CN117024129A - 一种铬掺杂二硅酸镧陶瓷的制备方法 - Google Patents
一种铬掺杂二硅酸镧陶瓷的制备方法 Download PDFInfo
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- XVZQXGDGTFEANZ-UHFFFAOYSA-N lanthanum(3+);trioxido(trioxidosilyloxy)silane Chemical compound [La+3].[La+3].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] XVZQXGDGTFEANZ-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000000919 ceramic Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000011651 chromium Substances 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 27
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 21
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 229910017563 LaCrO Inorganic materials 0.000 claims abstract description 15
- 230000008569 process Effects 0.000 claims abstract description 11
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
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- 239000006082 mold release agent Substances 0.000 claims 3
- 150000002500 ions Chemical class 0.000 abstract description 4
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- 230000001105 regulatory effect Effects 0.000 abstract description 2
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- 241000579895 Chlorostilbon Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明公开了一种铬掺杂二硅酸镧陶瓷的制备方法，采用不同原料配比的LaCrO3和SiO2粉末，利用放电等离子烧结技术在1300～1500℃下直接制备铬掺杂的La2Si2O7陶瓷。本发明利用LaCrO3与SiO2粉末通过放电等离子技术制备铬掺杂二硅酸镧陶瓷块材，与现有制备方法相比，有效降低烧结温度，缩短制备周期且工艺简单。另外，本发明可通过改变原料配比来调控Cr离子的掺杂位置，进而改变二硅酸镧的性质，使其满足不同的应用需求，加强其工业生产和应用。本发明制备的铬掺杂的二硅酸镧陶瓷具有良好的高温相稳定性、较高的显微硬度和较小的断裂韧性，其力学性能随原料配比差异而发生改变。
Description
技术领域
本发明属于无机非金属材料制备技术领域，具体涉及一种铬掺杂二硅酸镧陶瓷的制备方法。
背景技术
二硅酸镧陶瓷(La2Si2O7)是一种具有良好绝缘性和高温稳定性的陶瓷材料，其具有较高的硬度、较低的介电常数、良好的机械强度和优异的热稳定性能，可以在高温高压、较恶劣的环境下使用。由于其性能优异，被广泛应用于微波电子学、光电子学、传感器、生物技术、航空航天等领域，其中，它可以作为微波陶瓷元器件、高温导电介质、高压绝缘体、气敏元件、光学陶瓷和生物医学器械等材料。
目前关于La2Si2O7陶瓷的制备方法，主要有固相法、溶胶-凝胶法、热分解法和液相共沉淀法等方法，而这些方法存在工艺繁琐、生产成本高、产品纯度低等不足，进而限制了其工业生产和应用。比如固相法主要将SiO2和La2O3粉末按照化学计量比例混合均匀，在高温、氧气气氛下进行热处理，由于高温下原料的化学反应比较激烈，可能会出现粉末团聚、结块等问题，导致纯度较低；溶胶凝胶法将稀释的LaCl3和TEOS(四乙氧基硅烷)混合，将凝胶热处理后得到产品粉末，虽纯度较高，但成本较高，工艺时间长，且过程中可能会对人体健康有害；热分解法是将La(NO3)3和Si(OEt)4混合，蒸发干燥后在空气气氛下热处理，经过多次煅烧和研磨后得到La2Si2O7粉末，但存在高能耗、制备纯度不高等不足；共沉淀法以La(NO3)3和Si(NO3)4为原料，在碱性环境下进行共沉淀反应，得到沉淀后经过水洗、过滤、干燥、煅烧等步骤得到粉末产品，整个过程繁杂且周期长。
发明内容
由于二硅酸镧陶瓷的现有制备工艺存在些许不足，本发明提供一种有效降低烧结温度，缩短制备周期且工艺简单的铬掺杂二硅酸镧陶瓷的制备方法。
为了实现上述目的，本发明采用以下技术方案：
一种铬掺杂二硅酸镧陶瓷的制备方法，包括以下步骤：
(1)将LaCrO3和SiO2原料粉末的混合；
(2)将研磨后的粉末倒入模具中，并进行烧结；
烧结过程中全程真空处理，并施加30-45MPa的轴向压力；先以80-120℃/min的升温速率升温至1300-1500℃，然后保温≥5min后开始降温。
特别的，步骤(1)中，所述LaCrO3和SiO2的摩尔比为0.5-1.55:1。
步骤(1)中，所述LaCrO3中位粒径为0.4-0.6μm。
步骤(1)中，所述SiO2为纳米SiO2。
特别的，步骤(2)中，利用放电等离子烧结炉烧结。
步骤(2)中，降温时减少放电等离子烧结炉的输出电流直到输出电流为0，然后利用冷水辅助降温。
步骤(2)中，烧结前，模具内壁涂抹脱模剂，脱模剂优选为BN脱模剂步骤(2)中，烧结前，在模具内放置碳纸，阻隔粉末与模具粘结。
与现有技术相比，本发明的有益效果为：
(1)本发明首次使用LaCrO3与SiO2粉末通过放电等离子技术制备铬掺杂二硅酸镧陶瓷块材，与现有制备方法相比，有效降低烧结温度，缩短制备周期且工艺简单。本发明通过改变原料配比可调控Cr离子的掺杂位置，La/Si原料比小于1时，Cr离子更容易进入La位，引起晶格畸变，影响其结构和形貌；La/Si原料比大于1时，Cr离子更容易进入Si位，改变其导电等性质。因此，可根据具体用途和性质需求来改变原料配比进而制备不同Cr掺杂位置的La2Si2O7陶瓷；使其满足不同的应用需求，加强其工业生产和应用。
(2)本发明制备的铬掺杂的二硅酸镧陶瓷具有良好的高温相稳定性、较高的显微硬度和较小的断裂韧性，其力学性能随原料配比差异而发生改变，当LaCrO3/SiO2原料摩尔配比为1.1-1.55时，其体积密度为为4.85-5.39g/cm3,显微硬度为8.22-9.23GPa，断裂韧性为2.24-2.80MPa·m1/2。
附图说明
图1本发明中制备的铬掺杂二硅酸镧的显微形貌。
图2本发明中不同原料配比的铬掺杂二硅酸镧的XRD图谱。
图3本发明中不同原料配比的铬掺杂二硅酸镧的体积密度。
图4本发明中不同原料配比的铬掺杂二硅酸镧的显微硬度。
图5本发明中不同原料配比的铬掺杂二硅酸镧的断裂韧性。
具体实施方式
为了更好地理解本发明，下面结合具体实施例对本发明作进一步的描述，其中实施例中使用的术语是为了描述特定的具体实施方案，不构成对本发明保护范围的限制。
实施例1：
本实施例中一种铬掺杂二硅酸镧陶瓷的制备方法如下：
步骤1：LaCrO3和SiO2原料粉末的混合
首先，将LaCrO3粉末和SiO2粉末按摩尔比1.1:1的比例进行称重，以无水乙醇为介质经行星式球磨机以转速500r/min球磨0.5h，使两种粉末混合均匀；接着将混合粉末置于鼓风干燥箱90℃干燥12h，待干燥结束后通过玛瑙研钵将混合粉末再次研磨0.5h。
其中LaCrO3粉末的中位粒径为0.5μm；SiO2粉末为纳米级。
步骤2：铬掺杂二硅酸镧的制备
称取上述研磨后的混合粉末，将混合粉末倒入石墨模具中，其中模具内壁涂抹BN脱模剂和粉末与石墨压头间使用碳纸阻隔，将石墨模具置于放电等离子烧结炉中抽真空，并施加30MPa的轴向压力。
先以100℃/min的升温速率升温至1300℃，烧结过程保持真空，然后保温5min后开始降温，通过减小输出电流缓慢降温以达到减小热应力的目的，随后在冷水机的辅助下降温至室温，得到翠绿色的二硅酸镧陶瓷。
实施例2：
本实施例中一种铬掺杂二硅酸镧陶瓷的制备方法如下：
步骤1：LaCrO3和SiO2原料粉末的混合
首先，将LaCrO3粉末和SiO2粉末按摩尔比1.55:1的比例进行称重，以无水乙醇为介质经行星式球磨机以转速500r/min球磨0.5h，使两种粉末混合均匀；接着将混合粉末置于鼓风干燥箱90℃干燥12h，待干燥结束后通过玛瑙研钵将混合粉末再次研磨0.5h。
其中LaCrO3粉末的中位粒径为0.5μm；SiO2粉末为纳米级。
步骤2：铬掺杂二硅酸镧的制备
称取上述研磨后的混合粉末，将混合粉末倒入石墨模具中，其中模具内壁涂抹BN脱模剂和粉末与石墨压头间使用碳纸阻隔，将石墨模具置于放电等离子烧结炉中抽真空，并施加30MPa的轴向压力。
具体烧结工艺如下：先以100℃/min的升温速率升温至1500℃，烧结过程保持真空，然后保温5min后开始降温，通过减小输出电流缓慢降温以达到减小热应力的目的，随后在冷水机的辅助下降温至室温，得到翠绿色的二硅酸镧陶瓷。
实施例3
与实施例1类似，不同点在于，LaCrO3和SiO2的摩尔比为1.25:1。
实施例4
与实施例1类似，不同点在于，LaCrO3和SiO2的摩尔比为1.40:1。
实验结果
经检测，实施例1制备的铬掺杂的二硅酸镧陶瓷为纯相，如图1所示；XRD图谱向小角度方向发生些许偏移，如图2所示；表明Cr掺杂在了Si位，其体积密度为4.86g/cm3，显微硬度为8.22GPa，断裂韧性为2.24MPa·m1/2。
实施例2制备的铬掺杂的二硅酸镧陶瓷仍为纯相，XRD图谱向小角度方向发生较多偏移，如图2所示；说明随着LaCrO3/SiO2原料摩尔比增大，更多的Cr元素掺杂在了Si位，同时其体积密度增大，值为5.39g/cm3，力学强度也进一步提高，显微硬度为8.95GPa，断裂韧性为2.80MPa·m1/2。
实施例3、实施例4的二硅酸镧陶瓷仍为纯相；不同比例下的XRD图谱如图2所示；体积密度如图3所示、显微硬度如图4所示、断裂韧性如图5所示；可见随着配比的笔筒，其力学性能有着相应的变化，但其变化为非线性相关。
上述详细说明是针对本发明其中之一可行实施例的具体说明，该实施例并非用以限制本发明的专利范围，凡未脱离本发明所为的等效实施或变更，均应包含于本发明技术方案的范围内。
Claims (9)
1.一种铬掺杂二硅酸镧陶瓷的制备方法，其特征在于，包括以下步骤：
(1)将LaCrO3和SiO2原料粉末的混合；
(2)将研磨后的粉末倒入模具中，并进行烧结；
烧结过程中全程真空处理，并施加30-45MPa的轴向压力；先以80-120℃/min的升温速率升温至1300-1500℃，然后保温≥5min后开始降温。
2.根据权利要求1所述的铬掺杂二硅酸镧陶瓷的制备方法，其特征在于，步骤(1)中，所述LaCrO3和SiO2的摩尔比为0.5-1.55:1。
3.根据权利要求1所述的铬掺杂二硅酸镧陶瓷的制备方法，其特征在于，步骤(1)中，所述LaCrO3中位粒径为0.4-0.6μm。
4.根据权利要求1所述的铬掺杂二硅酸镧陶瓷的制备方法，其特征在于，步骤(1)中，所述SiO2为纳米SiO2。
5.根据权利要求1所述的铬掺杂二硅酸镧陶瓷的制备方法，其特征在于，步骤(2)中，利用放电等离子烧结炉烧结。
6.根据权利要求5所述的铬掺杂二硅酸镧陶瓷的制备方法，其特征在于，步骤(2)中，降温时减少放电等离子烧结炉的输出电流直到输出电流为0，然后利用冷水辅助降温。
7.根据权利要求1所述的铬掺杂二硅酸镧陶瓷的制备方法，其特征在于，步骤(2)中，烧结前，模具内壁涂抹脱模剂。
8.根据权利要求7所述的铬掺杂二硅酸镧陶瓷的制备方法，其特征在于，步骤(2)中，所述脱模剂为BN脱模剂。
9.根据权利要求1所述的铬掺杂二硅酸镧陶瓷的制备方法，其特征在于，步骤(2)中，烧结前，在模具内放置碳纸，阻隔粉末与模具粘结。
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