CN114409380A - 一种ito靶材废料的回收利用方法 - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000002699 waste material Substances 0.000 title claims abstract description 31
- 238000004064 recycling Methods 0.000 title claims abstract description 23
- 239000013077 target material Substances 0.000 title abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 54
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 34
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005238 degreasing Methods 0.000 claims abstract description 12
- 238000012216 screening Methods 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims description 45
- 239000002245 particle Substances 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 27
- 239000002270 dispersing agent Substances 0.000 claims description 26
- 239000002002 slurry Substances 0.000 claims description 15
- 230000001804 emulsifying effect Effects 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000011268 mixed slurry Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 239000011230 binding agent Substances 0.000 claims description 8
- 238000004945 emulsification Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 150000001414 amino alcohols Chemical class 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
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- 238000001035 drying Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims 2
- 238000007873 sieving Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000000498 ball milling Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- 229910052738 indium Inorganic materials 0.000 abstract description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 238000001694 spray drying Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 239000000523 sample Substances 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
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- 238000000576 coating method Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 238000003921 particle size analysis Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
本发明提供一种ITO靶材废料的回收利用方法,本发明主要是回收氧化铟含量90~95%的ITO废料,将ITO粉进行筛分,小于1mm的粉料和氧化铟进行球磨生产低含量二氧化锡的ITO靶材。该方法略去了将废料转化成金属铟,再生产成氧化铟的过程,大大降低了生产成本。本发明经过球磨生产低含量二氧化锡的ITO靶材,如97/3的ITO靶材,生产的97/3靶材相对密度可以达到99.7%,晶粒尺寸在10μm。本技术去除了回收粉末脱脂工序,直接乳化砂磨,缩短废料的回收工序,从而降低生产成本,提高了经济效益。
Description
技术领域
本发明涉及电子陶瓷材料技术领域,具体涉及一种ITO靶材废料的回收利用方法。
背景技术
氧化铟锡靶材(ITO靶材)是一种电子陶瓷材料,主要用于磁控溅射镀制ITO膜。氧化铟锡靶材主要分为两类靶材:平面靶材和旋转靶材。广泛应用的主要是90/10、93/7、95/5(90/10是指氧化铟:氧化锡的质量比)的靶材,旋转靶材制备过程中产生大量的余料。如:ITO浆料的喷雾干燥,冷等静压后,靶材坯体表面凹凸不平,需要经过车床进行车床加工,在加工产生大量的余料,约有10%以上的车床余料。
这些余料粉末通常会经过回收工艺重新提炼成精铟,再生产氧化铟和ITO粉,大大增加了生产成本。要降低ITO靶材的生产成本,一方面要减少车床余料的产生,另一方面,要减少余料回收利用的成本。90/10,93/7和95/5的ITO靶材余料回收利用生产出相同比例的ITO靶材相对密度95%,难以到达要求。
发明内容
本发明的目的在于克服现有技术存在的不足之处而提供一种ITO靶材废料的回收利用方法。
为实现上述目的,本发明采取的技术方案为:
一种ITO靶材废料的回收利用方法,包括以下步骤:
(1)筛分:收集ITO车床废料进行筛分,选择筛网孔径小于1mm的筛网,收集粒径小于1mm的ITO靶材废料,粒径大于1mm的靶材废料进行破碎后再次过筛;
(2)将步骤(1)收集到的ITO粉料进行乳化砂磨,乳化机转速为5000~8000rpm,采用马尔文激光粒度测定仪测定其粒度,当ITO粉料的粒径D50<0.2μm且D90<0.5μm时,则为合格,停止砂磨;
(3)将氧化铟粉料进行乳化砂磨,采用马尔文激光粒度测定仪测定其粒度,当氧化铟粉料的粒径D50<0.2μm且D90<0.5μm时,则为合格,停止砂磨;
(4)将步骤(2)所得ITO浆料与步骤(3)所得氧化铟浆料混合砂磨,当混合浆料的粒径D50<0.2μm且D90<0.5μm时,加入粘结剂继续砂磨30~60min;
(5)将步骤(4)制得的混合浆料进行干燥,使混合浆料的水分含量为0.2~0.5%,得到ITO生坯;
(6)将ITO生坯转入模具中,进行冷等静压;
(7)将步骤(6)压制好的靶坯由150℃升至500℃进行脱脂烧结,升温过程中每升温100~150℃保温1~5h;脱脂烧结后,进行第一升温烧结,第一升温烧结是将温度由500℃升至1200℃进行烧结,升温过程中在温度升至900℃、1100℃、1200℃时各保温1~5h;第一升温烧结后,进行第二升温烧结,第二升温烧结是将温度由1200℃升至1600℃进行烧结,升温过程中每升温100~150℃保温1~10h;烧结过程中通入氧气,氧气流量为50~100L/min;
(8)保温结束后,降温至1350~1400℃,再升温至1550~1600℃,保温1~5h,得到ITO靶材。
本发明技术提供一种ITO靶材生产过程废料回收利用方法,该技术主要是回收氧化铟含量90~95%的ITO废料,将ITO粉进行筛分,小于1mm的粉料和氧化铟进行球磨生产低含量二氧化锡的ITO靶材。该方法略去了将废料转化成金属铟,再生产成氧化铟的过程,大大降低了生产成本。
作为本发明的优选技术方案,所述步骤(2)中乳化砂磨过程中,加入分散剂和水,所述分散剂占ITO粉料重量的0.1~2%,所述水占ITO粉料重量的30~40%;所述分散剂为氨基醇类分散剂和氨水的混合物。
作为本发明的优选技术方案,所述步骤(3)中乳化砂磨过程中,加入分散剂和水,所述分散剂占氧化铟粉料重量的0.5~2%,所述水占氧化铟粉料重量的20~40%;所述分散剂为氨基醇类分散剂和氨水的混合物。
作为本发明的优选技术方案,所述步骤(5)的干燥温度为200~250℃。
作为本发明的优选技术方案,所述步骤(6)的压力为300~400MPa。发明人通过研究发现,如果压力过低,胚体密度低,进而导致烧结的靶材密度低。
作为本发明的优选技术方案,所述步骤(7)中,脱脂烧结的升温速率是0.2~0.5℃/min;第一升温烧结的升温速率是0.1~0.5℃/min;第二升温烧结的升温速率是0.1~0.3℃/min。发明人之所以选择本方案的升温速率,是因为如果升温速率过快的话,则使得脱脂不完全,并且制得的靶材容易开裂。
作为本发明的优选技术方案,所述步骤(8)中,以0.5~1℃/min的降温速率降温至1350~1400℃;以0.1~0.5℃/min的升温速率升温至1550~1600℃。本发明通过增加一步降温再升温烧结工序,可以促进靶材中孔径的收缩,进而提高靶材密度。
作为本发明的优选技术方案,所述步骤(8)中得到的ITO靶材的相对密度大于99.7%,纯度大于99.99%。
作为本发明的优选技术方案,所述步骤(8)中得到的ITO靶材中In2O3/SnO2质量比为97/3。本发明方案是通过氧化铟含量90%~95%的ITO废料,经过球磨生产低含量二氧化锡的ITO靶材,如97/3的ITO靶材,生产的97/3靶材相对密度可以达到99.7%,晶粒尺寸在10μm。
与现有技术相比,本发明具有以下有益效果:本技术是通过氧化铟含量90%~95%的ITO废料,经过球磨生产低含量二氧化锡的ITO靶材,如97/3的ITO靶材,生产的97/3靶材相对密度可以达到99.7%,晶粒尺寸在10μm。本技术去除了回收粉末脱脂工序,直接乳化砂磨,缩短废料的回收工序,从而降低生产成本,提高了经济效益。
具体实施方式
为更好的说明本发明的目的、技术方案和优点,下面将结合具体实施例对本发明作进一步说明。
实施例1
本发明所述一种ITO靶材废料的回收利用方法,包括以下步骤:
(1)称取14.5kg的小于1mm的90/10的ITO粉末进行乳化和砂磨,加入占90/10的ITO粉末重量为0.5%的分散剂(分散剂为氨基醇类分散剂和氨水的混合物)和30%的纯水,砂磨2小时,检测马尔文,当粉料的粒径D50<0.2μm且D90<0.5μm时,视为合格停止砂磨;
(2)称取34kg氧化铟进行乳化,加入占氧化铟粉末重量为1.5%的分散剂(分散剂为氨基醇类分散剂和氨水的混合物)和20%的纯水,乳化后进行砂磨2小时,检测马尔文,当粉料的粒径D50<0.2μm且D90<0.5μm时,视为合格停止砂磨;
(3)将乳化后的90/10ITO浆料加入砂磨后的氧化铟浆料中,加占混合浆料重量为3.5%的粘结剂,使组分充分混合均匀,检测二氧化锡浆料含量2.98%。
(4)将混合后97/3ITO浆料进行喷雾干燥,喷雾干燥温度250℃,得到97/3的ITO粉,将97/3的ITO粉转入模具中,在400MPa下进行冷等静压,得到密度在4.5g/cm3左右的靶材胚体。
(5)靶材胚体进行烧结,在150~500℃进行脱脂烧结,升温速率0.5℃/min,在250℃、400℃,500℃保温1小时。继续升温在500~1200℃烧结,升温速率0.3℃/min,在900℃、1100℃、1200℃度各保温3小时。继续升温在1200~1580℃。升温速率0.25℃/min,在1350℃、1450℃保温4小时,在1580℃保温8小时。烧结过程中通入氧气
(6)保温结束后以0.5℃/min降温至1350℃,在以0.25℃/min,升温至1590℃保温5小时,烧结过程中通入氧气。
(7)保温结束后以2℃/min降至室温,得到97/3ITO靶材。测得相对密度为99.75%,采用四探针法测得电阻率为110μΩ.cm,纯度为4N。
实施例2
本发明所述一种ITO靶材废料的回收利用方法,包括以下步骤:
(1)称取25kg的小于1mm的93/7的ITO粉末进行乳化和砂磨加入1%的分散剂,砂磨2小时,经CPS纳米粒度分析系检测,当粉料的粒径D50<0.2μm且D90<0.5μm时,检测CPS合格;
(2)称取34kg氧化铟进行乳化,加入1.5%的分散剂,乳化后进行砂磨2小时,检测马尔文,当粉料的粒径D50<0.2μm且D90<0.5μm时,视为合格;
(3)将乳化后ITO的93/7ITO浆料加入到砂磨后的氧化铟中,加入3.5%的粘结剂,使氧化铟和ITO粉颗粒变细,且组分充分混合均匀,二氧化锡浆料含量3.05%。
(4)将ITO浆料进行喷雾干燥,喷雾干燥温度250℃,得到97/3的ITO粉;将97/3的ITO粉转入模具中,在400MPa下进行冷等静压,得到密度在4.5g/cm3左右的靶材胚体。
(5)将靶材胚体进行烧结,在150~500℃进行脱脂烧结,升温速率0.5℃/min,在250℃、400℃,500℃保温1小时。继续升温在500~1200℃烧结,升温速率0.3℃/min,在900℃、1100℃、1200℃度各保温3小时。继续升温在1200~1600℃,升温速率0.25℃/min,在1350℃、1450℃保温4小时,在1560℃保温8小时。烧结过程中通入氧气。
(6)保温结束以0.5℃/min降温至1350℃,在以0.25℃/min,升温至1580℃保温4小时,烧结过程中通入氧气。
(7)保温结束后以2℃/min降至室温,得到97/3ITO靶材。测得相对密度为99.78%,采用四探针法测得电阻率为113μΩ.cm,纯度为4N。
实施例3
本发明所述一种ITO靶材废料的回收利用方法,包括以下步骤:
(1)称取45kg的小于1mm的95/5的ITO粉末进行乳化和砂磨,加入2%的分散剂,砂磨4小时,检测CPS,当粉料的粒径D50<0.2μm且D90<0.5μm时,合格;
(2)称取30kg氧化铟进行乳化,加入1.5%的分散剂,乳化后进行砂磨2小时,检测马尔文,当粉料的粒径D50<0.2μm且D90<0.5μm时,合格;
(3)将乳化后ITO的95/5ITO浆料加入到砂磨后的氧化铟粉料中,加入4%的粘结剂,使氧化铟和ITO粉颗粒变细,且组分充分混合均匀,二氧化锡浆料含量2.98%。
(4)将ITO浆料进行喷雾干燥,喷雾干燥温度250℃得到97/3的ITO粉,将97/3的ITO粉转入模具中,在400MPa下进行冷等静压,得到密度在4.5g/cm3左右的靶材胚体。
(5)将靶材胚体进行烧结,在150~500℃进行脱脂烧结,升温速率0.5℃/min,在250℃、400℃,500℃保温1小时。继续升温在500~1200℃烧结,升温速率0.3℃/min,在900℃、1100℃、1200℃度各保温3小时。继续升温在1200~1600℃,升温速率0.25℃/min,在1350℃、1450℃保温4小时,在1550℃保温10小时。烧结过程中通入氧气。
(6)保温结束后以0.5℃/min降温至1350℃,在以0.25℃/min,升温至1580℃保温5小时,烧结过程中通入氧气。
(7)保温结束后以2℃/min降至室温,得到97/3ITO靶材。测得相对密度为99.79%,采用四探针法测得电阻率为115μΩ.cm,纯度为4N。
对比例1
本发明所述ITO靶材废料的回收利用方法的一种对比例,本对比例与实施例1的唯一区别在于:本对比例的90/10的ITO靶材废料和氧化铟粉料不进过乳化砂磨,直接进行喷雾干燥。得到的97/3ITO靶材二氧化锡分布不均匀,影响镀膜的性能。由于乳化砂磨可以使氧化铟和氧化锡混合均匀,如果不经过乳化磨砂,则不能直接喷雾干燥,最终使得二氧化锡分布不均匀。
对比例2
本发明所述ITO靶材废料的回收利用方法的一种对比例,本对比例与实施例1的唯一区别在于,本对比例的所有烧结工序的升温速率都为1℃/min。得到的得到的97/3ITO靶材密度低,空洞较多,升温速率过快靶材出现开裂。
对比例3
本发明所述ITO靶材废料的回收利用方法的一种对比例,本对比例与实施例1的唯一区别在于,本对比例不经过降温再升温烧结工序(即实施例的步骤(6))。得到的97/3ITO靶材密度较低,靶材烧结合格率只有50%,生产成本较高。
最后所应当说明的是,以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。
Claims (10)
1.一种ITO靶材废料的回收利用方法,其特征在于,包括以下步骤:
(1)筛分:收集粒径小于1mm的ITO靶材废料,粒径大于1mm的靶材废料进行破碎后再次过筛;
(2)将步骤(1)收集到的ITO粉料进行乳化砂磨,当ITO粉料的粒径D50<0.2μm且D90<0.5μm时,停止砂磨;
(3)将氧化铟粉料进行乳化砂磨,当氧化铟粉料的粒径D50<0.2μm且D90<0.5μm时,停止砂磨;
(4)将步骤(2)所得ITO浆料与步骤(3)所得氧化铟浆料混合砂磨,当混合浆料的粒径D50<0.2μm且D90<0.5μm时,加入粘结剂继续砂磨30~60min;
(5)将步骤(4)制得的混合浆料进行干燥,使混合浆料的水分含量为0.2~0.5%,得到ITO生坯;
(6)将ITO生坯进行冷等静压;
(7)将步骤(6)压制好的靶坯由150℃升至500℃进行脱脂烧结,升温过程中每升温100~150℃保温1~5h;脱脂烧结后,进行第一升温烧结,第一升温烧结是将温度由500℃升至1200℃进行烧结,升温过程中在温度升至900℃、1100℃、1200℃时各保温1~5h;第一升温烧结后,进行第二升温烧结,第二升温烧结是将温度由1200℃升至1600℃进行烧结,升温过程中每升温100~150℃保温1~10h;烧结过程中通入氧气,氧气流量为50~100L/min;
(8)保温结束后,降温至1350~1400℃,再升温至1550~1600℃,保温1~5h,得到ITO靶材。
2.根据权利要求1所述ITO靶材废料的回收利用方法,其特征在于,所述步骤(2)中乳化砂磨过程中,加入分散剂和水,所述分散剂占ITO粉料重量的0.1~2%,所述水占ITO粉料重量的30~40%;所述分散剂为氨基醇类分散剂和氨水的混合物。
3.根据权利要求1所述ITO靶材废料的回收利用方法,其特征在于,所述步骤(3)中乳化砂磨过程中,加入分散剂和水,所述分散剂占氧化铟粉料重量的0.5~2%,所述水占氧化铟粉料重量的20~40%;所述分散剂为氨基醇类分散剂和氨水的混合物。
4.根据权利要求1所述ITO靶材废料的回收利用方法,其特征在于,所述步骤(4)中,加入的粘结剂为聚乙烯醇粘结剂,聚乙烯醇粘结剂的加入量为混合浆料重量的2~5%。
5.根据权利要求1所述ITO靶材废料的回收利用方法,其特征在于,所述步骤(5)的干燥温度为200~250℃。
6.根据权利要求1所述ITO靶材废料的回收利用方法,其特征在于,所述步骤(6)的压力为300~400MPa。
7.根据权利要求1所述ITO靶材废料的回收利用方法,其特征在于,所述步骤(7)中,脱脂烧结的升温速率是0.2~0.5℃/min;第一升温烧结的升温速率是0.1~0.5℃/min;第二升温烧结的升温速率是0.1~0.3℃/min。
8.根据权利要求1所述ITO靶材废料的回收利用方法,其特征在于,所述步骤(8)中,以0.5~1℃/min的降温速率降温至1350~1400℃;以0.1~0.5℃/min的升温速率升温至1550~1600℃。
9.根据权利要求1所述ITO靶材废料的回收利用方法,其特征在于,所述步骤(8)中得到的ITO靶材的相对密度大于99.7%,纯度大于99.99%。
10.根据权利要求1所述ITO靶材废料的回收利用方法,其特征在于,所述步骤(8)中得到的ITO靶材中In2O3/SnO2质量比为97/3。
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