CN116178006A - 一种高导电性氧化钛靶材及其制备方法 - Google Patents
一种高导电性氧化钛靶材及其制备方法 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000013077 target material Substances 0.000 claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 43
- 239000002245 particle Substances 0.000 claims abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 239000011812 mixed powder Substances 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000007731 hot pressing Methods 0.000 claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 238000003754 machining Methods 0.000 claims abstract description 12
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract description 11
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000007873 sieving Methods 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000011265 semifinished product Substances 0.000 claims description 12
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- 238000005520 cutting process Methods 0.000 claims description 8
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- 229920005646 polycarboxylate Polymers 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
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- 239000010955 niobium Substances 0.000 description 23
- 238000005336 cracking Methods 0.000 description 10
- 239000004408 titanium dioxide Substances 0.000 description 10
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- 239000013078 crystal Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000002120 nanofilm Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
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- 238000003825 pressing Methods 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
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- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供一种高导电性氧化钛靶材及其制备方法,属于半导体光电材料领域。该方法为:将氧化铌和氧化钛粉末混合后加入分散剂和水,球磨、烘干研磨后得到混合粉末颗粒;随后进行煅烧、过筛处理、真空热压烧结,冷却后进行机加工后处理即得。以质量百分比计,所得靶材包括90~99%的TiO2和1~10%的Nb2O5,杂质含量≦0.01%。制备方法原料易得,工艺操作简单,使用常规真空热压烧结及加工设备就能完成大规模的工业化生产。同时所得靶材可用作太阳能电池光电器件和显示屏用的薄膜原材料,导电性良好,内部组织晶粒均匀且细小、纯度高、致密度高,不存在间隙缺陷,不容易开裂,机加工性能优良;在满足良好的镀膜性能的同时,有利改善膜层的导电性和透光率。
Description
技术领域
本发明涉及半导体光电材料领域,尤其涉及一种高导电性氧化钛靶材及其制备方法。
背景技术
二氧化钛的两种常见晶型结构中,锐钛矿相光催化活性高,金红石相紫外线吸收能力强。将它们制备成二氧化钛纳米薄膜后,由于其晶粒尺寸细化而具有纳米材料的小尺寸效应、量子效应及表面与界面效应等特殊的纳米效应,涂覆在玻璃、陶瓷等基体表面具有湿敏、气敏、光催化、超亲水、高折射率、高介电常数、化学性质稳定等性能,因而在传感器件、光电转换、环保自清洁等领域得到了广泛的应用。
CN104557021A中公开了一种陶瓷靶材,将TiO2和Nb粉混合后,使用真空热压工艺制成;CN102320824A中公开了一种二氧化钛靶材,通过溶液反应先制得金属离子掺杂的二氧化钛粉体,再将其压制和烧结来制备。CN108203297A中公开了一种氧化钛靶材,对氧化钛纳米粉体改性,再压制成型为陶瓷坯体,在真空气氛或惰性气氛下,进行烧结得到所述氧化钛靶材。上述方法存在以下不足:(1)Nb粉的添加虽然有助于提升TiO2靶材的导电性,但是由于粒度和密度的差异,Nb粉不易在TiO2粉体中分布均匀,这会进一步影响靶材的性能和密度均一性;(2)通过溶液反应先制得金属离子掺杂的二氧化钛粉体,再进行烧结,效率较低,不易规模化量产;(3)纯二氧化钛靶材导电性差,电阻率高。
有鉴于此,特提出本发明。
发明内容
本申请的目的在于提供一种高导电性氧化钛靶材及其制备方法,以解决上述问题。
为实现以上目的,本申请采用以下技术方案:
一种高导电性氧化钛靶材制备方法,其特征在于,包括如下步骤:
S1:将氧化铌和氧化钛粉末混合后加入分散剂和水,球磨得到混合浆料,将所述混合浆料进行烘干研磨处理,得到混合粉末颗粒。
进一步地,所述氧化铌和氧化钛的质量比为(90~99):(1~10)。
优选地,所述氧化铌和氧化钛粉末的纯度不小于99.99%,初始粒径为微米级。掺杂粉末同为陶瓷粉末,易混合均匀,可以提高靶材密度均匀性,改善了用铌金属粉末不易混合均匀的问题。
进一步地,所述分散剂为聚羧酸盐;
优选地,所述分散剂的加入量为所述氧化铌和氧化钛总质量的0.5~0.8%。
进一步地,经所述烘干研磨处理后,控制所述混合粉末颗粒的粒径为0.5μm~1μm。控制所述粒径范围可以提高混合均匀性的同时,为后续提高煅烧和真空热压烧结的效率打下基础。
S2:将步骤S1所得的混合粉末颗粒进行煅烧,随后过筛处理。
进一步地,所述煅烧的温度为800~1000℃,所述煅烧的时间为3~6h。
优选地,所述煅烧时,先将所述混合粉末颗粒升温至550~650℃,保温0.5~2h。所述保温过程可以使所述混合粉末颗粒中的有机物、水等杂质挥发完全,随后再升温至800~1000℃进行煅烧。否则,直接升至800~1000℃煅烧,其中的有机物在没有完全挥发时会变成碳,导致粉料中残余的C元素含量增加,对纯度产生不利的影响。
二氧化钛在800℃以上时,晶型开始由锐钛型转变为金红石型,通过在800℃~1000℃下煅烧,一方面可以保证粉料提前转变为金红石型,粉料一致性较好,晶型转变过程中,相对密度会发生一定变化,提前完成晶型转变热压时比较稳定,靶材不易产生缺陷;一方面Nb2O5和TiO2粉末可提前发生固溶反应,提高靶材致密度。
S3:将步骤S2过筛后的粉末进行真空热压烧结,之后随炉冷却至室温,获得靶材半成品,即靶材坯体。
进一步地,所述真空热压烧结为以2.5~4℃/min升至1100~1200℃,保温2~4h;烧结压力10~20MPa,保压时间2~4h。
优选地,所述真空热压烧结后,随炉冷却之前,先以1.5~3℃/min冷却至800~900℃。
Nb2O5烧结温度一般在1200℃以上,如掺杂Nb2O5比例过多,相应烧结温度也需提高,但过高的温度会导致TiO2出现过烧,内部可能出现缺陷;所以,控制合适的掺杂的比例和烧结温度非常重要。
S4:将步骤S3所得的靶材半成品进行机加工,表面打磨,尺寸修整,即得。
进一步地,所述机加工包括水割和磨床。水割可以很好的防止本发明中的靶材崩裂。
本发明还提供一种以上述的制备方法制得的高导电性氧化钛靶材,以质量百分比计,所述靶材包括90~99%的TiO2和1~10%的Nb2O5,杂质含量≦0.01%;
优选地,所述靶材包括94~96%的TiO2和4~6%的Nb2O5,杂质含量≦0.01%。
本申请的制备方法原料易得,工艺操作简单,使用常规真空热压烧结及加工设备就能完成大规模的工业化生产。同时所得靶材可用作太阳能电池光电器件和显示屏用的薄膜原材料,导电性良好,内部组织晶粒均匀且细小、纯度高、致密度高,不存在间隙缺陷,不容易开裂,机加工性能优良;在满足良好的镀膜性能的同时,有利改善膜层的导电性和透光率。
附图说明
为了更清楚地说明本申请实施例的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,应当理解,以下附图仅示出了本申请的某些实施例,因此不应被看作是对本申请范围的限定。
图1为本发明实施例4的高导电性氧化钛靶材的SEM图。
具体实施方式
下面将结合具体实施例对本申请的实施方案进行详细描述,但是本领域技术人员将会理解,下列实施例仅用于说明本申请,而不应视为限制本申请的范围。实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。
实施例1
一种高导电性氧化钛靶材的制备方法,如图1所示的工艺流程:
(1)按照质量比为99:1选取TiO2和Nb2O5粉末原料,粉末粒径控制在10μm以下,加入水作为球磨介质,加入占TiO2和Nb2O5粉末总质量0.6%的聚羧酸盐D305,将混合后的浆料球磨6h,随后在120℃下进行烘干研磨处理后,控制所述混合粉末颗粒的粒径为0.5μm~1μm之间;
(2)将步骤(1)所得的混合粉末颗粒以1.5℃/min升至600℃,保温1h;再以1.5℃/min升至950℃进行煅烧,保温5h,随后100目过筛处理;
(3)将步骤(2)中过筛后的粉末进行真空热压烧结,具体是以3℃/min升温至1180℃,压力17MPa,保温保压3h;随后以2.3℃/min降温至900℃,最后随炉冷却至室温,得到靶材半成品;
(4)将靶材进行表面机加工打磨,水割为所需尺寸,获得所述的高导电性氧化钛靶材。
所得的高导电性氧化钛靶材致密度可以达到98.6%,电阻率可达0.5~1Ω·cm,无开裂。
实施例2
一种高导电性氧化钛靶材的制备方法,如下:
(1)按照质量比为98:2选取TiO2和Nb2O5粉末原料,粉末粒径控制在10μm以下,加入水作为球磨介质,加入占TiO2和Nb2O5粉末总质量0.6%的聚羧酸盐D305,将混合后的浆料球磨6h,随后在110℃下进行烘干研磨处理后,控制所述混合粉末颗粒的粒径为0.5μm~1μm之间;
(2)将步骤(1)所得的混合粉末颗粒以1.5℃/min升至600℃,保温1h;再以1.5℃/min升至950℃进行煅烧,保温5h,随后100目过筛处理;
(3)将步骤(2)中过筛后的粉末进行真空热压烧结,具体是以3℃/min升温至1180℃,压力17MPa,保温保压3h;随后以2.3℃/min降温至900℃,最后随炉冷却至室温,得到靶材半成品;
(4)将靶材进行表面机加工打磨,水割为所需尺寸,获得所述的高导电性氧化钛靶材。
所得的高导电性氧化钛靶材致密度可以达到98.2%,电阻率可达1~5x10-1Ω·cm,无开裂。
实施例3
一种高导电性氧化钛靶材的制备方法,如下:
(1)按照质量比为96:4选取TiO2和Nb2O5粉末原料,粉末粒径控制在10μm以下,加入水作为球磨介质,加入占TiO2和Nb2O5粉末总质量0.6%的聚羧酸盐D305,将混合后的浆料球磨6h,随后在110℃下进行烘干研磨处理后,控制所述混合粉末颗粒的粒径为0.5μm~1μm之间;
(2)将步骤(1)所得的混合粉末颗粒以1.5℃/min升至600℃,保温1h;再以1.5℃/min升至950℃进行煅烧,保温5h,随后100目过筛处理;
(3)将步骤(2)中过筛后的粉末进行真空热压烧结,具体是以3℃/min升温至1180℃,压力17MPa,保温保压3h;随后以2.3℃/min降温至900℃,最后随炉冷却至室温,得到靶材半成品;
(4)将靶材进行表面机加工打磨,水割为所需尺寸,获得所述的高导电性氧化钛靶材。
所得的高导电性氧化钛靶材致密度可以达到97.9%,电阻率可达0.5~1x10-1Ω·cm,无开裂。
实施例4
一种高导电性氧化钛靶材的制备方法,如下:
(1)按照质量比为94:6选取TiO2和Nb2O5粉末原料,粉末粒径控制在10μm以下,加入水作为球磨介质,加入占TiO2和Nb2O5粉末总质量0.6%的聚羧酸盐D305,将混合后的浆料球磨6h,随后在110℃下进行烘干研磨处理后,控制所述混合粉末颗粒的粒径为0.5μm~1μm之间;
(2)将步骤(1)所得的混合粉末颗粒以1.5℃/min升至600℃,保温1h;再以1.5℃/min升至950℃进行煅烧,保温5h,随后100目过筛处理;
(3)将步骤(2)中过筛后的粉末进行真空热压烧结,具体是以3℃/min升温至1180℃,压力17MPa,保温保压3h;随后以2.3℃/min降温至900℃,最后随炉冷却至室温,得到靶材半成品;
(4)将靶材进行表面机加工打磨,水割为所需尺寸,获得所述的高导电性氧化钛靶材。
所得的高导电性氧化钛靶材致密度可以达到97.7%,电阻率可达1~5x10-2Ω·cm,无开裂。
实施例5
一种高导电性氧化钛靶材的制备方法,如下:
(1)按照质量比为96:4选取TiO2和Nb2O5粉末原料,粉末粒径控制在10μm以下,加入水作为球磨介质,加入占TiO2和Nb2O5粉末总质量0.6%的聚羧酸盐D305,将混合后的浆料球磨6h,随后在120℃下进行烘干研磨处理后,控制所述混合粉末颗粒的粒径为0.5μm~1μm之间;
(2)将步骤(1)所得的混合粉末颗粒以1.5℃/min升至600℃,保温1h;再以1.5℃/min升至950℃进行煅烧,保温5h,随后100目过筛处理;
(3)将步骤(2)中过筛后的粉末进行真空热压烧结,具体是以3℃/min升温至1180℃,压力17MPa,保温保压3h;随后随炉冷却至室温,得到靶材半成品;
(4)将靶材进行表面机加工打磨,水割为所需尺寸,获得所述的高导电性氧化钛靶材。
所得的高导电性氧化钛靶材致密度可以达到97.9%,电阻率可达0.5~1x10-1Ω·cm,出现开裂。
实施例6
与实施例1基本相同,区别仅在于步骤(2)为:将步骤(1)所得的混合粉末颗粒以1.5℃/min升至550℃,保温1h;再以1.5℃/min升至800℃进行煅烧,保温5h,随后100目过筛处理。
所得的高导电性氧化钛靶材致密度可以达到98.0%,电阻率可达0.5~1Ω·cm,无开裂。
实施例7
与实施例1基本相同,区别仅在于步骤(3)为:将步骤(2)中过筛后的粉末进行真空热压烧结,具体是以2.5℃/min升温至1100℃,压力20MPa,保温保压4h;随后以5℃/min降温至800℃,最后随炉冷却至室温,得到靶材半成品。
所得的高导电性氧化钛靶材致密度可以达到98.4%,电阻率可达0.5~1Ω·cm,出现开裂。
对比例1
与实施例3基本相同,不同之处在于没有步骤(2)的煅烧处理。
所得的氧化钛靶材致密度可以达到95.0%,电阻率可达1~5x10-1Ω·cm,出现开裂。
实施例1~7及对比例1所制得的靶材性能测试数据见表1。
表1实施例1~7及对比例1所制得的靶材性能测试数据
由表1可以看出,相同烧结条件下,氧化铌掺的比例越高,电性越好,但是密度会越低。综合考量,电性达到1×10-1Ω·cm以下和密度达到97.7%以上为最佳效果。同时,烧结时降温速率和节奏的控制也是重要影响因素,同时可以防止靶材开裂。
最后应说明的是:以上各实施例仅用以说明本申请的技术方案,而非对其限制;尽管参照前述各实施例对本申请进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本申请各实施例技术方案的范围。
此外,本领域的技术人员能够理解,尽管在此的一些实施例包括其它实施例中所包括的某些特征而不是其它特征,但是不同实施例的特征的组合意味着处于本申请的范围之内并且形成不同的实施例。例如,在上面的权利要求书中,所要求保护的实施例的任意之一都可以以任意的组合方式来使用。公开于该背景技术部分的信息仅仅旨在加深对本申请的总体背景技术的理解,而不应当被视为承认或以任何形式暗示该信息构成已为本领域技术人员所公知的现有技术。
Claims (10)
1.一种高导电性氧化钛靶材制备方法,其特征在于,包括如下步骤:
S1:将氧化铌和氧化钛粉末混合后加入分散剂和水,球磨得到混合浆料,将所述混合浆料进行烘干研磨处理,得到混合粉末颗粒;
S2:将步骤S1所得的混合粉末颗粒进行煅烧,随后过筛处理;
S3:将步骤S2过筛后的粉末进行真空热压烧结,之后随炉冷却至室温,获得靶材半成品;
S4:将步骤S3所得的靶材半成品进行机加工,表面打磨,尺寸修整,即得。
2.根据权利要求1所述的制备方法,其特征在于,步骤S1中,所述氧化铌和氧化钛的质量比为(90~99):(1~10);
优选地,所述氧化铌和氧化钛的质量比为(94~96):(4~6)。
优选地,所述氧化铌和氧化钛粉末的纯度不小于99.99%,初始粒径为微米级。
3.根据权利要求1所述的制备方法,其特征在于,步骤S1中,所述分散剂为聚羧酸盐;
优选地,所述分散剂的加入量为所述氧化铌和氧化钛总质量的0.5~0.8%。
4.根据权利要求1所述的制备方法,其特征在于,步骤S1中,经所述烘干研磨处理后,控制所述混合粉末颗粒的粒径为0.5μm~1μm。
5.根据权利要求1所述的制备方法,其特征在于,步骤S2中,所述煅烧的温度为800~1000℃,所述煅烧的时间为3~6h。
6.根据权利要求5所述的制备方法,其特征在于,步骤S2中,所述煅烧时,先将所述混合粉末颗粒升温至550~650℃,保温0.5~2h。
7.根据权利要求1所述的制备方法,其特征在于,步骤S3中,所述真空热压烧结为以2.5~4℃/min升至1100~1200℃,保温2~4h;烧结压力10~20MPa,保压时间2~4h。
8.根据权利要求7所述的制备方法,其特征在于,步骤S3中,所述真空热压烧结后,随炉冷却之前,先以1.5~3℃/min冷却至800~900℃。
9.根据权利要求1所述的制备方法,其特征在于,步骤S4中,所述机加工包括水割和磨床。
10.一种权利要求1~9任一项所述的制备方法制得的高导电性氧化钛靶材,其特征在于,以质量百分比计,所述靶材包括90~99%的TiO2和1~10%的Nb2O5,杂质含量≦0.01%;
优选地,所述靶材包括94~96%的TiO2和4~6%的Nb2O5,杂质含量≦0.01%。
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