CN110002851A - A kind of laminated perovskite Ca3Mn2O7The preparation method of ceramic material - Google Patents
A kind of laminated perovskite Ca3Mn2O7The preparation method of ceramic material Download PDFInfo
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- CN110002851A CN110002851A CN201910272140.7A CN201910272140A CN110002851A CN 110002851 A CN110002851 A CN 110002851A CN 201910272140 A CN201910272140 A CN 201910272140A CN 110002851 A CN110002851 A CN 110002851A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/442—Carbonates
Abstract
The present invention relates to a kind of laminated perovskite Ca3Mn2O7The preparation method of ceramic material, with CaCO3、MnO2It is refined and is uniformly mixed by the compound particles that the method for mechanical ball mill makes to meet stoichiometric ratio for presoma, sintering can prepare laminated perovskite Ca at a temperature of tabletting and 1000-1150 DEG C again later3Mn2O7Ceramic material simplifies preparation step, reduces hand labor investment, easy to implement, and calcines and sintering temperature is lower, and crystal relies on manual operation low at Xiang Wending, improves the success rate of preparation.
Description
Technical field
The present invention relates to functional material preparation technical fields, and in particular to a kind of laminated perovskite Ca3Mn2O7Ceramic material
Preparation method.
Background technique
Multi-ferroic material is a kind of a kind of functional material for possessing a variety of amazing physics phenomenas and application prospect, Neng Goutong
The a variety of iron sexual functions of Shi Yongyou have caused the extensive of academia due to its very big application potential in information material field
Interest, interior in the past twenty years, the research and application of multi-ferroic material are always many interested fields of scientist, will
Material with magnetoelectric effect becomes magnetoelectric material or magnetoelectricity body, can apply and read autotelegraph hard disk, multiferroic in multi-state memory, magnetic
In the related devices such as memory, modern society can satisfy to low-power consumption, high density, portable and multifunctional novel information apparatus
Urgent need.
Laminated perovskite Ca3Mn2O7Ceramic material is read as one of multi-ferroic material in area information storage magnetic
There is huge application prospect in terms of autotelegraph hard disk and microwave device, so how simple and effective reliably prepares high quality stratiform
Perovskite Ca3Mn2O7Ceramic material is always researcher in the direction of effort.In preparation method in the prior art, due to layer
Shape perovskite Ca3Mn2O7Structure is complicated for ceramic material, and high temperature is easy to produce Mn oxide miscellaneous phase, thus its preparation process it is cumbersome and
Required temperature is higher, such as the Ca of Guiblin report3Mn2O7Need 2.2 × 107KPa pressure, the Ca of the reports such as Zhu3Mn2O7
It needs in O2It is sintered under atmosphere protection, the Ca of Liu et al. report3Mn2O71400 DEG C of sintering after 1200 DEG C of pre-burnings are needed, it is intermediate
It needs constantly to smash and re-grind.The above various preparation method conditions require harshness, and preparation procedure is cumbersome, manual operation
Journey is more, and crystal property is affected by manual operation, and error and failure rate are higher, is unfavorable for being mass produced and pushing away extensively
Wide application.
Therefore, how a kind of laminated perovskite Ca that simple and effective is easily-controllable is provided3Mn2O7The preparation method of ceramic material is
Those skilled in the art's urgent problem to be solved.
Summary of the invention
In view of this, the present invention provides a kind of laminated perovskite Ca3Mn2O7The preparation method of ceramic material overcomes at present
Laminated perovskite Ca3Mn2O7Method existing for ceramic material preparation process is complicated, process is various, temperature is higher, unstable etc. lacks
It falls into, proposes that a kind of simple and stability and high efficiency prepares laminated perovskite Ca3Mn2O7The method of ceramic material.
To achieve the goals above, the present invention specifically uses following technological means:
A kind of laminated perovskite Ca provided by the invention3Mn2O7The preparation method of ceramic material, comprising the following steps:
(1) CaCO is weighed respectively3And MnO2Be uniformly mixed, be placed in ball mill and be added liquid ball-milling medium progress
Ball milling 10-36h takes out mixture drying later, obtains premix presoma；
(2) the premix presoma that the step (1) obtains is placed in ball mill and is dry grinded, what dry grinding terminated uniformly to refine
Precursor powder；
(3) that precursor powder made from the step (2) is placed in Muffle furnace under the conditions of 1000-1100 DEG C calcining is more
It is secondary, each 18-32h, and mixture is ground after calcining gap and last time calcining, obtain raw material powder；
(4) raw material powder that the step (3) obtains is placed in mold and is made into ceramic green sheet, be placed in Muffle furnace
It is sintered under the conditions of 1000-1150 DEG C more than for 24 hours to get laminated perovskite Ca3Mn2O7Ceramic material.
Further, the CaCO in the step (1)3And MnO2Molar ratio is 3:2
Preferably, the ball milling in the step (1) is the revolving speed ball milling for using planetary ball mill with 300-500r/min,
Liquid ball-milling medium is alcohol or deionization.
Preferably, the drying steps in the step (1) are that first drying is evaporated liquid ball in 40-60 DEG C of thermostatic drying chamber
Grinding media, be placed in 120-220 DEG C of drying box and keep 10-24h.
The beneficial effect of above-mentioned optimal technical scheme is: can make medium slow evaporation under the conditions of 40-60 DEG C, prevent bumping from rising
Cause mixing uneven；The liquid ball-milling medium that can be volatilized to greatest extent in mixing under the conditions of 120-220 DEG C, reduces subsequent dry method
Agglomeration incidence in ball milling.
Preferably, it carries out preceding premix presoma is placed in 900 DEG C of environment of the step (2) and calcines 10-12h.
The beneficial effect of above-mentioned optimal technical scheme is: CaCO at a temperature of this3Start to decompose into CaO and CO2, CaO is easier to
With MnO2Reaction generates final product.
Preferably, the ball milling in the step (2) use zirconium oxide, stainless steel or Talide ball grinder with
The revolving speed dry ball milling of 300-500r/min.
Preferably, 2-5h is spaced in the step (2) in mechanical milling process to be sampled and utilize tester observation particle thin
Change degree, until sample X-ray diffraction spectrum main peak halfwidth >=0.4 ° stops ball milling.
Preferably, the calcining number in the step (3) is at least twice.
The beneficial effect of above-mentioned optimal technical scheme is: repeatedly calcining can effectively improve Ca3Mn2O7Crystalline quality and
Purity.
In conclusion compared with prior art, the present invention has following technical effect that the present invention passes through wet ball grinding first
It is uniformly mixed raw material and obtains mixing presoma, carrying out processing to mixing presoma by dry method mechanical ball-milling method later makes forerunner
The refinement of body particle and further full and uniform mixing；It is calcined and is sintered again later, simplify preparation step, reduce people
Work working feature, it is easy to implement, and, gained crystal purity height lower with sintering temperature is calcined, and it is low to manual operation dependence, it mentions
The success rate of preparation is risen.
Figure of description
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 attached drawing is that the dry milled process of the embodiment of the present invention 1 samples sample diffraction map；
Fig. 2 attached drawing is laminated perovskite Ca made from the embodiment of the present invention 13Mn2O7Ceramic material diffracting spectrum；
Fig. 3 attached drawing is that the dry milled process of the embodiment of the present invention 2 samples sample diffraction map；
Fig. 4 attached drawing is laminated perovskite Ca made from the embodiment of the present invention 23Mn2O7Ceramic material diffracting spectrum；
Fig. 5 attached drawing is that conventional solid sintering process prepares perovskite Ca3Mn2O7The repeated experiment diffracting spectrum of ceramic material；
Fig. 6 attached drawing is laminated perovskite Ca made from the embodiment of the present invention 23Mn2O7The repeated experiment diffraction of ceramic material
Map.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
A kind of laminated perovskite Ca3Mn2O7The preparation method of ceramic material, comprising the following steps:
(1) 30.03g CaCO is weighed respectively3And 17.39gMnO2Be uniformly mixed, be placed on the polytetrafluoro equipped with agate ball
In ethylene tank, alcohol 60ml is added, later with the revolving speed wet-milling 12h of 500r/min on planetary ball mill, takes out later mixed
Conjunction object, which is placed in 50 DEG C of freeze-day with constant temperature, is evaporated alcohol, then is warming up to 150 DEG C and keeps for 24 hours, thorough drying composite, before obtaining premix
Drive body；
(2) the premix presoma that step (1) obtains is placed in the zirconium oxide tank equipped with agate ball, with 500r/min's
Revolving speed dry grinding samples every 5h during dry grinding and observes particle degree of refinement by X-ray diffraction, reaches in main peak halfwidth
Terminate ball milling at 0.4 ° or more, obtains the precursor powder uniformly refined；
(3) precursor powder made from step (2) is placed in Muffle furnace and is calcined twice under the conditions of 1000-1100 DEG C,
Every time for 24 hours, and after calcining gap and last time calcining grinding 1h is carried out to mixture in the agate mortar, obtains raw material powder
End；
(4) raw material powder that step (3) obtains is placed in mold and is made into ceramic green sheet, be placed in Muffle furnace
It is sintered under the conditions of 1000-1150 DEG C for 24 hours to get laminated perovskite Ca3Mn2O7Ceramic material.
Wherein, sampling and testing map is as shown in Fig. 1 in the dry milled process of step (2), is determined by calculating halfwidth
It dry grinds the time；
Obtained laminated perovskite Ca3Mn2O7The diffracting spectrum of ceramic material is as shown in Fig. 2, as shown in Figure 2, the present invention
Successfully prepare laminated perovskite Ca3Mn2O7Ceramic material.
Embodiment 2
A kind of laminated perovskite Ca3Mn2O7The preparation method of ceramic material, comprising the following steps:
(1) 30.03g CaCO is weighed respectively3With 17.39g MnO2Be uniformly mixed, poly- four be placed on equipped with agate ball
In vinyl fluoride tank, alcohol 60ml is added, is taken out later on planetary ball mill with the revolving speed wet-milling 12h of 500r/min later
Mixture is placed in 50 DEG C of freeze-day with constant temperature and is evaporated alcohol, then is warming up to 150 DEG C and keeps for 24 hours, and thorough drying composite must premix
Presoma；
(2) the premix presoma that step (1) obtains is placed in Muffle furnace in 900 DEG C and calcines 1h, later natural cooling
Taking-up is placed in the zirconium oxide tank equipped with agate ball, is dry grinded with the revolving speed of 500r/min, is sampled and lead to every 5h during dry grinding
X-ray diffraction observation particle degree of refinement is crossed, terminates ball milling when main peak halfwidth reaches 0.4 ° or more, obtains before uniformly refining
Drive body powder；
(3) precursor powder made from step (2) is placed in Muffle furnace and is calcined twice under the conditions of 1000-1100 DEG C,
Every time for 24 hours, and after calcining gap and last time calcining grinding 10h is carried out to mixture in the agate mortar, obtains raw material powder
End；
(4) raw material powder that step (3) obtains is placed in mold and is made into ceramic green sheet, be placed in Muffle furnace
It is sintered under the conditions of 1000-1150 DEG C for 24 hours to get laminated perovskite Ca3Mn2O7Ceramic material.
Wherein, sampling and testing map is as shown in Fig. 3 in the dry milled process of step (2), is determined by calculating halfwidth
It dry grinds the time, and from the figure 3, it may be seen that precalcining can be further reduced the dry grinding time；
Obtained laminated perovskite Ca3Mn2O7The diffracting spectrum of ceramic material is as shown in figure 4, as shown in Figure 4, the present invention
Successfully prepare laminated perovskite Ca3Mn2O7Ceramic material.
And it should be further noted that the method system that conventional solid sintering process and the embodiment of the present invention 2 is respectively adopted
Standby perovskite Ca3Mn2O7Ceramic material simultaneously carries out repeated experiment, as a result shown in attached drawing 5-6, by attached drawing 5 and attached drawing 6 it is found that originally
Ca made from the technical solution of invention3Mn2O7Not only crystal purity is high, and repeats still to keep high-purity after testing, that is, is prepared into
Power is high.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For device disclosed in embodiment
For, since it is corresponded to the methods disclosed in the examples, so being described relatively simple, related place is said referring to method part
It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (8)
1. a kind of laminated perovskite Ca3Mn2O7The preparation method of ceramic material, which comprises the following steps:
(1) CaCO is weighed respectively3And MnO2Be uniformly mixed, be placed in ball mill and be added liquid ball-milling medium carry out ball milling
10-36h takes out mixture drying later, obtains premix presoma；
(2) the premix presoma that the step (1) obtains is placed in ball mill and is dry grinded, obtain the precursor powder uniformly refined；
(3) precursor powder made from the step (2) is placed in Muffle furnace under the conditions of 1000-1100 DEG C and is calcined repeatedly,
Each 18-32h, and mixture is ground after calcining gap and last time calcining, obtain raw material powder；
(4) raw material powder that the step (3) obtains is placed in mold and is made into ceramic green sheet, be placed in Muffle furnace
It is sintered under the conditions of 1000-1150 DEG C above to get laminated perovskite Ca for 24 hours3Mn2O7Ceramic material.
2. a kind of laminated perovskite Ca according to claim 13Mn2O7The preparation method of ceramic material, which is characterized in that
CaCO in the step (1)3And MnO2Molar ratio is 3:2.
3. a kind of laminated perovskite Ca according to claim 13Mn2O7The preparation method of ceramic material, which is characterized in that
Ball milling in the step (1) is the revolving speed ball milling for using planetary ball mill with 300-500r/min, and liquid ball-milling medium is
Alcohol or deionization.
4. a kind of laminated perovskite Ca according to claim 13Mn2O7The preparation method of ceramic material, which is characterized in that
Drying steps in the step (1) are that first drying is evaporated liquid ball-milling medium in 40-60 DEG C of thermostatic drying chamber, be placed on
10-24h is kept in 120-220 DEG C of drying box.
5. a kind of laminated perovskite Ca according to claim 13Mn2O7The preparation method of ceramic material, which is characterized in that
It carries out preceding premix presoma is placed in 900 DEG C of environment of the step (2) and calcines 5-12h.
6. a kind of laminated perovskite Ca according to claim 13Mn2O7The preparation method of ceramic material, which is characterized in that
Ball milling in the step (2) uses zirconium oxide, stainless steel or Talide ball grinder to turn with 400-600r/min
Fast dry ball milling.
7. a kind of laminated perovskite Ca according to claim 13Mn2O7The preparation method of ceramic material, which is characterized in that
2-5h is spaced in the step (2) in mechanical milling process to be sampled and tester is utilized to observe particle degree of refinement, until sample X is penetrated
Line diffraction spectra main peak halfwidth >=0.4 ° stops ball milling.
8. a kind of laminated perovskite Ca according to claim 13Mn2O7The preparation method of ceramic material, which is characterized in that
Calcining number in the step (3) is at least twice.
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| CN111747383A (en) * | 2020-05-23 | 2020-10-09 | 北京工业大学 | Ruddlesden-Popper layered perovskite structure single-phase ferroelectric photovoltaic material |
| CN114656243A (en) * | 2022-02-25 | 2022-06-24 | 纯钧新材料(深圳)有限公司 | Calcium-manganese-oxygen thermoelectric material and preparation method thereof |
| CN116675518A (en) * | 2023-06-01 | 2023-09-01 | 江西理工大学 | Single-layer and double-layer perovskite multiferroic multiphase material, and preparation method and application thereof |
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| CN116675518A (en) * | 2023-06-01 | 2023-09-01 | 江西理工大学 | Single-layer and double-layer perovskite multiferroic multiphase material, and preparation method and application thereof |
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