CN108063182B - A kind of preparation method of electrode of piezoelectric composite element - Google Patents
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- 239000002131 composite material Substances 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 26
- 238000004544 sputter deposition Methods 0.000 claims abstract description 21
- 125000000524 functional group Chemical group 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 239000010410 layer Substances 0.000 claims description 60
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005238 degreasing Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 230000007704 transition Effects 0.000 claims description 4
- 239000011241 protective layer Substances 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 2
- 239000012459 cleaning agent Substances 0.000 claims 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims 2
- 238000001035 drying Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 description 6
- 125000004429 atom Chemical group 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 3
- 125000004430 oxygen atom Chemical group O* 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
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- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
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- H—ELECTRICITY
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- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/04—Treatments to modify a piezoelectric or electrostrictive property, e.g. polarisation characteristics, vibration characteristics or mode tuning
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- H—ELECTRICITY
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- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/08—Shaping or machining of piezoelectric or electrostrictive bodies
- H10N30/085—Shaping or machining of piezoelectric or electrostrictive bodies by machining
- H10N30/086—Shaping or machining of piezoelectric or electrostrictive bodies by machining by polishing or grinding
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Abstract
Description
技术领域technical field
本发明属于先进制造技术领域，涉及一种压电复合元件电极制备方法。The invention belongs to the field of advanced manufacturing technology, and relates to a method for preparing an electrode of a piezoelectric composite element.
背景技术Background technique
压电复合元件由压电陶瓷和聚合物复合而成，兼具压电陶瓷的高压电性能和聚合物的低声阻抗特点，是船舶水听器、医疗超声探头、红外探测器、超声流量计等的关键元件。压电复合元件电极对压电复合元件性能至关重要，要求具有低电阻、高结合强度和强焊接性，以满足压电元件的高灵敏、抗震动、高可靠等高性能要求。Piezoelectric composite components are composed of piezoelectric ceramics and polymers. They have both the high-voltage properties of piezoelectric ceramics and the low acoustic impedance of polymers. They are ideal for ship hydrophones, medical ultrasonic probes, infrared detectors, and ultrasonic flow key components of the meter. The electrodes of piezoelectric composite elements are crucial to the performance of piezoelectric composite elements, and require low resistance, high bonding strength and strong weldability to meet the high performance requirements of piezoelectric elements such as high sensitivity, anti-vibration, and high reliability.
目前压电陶瓷电极普遍采用背银工艺，将银浆涂敷压电陶瓷表面，经700-800℃高温烧结形成电极。但是，由于压电复合元件中聚合物工作温度一般低于150℃，背银工艺的高温过程将导致聚合物变形、碳化等劣化，破坏压电复合元件。At present, the piezoelectric ceramic electrodes generally adopt the back-silver process, and the silver paste is coated on the surface of the piezoelectric ceramics, and the electrodes are formed by sintering at a high temperature of 700-800°C. However, since the working temperature of the polymer in the piezoelectric composite element is generally lower than 150°C, the high-temperature process of the back-silver process will lead to deterioration of the polymer such as deformation and carbonization, and damage the piezoelectric composite element.
发明内容Contents of the invention
本发明要解决的技术难题是克服上述技术方法的不足，发明一种压电复合元件电极制作的方法。The technical problem to be solved by the present invention is to overcome the deficiencies of the above-mentioned technical methods and to invent a method for making electrodes of piezoelectric composite elements.
本发明的技术方案为：Technical scheme of the present invention is:
一种压电复合元件电极制备方法，首先，通过机械研磨的方法对压电复合元件表面进行预处理，使之具有良好的平面度及合适的粗糙度。其次，对PZT压电复合元件表面改性以增加其表面能，具体为采用紫外线照射复合元件表面，使其表面产生含氧极性官能团，提高压电复合元件表面与金属层之间的结合强度。最后，溅射微米级的金属薄膜作为压电复合元件的电极。具体步骤如下：A method for preparing piezoelectric composite element electrodes. Firstly, the surface of the piezoelectric composite element is pretreated by mechanical grinding to make it have good flatness and proper roughness. Secondly, the surface of the PZT piezoelectric composite element is modified to increase its surface energy, specifically, the surface of the composite element is irradiated with ultraviolet rays to generate oxygen-containing polar functional groups on the surface, and the bonding strength between the surface of the piezoelectric composite element and the metal layer is improved. . Finally, micron-sized metal films are sputtered as electrodes of piezoelectric composite elements. Specific steps are as follows:
1)压电复合元件表面预处理1) Surface pretreatment of piezoelectric composite components
首先，采用自动压力研磨抛光机对压电复合元件进行研磨处理，使其表面平面度低于1μm，粗糙度低于800nm，以满足电极层溅射的要求；其次，采用无水乙醇、丙酮、去离子水进行超声清洗，去除压电复合元件表面附着的有机杂质；最后，采用除油液对压电复合元件进行除油处理，去除皂化油和矿物油。Firstly, use an automatic pressure grinding and polishing machine to grind the piezoelectric composite element, so that the surface flatness is less than 1 μm, and the roughness is less than 800 nm, so as to meet the requirements of electrode layer sputtering; secondly, use absolute ethanol, acetone, Ultrasonic cleaning is performed with deionized water to remove organic impurities attached to the surface of the piezoelectric composite element; finally, the piezoelectric composite element is degreased with degreasing fluid to remove saponified oil and mineral oil.
2)压电复合元件表面改性2) Surface modification of piezoelectric composite components
对预处理后的压电复合元件进行烘干处理，去除多余的水分等，利用紫外线照射机在输出功率为8～16mW/cm2的条件下照射复合元件表面3～8min，使其表面产生含氧极性官能团，官能团与电极层的金属原子能够产生强烈的相互作用，使得复合元件表面与金属原子之间产生强化学键，进而得到强的化学键力，提高电极与复合元件表面之间的结合强度。Dry the pretreated piezoelectric composite element to remove excess water, etc., and use an ultraviolet irradiation machine to irradiate the surface of the composite element for 3 to 8 minutes under the condition of an output power of 8 to 16mW/ cm2 , so that the surface contains Oxygen polar functional groups, the functional groups and the metal atoms of the electrode layer can have a strong interaction, making strong chemical bonds between the surface of the composite element and the metal atoms, thereby obtaining a strong chemical bond force and improving the bonding strength between the electrode and the surface of the composite element .
3)制备压电复合元件电极3) Preparation of piezoelectric composite element electrodes
在表面改性后的压电复合元件表面溅射金属层1作为压电复合元件电极的过渡层，金属层1的金属原子与复合元件表面的氧原子形成的金属氧化物不仅利于过渡层的继续生长，而且能够显著地提高金属层1与压电复合元件表面的结合强度。溅射金属层2作为压电复合元件电极的中间保护层，金属层2有效地避免焊接时高温熔融焊锡对金属层1的破坏。溅射金属层3作为压电复合元件电极的表面保护层，金属层3提高了电极的可焊接性以及抗氧化性。The metal layer 1 is sputtered on the surface of the piezoelectric composite element after surface modification as the transition layer of the electrode of the piezoelectric composite element. The metal oxide formed by the metal atoms of the metal layer 1 and the oxygen atoms on the surface of the composite element is not only conducive to the continuation of the transition layer growth, and can significantly improve the bonding strength between the metal layer 1 and the surface of the piezoelectric composite element. The sputtered metal layer 2 is used as an intermediate protective layer for the electrode of the piezoelectric composite element, and the metal layer 2 effectively avoids damage to the metal layer 1 caused by high-temperature molten solder during welding. The sputtered metal layer 3 is used as the surface protection layer of the electrode of the piezoelectric composite element, and the metal layer 3 improves the weldability and oxidation resistance of the electrode.
所述的金属层1为Ti电极层，Ti电极层溅射在压电复合元件表面，溅射时间为10～15min，Ti电极层层厚为80～100nm。金属层2为Cu电极层，Cu电极层溅射在Ti电极层的表面，溅射时间为30～45min，Cu电极层层厚为1500～2000nm。金属层3为Ag电极层，Ag电极层溅射在Cu电极层表面，溅射时间为12～18min，Ag电极层层厚为300～500nm。The metal layer 1 is a Ti electrode layer, and the Ti electrode layer is sputtered on the surface of the piezoelectric composite element, the sputtering time is 10-15 minutes, and the thickness of the Ti electrode layer is 80-100 nm. The metal layer 2 is a Cu electrode layer, the Cu electrode layer is sputtered on the surface of the Ti electrode layer, the sputtering time is 30-45min, and the thickness of the Cu electrode layer is 1500-2000nm. The metal layer 3 is an Ag electrode layer, the Ag electrode layer is sputtered on the surface of the Cu electrode layer, the sputtering time is 12-18 min, and the thickness of the Ag electrode layer is 300-500 nm.
本发明的有益效果：本发明制备得到的压电复合元件表面电极电阻低、结合强度高、焊接性强，利于大批量生产及商业化推广应用。Beneficial effects of the present invention: the piezoelectric composite element prepared by the present invention has low surface electrode resistance, high bonding strength and strong weldability, which is beneficial to mass production and commercial popularization and application.
附图说明Description of drawings
图1为PZT压电复合元件电极制备工艺路线图；图中依次为：A为PZT压电复合元件；B为PZT压电复合元件的研磨；C为PZT压电复合元件的清洗与除油；D为紫外线照射处理；E为PZT压电复合元件电极的制备。Figure 1 is the process roadmap for the preparation of electrodes of PZT piezoelectric composite elements; the sequence in the figure is: A is the PZT piezoelectric composite element; B is the grinding of the PZT piezoelectric composite element; C is the cleaning and degreasing of the PZT piezoelectric composite element; D is ultraviolet irradiation treatment; E is the preparation of PZT piezoelectric composite element electrodes.
图2为PZT复合元件电极示意图；Fig. 2 is the schematic diagram of the electrode of PZT composite element;
图中：1PZT压电复合元件电极的Ag电极层；2PZT压电复合元件电极的Cu电极层；3PZT压电复合元件电极的Ti电极层。In the figure: the Ag electrode layer of the 1PZT piezoelectric composite element electrode; the Cu electrode layer of the 2PZT piezoelectric composite element electrode; the Ti electrode layer of the 3PZT piezoelectric composite element electrode.
具体实施方式Detailed ways
以下结合技术方案和附图详细说明本发明的具体实施方式。The specific implementation manners of the present invention will be described in detail below in conjunction with the technical solutions and accompanying drawings.
首先，先后利用自动压力研磨抛光机对PZT压电复合元件进行研磨；随后进行去杂质及除油处理；然后，通过紫外线照射对PZT压电复合元件表面改性；最后，在PZT压电复合元件表面溅射一定厚度的Ti、Cu、Ag作为PZT压电复合元件电极。Firstly, the PZT piezoelectric composite element was ground successively by using an automatic pressure grinding and polishing machine; then impurities and oil were removed; then, the surface of the PZT piezoelectric composite element was modified by ultraviolet irradiation; finally, the PZT piezoelectric composite element A certain thickness of Ti, Cu, Ag is sputtered on the surface as the electrode of the PZT piezoelectric composite element.
实施例1的具体实施步骤如下：The specific implementation steps of embodiment 1 are as follows:
1)PZT压电复合元件表面处理1) Surface treatment of PZT piezoelectric composite components
本实施例中PZT压电复合元件的尺寸为10mm×10mm×3mm(长×宽×厚)。按照以下顺序进行：对其利用自动压力研磨抛光机进行研磨处理，转速为50rpm，研磨时间为40min，使之表面平整度与粗糙度分别低于1μm和800nm；将PZT压电复合元件先后放入丙酮、无水乙醇、去离子水中常温下各超声清洗20min，以去除表面附着的灰尘杂质；放入40℃的除油液中除油10min，以去除表面的皂化油和矿物油；放入温度为60℃的烘箱中烘干35min；The size of the PZT piezoelectric composite element in this embodiment is 10mm×10mm×3mm (length×width×thickness). Carry out in the following order: Grind it with an automatic pressure grinding and polishing machine, the rotation speed is 50rpm, and the grinding time is 40min, so that the surface flatness and roughness are lower than 1μm and 800nm respectively; the PZT piezoelectric composite elements are put into the Acetone, absolute ethanol, and deionized water were ultrasonically cleaned at room temperature for 20 minutes to remove dust and impurities attached to the surface; put in a degreasing solution at 40°C for 10 minutes to remove saponified oil and mineral oil on the surface; Dry in an oven at 60°C for 35 minutes;
2)PZT压电复合元件表面改性2) Surface modification of PZT piezoelectric composite elements
对PZT复合元件表面在输出功率为8mW/cm2的条件下进行8min的紫外线照射处理，使复合元件表面产生含氧极性官能团，含氧极性官能团同金属原子强烈作用产生了强化学键而提高了金属层与复合元件表面之间化学键力，从而显著地提高了金属电极与复合元件之间的结合强度；The surface of the PZT composite element is irradiated with ultraviolet rays for 8 minutes under the condition of an output power of 8mW/cm2, so that the surface of the composite element generates oxygen-containing polar functional groups, and the oxygen-containing polar functional groups strongly interact with metal atoms to form strong chemical bonds and improve The chemical bond force between the metal layer and the surface of the composite element, thereby significantly improving the bonding strength between the metal electrode and the composite element;
3)PZT压电复合元件电极制备3) Electrode preparation of PZT piezoelectric composite element
完成PZT压电复合元件的表面预处理后，为增加电极与PZT压电复合元件的结合强度，首先要通过磁控溅射方法在PZT压电复合元件表面制备电极，溅射功率为200w，本底真空度为4×10-4Pa，经过10min的溅射制备100nm厚的Ti电极来作为PZT压电复合元件电极的过渡层，Ti原子同PZT压电复合元件表面上吸附的氧原子以及陶瓷氧化物中的氧原子相结合形成Ti的氧化物，极大地提高了Ti电极层与压电复合元件表面之间的结合强度，经过30min的溅射在Ti电极表面制备1500nm厚的Cu电极来避免焊接时高温焊锡对Ti电极层的破坏，再经过12min的溅射在Cu电极表面制备300nm厚的Ag电极作为抗氧化的PZT压电复合元件电极的焊接层，以获得良好的可焊接能力以及低电阻。After the surface pretreatment of the PZT piezoelectric composite element is completed, in order to increase the bonding strength between the electrode and the PZT piezoelectric composite element, the electrode must first be prepared on the surface of the PZT piezoelectric composite element by magnetron sputtering. The sputtering power is 200w. The bottom vacuum is 4×10 -4 Pa. After 10 minutes of sputtering, a 100nm thick Ti electrode is prepared as the transition layer of the electrode of the PZT piezoelectric composite element. The Ti atoms are the same as the oxygen atoms adsorbed on the surface of the PZT piezoelectric composite element and ceramics Oxygen atoms in the oxide combine to form Ti oxide, which greatly improves the bonding strength between the Ti electrode layer and the surface of the piezoelectric composite element. After 30 minutes of sputtering, a 1500nm thick Cu electrode is prepared on the surface of the Ti electrode to avoid The damage of high-temperature solder to the Ti electrode layer during welding, and then sputtering for 12 minutes to prepare a 300nm thick Ag electrode on the surface of the Cu electrode as the welding layer of the oxidation-resistant PZT piezoelectric composite element electrode to obtain good weldability and low resistance.
实施例2的中，步骤2)中对PZT复合元件表面改性的输出功率为12mW/cm2，紫外线照射时间5min；步骤3)中的溅射Ti电极层时间为12min，溅射Cu电极层时间为40min，溅射Ag电极层时间为15min；其他条件与实施例1相同。In embodiment 2, the output power to the surface modification of PZT composite element in step 2) is 12mW/cm , the ultraviolet irradiation time 5min; Step 3) in the sputtering Ti electrode layer time is 12min, sputtering Cu electrode layer time 40min, and the time for sputtering the Ag electrode layer was 15min; other conditions were the same as in Example 1.
实施例3的中，步骤2)中对PZT复合元件表面改性的输出功率为16mW/cm2，紫外线照射时间3min；步骤3)中的溅射Ti电极层时间为15min，溅射Cu电极层时间为45min，溅射Ag电极层时间为18min；其他条件与实施例1相同。In embodiment 3, the output power to the surface modification of PZT composite element in step 2) is 16mW/cm , the ultraviolet irradiation time 3min; Step 3) in the sputtering Ti electrode layer time is 15min, sputtering Cu electrode layer time 45min, and the time for sputtering the Ag electrode layer was 18min; other conditions were the same as in Example 1.
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| CN1565078A (en) * | 2002-07-31 | 2005-01-12 | 株式会社村田制作所 | Piezoelectric component and production method therefor |
| DE102005046295A1 (en) * | 2005-09-28 | 2007-03-29 | Michael Johannes Jensen | Process for production of a piezoelectric heat converter metallizing of a piezoelectric material bonded to a ceramic layer useful miniature piezoelectric technology formation of troughs in the piezoelectric ceramic by UV laser treatment |
| KR101476742B1 (en) * | 2013-11-14 | 2014-12-29 | 포항공과대학교 산학협력단 | Method for manufacturing nano generator |
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