CN114446661B - Multilayer ceramic capacitor based on chemical mechanical polishing and preparation method thereof - Google Patents
Multilayer ceramic capacitor based on chemical mechanical polishing and preparation method thereof Download PDFInfo
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- 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
- H01G4/30—Stacked capacitors
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
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- 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
- H01G4/005—Electrodes
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- 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
- H01G4/228—Terminals
- H01G4/232—Terminals electrically connecting two or more layers of a stacked or rolled capacitor
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- 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
- H01G4/30—Stacked capacitors
- H01G4/306—Stacked capacitors made by thin film techniques
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- 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
- H01G4/12—Ceramic dielectrics
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present application provides a multilayer ceramic capacitor based on chemical mechanical polishing and a method for manufacturing the same by growing SiO on a substrate 2 The sacrificial layer and the ceramic film layer are respectively subjected to chemical mechanical polishing and electrode sputtering, the two ceramic film layers are bonded, and then SiO is corroded 2 The sacrificial layer releases the ceramic film layer, the electrodes are sputtered at the two ends of the released ceramic film layer, and the electrodes at the two ends of the ceramic film layer are immersed and sealed after repeated for a plurality of times and then calcined at high temperature, so that the multilayer ceramic capacitor is obtained. The method combines chemical mechanical polishing and indirect bonding to realize the manufacture of the multilayer ceramic capacitor, avoids temperature control in the process flow of a tape casting method, can realize the preparation of the ceramic film at normal temperature, reduces adverse effects on the film quality and performance in the processes of high temperature, cooling and drying, and obtains the piezoelectric ceramic film with high quality, low stress and high density; the high-temperature sintering process is not needed, the operation temperature is lower, and the yield of the ceramic film is ensured.
Description
Technical Field
The application belongs to the technical field of MEMS device processing and manufacturing, and particularly relates to a multilayer ceramic capacitor based on chemical mechanical polishing and a preparation method thereof.
Background
With the development of electronic technology, electronic devices and circuits are being miniaturized and integrated, and a capacitor is used as an energy storage element, is the most widely used electronic element in electronic equipment, has the yield accounting for about 40% of the total amount of the electronic element, and is widely applied to the aspects of blocking, coupling, bypass, filtering, tuning loops, energy conversion, control circuits and the like. Among them, the multilayer ceramic capacitor (MLCC, multilayer Ceramic Capacitor) is the most important member of the capacitor family, is one of the most widely used passive devices at present, it is widely applied in the military complete machine model of spaceflight, aviation, weapon, ship, etc., the reliability of MLCC is one of the reliability guarantee foundation of the whole machine; the inner electrode slurry is one of the main structural materials of the MLCC, and the quality of the inner electrode and the related process directly determine the inherent reliability of the MLCC. In order to meet the requirements of miniaturization and high-density assembly of circuits, in medium-high voltage circuits such as voltage doubling circuits, automobile electronic equipment, network interfaces, light source drivers and the like, the multilayer ceramic capacitor has the advantages of small volume, high voltage resistance, high reliability, suitability for surface mounting and the like, the use amount of the multilayer ceramic capacitor is larger and larger, particularly mobile communication products, computers, digital cameras and new generation digital household appliances, the demand for MLCC products is increased, and the development of the MLCC has potential along with the increasing popularization of light, thin, short, small and surface mounting technologies of electronic whole machine products. With China becoming a global main electronic information product manufacturing base, the total amount of domestic MLCC market demands presents a fast-growing situation, and provides a good opportunity for the development of domestic MLCC enterprises.
At present, the common method for manufacturing the MLCC is a tape casting method, and the film manufacturing process by the tape casting method comprises the steps of firstly adding a solvent into ceramic powder and a dispersing agent, and then adding a binder and a plasticizerThe slurry is obtained through ball milling twice, and the film is obtained through vacuum defoaming, filtering and other steps, and then through coating with a scraper on a running film belt and drying. The whole process of the casting method adopts vertical operation, the operation is slightly complicated and difficult, the thickness is uneven, and the stress residue is easy to exist. Because the bonding agent is added in the process to lead to the warping of the membrane, the bonding agent wrapping the ceramic powder particles can migrate to the surface of the blank sheet along with the volatilization of the solvent in the drying process and is dried into a polymer film, and the channels of the internal volume of the blank sheet to the surface are blocked to lead to inconsistent drying shrinkage between the edge and the middle, so that the warping occurs. The presence of stress shrinkage during drying also produces warping of the membrane. Incomplete vacuum bubble removal can cause the membrane to generate spot vacuum; uneven dispersion of the slurry can produce linear streaks that are too thick or too thin. Blade height nuances during blade coating can also cause non-uniform film thickness and even film properties such as d 33 And the density is greatly affected. The casting speed is difficult to control in the casting process, and the film cannot be formed due to the excessively high casting speed; the casting speed is too slow, so that a complete ceramic film can be manufactured, but the ferroelectric property of the film is influenced, and d 33 And lower. The casting method for preparing the ceramic film has the influence on ferroelectric performance such as higher coercive field.
Disclosure of Invention
In view of the above, the present application provides a multilayer ceramic capacitor based on chemical mechanical polishing and a method for manufacturing the same, which can avoid the problems of uneven thickness of a membrane, lower device performance, etc. generated when the multilayer ceramic capacitor is manufactured by a tape casting method, and further realize the manufacture of devices with high flatness, high performance, and high yield at a lower temperature.
The specific technical scheme of the application is as follows:
the application provides a preparation method of a multilayer ceramic capacitor based on chemical mechanical polishing, which comprises the following steps:
cleaning the substrate, and sequentially growing SiO on the substrate 2 A sacrificial layer and a ceramic thin film layer;
respectively carrying out chemical mechanical polishing on the ceramic film layers and sputtering electrodes, and bonding the two ceramic film layers;
corrosion of SiO 2 Releasing the ceramic film layer by the sacrificial layer, and sputtering electrodes on two ends of the released ceramic film layer;
repeatedly bonding the two ends of the ceramic film layer after sputtering the electrode for a plurality of times;
and immersing electrodes at two ends of the ceramic film layer, and calcining at high temperature to obtain the multilayer ceramic capacitor.
Preferably, the substrate is a sapphire substrate, and the material of the ceramic film is selected from CaSrZrO 3 、BaTiO 3 Or BaSrTiO 3 The material of the electrode is selected from Au or Pt. More preferably, the material of the ceramic film is selected from BaTiO 3 The material of the electrode is selected from Au.
Preferably, the cleaning of the substrate is specifically:
and cleaning the substrate by using acetone, alcohol and deionized water in sequence, and then carrying out high-temperature annealing treatment on the substrate.
Preferably, the SiO is grown by vapor deposition 2 The thickness of the sacrificial layer is 400-600 nm, and the thickness of the grown ceramic film layer is 2-5 mu m. More preferably, siO is grown 2 The thickness of the sacrificial layer was 500nm and the thickness of the grown ceramic thin film layer was 4 μm.
Preferably, the polishing pad material used in the chemical mechanical polishing is polyurethane, and the polishing liquid abrasive is selected from SiO 2 The grain size of the polishing liquid abrasive is 40-60 nm, and the rotating speed of the polishing disk is 50-80 r/min. More preferably, the particle size of the polishing liquid abrasive is 50nm, and the rotation speed of the polishing disk is 70r/min.
Preferably, the sputtering electrode is formed by a magnetron sputtering method, and the thickness of the sputtering electrode is 100-300 nm. More preferably, the thickness of the sputtering electrode is 200nm.
Preferably, the bonding temperature of the ceramic film layer is 200-250 ℃, the pressure is 1-3 kN, and the bonding time is 6-10 h. More preferably, the bonding temperature of the ceramic film layer is 230 ℃, the pressure is 2kN, and the bonding time is 8 hours.
Preferably, the dip sealing liquid for dip sealing the electrodes at the two ends is silver paste with the mass fraction of 70-90 wt%;
the high-temperature calcination temperature is 500-800 ℃ and the time is 60-80 min. More preferably, the sealing liquid for sealing the electrodes at the two ends is 79wt% of silver paste; the high-temperature calcination temperature is 600 ℃ and the time is 60min.
The application also provides a multilayer ceramic capacitor based on chemical mechanical polishing, which is prepared by the preparation method for preparing the multilayer ceramic capacitor based on chemical mechanical polishing.
Preferably, the diameter of the ceramic thin film layer is 5cm or more, the thickness is 5 μm or less, and the thickness of the sputtered metal electrode is 100nm or more.
The present application provides a multilayer ceramic capacitor based on chemical mechanical polishing and a method for manufacturing the same by growing SiO on a substrate 2 The sacrificial layer and the ceramic film layer are respectively subjected to chemical mechanical polishing and electrode sputtering, the two ceramic film layers are bonded, and then SiO is corroded 2 And releasing the ceramic film layer by the sacrificial layer, sputtering electrodes at two ends of the released ceramic film layer, repeating for a plurality of times, finally soaking the electrodes at two ends of the ceramic film layer, and calcining at a high temperature to obtain the multilayer ceramic capacitor. The method combines the chemical mechanical polishing and the indirect bonding to realize the manufacture of the multilayer ceramic capacitor, and the chemical mechanical polishing method is used for replacing the conventional casting method, so that the temperature control in the technological process of the casting method is avoided, the preparation of the ceramic film can be realized at normal temperature, the adverse effects on the film quality and performance in the high-temperature, cooling and drying processes are reduced, and the high-quality, low-stress and high-density piezoelectric ceramic film is obtained; the high-temperature sintering process is not needed, the operation temperature is lower, and the yield of the ceramic film is ensured. The multilayer ceramic capacitor based on chemical mechanical polishing and the preparation method thereof can be applied to the integrated circuit manufacture, the design of back-end circuits of microsensors, micro-actuators and the like.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a flowchart of a method for manufacturing a multilayer ceramic capacitor according to an embodiment of the present application;
FIG. 2 is a schematic cross-sectional view of a multilayer ceramic capacitor according to an embodiment of the present application after growing a thin film;
FIG. 3 is a schematic cross-sectional view of a multilayer ceramic capacitor according to an embodiment of the present application after polishing;
FIG. 4 is a schematic cross-sectional view of a multilayer ceramic capacitor according to an embodiment of the present application after sputtering electrodes;
FIG. 5 is a schematic cross-sectional structure of a multilayer ceramic capacitor according to an embodiment of the present application after bonding;
FIG. 6 is a schematic diagram showing a cross-sectional structure of a multilayer ceramic capacitor according to an embodiment of the present application after etching;
FIG. 7 is a schematic cross-sectional view of a multilayer ceramic capacitor according to an embodiment of the present disclosure after multiple repeated bonding;
FIG. 8 is a schematic cross-sectional view of a multilayer ceramic capacitor according to an embodiment of the present application after being dip-sealed;
illustration of: 1. a substrate; 2. SiO (SiO) 2 A sacrificial layer; 3. a ceramic thin film; 4. a metal electrode; 5. a metal terminal electrode.
Detailed Description
Referring to fig. 1, fig. 1 is a flowchart of a method for manufacturing a multilayer ceramic capacitor according to an embodiment of the present application.
The embodiment of the application provides a preparation method of a multilayer ceramic capacitor based on chemical mechanical polishing, which comprises the following steps:
s1: cleaning the substrate, and sequentially growing SiO on the substrate 2 A sacrificial layer and a ceramic thin film layer;
s2: respectively carrying out chemical mechanical polishing on the ceramic film layers and sputtering electrodes, and bonding the two ceramic film layers;
s3: corrosion of SiO 2 Releasing the ceramic film layer from the sacrificial layer after releaseSputtering electrodes at two ends of the ceramic film layer;
s4: repeatedly bonding the two ends of the ceramic film layer after sputtering the electrode for a plurality of times;
s5: and immersing electrodes at two ends of the ceramic film layer, and calcining at high temperature to obtain the multilayer ceramic capacitor.
The preparation of the ceramic film can be realized at normal temperature through chemical mechanical polishing, so that adverse effects on the film quality and performance in the high-temperature, cooling and drying processes are reduced, and the piezoelectric ceramic film with high quality, low stress and high density is obtained; the indirect bonding method does not need a high-temperature sintering process, has lower operation temperature, and ensures the yield of the ceramic film. The chemical mechanical polishing and indirect bonding are combined, so that the device preparation with high flatness, high performance and high yield can be realized at a lower temperature.
Referring to fig. 2 to 8, fig. 2 is a schematic cross-sectional structure of a multilayer ceramic capacitor according to an embodiment of the present application after growing a thin film; FIG. 3 is a schematic cross-sectional view of a multilayer ceramic capacitor according to an embodiment of the present application after polishing; FIG. 4 is a schematic cross-sectional view of a multilayer ceramic capacitor according to an embodiment of the present application after sputtering electrodes; FIG. 5 is a schematic cross-sectional structure of a multilayer ceramic capacitor according to an embodiment of the present application after bonding; FIG. 6 is a schematic diagram showing a cross-sectional structure of a multilayer ceramic capacitor according to an embodiment of the present application after etching; FIG. 7 is a schematic cross-sectional view of a multilayer ceramic capacitor according to an embodiment of the present disclosure after multiple repeated bonding; fig. 8 is a schematic cross-sectional structure of the multilayer ceramic capacitor according to the embodiment of the present application after dip sealing.
The preparation method of the multilayer ceramic capacitor based on chemical mechanical polishing in the embodiment of the application comprises the steps of firstly cleaning a substrate 1 and then sequentially growing SiO on the substrate 2 The sacrificial layer 2 and the ceramic film layer 3 are polished and leveled by adopting a chemical mechanical polishing method, and metal electrodes 4 are sputtered on the surfaces of the ceramic film layer 3 to bond the two ceramic film layers 3. Corrosion of SiO with reagents 2 The sacrificial layer releases the ceramic thin film layer 3 from the substrate 1, and the released ceramic thin film layer is subjected toAnd sputtering metal electrodes 4 at two ends of the ceramic film layer 3, repeatedly bonding the two ends of the ceramic film layer 3 after sputtering the metal electrodes for a plurality of times, finally soaking and sealing the metal electrodes at two ends of the ceramic film layer 3 to obtain metal terminal electrodes 5, and calcining at high temperature to obtain the multilayer ceramic capacitor.
According to an embodiment of the present application, the substrate is a sapphire substrate, and the material of the ceramic thin film is selected from CaSrZrO 3 、BaTiO 3 Or BaSrTiO 3 The material of the electrode is selected from Au or Pt.
According to the embodiment of the application, the substrate cleaning specifically comprises:
and cleaning the substrate by using acetone, alcohol and deionized water in sequence, and then carrying out high-temperature annealing treatment on the substrate.
It should be noted that the purpose of the substrate cleaning is to remove surface particulate matter to provide a smooth clean surface for subsequent film preparation.
According to the embodiment of the application, siO is grown by adopting a vapor deposition growth method 2 The thickness of the sacrificial layer is 400-600 nm, and the thickness of the grown ceramic film layer is 2-5 mu m.
Growth of SiO 2 The sacrificial layer is used for separating the sapphire substrate from the ceramic film in a later process, and the grown ceramic film layer can be used as a dielectric layer of the capacitor.
According to an embodiment of the present application, the polishing pad material used in chemical mechanical polishing is polyurethane, and the polishing liquid abrasive is selected from SiO 2 The grain size of the polishing liquid abrasive is 40-60 nm, and the rotating speed of the polishing disk is 50-80 r/min.
It should be noted that, compared with the casting method which is a vertical operation in the whole process, the chemical mechanical polishing method used in the application is simpler in process, less in factors influencing the quality of the film, easier in film thickness control, smoother in film and higher in precision. The chemical mechanical polishing method used in the application does not need temperature control, and reduces the adverse effects of high temperature, cooling and drying processes on the quality and performance of the film. The chemical mechanical polishing method is a chemical mechanical thinning polishing method, and the casting method is a film growth mechanism, so that the prepared film is better in compactness, and stress residues can be reduced in the manufacturing process. Therefore, the chemical mechanical polishing method can manufacture large-flatness processing, and can ensure that the damage and residual stress of the processing surface are thoroughly eliminated so as to meet the requirements of surface integrity and functional integrity. In addition, the chemical mechanical polishing method is nontoxic in material and does not cause harm to people and environment.
According to the embodiment of the application, the sputtering electrode adopts a magnetron sputtering method, and the thickness of the sputtering electrode is 100-300 nm.
The sputtered metal electrode may be used as an internal plate of the capacitor.
According to the embodiment of the application, the bonding temperature of the ceramic film layer is 200-250 ℃, the pressure is 1-3 kN, and the bonding time is 6-10 h.
After the ceramic thin film layers are bonded, a capacitor cell structure can be obtained.
According to the embodiment of the application, the dip sealing liquid for dip sealing the electrodes at the two ends is silver paste with the mass fraction of 70-90 wt%;
the high-temperature calcination temperature is 500-800 ℃ and the time is 60-80 min.
The end electrode after end capping does not have the basic function of an external electrode because the end electrode contains organic components, and the end electrode is sintered and compact by completely decomposing the organic components in the end electrode through high-temperature end firing treatment, so that the end electrode has the basic function of connecting the internal electrode because the internal electrode and the external electrode are well combined.
The embodiment of the application also provides a multilayer ceramic capacitor based on chemical mechanical polishing, which is prepared by the preparation method of the multilayer ceramic capacitor based on chemical mechanical polishing.
It should be noted that the piezoelectric ceramic film of the present application has the characteristics of high quality, low stress and high density, and the multilayer ceramic capacitor of the present application realizes the device preparation with high flatness, high performance and high yield.
The diameter of the ceramic thin film layer is 5cm or more, the thickness is 5 μm or less, and the thickness of the sputtered metal electrode is 100nm or more.
For the purposes of making the objects, features, and advantages of the present application more apparent and understandable, the technical solutions in the embodiments of the present application are clearly and completely described, and it is apparent that the embodiments described below are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
The reagents and materials used in the examples herein were either commercially available or self-made.
Example 1
Step one: and cleaning the substrate by using acetone, alcohol and deionized water in sequence, and then carrying out high-temperature annealing treatment on the substrate. SiO with thickness of 500nm on sapphire surface by vapor deposition method 2 As a sacrificial layer for separating the sapphire substrate from the ceramic thin film in a post process; continuing to use the vapor deposition method to deposit SiO 2 BaTiO with surface growth thickness of 4 μm 3 A thin film as a dielectric layer of the capacitor;
step two: spin-coating on glass substrate with photoresist AZ4620 for 2 times, placing into temporary bonding machine together with sapphire substrate with grown film, applying pressure of 2bar and temperature of 40deg.C for 30min to complete temporary bonding of sapphire substrate, and polishing with SF1 polishing solution model number 0CON-137 to obtain BaTiO 3 Polishing the film by using polyurethane as polishing pad material, wherein the polishing liquid abrasive is selected from SiO 2 The grain size of the polishing liquid abrasive is 50nm, the rotation speed of the polishing disk is 70r/min, the mass of the polishing clamp is 5kg, and the polishing is continuously carried out for 1.5h to obtain the BaTiO with smooth surface 3 A film;
step three, a step of performing; transfer of patterns to BaTiO using uv exposure techniques 3 The surface of the film, followed by the use of magnetron sputtering on the developed BaTiO 3 Au with the thickness of 200nm grows on the surface of the film to serve as an internal polar plate of the capacitor, then EVG520 is used for bonding the two films, the bonding temperature is 230 ℃, the bonding pressure is 2kN, and the bonding time is 8 hours, so that a capacitor unit structure is obtained;
step four: corrosion of SiO using hydrofluoric acid (49 wt.%) 2 Sacrificial layer releasing BaTiO 3 Sputtering electrodes at two ends of the thin film structure, repeating the first to third steps to finish the internal capacitance structure of the capacitor, cutting the prepared multilayer ceramic thin film into 0.2cm 0.5cm size, and sealing the electrodes at two ends by using 75wt% silver paste. The silver end electrode air sintering technology mainly adopts a chain end electrode sintering furnace, the temperature is 600 ℃, and the time is 60min.
The surface morphology of the polished ceramic film is tested by using an atomic force microscope, the Ra value is 425pm, the change rate of capacitance capacity of the obtained multilayer ceramic capacitor is 0+/-30 ppm/DEG C under the condition of-50 ℃ -125 ℃, the change rate of capacity along with frequency is less than +/-0.3% delta C under the high-frequency condition, the capacity drift or hysteresis is less than +/-0.05%, and the change of capacity relative life is less than +/-0.1%.
Example 2
Step one: and cleaning the substrate by using acetone, alcohol and deionized water in sequence, and then carrying out high-temperature annealing treatment on the substrate. SiO with thickness of 500nm on sapphire surface by vapor deposition method 2 As a sacrificial layer for separating the sapphire substrate from the ceramic thin film in a post process; continuing to use the vapor deposition method to deposit SiO 2 CaSrZrO with surface growth thickness of 4 μm 3 A thin film as a dielectric layer of the capacitor;
step two: spin-coating the glass substrate with photoresist AZ4620 for 2 times, placing the glass substrate and the sapphire substrate with the grown film into a temporary bonding machine, applying 2bar pressure and 40 ℃ temperature for 30min to complete temporary bonding of the sapphire substrate, and using model 0CON-137 SF1 polishing solution to bond CaSrZrO 3 Polishing the film by using polyurethane as polishing pad material, wherein the polishing liquid abrasive is selected from SiO 2 The grain size of the polishing liquid abrasive is 50nm, the rotation speed of the polishing disk is 70r/min, the mass of the polishing clamp is 5kg, and the polishing is continuously carried out for 1.5h to obtain the BaTiO with smooth surface 3 A film;
step three, a step of performing; transfer of patterns to CaSrZrO using ultraviolet exposure techniques 3 The surface of the film is then subjected to magnetic sputtering to form developed CaSrZrO 3 Au with thickness of 200nm grown on surface of film is used as internal polar plate of capacitorThen bonding the two films by using EVG520, wherein the bonding temperature is 230 ℃, the bonding pressure is 2kN, and the bonding time is 8 hours, so that a capacitor unit structure is obtained;
step four: corrosion of SiO using hydrofluoric acid (49 wt.%) 2 Sacrificial layer, release CaSrZrO 3 Sputtering electrodes at two ends of the thin film structure, repeating the first to third steps to finish the internal capacitance structure of the capacitor, cutting the prepared multilayer ceramic thin film into 0.2cm 0.5cm size, and sealing the electrodes at two ends by using 75wt% silver paste. The silver end electrode air sintering technology mainly adopts a chain end electrode sintering furnace, the temperature is 600 ℃, and the time is 60min.
The surface morphology of the polished ceramic film is tested by using an atomic force microscope, the Ra value is measured to be 420pm, the change rate of capacitance capacity of the obtained multilayer ceramic capacitor is 0+/-40 ppm/DEG C under the condition of-50 ℃ -125 ℃, the change rate of the capacity along with frequency is less than +/-0.5% delta C under the high-frequency condition, the capacity drift or hysteresis is less than +/-0.1%, and the change of the capacity relative life is less than +/-0.1%.
Example 3
Step one: and cleaning the substrate by using acetone, alcohol and deionized water in sequence, and then carrying out high-temperature annealing treatment on the substrate. SiO with thickness of 500nm on sapphire surface by vapor deposition method 2 As a sacrificial layer for separating the sapphire substrate from the ceramic thin film in a post process; continuing to use the vapor deposition method to deposit SiO 2 BaSrTiO with surface growth thickness of 4 μm 3 A thin film as a dielectric layer of the capacitor;
step two: spin-coating on glass substrate with photoresist AZ4620 for 2 times, placing into temporary bonding machine together with sapphire substrate with grown film, applying pressure of 2bar and temperature of 40deg.C for 30min to complete temporary bonding of sapphire substrate, and polishing with SF1 polishing solution model number 0CON-137 to obtain BaSrTiO 3 Polishing the film by using polyurethane as polishing pad material, wherein the polishing liquid abrasive is selected from SiO 2 The grain size of the polishing liquid abrasive is 50nm, the rotation speed of the polishing disk is 70r/min, the mass of the polishing clamp is 5kg, and the polishing is continuously carried out for 1.5h to obtain the BaTiO with smooth surface 3 A film;
step three, a step of performing; transfer of patterns to BaSrTiO using ultraviolet exposure techniques 3 The surface of the film is then subjected to BaSrTiO after development by magnetron sputtering 3 Au with the thickness of 200nm grows on the surface of the film to serve as an internal polar plate of the capacitor, then EVG520 is used for bonding the two films, the bonding temperature is 230 ℃, the bonding pressure is 2kN, and the bonding time is 8 hours, so that a capacitor unit structure is obtained;
step four: corrosion of SiO using hydrofluoric acid (49 wt.%) 2 Sacrificial layer releasing BaSrTiO 3 Sputtering electrodes at two ends of the thin film structure, repeating the first to third steps to finish the internal capacitance structure of the capacitor, cutting the prepared multilayer ceramic thin film into 0.2cm 0.5cm size, and sealing the electrodes at two ends by using 75wt% silver paste. The silver end electrode air sintering technology mainly adopts a chain end electrode sintering furnace, the temperature is 600 ℃, and the time is 60min.
The surface morphology of the polished ceramic film is tested by using an atomic force microscope, the Ra value is measured to be 420pm, the change rate of capacitance capacity of the obtained multilayer ceramic capacitor is 0+/-35 ppm/DEG C under the condition of-50 ℃ -125 ℃, the change rate of the capacity along with frequency is less than +/-0.2% delta C under the high-frequency condition, the capacity drift or hysteresis is less than +/-0.05%, and the change of the capacity relative life is less than +/-0.05%.
Example 4
Step one: and cleaning the substrate by using acetone, alcohol and deionized water in sequence, and then carrying out high-temperature annealing treatment on the substrate. SiO with thickness of 500nm on sapphire surface by vapor deposition method 2 As a sacrificial layer for separating the sapphire substrate from the ceramic thin film in a post process; continuing to use the vapor deposition method to deposit SiO 2 BaTiO with surface growth thickness of 4 μm 3 A thin film as a dielectric layer of the capacitor;
step two: spin-coating on glass substrate with photoresist AZ4620 for 2 times, placing into temporary bonding machine together with sapphire substrate with grown film, applying pressure of 2bar and temperature of 40deg.C for 30min to complete temporary bonding of sapphire substrate, and polishing with SF1 polishing solution model number 0CON-137 to obtain BaTiO 3 Polishing the film by using polyurethane as the polishing agentPolishing pad material, polishing liquid abrasive material is selected from SiO 2 The grain size of the polishing liquid abrasive is 50nm, the rotation speed of the polishing disk is 70r/min, the mass of the polishing clamp is 5kg, and the polishing is continuously carried out for 1.5h to obtain the BaTiO with smooth surface 3 A film;
step three, a step of performing; transfer of patterns to BaTiO using uv exposure techniques 3 The surface of the film, followed by the use of magnetron sputtering on the developed BaTiO 3 Pt with the thickness of 200nm grows on the surface of the film to serve as an internal polar plate of the capacitor, then EVG520 is used for bonding the two films, the bonding temperature is 230 ℃, the pressure is 2kN, and the bonding time is 8 hours, so that a capacitor unit structure is obtained;
step four: corrosion of SiO using hydrofluoric acid (49 wt.%) 2 Sacrificial layer releasing BaTiO 3 Sputtering electrodes at two ends of the thin film structure, repeating the first to third steps to finish the internal capacitance structure of the capacitor, cutting the prepared multilayer ceramic thin film into 0.2cm 0.5cm size, and sealing the electrodes at two ends by using 75wt% silver paste. The silver end electrode air sintering technology mainly adopts a chain end electrode sintering furnace, the temperature is 600 ℃, and the time is 60min.
The surface morphology of the polished ceramic film is tested by using an atomic force microscope, the Ra value is measured to be 410pm, the capacitance capacity change rate of the obtained multilayer ceramic capacitor is 0+/-25 ppm/DEG C under the condition of-50 ℃ -125 ℃, the capacity change rate with frequency is less than +/-0.3% delta C under the high-frequency condition, the capacity drift or hysteresis is less than +/-0.1%, and the capacity relative life change is less than +/-0.1%.
Example 5
Step one: and cleaning the substrate by using acetone, alcohol and deionized water in sequence, and then carrying out high-temperature annealing treatment on the substrate. SiO with thickness of 400nm on sapphire surface by vapor deposition method 2 As a sacrificial layer for separating the sapphire substrate from the ceramic thin film in a post process; continuing to use the vapor deposition method to deposit SiO 2 BaTiO with surface growth thickness of 2 μm 3 A thin film as a dielectric layer of the capacitor;
step two: spin-coating the glass substrate with photoresist AZ4620 for 2 times, and the spin-coating is the same as the sapphire substrate with the grown filmPlacing into a temporary bonding machine, applying 2bar pressure and 40 deg.C for 30min to complete temporary bonding of sapphire substrate, and polishing with SF1 polishing solution model 0CON-137 to obtain BaTiO 3 Polishing the film by using polyurethane as polishing pad material, wherein the polishing liquid abrasive is selected from SiO 2 The grain size of the polishing liquid abrasive is 40nm, the rotation speed of the polishing disk is 50r/min, the mass of the polishing clamp is 5kg, and the polishing is continuously carried out for 1.5h to obtain the BaTiO with smooth surface 3 A film;
step three, a step of performing; transfer of patterns to BaTiO using uv exposure techniques 3 The surface of the film, followed by the use of magnetron sputtering on the developed BaTiO 3 Au with the thickness of 100nm grows on the surface of the film to serve as an internal polar plate of the capacitor, then EVG520 is used for bonding the two films, the bonding temperature is 200 ℃, the pressure is 1kN, and the bonding time is 6h, so that a capacitor unit structure is obtained;
step four: corrosion of SiO using hydrofluoric acid (49 wt.%) 2 Sacrificial layer releasing BaTiO 3 Sputtering electrodes at two ends of the thin film structure, repeating the first to third steps to finish the internal capacitance structure of the capacitor, cutting the prepared multilayer ceramic thin film into 0.2cm 0.5cm size, and sealing the electrodes at two ends by using 70wt% silver paste. The silver end electrode air sintering technology mainly adopts a chain end electrode sintering furnace, the temperature is 500 ℃, and the time is 70min.
The surface morphology of the polished ceramic film is tested by using an atomic force microscope, the Ra value is 428pm, the change rate of capacitance capacity of the obtained multilayer ceramic capacitor is 0+/-20 ppm/DEG C under the condition of-50 ℃ -125 ℃, the change rate of capacity along with frequency is less than +/-0.5% delta C under the high-frequency condition, the capacity drift or hysteresis is less than +/-0.05%, and the change of capacity relative life is less than +/-0.05%.
Example 6
Step one: and cleaning the substrate by using acetone, alcohol and deionized water in sequence, and then carrying out high-temperature annealing treatment on the substrate. SiO with thickness of 600nm on sapphire surface by vapor deposition method 2 As a sacrificial layer for separating the sapphire substrate from the ceramic thin film in a post process; continuing to use the vapor deposition method to deposit SiO 2 BaTiO with surface growth thickness of 5 μm 3 A thin film as a dielectric layer of the capacitor;
step two: spin-coating on glass substrate with photoresist AZ4620 for 2 times, placing into temporary bonding machine together with sapphire substrate with grown film, applying pressure of 2bar and temperature of 40deg.C for 30min to complete temporary bonding of sapphire substrate, and polishing with SF1 polishing solution model number 0CON-137 to obtain BaTiO 3 Polishing the film by using polyurethane as polishing pad material, wherein the polishing liquid abrasive is selected from SiO 2 The grain size of the polishing liquid abrasive is 60nm, the rotation speed of the polishing disk is 80r/min, the mass of the polishing clamp is 5kg, and the polishing is continuously carried out for 1.5h to obtain the BaTiO with smooth surface 3 A film;
step three, a step of performing; transfer of patterns to BaTiO using uv exposure techniques 3 The surface of the film, followed by the use of magnetron sputtering on the developed BaTiO 3 Au with the thickness of 300nm grows on the surface of the film to serve as an internal polar plate of the capacitor, then EVG520 is used for bonding the two films, the bonding temperature is 250 ℃, the bonding pressure is 3kN, and the bonding time is 10 hours, so that a capacitor unit structure is obtained;
step four: corrosion of SiO using hydrofluoric acid (49 wt.%) 2 Sacrificial layer releasing BaTiO 3 Sputtering electrodes at two ends of the thin film structure, repeating the first to third steps to finish the internal capacitance structure of the capacitor, cutting the prepared multilayer ceramic thin film into 0.2cm 0.5cm size, and sealing the electrodes at two ends by using silver paste with the mass fraction of 90 wt%. The silver end electrode air sintering technology mainly adopts a chain end electrode sintering furnace, the temperature is 800 ℃, and the time is 80min.
The surface morphology of the polished ceramic film is tested by using an atomic force microscope, the Ra value is 414pm, the capacitance change rate of the obtained multilayer ceramic capacitor is 0+/-36 ppm/DEG C under the condition of-50 ℃ -125 ℃, the capacitance change rate with frequency is less than +/-0.3% delta C under the high-frequency condition, the capacitance drift or hysteresis is less than +/-0.05%, and the capacitance relative life change is less than +/-0.1%.
In summary, the present application is directed to the growth of SiO on a substrate 2 The sacrificial layer and the ceramic film layer are used for respectively carrying out chemical mechanical polishing on the ceramic film layerSputtering electrode, bonding two ceramic film layers, and corroding SiO 2 And releasing the ceramic film layer by the sacrificial layer, sputtering electrodes at two ends of the released ceramic film layer, finally soaking the electrodes at two ends of the ceramic film layer, and calcining at a high temperature to obtain the multilayer ceramic capacitor.
The preparation method of the multilayer ceramic capacitor based on chemical mechanical polishing combines the chemical mechanical polishing and the indirect bonding method to realize the manufacture of the multilayer ceramic capacitor, and the chemical mechanical polishing method is used for replacing the conventional casting method, so that the temperature control in the technological process of the casting method is avoided, the preparation of the ceramic film can be realized at normal temperature, and the adverse effects on the film quality and performance in the high-temperature, cooling and drying processes are reduced. The high-temperature sintering process is not needed, the operation temperature is lower, and the yield of the ceramic film is ensured.
The multilayer ceramic capacitor based on chemical mechanical polishing has the characteristics of high quality, low stress and high density, and realizes the preparation of devices with high flatness, high performance and high yield.
The above embodiments are merely for illustrating the technical solution of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (8)
1. A method for manufacturing a multilayer ceramic capacitor based on chemical mechanical polishing, comprising the steps of:
cleaning the substrate, and sequentially growing SiO on the substrate 2 A sacrificial layer and a ceramic thin film layer;
respectively carrying out chemical mechanical polishing on the ceramic film layers and sputtering electrodes, and bonding the two ceramic film layers;
corrosion of SiO 2 Sacrificial layer releasing ceramic filmSputtering electrodes on two ends of the released ceramic film layer;
repeatedly bonding the two ends of the ceramic film layer after sputtering the electrode for a plurality of times;
immersing electrodes at two ends of the ceramic film layer, and calcining at high temperature to obtain a multilayer ceramic capacitor;
growing SiO by vapor deposition growth method 2 The thickness of the sacrificial layer is 400-600 nm, and the thickness of the grown ceramic film layer is 2-5 mu m;
the bonding temperature of the ceramic film layer is 200-250 ℃, the pressure is 1-3 kN, and the bonding time is 6-10 h;
wherein, the repeated bonding is carried out for a plurality of times to the two ends of the ceramic film layer after sputtering the electrode, specifically: etching the SiO2 sacrificial layer by using hydrofluoric acid to release a BaTiO3 film structure, sputtering electrodes at two ends, repeating the steps to finish the internal capacitance structure of the capacitor, cutting the prepared multilayer ceramic film into 0.2cm by 0.5cm, and sealing the electrodes at two ends by using silver paste.
2. The method for manufacturing a multilayer ceramic capacitor according to claim 1, wherein the substrate is a sapphire substrate, and the material of the ceramic thin film is selected from CaSrZrO 3 、BaTiO 3 Or BaSrTiO 3 The material of the electrode is selected from Au or Pt.
3. The method for manufacturing a multilayer ceramic capacitor according to claim 1, wherein the cleaning of the substrate is specifically:
and cleaning the substrate by using acetone, alcohol and deionized water in sequence, and then carrying out high-temperature annealing treatment on the substrate.
4. The method for manufacturing a multilayer ceramic capacitor according to claim 1, wherein the polishing pad material used in the chemical mechanical polishing is polyurethane, and the polishing liquid abrasive is selected from the group consisting of SiO 2 The grain size of the polishing liquid abrasive is 40-60 nm, and the rotating speed of the polishing disk is 50-80 r/min.
5. The method for manufacturing a multilayer ceramic capacitor according to claim 1, wherein the sputtering electrode is formed by a magnetron sputtering method, and the thickness of the sputtering electrode is 100 to 300nm.
6. The method for manufacturing a multilayer ceramic capacitor according to claim 1, wherein the sealing liquid for sealing the electrodes at both ends is silver paste with a mass fraction of 70-90 wt%;
the high-temperature calcination temperature is 500-800 ℃ and the time is 60-80 min.
7. A multilayer ceramic capacitor based on chemical mechanical polishing, characterized by being produced by the production method according to any one of claims 1 to 6.
8. The multilayer ceramic capacitor according to claim 7, wherein the ceramic thin film layer has a diameter of 5cm or more, a thickness of 5 μm or less, and a thickness of 100nm or more of the sputtered metal electrode.
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