CN109553409A - A kind of solid electrolyte film Li3PO4The preparation method and application of target - Google Patents
A kind of solid electrolyte film Li3PO4The preparation method and application of target Download PDFInfo
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- CN109553409A CN109553409A CN201811620256.7A CN201811620256A CN109553409A CN 109553409 A CN109553409 A CN 109553409A CN 201811620256 A CN201811620256 A CN 201811620256A CN 109553409 A CN109553409 A CN 109553409A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 11
- 229910001386 lithium phosphate Inorganic materials 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000005469 granulation Methods 0.000 claims abstract description 13
- 230000003179 granulation Effects 0.000 claims abstract description 11
- 238000000137 annealing Methods 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- 238000004544 sputter deposition Methods 0.000 claims abstract description 5
- 239000003792 electrolyte Substances 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 238000007731 hot pressing Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 238000000643 oven drying Methods 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 229910012305 LiPON Inorganic materials 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 102220043159 rs587780996 Human genes 0.000 description 2
- 239000002200 LIPON - lithium phosphorus oxynitride Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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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)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Physical Vapour Deposition (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses a kind of solid electrolyte film Li for belonging to ceramic target preparation technical field3PO4The preparation method and application of target.Specifically by Li3PO4Powder is placed in Cold pretreatment in Muffle furnace, and Li is made through granulation, hot pressed sintering, annealing, vacuum drying3PO4Target；Preparation method of the present invention is simple, easy to industrialized production, Li obtained3PO4Target dielectric constant is high, dielectric loss is low, relative density be it is controllable within the scope of 50%-100%, prepare all solid state electrolyte film suitable for sputtering.
Description
Technical field
The invention belongs to ceramic target preparation technical field, in particular to a kind of solid electrolyte film Li3PO4Target
Preparation method and application.
Background technique
The electrolyte of All-solid film batteries needs high ionic conductivity, low electronic conductivity, and can work
It is coexisted in potential range with positive and negative electrode stabilization.Amorphous LiPON (LiPON) is proved that can be used as one kind has prospect
Solid electrolyte material.The transition metal oxide yin of the lithium metal anode and high electrode current potential of LiPON and low electrode current potential
Pole is all highly stable when contacting, thus Li dendrite can be overcome well using LiPON electrolytic thin-membrane growth, passivation layer not
It is disconnected to thicken the problems such as low with battery cycle life.
The common preparation method of lithium phosphorus oxynitride is magnetron sputtering at present, and correlative study passes through in N2Middle radio frequency magnetron splashes
It penetrates and has been successfully prepared LiPON film；However, to obtain the LiPON electrolytic thin-membrane haveing excellent performance, high quality is needed
Li3PO4Target.
Summary of the invention
The purpose of the present invention is to provide a kind of solid electrolyte film Li3PO4The preparation method and application of target, tool
Body technique scheme is as follows:
A kind of solid electrolyte film Li3PO4The preparation method of target is specifically, by Li3PO4Powder is placed in Muffle furnace
Li is made through granulation, hot pressed sintering, annealing, vacuum drying in middle Cold pretreatment3PO4Target.
The Li3PO4Powder granularity is 10-100 μm, and purity is 99.9% or more.
The Cold pretreatment temperature is 100~300 DEG C.
Li after the granulation3PO4The median D50 of powder is 30-50 μm.
The hot pressed sintering specifically: powder after granulation is fitted into graphite jig and is placed in hot pressing furnace, is heated up after vacuumizing,
Temperature reaches 300~600 DEG C, applying argon gas pressurization；Temperature be raised to 600-1000 DEG C, pressure reach heat-insulation pressure keeping 1- after 10-50Mpa
8h；Heating power supply is closed, starts to cool down, temperature is down to 600~800 DEG C, and pressure release to normal pressure, furnace cooling obtains Li3PO4Blank.
The annealing temperature is 600-1000 DEG C.
To the Li obtained after the annealing3PO4Blank is machined, cleaned, drying and processing, and Li is made3PO4
Target.
The vacuum drying is vacuum oven drying, drying time 8-24h.
The Li3PO4Target purity >=99.9%, relative density 50%-100%, dielectric constant 5~10.
The Li of the preparation method preparation3PO4Target prepares all solid state electrolyte film for sputtering.
The invention has the benefit that
(1) present invention can remove Li by carrying out Cold pretreatment to raw material3PO4The remaining crystallization water, has in powder
Conducive to follow-up sintering process；Pretreated powder is granulated, the intensity for enhancing hot pressed sintering target is conducive to；
(2) present invention prepares Li using heat pressing process3PO4Target does not add any additive and carries out Ar-sintering,
Obtained target even density is controllable, and relative to pressureless sintering, required sintering temperature is greatly reduced；The present invention is not by
Same hot-pressing sintering technique, may be implemented Li3PO4Target density 50%-100% is controllable；
(3) present invention is using annealing Li3PO4Target blank can eliminate target internal residual stress, avoid sputtering
The problem of Shi Yingli causes target to crack；
(4) for target by the way of vacuum drying, relatively common drying is easier to removal Li after present invention annealing3PO4Target
The moisture of interior remaining；
(5) Li prepared by the present invention3PO4Target, dielectric constant is high, and dielectric loss is low, is conducive to improve Li3PO4Target exists
Stability in sputtering process.
Specific embodiment
The present invention provides a kind of solid electrolyte film Li3PO4The preparation method and application of target, below with reference to reality
Applying example, the present invention is described further.
Embodiment 1
Solid electrolyte film Li is prepared as steps described below3PO4Target:
(1) by the Li of purity 99.9%3PO4Powder is placed in Muffle furnace in 150 DEG C of progress Cold pretreatments, pre- to low temperature
Treated, and powder carries out granulation processing, D50=38 μm of the powder granularity after granulation；
(2) powder after granulation is packed into graphite jig and is placed in heating in vacuum in hot pressing furnace: started to warm up after vacuumizing, temperature
When reaching 500 DEG C, applying argon gas, and start to pressurize；When temperature is raised to 800 DEG C, pressure reaches 28Mpa, start heat-insulation pressure keeping；It protects
After warm pressure maintaining 2 hours, heating power supply is closed, starts to cool down；Etc. temperature be down to 600 DEG C, gradually slow pressure release, until normal pressure；With furnace
It is cooled to room temperature, takes out graphite jig and obtain Li3PO4Blank；
(3) by gained Li3PO4Blank is made annealing treatment at 800 DEG C, obtains Li3PO4Target blank；To Li3PO4Target
Material blank is machined, cleaned, vacuum drying, obtains Li3PO4Target.
Li prepared by embodiment 13PO4Target purity 99.9%, target sizeTarget relative density
87%, target dielectric constant 5.35.
Embodiment 2
Solid electrolyte film Li is prepared as steps described below3PO4Target:
(1) by the Li of purity 99.9%3PO4Powder is placed in Muffle furnace in 150 DEG C of progress Cold pretreatments, pre- to low temperature
Treated, and powder carries out granulation processing, D50=42 μm of the powder granularity after granulation；
(2) powder after granulation is packed into graphite jig and is placed in heating in vacuum in hot pressing furnace: started to warm up after vacuumizing, temperature
When reaching 500 DEG C, applying argon gas, and start to pressurize；When temperature is raised to 900 DEG C, pressure reaches 30Mpa, start heat-insulation pressure keeping；It protects
After warm pressure maintaining 6 hours, heating power supply is closed, starts to cool down；Etc. temperature be down to 650 DEG C, gradually slow pressure release, until normal pressure；With furnace
It is cooled to room temperature, takes out graphite jig and obtain Li3PO4Blank；
(3) by gained Li3PO4Blank is made annealing treatment at 900 DEG C, obtains Li3PO4Target blank；Target blank into
Row machining, cleaning, vacuum drying, obtain Li3PO4Target.
Li prepared by embodiment 23PO4Target purity 99.9%, 125 × 200 × 8mm of target size, target relative density
94%, target dielectric constant 6.29.
Claims (9)
1. a kind of solid electrolyte film Li3PO4The preparation method of target, which is characterized in that by Li3PO4Powder is placed in Muffle
Li is made through granulation, hot pressed sintering, annealing, vacuum drying in Cold pretreatment in furnace3PO4Target.
2. preparation method according to claim 1, which is characterized in that the Li3PO4Powder granularity is 10-100 μm.
3. preparation method according to claim 1, which is characterized in that the Cold pretreatment temperature is 100~300 DEG C.
4. preparation method according to claim 1, which is characterized in that Li after the granulation3PO4The median D50 of powder
It is 30-50 μm.
5. preparation method according to claim 1, which is characterized in that the hot pressed sintering specifically: by powder after granulation
It is fitted into graphite jig to be placed in hot pressing furnace, heat up after vacuumizing, temperature reaches 300~600 DEG C, applying argon gas pressurization；Temperature is raised to
600-1000 DEG C, pressure reach heat-insulation pressure keeping 1-8h after 10-50Mpa；600~800 DEG C are cooled to, pressure release to normal pressure is cold with furnace
But Li is obtained3PO4Blank.
6. preparation method according to claim 1, which is characterized in that the annealing temperature is 600-1000 DEG C.
7. preparation method according to claim 1, which is characterized in that the vacuum drying is vacuum oven drying, is dried
The dry time is 8-24h.
8. preparation method according to claim 1, which is characterized in that the Li3PO4Target purity >=99.9%, it is relatively close
Degree is 50%-100%, dielectric constant 5~10.
9. the Li of any one of the claim 1~8 preparation method preparation3PO4To prepare all solid state electrolyte thin for sputtering for target
Film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811620256.7A CN109553409A (en) | 2018-12-28 | 2018-12-28 | A kind of solid electrolyte film Li3PO4The preparation method and application of target |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811620256.7A CN109553409A (en) | 2018-12-28 | 2018-12-28 | A kind of solid electrolyte film Li3PO4The preparation method and application of target |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627481A (en) * | 2019-10-18 | 2019-12-31 | 先导薄膜材料（广东）有限公司 | High-purity Ga2O3Preparation method of target material |
| 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 |
| CN116253570A (en) * | 2023-03-20 | 2023-06-13 | 超威电源集团有限公司 | LiPON target material and preparation method and application of film |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627481A (en) * | 2019-10-18 | 2019-12-31 | 先导薄膜材料（广东）有限公司 | High-purity Ga2O3Preparation method of target material |
| CN110627481B (en) * | 2019-10-18 | 2022-07-12 | 先导薄膜材料（广东）有限公司 | High-purity Ga2O3Preparation method of target material |
| 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 |
| CN116253570A (en) * | 2023-03-20 | 2023-06-13 | 超威电源集团有限公司 | LiPON target material and preparation method and application of film |
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