CN106032323B - 一种以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法 - Google Patents
一种以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法 Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 133
- 239000000919 ceramic Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910010038 TiAl Inorganic materials 0.000 title 1
- 239000002994 raw material Substances 0.000 claims abstract description 40
- 238000005245 sintering Methods 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000000227 grinding Methods 0.000 claims abstract description 14
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 238000009837 dry grinding Methods 0.000 claims abstract description 4
- 239000010936 titanium Substances 0.000 claims description 45
- 239000004615 ingredient Substances 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000003801 milling Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
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- 238000001816 cooling Methods 0.000 description 5
- 229960000935 dehydrated alcohol Drugs 0.000 description 5
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- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- OQPDWFJSZHWILH-UHFFFAOYSA-N [Al].[Al].[Al].[Ti] Chemical compound [Al].[Al].[Al].[Ti] OQPDWFJSZHWILH-UHFFFAOYSA-N 0.000 description 1
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- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 229910021324 titanium aluminide Inorganic materials 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，具体为一种以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法。采用TiAl粉、TiC粉为反应原材料，原料的摩尔比为n(TiAl)：n(TiC)＝1:(0.8～1.0)。首先将TiAl和TiC粉末湿法球磨为浆料。将浆料进行烘干和真空干燥，干燥后的粉体再进行干磨。将干磨后的粉体成型并装入包套进行热等静压烧结或装入石墨模具进行真空热压烧结。烧结后的材料先机加工去除表面可能的污染物，然后经破碎、筛分、酸洗、干燥等工艺得到粉体。采用TiAl粉为原料减少了中间反应步骤，获得材料品质好，纯度高达99wt％，可作为表面工程、增强相、新型二元层状材料前驱体等材料使用。
Description
技术领域
本发明涉及陶瓷材料领域，具体为一种以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法。
背景技术
作为一种三元层状可加工陶瓷，Ti2AlC陶瓷具有MAX相族材料的结构和特点。MAX相的结构一般可描述为：在结晶密堆的M原子钟插入纯A原子层，X 原子填入M组成的八面体间隙内。对Ti2AlC陶瓷而言M为Ti原子，A为Al原子，X为C原子。这种结构使MAX材料同时具有共价键、金属键、离子键，兼具陶瓷和金属的性质，如：导电、化学稳定性好、熔点高特点。具体到Ti2AlC陶瓷而言，具有高的力学强度，良好的抗氧化性，良好的抗化学和热腐蚀性，良好的抗热冲击性，高温下抗损伤和一定的自修护能力，同时具有传统陶瓷所不具备的可加工性。上述特点使得Ti2AlC陶瓷在最近十几年内成为研究的热点。这些热点不仅包括了Ti2AlC块体材料作为结构材料的应用，同时在表面工程领域和作为新型二元层状材料MXene的原料也备受关注，但是在新领域的应用需要纯度极高不含其它反应残留物的粉体材料。然而追求快速，大量合成该材料的粉体的方法如自蔓延反应、放电等离子烧结、微波烧结等都含有一定的反应物残留或其他 MAX相产物。以前的文献和专利中用于合成Ti2AlC材料的原料一般大于等于3 种，导致中间反应过程复杂，烧结时间长，烧结过程易产生成分挥发等。因此，获得纯度极高的MAX相粉体同时大量经济的合成一直没法同时得到满足。
发明内容
本发明的目的在于提供一种以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法，为了解决现有制备Ti2AlC粉体材料方法上存在反应原料多，反应中间复杂，反应无法精确控制，工艺复杂时间长，以及制备出的Ti2AlC粉体纯度不够，难以满足新的应用领域的需要等问题，Ti2AlC粉体材料的纯度高达99wt％，且易于工业化生产。
本发明的技术方案如下：
一种以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法，采用TiAl粉、TiC粉为反应原材料，原料的摩尔比为n(TiAl)：n(TiC)＝1:(0.8～1.0)。
所述的以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法，具体步骤如下：
(1)配料：所采用TiAl粉、TiC粉体原料经过湿磨、浆料烘干和干磨；
(2)成型：将配料好的粉体原料用压机和模具干压成型，并装入纯钛包套或直接装入石墨模具中施加5MPa以下压力；
(3)烧结：将装入纯钛包套的粉体进行热等静压工艺烧结，或者装入石墨模具的粉体进行热压烧结；
(4)机加工：将烧结获得的Ti2AlC块体机加工去除含杂质的表面，然后用破碎机进行破碎；
(5)磨粉：将破碎后的块体进行细磨获得微米尺度的粉体；
(6)粉体后处理：将细磨粉进行筛分、酸洗、干燥最终得到所需的粉体。
所述的以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法，在X-射线衍射表征下纯度为99wt％以上的Ti2AlC粉体，在X-射线衍射检测下TiC、钛铝化合物、其它MAX相陶瓷产物为1wt％以下。
所述的以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法，烧结过程热等静压烧结在真空或氩气气氛下，烧结压力在50～200MPa，烧结温度在500～1500℃；热压烧结气氛在真空或氩气气氛下，烧结压力在10～50MPa，烧结温度在550～ 1550℃。
所述的以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法，磨粉过程用圆盘粉碎机磨粉、雷蒙磨磨粉、气流磨磨粉或球磨磨粉。
所述的以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法，粉体后处理过程中，粉体酸洗采用质量分数1％～15％的盐酸或硫酸进行清洗，然后去离子水洗净。
本发明具有以下优点及有益效果：
1.本发明直接采用TiAl粉体为反应的原料粉体，避免在热压烧结过程中低熔点组元沸腾挥发影响成分稳定。同时，避免中间反应放热导致的烧结过程中模具或包套易被破坏和烧结过程工艺难度高的问题。
2.本发明合成制备的Ti2AlC粉体纯度达99wt％，可满足用于作为表面工程的材料、增强相材料、新型二元层状材料前驱体等。
3.本发明采用的工艺步骤都是成熟的工艺和设备体系，但原料减少为两种，且烧结难度降低，易于掌握，便于推广和大规模生产。
4.本发明通过选择不同的粉体加工设备和参数最终获得的粉体产品粒度可调，粉体能满足多种使用要求。
附图说明
图1为实施例1后获得的粉体X-射线衍射图谱，粉体中Ti2AlC含量达到 99wt％。图中，横坐标2Theta为衍射角(deg.)，纵坐标Intensity为强度。
图2为实施例1后获得的Ti2AlC粉体粒度分布，粉体粒度中径在32微米左右。图中，横坐标Particle Size为粒度(微米)，纵坐标Volume为体积百分含量 (％)。
图3为实施例2后获得的热喷涂Ti2AlC粉体，粉体中径在70微米左右。图中，横坐标Particle Size为粒度(微米)，纵坐标Volume为体积百分含量(％)。
图4为实施例2后获得的Ti2AlC冷喷涂粉体，粉体粒度中径在25微米左右。图中，横坐标Particle Size为粒度(微米)，纵坐标Volume为体积百分含量(％)。
图5为实施例4后获得的Ti2AlC粉体粒度，粉体中径在0.3微米左右。图中，横坐标Particle Size为粒度(微米)，纵坐标Volume为体积百分含量(％)。
图6和图7为实施例2后获得的中径在25微米的粉体的电子扫描图像照片。
具体实施方式
在具体实施过程中，本发明提供的Ti2AlC粉体采用TiAl粉、TiC粉体为原料，其中TiAl粉采用化学成分为Ti50Al50的粉体，TiAl粉纯度99wt％，TiC粉体纯度99.8wt％，原料的摩尔比为n(TiAl)：n(TiC)＝1:(0.9～1.0)。首先将TiAl 粉和TiC粉搅拌混合均匀，将搅拌混合均匀的粉末加入酒精(无水乙醇)进行湿法球磨20～40分钟，形成混合更加均匀的原料浆料。将浆料进行烘干、真空干燥或鼓风干燥，将干燥后获得的粉体用球磨设备进行干磨5～15分钟。将干磨后的粉体成型，并装入钛合金包套中进行热等静压烧结或装入石墨模具中进行真空热压烧结。烧结后的材料先机加工去除表面可能的污染物，然后进行破碎、筛分、酸洗、干燥等工艺得到粉体。
下面结合附图和实施例对本发明作进一步详细说明，但不限定本发明。
实施例1
原料粉末按摩尔比n(TiAl)：n(TiC)＝1:0.9配料，原料共计4公斤，混合均匀，加入无水乙醇3L，装入10L的振动球磨装置，振动频率50Hz，振幅5mm，球磨时间30分钟。将球磨后的浆料倒出，放入鼓风干燥箱内低温干燥，待酒精含量降至85wt％以下时，加热烘干。烘干后的粉体再放入振动球磨机用相同参数干磨10分钟，得到混合均匀的粉体原料。将原料装入直径为150mm的石墨模具放入热压烧结炉，先施加5MPa压力，当真空度达到10-3Pa时开始升温再次加压，升温至1400℃，压力30MPa，保温保压2小时然后随炉冷却。将获得的块体用车床车去外表3mm，用液压机压碎，将压碎后的块体用颚式破碎机破碎为不大于 10mm的小块。将进行10次破碎工艺获得40公斤Ti2AlC小块用小型雷蒙磨机进行细磨获得粒度中径在32微米的粉体，粒度分布如图2所示。然后对粉体用质量分数为10％的盐酸进行酸洗，再用去离子水洗净，然后进行真空干燥。最终获得纯度为99wt％，成分如图1所示，中径在32微米的Ti2AlC粉体。
实施例2
原料粉末按摩尔比n(TiAl)：n(TiC)＝1:0.95配料，原料共计4公斤，混合均匀，加入无水乙醇3L，装入10L的搅拌球磨装置，搅拌转速250r/min，球磨时间30分钟。将球磨后的浆料倒出，放入鼓风干燥箱内低温干燥，待酒精含量降至 90wt％以下时，加热烘干。烘干后的粉体再放入搅拌球磨机用相同参数干磨10分钟，得到混合均匀的粉体原料。将配料好的粉体原料用液压机和不锈钢模具干压成型。将10次配料和成型和块体装入直径为100mm、长200mm的纯钛包套中，将这批包套放入大型热等静压烧结炉，先抽真空后通入氩气保护，升温至1350℃压力100MPa，保温保压4小时然后随炉冷却。将获得的块体用车床车去外表3mm，用液压机压碎，将压碎后的块体用颚式破碎机破碎为不大于10mm的小块。破碎获得的小块用小型圆盘粉碎磨机进行细磨获得粒度中径在50微米的粉体，然后对粉体用质量分数为8％的盐酸进行酸洗，再用去离子水洗净，然后进行真空干燥和筛分。最终获得纯度为99wt％的Ti2AlC粉体，筛分后粒度分布如图3所示中径为70微米的粉体可用于超音速火焰喷涂，粒度分布如图4中径为25微米的粉体，电子扫描照片见图6和图7，该粉体可用作冷喷涂粉体。
实施例3
原料粉末按摩尔比n(TiAl)：n(TiC)＝1:0.925配料，原料共计4公斤，混合均匀，加入无水乙醇3L，装入10L的振动球磨装置，振动频率50Hz，振幅5mm，球磨时间30分钟。将球磨后的浆料倒出，放入鼓风干燥箱内低温干燥，待酒精含量降至90wt％以下时，加热烘干。烘干后的粉体再放入振动球磨机用相同参数干磨10分钟，得到混合均匀的粉体原料。将原料装入直径为120mm的石墨模具放入热压烧结炉，先施加5MPa压力，当真空度达到10-3Pa时通入氩气并开始升温再次加压，升温至1400℃，压力15MPa并保温保压2小时然后随炉冷却。升温至1400℃保温2小时然后随炉冷却。将获得的块体用车床车去外表3mm，用液压机压碎，将压碎后的块体用颚式破碎机破碎为不大于10mm的小块。破碎获得的小块用小型圆盘粉碎磨机进行细磨获得粒度中径在50微米的粉体，然后用气流磨进行进一步粉碎，获得粒度中径在2～3微米的细小粉体。对粉体用质量分数为 10％的盐酸进行酸洗，再用去离子水洗净，然后用滤膜进行真空抽滤。抽滤后再进行烘干，最终获得纯度为99wt％的Ti2AlC中径粒度在2～3微米的粉体。
实施例4
原料粉末按摩尔比n(TiAl)：n(TiC)＝1:0.96配料，原料共计4公斤，混合均匀，加入无水乙醇3L，装入10L的搅拌球磨装置，搅拌转速250r/min，球磨时间30分钟。将球磨后的浆料倒出，放入鼓风干燥箱内低温干燥，待酒精含量降至 90wt％以下时，加热烘干。烘干后的粉体再放入搅拌球磨机用相同参数干磨10分钟，得到混合均匀的粉体原料。将配料好的粉体原料用液压机和不锈钢模具干压成型。成型得到原料装入直径为38mm长80mm的纯钛包套中，将这批包套放入小型热等静压烧结炉，先抽真空后通入氩气保护，升温至1350℃压力150MPa，保温保压4小时然后随炉冷却。将获得的块体用车床车去外表3mm，用高速钻床破碎为小块和粉末。破碎获得的小块及粉末用小型圆盘粉碎机进行细磨获得粒度中径在50微米的粉体，然后将粉体装入大型行星球磨装置细磨。然后对粉体用质量分数为12％的盐酸进行酸洗，再用去离子水洗净，然后用滤膜进行真空抽滤，抽滤后再进行烘干。最终获得纯度为99wt％，粒度分布如图5所示中径为0.3微米的Ti2AlC粉体。
实施例结果表明，本发明制备的粉体材料纯度极高，组织致密，反应原材料减少为两种，采用TiAl粉为原料减少了中间反应步骤，获得材料品质好，纯度高达99wt％以上。
Claims (4)
1.一种以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法，其特征在于，采用TiAl粉、TiC粉为反应原材料，原料的摩尔比为n(TiAl)：n(TiC)＝1:(0.8～1.0)，具体步骤如下：
(1)配料：首先将TiAl粉和TiC粉搅拌混合均匀，将搅拌混合均匀的粉末加入酒精进行湿法球磨20～40分钟，形成混合更加均匀的原料浆料；将浆料进行烘干、真空干燥或鼓风干燥，将干燥后获得的粉体用球磨设备进行干磨5～15分钟；
(2)成型：将配料好的粉体原料用压机和模具干压成型，并装入纯钛包套或直接装入石墨模具中施加5MPa以下压力；
(3)烧结：将装入纯钛包套的粉体进行热等静压工艺烧结，或者装入石墨模具的粉体进行热压烧结；
(4)机加工：将烧结获得的Ti2AlC块体机加工去除含杂质的表面，然后用破碎机进行破碎；
(5)磨粉：将破碎后的块体进行细磨获得微米尺度的粉体；
(6)粉体后处理：将细磨粉进行筛分、酸洗、干燥最终得到所需的粉体；
在X-射线衍射表征下纯度为99wt％以上的Ti2AlC粉体，在X-射线衍射检测下TiC、钛铝化合物、其它MAX相陶瓷产物为1wt％以下。
2.根据权利要求1所述的以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法，其特征在于，烧结过程热等静压烧结在真空或氩气气氛下，烧结压力在50～200MPa，烧结温度在500～1500℃；热压烧结气氛在真空或氩气气氛下，烧结压力在10～50MPa，烧结温度在550～1550℃。
3.根据权利要求1所述的以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法，其特征在于，磨粉过程用圆盘粉碎机磨粉、雷蒙磨磨粉、气流磨磨粉或球磨磨粉。
4.根据权利要求1所述的以TiAl粉体为原料的Ti2AlC陶瓷粉体制备方法，其特征在于，粉体后处理过程中，粉体酸洗采用质量分数1％～15％的盐酸或硫酸进行清洗，然后去离子水洗净。
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| CN103601498A (zh) * | 2013-10-21 | 2014-02-26 | 陕西科技大学 | 一种Ti3AlC2 陶瓷粉料的制备方法 |
| CN105218100A (zh) * | 2015-10-12 | 2016-01-06 | 陕西科技大学 | 一种低温制备Ti2AlC陶瓷材料的方法 |
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