CN114478029B - Preparation of ABO 3 Method for manufacturing perovskite ceramic block - Google Patents
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Abstract
The invention relates to ABO 3 The technical field of preparation of perovskite ceramic blocks, aims to solve the problem that the prior art cannot prepare the block ceramic in one step from synthesis, and discloses a method for preparing ABO 3 A method of forming a perovskite ceramic block comprising the steps of: selection of ABO 3 Using hydrates of the metal element A and the metal element B as initial raw materials, weighing the initial raw materials, grinding and mixing to obtain a mixture; moving the mixture into a WC-Co high-temperature die, firstly heating the mixture in a non-pressure state, and then applying uniaxial pressure after heat preservation; continuously heating to the target temperature, preserving heat and pressure, and naturally cooling to room temperature to obtain compact ABO 3 A nanocrystalline ceramic block. The invention can realize low-temperature synthesis and densification of the target ceramic by one step through reactive cold sintering, greatly simplifies the preparation process and flow of the ceramic block, shortens the preparation period and reduces the energy consumption.
Description
Technical Field
The invention relates to ABO 3 The technical field of preparation of perovskite ceramic blocks, in particular to preparation of ABO 3 A method for manufacturing perovskite ceramic blocks.
Background
Perovskites are one of the most important materials in the electronic ceramic industry. BaTiO 2 3 As a typical ABO 3 Perovskite ceramics having a very high dielectric constant at room temperature, based on BaTiO 3 The resulting multilayer ceramic capacitor (MLCC) is used in an amount exceeding three trillion billions per year, and thus is widely used as a dielectric material for ceramic capacitors. Conventional BaTiO 3 The process for the preparation of bulk ceramics generally comprises two steps, first of all the synthesis of BaTiO 3 Powder, then pressing the powder into a green body, and sintering at 1300-1400 ℃. At present, for BaTiO 3 The synthesis of the method mostly adopts a coprecipitation method, a hydrothermal synthesis method, a sol-gel method and the like, and the methods have high cost and low efficiency and are difficult to meet the requirements of industrial production. For BaTiO 3 Sintering of, typically BaTiO 3 Pressing the powder into a green body, and carrying out high-temperature long-time heat preservation and sintering. However, high temperature not only causes excessive grain growth, but also causes excessive growth of grainsCausing volatilization of Ba and weakening BaTiO to a certain extent 3 The dielectric properties of (2); in addition, the dielectric layer thickness of the MLCC reaches the process node of 1 μm, which puts strict requirements on the grain size of the dielectric material. To weaken BaTiO 3 Coarsening of crystal grains during sintering has been used to prepare BaTiO by various advanced sintering techniques such as spark plasma sintering, microwave sintering, flash sintering and the like 3 And (3) a block body. These techniques reduce the sintering temperature or shorten the sintering time by introducing an external field effect, thereby suppressing BaTiO to some extent 3 The crystal grains are coarsened. However, the sintering temperature in these processes is still as high as thousands of degrees, and thus it is difficult to obtain fine crystalline ceramics.
To achieve low temperature sintering of ceramics, the prior art has added transient solvents to the target powder at low temperatures (f: (a) (b))<Under the synergistic action of 300 ℃ and high pressure (350-500 MPa), the densification process of the material is realized through a dissolution-reprecipitation mechanism. However, this work only involves sintering of ceramic powder, and is not concerned with the synthesis of ceramic powder. The prior art also discloses a low-temperature cold sintering preparation method of the barium titanate ferroelectric ceramic, which utilizes the hydrothermal precursor suspension of barium titanate as liquid-phase auxiliary BaTiO 3 The cold sintering process of (2). However, this method still requires the use of BaTiO 3 The nano powder is used as a raw material, the hydrothermal precursor suspension is only used as a small amount of liquid phase additive (mass fraction is 20 wt.%) to assist densification, and the blank obtained by cold sintering is subjected to secondary sintering at 850-950 ℃ to obtain high-density and well-crystallized BaTiO 3 Bulk, but secondary sintering results in BaTiO 3 And coarsening crystal grains. In conclusion, since the synthesis and sintering of powder are often mutually independent procedures, the prior art has the problem that the bulk ceramic cannot be prepared in one step from the synthesis.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for preparing ABO 3 A method for manufacturing perovskite ceramic blocks.
In order to achieve the purpose, the invention adopts the following technical scheme:
preparation of ABO 3 A method of forming a perovskite ceramic block comprising the steps of:
step 1: selection of ABO 3 Using hydrates of the metal element A and the metal element B as initial raw materials, weighing the initial raw materials, grinding and mixing to obtain a mixture;
step 2: moving the mixture into a WC-Co high-temperature die, firstly heating the mixture in a non-pressure state, and then applying uniaxial pressure after heat preservation;
and step 3: continuously heating to the target temperature, preserving heat and pressure, and naturally cooling to room temperature to obtain compact ABO 3 A nanocrystalline ceramic mass.
Preferably, said ABO 3 Perovskite-type ceramics include, but are not limited to, baTiO 3 ，SrTiO 3 ， MgTiO 3 ，CaTiO 3 ，BaZrO 3 ，Ba x Sr (1-x) TiO 3 Wherein x =0-1.
Preferably, the hydrate as the starting material is selected based on a substance which is easily reacted under a low temperature condition of less than 450 ℃.
Preferably, the hydrate as the starting material includes, but is not limited to, ba (OH) 2 ·8H 2 O， Sr(OH) 2 ·8H 2 O，Mg(OH) 2 ，Ca(OH) 2 ，H 2 TiO 3 ，Zr(OH) 4 。
Preferably, the molar ratio of the two starting materials weighed in step 1 is 1 to 1.15.
Preferably, the molar ratio of the two starting materials weighed in step 1 is between 1.05 and 1.1.
Preferably, the grinding method for the starting materials in the step 1 is ball milling; the ball milling speed is 1000-3000rpm, and the ball milling time is 5-30min.
Preferably, when the starting materials are subjected to ball milling, the ball-to-material ratio is 5:1.
preferably, the WC-Co high-temperature die is 600MPa, and the maximum usable temperature is 500 ℃.
Preferably, in the step 2, the mixture is heated to 80-120 ℃ under a non-pressure state, and uniaxial pressure is applied after the temperature is kept for 5-20 min.
Preferably, the uniaxial pressure in the step 2 is 200-600MPa.
Preferably, the target temperature in step 3 is 100-450 ℃.
Preferably, the heat preservation time after the temperature is raised to the target temperature in the step 3 is 0-120min.
The beneficial effects of the invention are as follows:
1. compared with the existing ceramic preparation technology, the invention can realize low-temperature synthesis and densification of the target ceramic by one step through reactive cold sintering, greatly simplifies the preparation process and flow of the ceramic block, shortens the preparation period and reduces the energy consumption.
2. The target ceramic (ABO) of the present invention is compared to existing cold sintering techniques 3 ) The synthesis of the powder is realized in the low-temperature cold sintering process, and the target powder synthesized in advance is not used, so that the synthesis and densification are really realized in one step. Moreover, the prepared ceramic block has high density and good crystallization, and does not need secondary high-temperature sintering, thereby avoiding coarsening of crystal grains.
3. Compared with the existing external field auxiliary ceramic sintering technology, the reaction cold sintering process involved in the invention does not need to involve complex auxiliary equipment such as electric field/microwave and the like, heat is provided by means of self reaction, and the synthesis and densification processes of the ceramic are realized under the condition of not exceeding 450 ℃ by virtue of synergistic effects of temperature provided in the cold sintering process, applied pressure and the like; moreover, due to the lower operation temperature, the prepared ceramic has the advantages of fine grains, uniformity, compactness and small block deformation, and has wide application value.
4. According to the invention, a series of single-phase and element-doped perovskite ceramic blocks can be prepared by changing the type and proportion of the used hydrate; in addition, the grain size, the relative density and the ceramic performance of the ceramic block can be flexibly regulated and controlled by changing parameters such as temperature, uniaxial pressure, heat preservation time, pressurization mode and the like in the cold sintering process, and the method has the advantages of simplicity in operation, high efficiency, strong controllability and the like.
Drawings
FIG. 1 is a graph of temperature and applied pressure as a function of time as employed in example 1 of the present invention;
FIG. 2 is an XRD pattern of the ceramics obtained in examples 1, 2, 3, 4, 5 of the present invention;
FIG. 3 is a schematic representation of BaTiO obtained in inventive example 1 3 A micro-topography of the ceramic fracture;
FIG. 4 shows SrTiO 2 obtained in example 2 of the present invention 3 A micro-topography of the ceramic fracture;
FIG. 5 shows BaZrO obtained in example 3 of the present invention 3 A micro-topography of the ceramic fracture;
FIG. 6 shows Ba obtained in example 5 of the present invention 0.5 Sr 0.5 TiO 3 A micro-topography of the ceramic fracture;
FIG. 7 shows BaTiO obtained in example 6 of the present invention 3 A micro-topography of the ceramic fracture;
FIG. 8 shows BaTiO obtained in example 7 of the present invention 3 A micro-topography of the ceramic fracture;
FIG. 9 shows BaTiO obtained in example 8 of the present invention 3 A micro-topography of the ceramic fracture.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Preparation of ABO 3 A method of forming a perovskite ceramic block comprising the steps of: selection of ABO 3 Using hydrates of the metal element A and the metal element B as initial raw materials, weighing the initial raw materials, grinding and mixing to obtain a mixture; moving the mixture into a WC-Co high-temperature die, firstly heating the mixture in a non-pressure state, and then applying uniaxial pressure after heat preservation; continuously heating to the target temperature, preserving heat and pressure, and naturally cooling to room temperature to obtain compact ABO 3 A nanocrystalline ceramic mass.
Example 1
Step 1: a Ba/Ti ratio of 1 was selected and 0.473g of Ba (OH) was weighed out separately 2 ·8H 2 O and 0.147g H 2 TiO 3 The two raw materials are simultaneously put into a ball milling tank, the ball material ratio is kept at 5, and the ball milling tank is kept at the rotating speed of 1200rpm for 10min, so that uniformly dispersed Ba (OH) is obtained 2 ·8H 2 O/ H 2 TiO 3 Mixing the powder;
step 2: transferring the mixed composite powder into a WC-Co high-temperature die with the inner diameter of 12 mm;
and step 3: heating the raw materials under non-pressure state, heating the powder to 100 deg.C, keeping the temperature for 5min, applying uniaxial pressure of 500MPa, and continuously heating to 300 deg.C for 60min;
and 4, step 4: naturally cooling the sample to room temperature to obtain the BaTiO 3 The synchronous synthesis and sintering process of (2);
the relative density of the sample was measured by mass/volume method to be 90.5%, and the BaTiO content in the sample was measured using Nano Measurer software 3 Has an average grain size of 55. + -.2 nm.
Example 2
This example differs from example 1 in that: the initial raw material is Sr (OH) 2 · 8H 2 O and H 2 TiO 3 Wherein the Sr/Ti ratio is 1.05, 0.418g of Sr (OH) was weighed in each case 2 · 8H 2 O and 0.147g H 2 TiO 3 SrTiO was obtained in the same manner as in example 1 except for the other parameters and procedure 3 XRD pattern of the sample is shown in figure 2 (SrTiO) 3 Spectral line), the characteristic peak of the sample completely corresponds to SrTiO 3 A standard map of (a). The relative compactness of the sample is 92%, and the average grain size is 28 +/-5 nm. The fracture micro-topography of the resulting sample is shown in fig. 4.
Example 3
This example differs from example 1 in that: the initial raw material is Ba (OH) 2 · 8H 2 O and Zr (OH) 4 Separately, 0.473g of Ba (OH) was weighed 2 ·8H 2 O and 0.376g Zr (OH) 4 First, weighed Zr (OH) 4 Ball milling was carried out at 3000rpm for 15min separately, and then Ba (OH) 2 ·8H 2 O and ball-milled Zr (OH) 4 Blending, other parameters and proceduresExample 1 same, baZrO 3 The XRD pattern of the sample is shown in figure 2 (BaZrO) 3 Spectral line), the characteristic peak of the sample completely corresponds to BaZrO 3 A standard map of (a). The relative density of the sample is 90%, and the average grain size is 60 +/-5 nm. The fracture micro-topography of the resulting sample is shown in FIG. 5.
Example 4
This example differs from example 1 in that: the initial raw material is Ba (OH) 2 ·8H 2 O、Sr(OH) 2 ·8H 2 O and H 2 TiO 3 0.426g of Ba (OH) was weighed out separately 2 ·8H 2 O, 0.04g Sr (OH) 2 ·8H 2 O and 0.147g H 2 TiO 3 Heating the mixed powder to 90 ℃, preserving the heat for 15min, then applying uniaxial pressure of 500MPa, and then continuously heating to 400 ℃ for 60min; other parameters and procedure were the same as in example 1 to obtain Ba 0.9 Sr 0.1 TiO 3 XRD pattern of the sample is shown in figure 2 (Ba) 0.9 Sr 0.1 TiO 3 Spectral lines). The relative density of the sample is 95%, and the average grain size is 45 +/-6 nm.
Example 5
This example differs from example 1 in that: the initial raw material is Ba (OH) 2 ·8H 2 O、Sr(OH) 2 ·8H 2 O and H 2 TiO 3 Wherein the ratio of (Ba + Sr)/Ti is 1.10, 0.260g of Ba (OH) was weighed out separately 2 ·8H 2 O, 0.219g of Sr (OH) 2 ·8H 2 O and 0.147g H 2 TiO 3 Ba was obtained in the same manner as in example 1 except for the other parameters and steps 0.5 Sr 0.5 TiO 3 XRD pattern of the sample is shown in figure 2 (Ba) 0.5 Sr 0.5 TiO 3 Spectral line), the relative density is 95%, and the average grain size is 45 +/-6 nm. The fracture micro-topography of the resulting sample is shown in fig. 6.
Example 6
This example differs from example 1 in that: the Ba/Ti ratio was 1.05, i.e., 0.497g of Ba (OH) was weighed out separately 2 ·8H 2 O and 0.147g H 2 TiO 3 As a raw material, objectThe temperature was 250 ℃ and the other parameters and procedure were the same as in example 1 to obtain BaTiO 3 The relative density of the sample was 93% and the average grain size was 68 ± 4nm. The fracture micro-topography of the resulting sample is shown in FIG. 7.
Example 7
This example differs from example 1 in that: the stated Ba/Ti ratio was 1.10, i.e., 0.52g of Ba (OH) was weighed out separately 2 ·8H 2 O and 0.147g H 2 TiO 3 The holding time was 120min and other parameters and procedures were the same as in example 1, as the starting material, baTiO was obtained 3 The relative density of the sample was 97% and the average grain size was 74 + -5 nm. The fracture micro-topography of the resulting sample is shown in fig. 8.
Example 8
This example differs from example 1 in that: the stated Ba/Ti ratio was 1.15, i.e., 0.544g of Ba (OH) was weighed out separately 2 ·8H 2 O and 0.147g H 2 TiO 3 As a raw material, a uniaxial pressure of 600MPa was applied and other parameters and procedures were the same as in example 1 to obtain BaTiO 3 The relative density of the sample was 97.5% and the average grain size was 85 ± 4nm. The fracture micro-topography of the resulting sample is shown in fig. 9.
Compared with the existing ceramic preparation technology, the invention can realize low-temperature synthesis and densification of the target ceramic by one step through reactive cold sintering, greatly simplifies the preparation process and flow of the ceramic block, shortens the preparation period and reduces the energy consumption.
The target ceramic (ABO) of the present invention is compared to existing cold sintering techniques 3 ) The synthesis of (2) is realized in the process of low-temperature cold sintering, and the target powder synthesized in advance is not used, so that the synthesis and densification are really completed in one step. Moreover, the prepared ceramic block has high density and good crystallization, and secondary high-temperature sintering is not needed, so that coarsening of crystal grains is avoided.
Compared with the existing external field auxiliary ceramic sintering technology, the reaction cold sintering process involved in the invention does not need to involve complex auxiliary equipment such as electric field/microwave and the like, heat is provided by means of self reaction, and the synthesis and densification processes of the ceramic are realized under the condition of not exceeding 450 ℃ by virtue of synergistic effects of temperature provided in the cold sintering process, applied pressure and the like; moreover, due to the lower operation temperature, the prepared ceramic has the advantages of fine crystal grains, uniformity, compactness and small block deformation, and has wide application value.
According to the invention, a series of single-phase and element-doped perovskite ceramic blocks can be prepared by changing the type and proportion of the used hydrate; in addition, the grain size, the relative density and the ceramic performance of the ceramic block can be flexibly regulated and controlled by changing parameters such as temperature, uniaxial pressure, heat preservation time, pressurization mode and the like in the cold sintering process, and the method has the advantages of simplicity in operation, high efficiency, strong controllability and the like.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. Preparation of ABO 3 A method of forming a perovskite ceramic block, comprising the steps of:
step 1: selection of ABO 3 Taking hydrates of the metal element A and the metal element B as initial raw materials, weighing the initial raw materials, grinding and mixing to obtain a mixture;
and 2, step: moving the mixture into a WC-Co high-temperature die, firstly heating the mixture in a non-pressure state, and then applying uniaxial pressure after heat preservation;
and step 3: continuously heating to the target temperature, preserving heat and pressure, and naturally cooling to room temperature to obtain compact ABO 3 A nanocrystalline ceramic block;
the hydrate as the starting material is selected based on a substance which is easily reacted at a low temperature of less than 450 deg.C, and includes, but is not limited to, ba (OH) 2 ·8H 2 O，Sr(OH) 2 ·8H 2 O，
Mg(OH) 2 ，Ca(OH) 2 ，H 2 TiO 3 ，Zr(OH) 4 ；
The molar ratio of the two initial raw materials weighed in the step 1 is 1-1.15;
the WC-Co high-temperature die has the maximum usable temperature of 500 ℃ under 600 MPa;
in the step 2, heating the mixture to 80-120 ℃ in a non-pressure state, preserving heat for 5-20min, and then applying uniaxial pressure;
the target temperature in step 3 is 100-450 ℃.
2. A method of preparing ABO according to claim 1 3 Method for forming a perovskite ceramic block, characterized in that said ABO 3 Perovskite-type ceramics include, but are not limited to, baTiO 3 ，SrTiO 3 ，MgTiO 3 ，CaTiO 3 ，BaZrO 3 ，Ba x Sr (1-x) TiO 3 Wherein x =0-1.
3. A method of preparing ABO according to claim 1 3 The method for preparing the perovskite ceramic block is characterized in that the grinding method for the initial raw materials in the step 1 is ball milling;
the ball milling speed is 1000-3000rpm, and the ball milling time is 5-30min.
4. A method of preparing ABO according to claim 1 3 The method for preparing the perovskite ceramic block is characterized in that the uniaxial pressure in the step 2 is 200-600MPa.
5. A method of preparing ABO according to claim 1 3 The method for preparing the perovskite ceramic block is characterized in that the holding time after the temperature is raised to the target temperature in the step 3 is 0-120min.
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| CN109133911A (en) * | 2018-09-25 | 2019-01-04 | 桂林电子科技大学 | A kind of method of ultra-low temperature cold sintering zno-based ceramics |
| CN110498680A (en) * | 2019-09-16 | 2019-11-26 | 苏州科技大学 | The perovskite ferroelectric ceramics and preparation method and application of twin crystal grain particle diameter distribution structure |
| CN112062591A (en) * | 2020-09-21 | 2020-12-11 | 吉林大学 | ZrO (ZrO)2Low-temperature rapid sintering method of ceramic and metal, connecting piece and device |
| CN112500154A (en) * | 2020-12-18 | 2021-03-16 | 杭州电子科技大学 | Method for preparing LiF-based core-shell structure microwave dielectric ceramic based on cold sintering process |
| CN113023764A (en) * | 2021-03-19 | 2021-06-25 | 襄阳汽车职业技术学院 | Preparation method of copper-based perovskite nanocrystalline film |
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