CN105906328A - 一种氧化铝荧光陶瓷材料及其制备方法和应用 - Google Patents
一种氧化铝荧光陶瓷材料及其制备方法和应用 Download PDFInfo
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- CN105906328A CN105906328A CN201610253258.1A CN201610253258A CN105906328A CN 105906328 A CN105906328 A CN 105906328A CN 201610253258 A CN201610253258 A CN 201610253258A CN 105906328 A CN105906328 A CN 105906328A
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- aluminium oxide
- calcium
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- ceramic material
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 173
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 75
- 239000000203 mixture Substances 0.000 claims abstract description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 18
- 238000004020 luminiscence type Methods 0.000 claims abstract description 12
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 9
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 9
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 238000010345 tape casting Methods 0.000 claims abstract description 8
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 36
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 33
- MKPXGEVFQSIKGE-UHFFFAOYSA-N [Mg].[Si] Chemical compound [Mg].[Si] MKPXGEVFQSIKGE-UHFFFAOYSA-N 0.000 claims description 33
- 229910052791 calcium Inorganic materials 0.000 claims description 33
- 239000011575 calcium Substances 0.000 claims description 33
- 230000008569 process Effects 0.000 claims description 32
- 239000002002 slurry Substances 0.000 claims description 31
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 17
- 238000005266 casting Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 13
- 239000011812 mixed powder Substances 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 230000005284 excitation Effects 0.000 claims description 8
- 238000007766 curtain coating Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000009499 grossing Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 238000005488 sandblasting Methods 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000005245 sintering Methods 0.000 abstract description 7
- 230000005540 biological transmission Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 2
- LAZOHFXCELVBBV-UHFFFAOYSA-N [Mg].[Ca].[Si] Chemical compound [Mg].[Ca].[Si] LAZOHFXCELVBBV-UHFFFAOYSA-N 0.000 abstract 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract 2
- 239000000919 ceramic Substances 0.000 description 38
- 230000004907 flux Effects 0.000 description 15
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 9
- 238000002834 transmittance Methods 0.000 description 9
- 238000005286 illumination Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 229920001223 polyethylene glycol Polymers 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000005538 encapsulation Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 230000001678 irradiating effect Effects 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003698 laser cutting Methods 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
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Abstract
本发明涉及半导体技术领域,具体涉及一种氧化铝荧光陶瓷材料,其主要由按质量百分比计的70‑99%的基料氧化铝和1‑30%的钙镁硅成分添加荧光粉经流延法制坯、再经烧结而成,其中所述的钙镁硅成分是指氧化镁或滑石粉与二氧化硅及碳酸钙的混合物,所述的荧光粉添加量以氧化铝和钙镁硅成分总质量计为10‑30%但不等于10%。本发明还提供了该材料的制备方法和应用。本发明的氧化铝荧光陶瓷材料,具有成本低和透光效果好,360度发光更均匀的特点。
Description
技术领域
本发明涉及半导体技术领域,具体涉及一种用流延法、模压成型工艺所制成的氧化铝荧光陶瓷材料。
背景技术
LED灯丝灯因具有360度全发光、无频闪、不发烫、长寿命、缓衰减等特性广受关注,LED发光是靠芯片激发荧光粉产生均匀照明,2013年广州国际照明LED展览会(光亚展)只有2家参展商展示LED灯丝灯;2014年有50多家LED照明企业展示各种各样的LED灯丝灯;2014年10月底结束的香港HKTDC的国际LED灯展有将近200家企业展示LED灯丝灯;2015年春全国设计生产灯丝灯企业已达600多家。市场需求的热度快速升温,特别是纳米半透明陶瓷灯丝的发明成功使用,不仅降低了产品成本,有效解决相关灯丝灯的技术,达到高“性价比”产品,国际市场对技术创新的LED灯丝灯迅速认可,市场需求成倍增加。LED灯丝灯采用高电压、小电流的HVLEDS创新技术,灯丝灯在点亮工作时只赋予10-15mA的小电流驱动即可发光。传统5W的LED球泡点亮时的灯头瓶颈温度可达75-95摄氏度,面同功率的LED灯丝灯点亮8小时后A60玻璃泡的温度在36摄氏度以下,可以实现真正的安全使用。许多真正实现360度均匀发光这就需要材料的透光性增加,玻璃有好的透光性但它有一个致命缺陷是导热性极差,导热系数只有0.5左右,蓝宝石具有好的透光性但价格太高,纳米半透明陶瓷虽有高性价比产品,但透明度还没有达到更好。本发明新开发的荧光陶瓷既有陶瓷的良好导热(导热系数在20瓦/米·度左右),又有生产LED在表面通过胶与荧光粉混合在表面封胶无法比拟的均匀性,且后序可以实现单面点胶,工序简化效果更好成本更优的性能。也可以用于COB封装360度发光的球泡灯,市场前景广阔。本发明与传统最大区别在于将荧光粉通过改进配方和生产工艺均匀分布在陶瓷内部。
应该说,在本发明之前还不存在真正意义上的氧化铝荧光陶瓷材料。
发明内容
针对现有技术存在的上述问题和缺陷,本发明旨在提供一种氧化铝荧光陶瓷材料,以期能够改善氧化铝陶瓷材料存在的透明度不高、价格太高的问题,从而提供一种更具有市场应用价值的氧化铝荧光陶瓷材料。本发明同时还提供了该氧化铝荧光陶瓷的制备方法和应用。制备方法具有工艺成熟、操作简单的特点。
为实现本发明的目的,发明人提供如下的技术方案:
首先,发明人提供了一种氧化铝荧光陶瓷材料,其主要由按质量百分比计的70-99%的基料氧化铝和1-30%的钙镁硅成分添加荧光粉经流延法制坯、再经烧结而成,其中所述的钙镁硅成分是指氧化镁或滑石粉(滑石主要成分为含水硅酸镁)与二氧化硅及碳酸钙的混合物,所述的荧光粉添加量以氧化铝和钙镁硅成分总质量计为10-30%但不等于10%。
氧化铝荧光陶瓷是一种以氧化铝(Al2O3)为主体和加入荧光粉制成的陶瓷材料。发明人研究发现,将荧光粉和氧化铝按适宜比例混合通过流延法和烧结,能够得到真正实现360度均匀发光的材料,导热系数可达20瓦/米·度左右,可以实现真正的安全使用。流延法是制备薄膜陶瓷的一种重要的方法,其过程是,将制备好的陶瓷浆料从料斗上部流到基带上,通过基带与刮刀的相对运动形成素坯,在表面张力的作用下,形成光滑的上表面。
作为优选,本发明中,所述的荧光粉性能满足:激发波长430-480nm、发光峰值550-558nm、相对亮度95-105%及密度3.7g/cm3以上。只有满足该要求的荧光粉才能实现发明目的。
作为优选,本发明中,所述的荧光粉D50为5-20μm、氧化铝粉体粒径满足:D50为1-6μm、钙镁硅成分粉体粒径满足:D50为1-6μm。对粉体粒径的控制主要是出于流延法工艺的需求。颗粒大小控制在需要的范围,可提高流延产品的表面质量。
本发明还提供了上述的一种氧化铝荧光陶瓷材料的制备方法,包括如下步骤:
(1)按照质量百分比70-99%的基料氧化铝和1-30%的钙镁硅成分备料,将氧化铝和钙镁硅成分混合,混合粉料中加入部分分散剂进行球磨处理,然后加入溶剂先溶的粘结剂和余量分散剂,再加入荧光粉再次进行球磨处理,得到流延浆料,其中:分散剂的加入量以钙镁硅成分与氧化铝混合粉料质量计为0.1-1%,溶剂加入量以钙镁硅成分与氧化铝混合粉料质量计为15-45%,粘结剂加入量以钙镁硅成分与氧化铝混合粉料质量计为2-10%;所述的钙镁硅成分是指氧化镁或滑石粉与二氧化硅及碳酸钙的混合物,
本步骤的目的在于将粉料充分均匀混合,并将粘结剂均匀分散,使浆料具有一定的柔软性。
(2)测定温度和粘度后的流延浆料,过滤后输入真空脱泡机进行脱泡处理,
测定温度和粘度后的流延浆料,其目的在于控制出浆气压及出浆速度。
脱泡处理,即浆料在真空脱泡机中抽真空,把浆料中的气泡抽出的过程。此步骤的目的在于保证浆料的致密性,提高浆料粘度,以符合流延所需的粘度。
(3)再次测定温度和粘度后通过过滤器进行流延制备料带,
(4)料带做时效处理,温度控制在10℃-30℃ 之内,湿度控制在55±25%RH之间,放置时间不少于7天且不多于一年,
由于在流延过程中温度等有一定的差异,通过时效处理可以提高整体料带的一致性。并且采取封装,可以提高时效处理时环境的稳定性,以此来使料带收缩至一个更稳定的状态,精度控制的更加好。
(5)将上述步骤得到的料带根据需要加工处理成生坯基片,
(6)将上述生坯基片在最高温度为1500℃~1750℃的环境下进行烧结处理,得到熟坯基片,其中:温度从常温到1750℃,时间为10-45小时,这是一个逐步升温和降温的过程,将陶瓷基片从生坯转变为熟坯,即烧结成品。
(7)将烧结成型后的熟坯基片进行表面喷砂处理,
将清洗干净的产品小心整理好后,用气枪吹去表面残留吸附的杂质,用干净的薄膜盖好。此步骤目的在于去除基片表面的防粘砂,避免在之后的抚平中产生影响。
(8)将经过上述步骤处理过的基片放置于最高温度为1200℃~1400℃的环境中进行抚平处理。此步骤目的在于将基片抚平,调整其平整度。温度视不同比例配方进行调整。
作为优选,本发明中,所述的荧光粉性能满足:激发波长430-480nm、发光峰值550-558nm、相对亮度95-105%及密度3.7g/cm3以上;所述的荧光粉D50为12-20μm、氧化铝粉体粒径满足:D50为1-6μm、钙镁硅成分粉体粒径满足:D50为1-6μm。
作为优选,本发明中,所述的溶剂采用甲苯或酒精等;粘结剂采用PVB(聚乙烯醇缩丁醛的简称)和PEG(聚乙二醇的简称)等;分散剂采用W-S80等。
作为优选,本发明中,所述的球磨处理的时间两次一共为30-80小时。主要是为了得到粒度适宜的流延浆料,便于进行下一步处理。
作为优选,本发明中,所述的步骤(2)中测定温度和粘度,应满足浆料温度为20-50℃、粘度在3000-30000CPS之间,过滤采用80目~500目的不锈钢过滤网,脱泡处理的时间≥2个小时;步骤(3)中再次测定温度和粘度,应满足浆料温度为20-45℃、粘度在5000-30000CPS之间,过滤器的过滤网目数大于50目。采用80目~500目的不锈钢过滤网的作用是将粒径大于5.5μm颗粒和异物排出,使颗粒大小控制在需要的范围,提高了流延产品的表面质量;由于步骤(1)中产出的粉料与粘结剂和溶剂粘结在一起,因此过滤后其颗粒粒径小于5.5μm。
作为优选,本发明中,所述的步骤(5)中根据需要加工处理是指根据成品的尺寸和形状需要对生坯带加工处理。后期加工时可以免除使用激光切割技术,避免激光加工对陶瓷基片造成损伤。
本发明还提供了上述的一种氧化铝荧光陶瓷材料在照明材料中的应用,所述照明材料包括并不限于LED、COB等。
实验表明,本发明比正常氧化铝陶瓷透光性能更好,成本低,做成LED支架相比玻璃漏出蓝光更少。比如实施例1中,在相同设备和光源条件下,先用光直接照射得到光通量为14.656LM,在半透明陶瓷遮光照射得到光通量为2.985.LM,利用荧光陶瓷遮光照射后得到光通量为5.5340LM,说明荧光陶瓷比半透明陶瓷透光率高85%。
与现有技术相比,本发明具有以下优点:
1、透光率高:透光效果比纳米半透明陶瓷高80%以上,360度发光更均匀,光效好,不漏蓝光。
2、成本低:大大低于同含量透明氧化铝成本;透明氧化铝陶瓷是原料纯度在99.99%以上且需要在气氛烧成炉中进行烧成,本发明产品在普通70-99%含量的氧化铝陶瓷基础上通过加入特殊荧光材料通过流延法高温烧成中批量生产,具有性价比高的强大优势。
3、本发明主要特点在于在原有的陶瓷生产工艺上改进配方增加荧光粉在陶瓷生产过程中充分混合,具体均匀性好、比一般陶瓷材料透光率高(透光率提高80%以上)、后序制作简化工序降低成本的特点,主要是提高了一般陶瓷透光率和改善了荧光发光的均匀性,可以减少后工序表面敷荧光粉,实现真正的高性价比产品制作。
具体实施方式
下面结合实施例,更具体地说明本发明的内容。应当理解,本发明的实施并不局限于下面的实施例,对本发明所做的任何形式上的变通和/或改变都将落入本发明保护范围。
在本发明中,若非特指,所有的设备和原料等均可从市场购得或是本行业常用的。下述实施例中的方法,如无特别说明,均为本领域的常规方法。
实施例
1
1、备料
荧光粉10.1kg,氧化铝70kg,钙镁硅成分(氧化镁9.05kg、二氧化硅16kg和碳酸钙4.95kg),甲苯22kg,PVB 4.2kg,PEG1.5kg,W-S80 0.6kg。
荧光粉性能满足:激发波长430-480nm、发光峰值550-558nm、相对亮度95-105%及密度3.7g/cm3以上;所述的荧光粉D50为12-20μm,氧化铝粉体粒径满足:D50为1-6μm,钙镁硅成分粉体粒径满足:D50为1-6μm,
2、按下述步骤制备氧化铝荧光陶瓷材料:
(1)将钙镁硅成分粉料与氧化铝混合,混合粉料中第一次配料加入S80球磨4小时,第二次配料加入用甲苯先溶的PVB和PEG,加入荧光粉再次球磨30小时,得到流延浆料;
(2)测定温度和粘度后的流延浆料,浆料温度为30-50℃、粘度在3000-5000CPS,过滤后输入真空脱泡机进行脱泡处理,过滤采用280目的不锈钢过滤网,脱泡处理的时间≥2个小时,
(3)再次测定温度和粘度后通过过滤器进行流延制备料带,浆料温度为25-40℃、粘度在8000-15000CPS,过滤器的过滤网目数大于150目,
(4)料带做时效处理,放置在料带库,采取封装,温度控制在10℃-30℃ 之内,湿度控制在55±25%RH之间,放置时间不少于7天且不多于一年,
(5)将上述步骤得到的料带根据成品的尺寸和形状需要对生坯带作冲切等加工处理成生坯基片,
(6)将上述生坯基片在最高温度为1500℃~1750℃的环境下进行烧结处理,得到熟坯基片,其中:温度从常温到1750℃,时间为25小时左右,这是一个逐步升温和降温的过程,将陶瓷基片从生坯转变为熟坯,即烧结成品。
(7)将烧结成型后的熟坯基片进行表面喷砂处理,
将清洗干净的产品小心整理好后,用气枪吹去表面残留吸附的杂质,用干净的薄膜盖好。
(8)将经过上述步骤处理过的基片放置于最高温度为1200℃~1400℃的环境中进行抚平处理。
将得到的氧化铝荧光陶瓷材料用于LED照明产品。经检测,做成的LED支架,在相同设备和光源条件下,先用光直接照射得到光通量为14.656LM,在半透明陶瓷遮光照射得到光通量为2.985LM,利用荧光陶瓷遮光照射后得到光通量为5.534LM,说明荧光陶瓷比半透明陶瓷透光率高85%。
实施例
2
1、备料
荧光粉15kg,氧化铝99kg,钙镁硅成分(氧化镁0.3kg、二氧化硅0.5kg和碳酸钙0.2kg),甲苯30kg,PVB7 kg,PEG2.3kg,W-S80 0.6kg。
荧光粉性能满足:激发波长430-480nm、发光峰值550-558nm、相对亮度95-105%及密度3.7g/cm3以上;所述的荧光粉D50为12-20μm,氧化铝粉体粒径满足:D50为1-6μm,
2、按下述步骤制备氧化铝荧光陶瓷材料:
(1)将钙镁硅成分粉料与氧化铝混合,混合粉料中第一次配料加入S80球磨4小时,第二次配料加入用甲苯先溶的PVB和PEG,加入荧光粉再次球磨时间48小时,得到流延浆料,
(2)测定温度和粘度后的流延浆料,浆料温度为35-50℃、粘度在3000-6000CPS,过滤后输入真空脱泡机进行脱泡处理,过滤采用280目的不锈钢过滤网,脱泡处理的时间≥2个小时,
(3)再次测定温度和粘度后通过过滤器进行流延制备料带,浆料温度为30-35℃、粘度在10000-20000CPS,过滤器的过滤网目数大于100目,
(4)料带做时效处理,放置在料带库,采取封装,温度控制在10℃-30℃ 之内,湿度控制在55±25%RH之间,放置时间不少于1天且不多于一年,
(5)将上述步骤得到的料带根据成品的尺寸和形状需要对生坯带作冲切等加工处理成生坯基片,
(6)将上述生坯基片在最高温度为1600℃~1750℃的环境下进行烧结处理,得到熟坯基片,其中:温度从常温到1750℃,时间为30小时左右,这是一个逐步升温和降温的过程,将陶瓷基片从生坯转变为熟坯,即烧结成品。
(7)将烧结成型后的熟坯基片进行表面喷砂处理,
将清洗干净的产品小心整理好后,用气枪吹去表面残留吸附的杂质,用干净的薄膜盖好。
(8)将经过上述步骤处理过的基片放置于最高温度为1200℃~1400℃的环境中进行抚平处理。
将得到的氧化铝荧光陶瓷材料用于LED照明产品。经检测,做成的LED支架,在相同设备和光源条件下,先用光直接照射得到光通量为14.656LM,在半透明陶瓷遮光照射得到光通量为2.985LM,利用荧光陶瓷遮光照射后得到光通量为5.6865LM,说明荧光陶瓷比半透明陶瓷透光率高90%。
实施例3
1、备料
荧光粉220kg,氧化铝80kg,钙镁硅成分(氧化镁6.13kg、二氧化硅10.9kg和碳酸钙2.97kg),甲苯25kg,PVB 6kg,PEG2kg,W-S80 0.5kg。
荧光粉性能满足:激发波长430-480nm、发光峰值550-558nm、相对亮度95-105%及密度3.7g/cm3以上;所述的荧光粉D50为12-20μm,氧化铝粉体粒径满足:D50为1-6μm,钙镁硅成分粉体粒径满足:D50为1-6μm,
2、按下述步骤制备氧化铝荧光陶瓷材料:
(1)将钙镁硅成分粉料与氧化铝混合,混合粉料中第一次配料加入S80球磨4小时,第二次配料加入用甲苯先溶的PVB和PEG,加入荧光粉再次球磨时间48小时,得到流延浆料,
(2)测定温度和粘度后的流延浆料,浆料温度为45-50℃、粘度在8000-10000CPS,过滤后输入真空脱泡机进行脱泡处理,过滤采用200目的不锈钢过滤网,脱泡处理的时间≥2个小时,
(3)再次测定温度和粘度后通过过滤器进行流延制备料带,浆料温度为30-45℃、粘度在15000-18000CPS,过滤器的过滤网目数大于50目,
(4)料带做时效处理,放置在料带库,采取封装,温度控制在10℃-30℃ 之内,湿度控制在55±25%RH之间,放置时间不少于1天且不多于一年,
(5)将上述步骤得到的料带根据成品的尺寸和形状需要对生坯带作冲切等加工处理成生坯基片,
(6)将上述生坯基片在最高温度为1500℃~1750℃的环境下进行烧结处理,得到熟坯基片,其中:温度从常温到1750℃,时间为45小时左右,这是一个逐步升温和降温的过程,将陶瓷基片从生坯转变为熟坯,即烧结成品。
(7)将烧结成型后的熟坯基片进行表面喷砂处理,
将清洗干净的产品小心整理好后,用气枪吹去表面残留吸附的杂质,用干净的薄膜盖好。
(8)将经过上述步骤处理过的基片放置于最高温度为1200℃~1400℃的环境中进行抚平处理。
将得到的氧化铝荧光陶瓷材料用于LED照明产品。经检测,做成的LED支架,在相同设备和光源条件下,先用光直接照射得到光通量为14.656LM,在半透明陶瓷遮光照射得到光通量为2.985LM,利用荧光陶瓷遮光照射后得到光通量为5.552LM,说明荧光陶瓷比半透明陶瓷透光率高86%。
实施例4
1、备料
荧光粉30kg,氧化铝80kg,钙镁硅成分(氧化镁6kg、二氧化硅10.9kg和碳酸钙3.1kg),甲苯17.6kg,PVB 7kg,PEG0.6kg,W-S80:0.6kg。
荧光粉性能满足:激发波长430-480nm、发光峰值550-558nm、相对亮度95-105%及密度3.7g/cm3以上;所述的荧光粉D50为12-20μm,氧化铝粉体粒径满足:D50为1-6μm,钙镁硅成分粉体粒径满足:D50为1-6μm,
2、按下述步骤制备氧化铝荧光陶瓷材料:
(1)将钙镁硅成分粉料与氧化铝混合,混合粉料中第一次配料加入S80球磨4小时,第二次配料加入用甲苯先溶的PVB和PEG,加入荧光粉再次球磨时间48小时,得到流延浆料,
(2)测定温度和粘度后的流延浆料,浆料温度为35-45℃、粘度在2000-4000CPS,过滤后输入真空脱泡机进行脱泡处理,过滤采用180目的不锈钢过滤网,脱泡处理的时间≥2个小时,
(3)再次测定温度和粘度后通过过滤器进行流延制备料带,浆料温度为30-40℃、粘度在12000-17000CPS,过滤器的过滤网目数大于150目,
(4)料带做时效处理,放置在料带库,采取封装,温度控制在10℃-30℃ 之内,湿度控制在55±25%RH之间,放置时间不少于1天且不多于一年,
(5)将上述步骤得到的料带根据成品的尺寸和形状需要对生坯带作冲切等加工处理成生坯基片,
(6)将上述生坯基片在最高温度为1500℃~1750℃的环境下进行烧结处理,得到熟坯基片,其中:温度从常温到1750℃,时间为20小时左右,这是一个逐步升温和降温的过程,将陶瓷基片从生坯转变为熟坯,即烧结成品。
(7)将烧结成型后的熟坯基片进行表面喷砂处理,
将清洗干净的产品小心整理好后,用气枪吹去表面残留吸附的杂质,用干净的薄膜盖好。
(8)将经过上述步骤处理过的基片放置于最高温度为1200℃~1400℃的环境中进行抚平处理。
将得到的氧化铝荧光陶瓷材料用于LED照明产品。经检测,做成的LED支架,在相同设备和光源条件下,先用光直接照射得到光通量为14.656LM,在半透明陶瓷遮光照射得到光通量为2.985LM,利用荧光陶瓷遮光照射后得到光通量为5.6118LM,说明荧光陶瓷比半透明陶瓷透光率高88%。
Claims (10)
1.一种氧化铝荧光陶瓷材料,其特征在于主要由按质量百分比计的70-99%的基料氧化铝和1-30%的钙镁硅成分添加荧光粉经流延法制坯、再经烧结而成,其中所述的钙镁硅成分是指氧化镁或滑石粉与二氧化硅及碳酸钙的混合物,所述的荧光粉添加量以氧化铝和钙镁硅成分总质量计为10-30%但不等于10%。
2. 根据权利要求1所述的一种氧化铝荧光陶瓷材料,其特征在于,所述的荧光粉性能满足:激发波长430-480nm、发光峰值550-558nm、相对亮度85-90%及密度3.7g/cm3以上。
3. 根据权利要求1所述的一种氧化铝荧光陶瓷材料,其特征在于,所述的荧光粉D50为5-20μm、氧化铝粉体粒径满足:D50为1-6μm、钙镁硅成分粉体粒径满足:D50为1-6μm。
4.一种氧化铝荧光陶瓷材料的制备方法,其特征在于包括如下步骤:
(1)按照质量百分比70-99%的基料氧化铝和1-30%的钙镁硅成分备料,将氧化铝和钙镁硅成分混合,混合粉料中加入部分分散剂进行球磨处理,然后加入溶剂先溶的粘结剂和余量分散剂,再加入荧光粉再次进行球磨处理,得到流延浆料,其中:分散剂的加入量以钙镁硅成分与氧化铝混合粉料质量计为0.1-1%,溶剂加入量以钙镁硅成分与氧化铝混合粉料质量计为15-45%,粘结剂加入量以钙镁硅成分与氧化铝混合粉料质量计为2-10%;所述的钙镁硅成分是指氧化镁或滑石粉与二氧化硅及碳酸钙的混合物,
(2)测定温度和粘度后的流延浆料,过滤后输入真空脱泡机进行脱泡处理,
(3)再次测定温度和粘度后通过过滤器进行流延制备料带,
(4)料带做时效处理,温度控制在10℃-30℃ 之内,湿度控制在55±25%RH之间,放置时间1不多于一年,
(5)将上述步骤得到的料带根据需要加工处理成生坯基片,
(6)将上述生坯基片在最高温度为1500℃~1750℃的环境下进行烧结处理,得到熟坯基片,其中:温度从常温到1750℃,时间为10-45小时,
(7)将烧结成型后的熟坯基片进行表面喷砂处理,
(8)将经过上述步骤处理过的基片放置于最高温度为1200℃~1400℃的环境中进行抚平处理。
5.根据权利要求4所述的一种氧化铝荧光陶瓷材料的制备方法,其特征在于所述的荧光粉性能满足:激发波长430-480nm、发光峰值550-558nm、相对亮度95-105%及密度3.7g/cm3以上;所述的荧光粉D50为5-20μm、氧化铝粉体粒径满足:D50为1-6μm、钙镁硅成分粉体粒径满足:D50为1-6μm。
6.根据权利要求4所述的一种氧化铝荧光陶瓷材料的制备方法,其特征在于所述的溶剂采用甲苯或酒精;粘结剂采用PVB和PEG;分散剂采用W-S80。
7.根据权利要求4所述的一种氧化铝荧光陶瓷材料的制备方法,其特征在于所述的球磨处理的时间两次一共为10-80小时。
8.根据权利要求4所述的一种氧化铝荧光陶瓷材料的制备方法,其特征在于所述的步骤(2)中测定温度和粘度,应满足浆料温度为20-50℃、粘度在3000-20000CPS之间,过滤采用120目~500目的不锈钢过滤网,脱泡处理的时间≥2个小时;步骤(3)中再次测定温度和粘度,应满足浆料温度为20-45℃、粘度在5000-30000CPS之间,过滤器的过滤网目数大于50目。
9. 根据权利要求4所述的一种氧化铝荧光陶瓷材料的制备方法,其特征在于所述的步骤(5)中根据需要加工处理是指根据成品的尺寸和形状需要对生坯带加工处理。
10. 根据权利要求1-3之一所述的一种氧化铝荧光陶瓷材料在照明材料中的应用,其特征在于,所述照明材料包括LED、COB。
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