CN107026018A - A kind of solid film capacitor with self-repair function and preparation method thereof - Google Patents
A kind of solid film capacitor with self-repair function and preparation method thereof Download PDFInfo
- Publication number
- CN107026018A CN107026018A CN201710135137.1A CN201710135137A CN107026018A CN 107026018 A CN107026018 A CN 107026018A CN 201710135137 A CN201710135137 A CN 201710135137A CN 107026018 A CN107026018 A CN 107026018A
- Authority
- CN
- China
- Prior art keywords
- self
- aluminium
- capacitor
- solid film
- repair function
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003990 capacitor Substances 0.000 title claims abstract description 95
- 239000007787 solid Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000011521 glass Substances 0.000 claims abstract description 69
- 239000004411 aluminium Substances 0.000 claims abstract description 53
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 53
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 53
- 230000000694 effects Effects 0.000 claims abstract description 37
- 239000000758 substrate Substances 0.000 claims abstract description 16
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 34
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- CFOAUMXQOCBWNJ-UHFFFAOYSA-N [B].[Si] Chemical compound [B].[Si] CFOAUMXQOCBWNJ-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 238000000576 coating method Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000004210 ether based solvent Substances 0.000 claims description 15
- 230000001476 alcoholic effect Effects 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 14
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 13
- 239000004327 boric acid Substances 0.000 claims description 13
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 13
- 238000001704 evaporation Methods 0.000 claims description 12
- 230000008020 evaporation Effects 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229960000583 acetic acid Drugs 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 9
- 239000012362 glacial acetic acid Substances 0.000 claims description 9
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 230000004044 response Effects 0.000 claims description 4
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 241000165940 Houjia Species 0.000 claims 1
- 239000003792 electrolyte Substances 0.000 abstract description 14
- 238000004146 energy storage Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000010408 film Substances 0.000 description 76
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 41
- 230000007547 defect Effects 0.000 description 11
- 230000005611 electricity Effects 0.000 description 10
- 230000037427 ion transport Effects 0.000 description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 229910052796 boron Inorganic materials 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 229910052715 tantalum Inorganic materials 0.000 description 5
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 230000008439 repair process Effects 0.000 description 2
- 239000006163 transport media Substances 0.000 description 2
- 206010020741 Hyperpyrexia Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000011104 metalized film Substances 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/33—Thin- or thick-film capacitors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/10—Metal-oxide dielectrics
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
- Semiconductor Integrated Circuits (AREA)
Abstract
The present invention relates to a kind of solid film capacitor with self-repair function and preparation method thereof, the capacitor includes substrate base (1), lower electrode (2), activity glass doped aluminium film (3), upper electrode (4), described lower electrode (2) is coated on substrate base (1) surface, and described activity glass doped aluminium film (3) is arranged between upper electrode (4) and lower electrode (2).Compared with prior art, the present invention has structure and preparation technology simple, and dielectric properties are good, can realize selfreparing, and energy storage density is high, and uses solid film as dielectric, the advantages of inside is not present electrolyte, thus safe and reliable.
Description
Technical field
The invention belongs to technical field of capacitor preparation, be related to a kind of solid film capacitor with self-repair function and
Its preparation method.
Background technology
During the manufacture and use of capacitor, deielectric-coating inevitably various defects are realized
One of key technology that deielectric-coating works under high field is dielectric defect self-healing or selfreparing.Tradition has self-repair function
Capacitor have aluminium electrolutic capacitor, tantalum electrolytic capacitor and metallic film capacitor etc..
Aluminium electrolutic capacitor be using electrolyte as negative electrode, in the presence of outer making alive, the O in non-solid electrolyte2-
Rapidly it is transported to fault location and the Al for ionizing out from aluminium substrate3+With reference to, oxide-film is re-formed at oxide-film destruction,
Capacitor is set to recover normal work ability, this ability is referred to as self-healing or the self-repair function of electrolytic capacitor.Tantalum solid capacitor
The self-healing action of device mainly flows through high current in the fault location of tantalum pentoxide film and produces hyperpyrexia, makes the MnO as negative electrode2
Material is decomposed into the Mn of high resistant2O3, make metal tantalum aoxidize to form oxide-film while discharging oxygen, defect blocked, and then repair scarce
Fall into the influence caused.Metallic film capacitor is the surface evaporation layer of metal film in polyester film instead of metal foil conduct
Electrode.When the minute portions of electrode cause short circuit because of dielectric fragility, cause the electrode metal of short-circuit peripheral portion, meeting
Because of the electrostatic energy or short circuit current flow of capacitor institute band at that time, and trigger it is greater area of dissolve and evaporate and recover insulation, make
Capacitor recovers the effect of capacitor once again.
The self-healing feature of electrolytic capacitor is only the small weakness of part for repairing electrolytic capacitor, is lacked for great
Fall into, big leakage current such as occur, puncture, then capacitor failure is inevitable.For aluminium electrolutic capacitor, its capacitance
It is low, it is bulky, it is necessary to which electrolyte realizes its defect selfreparing.But make capacitor just because of the presence of these electrolyte
Safety and reliability is greatly affected, such as the leakage problem of electrolyte；After electrolytic capacitor works long hours, electrolyte
Caused capacitor explosion issues；In electrolytic capacitor, electrolyte and its protection device occupy big quantity space, significantly limit
The problems such as raising of its energy storage density；With electrolyte dry-out in aluminium electrolutic capacitor, the cathode areas meeting of aluminium electrolutic capacitor
Greatly reduce, while the distance of positive and negative electrode also increases therewith, and this increase is no longer the high aluminum oxide of dielectric constant, this
The capacitance of sample aluminium electrolutic capacitor will be greatly reduced and fail, and make the problem of aluminium electrolutic capacitor has short life.Tantalum solid-state
Capacitor is because of the MnO using solid-state2As electrolyte, safety and stability are all better than electrolytic capacitor, but its is expensive, electricity
Capacity is smaller, is of limited application, and the MnO in tantalum capacitor2The volume ratio occupied is larger, can so limit its own storage
The raising of energy density.Metallic film capacitor also has its inherent shortcoming：One is due to metallized capacitance in long-term work condition
In easily occur capacity lose and self-healing after capacity can be caused to reduce；Further drawback for tolerance high current ability it is poor, this be by
Thinner than metal foil much in layer of metallized film, carrying high current ability is weaker.
In addition, Chinese patent CN103971933A discloses a kind of solid film capacitor and preparation method thereof, this electricity
(ion near particularly at dielectric defect is more using active oxidation aluminium film ion transport active under high field for container
It is active), the electrode interface near ion transport to defect is realized into anodic oxidation, and then realize the selfreparing of fault location.With
Aluminium electrolutic capacitor is different, liquid electrolyte is not present in such a capacitor, but use the active oxygen acted on electrolyte
Change aluminium solid film as the provider of oxygen in anodic oxidation, it is to avoid electrolyte has the problem of bringing, but the capacitor
Need to regenerate a kind of oxide-film of barrier type between pellumina and electrode and repaired, therefore limit electrode needs
It is valve metal with anodic oxidation function etc., thus strongly limit its application conditions.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind has selfreparing work(
Solid film capacitor of energy and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions：A kind of solid film electricity with self-repair function
Container, it is characterised in that the capacitor includes substrate base, lower electrode, activity glass doped aluminium film, top electricity
Pole, described lower electrode is coated on substrate base surface, and described activity glass doped aluminium film is arranged on top
Between electrode and lower electrode.
It is thin that described lower electrode and the material of upper electrode include Al films, Au films, Pt films, Ti films or Ag
Film.
The thickness of described lower electrode is 100~150nm, and described upper electrode thickness is 50~150nm.
Doped-glass in described activity glass doped aluminium film is silicon boron glass.
The thickness of described activity glass doped aluminium film is 150~250nm.
A kind of preparation method of the solid film capacitor with self-repair function, it is characterised in that the preparation method bag
Include following steps：
(1) glass sol precursor is prepared：Tetraethyl orthosilicate is added in water, the alcoholic solution of hydrochloric acid, normal temperature mixing is stirred
Mix, then add the alcoholic solution of boric acid, be stirred at room temperature, obtain silicon boron glass colloidal sol；
(2) aluminium-alcohol salt is ground, be subsequently added in alcohol ether solvents, 60~70 DEG C of constant temperature stir 30~60min, so
After add silicon boron glass colloidal sol made from appropriate step (1), 60~70 DEG C of constant temperature stir 30~60min, add acetylacetone,2,4-pentanedione,
70~80 DEG C of constant temperature stir 30~60min, are eventually adding glacial acetic acid, and 30~60min, question response knot are stirred in 80~90 DEG C of constant temperature
Shu Hou, is gradually cooling to room temperature, filtering, and activity glass doped aluminium sol precursor is made；
(3) layer of conductive film is prepared on substrate base using evaporation coating method or magnetron sputtering method, is used as bottom electricity
Pole；
(4) activity glass doped aluminium sol precursor made from step (2) is coated in bottom made from step (3)
On electrode surface, this process is carried out 5~7 times, carry out the pre-heat treatment after coating every time, carried out after thickness needed for reaching at annealing
Reason, is made activity glass doped aluminium film；
(5) using evaporation coating method or magnetron sputtering method made from step (4) on activity glass doped aluminium film
Layer of conductive film is prepared as upper electrode, solid film capacitor unit is made.
(6) combine, sealed by dielectric by the capacitor unit prepared in step (5) or by capacitor unit
Dress solidification, then two ends lead is carried out, the solid film capacitor with self-repair function is made.
The mass ratio of tetraethyl orthosilicate and water, hydrochloric acid, boric acid described in step (1) is：30:5.8:0.5:4.5, it is described
Boric acid alcoholic solution concentration be 31%.
Aluminium-alcohol salt described in step (2) is aluminium isopropoxide, and described alcohol ether solvents are ethylene glycol ethyl ether, described alfol
The concentration that salt adds resulting solution after alcohol ether solvents is 0.3~0.4mol/L；Described aluminium-alcohol salt, the quality of silicon boron glass colloidal sol
Than for 3~75：1；The addition of described acetylacetone,2,4-pentanedione is 1 for the mol ratio with aluminium isopropoxide:1st, the addition of glacial acetic acid is
Volume ratio with alcohol ether solvents is 1:5.
The pre-heat treatment condition described in step (4) is 150 DEG C of 3~5min of processing, is warming up to 300 DEG C of 3~5min of processing,
Be continuously heating to 450 DEG C of processing 5min, be then cooled to 300 DEG C of 3~5min of processing, continue to be cooled to 150 DEG C of processing 3~
5min。
Annealing condition described in step (4) is slowly dropped to room temperature after being incubated 3h for 450~600 DEG C.
Compared with prior art, the present invention uses activity glass doped aluminium film as the dielectric in capacitor,
It is particularly attached at dielectric defect simultaneously using activated silica boron glass doped aluminium film ion transport active under high field
Near ion is more active, realizes the ion transport medium similar to electrolyte effect in aluminium electrolutic capacitor, and ion is defeated
It is transported near defect and is combined, and then realizes the selfreparing of defect, meanwhile, silicon boron glass is doped into aluminum oxide film, energy
Glass network structure is enough formed, strengthens the structural stability of oxide-film, and then improves disruptive field intensity and energy storage density, in addition, originally
Invention does not have particular/special requirement to electrode, can be with broader applications.The invention has the characteristics that：
1. structure and preparation technology are simple, it is easy to large-scale mass production；
2. low raw-material cost, greatly reduces production cost；
3. belonging to solid-state capacitor, electrolyte is not present in inside, and safety and reliability is high；
4. dielectric properties are good, leakage current is low, and breakdown voltage is high, and operating voltage is high；
5. energy storage density is high, Miniaturized, minimize or applied to IC manufacturing；
6. capacitor has self-repair function, the selfreparing under working condition can be realized, capacitor is greatly improved
Service life；
7. a pair electrode material does not have particular/special requirement, there is broader practice space.
Brief description of the drawings
Fig. 1 is capacitor unit schematic cross-section of the invention；
Fig. 2 is used as VA characteristic curve schematic diagrames of the Top electrode Pt as bottom electrode for the capacitor unit Au of the present invention；
Fig. 3 is used as VA characteristic curve schematic diagrames of the Top electrode Pt as bottom electrode for the capacitor unit Al of the present invention；
Description of symbols in figure：
1-substrate base, 2-lower electrode, 3-activity glass doped aluminium film, 4-upper electrode.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.The present embodiment is with technical solution of the present invention
Premised on implemented, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to
Following embodiments, those skilled in the art do not depart from improvement and repair that scope made according to the announcement of the present invention
Changing all should be within protection scope of the present invention.
Embodiment 1
As shown in figure 1, be the present invention capacitor unit schematic cross-section, the capacitor unit include substrate base 1, under
Portion's electrode 2, activated silica boron glass doped aluminium film 3 and upper electrode 4, described lower electrode 2 are coated in substrate base 1
On surface, described activated silica boron glass doped aluminium film 3 is arranged between upper electrode 4 and lower electrode 2.Described
Lower electrode 2 is conductive film (Pt films), and upper electrode 4 is conductive film (Au films).The lower electrode 2 of capacitor unit
Thickness is 150nm, and the thickness of activated silica boron glass doped aluminium film 3 is 210nm, and the thickness of upper electrode 4 is 100nm.
Wherein, the preparation of the solid film capacitor comprises the following steps：
(1) 3g tetraethyl orthosilicates and 0.75g alcohol at normal temperature are mixed, then mixed 0.45g boric acid with 1g ethanol
Add, 5~20min of stirring at normal temperature, 1g acetic acid (or 0.5g hydrochloric acid) and 0.58g water added afterwards, 40 DEG C are stirred 10~30min,
And beaker mouthful is sealed with preservative film, solution is transparent to obtain silicon boron glass colloidal sol；
(2) 0.02mol aluminium isopropoxides are ground, be subsequently added in 50ml ethylene glycol ethyl ethers ether solvents, 60 DEG C of constant temperature
30min is stirred, silicon boron glass colloidal sol made from 1g steps (1) is then added, 60 DEG C of constant temperature stir 30min, added afterwards
0.02mol acetylacetone,2,4-pentanediones, 70 DEG C of constant temperature stir 30min, finally add 10ml glacial acetic acid, and 80 DEG C of constant temperature stir 30min, treat anti-
After should terminating, room temperature is gradually cooling to, is filtered, activity glass doped aluminium sol precursor is made；
(3) one layer of lower electrode 2 (Pt films) is prepared on substrate base using magnetron sputtering method；
(4) activity glass doped aluminium sol precursor made from step (2) is coated in bottom made from step (3)
On electrode surface, this process is carried out 7 times, carries out the pre-heat treatment after coating every time, the condition of described the pre-heat treatment is at 150 DEG C
5min is managed, 300 DEG C of processing 5min are warming up to, 450 DEG C of processing 5min are continuously heating to, 300 DEG C of processing 5min are then cooled to, after
It is continuous to be cooled to 150 DEG C of processing 5min, after the completion of made annealing treatment, described annealing condition is that 3h is warming up to after 450 DEG C
3h is incubated, activity glass doped aluminium film 3 is made；
(5) one layer of top is being prepared using magnetron sputtering method on activity glass doped aluminium film 3 made from step (4)
Electrode 4 (Au films), is made solid film capacitor unit；
(6) combine, be packaged by dielectric solid by the capacitor unit prepared in (5) or by capacitor unit
Change, then carry out two ends lead, the solid film capacitor with self-repair function is made.
During work, solid film capacitor is used as the electricity in capacitor using activated silica boron glass doped aluminium film 3
Medium, while using the ion transport active under high field of activated silica boron glass doped aluminium film 3, particularly in dielectric
Ion near fault location is more active, realizes the ion transport medium similar to electrolyte effect in aluminium electrolutic capacitor,
It will be combined near ion transport to defect, and then realize the selfreparing of defect.
Embodiment 2
In the present embodiment, upper electrode is the Al membrane electrodes prepared using evaporation coating method, remaining be the same as Example 1.
Embodiment 3
In the present embodiment, upper electrode is the Ti membrane electrodes prepared using magnetron sputtering method, remaining be the same as Example 1.
Embodiment 4
In the present embodiment, in the preparation process of solid film capacitor unit, the silicon boron glass content of doping is 0.2g, its
Remaining be the same as Example 1.
Embodiment 5
In the present embodiment, in the preparation process of solid film capacitor unit, the silicon boron glass content of doping is 0.2g, on
Portion's electrode is the Al membrane electrodes prepared using evaporation coating method, remaining be the same as Example 1.
Embodiment 6
In the present embodiment, in the preparation process of solid film capacitor unit, the silicon boron glass content of doping is 0.2g, on
Portion's electrode is the Ti membrane electrodes prepared using magnetron sputtering method, remaining be the same as Example 1.
Embodiment 7
In the present embodiment, lower electrode is the Al membrane electrodes prepared using evaporation coating method, and thickness is 100nm, remaining
Be the same as Example 1.
Embodiment 8
In the present embodiment, lower electrode is the Ti membrane electrodes prepared using magnetron sputtering method, and thickness is 100nm, remaining
Be the same as Example 1.
Embodiment 9
A kind of preparation method of the solid film capacitor with self-repair function, the preparation method comprises the following steps：
(1) glass sol precursor is prepared：Tetraethyl orthosilicate is added in water, the alcoholic solution of hydrochloric acid, normal temperature mixing is stirred
Mix, then add the alcoholic solution of boric acid, be stirred at room temperature, obtain silicon boron glass colloidal sol；The addition of described tetraethyl orthosilicate
For 30g, described water, the content 5.8g of the alcoholic solution reclaimed water of hydrochloric acid, the content 0.5g of hydrochloric acid, the addition of described boric acid
For 4.5g, the concentration of the alcoholic solution of described boric acid is 31%.
(2) aluminium-alcohol salt is ground, be subsequently added in alcohol ether solvents, 60 DEG C of constant temperature stir 60min, then added suitable
Silicon boron glass colloidal sol made from step (1) is measured, 60 DEG C of constant temperature stir 60min, add acetylacetone,2,4-pentanedione, 70 DEG C of constant temperature stirrings
60min, is eventually adding glacial acetic acid, in 80 DEG C of constant temperature stirring 60min, after question response terminates, is gradually cooling to room temperature, filters, system
Obtain activity glass doped aluminium sol precursor；Described aluminium-alcohol salt is aluminium isopropoxide, and described alcohol ether solvents are ethylene glycol
Ether, the concentration that described aluminium-alcohol salt adds resulting solution after alcohol ether solvents is 0.34mol/L；Described aluminium-alcohol salt, silicon boron glass
The mass ratio of glass colloidal sol is 3.2；The addition of described acetylacetone,2,4-pentanedione is that 0.02mol, the addition of glacial acetic acid are 10ml.
(3) layer of conductive film is prepared on substrate base using evaporation coating method or magnetron sputtering method, is used as bottom electricity
Pole；
(4) activity glass doped aluminium sol precursor made from step (2) is coated in bottom made from step (3)
On electrode surface, this process is carried out 5 times, carry out the pre-heat treatment after coating every time, made annealing treatment after thickness needed for reaching, made
Obtain activity glass doped aluminium film；Described the pre-heat treatment condition is 150 DEG C of processing 3min, is warming up to 300 DEG C of processing
3min, is continuously heating to 450 DEG C of processing 5min, is then cooled to 300 DEG C of processing 3min, continues to be cooled to 150 DEG C of processing 3min.
Described annealing condition is slowly dropped to room temperature after being incubated 3h for 450 DEG C.
(5) using evaporation coating method or magnetron sputtering method made from step (4) on activity glass doped aluminium film
Layer of conductive film is prepared as upper electrode, solid film capacitor unit is made.
(6) combine, sealed by dielectric by the capacitor unit prepared in step (5) or by capacitor unit
Dress solidification, then two ends lead is carried out, the solid film capacitor with self-repair function is made.
Gained has the solid film capacitor of self-repair function, and the thickness of lower electrode is 100nm, described top electricity
Pole thickness is 50nm.The thickness of described activity glass doped aluminium film is 150nm.
Embodiment 10
A kind of preparation method of the solid film capacitor with self-repair function, the preparation method comprises the following steps：
(1) glass sol precursor is prepared：Tetraethyl orthosilicate is added in water, the alcoholic solution of hydrochloric acid, normal temperature mixing is stirred
Mix, then add the alcoholic solution of boric acid, be stirred at room temperature, obtain silicon boron glass colloidal sol；The addition of described tetraethyl orthosilicate
For 30g, described water, the content 5.8g of the alcoholic solution reclaimed water of hydrochloric acid, the content 0.5g of hydrochloric acid, the addition of described boric acid
For 4.5g, the concentration of the alcoholic solution of described boric acid is 31%.
(2) aluminium-alcohol salt is ground, be subsequently added in alcohol ether solvents, 70 DEG C of constant temperature stir 30min, then added suitable
Silicon boron glass colloidal sol made from step (1) is measured, 70 DEG C of constant temperature stir 30min, add acetylacetone,2,4-pentanedione, 80 DEG C of constant temperature stirrings
30min, is eventually adding glacial acetic acid, in 90 DEG C of constant temperature stirring 30min, after question response terminates, is gradually cooling to room temperature, filters, system
Obtain activity glass doped aluminium sol precursor；Described aluminium-alcohol salt is aluminium isopropoxide, and described alcohol ether solvents are ethylene glycol
Ether, the concentration that described aluminium-alcohol salt adds resulting solution after alcohol ether solvents is 0.39mol/L；Described aluminium-alcohol salt, silicon boron glass
The mass ratio of glass colloidal sol is 18.2；The addition of described acetylacetone,2,4-pentanedione is that 0.02mol, the addition of glacial acetic acid are 10mol.
(3) layer of conductive film is prepared on substrate base using evaporation coating method or magnetron sputtering method, is used as bottom electricity
Pole；
(4) activity glass doped aluminium sol precursor made from step (2) is coated in bottom made from step (3)
On electrode surface, this process is carried out 7 times, carry out the pre-heat treatment after coating every time, made annealing treatment after thickness needed for reaching, made
Obtain activity glass doped aluminium film；Described the pre-heat treatment condition is 150 DEG C of processing 5min, is warming up to 300 DEG C of processing
5min, is continuously heating to 450 DEG C of processing 5min, is then cooled to 300 DEG C of processing 5min, continues to be cooled to 150 DEG C of processing 5min.
Described annealing condition is slowly dropped to room temperature after being incubated 3h for 600 DEG C.
(5) using evaporation coating method or magnetron sputtering method made from step (4) on activity glass doped aluminium film
Layer of conductive film is prepared as upper electrode, solid film capacitor unit is made.
(6) combine, sealed by dielectric by the capacitor unit prepared in step (5) or by capacitor unit
Dress solidification, then two ends lead is carried out, the solid film capacitor with self-repair function is made.
Gained has the solid film capacitor of self-repair function, and the thickness of lower electrode is 150nm, described top electricity
Pole thickness is 150nm.The thickness of described activity glass doped aluminium film is 250nm.
The performance of the various embodiments described above products obtained therefrom is as follows：
Claims (10)
1. a kind of solid film capacitor with self-repair function, it is characterised in that the capacitor include substrate base (1),
Lower electrode (2), activity glass doped aluminium film (3), upper electrode (4), described lower electrode (2) are coated in substrate
On substrate (1) surface, described activity glass doped aluminium film (3) be arranged on upper electrode (4) and lower electrode (2) it
Between.
2. a kind of solid film capacitor with self-repair function according to claim 1, it is characterised in that described
The material of lower electrode (2) and upper electrode (4) includes Al films, Au films, Pt films, Ti films or Ag films.
3. a kind of solid film capacitor with self-repair function according to claim 1, it is characterised in that described
The thickness of lower electrode (2) is 100~150nm, and described upper electrode thickness is 50~150nm.
4. a kind of solid film capacitor with self-repair function according to claim 1, it is characterised in that described
Doped-glass in activity glass doped aluminium film (3) is silicon boron glass.
5. a kind of solid film capacitor with self-repair function according to claim 1, it is characterised in that described
The thickness of activity glass doped aluminium film (3) is 150~250nm.
6. a kind of preparation method of the solid film capacitor as claimed in claim 1 with self-repair function, its feature exists
In the preparation method comprises the following steps：
(1) glass sol precursor is prepared：Tetraethyl orthosilicate is added in water, the alcoholic solution of hydrochloric acid, normal temperature is mixed, so
The alcoholic solution of boric acid is added afterwards, is stirred at room temperature, is obtained silicon boron glass colloidal sol；
(2) aluminium-alcohol salt is ground, be subsequently added in alcohol ether solvents, 60~70 DEG C of constant temperature stir 30~60min, Ran Houjia
Enter silicon boron glass colloidal sol made from appropriate step (1), 60~70 DEG C of constant temperature stir 30~60min, add acetylacetone,2,4-pentanedione, 70~
80 DEG C of constant temperature stir 30~60min, are eventually adding glacial acetic acid, and 30~60min is stirred in 80~90 DEG C of constant temperature, and question response terminates
Afterwards, room temperature is gradually cooling to, is filtered, activity glass doped aluminium sol precursor is made；
(3) layer of conductive film is prepared on substrate base using evaporation coating method or magnetron sputtering method, is used as lower electrode；
(4) activity glass doped aluminium sol precursor made from step (2) is coated in lower electrode made from step (3)
On surface, this process is carried out 5~7 times, carry out the pre-heat treatment after coating every time, made annealing treatment after thickness needed for reaching, made
Obtain activity glass doped aluminium film；
(5) prepared using evaporation coating method or magnetron sputtering method made from step (4) on activity glass doped aluminium film
Solid film capacitor unit is made as upper electrode in layer of conductive film.
(6) combine, be packaged by dielectric solid by the capacitor unit prepared in step (5) or by capacitor unit
Change, then carry out two ends lead, the solid film capacitor with self-repair function is made.
7. a kind of preparation method of solid film capacitor with self-repair function according to claim 6, its feature
It is, the mass ratio of tetraethyl orthosilicate and water, hydrochloric acid, boric acid described in step (1) is：30:5.8:0.5:4.5, it is described
The concentration of the alcoholic solution of boric acid is 31%.
8. a kind of preparation method of solid film capacitor with self-repair function according to claim 6, its feature
It is, the aluminium-alcohol salt described in step (2) is aluminium isopropoxide, described alcohol ether solvents are ethylene glycol ethyl ether, described aluminium-alcohol salt
The concentration for adding resulting solution after alcohol ether solvents is 0.3~0.4mol/L；Described aluminium-alcohol salt, the mass ratio of silicon boron glass colloidal sol
For 3~75：1；The addition of described acetylacetone,2,4-pentanedione is 1 for the mol ratio with aluminium isopropoxide:1st, the addition of glacial acetic acid be with
The volume ratio of alcohol ether solvents is 1:5.
9. a kind of preparation method of solid film capacitor with self-repair function according to claim 6, its feature
It is, the pre-heat treatment condition described in step (4) is 150 DEG C of 3~5min of processing, is warming up to 300 DEG C of 3~5min of processing, after
It is continuous to be warming up to 450 DEG C of processing 5min, 300 DEG C of 3~5min of processing are then cooled to, continue to be cooled to 150 DEG C of 3~5min of processing.
10. a kind of preparation method of solid film capacitor with self-repair function according to claim 6, its feature
It is, the annealing condition described in step (4) is slowly dropped to room temperature after being incubated 3h for 450~600 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710135137.1A CN107026018B (en) | 2017-03-08 | 2017-03-08 | A kind of solid film capacitor and preparation method thereof with self-repair function |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710135137.1A CN107026018B (en) | 2017-03-08 | 2017-03-08 | A kind of solid film capacitor and preparation method thereof with self-repair function |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107026018A true CN107026018A (en) | 2017-08-08 |
| CN107026018B CN107026018B (en) | 2019-03-01 |
Family
ID=59526246
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710135137.1A Expired - Fee Related CN107026018B (en) | 2017-03-08 | 2017-03-08 | A kind of solid film capacitor and preparation method thereof with self-repair function |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107026018B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107799415A (en) * | 2017-10-21 | 2018-03-13 | 河南大学 | A kind of method that chemical solution method prepares boron doping oxide dielectric film |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW222615B (en) * | 1990-08-23 | 1994-04-21 | Aluminum Co Of America | |
| KR20080073174A (en) * | 2007-02-05 | 2008-08-08 | 주식회사 지믹스 | Dielectric compositions for y5v type multilayer ceramic chip capacitors, and manufacturing method thereof |
| CN100567189C (en) * | 2005-04-11 | 2009-12-09 | 三星电机株式会社 | Be used for dielectric glass powder, laminated ceramic capacitor and manufacture method thereof |
| CN103971933A (en) * | 2014-05-12 | 2014-08-06 | 同济大学 | Solid state thin film capacitor and preparation method thereof |
| CN105513795A (en) * | 2016-01-19 | 2016-04-20 | 同济大学 | Hydrated alumina dielectric thin film with solid electrolyte function and preparation thereof |
| CN105869888A (en) * | 2016-03-31 | 2016-08-17 | 同济大学 | Solid-state thin film integrated circuit capacitor having self-repairing effect and fabrication method thereof |
-
2017
- 2017-03-08 CN CN201710135137.1A patent/CN107026018B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW222615B (en) * | 1990-08-23 | 1994-04-21 | Aluminum Co Of America | |
| CN100567189C (en) * | 2005-04-11 | 2009-12-09 | 三星电机株式会社 | Be used for dielectric glass powder, laminated ceramic capacitor and manufacture method thereof |
| KR20080073174A (en) * | 2007-02-05 | 2008-08-08 | 주식회사 지믹스 | Dielectric compositions for y5v type multilayer ceramic chip capacitors, and manufacturing method thereof |
| CN103971933A (en) * | 2014-05-12 | 2014-08-06 | 同济大学 | Solid state thin film capacitor and preparation method thereof |
| CN105513795A (en) * | 2016-01-19 | 2016-04-20 | 同济大学 | Hydrated alumina dielectric thin film with solid electrolyte function and preparation thereof |
| CN105869888A (en) * | 2016-03-31 | 2016-08-17 | 同济大学 | Solid-state thin film integrated circuit capacitor having self-repairing effect and fabrication method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107799415A (en) * | 2017-10-21 | 2018-03-13 | 河南大学 | A kind of method that chemical solution method prepares boron doping oxide dielectric film |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107026018B (en) | 2019-03-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103971933B (en) | Solid state thin film capacitor and preparation method thereof | |
| JP4635474B2 (en) | Photoelectric conversion element and transparent conductive substrate used therefor | |
| JP4504456B1 (en) | Method for producing dye-sensitized solar cell | |
| JP4674435B2 (en) | Photoelectric conversion element | |
| JP4635473B2 (en) | Method for manufacturing photoelectric conversion element and method for manufacturing semiconductor electrode | |
| TW200924212A (en) | Pigment sensitizing photoelectric conversion element, and its manufacturing method | |
| JPWO2008004553A1 (en) | Dye-sensitized solar cell module and manufacturing method thereof | |
| KR101470680B1 (en) | Dye-sensitized solar cell and electrode substrate therefor, method of producing an electrode substrate, and paste for forming a semiconductor porous layer | |
| JP2010021091A (en) | Semiconductor electrode, and dye-sensitized photo-electrochemical cell using the same | |
| JP2000285974A (en) | Photosensitized photovolatic power generation element | |
| JP2000285979A (en) | Photosensitized photovoltaic generation element | |
| CN107026018B (en) | A kind of solid film capacitor and preparation method thereof with self-repair function | |
| JP2016127166A (en) | Power storage element and manufacturing method for the same | |
| JP2005158379A (en) | Photoelectric conversion element, its manufacturing method, electronic device and its manufacturing method | |
| CN112194372B (en) | Glass-ceramic composite film solid garnet electrolyte and preparation method thereof | |
| JP4678125B2 (en) | PHOTOELECTRIC CONVERSION ELEMENT AND ITS MANUFACTURING METHOD, ELECTRONIC DEVICE AND ITS MANUFACTURING METHOD | |
| CN107068399B (en) | A kind of high energy storage density solid film capacitor and preparation method thereof | |
| CN105826430A (en) | Preparation method for multi-functional film of solar cell | |
| JP2000319018A (en) | Porous titanium oxide thin film md photoelectric convertor using the film | |
| US9692052B2 (en) | Electrode material for battery, electrode material paste for battery, and solar cell using same, storage battery, and method for manufacturing solar cell | |
| JP2001196104A (en) | Photoelectric transducer, its manufacturing method and porous titanium oxide semiconductor electrode | |
| CN108492987B (en) | Solid-state film capacitor with self-repairing function and preparation method thereof | |
| JP2017059455A (en) | Power storage element and manufacturing method for the same | |
| JP4595337B2 (en) | Method for producing negative electrode in dye-sensitized solar cell | |
| JP2002075476A (en) | Photoelectric conversion film, photoelectric conversion electrode, and photoelectric conversion element |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190301 |