Sodium bismuth titanate-barium titanate lead-free transparent electro-optic ceramics and preparation method thereof

A technology of sodium bismuth titanate and electro-optic ceramics, applied in the direction of the structure/shape of the active medium, can solve the problems of difficult control of volatilization, opacity of ceramics, long sintering time, etc. The effect of coefficients

Active Publication Date: 2016-08-17
江苏先进无机材料研究院
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Problems solved by technology

To prepare NBT-BT optoceramics by hot pressing and sintering, in order to completely eliminate pores, the sintering time of the material is longer, and the corresponding Na 2 O, Bi 2 o 3 It is difficult to control the volatilization of ceramics, and the composition of ceramics is easy to deviate from the design to form impurity phases. If the sintering system control is not ideal during the volatilization process of volatile components, more pores will be formed in the material.
Due to light irradiation on the impurity phase and pores, light absorption, reflection, refraction, scattering, etc. will occur, which will cause the ceramics to be opaque.

Method used

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  • Sodium bismuth titanate-barium titanate lead-free transparent electro-optic ceramics and preparation method thereof
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  • Sodium bismuth titanate-barium titanate lead-free transparent electro-optic ceramics and preparation method thereof

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[0031] The invention provides a preparation method of sodium bismuth titanate-barium titanate lead-free transparent opto-ceramic. The chemical composition of the sodium bismuth titanate-barium titanate lead-free transparent opto-ceramic is (1-x)(Na 0.5 Bi 0.5 )TiO 3 -xBaTiO 3 , where 0.05≤x≤0.08. The preparation method adopts an oxygen-passing-hot pressing sintering process, and by controlling the powder synthesis and sintering technology, the generation of impurity phases is suppressed and the pores are eliminated, so as to achieve the purpose of improving the optical transmittance and electro-optical effect of the material. Specifically, as an example, the preparation method of the present invention may include the following steps.

[0032] (1) Ingredients: using Na 2 CO 3 , Bi 2 O 3 , TiO 2 , BaCO 3 As raw materials, each raw material powder is accurately weighed according to the chemical composition of the above-mentioned sodium bismuth titanate-barium titanate le...

Embodiment 1

[0051] Press (1-x)(Na 0.5 Bi 0.5 )TiO 3 -xBaTiO 3 , where x=0.06 ingredients, using φ2mm ZrO 2 The mixed ball was used as the ball milling medium for planetary ball milling for 6 hours. After drying, the obtained raw meal was ground into powder, and then passed through a 200-mesh sieve to keep the components uniform. After sieving, the powder was put into an alumina crucible and pre-fired at 850°C for 2 hours to synthesize. After the synthesis, the powder was pulverized and passed through a 100-mesh sieve, planetary ball milled for 4 hours, and then dried and added with a mass concentration of 6% PVA binder. The pressure is 300MP, the forming mold is a cylinder of φ20×15, and then oxygen-passing-hot pressing is used for sintering. The parameters of the sintering process are: from room temperature to 900°C at a heating rate of 200°C / hour, and hold for 1 hour; then at 100°C ℃ / hour to heat up, and gradually pressurize to 250MPa, then keep the pressure unchanged, after heating...

Embodiment 2

[0053] Press (1-x)(Na 0.5 Bi 0.5 )TiO 3 -xBaTiO 3 , where x=0.05, the ingredients are ZrO with φ2mm 2 The mixed ball was used as a ball milling medium for ball milling for 5 hours, and the obtained raw meal was ground into powder after drying, and then passed through a 200-mesh sieve to keep the components uniform. After sieving, the powder was put into an alumina crucible and pre-fired at 850°C for 3 hours to synthesize. After the synthesis, the powder was pulverized and passed through a 100-mesh sieve and then ball-milled for 4 hours. The mass concentration of 6% PVA binder was added. The molding pressure was 350 MPa, and the molding die was The φ20×15 cylinder was then sintered with oxygen and hot pressing. The parameters of the sintering process were as follows: from room temperature to 830°C at a heating rate of 200°C / hour, holding for 1 hour; then heating at 100°C / hour, and Gradually pressurize to 240MPa, then keep the pressure unchanged, heat up to 1000°C, keep warm...

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Abstract

The invention relates to a sodium bismuth titanate-barium titanate lead-free transparent electro-optic ceramic and a preparation method thereof; the electro-optic ceramic has the chemical composition of (1-x)(Na0.5Bi0.5)TiO3-xBaTiO3, wherein 0.05<=x<=0.08; the preparation method includes the steps: batching Na2CO3, Bi2O3, TiO2 and BaCO3 as raw materials according to the stoichiometric ratio, carrying out ball milling, and mixing evenly to obtain a powder; carrying out heat preservation on the powder for 2-4 h at the temperature of 850-950 DEG C, and thus obtaining a synthetic material; crushing the synthetic material, sieving, carrying out ball milling, adding a binder, and carrying out press molding to obtain a blank; next, placing the blank in a sintering furnace, heating up from room temperature to 800 DEG C-850 DEG C at the speed of 200 DEG C-250 DEG C / h, and carrying out heat preservation for 0.5-1.5 h; and heating up at the speed of 100 DEG C / h and gradually pressurizing to 200-250 MPa, followed by keeping the pressure unchanged, heating up to 1000 DEG C-1050 DEG C, then carrying out heat preservation for 2 h, then heating up to 1100 DEG C-1200 DEG C at the speed of 50 DEG C / h, carrying out heat and pressure preservation for 8-24 h, then releasing the pressure, cooling to 900 DEG C at the speed of 100 DEG C / h, and cooling to room temperature along with a furnace, wherein oxygen is introduced with the flow quantity of 3-5 L / minute when the heating is started and introduction of oxygen is stopped when the pressure is released.

Description

technical field [0001] The invention belongs to the field of transparent functional ceramic materials, in particular to a sodium bismuth titanate-barium titanate lead-free transparent electro-optical ceramic and a preparation method thereof. Background technique [0002] The development of optical communication is closely related to optical passive devices (optical switches, optical attenuators, optical couplers), and the quality of optical passive devices largely depends on the materials used to prepare them. At present, the electro-optic material widely used in optical passive devices at home and abroad is lithium niobate single crystal material. This kind of perovskite crystal has strong primary electro-optic effect, high Curie temperature and high response speed. However, due to the lack of breakthrough in growth technology for a long time, it is still difficult to grow lithium niobate crystals that meet the stoichiometric ratio, making it difficult for its performance t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01S3/06C04B35/475C04B35/622
Inventor 程文秀何夕云仇萍荪曾霞夏彬
Owner 江苏先进无机材料研究院
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