CN117069482A - 一种新能源汽车熔断器用氧化铝陶瓷及其制备方法 - Google Patents
一种新能源汽车熔断器用氧化铝陶瓷及其制备方法 Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 18
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002270 dispersing agent Substances 0.000 claims abstract description 9
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 9
- 239000011230 binding agent Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 18
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 18
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 10
- 239000004310 lactic acid Substances 0.000 claims description 9
- 235000014655 lactic acid Nutrition 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 150000007524 organic acids Chemical class 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
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- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 5
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 4
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 229910001940 europium oxide Inorganic materials 0.000 claims description 4
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 4
- 229940075624 ytterbium oxide Drugs 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 239000001530 fumaric acid Substances 0.000 claims description 2
- 235000011087 fumaric acid Nutrition 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 150000002910 rare earth metals Chemical class 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
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- 239000000919 ceramic Substances 0.000 description 2
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- 239000000463 material Substances 0.000 description 2
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- 238000001291 vacuum drying Methods 0.000 description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 239000000155 melt Substances 0.000 description 1
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- 239000011812 mixed powder Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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- 238000005185 salting out Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
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Abstract
本发明涉及陶瓷材料领域，具体为一种新能源汽车熔断器用氧化铝陶瓷及其制备方法，以重量份数计，由以下原料制成：α‑氧化铝80‑100份、氧化镁1‑5份、氧化镧0.5‑1份、稀土元素掺杂倍半氧化物0.1‑1份、粘结剂4‑10份、BKY分散剂0.1‑0.5份、水50‑80份，本发明所制备的氧化铝陶瓷具有极高的直线透光率和良好的力学强度，具有足够的强度承受冲击和振动，又具有断点可视，便于检修的优点，可以满足新能源汽车使用需求。
Description
技术领域
本发明涉及陶瓷材料领域，具体为一种新能源汽车熔断器用氧化铝陶瓷及其制备方法。
背景技术
熔断器是指当电流超过规定值时，以本身产生的热量使熔体熔断，断开电路的一种电器。熔断器被广泛应用于高低压配电系统和控制系统以及各种用电设备中，作为短路和过电流的保护器，是应用最普遍的保护器件之一。
随着新能源汽车越来越普及，新能源汽车上使用的熔断器，既需要满足普通配电系统中直流高压熔断器的熔断保护性能，同时，还需要具有足够的强度要能够承受道路车辆的冲击和振动，这是对新能源汽车高压系统内使用的熔断器的一类独特要求，目前熔断器多采用玻璃管体，其具有断点可视，便于检修的优点，但是玻璃管体的强度不高，难以满足新能源汽车使用需求。
发明内容
发明目的：针对上述技术问题，本发明提出了一种新能源汽车熔断器用氧化铝陶瓷及其制备方法。
所采用的技术方案如下：
一种新能源汽车熔断器用氧化铝陶瓷，以重量份数计，由以下原料制成：
α-氧化铝80-100份、氧化镁1-5份、氧化镧0.5-1份、稀土元素掺杂倍半氧化物0.1-1份、粘结剂4-10份、BKY分散剂0.1-0.5份、水50-80份。
进一步地，所述稀土元素掺杂倍半氧化物中的稀土元素为Nd、Eu、Dy、Sm、Yb中的任意一种或多种。
进一步地，所述稀土元素掺杂倍半氧化物中的倍半氧化物为Sc2O3和/或Y2O3。
进一步地，所述稀土元素掺杂倍半氧化物为Eu、Yb共掺杂Sc2O3。
进一步地，所述稀土元素掺杂倍半氧化物的制备方法如下：
将氧化铕、氧化镱、氧化钪溶于硝酸，边搅拌边将所得溶液滴加入氨水中，滴毕后于40-50℃水浴静置30-90min，将固体滤出后水洗、干燥后研磨、煅烧即可。
进一步地，煅烧温度为800-1000℃，煅烧时间为1-3h。
进一步地，所述粘结剂为有机酸改性聚乙烯醇。
进一步地，所述有机酸改性聚乙烯醇的制备方法如下：
将聚乙烯醇加入水中，搅拌加热使其溶解，再将有机酸缓慢加入，保温反应6-10h后，将反应液冷却至室温，边搅拌边将其滴加到丙酮中，将析出的产物过滤，用丙酮洗涤后干燥即可。
进一步地，所述有机酸为柠檬酸、乳酸、乙酸、富马酸、酒石酸、苹果酸、酒石酸中的任意一种或多种。
本发明还提供了一种新能源汽车熔断器用氧化铝陶瓷的制备方法：
将α-氧化铝、氧化镁、氧化镧、稀土元素掺杂倍半氧化物、BKY分散剂混合球磨后干燥，再与粘结剂、水混合造粒，过筛，倒入模具中压制成型，将得到的粗坯升温至600-800℃下保温排胶1-3h，再升温至1100-1300℃保温预烧1-3h，最后在氢气气氛下升温至1650-1850℃，保温烧结2-4h后降温至1300-1400℃保温2-4h后冷却至室温即可。
本发明的有益效果：
本发明提供了一种新能源汽车熔断器用氧化铝陶瓷，目前，稀土元素掺杂倍半氧化物多作为激光材料使用，发明人将其作为烧结助剂加入，使得烧结出来的氧化铝陶中气孔体积、晶粒尺寸、晶界宽度得到优化，无论是透光率还是力学性能都得到提高，聚乙烯醇经过有机酸改性后，破坏了聚乙烯醇链段的结构规整性，提高聚乙烯醇的水溶性，避免了聚乙烯醇析出结晶对陶瓷成型的不利影响，本发明所制备的氧化铝陶瓷具有极高的直线透光率和良好的力学强度，具有足够的强度承受冲击和振动，又具有断点可视，便于检修的优点，可以满足新能源汽车使用需求。
附图说明
图1为本发明实施例1中所制备氧化铝陶瓷的断面SEM图。
图2为本发明实施例1中所制备氧化铝陶瓷的照片。
具体实施方式
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。本发明未提及的技术均参照现有技术，除非特别指出，以下实施例和对比例为平行试验，采用同样的处理步骤和参数。
实施例1：
一种新能源汽车熔断器用氧化铝陶瓷，以重量份数计，由以下原料制成：
α-氧化铝95份、氧化镁3份、氧化镧1份、稀土元素掺杂倍半氧化物0.5份、乳酸改性聚乙烯醇8份、BYK161分散剂0.2份、水60份。
其中，稀土元素掺杂倍半氧化物为Eu、Yb共掺杂Sc2O3，具体制备方法如下：
将1.76g氧化铕、1.97g氧化镱、13.8g氧化钪加入到200mL 0.5M硝酸中，适当加热使其完全溶解得到均一溶液，冷却至室温后，边搅拌边将溶液滴加入300mL 25％氨水中，控制滴加速率约为5mL/min，滴毕后于50℃水浴静置60min，将反应液抽滤，所得固体水洗至中性后，50℃真空干燥10h后研磨过400目筛网，再转移至马弗炉中以10℃/min的速度升温至950℃煅烧2h后恢复室温即可。
乳酸改性聚乙烯醇的制备方法如下：
将聚合度为2500-2650(DP)的聚乙烯醇50g加入500mL水中，50℃水浴加热，机械搅拌使其完全溶解，再将125mL乳酸缓慢滴入，滴加时间为30min，滴毕后保温反应6-10h后，将反应液冷却至室温，边搅拌边将其滴加到5L丙酮中，将析出的产物过滤，用丙酮洗涤后50℃真空干燥10h即可。
上述新能源汽车熔断器用氧化铝陶瓷的制备方法：
将α-氧化铝、氧化镁、氧化镧、稀土元素掺杂倍半氧化物、BKY分散剂装入球磨罐中，以无水乙醇作为球磨介质，球料质量比为4：1，在300r/min转速下湿磨10h后，再于烘箱中60℃下干燥10h，所得混合粉料与乳酸改性聚乙烯醇、水混合造粒，过100目筛，倒入模具中压制成型，压制成型时先干压，干压时间为5min，压力为10MPa，然后冷等静压机在200MPa压力下压制5min，将得到的粗坯以20℃/min的速度升温至700℃下保温排胶2h，再以10℃/min的速度升温至1200℃保温预烧1h，最后在氢气气氛下以2℃/min的速度升温至1800℃，保温烧结3h后以10℃/min的速度降温至1300℃保温2h后随炉冷却至室温即可。
实施例2：
与实施例1基本相同，区别在于，以重量份数计，新能源汽车熔断器用氧化铝陶瓷由以下原料制成：
α-氧化铝100份、氧化镁5份、氧化镧1份、稀土元素掺杂倍半氧化物1份、乳酸改性聚乙烯醇10份、BYK161分散剂0.5份、水80份。
实施例3：
与实施例1基本相同，区别在于，以重量份数计，新能源汽车熔断器用氧化铝陶瓷由以下原料制成：
α-氧化铝80份、氧化镁1份、氧化镧0.5份、稀土元素掺杂倍半氧化物0.1份、乳酸改性聚乙烯醇5份、BYK161分散剂0.1份、水50份。
对比例1：
与实施例1基本相同，区别在于，不加入稀土元素掺杂倍半氧化物。
对比例2：
与实施例1基本相同，区别在于，用相同重量的氧化钪代替稀土元素掺杂倍半氧化物。
对比例3：
与实施例1基本相同，区别在于，直接将氧化铕、氧化镱和氧化钪加入代替稀土元素掺杂倍半氧化物。
对比例4：
与实施例1基本相同，区别在于，聚乙烯醇不经过乳酸改性。
性能测试：
将本发明实施例1-3及对比例1-4中所制备的氧化铝陶瓷分别制成性能测试所需试样；
①研磨抛光制成厚度为2mm，直径为10mm的圆形试样，用紫外-可见分光光度计(3010型，日本HITACHI)测试试样在可见光波长(650nm)的直线透光率；
②采用三点弯曲方法测试样品的抗弯强度，试样尺寸为3mm×4mm×36mm，每组试样测试5次，取平均值；
测试结果如下表1所示：
表1：
| 直线透光率/％ | 抗弯强度/MPa | |
| 实施例1 | 90.3 | 448 |
| 实施例2 | 88.5 | 420 |
| 实施例3 | 85.9 | 411 |
| 对比例1 | 82.1 | 385 |
| 对比例2 | 81.6 | 404 |
| 对比例3 | 83.5 | 424 |
| 对比例4 | 86.3 | 412 |
由上表1可知，本发明所制备的氧化铝陶瓷具有极高的直线透光率和良好的力学强度。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，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发明各实施例技术方案的精神和范围。
Claims (10)
1.一种新能源汽车熔断器用氧化铝陶瓷，其特征在于，以重量份数计，由以下原料制成：
α-氧化铝80-100份、氧化镁1-5份、氧化镧0.5-1份、稀土元素掺杂倍半氧化物0.1-1份、粘结剂4-10份、BKY分散剂0.1-0.5份、水50-80份。
2.如权利要求1所述的新能源汽车熔断器用氧化铝陶瓷，其特征在于，所述稀土元素掺杂倍半氧化物中的稀土元素为Nd、Eu、Dy、Sm、Yb中的任意一种或多种。
3.如权利要求1所述的新能源汽车熔断器用氧化铝陶瓷，其特征在于，所述稀土元素掺杂倍半氧化物中的倍半氧化物为Sc2O3和/或Y2O3。
4.如权利要求1所述的新能源汽车熔断器用氧化铝陶瓷，其特征在于，所述稀土元素掺杂倍半氧化物为Eu、Yb共掺杂Sc2O3。
5.如权利要求4所述的新能源汽车熔断器用氧化铝陶瓷，其特征在于，所述稀土元素掺杂倍半氧化物的制备方法如下：
将氧化铕、氧化镱、氧化钪溶于硝酸，边搅拌边将所得溶液滴加入氨水中，滴毕后于40-50℃水浴静置30-90min，将固体滤出后水洗、干燥后研磨、煅烧即可。
6.如权利要求5所述的新能源汽车熔断器用氧化铝陶瓷，其特征在于，煅烧温度为800-1000℃，煅烧时间为1-3h。
7.如权利要求1所述的新能源汽车熔断器用氧化铝陶瓷，其特征在于，所述粘结剂为有机酸改性聚乙烯醇。
8.如权利要求7所述的新能源汽车熔断器用氧化铝陶瓷，其特征在于，所述有机酸改性聚乙烯醇的制备方法如下：
将聚乙烯醇加入水中，搅拌加热使其溶解，再将有机酸缓慢加入，保温反应6-10h后，将反应液冷却至室温，边搅拌边将其滴加到丙酮中，将析出的产物过滤，用丙酮洗涤后干燥即可。
9.如权利要求8所述的新能源汽车熔断器用氧化铝陶瓷，其特征在于，所述有机酸为柠檬酸、乳酸、乙酸、富马酸、酒石酸、苹果酸、酒石酸中的任意一种或多种。
10.一种如权利要求1-9中任一项所述的新能源汽车熔断器用氧化铝陶瓷的制备方法，其特征在于，
将α-氧化铝、氧化镁、氧化镧、稀土元素掺杂倍半氧化物、BKY分散剂混合球磨后干燥，再与粘结剂、水混合造粒，过筛，倒入模具中压制成型，将得到的粗坯升温至600-800℃下保温排胶1-3h，再升温至1100-1300℃保温预烧1-3h，最后在氢气气氛下升温至1650-1850℃，保温烧结2-4h后降温至1300-1400℃保温2-4h后冷却至室温即可。
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