WO2016003306A1 - Procédé de fabrication de condensateurs ferroélectriques - Google Patents
Procédé de fabrication de condensateurs ferroélectriques Download PDFInfo
- Publication number
- WO2016003306A1 WO2016003306A1 PCT/RU2014/000476 RU2014000476W WO2016003306A1 WO 2016003306 A1 WO2016003306 A1 WO 2016003306A1 RU 2014000476 W RU2014000476 W RU 2014000476W WO 2016003306 A1 WO2016003306 A1 WO 2016003306A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- substrate
- vacuum
- dopant
- temperature
- barium titanate
- Prior art date
Links
- 239000003990 capacitor Substances 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 42
- 239000000919 ceramic Substances 0.000 claims abstract description 21
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000010949 copper Substances 0.000 claims abstract description 19
- 229910052802 copper Inorganic materials 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 18
- 239000002184 metal Substances 0.000 claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 238000000137 annealing Methods 0.000 claims abstract description 10
- 239000011651 chromium Substances 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims abstract description 7
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 6
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 6
- 239000007791 liquid phase Substances 0.000 claims abstract description 5
- 239000010955 niobium Substances 0.000 claims abstract description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000009833 condensation Methods 0.000 claims abstract description 4
- 230000005494 condensation Effects 0.000 claims abstract description 4
- 238000000151 deposition Methods 0.000 claims abstract description 4
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000008021 deposition Effects 0.000 claims abstract description 3
- 238000005275 alloying Methods 0.000 claims description 26
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- 238000001771 vacuum deposition Methods 0.000 claims description 3
- 239000002019 doping agent Substances 0.000 abstract description 32
- 230000015556 catabolic process Effects 0.000 abstract description 11
- 239000011572 manganese Substances 0.000 abstract description 2
- 238000007738 vacuum evaporation Methods 0.000 abstract description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract 1
- 230000005294 ferromagnetic effect Effects 0.000 abstract 1
- 229910052748 manganese Inorganic materials 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 18
- 238000009792 diffusion process Methods 0.000 description 15
- 150000002500 ions Chemical class 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 239000003985 ceramic capacitor Substances 0.000 description 8
- 150000002739 metals Chemical class 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical group [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 3
- 239000012790 adhesive layer Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000000313 electron-beam-induced deposition Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000004870 electrical engineering Methods 0.000 description 1
- 238000001017 electron-beam sputter deposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 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
- H01G7/00—Capacitors in which the capacitance is varied by non-mechanical means; Processes of their manufacture
- H01G7/06—Capacitors in which the capacitance is varied by non-mechanical means; Processes of their manufacture having a dielectric selected for the variation of its permittivity with applied voltage, i.e. ferroelectric capacitors
Definitions
- the invention relates to a technology for manufacturing capacitors with a dielectric made of ceramic based on barium titanate coated with a metal by atomization by vacuum evaporation.
- silver is used, which is applied to the substrate in the form of a paste.
- the adhesion of the functional coating to the substrate is provided by heat treatment in which silver diffuses into the surface layer.
- a more advanced technical solution is a method of manufacturing ferroceramic capacitors containing a ceramic dielectric based on barium titanate, on the metallized surfaces of which fixed electrode current collectors described in patent RU 2354632, 2007
- the known method includes the operation of forming a ceramic plate (substrate), on the surface of which a mixture is applied in equal proportions of finely dispersed (1-50 ⁇ m) copper powder with the substrate material, and then by hot pressing a plate with a surface composite layer is formed, which serves as an adhesive for fixing copper electrodes.
- the prepared ferroceramic plate on the surfaces of which a copper layer is deposited, is heated in vacuum, conducting photon annealing for fusion into a monolith of the electrode layer with a copper inclusion of an adhesive layer.
- the pressure is changed to atmospheric pressure within 15 minutes, cooling the product to a temperature of 25-30 ° C without oxygen.
- the method provides a 35-40% increase in the adhesion strength of the metal to the surface of the ceramic substrate.
- the known method does not significantly increase the capacitance of a ferro-ceramic capacitor.
- the technical problem to which the present invention is directed is to improve the known method for high-performance manufacturing of ferro-ceramic capacitors with increased specific capacitance and breakdown voltage.
- the required technical result is achieved by the fact that in the method of manufacturing ferroelectric capacitors, including forming a ceramic substrate, mainly based on barium titanate, applying an alloying coating, vacuum deposition of copper electrodes and vacuum annealing of the composite material according to the invention, the alloying coating is applied in the liquid phase by condensation from the vapor stream of vacuum-evaporated metals of a series: titanium, vanadium, chromium, manganese, niobium, at a substrate temperature of 150-350 ° C, after which ku alloying with coating is subjected to vacuum annealing, and the subsequent deposition of copper electrodes carried on directly heated to a temperature not higher than 600 ° C composite substrate.
- the differences of the proposed method provide, in comparison with existing analogues, an increase by an average of 6 times the specific capacitance of a ferro-ceramic capacitor and 3.5 times the breakdown voltage.
- the application of the alloying metal to the substrate in the liquid phase from the vapor stream and the subsequent vacuum annealing of the composite material provide effective mass transfer (thermal diffusion) of the alloying metal (dopant) to the substrate while combining surface and bulk diffusion of the alloying metal into the ceramic substrate.
- the dopant due to activation and mixing of the melt in the liquid bath, the dopant interacts with ferroceramics, forming solid solutions and chemical compounds.
- the diffusion zone is 120-150 ⁇ m, which, when double-sided doping, provides through doping of the substrate volume and the achievement of maximum targets.
- the temperature of the substrate array is maintained in the range of 150-350 ° C, while the temperature on the substrate surface reaches the melting temperature of the dopant due to the heat of condensation of the alloying material from the vapor stream, which ensures the state of the dopant on the substrate surface in the liquid phase during alloying .
- Doping with a dopant of a ceramic plate heated to a temperature of 150-350 ° C ensures the active interaction of the alloying metal in a liquid bath with barium titanate, increasing the penetration depth of the alloying elements into the plate, that is, the combination of surface and volume diffusion of the dopant.
- the heating temperature of the ceramic substrate during alloying is below 150 ° C, a strong adhesive bond of the alloying metal layer to the ferroceramic material is not ensured.
- the dielectric loss in the formed capacitor sharply increases.
- a vacuum annealing is carried out, in which the dopant penetrates deep into the ferroceramics.
- barrier layers are formed that increase the breakdown voltage, in addition, the dopant fills the pores that cause ionization breakdown. The diffusion process continues until the chemical potentials of the components of the entire prepared structure are equalized.
- Annealing in vacuum is combined with the application of an alloying metal to maintain the required diffusion temperature, excluding the oxidation of dopant.
- titanium, vanadium, chromium, manganese, niobium is explained by the fact that they have an ion radius of less than 0.066 ⁇ m, close in size to the ions of the crystal lattice of barium titanate, and an ionization energy of more than 6.7 eV, which allows alloying elements diffuse into the crystal lattice of the substrate material, thereby increasing the capacitance of the capacitor material while shifting the position of the titanium ion in the lattice.
- the higher ionization energy ensures the activation of the dopant when the barium titanate melt is mixed on the surface of the ceramic substrate when the molten bath is mixed, increasing the polarization of the domains of the composite base and the depth of diffusion, which multiply increases the purpose of the ferroelectric, in particular, breakdown voltage.
- a feature of the proposed method is that the alloying dopant layer formed on the surface of the ceramic plate serves as an adhesive layer on which the electrode layer of copper deposited is directly formed vacuum spraying, without breaking the process stream in a vacuum chamber.
- the temperature of the doped substrate does not exceed 600 ° C in order to exclude the interaction of copper with the material of the adhesive layer monolithically bonded to the ceramic base, thereby preventing the deterioration of the performance of the capacitor.
- Disks with a diameter of 6 mm and a thickness of 300 ⁇ m made of molded and sintered capacitor ferroceramics based on barium titanate of the Y5V temperature stability group (according to the Russian classification of the H30 group) are applied by electron beam spraying with a 8 ⁇ m thick alloy layer.
- a dopant - titanium (ion radius of 0.064 nm and an ionization energy of 6.82 eV) is applied to sample H30-1 at a substrate temperature of 200 ... 250 ° C
- a dopant - vanadium (ion radius of 0.059 is applied to the NZO-2 sample nm and ionization energy of 6.71 eV) at a substrate temperature of 190 ... 230 ° C
- a dopant - chromium (ion radius 0.35 nm and ionization energy of 6.764 eV) at a substrate temperature of 150 is applied to sample H30-3. .220 ° C.
- a layer of dopant is applied to the second side of the ceramic discs.
- the dopant layer on the surface of the NZO-1, N30-2, and NZO-3 samples is heated in vacuum from the thermoblock and annealed to obtain barium titanate-based material doped in bulk. Then, a double-sided copper coating is applied to the surface of the samples of the composite material doped with dopant by means of vacuum electron beam deposition at a substrate temperature of not more than 600 ° C.
- the result is a ceramic capacitor of group H30 in the form of a plate of doped ferroceramics with copper electrodes.
- Comparison sample NZO-4 is a ceramic capacitor made of molded and sintered capacitor ferroceramics based on barium titanate of the Y5V temperature stability group (according to the Russian classification of the NZO group) without an alloying additive and with silver electrodes deposited by thermal diffusion according to the prototype.
- a dopant - titanium (ion radius of 0.064 nm and an ionization energy of 6.82 eV) is applied to sample H70-1 at a substrate temperature of 250 ... 300 ° C
- a dopant - vanadium (ion radius of 0.059 is applied to sample H70-2 nm and ionization energy of 6.71 eV) at a substrate temperature of 200 ... 250 ° C
- a dopant - chromium (ion radius 0.35 nm and ionization energy of 6.76 eV) at a substrate temperature of 170 is applied to sample H70-3 ... 250 ° C.
- a layer of dopant is applied to the second side of the ceramic discs.
- the dopant layer on the surface of samples H70-1, H70-2, and H70-3 is heated in vacuum from the fuser and annealed to obtain 5 barium titanate-based material doped in bulk.
- a double-sided copper coating is applied to the surface of the samples of the composite material doped with dopant by means of vacuum electron beam deposition at a substrate temperature of not more than 600 ° C.
- a ceramic capacitor of the H70 group is obtained in the form of a plate of doped ferroceramics with copper electrodes.
- Comparison sample H70-4 is a ceramic capacitor made of molded and sintered capacitor ferroceramics based on 5 barium titanate of the group for temperature stability Y5V (according to the Russian classification of group H70) without alloying additive and with silver electrodes deposited by thermal diffusion according to the prototype.
- the table shows that as a result of doping the ferroceramics of the NZO group by the proposed method, compared with the prototype, the dielectric constant (hence, capacity) increased depending on the dopant by 5.0-6.6 times with a simultaneous increase in breakdown voltage by 3.2 -3.6 times.
- the growth in capacitance was from 5 to 6.8 times with a simultaneous increase in breakdown voltage by 3.6-4.0 times.
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Ceramic Capacitors (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
L'invention concerne une technologie de fabrication de condensateurs dotés d'un diélectrique en céramique à base de titanate de baryum avec un revêtement de métal appliqué par sa pulvérisation obtenue par évaporation sous vide. Le procédé de fabrication de condensateurs ferroélectriques comprend la formation d'un substrat céramique, de préférence sur une base de titanate de baryum, l'application d'un revêtement d'alliage, la pulvérisation sous vide d'électrodes en cuivre et le recuit sous vide d'un matériau composite. La nouveauté consiste en ce que le revêtement d'alliage est appliqué en phase liquide par condensation à partir d'un flux de vapeur d'un métal vaporisé sous vide dans la série: titane, vanadium, chrome, manganèse, niobium, à une température du substrat de 150-350°C, après quoi le substrat avec le revêtement à alliage est soumis à un recuit, et l'application des électrodes en cuivre s'effectue directement sur le substrat composite chauffé à une température inférieure ou égale à 600°C. On propose une solution technique qui facilite, en comparaison aux analogues existants, une hausse moyenne de la capacité spécifique d'un condensateur ferroélectrique avec un facteur 6 et de la tension de rupture avec un facteur 3,6 sans accroître les pertes diélectriques.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/RU2014/000476 WO2016003306A1 (fr) | 2014-06-30 | 2014-06-30 | Procédé de fabrication de condensateurs ferroélectriques |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/RU2014/000476 WO2016003306A1 (fr) | 2014-06-30 | 2014-06-30 | Procédé de fabrication de condensateurs ferroélectriques |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2016003306A1 true WO2016003306A1 (fr) | 2016-01-07 |
Family
ID=55019699
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/RU2014/000476 WO2016003306A1 (fr) | 2014-06-30 | 2014-06-30 | Procédé de fabrication de condensateurs ferroélectriques |
Country Status (1)
| Country | Link |
|---|---|
| WO (1) | WO2016003306A1 (fr) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04230011A (ja) * | 1990-05-31 | 1992-08-19 | Philips Gloeilampenfab:Nv | 単一層コンデンサーの製造方法 |
| JPH06342737A (ja) * | 1993-05-31 | 1994-12-13 | Iwasaki Electric Co Ltd | 非線形セラミックコンデンサの製造方法 |
| RU2044719C1 (ru) * | 1991-07-31 | 1995-09-27 | Витебское производственное объединение "Монолит" | Способ металлизации заготовок пьезокерамических элементов |
| RU2354632C2 (ru) * | 2007-02-19 | 2009-05-10 | Государственное образовательное учреждение высшего профессионального образования Кабардино-Балкарский государственный университет им. Х.М. Бербекова | Способ металлизации керамики |
| RU2523000C1 (ru) * | 2013-01-24 | 2014-07-20 | Общество с ограниченной ответственностью "ЭЛЕМЕНТ-22" | Способ изготовления сегнетоэлектрических конденсаторов |
-
2014
- 2014-06-30 WO PCT/RU2014/000476 patent/WO2016003306A1/fr active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04230011A (ja) * | 1990-05-31 | 1992-08-19 | Philips Gloeilampenfab:Nv | 単一層コンデンサーの製造方法 |
| RU2044719C1 (ru) * | 1991-07-31 | 1995-09-27 | Витебское производственное объединение "Монолит" | Способ металлизации заготовок пьезокерамических элементов |
| JPH06342737A (ja) * | 1993-05-31 | 1994-12-13 | Iwasaki Electric Co Ltd | 非線形セラミックコンデンサの製造方法 |
| RU2354632C2 (ru) * | 2007-02-19 | 2009-05-10 | Государственное образовательное учреждение высшего профессионального образования Кабардино-Балкарский государственный университет им. Х.М. Бербекова | Способ металлизации керамики |
| RU2523000C1 (ru) * | 2013-01-24 | 2014-07-20 | Общество с ограниченной ответственностью "ЭЛЕМЕНТ-22" | Способ изготовления сегнетоэлектрических конденсаторов |
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