料B重新研磨成粉末粒度为200nm-300nm,获得研磨料B;
S3、烧结预合成:
将步骤S1所得研磨料A和步骤S2所得研磨料B,混合均匀,进行压实,并置于高温炉中预烧,升温速度为120-150℃/h,650℃-700℃保温2h,获得烧结预合成料C;
S4、研磨与过筛:
将步骤S3获得的预合成料C压碎加入无水酒精作为分散剂置于球墨罐中球墨6h,得到粉末D粒度0.355mm-0.425mm;其中,所述的合成料C与无水酒精的质量体积比为0.2-0.6g/L;
S5、研磨造粒:
将步骤S4获得的粉末D添加PVA胶体,注胶后充分研磨,然后过45目的筛子过筛造粒,以保证粉料颗粒均匀;所述的PVA胶体的质量分数9%;
S6、压片排胶:
将步骤S5造粒完成的颗粒通过液压机压成直径为25mm,厚度为10mm的圆柱片;将该圆柱片置于高温炉中,以10℃/min升温速率,600℃保温1h,排出胶体;
S7、烧结:
将步骤S6所得排胶后的样品进行烧结,烧结温度为1230-1300℃,保温时间3h。
6.根据权利要求5所述的钽铌酸钾陶瓷的制备方法,其特征在于,在步骤S1制备研磨料A之前,对原料进行预处理:将Nb2O5、Ta2O5在800℃下煅烧30分钟,Na2O和CuO在500℃下煅烧30分钟,K2CO3在100℃下干燥1h。
7.根据权利要求6所述的钽铌酸钾陶瓷的制备方法,其特征在于,当0.36≤x≤0.38时,步骤S7中,烧结过程的升温速率为15-20℃/min,降温速率为6-8℃/min。
8.根据权利要求6所述的钽铌酸钾陶瓷的制备方法,其特征在于,当0.38≤x≤0.40时,步骤S7中,烧结过程的升温速率为7-10℃/min,降温速率为3-5℃/min。
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