CN106810255A - A kind of strontium cerate semitransparent ceramics and preparation method thereof - Google Patents
A kind of strontium cerate semitransparent ceramics and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 99
- XMHIUKTWLZUKEX-UHFFFAOYSA-N hexacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O XMHIUKTWLZUKEX-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 28
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims abstract description 54
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000011259 mixed solution Substances 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 24
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 21
- 239000011858 nanopowder Substances 0.000 claims abstract description 21
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 14
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229960002303 citric acid monohydrate Drugs 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 18
- 238000007731 hot pressing Methods 0.000 claims description 17
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 12
- 238000001272 pressureless sintering Methods 0.000 claims description 11
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000002834 transmittance Methods 0.000 abstract description 14
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 7
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 6
- 238000011160 research Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
一种铈酸锶半透明陶瓷及其制备方法,先将硝酸锶和六水硝酸铈溶于去离子水中,进行磁力搅拌后,加入硝酸锂和一水柠檬酸,再进行磁力搅拌,最后加入碱调节pH值至6~7;再对上述混合溶液进行蒸发结晶,形成凝胶,将凝胶置于干燥箱中进行干燥、研磨、最后进行退火,制备得到Sr2CeO4:Li+微纳米粉末;再在Sr2CeO4:Li+微纳米粉末中加入无水乙醇,进行研磨,干燥,制备得到Sr2CeO4:Li+陶瓷粉体;最后进行真空热压烧结,再在空气气氛下无压烧结,制备得到Sr2CeO4半透明陶瓷。通过本发明制备得到的Sr2CeO4半透明陶瓷致密度高、透光率好、发光效率高。另外本发明的制备方法具有烧结温度低,成本低,易于操作等优点,适于Sr2CeO4透明陶瓷材料的工业化生产。
A strontium cerate translucent ceramic and a preparation method thereof, first dissolving strontium nitrate and cerium nitrate hexahydrate in deionized water, performing magnetic stirring, adding lithium nitrate and citric acid monohydrate, performing magnetic stirring, and finally adding alkali Adjust the pH value to 6~7; then evaporate and crystallize the above mixed solution to form a gel, place the gel in a drying oven for drying, grinding, and finally annealing to prepare Sr 2 CeO 4 :Li + micro-nano powder ; then add absolute ethanol to the Sr 2 CeO 4 : Li + micro-nano powder, grind and dry to prepare Sr 2 CeO 4 : Li + ceramic powder; Press and sinter to prepare Sr 2 CeO 4 translucent ceramics. The Sr 2 CeO 4 translucent ceramic prepared by the invention has high density, good light transmittance and high luminous efficiency. In addition, the preparation method of the present invention has the advantages of low sintering temperature, low cost, easy operation, etc., and is suitable for industrial production of Sr 2 CeO 4 transparent ceramic materials.
Description
技术领域technical field
本发明涉及陶瓷材料制备领域,尤其涉及一种铈酸锶半透明陶瓷及其制备方法。The invention relates to the field of preparation of ceramic materials, in particular to a strontium cerate translucent ceramic and a preparation method thereof.
背景技术Background technique
透明陶瓷是20世纪50年代末、60年代初发展起来的一类新型无机材料,不仅具有陶瓷固有的耐高温、耐腐蚀、高强度、高硬度等特点,还具有玻璃的光学性质。很多国家对透明陶瓷进行了深入研究,并开发出一系列不同用途的透明陶瓷,部分透明陶瓷的性能已经能与相应的单晶媲美。这些性能各异的透明陶瓷正逐步应用于激光、照明、医疗器械、军事以及国防等重要科技领域。Transparent ceramics are a new type of inorganic material developed in the late 1950s and early 1960s. They not only have the inherent characteristics of high temperature resistance, corrosion resistance, high strength, and high hardness of ceramics, but also have the optical properties of glass. Many countries have carried out in-depth research on transparent ceramics and developed a series of transparent ceramics with different uses. The performance of some transparent ceramics has been comparable to that of corresponding single crystals. These transparent ceramics with different properties are gradually being used in important scientific and technological fields such as laser, lighting, medical equipment, military and national defense.
铈酸锶(Sr2CeO4)是一种具有一维链状结构的新型蓝色发光材料,属于正交晶系,晶胞参数a=6.11897Å, b=10.3495 Å, c=3.5970 Å,色坐标x=0.198, y=0.292, 发射峰位于460-490nm,室温下经紫外、X射线或阴极射线激发能够产生较高的发光效率。自1998年Danielson等人首次报道该材料以来,迅速成为新的研究热点。近年来,人们对Sr2CeO4微纳米材料的合成、发光性能、掺杂发光等进行了深入研究,并取得了较大的进展。但是迄今为止还未见Sr2CeO4透明陶瓷的相关报道,主要是因为Sr2CeO4为一维结构材料,对光的透射存在各向异性,陶瓷中的晶界对光有强散射;另外提高烧结温度会出现SrCeO3等杂相,难以获得Sr2CeO4透明陶瓷。因此如何减少气孔和散射、提高致密度是Sr2CeO4多晶陶瓷透明的关键,这也是制约Sr2CeO4透明陶瓷研究发展的瓶颈。因此,亟需研究开发一种低成本、易操作的Sr2CeO4透明陶瓷的制备方法,将对Sr2CeO4基透明陶瓷在闪烁探测器、照明等领域具有很好的应用前景。Strontium cerate (Sr 2 CeO 4 ) is a new type of blue luminescent material with a one-dimensional chain structure, which belongs to the orthorhombic crystal system. Coordinates x=0.198, y=0.292, the emission peak is located at 460-490nm, and can produce higher luminous efficiency after being excited by ultraviolet, X-ray or cathode ray at room temperature. Since the material was first reported by Danielson et al. in 1998, it has rapidly become a new research hotspot. In recent years, people have carried out in-depth research on the synthesis, luminescent properties, and doped luminescence of Sr 2 CeO 4 micro-nano materials, and made great progress. However, there have been no related reports on Sr 2 CeO 4 transparent ceramics so far, mainly because Sr 2 CeO 4 is a one-dimensional structure material, and there is anisotropy in the transmission of light, and the grain boundaries in ceramics have strong light scattering; in addition Impurities such as SrCeO 3 will appear when the sintering temperature is increased, making it difficult to obtain Sr 2 CeO 4 transparent ceramics. Therefore, how to reduce porosity and scattering and increase density is the key to the transparency of Sr 2 CeO 4 polycrystalline ceramics, which is also the bottleneck restricting the research and development of Sr 2 CeO 4 transparent ceramics. Therefore, there is an urgent need to research and develop a low-cost, easy-to-operate method for preparing Sr 2 CeO 4 transparent ceramics, which will have good application prospects for Sr 2 CeO 4 -based transparent ceramics in scintillation detectors, lighting and other fields.
发明内容Contents of the invention
为解决上述技术问题,本发明第一方面提供了一种铈酸锶半透明陶瓷的制备方法,包括以下步骤:In order to solve the above technical problems, the first aspect of the present invention provides a method for preparing strontium cerate translucent ceramics, comprising the following steps:
(1)将硝酸锶和六水硝酸铈溶于去离子水中,进行磁力搅拌;(1) Dissolve strontium nitrate and cerium nitrate hexahydrate in deionized water, and perform magnetic stirring;
(2)在步骤(1)得到的混合溶液中加入硝酸锂和一水柠檬酸,进行磁力搅拌;(2) Add lithium nitrate and citric acid monohydrate to the mixed solution obtained in step (1), and perform magnetic stirring;
(3)在步骤(2)得到的混合溶液中加入碱调节pH值至6~7;(3) adding alkali to the mixed solution obtained in step (2) to adjust the pH value to 6~7;
(4)将步骤(3)得到的混合溶液进行蒸发结晶,形成凝胶;(4) Evaporate and crystallize the mixed solution obtained in step (3) to form a gel;
(5)将步骤(4)得到的凝胶置于干燥箱中进行干燥、研磨、最后进行退火,制备得到Sr2CeO4:Li+微纳米粉末;(5) Place the gel obtained in step (4) in a drying oven for drying, grinding, and finally annealing to prepare Sr 2 CeO 4 :Li + micro-nano powder;
(6)在步骤(5)得到的Sr2CeO4:Li+微纳米粉末中加入无水乙醇,进行研磨,干燥,制备得到Sr2CeO4:Li+陶瓷粉体;(6) Add absolute ethanol to the Sr 2 CeO 4 : Li + micro-nano powder obtained in step (5), grind and dry to prepare Sr 2 CeO 4 : Li + ceramic powder;
(7)将步骤(6)得到的Sr2CeO4:Li+陶瓷粉体先进行真空热压烧结,再在空气气氛下无压烧结,制备得到Sr2CeO4半透明陶瓷。(7) The Sr 2 CeO 4 : Li + ceramic powder obtained in step (6) is first subjected to vacuum hot-pressing sintering, and then pressureless sintering in an air atmosphere to prepare Sr 2 CeO 4 translucent ceramics.
其中,所述硝酸锶、硝酸铈和硝酸锂的摩尔比为100:40~60:1~25。Wherein, the molar ratio of strontium nitrate, cerium nitrate and lithium nitrate is 100:40~60:1~25.
其中,所述的碱可以是氨水、三乙胺、三乙烯二胺、四甲基乙二胺中的任意一种或是几种的混合。Wherein, the base may be any one or a mixture of ammonia water, triethylamine, triethylenediamine, and tetramethylethylenediamine.
其中,所述步骤(1)中,磁力搅拌的时间为10~30min。Wherein, in the step (1), the time for magnetic stirring is 10-30 minutes.
其中,所述步骤(2)中,磁力搅拌的时间为30~60min。Wherein, in the step (2), the magnetic stirring time is 30-60 minutes.
其中,所述步骤(4)中,蒸发结晶的温度为80~100℃,时间为1~4h。Wherein, in the step (4), the evaporation crystallization temperature is 80-100° C., and the time is 1-4 hours.
其中,所述步骤(5)中,Wherein, in the step (5),
干燥的温度为110~150℃,时间为10~15h;The drying temperature is 110~150℃, and the drying time is 10~15h;
研磨的时间为30~60min;Grinding time is 30~60min;
退火的温度为800~1000℃,时间为1.5~4h。The annealing temperature is 800~1000℃, and the time is 1.5~4h.
其中,所述步骤(6)中,Wherein, in the step (6),
研磨的时间为30~60min;Grinding time is 30~60min;
干燥的温度为120~200℃,时间为12~36h。The drying temperature is 120~200℃, and the drying time is 12~36h.
其中,所述步骤(7)中,Wherein, in the step (7),
真空热压烧结的温度为800~1200℃,压力为80~120MPa,时间为2~4h;The temperature of vacuum hot pressing sintering is 800~1200℃, the pressure is 80~120MPa, and the time is 2~4h;
空气气氛下无压烧结的温度为1000~1200℃,时间为10~15h。The temperature of pressureless sintering in air atmosphere is 1000~1200℃, and the time is 10~15h.
本发明第二方面提供了一种铈酸锶半透明陶瓷,所述铈酸锶半透明陶瓷按照上述任意一项制备方法制备得到。The second aspect of the present invention provides a strontium cerate translucent ceramic, and the strontium cerate translucent ceramic is prepared according to any one of the above preparation methods.
本发明的有益效果:Beneficial effects of the present invention:
本发明提供的制备Sr2CeO4半透明陶瓷的方法,通过采用硝酸锶、硝酸铈和硝酸锂作为原料反应制备得到Sr2CeO4:Li+陶瓷粉体,再以Sr2CeO4:Li+陶瓷粉体作为陶瓷原料,先后使用了真空热压烧结和空气气氛无压烧结的工艺,真空热压烧结有利于陶瓷快速致密化,空气气氛下无压烧结时Li+离子作为烧结助剂,有利于致密度和透光率的进一步提高,获得的Sr2CeO4半透明陶瓷致密度高、透光率好、发光效率高。另外现有技术中制备陶瓷的烧结温度通常都高于1200℃,而本发明提供的真空热压烧结和空气气氛下的无压烧结温度都低于1200℃。因此本发明提供的制备方法成本低,易于操作,适于工业化生产。In the method for preparing Sr 2 CeO 4 translucent ceramics provided by the present invention, Sr 2 CeO 4 : Li + ceramic powder is prepared by using strontium nitrate, cerium nitrate and lithium nitrate as raw materials, and then Sr 2 CeO 4 : Li + Ceramic powder is used as a ceramic raw material, and the processes of vacuum hot pressing sintering and air atmosphere pressureless sintering have been used successively. Vacuum hot pressing sintering is conducive to the rapid densification of ceramics. It is beneficial to the further improvement of density and light transmittance, and the obtained Sr 2 CeO 4 translucent ceramic has high density, good light transmittance and high luminous efficiency. In addition, the sintering temperature for preparing ceramics in the prior art is usually higher than 1200°C, while the vacuum hot pressing sintering and the pressureless sintering temperature in air atmosphere provided by the present invention are both lower than 1200°C. Therefore, the preparation method provided by the invention has low cost, is easy to operate, and is suitable for industrial production.
附图说明Description of drawings
为了更清楚地说明本发明的技术方案,下面将对实施方式中需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施方式,对应本领域的普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to illustrate the technical solution of the present invention more clearly, the accompanying drawings that need to be used in the implementation will be briefly introduced below. Obviously, the accompanying drawings in the following description are only some implementations of the present invention, corresponding to common As far as the skilled person is concerned, other drawings can also be obtained based on these drawings on the premise of not paying creative work.
图1为本发明实施例1所得铈酸锶半透明陶瓷实物照片。Fig. 1 is the photo of the strontium cerate translucent ceramic obtained in Example 1 of the present invention.
图2为本发明实施例2所得铈酸锶半透明陶瓷实物照片。Fig. 2 is a physical photo of strontium cerate translucent ceramic obtained in Example 2 of the present invention.
图3为本发明实施例1和2所得铈酸锶半透明陶瓷的发射光谱。Fig. 3 is the emission spectrum of strontium cerate translucent ceramics obtained in Examples 1 and 2 of the present invention.
具体实施方式detailed description
以下是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也视为本发明的保护范围。The following are preferred embodiments of the present invention. It should be pointed out that for those skilled in the art, without departing from the principle of the present invention, some improvements and modifications can also be made, and these improvements and modifications are also considered as the present invention. protection scope of the invention.
本发明提供了一种铈酸锶半透明陶瓷的制备方法,包括以下步骤:The invention provides a method for preparing strontium cerate translucent ceramics, comprising the following steps:
(1)将硝酸锶和六水硝酸铈溶于去离子水中,进行磁力搅拌;(1) Dissolve strontium nitrate and cerium nitrate hexahydrate in deionized water, and perform magnetic stirring;
(2)在步骤(1)得到的混合溶液中加入硝酸锂和一水柠檬酸,进行磁力搅拌;(2) Add lithium nitrate and citric acid monohydrate to the mixed solution obtained in step (1), and perform magnetic stirring;
(3)在步骤(2)得到的混合溶液中加入碱调节pH值至6~7;(3) adding alkali to the mixed solution obtained in step (2) to adjust the pH value to 6~7;
(4)将步骤(3)得到的混合溶液进行蒸发结晶,形成凝胶;(4) Evaporate and crystallize the mixed solution obtained in step (3) to form a gel;
(5)将步骤(4)得到的凝胶置于干燥箱中进行干燥、研磨、最后进行退火,制备得到Sr2CeO4:Li+微纳米粉末;(5) Place the gel obtained in step (4) in a drying oven for drying, grinding, and finally annealing to prepare Sr 2 CeO 4 :Li + micro-nano powder;
(6)在步骤(5)得到的Sr2CeO4:Li+微纳米粉末中加入无水乙醇,进行研磨,干燥,制备得到Sr2CeO4:Li+陶瓷粉体;(6) Add absolute ethanol to the Sr 2 CeO 4 : Li + micro-nano powder obtained in step (5), grind and dry to prepare Sr 2 CeO 4 : Li + ceramic powder;
(7)将步骤(6)得到的Sr2CeO4:Li+陶瓷粉体先进行真空热压烧结,再在空气气氛下无压烧结,制备得到Sr2CeO4半透明陶瓷。(7) The Sr 2 CeO 4 : Li + ceramic powder obtained in step (6) is first subjected to vacuum hot-pressing sintering, and then pressureless sintering in an air atmosphere to prepare Sr 2 CeO 4 translucent ceramics.
在本发明实施方式中,所述硝酸锶、硝酸铈和硝酸锂的摩尔比为100:40~60:1~25。In an embodiment of the present invention, the molar ratio of strontium nitrate, cerium nitrate and lithium nitrate is 100:40~60:1~25.
优选地,所述硝酸锶、硝酸铈和硝酸锂的摩尔比为100:50:5~15。Preferably, the molar ratio of strontium nitrate, cerium nitrate and lithium nitrate is 100:50:5-15.
进一步优选地,所述硝酸锶、硝酸铈和硝酸锂的摩尔比为100:50:6,100:50:8,100:50:10,100:50:12,100:50:14。Further preferably, the molar ratios of strontium nitrate, cerium nitrate and lithium nitrate are 100:50:6, 100:50:8, 100:50:10, 100:50:12, 100:50:14.
在本发明实施方式中,所述的碱可以是氨水、三乙胺、三乙烯二胺、四甲基乙二胺中的任意一种或是几种的混合。In the embodiment of the present invention, the base may be any one or a mixture of ammonia water, triethylamine, triethylenediamine and tetramethylethylenediamine.
在本发明实施方式中,In the embodiment of the present invention,
所述步骤(1)中,磁力搅拌的时间为10~30min。In the step (1), the magnetic stirring time is 10-30 minutes.
所述步骤(2)中,磁力搅拌的时间为30~60min。In the step (2), the magnetic stirring time is 30-60 minutes.
所述步骤(4)中,蒸发结晶的温度为80~100℃,时间为1~4h。In the step (4), the temperature for evaporative crystallization is 80-100° C., and the time is 1-4 hours.
所述步骤(5)中,In the step (5),
干燥的温度为110~150℃,时间为10~15h;The drying temperature is 110~150℃, and the drying time is 10~15h;
研磨的时间为30~60min;Grinding time is 30~60min;
退火的温度为800~1000℃,时间为1.5~4h。The annealing temperature is 800~1000℃, and the time is 1.5~4h.
所述步骤(6)中,In the step (6),
研磨的时间为30~60min;Grinding time is 30~60min;
干燥的温度为120~200℃,时间为12~36h。The drying temperature is 120~200℃, and the drying time is 12~36h.
所述步骤(7)中,In said step (7),
真空热压烧结的温度为800~1200℃,压力为80~120MPa,时间为2~4h;The temperature of vacuum hot pressing sintering is 800~1200℃, the pressure is 80~120MPa, and the time is 2~4h;
空气气氛下无压烧结的温度为1000~1200℃,时间为10~15h。The temperature of pressureless sintering in air atmosphere is 1000~1200℃, and the time is 10~15h.
实施例1Example 1
本发明提供的一种铈酸锶半透明陶瓷材料的制备方法,包括如下步骤:A kind of preparation method of strontium cerate translucent ceramic material provided by the invention comprises the following steps:
(1)将2.11g硝酸锶和2.17g六水硝酸铈溶于200mL去离子水中,进行磁力搅拌15min;(1) Dissolve 2.11g of strontium nitrate and 2.17g of cerium nitrate hexahydrate in 200mL of deionized water, and stir magnetically for 15min;
(2)在步骤(1)得到的混合溶液中加入0.035g硝酸锂(n硝酸锶:n六水硝酸铈:n硝酸锂=100:50:5)和9.45g一水柠檬酸,进行磁力搅拌30min;(2) Add 0.035g lithium nitrate (n strontium nitrate: n cerium nitrate hexahydrate: n lithium nitrate = 100:50:5) and 9.45g citric acid monohydrate to the mixed solution obtained in step (1), and carry out magnetic stirring 30min;
(3)在步骤(2)得到的混合溶液中加入稀氨水调节pH值至6~7;(3) Add dilute ammonia water to the mixed solution obtained in step (2) to adjust the pH value to 6~7;
(4)将步骤(3)得到的混合溶液在80℃条件下蒸发结晶2h,形成凝胶;(4) Evaporate and crystallize the mixed solution obtained in step (3) at 80°C for 2 hours to form a gel;
(5)将步骤(4)得到的凝胶置于干燥箱中,在120℃条件下干燥12h,研磨30min,再置于马弗炉中于900℃条件下,退火2h,制备得到Sr2CeO4:Li+微纳米粉末;(5) Place the gel obtained in step (4) in a drying oven, dry at 120°C for 12 hours, grind for 30 minutes, and then place it in a muffle furnace at 900°C for 2 hours to prepare Sr 2 CeO 4 : Li + micro-nano powder;
(6)在步骤(5)得到的Sr2CeO4:Li+微纳米粉末中加入无水乙醇,研磨30min,在150℃条件下干燥24h,制备得到Sr2CeO4:Li+陶瓷粉体;(6) Add absolute ethanol to the Sr 2 CeO 4 : Li + micro-nano powder obtained in step (5), grind for 30 minutes, and dry at 150°C for 24 hours to prepare Sr 2 CeO 4 : Li + ceramic powder;
(7)将步骤(6)得到的Sr2CeO4:Li+陶瓷粉体先在950℃,90MPa条件下,真空热压烧结2h,再在1050℃的空气气氛下无压烧结10h,制备得到Sr2CeO4半透明陶瓷。(7) The Sr 2 CeO 4 : Li + ceramic powder obtained in step (6) was first sintered by vacuum hot pressing at 950°C and 90MPa for 2 hours, and then pressurelessly sintered at 1050°C for 10 hours in an air atmosphere to prepare Sr 2 CeO 4 translucent ceramics.
从图1可以看出,透过Sr2CeO4半透明陶瓷片能看到陶瓷片后的字符"Sr2CeO4",说明陶瓷片的透光率高,致密度高。It can be seen from Figure 1 that the characters "Sr 2 CeO 4 " behind the ceramic sheet can be seen through the Sr 2 CeO 4 translucent ceramic sheet, indicating that the ceramic sheet has high light transmittance and high density.
实施例2Example 2
本发明提供的一种铈酸锶半透明陶瓷材料的制备方法,包括如下步骤:A kind of preparation method of strontium cerate translucent ceramic material provided by the invention comprises the following steps:
(1)将2.11g硝酸锶和2.17g六水硝酸铈溶于200mL去离子水中,进行磁力搅拌25min;(1) Dissolve 2.11g of strontium nitrate and 2.17g of cerium nitrate hexahydrate in 200mL of deionized water, and stir magnetically for 25min;
(2)在步骤(1)得到的混合溶液中加入0.07g硝酸锂(n硝酸锶:n六水硝酸铈:n硝酸锂=100:50:10)和9.45g一水柠檬酸,进行磁力搅拌30min;(2) Add 0.07g lithium nitrate (n strontium nitrate: n cerium nitrate hexahydrate: n lithium nitrate = 100:50:10) and 9.45g citric acid monohydrate to the mixed solution obtained in step (1), and perform magnetic stirring 30min;
(3)在步骤(2)得到的混合溶液中加入稀氨水调节pH值至6~7;(3) Add dilute ammonia water to the mixed solution obtained in step (2) to adjust the pH value to 6~7;
(4)将步骤(3)得到的混合溶液在80℃条件下蒸发结晶2h,形成凝胶;(4) Evaporate and crystallize the mixed solution obtained in step (3) at 80°C for 2 hours to form a gel;
(5)将步骤(4)得到的凝胶置于干燥箱中,在120℃条件下干燥12h,研磨30min,再置于马弗炉中于900℃条件下,退火2h,制备得到Sr2CeO4:Li+微纳米粉末;(5) Place the gel obtained in step (4) in a drying oven, dry at 120°C for 12 hours, grind for 30 minutes, and then place it in a muffle furnace at 900°C for 2 hours to prepare Sr 2 CeO 4 : Li + micro-nano powder;
(6)在步骤(5)得到的Sr2CeO4:Li+微纳米粉末中加入无水乙醇,研磨30min,在150℃条件下干燥24h,制备得到Sr2CeO4:Li+陶瓷粉体;(6) Add absolute ethanol to the Sr 2 CeO 4 : Li + micro-nano powder obtained in step (5), grind for 30 minutes, and dry at 150°C for 24 hours to prepare Sr 2 CeO 4 : Li + ceramic powder;
(7)将步骤(6)得到的Sr2CeO4:Li+陶瓷粉体先在950℃,90MPa条件下,真空热压烧结2h,再在1050℃的空气气氛下无压烧结10h,制备得到Sr2CeO4半透明陶瓷。(7) The Sr 2 CeO 4 : Li + ceramic powder obtained in step (6) was first sintered by vacuum hot pressing at 950°C and 90MPa for 2 hours, and then pressurelessly sintered at 1050°C for 10 hours in an air atmosphere to prepare Sr 2 CeO 4 translucent ceramics.
从图2可以看出,透过Sr2CeO4半透明陶瓷片能看到陶瓷片后的字符"Sr2CeO4",而且比实施例1所得陶瓷片看到的更清晰,说明实施例2所得陶瓷片的透光率更好。As can be seen from Fig. 2, the character " Sr 2 CeO 4 " behind the ceramic sheet can be seen through the Sr 2 CeO 4 translucent ceramic sheet, and it is clearer than what the ceramic sheet obtained in Example 1 sees, illustrating that embodiment 2 The light transmittance of the obtained ceramic sheet is better.
从图3可以得到,通过本发明实施例1和实施例2提供的方法制备得到的Sr2CeO4半透明陶瓷片在355nm紫外光激发下,发出了很强的蓝光,峰值波长约为483nm。由此可以看出,当Li+浓度增大时,Sr2CeO4半透明陶瓷的发光峰强度是逐渐增大的,从图1和图2的对比效果也可以看出,实施例2制备得到的Sr2CeO4半透明陶瓷的透光率优于实施例1制备得到的Sr2CeO4半透明陶瓷。It can be seen from Fig. 3 that the Sr 2 CeO 4 translucent ceramic sheet prepared by the method provided in Example 1 and Example 2 of the present invention emits strong blue light with a peak wavelength of about 483nm under the excitation of 355nm ultraviolet light. It can be seen that when the Li + concentration increases, the luminescence peak intensity of the Sr 2 CeO 4 translucent ceramics gradually increases, and it can also be seen from the comparative effects of Figure 1 and Figure 2 that the preparation of Example 2 obtained The light transmittance of the Sr 2 CeO 4 translucent ceramics is better than that of the Sr 2 CeO 4 translucent ceramics prepared in Example 1.
实施例3Example 3
本发明提供的一种铈酸锶半透明陶瓷材料的制备方法,包括如下步骤:A kind of preparation method of strontium cerate translucent ceramic material provided by the invention comprises the following steps:
(1)将2.11g硝酸锶和2.17g六水硝酸铈溶于200mL去离子水中,进行磁力搅拌30min;(1) Dissolve 2.11g of strontium nitrate and 2.17g of cerium nitrate hexahydrate in 200mL of deionized water, and stir magnetically for 30min;
(2)在步骤(1)得到的混合溶液中加入0.105g硝酸锂(n硝酸锶:n六水硝酸铈:n硝酸锂=100:50:15)和9.45g一水柠檬酸,进行磁力搅拌50min;(2) Add 0.105g lithium nitrate (n strontium nitrate: n cerium nitrate hexahydrate: n lithium nitrate = 100:50:15) and 9.45g citric acid monohydrate to the mixed solution obtained in step (1), and carry out magnetic stirring 50min;
(3)在步骤(2)得到的混合溶液中加入三乙胺调节pH值至6~7;(3) Add triethylamine to the mixed solution obtained in step (2) to adjust the pH value to 6~7;
(4)将步骤(3)得到的混合溶液在90℃条件下蒸发结晶3h,形成凝胶;(4) Evaporate and crystallize the mixed solution obtained in step (3) at 90°C for 3 hours to form a gel;
(5)将步骤(4)得到的凝胶置于干燥箱中,在130℃条件下干燥14h,研磨40min,再置于马弗炉中于950℃条件下,退火3h,制备得到Sr2CeO4:Li+微纳米粉末;(5) Place the gel obtained in step (4) in a drying oven, dry at 130°C for 14h, grind for 40min, then place in a muffle furnace at 950°C, and anneal for 3h to prepare Sr 2 CeO 4 : Li + micro-nano powder;
(6)在步骤(5)得到的Sr2CeO4:Li+微纳米粉末中加入无水乙醇,研磨40min,在160℃条件下干燥30h,制备得到Sr2CeO4:Li+陶瓷粉体;(6) Add absolute ethanol to the Sr 2 CeO 4 : Li + micro-nano powder obtained in step (5), grind for 40 minutes, and dry at 160°C for 30 hours to prepare Sr 2 CeO 4 : Li + ceramic powder;
(7)将步骤(6)得到的Sr2CeO4:Li+陶瓷粉体先在1100℃,100MPa条件下,真空热压烧结3h,再在1100℃的空气气氛下无压烧结12h,制备得到Sr2CeO4半透明陶瓷。(7) The Sr 2 CeO 4 : Li + ceramic powder obtained in step (6) was first sintered by vacuum hot pressing at 1100°C and 100MPa for 3h, and then pressurelessly sintered at 1100°C for 12h in an air atmosphere to prepare Sr 2 CeO 4 translucent ceramics.
实施例4Example 4
本发明提供的一种铈酸锶半透明陶瓷材料的制备方法,包括如下步骤:A kind of preparation method of strontium cerate translucent ceramic material provided by the invention comprises the following steps:
(1)将2.11g硝酸锶和2.17g六水硝酸铈溶于200mL去离子水中,进行磁力搅拌30min;(1) Dissolve 2.11g of strontium nitrate and 2.17g of cerium nitrate hexahydrate in 200mL of deionized water, and stir magnetically for 30min;
(2)在步骤(1)得到的混合溶液中加入0.14g硝酸锂(n硝酸锶:n六水硝酸铈:n硝酸锂=100:50:20)和9.45g一水柠檬酸,进行磁力搅拌60min;(2) Add 0.14g lithium nitrate (n strontium nitrate: n cerium nitrate hexahydrate: n lithium nitrate = 100:50:20) and 9.45g citric acid monohydrate to the mixed solution obtained in step (1), and carry out magnetic stirring 60min;
(3)在步骤(2)得到的混合溶液中加入三乙烯二胺调节pH值至6~7;(3) Add triethylenediamine to the mixed solution obtained in step (2) to adjust the pH value to 6~7;
(4)将步骤(3)得到的混合溶液在95℃条件下蒸发结晶3.5h,形成凝胶;(4) Evaporate and crystallize the mixed solution obtained in step (3) at 95°C for 3.5 hours to form a gel;
(5)将步骤(4)得到的凝胶置于干燥箱中,在145℃条件下干燥12h,研磨50min,再置于马弗炉中于850℃条件下,退火3h,制备得到Sr2CeO4:Li+微纳米粉末;(5) Place the gel obtained in step (4) in a drying oven, dry at 145°C for 12 hours, grind for 50 minutes, and then place it in a muffle furnace at 850°C for 3 hours to prepare Sr 2 CeO 4 : Li + micro-nano powder;
(6)在步骤(5)得到的Sr2CeO4:Li+微纳米粉末中加入无水乙醇,研磨45min,在180℃条件下干燥30h,制备得到Sr2CeO4:Li+陶瓷粉体;(6) Add absolute ethanol to the Sr 2 CeO 4 : Li + micronano powder obtained in step (5), grind for 45 minutes, and dry at 180°C for 30 hours to prepare Sr 2 CeO 4 : Li + ceramic powder;
(7)将步骤(6)得到的Sr2CeO4:Li+陶瓷粉体先在1100℃,110MPa条件下,真空热压烧结4h,再在1050℃的空气气氛下无压烧结14h,制备得到Sr2CeO4半透明陶瓷。(7) The Sr 2 CeO 4 : Li + ceramic powder obtained in step (6) was first sintered by vacuum hot pressing at 1100°C and 110MPa for 4h, and then pressurelessly sintered at 1050°C for 14h in an air atmosphere to prepare Sr 2 CeO 4 translucent ceramics.
实施例5Example 5
本发明提供的一种铈酸锶半透明陶瓷材料的制备方法,包括如下步骤:A kind of preparation method of strontium cerate translucent ceramic material provided by the invention comprises the following steps:
(1)将2.11g硝酸锶和2.17g六水硝酸铈溶于200mL去离子水中,进行磁力搅拌35min;(1) Dissolve 2.11g of strontium nitrate and 2.17g of cerium nitrate hexahydrate in 200mL of deionized water, and stir magnetically for 35min;
(2)在步骤(1)得到的混合溶液中加入0.175g硝酸锂(n硝酸锶:n六水硝酸铈:n硝酸锂=100:50:25)和9.45g一水柠檬酸,进行磁力搅拌50min;(2) Add 0.175g lithium nitrate (n strontium nitrate: n cerium nitrate hexahydrate: n lithium nitrate = 100:50:25) and 9.45g citric acid monohydrate to the mixed solution obtained in step (1), and carry out magnetic stirring 50min;
(3)在步骤(2)得到的混合溶液中加入四甲基乙二胺调节pH值至6~7;(3) Add tetramethylethylenediamine to the mixed solution obtained in step (2) to adjust the pH value to 6~7;
(4)将步骤(3)得到的混合溶液在95℃条件下蒸发结晶1.5h,形成凝胶;(4) Evaporate and crystallize the mixed solution obtained in step (3) at 95°C for 1.5 hours to form a gel;
(5)将步骤(4)得到的凝胶置于干燥箱中,在135℃条件下干燥12h,研磨40min,再置于马弗炉中于850℃条件下,退火3h,制备得到Sr2CeO4:Li+微纳米粉末;(5) Place the gel obtained in step (4) in a drying oven, dry at 135°C for 12 hours, grind for 40 minutes, and then place it in a muffle furnace at 850°C for 3 hours to prepare Sr 2 CeO 4 : Li + micro-nano powder;
(6)在步骤(5)得到的Sr2CeO4:Li+微纳米粉末中加入无水乙醇,研磨60min,在180℃条件下干燥20h,制备得到Sr2CeO4:Li+陶瓷粉体;(6) Add absolute ethanol to the Sr 2 CeO 4 : Li + micro-nano powder obtained in step (5), grind for 60 minutes, and dry at 180°C for 20 hours to prepare Sr 2 CeO 4 : Li + ceramic powder;
(7)将步骤(6)得到的Sr2CeO4:Li+陶瓷粉体先在1150℃,110MPa条件下,真空热压烧结,再在1200℃的空气气氛下无压烧结10h,制备得到Sr2CeO4半透明陶瓷。(7) Sinter the Sr 2 CeO 4 : Li + ceramic powder obtained in step (6) at 1150°C and 110MPa under vacuum hot pressing, and then sinter without pressure at 1200°C for 10 hours in an air atmosphere to prepare Sr 2 CeO 4 translucent ceramics.
通过实验可知,上述5种实施方式都可以制备得到透光率较好的Sr2CeO4半透明陶瓷,为了更好的验证Li+浓度对Sr2CeO4半透明陶瓷的透光率及发射峰强度的影响,下面以实施例2为例,控制工艺参数不变,通过调整Li+的浓度来验证Sr2CeO4半透明陶瓷的透光率及发射峰强度;It can be seen from experiments that the above five implementation methods can prepare Sr 2 CeO 4 translucent ceramics with better light transmittance, in order to better verify the light transmittance and emission peak of Sr 2 CeO 4 Influence of intensity, take embodiment 2 as example below, control process parameter is constant, verify the light transmittance and emission peak intensity of Sr 2 CeO 4 translucent ceramics by adjusting the concentration of Li + ;
通过表1可以看出,当硝酸锶、六水硝酸铈和硝酸锂的摩尔比为100:50:1~25时,都可以制备得到Sr2CeO4半透明陶瓷,当Li+的浓度逐渐增大时,Sr2CeO4半透明陶瓷的透光率更优、发射峰也增强,但是随着Li+的浓度进一步增大,透光率逐渐降低,发射峰强度也逐渐减弱。因此,硝酸锶、六水硝酸铈和硝酸锂的摩尔比优选为100:50:5~15。It can be seen from Table 1 that when the molar ratio of strontium nitrate, cerium nitrate hexahydrate and lithium nitrate is 100:50:1~25, Sr 2 CeO 4 translucent ceramics can be prepared. When the concentration of Li + gradually increases When the concentration of Sr 2 CeO 4 is large, the light transmittance of Sr 2 CeO 4 translucent ceramics is better, and the emission peak is also enhanced, but with the further increase of Li + concentration, the light transmittance decreases gradually, and the emission peak intensity also gradually weakens. Therefore, the molar ratio of strontium nitrate, cerium nitrate hexahydrate and lithium nitrate is preferably 100:50:5~15.
为了验证本发明真空热压烧结和空气气氛下的无压烧结对本发明制备得到的Sr2CeO4半透明陶瓷的致密度及透光率的影响,下面以实施例2为参照,分别设置了对比实施例。In order to verify the influence of vacuum hot pressing sintering and pressureless sintering under air atmosphere of the present invention on the density and light transmittance of the Sr 2 CeO 4 translucent ceramics prepared in the present invention, the following uses Example 2 as a reference to set up comparisons Example.
对比实施例1Comparative Example 1
(1)将2.11g硝酸锶和2.17g六水硝酸铈溶于200mL去离子水中,进行磁力搅拌25min;(1) Dissolve 2.11g of strontium nitrate and 2.17g of cerium nitrate hexahydrate in 200mL of deionized water, and stir magnetically for 25min;
(2)在步骤(1)得到的混合溶液中加入0.07g硝酸锂(n硝酸锶:n六水硝酸铈:n硝酸锂=100:50:10)和9.45g一水柠檬酸,进行磁力搅拌30min;(2) Add 0.07g lithium nitrate (n strontium nitrate: n cerium nitrate hexahydrate: n lithium nitrate = 100:50:10) and 9.45g citric acid monohydrate to the mixed solution obtained in step (1), and perform magnetic stirring 30min;
(3)在步骤(2)得到的混合溶液中加入稀氨水调节pH值至6~7;(3) Add dilute ammonia water to the mixed solution obtained in step (2) to adjust the pH value to 6~7;
(4)将步骤(3)得到的混合溶液在80℃条件下蒸发结晶2h,形成凝胶;(4) Evaporate and crystallize the mixed solution obtained in step (3) at 80°C for 2 hours to form a gel;
(5)将步骤(4)得到的凝胶置于干燥箱中,在120℃条件下干燥12h,研磨30min,再置于马弗炉中于900℃条件下,退火2h,制备得到Sr2CeO4:Li+微纳米粉末;(5) Place the gel obtained in step (4) in a drying oven, dry at 120°C for 12 hours, grind for 30 minutes, and then place it in a muffle furnace at 900°C for 2 hours to prepare Sr 2 CeO 4 : Li + micro-nano powder;
(6)在步骤(5)得到的Sr2CeO4:Li+微纳米粉末中加入无水乙醇,研磨30min,在150℃条件下干燥24h,制备得到Sr2CeO4:Li+陶瓷粉体;(6) Add absolute ethanol to the Sr 2 CeO 4 : Li + micro-nano powder obtained in step (5), grind for 30 minutes, and dry at 150°C for 24 hours to prepare Sr 2 CeO 4 : Li + ceramic powder;
(7)将步骤(6)得到的Sr2CeO4:Li+陶瓷粉体在950℃,90MPa条件下,真空热压烧结2h,制备得到Sr2CeO4半透明陶瓷。(7) The Sr 2 CeO 4 : Li + ceramic powder obtained in step (6) was sintered under vacuum hot pressing at 950° C. and 90 MPa for 2 hours to prepare Sr 2 CeO 4 translucent ceramics.
对比实施例1相比本发明提供的实施例2,省去了空气气氛下的无压烧结工艺,通过对制备得到的Sr2CeO4半透明陶瓷进行检测,发现该对比实施例1制备得到的Sr2CeO4陶瓷相比实施例2得到的Sr2CeO4陶瓷更加疏松。Compared with Example 2 provided by the present invention, Comparative Example 1 omits the pressureless sintering process under the air atmosphere. By testing the prepared Sr 2 CeO 4 translucent ceramics, it is found that the prepared Comparative Example 1 The Sr 2 CeO 4 ceramic is more porous than the Sr 2 CeO 4 ceramic obtained in Example 2.
对比实施例2Comparative Example 2
(1)将2.11g硝酸锶和2.17g六水硝酸铈溶于200mL去离子水中,进行磁力搅拌25min;(1) Dissolve 2.11g of strontium nitrate and 2.17g of cerium nitrate hexahydrate in 200mL of deionized water, and stir magnetically for 25min;
(2)在步骤(1)得到的混合溶液中加入0.07g硝酸锂(n硝酸锶:n六水硝酸铈:n硝酸锂=100:50:10)和9.45g一水柠檬酸,进行磁力搅拌30min;(2) Add 0.07g lithium nitrate (n strontium nitrate: n cerium nitrate hexahydrate: n lithium nitrate = 100:50:10) and 9.45g citric acid monohydrate to the mixed solution obtained in step (1), and perform magnetic stirring 30min;
(3)在步骤(2)得到的混合溶液中加入稀氨水调节pH值至6~7;(3) Add dilute ammonia water to the mixed solution obtained in step (2) to adjust the pH value to 6~7;
(4)将步骤(3)得到的混合溶液在80℃条件下蒸发结晶2h,形成凝胶;(4) Evaporate and crystallize the mixed solution obtained in step (3) at 80°C for 2 hours to form a gel;
(5)将步骤(4)得到的凝胶置于干燥箱中,在120℃条件下干燥12h,研磨30min,再置于马弗炉中于900℃条件下,退火2h,制备得到Sr2CeO4:Li+微纳米粉末;(5) Place the gel obtained in step (4) in a drying oven, dry at 120°C for 12 hours, grind for 30 minutes, and then place it in a muffle furnace at 900°C for 2 hours to prepare Sr 2 CeO 4 : Li + micro-nano powder;
(6)在步骤(5)得到的Sr2CeO4:Li+微纳米粉末中加入无水乙醇,研磨30min,在150℃条件下干燥24h,制备得到Sr2CeO4:Li+陶瓷粉体;(6) Add absolute ethanol to the Sr 2 CeO 4 : Li + micro-nano powder obtained in step (5), grind for 30 minutes, and dry at 150°C for 24 hours to prepare Sr 2 CeO 4 : Li + ceramic powder;
(7)将步骤(6)得到的Sr2CeO4:Li+陶瓷粉体在1050℃的空气气氛下无压烧结10h,制备得到Sr2CeO4半透明陶瓷。(7) The Sr 2 CeO 4 : Li + ceramic powder obtained in step (6) was sintered without pressure in an air atmosphere at 1050° C. for 10 h to prepare Sr 2 CeO 4 translucent ceramics.
对比实施例2相比本发明提供的实施例2,省去了真空热压烧结工艺,通过对制备得到的Sr2CeO4半透明陶瓷进行检测,发现该对比实施例2制备得到的Sr2CeO4陶瓷相比实施例2得到的Sr2CeO4陶瓷更加疏松、透光率也较差、发光效率也更低。Compared with Example 2 provided by the present invention, Comparative Example 2 omits the vacuum hot pressing sintering process. By testing the prepared Sr 2 CeO 4 translucent ceramics, it is found that the Sr 2 CeO 4 prepared in Comparative Example 2 Compared with the Sr 2 CeO 4 ceramic obtained in Example 2, the 4 ceramic is more porous, has poorer light transmittance, and lower luminous efficiency.
由此可知,本发明提供的Sr2CeO4半透明陶瓷的制备方法,必须先在真空条件下进行热压烧结使陶瓷快速致密化;由于本发明提供的原料硝酸锂中的Li+能够作为烧结助剂,从而在空气气氛下进行无压烧结时,能够使铈酸锶陶瓷的致密度和透光率及发光效率进一步提高。It can be seen that the preparation method of Sr 2 CeO 4 translucent ceramics provided by the present invention must first be hot - pressed and sintered under vacuum conditions to make the ceramics rapidly densified; since the Li in the raw material lithium nitrate provided by the present invention can be used as a sintered Additives, so that the density, light transmittance and luminous efficiency of strontium cerate ceramics can be further improved when pressureless sintering is carried out in an air atmosphere.
以上实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都是属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。The above examples only express several implementations of the present invention, and the description thereof is relatively specific and detailed, but should not be construed as limiting the patent scope of the present invention. It should be pointed out that those skilled in the art can make several modifications and improvements without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent for the present invention should be based on the appended claims.
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