CN102249661A - Lithium phosphate target and preparation method thereof - Google Patents
Lithium phosphate target and preparation method thereof Download PDFInfo
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- CN102249661A CN102249661A CN 201110167850 CN201110167850A CN102249661A CN 102249661 A CN102249661 A CN 102249661A CN 201110167850 CN201110167850 CN 201110167850 CN 201110167850 A CN201110167850 A CN 201110167850A CN 102249661 A CN102249661 A CN 102249661A
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Abstract
The invention discloses a lithium phosphate target and a preparation method thereof. The target has the purity of more than or equal to 99.9 percent, the relative density of more than or equal to 98 percent and the average grain size of less than or equal to 50 micrometers. The preparation method for the target comprises the following steps of: (1) providing lithium phosphate powder, and hydraulically forming the lithium phosphate powder into a blank; (2) performing cold isostatic pressing processing on the blank; and (3) sintering the blank undergoing the step (2) in a furnace, wherein a multi-stage heating and pressurization mode is adopted in the sintering process. The lithium phosphate target prepared by the method has fine grain size and high density. Under proper conditions, the target is sputtered and a thin film with good performance can be obtained, so that the energy storage capacity and cycle times of an all-solid-state thin film lithium battery are increased.
Description
Technical field
The present invention relates to a kind of Trilithium phosphate target and preparation method thereof.
Background technology
The fast development of electron device microminiaturizations such as transmitter, MEMS, CMOS chip requires to have miniature fine and close power supply and its coupling that volume is little, in light weight, specific storage is high.Solid-State Thin Film Li-Ion Batteries is owing to have high power density, low self-discharge rate, good charge-discharge performance, shape and size and can design arbitrarily, and do not have that solution leaks, do not explode, advantage such as safe in utilization, obtain extensive concern in recent years at home and abroad, part country has realized suitability for industrialized production.This class battery can be used as the independence or the standby power supply of various portable microelectronic devices, and the power supply of MEMS, has still militarily all shown wide application prospect civilian.Solid-State Thin Film Li-Ion Batteries all has its ample scope for abilities in different field, as in space industry, this microbattery miniaturization, lightweight have considerable magnetism to aerospacecraft; Militarily, the jet laboratory of jet (JPL) of U.S. Sandia National Laboratory, Oak Ridge National Laboratory (ORNL), NASA (NASA) and The Air Force Research Laboratory all are used for film lithium ion battery at active development the microbattery chip technology of weapon Intellectualized monitoring and management system; Its purposes also comprises: miniature robot surveillance plane electrical source of power (comprising the camera head power supply), multiple microsensor, CMOS integrated circuit, smart card (SmartCard), biochip and intravital micro surgical tool of people and mini-medical device etc.
The core component electrolyte of solid-State Thin Film Li-Ion Batteries is the focus that people pay close attention to always, and Dui Ying film performance has directly determined the capacity and the work-ing life of battery with it.Therefore, superior in quality target also will become even more important.Generally speaking the production method of Trilithium phosphate target has four kinds of ordinary sinter method, hot isostatic pressing method, pressure sintering and pressure sinterings.Being compared as follows of these four kinds of methods:
1, ordinary sinter method: general employing is colded pressing and is added the preparation of agglomerating method.In the cold pressure procedure, in order to strengthen the formability of biscuit, can add 0.5%～2% binding agent therein, pressing pressure can not be too big, discharge by binding agent because need reserve enough passages, but that binding agent still has is residual, increased the foreign matter content of target.Because the relative density of biscuit is 60%～70%, after the target sintering was finished, the relative density of target can only reach 70%～90%.
, hot isostatic pressing method: this method can be more than pressure 100MPa, and sintering temperature is 600 ℃～1500 ℃ sintering targets, obtains relative density and be 98%～100% target.But this method technological process is complicated, mainly comprise: the powder pre-treatment, make jacket, shove charge sintering, remove jacket, following process etc., and finishing of each step have relatively high expectations, if target is less, the amount of finish of following process is bigger, and then utilization rate of raw materials is lower.
, pressure sintering: this method can be used refractory metal mould, ceramic die or graphite jig, carries out sintering under vacuum or other atmosphere protections, and general sintering pressure is 20～80MPa, can obtain relative density and be 98%～100% target.This method production cost is lower, and technological process is comparatively simple, mainly comprises: charging, sintering, the demoulding, following process etc., and also each step control is comparatively simple, and the stay in grade of product can obtain the work in-process near the product requirement size.
, the pressure sintering method: this method generally is used to produce ceramic target, carries out sintering under the condition of atmosphere protection, and sintering processing is the stage intensification of boosting.This production method cost is lower, and technological process is controlled, and key step comprises: hydraulic pressure compacting, isostatic cool pressing compacting, interim sintering, cooling control, following process etc., and each step simple to operate, core technology is a sintering process.
Yet its grain-size of Trilithium phosphate target of preparing according to the normal pressure atmosphere sintering process of prior art is bigger, and density is not high yet.Under proper condition, used the energy storage capacity and the cycle index of solid-State Thin Film Li-Ion Batteries of the resulting films of these targets of sputter also lower.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of Trilithium phosphate target and preparation method thereof is provided.
For solving above technical problem, the technical scheme that the present invention takes is: a kind of Trilithium phosphate target, its purity more than or equal to 99.9%, relative density more than or equal to 98%, average grain size is smaller or equal to 50 microns.
Preferably, the purity of described Trilithium phosphate target is more than or equal to 99.99%.
Further preferably, the purity of described Trilithium phosphate target is more than or equal to 99.999%.
Preferably, the relative density of described Trilithium phosphate target is more than or equal to 99%.
Preferably, the average crystal grain of described Trilithium phosphate target is smaller or equal to 10 microns.
A kind of preparation method of Trilithium phosphate target may further comprise the steps:
(1), the Trilithium phosphate powder is provided, and be blank with its shaped by fluid pressure;
(2), described blank is carried out isostatic cool pressing processing;
(3), will place stove to carry out sintering through the blank of step (2), during sintering, vacuum tightness is 10 in the stove
-4
~ 10
-3
Pa, at first the speed with 50 ~ 300 ℃/h rises to 600 ℃ ~ 800 ℃ with temperature, be incubated after 4 ~ 24 hours, charge into oxygen, and then temperature is risen to 800 ℃ ~ 900 ℃ with the speed of 100 ~ 400 ℃/h, be incubated after 4 ~ 24 hours, and then temperature risen to 900 ℃ ~ 1200 ℃ with the speed of 100 ~ 400 ℃/h, be incubated and reduce to normal temperature after 4 ~ 24 hours and promptly get described Trilithium phosphate target, rate of temperature fall is 20 ~ 100 ℃/h.
Preferably, in the step (1), the purity of described Trilithium phosphate powder is 99.90% ~ 99.99%, median size is 50 ~ 100nm.
Preferably, in the step (1), the operating pressure of described shaped by fluid pressure is 5 ~ 50MPa.
Preferably, in the step (2), the operating pressure of carrying out isostatic cool pressing processing is 200 ~ 300MPa.
Because the utilization of technique scheme, the present invention compared with prior art has following advantage and effect: owing in interim sintering process, charged into oxygen, avoided introducing impurity in the environment sintering process, also made target high densification more.According to the Trilithium phosphate target that preparation method of the present invention prepares, its grain-size is tiny and density is high.Under proper condition, the good film of these targets energy obtained performances of sputter, thereby the energy storage capacity and the cycle index of raising solid-State Thin Film Li-Ion Batteries.
Description of drawings
Fig. 1 is the sem photograph of the Trilithium phosphate target prepared according to method of the present invention.
Embodiment
Below the present invention is further detailed explanation, but the invention is not restricted to this embodiment.
According to present embodiment, prepare the Trilithium phosphate target as follows:
(1), be that 100nm, purity are that 99.95% Trilithium phosphate powder is a raw material with the median size, by grind, the method for screening removes the caking in the powder; Adopting hydropress is blank with the Trilithium phosphate powder hydraulic forming, and the pressure that moulding is used is 30MPa;
(2), blank is carried out isostatic cool pressing compacting, pressing pressure is 250MPa, and isostatic cool pressing processing can improve the compactness of blank, and the biscuit relative density after repressed is 60%;
(3), for guaranteeing in the high-temperature sintering process that flow and the bonding orderly stage of material are carried out, sintering process adopts multistage intensification pressing mode to finish sintering.Place stove to carry out sintering the blank after the compacting, during sintering, vacuum tightness is 8.0 * 10 in the stove -4 Pa rises to 600 ℃ with 100 ℃/h speed with temperature, is incubated and charges into 1atm oxygen after 8 hours, and then be warming up to 800 ℃ with the speed of 100 ℃/h,
Be incubated and charge into 8atm oxygen after 8 hours, and then temperature is risen to 1000 ℃, be incubated that the speed with 50 ℃/h cools the temperature to normal temperature after 6 hours with the speed of 200 ℃/h.
The target for preparing is taken out, with the mill method for processing target is worked into specified size then.
Trilithium phosphate target to above-mentioned preparation carries out scanning electron microscope analysis, and Fig. 1 is the gained sem photograph, therefrom can find out, the grain-size of Trilithium phosphate target is more tiny and density is high, and relative density is about 99.4%.
The foregoing description only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (9)
1. Trilithium phosphate target is characterized in that: the purity of described Trilithium phosphate target more than or equal to 99.9%, relative density more than or equal to 98%, average grain size is smaller or equal to 50 microns.
2. Trilithium phosphate target according to claim 1 is characterized in that: the purity of described Trilithium phosphate target is more than or equal to 99.99%.
3. Trilithium phosphate target according to claim 2 is characterized in that: the purity of described Trilithium phosphate target is more than or equal to 99.999%.
4. Trilithium phosphate target according to claim 1 is characterized in that: the relative density of described Trilithium phosphate target is more than or equal to 99%.
5. Trilithium phosphate target according to claim 1 is characterized in that: the average crystal grain of described Trilithium phosphate target is smaller or equal to 10 microns.
6. the preparation method of a Trilithium phosphate target is characterized in that, said method comprising the steps of:
(1), the Trilithium phosphate powder is provided, and be blank with its shaped by fluid pressure;
(2), described blank is carried out isostatic cool pressing processing;
(3), will place stove to carry out sintering through the blank of step (2), during sintering, vacuum tightness is 10 in the stove
-4~ 10
-3Pa, at first the speed with 50 ~ 300 ℃/h rises to 600 ℃ ~ 800 ℃ with temperature, be incubated after 4 ~ 24 hours, charge into oxygen, and then temperature is risen to 800 ℃ ~ 900 ℃ with the speed of 100 ~ 400 ℃/h, be incubated after 4 ~ 24 hours, and then temperature risen to 900 ℃ ~ 1200 ℃ with the speed of 100 ~ 400 ℃/h, be incubated and reduce to normal temperature after 4 ~ 24 hours and promptly get described Trilithium phosphate target, rate of temperature fall is 20 ~ 100 ℃/h.
7. the preparation method of Trilithium phosphate target according to claim 6 is characterized in that: in the step (1), the purity of described Trilithium phosphate powder is 99.90% ~ 99.99%, median size is 50 ~ 100nm.
8. the preparation method of Trilithium phosphate target according to claim 6 is characterized in that: in the step (1), the operating pressure of described shaped by fluid pressure is 5 ~ 50MPa.
9. the preparation method of Trilithium phosphate target according to claim 6 is characterized in that: in the step (2), the operating pressure of carrying out isostatic cool pressing processing is 200 ~ 300MPa.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584205A (en) * | 2012-02-21 | 2012-07-18 | 苏州晶纯新材料有限公司 | Method for manufacturing yttrium barium copper oxide target |
| JP2013216553A (en) * | 2012-04-11 | 2013-10-24 | Kobelco Kaken:Kk | Li-CONTAINING PHOSPHORIC ACID COMPOUND SINTERED BODY AND SPUTTERING TARGET, AND METHOD FOR MANUFACTURING THE SAME |
| CN105256275A (en) * | 2015-11-03 | 2016-01-20 | 基迈克材料科技（苏州）有限公司 | Electrolyte layer material lithium phosphate target material powder metallurgy preparation technology for thin film lithium batteries |
| CN105385996A (en) * | 2015-11-03 | 2016-03-09 | 基迈克材料科技（苏州）有限公司 | Powder metallurgy preparation technology of anode material lithium cobalt oxide targets for thin film lithium battery |
| CN105984904A (en) * | 2016-01-07 | 2016-10-05 | 惠州市佰特瑞科技有限公司 | Preparation method of lithium nickelate target |
| CN114057480A (en) * | 2021-11-17 | 2022-02-18 | 鄂尔多斯市紫荆创新研究院 | Lithium phosphate solid electrolyte target material for preparing thin film lithium battery and preparation method |
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| CN102206802A (en) * | 2010-03-29 | 2011-10-05 | 北京品一材料科技有限责任公司 | All-solid-state film lithium ion battery related target material and manufacturing method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584205B (en) * | 2012-02-21 | 2013-07-10 | 苏州晶纯新材料有限公司 | Method for manufacturing yttrium barium copper oxide target |
| CN102584205A (en) * | 2012-02-21 | 2012-07-18 | 苏州晶纯新材料有限公司 | Method for manufacturing yttrium barium copper oxide target |
| KR101648656B1 (en) * | 2012-04-11 | 2016-08-16 | 가부시키가이샤 코베루코 카겐 | Li-CONTAINING PHOSPHATE COMPOUND SINTERED BODY AND SPUTTERING TARGET, AND METHOD FOR MANUFACTURING SAID Li-CONTAINING PHOSPHATE COMPOUND SINTERED BODY |
| JP2013216553A (en) * | 2012-04-11 | 2013-10-24 | Kobelco Kaken:Kk | Li-CONTAINING PHOSPHORIC ACID COMPOUND SINTERED BODY AND SPUTTERING TARGET, AND METHOD FOR MANUFACTURING THE SAME |
| KR20140143173A (en) * | 2012-04-11 | 2014-12-15 | 가부시키가이샤 코베루코 카겐 | Li-CONTAINING PHOSPHORIC-ACID COMPOUND SINTERED BODY AND SPUTTERING TARGET, AND METHOD FOR MANUFACTURING SAID Li-CONTAINING PHOSPHORIC-ACID COMPOUND SINTERED BODY |
| CN104245623A (en) * | 2012-04-11 | 2014-12-24 | 株式会社钢臂功科研 | Li-CONTAINING PHOSPHORIC-ACID COMPOUND SINTERED BODY AND SPUTTERING TARGET, AND METHOD FOR MANUFACTURING SAID LI-CONTAINING PHOSPHORIC-ACID COMPOUND SINTERED BODY |
| EP2837610A1 (en) * | 2012-04-11 | 2015-02-18 | Kobelco Research Institute, Inc. | Li-CONTAINING PHOSPHORIC-ACID COMPOUND SINTERED BODY AND SPUTTERING TARGET, AND METHOD FOR MANUFACTURING SAID LI-CONTAINING PHOSPHORIC-ACID COMPOUND SINTERED BODY |
| US9892891B2 (en) | 2012-04-11 | 2018-02-13 | Kobelco Research Institute, Inc. | Li-containing phosphoric-acid compound sintered body and sputtering target, and method for manufacturing said Li-containing phosphoric-acid compound sintered body |
| CN105256275A (en) * | 2015-11-03 | 2016-01-20 | 基迈克材料科技（苏州）有限公司 | Electrolyte layer material lithium phosphate target material powder metallurgy preparation technology for thin film lithium batteries |
| CN105385996A (en) * | 2015-11-03 | 2016-03-09 | 基迈克材料科技（苏州）有限公司 | Powder metallurgy preparation technology of anode material lithium cobalt oxide targets for thin film lithium battery |
| CN105984904A (en) * | 2016-01-07 | 2016-10-05 | 惠州市佰特瑞科技有限公司 | Preparation method of lithium nickelate target |
| CN114057480A (en) * | 2021-11-17 | 2022-02-18 | 鄂尔多斯市紫荆创新研究院 | Lithium phosphate solid electrolyte target material for preparing thin film lithium battery and preparation method |
| CN114057480B (en) * | 2021-11-17 | 2023-03-14 | 鄂尔多斯市紫荆创新研究院 | Lithium phosphate solid electrolyte target material for preparing thin film lithium battery and preparation method |
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