CN103664171A - Ferrous acid lutecium ceramic material and preparation method and application thereof - Google Patents
Ferrous acid lutecium ceramic material and preparation method and application thereof Download PDFInfo
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- CN103664171A CN103664171A CN201310578681.5A CN201310578681A CN103664171A CN 103664171 A CN103664171 A CN 103664171A CN 201310578681 A CN201310578681 A CN 201310578681A CN 103664171 A CN103664171 A CN 103664171A
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- ferrous acid
- stupalith
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- acid lutetium
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Abstract
The invention provides a preparation method for ferrous acid lutecium ceramic material. According to the method, Lu(NO3)3 powder and Fe(NO3)3 powder are taken as the raw materials, ammonium bicarbonate is taken as the precipitator, precursor powder is prepared through a chemical coprecipitation method, and the precursor powder is ball milled, sieved and sintered under heat insulation condition, thus obtaining the ferrous acid lutecium ceramic material. The preparation method is simple; the prepared material has uniform components and high compactness, is applicable to preparation of a ferrous acid lutecium membrane through pulsed laser deposition and a magnetron sputtering system. The invention also provides the application of the ferrous acid lutecium ceramic material in preparation of the ferrous acid lutecium membrane.
Description
Technical field
The invention belongs to microelectronics technology, be specifically related to a kind of ferrous acid lutetium stupalith and its preparation method and application.
Background technology
The outstanding electric property of ferroelectric material has bred its wide application prospect, and its electronic component has the many merits such as integrated level is high, energy consumption is little, fast response time.And investigator combines ferroelectric material with other technology at present, make the new integrated ferroelectric material property being born more outstanding.Ferroelectric membranc is paid close attention to widely because of its application at electronics and optics, particularly the research of ferroelectric film memory is the focus of studying both at home and abroad, a kind of high-quality ferroelectric membranc should have the component of stoichiometric ratio, the structure of densification and crystallization, monocrystalline or have a kind of polycrystalline structure and large-area homogeneity of preferred orientation at least.
The method of preparing at present film has a lot: pulsed laser deposition, magnetron sputtering, atomic layer epitaxy, gas phase epitaxy of metal organic compound, molecular beam epitaxy etc., wherein sputtering sedimentation becomes and prepares high-quality thin-film utilisation technology the most widely.Yet for sputtering sedimentation, the critical materials ceramic target of preparing high-quality film accounts for very large production cost.At preparation of target materials and process aspect, the stupalith target that normal pressure-sintered mode obtains high-compactness cheaply becomes development trend.High-compactness is the generation that reduces " stain " in deposition process, the key that improves yield rate and film quality.
The current preparation method about ferrous acid lutetium pottery and characteristic research are seldom.Anxious a kind of preparation technology to be developed material component simple and that prepare is even, density is high, can be applicable to the stupalith that pulsed laser deposition and magnetic control sputtering system are prepared ferrous acid lutetium film.
Summary of the invention
The object of this invention is to provide a kind of technique simple, the lower-cost ferrous acid lutetium stupalith of preparing is prepared ferrous acid lutetium film as target for pulsed laser deposition.
The present invention proposes a kind of preparation method of ferrous acid lutetium stupalith, with Lu (NO
3)
3and Fe (NO
3)
3powder is raw material, usings bicarbonate of ammonia as precipitation agent, by chemical coprecipitation, makes powder, then through ball milling, sieve, after heat preservation sintering, obtain object product ferrous acid lutetium stupalith, comprise the following steps:
(1) described raw material is added in described precipitant solution, ageing in air after stirring, obtains precipitation after filtering, and through washing, is precipitated cake piece after oven dry, is pulverized powdered in crucible; Wherein, Lu (NO in raw material
3)
3and Fe (NO
3)
3the mole dosage ratio of powder is (0.95～1): (1～1.05).Preferably, raw material Lu (NO
3)
3and Fe (NO
3)
3the mole dosage ratio of powder is 1: 1.
(2) powder step (1) being obtained adds deionized water or dehydrated alcohol, and ball milling in ball grinder carries out presintering in retort furnace after oven dry.
(3) powder step (2) being obtained is placed in ball grinder ball milling again, after drying, after granulation, sieves, and extrusion forming, 1200 ℃ of high temperature sinterings in retort furnace, obtain described ferrous acid lutetium stupalith.
Wherein, the raw material powder obtaining in step (1) be by chemical coprecipitation, prepared resulting.
Wherein, the Ball-milling Time in described step (2) is 5～12 hours; Ball milling speed is 350r/min.Preferably, described Ball-milling Time is 7 hours.
Wherein, the pre-sintering temperature in described step (2) is 700～900 ℃, and the presintering time is 2～3 hours.Preferably, described calcined temperature is 800 ℃, and the pre-burning time is 2 hours.
Wherein, described extrusion forming is normal pressure or isostatic pressing.
Wherein, described high temperature sintering is normal pressure-sintered, hot pressed sintering or plasma discharge sintering.
The invention provides a kind of ferrous acid lutetium stupalith preparing by the inventive method.Described ferrous acid lutetium stupalith, learns that through XRD test its principal phase is LuFeO
3, be quasi-perovskite structure, the film that uses pulsed laser deposition to obtain, smooth surface, does not have the situation that occurs " stain " to show that its density is high.
The present invention also provides a kind of application of ferrous acid lutetium stupalith, wherein, using described ferrous acid lutetium stupalith as target, is directly preparing the application in ferrous acid lutetium film by pulsed laser deposition.
The present invention also provides a kind of preparation method of ferroelectric sour lutetium film, first by ferrous acid lutetium stupalith preparation method disclosed by the invention, carry out successively step (1), (2), (3) and obtain ferrous acid lutetium stupalith, further, described ferrous acid lutetium stupalith is directly prepared to described ferrous acid lutetium film (LuFeO by pulsed laser deposition one step
3film).Wherein, use pulse laser sediment method, on nickel acid lanthanum substrate, deposit LuFeO
3film, with the pulse laser of certain energy, under the atmosphere of oxygen, laser is beaten and on target, is produced plumage brightness, is then deposited on the substrate after heating, thereby forms ferrous acid lutetium film.
Beneficial effect of the present invention comprises, powder granule that preparation technology is simple, energy consumption is low, prepare is tiny, be evenly distributed; The component of the product ferrous acid lutetium ceramic target preparing is even, density is high, is very suitable for preparing the needed material of ferrous acid lutetium film as pulsed laser deposition and magnetic control sputtering system.
Accompanying drawing explanation
Ferrous acid lutetium stupalith (LuFeO3 stupalith) the surface topography SEM figure of Fig. 1 for obtaining according to ferrous acid lutetium stupalith preparation method of the present invention, collection of illustrative plates shows that ceramic particle is tiny and is evenly distributed, density is high.
The XRD material phase analysis collection of illustrative plates that Fig. 2 is the ferrous acid lutetium stupalith (LuFeO stupalith) that obtains by ferrous acid lutetium stupalith preparation method of the present invention, collection of illustrative plates shows LuFeO
3target principal crystalline phase is LuFeO
3.
The LuFeO of Fig. 3 for obtaining by the ferroelectric sour lutetium method for manufacturing thin film of the present invention
3the XRD material phase analysis collection of illustrative plates of film; Collection of illustrative plates shows to utilize LuFeO of the present invention
3stupalith can depositing high-quality LuFeO as target
3film.
Embodiment
In conjunction with following specific embodiments and the drawings, the present invention is described in further detail, and protection content of the present invention is not limited to following examples.Do not deviating under the spirit and scope of inventive concept, variation and advantage that those skilled in the art can expect are all included in the present invention, and take appending claims as protection domain.Implement process of the present invention, condition, reagent, experimental technique etc., except the content of mentioning specially below, be universal knowledege and the common practise of this area, the present invention is not particularly limited content.
Prepare ferrous acid lutetium stupalith (LuFeO stupalith), first adopt chemical coprecipitation to prepare needed powder, then obtain stupalith through high temperature sintering, comprise the steps:
Step (1): press chemical general formula LuFeO
3the stoichiometric ratio of middle Lu, Fe, takes raw material Lu (NO according to mol ratio at 1: 1
3)
3and Fe (NO
3)
3powder.Using bicarbonate of ammonia as precipitation agent.Powder is added in precipitant solution, constantly stir simultaneously, be placed on afterwards in air ageing 24 hours, then filter out required precipitation, use successively deionized water, absolute ethanol washing, is finally placed on the precipitation of acquisition in baking oven and is dried 48 hours, and the precipitation cake piece after oven dry pulverizes powdered in high purity aluminium oxide crucible.Raw material Lu (NO
3)
3and Fe (NO
3)
3the mole dosage ratio of powder can also be 0.95: 1 or 1: 1.05, all can obtain identical experimental result.
Step (2): put into ball grinder with the speed ball milling of 350r/min after the raw material powder that step (1) is obtained adds deionized water or dehydrated alcohol, then put into drying in oven, the powder of oven dry is placed on to pre-burning in retort furnace, afterwards the material after pre-burning is pulverized into powder again in crucible.
Step (3): will powder be put into ball grinder ball milling again according to the technique of step (2), after drying, after granulation, sieve, last extrusion forming, puts into retort furnace, at 1000～1200 ℃ of heat preservation sinterings, within 2～4 hours, obtains product ferrous acid lutetium stupalith.
The preparation of embodiment 1 ferrous acid lutetium stupalith
With Lu (NO
3)
3and Fe (NO
3)
3powder is raw material, 1: the 1 in molar ratio coprecipitation reaction of preparing burden and carry out, then obtain LuFeO through mixing, washing, oven dry and grinding
3precursor powder.In order to make powder more even, then add deionized water or dehydrated alcohol to do ball-milling medium, utilize planetary ball mill, with the rotating speed mixing and ball milling of 350r/min 7 hours.Dry the powder after ball milling, then put pre-burning in retort furnace into, with 3 degree/minute heat-up rate rise to 800 degree, be incubated 2 hours, then naturally cool to room temperature.By reacted powder secondary ball milling 7 hours, dry for standby.Powder after and secondary ball milling synthetic through high temperature is inserted in steel die, carry out axial pressure moulding, make biscuit.Finally the biscuit of compression moulding is put into retort furnace again, with 2 degree/minute speed, rise to 1200 ℃, and be incubated 2 hours, then naturally cooling is cooled to room temperature, and blow-on sampling, obtains product ferrous acid lutetium stupalith, its surface topography SEM figure, as shown in Figure 1, collection of illustrative plates shows that ceramic particle is tiny and is evenly distributed, and density is high.The XRD material phase analysis collection of illustrative plates of product ferrous acid lutetium stupalith, as shown in Figure 2, collection of illustrative plates shows LuFeO
3target principal crystalline phase is LuFeO
3.
Embodiment 2 ferrous acid lutetium film (LuFeO
3film) preparation
Utilize the stupalith of embodiment 1 preparation as target, adopt pulsed laser deposition technique, on nickel acid lanthanum substrate, deposit LuFeO
3film, operating air pressure is oxygen 0.2Pa, and pulsed laser energy is 400mJ, and frequency is 5Hz, depositing time 30 minutes, substrate need pass through heat temperature raising.Utilize pulsed laser deposition technique to deposit on nickel acid lanthanum substrate, and in oxygen atmosphere 700 ℃ of LuFeO that insulation obtained after 1 hour
3film, this LuFeO
3the XRD material phase analysis collection of illustrative plates of film as shown in Figure 3, shows to utilize aforementioned LuFeO
3stupalith can depositing high-quality LuFeO as target
3film.
Claims (9)
1. a preparation method for ferrous acid lutetium stupalith, is characterized in that, with Lu (NO
3)
3and Fe (NO
3)
3powder is raw material, usings bicarbonate of ammonia as precipitation agent, by chemical coprecipitation, makes precursor powder, then through ball milling, sieve, after heat preservation sintering, obtain described ferrous acid lutetium stupalith; Comprise the following steps:
(1) described raw material is added in described precipitant solution, ageing in air after stirring, obtains precipitation after filtering, and through washing, is precipitated cake piece after oven dry, is pulverized powdered in crucible; Wherein, Lu (NO in raw material
3)
3and Fe (NO
3)
3the mole dosage ratio of powder is (0.95～1): (1～1.05).
(2) powder step (1) being obtained adds deionized water or dehydrated alcohol, and ball milling in ball grinder carries out presintering in retort furnace after oven dry;
(3) powder step (2) being obtained be placed in ball grinder again ball milling mix, after drying, then granulation sieves, extrusion forming with 1200 ℃ of high temperature sinterings, obtains described ferrous acid lutetium stupalith in retort furnace.
2. preparation method as claimed in claim 1, is characterized in that, the Ball-milling Time in described step (2) is 5～12 hours; Ball milling speed is 350r/min.
3. preparation method as claimed in claim 1, is characterized in that, the pre-sintering temperature in described step (2) is 700～900 ℃, and the presintering time is 2～3 hours.
4. preparation method as claimed in claim 1, is characterized in that, described extrusion forming is normal pressure or isostatic pressing.
5. preparation method as claimed in claim 1, is characterized in that, described high temperature sintering is normal pressure-sintered, hot pressed sintering or plasma discharge sintering.
6. the ferrous acid lutetium stupalith preparing by method described in claim 1-5 any one, is characterized in that, described ferrous acid lutetium stupalith learns that through XRD test its principal phase is LuFeO
3, be quasi-perovskite structure, the film that uses pulsed laser deposition to obtain, smooth surface, does not occur that the situation of stain shows that its density is high.
7. the application of ferrous acid lutetium stupalith as claimed in claim 6, is characterized in that, described ferrous acid lutetium stupalith is applied to pulsed laser deposition as target and prepares ferrous acid lutetium film.
8. the preparation method of a ferrous acid lutetium film, it is characterized in that, first by carrying out successively step (1), (2), (3) described in claim 1, obtain ferrous acid lutetium stupalith, then, using described ferrous acid lutetium stupalith as target, by pulsed laser deposition, can a step directly prepare described LuFeO
3film.
9. the preparation method of ferrous acid lutetium film as claimed in claim 8, is characterized in that, uses pulse laser sediment method, on nickel acid lanthanum substrate, deposits LuFeO
3film, with pulse laser, under the atmosphere of oxygen, laser is beaten and on target, is produced plumage brightness, is then deposited on the substrate after heating, thereby forms ferrous acid lutetium film.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110282973A (en) * | 2019-06-19 | 2019-09-27 | 安阳师范学院 | A kind of high impedance LuFeO3The preparation method of ceramic material |
| CN112281128A (en) * | 2020-10-31 | 2021-01-29 | 贵阳学院 | Preparation method of perovskite type samarium ferrite target material for magnetron sputtering |
| CN114751460A (en) * | 2022-04-11 | 2022-07-15 | 北京化工大学 | Sol-gel preparation method of rare earth ferrite lutetium ferrite film |
Citations (3)
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|---|---|---|---|---|
| CN1267654A (en) * | 2000-04-06 | 2000-09-27 | 中国科学院上海技术物理研究所 | Preparation of ferroelectric lead zirconate titanate film material |
| CN101665915A (en) * | 2009-10-13 | 2010-03-10 | 华东师范大学 | Method for preparing bismuth ferric film material |
| JP2012223808A (en) * | 2011-04-21 | 2012-11-15 | Sumitomo Electric Ind Ltd | Surface treatment method |
-
2013
- 2013-11-18 CN CN201310578681.5A patent/CN103664171A/en active Pending
Patent Citations (3)
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|---|---|---|---|---|
| CN1267654A (en) * | 2000-04-06 | 2000-09-27 | 中国科学院上海技术物理研究所 | Preparation of ferroelectric lead zirconate titanate film material |
| CN101665915A (en) * | 2009-10-13 | 2010-03-10 | 华东师范大学 | Method for preparing bismuth ferric film material |
| JP2012223808A (en) * | 2011-04-21 | 2012-11-15 | Sumitomo Electric Ind Ltd | Surface treatment method |
Non-Patent Citations (2)
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|---|
| L P ZHU ET AL.: "Optical properties of LuFeO3 thin films prepared by pulsed laser deposition", 《JOURNAL OF PHYSICS: CONFERENCE SERIES》, vol. 276, 31 December 2011 (2011-12-31) * |
| 许庭静: "铁酸镥铁电材料的合成、微结构及性质研究", 《中国优秀硕士学位论文全文数据库 信息科技辑》, no. 03, 15 March 2011 (2011-03-15) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110282973A (en) * | 2019-06-19 | 2019-09-27 | 安阳师范学院 | A kind of high impedance LuFeO3The preparation method of ceramic material |
| CN112281128A (en) * | 2020-10-31 | 2021-01-29 | 贵阳学院 | Preparation method of perovskite type samarium ferrite target material for magnetron sputtering |
| CN114751460A (en) * | 2022-04-11 | 2022-07-15 | 北京化工大学 | Sol-gel preparation method of rare earth ferrite lutetium ferrite film |
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Application publication date: 20140326 |