TW381067B - Method for producing low-temperature firing piezoelectric ceramics - Google Patents
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五、發明説明(l ) A7 B7 發明背景 · 以PbZr03-PbTi〇3(PZT)爲主成份的壓電 優良的壓電性質,早自1 950年代起即被廣泛 件、擴音器、超音波振動子、蜂鳴器、壓電 延遲線等電氣-機械能量轉換元件上 般 陶瓷由於具有 運用於點火元 濾波器和壓電 用的PZT壓電 在此高溫下燒 質和顯微結構 元件小型化、 電材料的發展 作方法是先利 至1 OOum的陶 燒結而成,由 數十至上百之 ί占有很高之比 抗氧化、能於 例如常用的 能使用的溫度 陶瓷其燒結溫度需達1 2 5 0 °C〜1 3 5 0 °C間 結會引起氧化鉛嚴重揮發,使材料的壓電 控制不易,且會引起環境污染;此外,隨g 低操作電壓的發展趨勢,積層式元件已成壓 主流之一,以積層式壓電致動器爲例,其製 用刮刀成型法(Doctor Blade)製作厚度爲1 〇 瓷薄片,經塗附電極後,再熱壓疊積、共同 於爲獲得較大位移量,所需疊積的層數在 間,以致內部電極在致動器硏製的成本上 例,而在積層式元件中所用的電極材料爲能 高溫共燒,需使用白金、鈀、銀等貴重金屬 鈀銀合金,隨著鈀含量的增加,電極材料所 隨之增加,相對地成本亦隨之上揚,其中p|}/Ag = 30/70所 --------< -裝------訂------:级 (請先閲讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消費合作社印製 能使用的溫度在1 150 t以下,至於純銀膠的 96〇 °C以下,因此如何降低壓電陶瓷的燒結溫 層式壓電致動器的重要關鍵之一。總之,發展 °c以下)的壓電陶瓷,不僅能減少能源損耗及 境污染,且能使積層式壓電元件共燒用的內Μ極改用以銀 爲主的電極材料,大幅降低製作成本。 燒結溫度則在 度成爲硏製積 低溫燒結(960 降低可能的環 本紙張尺度適用中國國家標準(CNS〉Α4規格(210 X 297公釐) A7 B7 五、發明説明( 在高壓電應變常數(d33)和機電偶合係數 料硏發方面’ PbZr03-PbTib3二元系壓電材料 高Kp之要求,但燒結溫度往往高達1250°C以 材料的燒結溫度降低,並維持高d33及高Kp (K p)的壓電材 雖可達高d33、 上;爲使壓電 的良好壓電性 質,在成份的調整上可添加一至兩種弛叆性鐵電材料 (Relaxor F e r r o e 1 e c tr i c s) 如 Pb(Ni1/3Nb 3)03(PNN)V. Description of the invention (l) A7 B7 Background of the invention · PbZr03-PbTi〇3 (PZT) as the main component of the piezoelectric excellent piezoelectric properties, as early as the 1950s, it has been widely used parts, loudspeakers, ultrasound Ceramics such as vibrators, buzzers, piezoelectric delay lines, and other electrical-mechanical energy conversion elements have PZT piezoelectrics used for igniter filters and piezoelectrics. At this high temperature, the burn-in and microstructure components are miniaturized. The development method of electrical materials is firstly sintered with ceramics up to 100 μm. From tens to hundreds of ceramics, it has a high ratio of oxidation resistance and can be used at, for example, commonly used temperature ceramics. The sintering temperature must reach 1 The junction between 2 0 0 ° C and 1 350 ° C will cause severe volatilization of lead oxide, making piezoelectric control of the material difficult, and causing environmental pollution. In addition, with the development trend of low operating voltage g, multilayer components have been It is one of the mainstreams. Taking laminated piezoelectric actuators as an example, the manufacturing method uses doctor blade to make a porcelain slice with a thickness of 10. After coating the electrodes, it is then hot-pressed and stacked together. To obtain a large amount of displacement, the layer to be stacked In the meantime, the cost of the internal electrode being fabricated by the actuator is the same as the above example, and the electrode material used in the multilayer component is capable of co-firing at high temperatures. Platinum, palladium, silver and other precious metals such as palladium-silver alloys are required. As the content increases, the electrode material increases, and the relative cost also rises. Among them, p |} / Ag = 30/70 .-------- <-装 ------ Order- -----: Grade (please read the notes on the back before filling this page) The temperature printed by the Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs can be used below 1 150 t, as for the pure silver glue below 96 ° C, Therefore, how to reduce the sintered stratospheric piezoelectric actuator of piezoelectric ceramics is one of the important keys. In short, the development of piezoelectric ceramics below ° c can not only reduce energy loss and environmental pollution, but also change the inner M pole used for multilayer piezoelectric element co-firing to silver-based electrode materials, which greatly reduces the production cost . The sintering temperature becomes low-temperature sintering at a temperature of 960 ° C. (960) The reduction of the possible size of the paper is applicable to Chinese national standards (CNS> A4 specifications (210 X 297 mm). A7 B7 V. Description of the invention (In the high-voltage electrical strain constant ( d33) and electromechanical coupling coefficient material development 'PbZr03-PbTib3 binary system piezoelectric material requires high Kp, but the sintering temperature is often as high as 1250 ° C, the sintering temperature of the material is reduced, and high d33 and high Kp (K p Although the piezoelectric material can reach high d33, high; in order to make the piezoelectric good piezoelectric properties, one or two relaxation ferroelectric materials (Relaxor Ferroe 1 ec tr ics) such as Pb can be added to the composition adjustment. (Ni1 / 3Nb 3) 03 (PNN)
Pb(Zni,3N.b2/3)〇3 (PZN)矛口 Pb(Mgi/3Nb2/3)〇3(.)MN)二種,且 其成份均取在所謂的MPB(Morphotropic Ph 附近,亦即 Tetrahedral和Rhombohedral兩相 ase Boundary) 共存區域,以 獲得較高的d33和Kp値。1977年日本的Bunno等人提出 PNN-PZ-PT的三元系相圖後,1981年Sony公 報導PNN-PZN-PZ-PT四元系壓電陶瓷在氧氣 °C〜1 200燒結,並獲致良好的壓電特性;^ 人在美國專利第4,765,9 19號中詳細描述 Bi203、Nb205等Donor的PNN-PZ-PT壓電陶瓷 而其所需的燒結溫度在1 200 °C〜1 300 °C ; 司的 Kitamura 氛中能於1 1 5 0 88年 Tomita等 添加Sb203 、 的各種特性, 1989年美國的 : HI I n IK ^ ^^^1 n m^i 11^11 n^i 1 -OJ (請先閱讀背面之注意事項再填湾本頁) 經濟部中央標準局員工消費合作社印製 1 980年日本Pb (Zni, 3N.b2 / 3) 〇3 (PZN) spear mouth Pb (Mgi / 3Nb2 / 3) 〇3 (.) MN), and its components are taken near the so-called MPB (Morphotropic Ph, also near That is, Tetrahedral and Rhombohedral two-phase ase Boundary) coexist region to obtain higher d33 and Kp 値. In 1977, Bunno and others in Japan proposed the ternary phase diagram of PNN-PZ-PT. In 1981, the Sony Gazette PNN-PZN-PZ-PT quaternary piezoelectric ceramics was sintered at oxygen ° C ~ 1 200 and obtained Good piezoelectric characteristics; ^ US Pat. No. 4,765,9 19 describes in detail P203-PZ-PT piezoelectric ceramics such as Bi203 and Nb205, and the required sintering temperature is 1 200 ° C ~ 1 300 ° C; In the Kitamura atmosphere of the company, various properties of Sb203 can be added to Tomita and others in 1988. In the United States in 1989: HI I n IK ^ ^^^ 1 nm ^ i 11 ^ 11 n ^ i 1 -OJ (Please read the notes on the back before filling in this page.) Printed by the Consumer Cooperatives of the Central Standards Bureau, Ministry of Economic Affairs, Japan, 1980
Choi等人報導PMN-PT壓電陶瓷於1 250°C燒結,其d33値可 達669pC/N :目前所知最低燒結溫度的商用b末爲日本東 北金屬公司用於製作積層式壓電致動器、f扁號爲N-1 0的 PNN-PZ-PT三元系壓電陶瓷,其燒結溫度可泜至1100°C。 利用助燒劑以降低壓電陶瓷燒結溫度所作的硏究,最 早爲1 979年美國的Schulze等人提出在PZT陶瓷中添加大 量的Pb5Ge3Ou (高達30wt%)能使燒結溫度至1〇〇〇 °C以 下,但因添加量太高以至壓電特性顯著下降 2 本紙張尺度適用中國國家標準(CNS ) A4規格(2丨0 X 297公釐) 五、發明説明(3 ) + NaF),使 PZT 料的介電常數Choi et al. Reported that PMN-PT piezoelectric ceramics were sintered at 1 250 ° C, with a d33 値 of up to 669 pC / N: the lowest commercial sintering temperature currently known is not used by Tohoku Metals Corporation to make laminated piezoelectric actuators. The sintering temperature of the PNN-PZ-PT ternary series piezoelectric ceramics with f-number N-1 0 can reach 1100 ° C. Researches on using sintering aids to reduce the sintering temperature of piezoelectric ceramics. As early as 1979, Schulze et al. Of the United States proposed that adding a large amount of Pb5Ge3Ou (up to 30% by weight) in PZT ceramics can bring the sintering temperature to 1000 °. Below C, but the piezoelectric properties are significantly reduced due to the high amount of addition 2 The paper size applies the Chinese National Standard (CNS) A4 specification (2 丨 0 X 297 mm) V. Description of the invention (3) + NaF) makes PZT Dielectric constant
的 Takahashi 在 PZT 中加入 5〜1 5mol%(2PbF 的燒結溫度由1 2 9 0 °c 至8 0 0 °c,但材 (ε^) ’機電偶合係數(kr)和機械品質係數(Qm)均隨添加量之 an於美國專利 使PZT陶瓷的 下降。1 980年 BaTi,03的燒結 電容器產業隨 (fie02、Si02 等 點的化合物, CdO 、 CuO 、 的性質。所以, 末爲助燒劑, 增加而明顯降低:1 98 1年Witter和Buchan 第4,2 83,2 8 8號指出,添加0.25〜6wt%V205能 燒結溫度降至960 °C,但其壓電特性會隨之 代初期BaTi03的低溫燒結技術已臻成熟, 溫度由1300 °C以上降至1100 °C,積層陶瓷 之蓬勃發展,其中所用的助燒劑由B203 玻璃形成劑爲主體(GlassFormer)以合成低熔 再加上能進入鈣鈦礦結構的PbO、BaO、 持良好的壓電 ,用以降低摻 結溫度至9 0 0 換能器、濾波 料。此外,成 B2〇3玻璃降低 03 、 Si02 、Takahashi added 5 ~ 1 5mol% (2PbF sintering temperature from 1 2 0 ° C to 8 0 0 ° C in PZT, but the material (ε ^) 'mechanical coupling coefficient (kr) and mechanical quality coefficient (Qm) The addition of an amount in the U.S. patent makes the PZT ceramics decline. In 1980, the sintered capacitor industry of BaTi, 03 followed the properties of (fie02, Si02, etc. compounds, CdO, CuO, and so on. Therefore, it is not a sintering aid, Increase and decrease significantly: 1 98 1 Witter and Buchan No. 4, 2 83, 2 8 8 pointed out that the addition of 0.25 ~ 6wt% V205 can reduce the sintering temperature to 960 ° C, but its piezoelectric characteristics will follow the initial generation of BaTi03. The low-temperature sintering technology has matured, and the temperature has dropped from more than 1300 ° C to 1100 ° C. The multilayer ceramics have developed vigorously. The sintering aid used in it is B203 glass former as the main body (GlassFormer) to synthesize low-melting and energy. The PbO and BaO entering the perovskite structure have a good piezoelectricity to reduce the doping temperature to 900 transducers and filter materials. In addition, the formation of B2O3 glass reduces 03, Si02,
ZnO ' Bi203等修飾齊!j(Modifier)以調整材料 往後壓電材料低溫燒結的硏究多選用玻璃粉 例如1 9 8 6年成功大學的S.Y. Cheng等人,_摻有Nb205的 PZT中加入Li2C03、Na2C03、B2〇3爲助燒劑,但其燒結 溫度只能降至1〇7〇 °C。1 989年中國大陸的桂治輪等人 在摻有錳的PZT材料添加1〜5wt%的B203-Bi203-Cd0,有 效地使燒結溫度由1250 °C降至96(TC,並維 特性,此外,他們也利用Pb0-Si02爲助燒劑 有錳鎘的PNN-PZ-PT三元系壓電陶瓷的燒 °c ’桂治輪等人的硏究目的在開發用於硏製 器所需之高Qm、高κρ、低溫燒結的壓電材 功大學的吳朗等人於1 993年報導利用pbO-壓電材料的燒結溫度。上述硏究均添加B %五、發明説明(4 ) kl B7 G eCh等玻璃形成劑以增加壓電材料在助燒 低助燒劑的熔點,但因^離子半徑小,無法 格’會使玻璃相殘留在晶粒邊界上,對材料 能產生不良影響。 發明目的 本發明即針對高d33、高Kp壓電陶瓷低溫燒結之需要 在 PXN-PbZr03-PbTi03 壓電陶瓷,其中 ΡΧΝ=:ΡΝΝ、ΡΖΝ 或 ΡΜΝ’加入不含8203、Ge02、Si02等玻璃形^劑的助燒劑 使高d33、高KP壓電陶瓷能於960°C以下燒結 好的壓電及介電等電氣性質,在用於製作壓 低鉛污染,並減少積層式壓電元件內部電極 劑的溶解及降 溶入鈣鈦礦晶 的機械性質可 ,並能保持良 電元件時能降 所需成本。 (請先閱讀背面之注意事項再填寫本頁)ZnO 'Bi203 and other modifications! j (Modifier) is used to adjust the material for low-temperature sintering of piezoelectric materials. Mostly, glass powder is used. For example, SY Cheng and others at Chenggong University in 1986. Li2C03, Na2C03, and B203 are added to PZT doped with Nb205. It is a sintering aid, but its sintering temperature can only be reduced to 1070 ° C. In 1989, Guizhi Lun and others in China added 1 ~ 5wt% of B203-Bi203-Cd0 to PZT material doped with manganese, which effectively reduced the sintering temperature from 1250 ° C to 96 ° C, and maintained the characteristics. In addition, They also used Pb0-Si02 as a sintering aid for the firing of PNN-PZ-PT ternary piezoelectric ceramics with manganese and cadmium. C 'Guizhi Lun et al's research purpose was to develop the high Qm required for the controller , High-κρ, low-temperature sintered piezoelectric materials Wu Lang of Gong University et al. Reported in 1 993 that the sintering temperature of pbO-piezoelectric materials was used. All the above studies were added with B%. V. Description of the invention (4) kl B7 G eCh The glass-forming agent is added to increase the melting point of the piezoelectric material in the low-burning and low-burning agent, but the small ionic radius prevents the glass phase from remaining on the grain boundary, which can adversely affect the material. The invention refers to the need for low temperature sintering of high d33 and high Kp piezoelectric ceramics. PXN-PbZr03-PbTi03 piezoelectric ceramics, where PXN =: PNN, PZN or PMN 'are added without the aid of glass-based agents such as 8203, Ge02, and Si02. The sintering agent enables high-d33 and high-KP piezoelectric ceramics to be sintered below 960 ° C. The gas properties can be used to reduce lead pollution and reduce the mechanical properties of the dissolution of the internal electrode agent of the laminated piezoelectric element and reduce the dissolution into the perovskite crystals, and can reduce the cost when maintaining a good electrical component. (Please read the notes on the back before filling out this page)
圖式說明 B1 — ^ 0.40PNN-0.23PZ-0.37PT^ 1 的燒結密度與燒結溫度之關係圖。 圖二係 0.40PNN-0.23PZ-0.37PT添加 1 的d33 ' Kp與燒結溫度之關係圖。 本發明之詳細說明 本發明在壓電材料配製方面,使用PbO 3wt%助燒劑 3wt%助燒劑Illustration of the relationship between sintering density and sintering temperature of B1 — ^ 0.40PNN-0.23PZ-0.37PT ^ 1. Figure 2 shows the relationship between d33 'Kp and sintering temperature of 0.40PNN-0.23PZ-0.37PT with 1 added. Detailed description of the present invention In the preparation of piezoelectric materials, the present invention uses PbO 3wt% burning aid 3wt% burning aid
NiO 、 ZnO 、-1· 經濟部中央標準局員工消費合作社印製NiO, ZnO, -1 Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs
MgO、Nb2〇5、Ti〇2、Zr〇2爲原料,依 PXN-IfbZr03-PbTiO 之計量比,其中PXN = PNN、PZN或PMN 末,再以Zr〇2球溼磨混合,烘乾後於850 °C 〜6小時以合成鈣鈦礦結構;不含B2〇3、G 玻璃形成劑、低溫燒結用的助燒劑,其成份爲 或 PbO)- z(CuO 或 ZnO),其中 x+ y + z = 稱量所需的粉 〜900鍛燒3 e02、Si02 等 xCd0-y(Bi203 ,0.40 $ x 4 本紙張尺度適用中國國家標準(CNS ) Λ4規格(210X 297公釐) 部 tMgO, Nb205, Ti〇2, Zr〇2 are used as raw materials, according to the measurement ratio of PXN-IfbZr03-PbTiO, where PXN = PNN, PZN or PMN, and then wet-milled with Zr〇2 balls and mixed. 850 ° C ~ 6 hours to synthesize perovskite structure; does not contain B203, G glass forming agent, low temperature sintering aid, its composition is or PbO)-z (CuO or ZnO), where x + y + z = powder required for weighing ~ 900 calcined 3 e02, Si02, etc. xCd0-y (Bi203, 0.40 $ x 4) This paper size is applicable to the Chinese National Standard (CNS) Λ4 specification (210X 297 mm) Department t
A 標 準 員 工 消 費 合 作 杜 印 製 Α7 Β7 五、發明説明(5 ) S 0.80 , 0.20S 0.50 , 〇$ 〇.2〇 , 依比例稱量、 溼磨混合,於5 00 °C〜70、°C鍛燒3〜6小日: f ’隨後取1〜 5wt %助燒劑與壓電粉末,一起以Zr〇2球涯 磨混合,烘乾 後添加1〜2wt % PVA進行造粒,經過篩〗 i乞壓成1 5 m m φ xl.5mm1'的圓片;圓片放在坩鍋中加蓋密閉 燒結,也可以 在高溫爐中敞開燒結,燒結溫度爲8 5 0 °C〜 1 000 °C,燒結 時間3〜6小時;燒結後的試片先將厚度磨 至1 mm左右, 經3um Al2〇3粉末拋光後,雙面塗以銀膠作 爲電極,極化 時將試片置於60〜100 °C左右的Silicon oil 中,施以2 0〜 3 Ok V/cm左右之電場極化5〜10分鐘;極化 後的試片於室 溫放置24小時,量測頻率爲1 KHz時的ε 3 3及tan 6値’ 壓電參數之量測採用IRE Standards測試規| 范,以 HP4194 阻抗分析儀量測試片的共振頻率與反共振頻 率,從而求出 材料的Kp、Qm,至於材料的壓力應變常數 則以 d33 meter 量得。 實例 依 0.40PNN-0.23PZ-0.37PT 之計量比 1秤取適量的 PbO、NiO、Nb2〇5、Ti〇2、Zr〇2 粉末,3 求磨1 6小時, 烘乾後於85 0 t鍛燒3小時以合成鈣鈦礦結 構,助燒劑的 成份取 〇_50CdO-0.45Bi203-0.05CuO,依比侈 j稱量、溼磨混 合16小時,於600 °C鍛燒3小時,隨後取1 〜3 w t %助燒 劑與主成份 0.40PNN-0.23PZ-0.37PT 粉末, --起以Zr02球 溼磨混合20小時,經烘乾、造粒、成型,於 850。。〜1〇〇0 °C燒結時間3〜6小時,燒結後的試片經硏| _ 5 丨1後,雙面塗 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) ...................... 衣 訂 請 先 閲 讀 背 ιέ 事 項 再 填 寫 本 頁 五、發明説明(6) ΑΊ B7 以銀膠作爲電極,極化條件爲90 °C、20kV|/cm、6分鐘; 極化後的試片於室溫放24小時,再進行各項電性測試 表一是不加助燒劑的0.40PNN-0.23PZ- 0.37PT粉末於^ 1 05 0 °C〜1?0 0 t燒結3小時所測得的材料ψ性,其中燒結 理論密度),以 成份在1 2 0 〇。(3 1.8 % , tL = 密度需在1 1 50 °c以上才能達7.9g/cm3 (96 % 致在此溫度下的壓電及介電參數均偏低,此 4 163 燒結可得最佳特性:ε 3: 610pC/N , kp=0.69 。 圖一顯示 0.40PNN-0.23PZ-0.37PT 添加 tai 1 wt %助燒劑 0.50CdO-0.45Bi2〇3-〇 〇5CuO,其燒結溫度需 2 950 °C,密A Standard Employee Consumption Cooperation Du printed A7 B7 V. Description of the invention (5) S 0.80, 0.20S 0.50, 〇 $ 〇0.20, weighed in proportion, wet-milled and mixed, at 5 00 ° C ~ 70, ° C Calcination for 3 ~ 6 small days: f 'Subsequently take 1 ~ 5wt% of the burning aid and piezoelectric powder, mix them together with Zr〇2 ball mill, dry and add 1 ~ 2wt% PVA for granulation, and pass through the sieve〗 i Be pressed into a 15 mm φ xl.5mm1 'wafer; the wafer is placed in a crucible and sealed and sintered. It can also be opened in a high temperature furnace. The sintering temperature is 8 50 ° C ~ 1 000 ° C. The sintering time is 3 to 6 hours; the sintered test piece is ground to a thickness of about 1 mm, polished with 3um Al203 powder, and coated with silver glue on both sides as the electrode. In Silicon oil at about 100 ° C, an electric field of about 20 to 3 Ok V / cm is applied for 5 to 10 minutes for polarization; the polarized test piece is left at room temperature for 24 hours, and the measurement frequency is 1 KHz. ε 3 3 and tan 6 値 'piezoelectric parameters are measured using the IRE Standards test gauge | Fan, using the HP4194 impedance analyzer to measure the resonance frequency and anti-communication of the test piece Frequency, thereby obtaining the material Kp, Qm, as to pressure of the material strain constant d33 meter the amount of available places. Example: According to the measurement ratio of 0.40PNN-0.23PZ-0.37PT, 1 weigh the appropriate amount of PbO, NiO, Nb205, Ti〇2, Zr〇2 powder, and then grind for 16 hours. After drying, forging at 85 0 t Burn for 3 hours to synthesize the perovskite structure. The composition of the sintering aid is 0-50CdO-0.45Bi203-0.05CuO, weighed according to luxury j, mixed by wet milling for 16 hours, and calcined at 600 ° C for 3 hours. 1 ~ 3 wt% of burn aid with 0.40PNN-0.23PZ-0.37PT powder as main component, --- Wet mill with Zr02 ball for 20 hours, dry, granulate, and shape at 850. . ~ 100 ° C sintering time is 3 ~ 6 hours. After the sintered test piece has undergone 硏 | _ 5 丨 1, the size of the double-sided coated paper is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) .. .......... Please read the back of the clothes order first and then fill out this page. V. Description of the invention (6) ΑΊ B7 With silver glue as the electrode, polarization conditions 90 ° C, 20kV | / cm, 6 minutes; The polarized test piece was left at room temperature for 24 hours, and then subjected to various electrical tests. Table 1 is 0.40PNN-0.23PZ- 0.37PT without adding a combustion aid. The ψ properties of the powder were measured after sintering the powder at ^ 1 05 0 ° C ~ 1? 0 0 t for 3 hours (the theoretical density of sintering), with the composition at 1 2 0 0. (3 1.8%, tL = density needs to be above 1 1 50 ° c to reach 7.9g / cm3 (96% due to low piezoelectric and dielectric parameters at this temperature, this 4 163 sintering can obtain the best characteristics : Ε 3: 610pC / N, kp = 0.69. Figure 1 shows 0.40PNN-0.23PZ-0.37PT with the addition of tai 1 wt% sintering agent 0.50CdO-0.45Bi2〇3-〇〇5CuO, and its sintering temperature needs 2 950 ° C, dense
度才能達7.9g/cm3以上,添加量增至2〜 °C即可得良好的緻密度。 圖二顯示添加lwt%助燒劑的0.40PNN wt %,在 9〇〇The density can reach more than 7.9g / cm3, and the added amount can be increased to 2 ~ ° C to obtain good density. Figure 2 shows 0.40PNN wt% with lwt% burning aid at 900.
0.23PZ-0.37PT 需在1 000°C才能得到較高的d33和Kp値,添加量爲2wt%者 C請先閑讀背面之注意事項再填寫本頁} -=& 經濟部令央橾準局員工消費合作社印製 在9 0 0 °C〜1 0 0 0 °C均具有良好的壓電特性(d Kpg 0.63),但當添加量增至3wt%時,材料 略微下降。 表二爲添加2wt%助燒劑的0.4 0PNN-0 電陶瓷於850 °C〜1 〇〇〇 °C燒結3〜6小時所 性,其中在8 5 0 °C燒結3小時,密度即達7 結時間即使延至6小時所得壓電及介電參數 結溫度升至9 0 0 °C後,燒結時間爲3或6小4 ’所得壓電特 性與95 0 °C、1 000 °C者相當,顯示本材料對 感,在很寬的溫度範圍內所得的P、 3 ^ 540pC/N > 的壓電係數會 3PZ-0.37PT 壓 測得的材料特 9g/cm3,但燒 仍偏低;而燒 L. 3 3 燒結溫度不敏 t a η 5 、d 3 3 和 6 本紙張尺度適用中國國家標率(CNS ) A4規格(2丨OX297公釐) 部 t 央 標 準 局 員 工 消 k 合 社 印 製 A7 B7 五、發明説明(7 ) Kp變,化均很小。在不做PbO氣氛補償的開 放式燒結試驗 中’同樣在900 °c燒結 < 小時所得到的介電 、壓電特性與 有PbO氣氛補償者相當,故添加Cd〇_Bi2〇3_ CuO後於低溫 進行燒結能大幅降低PbO揮發,減少可能的 環境污染,且 燒結溫度降至900 °C時用於製作積層式壓電 元件所使用的 內部電極可改採銀電極,取代昂貴的白金或 鈀,能大幅降 低元件的製作成本。此外,本材料於900 t 燒結所得的試 片磨薄至25// m,g登明具有不錯的機械強 度。 7 本紙張尺度適用中國國家標隼(CNS〉A4規格(210X297公釐) 請 聞 背 面 意 Φ 項 再 填 寫 本 頁 訂 A7 B7 經濟部中央標準局員工消費合作社印製 五、發明説明(8) 表一 ··不添加助燒劑的0.40PNN-0.23PZ-0.37PT燒結j • 憲的所有特性 Tsint Time P (g/cm3) ^ 33 tan 5(%) ^33 Kp Qm 1050°C 3h 7.61 2993 2.07 506 0.589 70 1100°C 3h 7.80 3149 1.86 533 0.624 74 1150°C 3h 7.90 3502 1.84 555 0.654 70 1200°C 3h 7.96 4163 1.80 610 0.696 63 表二:添力口2wt% 助燒劑的0.40PNN-0.23PZ-0.37PT燒 結體的所有特性 Tsint Time p (g/cm3) ε 33 tan δ (%) d33 Kp Qm 85〇t: 3h 7.93 3430 2.50 475 0.569 67 850〇C 6h 7.98 3688 2.16 527 0.590 62 900°C 3h 7.95 3987 2.05 540 0.635 65 900°C 6h 7.96 3756 2.10 555 0.648 63 900。。* 6h 8.00 3860 2.09 545 0.640 63 950¾ 3h 8.02 3860 2.09 550 0.645 62 1000°C 3h 8.00 3915 1.95 560 0.650 65 A開放式燒結 8 --------1 裝丨_^--.丨-訂------ (請先閱讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐〉0.23PZ-0.37PT need to be at 1000 ° C to get higher d33 and Kp 者, if the amount is 2wt% C, please read the precautions on the back before filling this page}-= & Ministry of Economic Affairs The quasi-station employee consumer cooperative has good piezoelectric characteristics (d Kpg 0.63) printed at 900 ° C to 100 ° C, but when the amount is increased to 3wt%, the material slightly decreases. Table 2 shows the properties of 0.4 0PNN-0 electric ceramics with 2wt% sintering aid at 850 ° C ~ 1000 ° C for 3 ~ 6 hours. Among them, it is sintered at 850 ° C for 3 hours, and the density is 7 Even if the junction time is extended to 6 hours, the piezoelectric and dielectric parameters obtained after the junction temperature rises to 9 0 ° C, the sintering time is 3 or 6 hours, and the obtained piezoelectric characteristics are equivalent to those of 95 0 ° C, 1 000 ° C. It shows the alignment of this material. The piezoelectric coefficient of P, 3 ^ 540pC / N > obtained over a wide temperature range will be 3PZ-0.37PT. The measured material is 9g / cm3, but the firing is still low; and Burning L. 3 3 Sintering temperature insensitivity ta η 5, d 3 3 and 6 This paper size is applicable to China National Standards (CNS) A4 specifications (2 丨 OX297 mm) Ministry t Central Standards Bureau staff printing A7 B7 V. Description of the invention (7) Kp changes and the chemical conversion is small. In the open-type sintering test without PbO atmosphere compensation, the dielectric and piezoelectric characteristics obtained after sintering at 900 ° C for <hours are comparable to those with PbO atmosphere compensation. Therefore, Cd〇_Bi2〇3_ CuO was added after Sintering at low temperature can greatly reduce the volatilization of PbO and reduce possible environmental pollution. When the sintering temperature drops to 900 ° C, the internal electrode used to make the multilayer piezoelectric element can be replaced with silver electrode instead of expensive platinum or palladium. Can significantly reduce the cost of manufacturing components. In addition, the test piece sintered at 900 t was thinned to 25 // m, and g Dengming had good mechanical strength. 7 This paper size applies to the Chinese national standard (CNS> A4 size (210X297mm) Please read the Φ item on the back and fill in this page to order A7 B7 Printed by the Staff Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 5. Form of Invention (8) 1. · 0.40PNN-0.23PZ-0.37PT sintering without the addition of a combustion aid j • All properties of the constitution Tsint Time P (g / cm3) ^ 33 tan 5 (%) ^ 33 Kp Qm 1050 ° C 3h 7.61 2993 2.07 506 0.589 70 1100 ° C 3h 7.80 3149 1.86 533 0.624 74 1150 ° C 3h 7.90 3502 1.84 555 0.654 70 1200 ° C 3h 7.96 4163 1.80 610 0.696 63 Table 2: 0.40 PNN-0.23PZ of Timlikou 2wt% burn aid All characteristics of -0.37PT sintered body Tsint Time p (g / cm3) ε 33 tan δ (%) d33 Kp Qm 85〇t: 3h 7.93 3430 2.50 475 0.569 67 850 ° C 6h 7.98 3688 2.16 527 0.590 62 900 ° C 3h 7.95 3987 2.05 540 0.635 65 900 ° C 6h 7.96 3756 2.10 555 0.648 63 900 ... * 6h 8.00 3860 2.09 545 0.640 63 950¾ 3h 8.02 3860 2.09 550 0.645 62 1000 ° C 3h 8.00 3915 1.95 560 0.650 65 A open sintering 8 -------- 1 Install 丨 _ ^-. 丨 -Order ------ (Please read the Precautions to fill out this page) This paper scale applicable Chinese National Standard (CNS) A4 size (210X297 mm>
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CN111875374A (en) * | 2020-08-06 | 2020-11-03 | 湖北大学 | Low-temperature sintered niobium-nickel-lead zirconate titanate piezoelectric ceramic material and preparation method thereof |
CN116854472A (en) * | 2023-09-04 | 2023-10-10 | 中国科学院上海硅酸盐研究所 | Microwave dielectric material and preparation method thereof |
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Cited By (3)
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CN111875374A (en) * | 2020-08-06 | 2020-11-03 | 湖北大学 | Low-temperature sintered niobium-nickel-lead zirconate titanate piezoelectric ceramic material and preparation method thereof |
CN116854472A (en) * | 2023-09-04 | 2023-10-10 | 中国科学院上海硅酸盐研究所 | Microwave dielectric material and preparation method thereof |
CN116854472B (en) * | 2023-09-04 | 2023-12-08 | 中国科学院上海硅酸盐研究所 | Microwave dielectric material and preparation method thereof |
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