CN113735564A - 一种Nb掺杂IZO靶胚及其制备方法 - Google Patents
一种Nb掺杂IZO靶胚及其制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 238000007731 hot pressing Methods 0.000 claims abstract description 21
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000011049 filling Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000005469 granulation Methods 0.000 claims abstract description 6
- 230000003179 granulation Effects 0.000 claims abstract description 6
- 238000001238 wet grinding Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 239000010439 graphite Substances 0.000 claims description 15
- 229910002804 graphite Inorganic materials 0.000 claims description 15
- 238000001291 vacuum drying Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 238000003801 milling Methods 0.000 claims description 13
- 229910052582 BN Inorganic materials 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 56
- 239000011787 zinc oxide Substances 0.000 description 28
- 239000013077 target material Substances 0.000 description 18
- 238000012360 testing method Methods 0.000 description 11
- 239000011701 zinc Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 229910052725 zinc Inorganic materials 0.000 description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 6
- 230000007547 defect Effects 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 6
- 229920001223 polyethylene glycol Polymers 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 3
- 229910001195 gallium oxide Inorganic materials 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
- 229910001887 tin oxide Inorganic materials 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910003437 indium oxide Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 238000005477 sputtering target Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 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 description 1
- 239000008358 core component Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 239000010442 halite Substances 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000009700 powder processing Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种Nb掺杂IZO靶胚及其制备方法,所述靶胚由下列质量份数的氧化物烧结而成:In2O3 90份、ZnO 8份、Nb2O5 0.01‑0.1份。所述制备方法包括(1)混料湿磨、(2)干燥、(3)造粒、(4)装模、(5)热压烧结等步骤。本发明Nb掺杂IZO靶胚具有较高的纯度和强度,导电率等性能较佳。上述技术效果的取得,是产品配方、制备方法等多个技术手段综合作用的结果。
Description
技术领域
本发明涉及金属粉末加工,尤其涉及同时用压实和烧结方法加工金属粉末制品。
背景技术
靶材是磁控溅射过程中的基本耗材,不仅使用量大,而且靶材质量的好坏对薄膜的性能起着至关重要的决定作用。靶材应用领域比较广泛,主要包括光学靶材、显示薄膜用靶材、半导体领域用靶材、记录介质用靶材、超导靶材等。其中半导体领域用靶材、显示用靶材和记录介质用靶材是当前使用最为广泛的三大靶材。为提升薄膜制备速率和保证薄膜的生长质量,溅射靶材要达到一定的指标要求。现有技术中,把控制靶材质量的关键因素概括为纯度、致密度、强度、晶粒尺寸及尺寸分布等几个方面。
近年来,液晶显示、有源有机发光二极管显示以及柔性显示等平板显示技术迅猛发展,作为核心部件的薄膜晶体管(TFT)的重要性不言而喻。其中,基于氧化物半导体的TFT以其较高的载流子迁移率、良好的电学均匀性、高的可见光透过性、较低的制备温度、以及较低的成本等优势受到广泛的关注。
现有技术中,光透过性及导电性优异的铟锡氧化物 (Indium Tin Oxide,ITO)膜是TFT的主流。但是,ITO膜的耐湿性较差,有因湿气导致电阻值增大的缺点。为了改善上述缺点,本技术领域正在研究包含In、Zn、O的氧化铟锌(In2O3-ZnO,IZO)半导体,IZO具有较高的载流子迁移率、大的禁带宽度,可以满足大尺寸、高分辨率、高开口率等显示要求,具有极大的应用潜力。
作为IZO靶材的主要原料之一,ZnO属于一种Ⅱ-Ⅵ族半导体材料,常温下其禁带宽度为3.37eV,激子结合能为60meV。由于其低介电常量、高的化学稳定性、优异的压电、光电等特性,使其在光学、催化剂、太阳能电池等方面具有很大潜力的应用价值。氧化锌拥有六方纤锌矿型、立方闪锌矿型及四方岩盐矿型三种结构晶型。但是,ZnO有着自身的点缺陷,具体来说,ZnO的本征点缺陷主要有六种,分别是锌间隙Znj、锌空位VZn、反位锌Zno、氧间隙Oj、氧空位Vo及反位氧OZn。六种点缺陷中主要的施主缺陷是锌间隙与氧空位,这也是本征氧化锌呈N型的主要原因。未掺杂的氧化锌载流子浓度较低,通过掺杂合适的元素,可以大幅度提高其载流子浓度,以满足该材料在现代工业领域的应用要求。
为了改善ZnO在靶材中的性能,现有技术中进行了诸多尝试。譬如:中国专利文献CN104619673A、CN104619674A披露了一种氧化物烧结体及溅射靶,将氧化锌、氧化铟、氧化镓和氧化锡混合并烧结而得到的氧化物烧结体;中国专利文献CN104416160A披露了一种高致密度氧化锌基靶材,以氧化锌作为主源,掺杂源至少为氧化铟粉末、氧化镓粉末、氧化锂粉、锰粉、氧化钇粉、氧化锆粉、钨粉、银粉、铜粉、氧化锡粉、铋粉、钴粉、镍粉、钛粉、钼粉、铬粉、氧化钒粉、硼粉和氧化铝粉末中的一种;所述锌源和氧源的总质量与所述掺杂源的质量比为5:1至500:1;中国专利文献CN108947518A披露了一种多元掺杂的ZnO镀膜材料,组分包括氧化锌粉体与掺杂氧化物粉体,掺杂粉体选自氧化镓、氧化钇、氧化锡、氧化硅、氧化钛中的一种;美国专利文献US20190177230A1披露了一种氧化物烧结体,其中包括锌、铟、镓、锆和锡等元素;日本专利文献JP2015189632A披露了一种氧化物烧结体,其中包括In、Ga、Zn、Hf和Zr等元素。
上述现有技术存在一个共同的问题,那就是靶材中ZnO的比例很大,虽然采用了掺杂等技术进行改善,但ZnO的固有缺陷并没有完全被克服。因此,如何通过调整掺杂配方及制备方法来克服ZnO的固有缺陷,从而提高IZO靶材的性能成为亟待解决的技术问题。
发明内容
本发明所要解决的技术问题是提供一种掺杂IZO靶胚,使其具有较高的强度且导电率性能佳。
本发明所要解决的另一个技术问题是提供一种Nb掺杂IZO靶胚的制备方法,目的是通过该方法制备出靶胚,并且使产品能达到上述标准。
为了解决上述技术问题,本发明采用如下技术方案:
Nb掺杂IZO靶胚,由下列质量份数的氧化物烧结而成:In2O3 90份、ZnO 8份、Nb2O50.01-0.1份。
优选的,所述靶胚由下列质量份数的氧化物烧结而成:In2O3 90份、ZnO 8份、Nb2O50.05份。
进一步的,所述的方法包括下列步骤:
(1)混料湿磨:将In2O3、ZnO、Nb2O5三种粉体按质量比加入到球磨罐中,加入粘合剂、去离子水、磨球,进行充分磨混;
(2)干燥:置于真空干燥箱中进行干燥;
(3)造粒:采用喷雾造粒机进行造粒,得到Nb掺杂IZO粉体;
(4)装模:取石墨模具,喷涂氮化硼,装入前步所得Nb掺杂IZO粉体;
(5)热压烧结:将石墨模具置入热压烧结炉中进行真空热压烧结,脱模,即得。
优选的,所述第(1)步中,所述粘合剂为PEG。进一步的,所述PEG的用量是2wt.%。
优选的,所述第(1)步中,所述磨混的时间是24h。
优选的,所述第(2)步中,真空干燥的温度是85℃,真空干燥的时间是48h。
优选的,所述第(5)步,热压烧结的步骤如下:
(5-1)0℃升温到500℃,升温30min,保温30min,保压20Mpa;
(5-2)500℃升温到800℃,升温30min,保温60min, 保压25Mpa;
(5-3)800℃升温到1000℃,升温20min,保温60min, 保压18Mpa;
(5-4)1000℃降温到500℃,降温40min,保压16 Mpa;
(5-5)500℃降温到室温,降温40min。
为了保证成品的纯度,所述In2O3、ZnO、Nb2O5三种粉体的纯度均大于99.99%。
与现有技术相比,本发明的有益技术效果至少可以体现在如下几个方面:
1.产品有较高的强度,导电率性能较佳
由下文实施例的测试结果可知,本发明Nb掺杂IZO靶胚各项性能较佳,均优于现有技术制备的IZO掺杂靶材(按对比例1制备)。
(1)本发明Nb掺杂IZO靶胚的抗弯强度达到114.5-122.5MPa,远高于对比例的99.3MPa。
(2)本发明Nb掺杂IZO靶胚的导电率佳。电阻率达到1.3-1.5×10-4Ω·cm,远低于对比例1的11.6×10-4Ω·cm。
采用本发明的烧结方法,有利于提升产品的综合性能
由实施例3与对比例2的数据对比可知,实施例3制备的Nb掺杂IZO靶胚,其各项性能均优于对比例2。实施例3与对比例2的唯一区别是烧结的方式不一样。结果表明,采用本发明的烧结方法,有利于提升产品的综合性能,其原理并不明确,有待进一步的探讨。
综上所述,本发明Nb掺杂IZO靶胚具有较高的纯度,强度、导电率等性能较佳。上述技术效果的取得,是产品配方、制备方法等多个技术手段综合作用的结果。
试验例 Nb掺杂IZO靶胚的性能测试
1.试验方法
下文所述实施例及对比例制成的Nb掺杂IZO靶胚,分别采用下列方法进行性能测试:
1.1 抗弯强度
本发明采用三点抗弯法测试Nb掺杂IZO靶胚的强度,采用的设备是电子万能试验机。通过多次测量,对测得的数据进行统计来判断靶材实际强度。
抗弯强度计算公式为:σ=3PL/2bh2。
其中:P—断裂载荷;L—支点跨距;b—样品宽度;h—样品高度。
电阻率
采用四探针测试仪测量样品电阻率,选取多个区域进行测量,取平均值。
试验结果
试验结果见表1。结果表明:(1)本发明Nb掺杂IZO靶胚有较高的强度,导电率性能较佳;(2)采用本发明的烧结方法,有利于提升产品的综合性能。
表1 Nb掺杂IZO靶胚的性能测试
具体实施方式
下面结合实施例对本发明的技术方案做进一步的说明。
实施例1 Nb掺杂IZO靶胚的制备
配方:In2O3 90份、ZnO 8份、Nb2O5 0.01份。In2O3、ZnO、Nb2O5三种原料粉体的纯度均大于99.99%。
制备方法:
(1)混料湿磨:将In2O3、ZnO、Nb2O5三种粉体按质量比加入到球磨罐中,加入粘合剂、去离子水、磨球,进行充分磨混;
所述粘合剂为PEG(聚乙二醇,polyethylene glycol,下同),用量为2wt.%;
磨混的时间是24h。
(2)干燥:置于真空干燥箱中进行干燥;
真空干燥的温度是85℃,真空干燥的时间是48h。
(3)造粒:采用喷雾造粒机进行造粒,得到Nb掺杂IZO粉体;
(4)装模:取石墨模具,喷涂氮化硼,装入前步所得Nb掺杂IZO粉体;
(5)热压烧结:将石墨模具置入热压烧结炉中进行真空热压烧结,脱模,即得;
热压烧结的步骤如下:
(5-1)0℃升温到500℃,升温30min,保温30min,保压20Mpa;
(5-2)500℃升温到800℃,升温30min,保温60min, 保压25Mpa;
(5-3)800℃升温到1000℃,升温20min,保温60min, 保压18Mpa;
(5-4)1000℃降温到500℃,降温40min,保压16 Mpa;
(5-5)500℃降温到室温,降温40min。
产品性能测试:详见前文试验例。
实施例2 Nb掺杂IZO靶胚的制备
配方:In2O3 90份、ZnO 8份、Nb2O5 0.1份。In2O3、ZnO、Nb2O5三种原料粉体的纯度均大于99.99%。
制备方法:
(1)混料湿磨:将In2O3、ZnO、Nb2O5三种粉体按质量比加入到球磨罐中,加入粘合剂、去离子水、磨球,进行充分磨混;
所述粘合剂为PEG,用量为2wt.%;
磨混的时间是24h。
(2)干燥:置于真空干燥箱中进行干燥;
真空干燥的温度是85℃,真空干燥的时间是48h。
(3)造粒:采用喷雾造粒机进行造粒,得到Nb掺杂IZO粉体;
(4)装模:取石墨模具,喷涂氮化硼,装入前步所得Nb掺杂IZO粉体;
(5)热压烧结:将石墨模具置入热压烧结炉中进行真空热压烧结,脱模,即得;
热压烧结的步骤如下:
(5-1)0℃升温到500℃,升温30min,保温30min,保压20Mpa;
(5-2)500℃升温到800℃,升温30min,保温60min, 保压25Mpa;
(5-3)800℃升温到1000℃,升温20min,保温60min, 保压18Mpa;
(5-4)1000℃降温到500℃,降温40min,保压16 Mpa;
(5-5)500℃降温到室温,降温40min。
产品性能测试:详见前文试验例。
实施例3 Nb掺杂IZO靶胚的制备
配方:In2O3 90份、ZnO 8份、Nb2O5 0.05份。In2O3、ZnO、Nb2O5三种原料粉体的纯度均大于99.99%。
制备方法:
(1)混料湿磨:将In2O3、ZnO、Nb2O5三种粉体按质量比加入到球磨罐中,加入粘合剂、去离子水、磨球,进行充分磨混;
所述粘合剂为PEG,用量为2wt.%;
磨混的时间是24h。
(2)干燥:置于真空干燥箱中进行干燥;
真空干燥的温度是85℃,真空干燥的时间是48h。
(3)造粒:采用喷雾造粒机进行造粒,得到Nb掺杂IZO粉体;
(4)装模:取石墨模具,喷涂氮化硼,装入前步所得Nb掺杂IZO粉体;
(5)热压烧结:将石墨模具置入热压烧结炉中进行真空热压烧结,脱模,即得;
热压烧结的步骤如下:
(5-1)0℃升温到500℃,升温30min,保温30min,保压20Mpa;
(5-2)500℃升温到800℃,升温30min,保温60min, 保压25Mpa;
(5-3)800℃升温到1000℃,升温20min,保温60min, 保压18Mpa;
(5-4)1000℃降温到500℃,降温40min,保压16 Mpa;
(5-5)500℃降温到室温,降温40min。
产品性能测试:详见前文试验例。
对比例1 IZO掺杂靶材的制备
参照中国专利文献CN104619673A实施例NO.1方法制备。
对比例2 Nb掺杂IZO靶胚的制备
热压烧结的步骤步骤如下:
烧结温度1000℃,保温时间200min, 保压20Mpa。
余同实施例3。
显然,上述实施例仅仅是为清楚地说明技术方案而作的举例,并非对本发明实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明要求的保护范围之内。
Claims (9)
1.一种Nb掺杂IZO靶胚,其特征在于,所述靶胚由下列质量份数的氧化物烧结而成:In2O3 90份、ZnO 8份、Nb2O5 0.01-0.1份。
2.一种Nb掺杂IZO靶胚,其特征在于,所述靶胚由下列质量份数的氧化物烧结而成:In2O3 90份、ZnO 8份、Nb2O5 0.05份。
3.权利要求1所述Nb掺杂IZO靶胚的制备方法,其特征在于,所述的方法包括下列步骤:
(1)混料湿磨:将In2O3、ZnO、Nb2O5三种粉体按质量比加入到球磨罐中,加入粘合剂、去离子水和磨球,进行充分磨混;
(2)干燥:置于真空干燥箱中进行干燥;
(3)造粒:采用喷雾造粒机进行造粒,得到Nb掺杂IZO粉体;
(4)装模:取石墨模具,喷涂氮化硼,装入前步所得Nb掺杂IZO粉体;
(5)热压烧结:将石墨模具置入热压烧结炉中进行真空热压烧结,脱模,即得。
4.根据权利要求3所述Nb掺杂IZO靶胚的制备方法,其特征在于,所述第(1)步中,所述粘合剂为PEG。
5.根据权利要求4所述Nb掺杂IZO靶胚的制备方法,其特征在于,所述PEG的用量是2wt.%。
6.根据权利要求3所述Nb掺杂IZO靶胚的制备方法,其特征在于,所述第(1)步中,所述磨混的时间是24h。
7.根据权利要求3所述Nb掺杂IZO靶胚的制备方法,其特征在于,所述第(2)步中,真空干燥的温度是85℃,真空干燥的时间是48h。
8.根据权利要求3所述Nb掺杂IZO靶胚的制备方法,其特征在于,所述第(5)步,热压烧结的步骤如下:
(5-1)0℃升温到500℃,升温30min,保温30min,保压20Mpa;
(5-2)500℃升温到800℃,升温30min,保温60min, 保压25Mpa;
(5-3)800℃升温到1000℃,升温20min,保温60min, 保压18Mpa;
(5-4)1000℃降温到500℃,降温40min,保压16 Mpa;
(5-5)500℃降温到室温,降温40min。
9.根据权利要求3-8任一项所述Nb掺杂IZO靶胚的制备方法,其特征在于,所述In2O3、ZnO、Nb2O5三种粉体的纯度均大于99.99%。
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