CN114804854A - 一种azo靶材及其制备方法 - Google Patents
一种azo靶材及其制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 34
- 239000002270 dispersing agent Substances 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 23
- JYMITAMFTJDTAE-UHFFFAOYSA-N aluminum zinc oxygen(2-) Chemical compound [O-2].[Al+3].[Zn+2] JYMITAMFTJDTAE-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 14
- 239000003292 glue Substances 0.000 claims abstract description 13
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- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 239000011787 zinc oxide Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000000178 monomer Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 150000003512 tertiary amines Chemical class 0.000 claims description 10
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 9
- 229910052731 fluorine Inorganic materials 0.000 claims description 9
- 239000011737 fluorine Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000013077 target material Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- LIWAQLJGPBVORC-UHFFFAOYSA-N ethylmethylamine Chemical compound CCNC LIWAQLJGPBVORC-UHFFFAOYSA-N 0.000 claims description 6
- 229910000611 Zinc aluminium Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- MFFLHHWQAYZAGJ-UHFFFAOYSA-N 1,1,1-trifluoro-6-iodohexane Chemical compound FC(F)(F)CCCCCI MFFLHHWQAYZAGJ-UHFFFAOYSA-N 0.000 claims description 3
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000003431 cross linking reagent Substances 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
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- 239000001913 cellulose Substances 0.000 abstract description 2
- 239000011230 binding agent Substances 0.000 abstract 1
- JAONJTDQXUSBGG-UHFFFAOYSA-N dialuminum;dizinc;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Zn+2].[Zn+2] JAONJTDQXUSBGG-UHFFFAOYSA-N 0.000 description 20
- 239000010408 film Substances 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical group C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 4
- 239000011858 nanopowder Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 3
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- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
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- 229920002873 Polyethylenimine Polymers 0.000 description 1
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- 238000004220 aggregation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 238000002834 transmittance Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
本发明涉及一种AZO靶材及其制备方法,属于光电材料技术领域,包括如下步骤:将氧化锌铝粉体、预混液和分散剂混合,混合后经过球磨,混合好后加入引发剂和催化剂,倒入模具中固化,固化后得到坯体;将得到的坯体进行排胶;排胶后,在惰性气体氛围下进行烧结,得到一种AZO靶材,本发明中通过在惰性气体下进行烧结,提高烧结过程的氧分压,减少氧气的释放,减少烧结过程中的损失。本发明中制备的分散剂属于纤维素类分散剂,由环氧季铵盐与半纤维素反应制备而成,该分散剂与氧化锌铝粉体之间相互作用,吸附在氧化锌铝粉体表面,增加其分散效果,配合烧结环境提高产品质量。
Description
技术领域
本发明属于光电材料技术领域,具体地,涉及一种AZO靶材及其制备方法。
背景技术
AZO靶材即为氧化锌铝靶材,以氧化锌为主,掺杂氧化铝,是制备AZO薄膜的重要原料,氧化锌铝(aluminumzincoxide,AZO)自然资源丰富,其透明导电薄膜的禁带宽度为3.3~3.7eV,可见光透过率为80%~90%,电阻率为10-3~10-4Ωcm,折射率为1.85~1.9,光电性能基本与氧化铟锡(indiumtinoxide,ITO)透明导电薄膜相当,是优良的TCO层材料,具有广阔的应用前景。
表面高活性羟基结构是纳米粉体团聚的根源。由于羟基层中氧的两端一边是高价金属离子,另一边是小电荷氢离子,结构不平衡,表面过剩能较大,使羟基继续以物理吸附的形式吸附水等极性物质。当吸附层达到一定厚度,纳米粉表面就形成水膜,从而产生另一种大的吸引力。由于纳米粉末曲率半径小,使相互接触的水膜毛细表面力变得很大(可达几百MPa),必然导致粉体间相互聚集、凝结,故纳米粉体很难用机械混合法制备均匀的粉体,影响成品质量。
发明内容
为了解决背景技术中提到的技术问题,本发明提供一种AZO靶材及其制备方法。
本发明的目的可以通过以下技术方案实现:
一种AZO靶材的制备方法,包括如下步骤:
将氧化锌铝粉体、预混液和分散剂混合,混合后经过球磨,混合好后加入引发剂和催化剂,倒入模具中固化,固化后得到坯体;将得到的坯体进行排胶;排胶后,在惰性气体氛围下,进行烧结,得到一种AZO靶材。
所述分散剂通过如下步骤制备:
步骤一、在氮气保护条件下,将叔胺含氟单体和无水甲醇混合,升温至55℃,缓慢滴加环氧氯丙烷和无水甲醇的混合物,控制叔胺含氟单体与环氧氯丙烷的摩尔比为1:1.2;保持温度反应6h,用无水乙醚洗脱,真空干燥5h,得到环氧季铵盐;
步骤二、将半纤维素、氢氧化钠和去离子水混合,然后升温至40℃,搅拌30min,然后加入环氧季铵盐,升温至65℃,搅拌4h,搅拌结束后,用盐酸调节pH值为7左右,加入乙醇沉淀,经过过滤干燥,得到分散剂。分散剂的主体部分为半纤维素,通过对其进行处理,得到的分散剂,在粉体表面形成稳定的吸附膜,相对于小分子分散剂其效果更加稳定,且通过引入含氟的环氧季铵盐,在分散剂的结构中引入了氟,降低了氧化锌铝粉体表面的表面能,粉体混合效果好,便于后续工序的进行。分散剂中的氟可以抑制吸附氧的形成,有利于提高材料的热稳定性。提高成品的致密度,保证产品质量。
进一步地,所述半纤维素、环氧季铵盐、氢氧化钠和去离子水的用量比为1g:1.5g:0.2g:10mL。其中,半纤维素的相对分子质量为14000左右。
进一步地,按重量份计,靶材包括如下原料:100-110份氧化锌铝粉体、35-40份预混液、4-5份分散剂、0.1-0.2份引发剂和0.4-0.5份催化剂;所述预混液包括如下重量份原料:20-30份单体、5-8份交联剂、70-80份水。
进一步地,单体为丙烯酰胺、甲基丙烯酰胺中的一种。
进一步地,所述交联剂为N,N′-亚甲基双丙烯酰胺。
进一步地,叔胺含氟单体通过如下步骤制备:
将1mol甲乙胺加入0.2mol6,6,6-三氟-1-碘代己烷和20mL的吡啶的混合物中,在80℃下搅拌4h,将得到的反应液用10wt%的氢氧化钠水溶液洗涤,然后减压浓缩除去溶剂,用硫酸镁干燥真空蒸馏后,得到叔胺含氟单体。
进一步地,所述氧化锌铝粉体为含氧化锌与氧化铝的粉体,或者含氧化锌与铝的粉体,氧化锌所占质量分数为95-98%,其余为氧化铝或者为铝,粉体的粒径在100-300nm范围。
进一步地,球磨时球料的比例为1.2:1,在行星式球磨机上球磨24h。
进一步地,固化温度为30-40℃。
进一步地,排胶过程为:将得到的坯体放入乙醇中,放置10h,然后取出干燥。
进一步地,所述惰性气体为氩气。
在制备AZO靶材的过程中需要进行高温烧结,其中,ZnO在高温条件下容易失氧,烧成后会留下气孔,致使其密度降低,且留下的气孔会对影响AZO靶材的电导率。
进一步地,烧结过程为:以升温速率为10℃/min,升温至烧结温度1400-1500℃,保温30min后,降温至1100-1200℃,进行保温16h。
本发明的有益效果:
本发明中通过在惰性气体下进行烧结,提高烧结过程的氧分压,减少氧气的释放,减少烧结过程中的损失,烧结过程中,温度维持在1100-1200℃,高于该温度时会加剧失氧过程,造成气孔的产生,影响其密度;低于该温度时AZO靶材中的晶粒不紧凑,也会影响产品质量。
本发明中制备的分散剂属于纤维素类分散剂,由环氧季铵盐与半纤维素反应制备而成,该分散剂与氧化锌铝粉体之间相互作用,吸附在氧化锌铝粉体表面,增加其分散效果,配合烧结环境提高产品质量。可以应用于薄膜太阳能电池的电极、透明导电玻璃与柔性膜、等离子显示、红外反射与防护等领域。
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它实施例,都属于本发明保护的范围。
实施例1
本实施例提供了一种分散剂:
步骤一、将1mol甲乙胺加入0.2mol6,6,6-三氟-1-碘代己烷和20mL的吡啶的混合物中,在80℃下搅拌4h,将得到的反应液用10wt%的氢氧化钠水溶液洗涤,然后减压浓缩除去溶剂,用硫酸镁干燥真空蒸馏后,得到叔胺含氟单体;
在氮气保护条件下,将叔胺含氟单体和无水甲醇混合,升温至55℃,缓慢滴加环氧氯丙烷和无水甲醇的混合物,控制叔胺含氟单体与环氧氯丙烷的摩尔比为1:1.2;保持温度反应6h,用无水乙醚洗脱,真空干燥5h,得到环氧季铵盐;
步骤二、将半纤维素、氢氧化钠和去离子水混合,然后升温至40℃,搅拌30min,然后加入环氧季铵盐,升温至65℃,搅拌4h,搅拌结束后,用盐酸调节pH值为7左右,加入乙醇沉淀,经过过滤干燥,得到分散剂。半纤维素、环氧季铵盐、氢氧化钠和去离子水的用量比为1g:1.5g:0.2g:10mL。其中,半纤维素的相对分子质量为14000左右。
实施例2
一种AZO靶材的制备方法,包括如下步骤:
将100份氧化锌铝粉体、35份预混液和4份实施例1制备的分散剂混合,混合后经过球磨,球磨时球料的比例为1.2:1,在行星式球磨机上球磨24h,混合好后加入0.1份引发剂和0.4份催化剂,倒入模具中固化,固化温度为30℃,固化后得到坯体;将得到的坯体进行排胶;将得到的坯体放入乙醇中,放置10h,然后取出干燥,排胶后,在氩气气体氛围下,进行烧结,以升温速率为10℃/min,升温至烧结温度1400℃,保温30min后,降温至1100℃,进行保温16h,得到一种AZO靶材。其中,预混液包括如下重量份原料:20份丙烯酰胺、5份N,N′-亚甲基双丙烯酰胺、70份水。
氧化锌铝粉体为含氧化锌与氧化铝的粉体,或者含氧化锌与铝的粉体,氧化锌所占质量分数为95%,其余为氧化铝或者为铝,粉体的粒径在100-300nm范围。
实施例3
一种AZO靶材的制备方法,包括如下步骤:
将105份氧化锌铝粉体、38份预混液和5份实施例1制备的分散剂混合,混合后经过球磨,球磨时球料的比例为1.2:1,在行星式球磨机上球磨24h,混合好后加入0.2份引发剂和0.5份催化剂,倒入模具中固化,固化温度为35℃,固化后得到坯体;将得到的坯体进行排胶;将得到的坯体放入乙醇中,放置10h,然后取出干燥,排胶后,在氩气气体氛围下,进行烧结,以升温速率为10℃/min,升温至烧结温度1450℃,保温30min后,降温至1150℃,进行保温16h,得到一种AZO靶材。其中,预混液包括如下重量份原料:25份丙烯酰胺、6份N,N′-亚甲基双丙烯酰胺、75份水。
氧化锌铝粉体为含氧化锌与氧化铝的粉体,或者含氧化锌与铝的粉体,氧化锌所占质量分数为96%,其余为氧化铝或者为铝,粉体的粒径在100-300nm范围。
实施例4
一种AZO靶材的制备方法,包括如下步骤:
将110份氧化锌铝粉体、40份预混液和5份实施例1制备的分散剂混合,混合后经过球磨,球磨时球料的比例为1.2:1,在行星式球磨机上球磨24h,混合好后加入0.2份引发剂和0.5份催化剂,倒入模具中固化,固化温度为40℃,固化后得到坯体;将得到的坯体进行排胶;将得到的坯体放入乙醇中,放置10h,然后取出干燥,排胶后,在氩气气体氛围下,进行烧结,以升温速率为10℃/min,升温至烧结温度1500℃,保温30min后,降温至1200℃,进行保温16h,得到一种AZO靶材。其中,预混液包括如下重量份原料:30份甲基丙烯酰胺、8份N,N′-亚甲基双丙烯酰胺、80份水。
氧化锌铝粉体为含氧化锌与氧化铝的粉体,或者含氧化锌与铝的粉体,氧化锌所占质量分数为98%,其余为氧化铝或者为铝,粉体的粒径在100-300nm范围。
对比例1
与实施例3相比,将分散剂换成聚乙烯亚胺,其余原料及制备过程保持不变。
对比例2
与实施例3相比,将氩气气体氛围换成真空氛围,其余原料及制备过程保持不变。
对实施例2-4和对比例1-2制备的靶材进行测试,相对密度采用阿基米德排水法进行测定;电阻率采用《GB/T4326非本征半导体单晶霍尔迁移率和霍尔系数测量方法》测定,测试结果如下表1所示:
表1
实施例2 | 实施例3 | 实施例4 | 对比例1 | 对比例2 | |
相对密度(%) | 99.95 | 99.96 | 99.96 | 99.09 | 95.74 |
电阻率(mΩ·cm) | 0.9X10<sup>-3</sup> | 0.9X10<sup>-3</sup> | 0.9X10<sup>-3</sup> | 1.1X10<sup>-3</sup> | 1.5X10<sup>-3</sup> |
从测试数据可知,本发明制备的靶材的电阻率均小于1X10-3mΩ·cm,相对密度大于99.95%,可以应用于薄膜太阳能电池的电极、透明导电玻璃与柔性膜、等离子显示、红外反射与防护等领域。
在说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (9)
1.一种AZO靶材的制备方法,其特征在于,包括如下步骤:
将氧化锌铝粉体、预混液和分散剂混合,混合后经过球磨,混合好后加入引发剂和催化剂,倒入模具中固化,固化后得到坯体;将得到的坯体进行排胶;排胶后,在惰性气体氛围下,进行烧结,得到一种AZO靶材;
所述分散剂通过如下步骤制备:
步骤一、在氮气保护条件下,将叔胺含氟单体和无水甲醇混合,升温至55℃,缓慢滴加环氧氯丙烷和无水甲醇的混合物,保持温度反应6h,得到环氧季铵盐;
步骤二、将半纤维素、氢氧化钠和去离子水混合,然后升温至40℃,搅拌30min,然后加入环氧季铵盐,升温至65℃,搅拌4h,得到分散剂。
2.根据权利要求1所述的一种AZO靶材的制备方法,其特征在于,按重量份计,靶材包括如下原料:100-110份氧化锌铝粉体、35-40份预混液、4-5份分散剂、0.1-0.2份引发剂和0.4-0.5份催化剂;所述预混液包括如下重量份原料:20-30份单体、5-8份交联剂、70-80份水。
3.根据权利要求1所述的一种AZO靶材的制备方法,其特征在于,叔胺含氟单体通过如下步骤制备:
将1mol甲乙胺加入0.2mol 6,6,6-三氟-1-碘代己烷和20mL的吡啶的混合物中,在80℃下搅拌4h,将得到的反应液用10wt%的氢氧化钠水溶液洗涤,然后减压浓缩除去溶剂,用硫酸镁干燥真空蒸馏后,得到叔胺含氟单体。
4.根据权利要求1所述的一种AZO靶材的制备方法,其特征在于,所述氧化锌铝粉体为含氧化锌与氧化铝的粉体,或者含氧化锌与铝的粉体,氧化锌所占质量分数为95-98%。
5.根据权利要求1所述的一种AZO靶材的制备方法,其特征在于,固化温度为30-40℃。
6.根据权利要求1所述的一种AZO靶材的制备方法,其特征在于,排胶过程为:将得到的坯体放入乙醇中,放置10h,然后取出干燥。
7.根据权利要求1所述的一种AZO靶材的制备方法,其特征在于,所述惰性气体为氩气。
8.根据权利要求1所述的一种AZO靶材的制备方法,其特征在于,烧结过程为:以升温速率为10℃/min,升温至烧结温度1400-1500℃,保温30min后,降温至1100-1200℃,进行保温16h。
9.一种AZO靶材,其特征在于,根据权利要求1-8任意一项所述的制备方法制成。
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