CN108530054A - The preparation method of target used in a kind of all solid state electrolyte thin film sputtering - Google Patents

The preparation method of target used in a kind of all solid state electrolyte thin film sputtering Download PDF

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Publication number
CN108530054A
CN108530054A CN201810460996.2A CN201810460996A CN108530054A CN 108530054 A CN108530054 A CN 108530054A CN 201810460996 A CN201810460996 A CN 201810460996A CN 108530054 A CN108530054 A CN 108530054A
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target
preparation
solid state
sio
ball
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Inventor
薛文东
王玉田
戎马屹飞
胡凯
王兴宇
白立雄
李勇
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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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
    • C04B35/447—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 based on phosphates, e.g. hydroxyapatite
    • 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
    • C04B35/16—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 based on silicates other than clay
    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
    • C04B2235/3203—Lithium oxide or oxide-forming salts thereof

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The preparation method of target, belongs to field of lithium ion battery used in a kind of all solid state electrolyte thin film sputtering.Target material composition is Li3PO4·Li2SiO3Target is made using the method for compacting sintering, and preparation process is as follows：(1) by the Li of SILVER REAGENT2CO3, SiO2And NH4H2PO4It mixes according to a certain percentage；(2) by mixture and Al2O3Ball mixes, ratio of grinding media to material 1:12, abrasive media is deionized water；Ball milling is carried out in ball grinder, Ball-milling Time is 45 51h, and PEG 2000 is added in ball milling last 4 hours；(3) after ball milling, powder is dried into 22 26h, carries out sieving and granulation processing；(4) powder pressing is molded by the way of dry-pressing formed；(5) it and then is sintered in air and obtains Li3PO4·Li2SiO3Target, a diameter of 76.2mm of target, thickness 3mm.The target consistency that the method for the present invention is prepared is higher, has enough purity and intensity.

Description

The preparation method of target used in a kind of all solid state electrolyte thin film sputtering
Technical field
The invention belongs to the preparation methods of target used in field of lithium ion battery more particularly to solid electrolyte film.
Background technology
With the continuous micromation of electronic device, people increasingly pay attention to the research to solid-State Thin Film Li-Ion Batteries. The performance of lithium ion battery depends on the structure and performance of inside battery material.Wherein solid state thin-film electrolyte is that restriction is cell performance The key that can be further promoted.
It is the LiPON films of U.S.'s Oak Ridge National Laboratory research and development that electrolytic thin-membrane is widely used at present.LiPON is thin All highly stable, the institute when transition metal oxide cathode of the lithium metal anode and high electrode current potential of film and low electrode current potential contacts With using LiPON electrolytic thin-membranes can be very good to overcome lithium dendrite growth, passivation layer constantly thicken and battery cycle life The problems such as low, becomes a kind of electrolytic thin-membrane being widely used in solid lithium battery.
LiPON films have many advantages, such as electrolyte, but its reduction problem susceptible to hydrolysis in wet environment is tight The development of LiPON films used and hinder solid-state thin-film battery is inhibited again.This problem can pass through doped metal ion To improve the stability of LiPON films and prepare corresponding ceramic target by doping phosphoric acid powder for lithium.In view of target Quality equally determines the quality of deposition film, it is necessary to be unfolded to study to this content.The present invention prepares doping Si's Li3PO4Li2SiO3 targets.
Invention content
The object of the present invention is to provide consistency height is obtained, intensity is big, the high Li of purity3PO4·Li2SiO3The system of target Preparation Method.
The purpose of the present invention is what is be achieved through the following technical solutions：
The preparation method of target used in a kind of all solid state electrolyte thin film sputtering, it is characterised in that target material composition is Li3PO4·Li2SiO3Target is made using the method for compacting sintering, and specific preparation process is as follows：
(1) by the Li of SILVER REAGENT2CO3, SiO2And NH4H2PO4It mixes according to a certain percentage；
(2) by mixture and Al2O3Ball mixes, ratio of grinding media to material 1:12, abrasive media is deionized water；In ball grinder into PEG-2000 is added in ball milling last 4 hours in row ball milling, Ball-milling Time 45-51h；
(3) after ball milling, powder is dried into 22-26h, carries out sieving and granulation processing；
(4) powder pressing is molded by the way of dry-pressing formed；
(5) it and then is sintered in air and obtains Li3PO4·Li2SiO3Target.
Further, the target a diameter of 76.2mm, thickness 3mm of preparation.
Further, the Li2CO3, SiO2And NH4H2PO4Mixed proportion be 20-30%, 30-40%, 40%.
Further, mixture and Al2O3Ball mixes, ratio of grinding media to material 1:12, the liquid-solid ratio of deionized water and raw material is 1:1.
Further, the amount of the PEG-2000 of the addition is the 5% of powder amount.
Further, the sintering process is to be sintered 4-6h at 900-1200 DEG C in air.
In the present invention, sieving is and then to filter out to remove some mechanical impurity in powder and meet granularity requirements Powder particle.
In the present invention, the method being granulated using roller, time control is in 5-20min.
The advantages of target prepared in the present invention is that consistency is higher, and intensity is big, and purity is high.
Specific implementation mode
By silicon/lithium phosphate Li3PO4·Li2SiO3Then mixture is sintered at 900-1200 DEG C in air by compacting 5h obtains Li3PO4·Li2SiO3Target.
Embodiment one
Ball milling, by the Li of SILVER REAGENT2CO3, SiO2And NH4H2PO4It is mixed according to 20%, 40%, 40% ratio, grinding medium Matter is deionized water, and mill ball Al2O3, liquid-solid ratio example is 1:1, ball milling terminates first four hour, and 5wt.%PEG- is added 2000 forming agent,.
After ball milling, for 24 hours by powder drying, sieving and granulation processing are carried out.By powder pressing by the way of dry-pressing formed At the green body that size is 76.2mm × 3mm.
Then sintering 5h obtains Li at 900-1200 DEG C in air3PO4·Li2SiO3Target.
Embodiment two
Ball milling, by the Li of SILVER REAGENT2CO3, SiO2And NH4H2PO4It is mixed according to 25%, 35%, 40% ratio, grinding medium Matter is deionized water, mill ball Al2O3, liquid-solid ratio example is 1:1, ball milling terminates first four hour, and 5wt.%PEG-2000 is added Forming agent,.
After ball milling, for 24 hours by powder drying, sieving and granulation processing are carried out.By powder pressing by the way of dry-pressing formed At the green body that size is 76.2mm × 3mm.
Then sintering 5h obtains Li at 900-1200 DEG C in air3PO4·Li2SiO3Target.
Embodiment three
Ball milling, by the Li of SILVER REAGENT2CO3, SiO2And NH4H2PO4It is mixed according to 30%, 30%, 40% ratio, grinding medium Matter is deionized water, mill ball Al2O3, liquid-solid ratio example is 1:1, ball milling terminates first four hour, and 5wt.%PEG-2000 is added Forming agent,.
After ball milling, for 24 hours by powder drying, sieving and granulation processing are carried out.By powder pressing by the way of dry-pressing formed At the green body that size is 76.2mm × 3mm.
Then sintering 5h obtains Li at 900-1200 DEG C in air3PO4·Li2SiO3Target.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art The modification that not creative contribution can be made to the present embodiment as needed after reading this specification, but as long as in this hair Protection scope of the present invention is belonged in bright right.

Claims (7)

1. the preparation method of target used in a kind of all solid state electrolyte thin film sputtering, it is characterised in that target material composition Li3PO4· Li2SiO3Target is made using the method for compacting sintering, and specific preparation process is as follows：
(1) by the Li of SILVER REAGENT2CO3, SiO2And NH4H2PO4It mixes according to a certain percentage；
(2) by step (1) mixture and Al2O3Ball mixes, and abrasive media is deionized water；Ball milling, ball milling are carried out in ball grinder Time is 45-51h, and PEG-2000 is added in ball milling last 4 hours；
(3) after ball milling, powder is dried into 22-26h, carries out sieving and granulation processing；
(4) powder pressing is molded by the way of dry-pressing formed；
(5) it and then is sintered in air and obtains Li3PO4·Li2SiO3Target.
2. the preparation method of target used in all solid state electrolyte film according to claim 1, it is characterised in that the target Material a diameter of 76.2mm, thickness 3mm.
3. the preparation method of target used in all solid state electrolyte film according to claim 1, it is characterised in that step (1) The Li2CO3, SiO2And NH4H2PO4Mixed proportion be 20-30%, 30-40%, 40%.
4. the preparation method of target used in all solid state electrolyte film according to claim 1, it is characterised in that step (2) The mixture and Al2O3Ball mixes, ratio of grinding media to material 1:12, the liquid-solid ratio of deionized water and raw material is 1:1.
5. the preparation method of target used in all solid state electrolyte film according to claim 1, it is characterised in that step (2) The amount of the PEG-2000 of the addition is the 5% of powder amount.
6. the preparation method of target used in all solid state electrolyte film according to claim 1, it is characterised in that described to make Grain processing is granulated using roller, and time control is in 5-20min.
7. the preparation method of target used in all solid state electrolyte film according to claim 1, it is characterised in that sintered Journey is to be sintered 4-6h at 900-1200 DEG C in air.
CN201810460996.2A 2018-05-15 2018-05-15 The preparation method of target used in a kind of all solid state electrolyte thin film sputtering Pending CN108530054A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1860628A (en) * 2004-10-21 2006-11-08 松下电器产业株式会社 Negative electrode for battery and battery using same
CN106252720A (en) * 2016-08-30 2016-12-21 兰州空间技术物理研究所 A kind of preparation method of high ionic conductivity electrolytic thin-membrane
JP2018016858A (en) * 2016-07-28 2018-02-01 Ｊｘ金属株式会社 Sputtering target composed of sintered body of lithium oxide and lithium phosphate and manufacturing method of the same
CN107665974A (en) * 2016-07-27 2018-02-06 中国科学院大连化学物理研究所 A kind of lithium-sulfur cell negative pole and its preparation and application

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1860628A (en) * 2004-10-21 2006-11-08 松下电器产业株式会社 Negative electrode for battery and battery using same
CN107665974A (en) * 2016-07-27 2018-02-06 中国科学院大连化学物理研究所 A kind of lithium-sulfur cell negative pole and its preparation and application
JP2018016858A (en) * 2016-07-28 2018-02-01 Ｊｘ金属株式会社 Sputtering target composed of sintered body of lithium oxide and lithium phosphate and manufacturing method of the same
CN106252720A (en) * 2016-08-30 2016-12-21 兰州空间技术物理研究所 A kind of preparation method of high ionic conductivity electrolytic thin-membrane

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
申万等: "固态薄膜电解质LiSiPON和其性能研究", 《电源技术》 *

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