CS197406B1 - Piezzoceramic substance - Google Patents

Abstract

Piezoceramic material (I) contg. PbTiO3 (II), PbZrO3 (III) and PbB' 1-alpha B" alpha O3 (IV) also contains PbB"' 1-a Biv alpha O3 (V), (in which B' and B"' are Nb5+, W6+; B" and Biv are Zn2+, Mg2+, Co2+, Mn2+, Ni2+; alpha = 1/2 for W6+ and 1/3 for Nb5+; if B' and B"' are Nb5+, then B" is Mg2+, and Biv is not Mn2+), the proportions of the components being 30.0-52.5 (37.5-42.5)(mole)% (II); 25.0-47.6 (33.0-42.0)% (III); 1.5-28.4 (5.0-15.0)% (IV) and 2.3-29.4 (5.0-15.0)% (V). The material is used in radioelectronics, acoustics, hydroacoustics, ultrasonic delay guides and filter technology. Electrical parameters and mech. quality suited to each of these fields can be obtd. (I) opt. contains modifying oxides.

Description

of ₇ es FESENK0 JEVGENIJ GRIGORJEVLS, DANCIGER ALLA HOW TO CHOOSE, FILIPJEV VIKTOR SEEDS, \ ^/ Ã ..

The author of the invention NIKOLAJEVIC, GRINEVA LUDMIL DEMJANOVNA. ROGAC TATANA VENIAMINOVNA, FERON ANATOLIJ DMITRIJEVIC, AKBAJEVA GALINA MIXERY, HEAVY JEVGENIJ IVANOVICE, PANIC ANATOLIJ JEVGENJEVIC. LISICINA LUDMILA GRIGORJEVNA, JAVRIKOVA SVĚTLANA ALEXEJEVNA, DUDKINA SVĚTLANA IVANOVNA. NEVSKIJ ALEXANDR NIKOLAJEVIC, ALESIN VLADIMIR AFANASJEVIC, KUPRIJANOV MICHAIL FEDOTOVIC, BALJUNIS JEVGENIJ STANISLAVOVIC, MORDANOV BORIS PETROVIC, ZITOMIRSglJ GRJGORIJ ABRAMICOVA RRAMICOVA, EYE VASILIJ ARSANOVIC, ELISTA,

FELDMAN NAUM BORISOVIČ, SMAŽEVSKAYA JEKATERINA GERASIMOVA, MOSCOW (USSR)

Piezoceramic substance

BACKGROUND OF THE INVENTION The present invention relates to piezoceramic agents containing PbTiO4, PbZrO4, and, as a third component, Pblib3 / Me3 or lead metal tungstate pBW3 / 3О3, wherein Me is a divalent metal selected from zinc, manganese, cobalt and nickel. These substances are used in radio engineering and electronics, as well as in acoustics, hydroacoustics, ultrasonic delay lines and filtration technology.

It is known that the substances that lie in the morphotropic region of two- and three-component solid solutions have the greatest piezoelectric effect. As the number of components increases, the size of the morphotropic region increases and the range of assemblies increases in extreme values.

For known piezoceramic substances which represent a ternary system of lead titanate - lead zirconate - lead metalobioate or lead metal tungstate, in which the divalent metal is selected from the group of zinc, magnesium, cobalt, manganese and nickel, the morphotropic composition has the parameters given tab. 1.

It can be seen from Table 1 that in many systems the values of the dielectric constant, the electromechanical coupling factor and the mechanical quality are insufficiently high. The dielectric losses known in some systems are high.

In addition, in many cases, for example in the development of high-frequency ultrasonic transducers, substances with a lower dielectric constant 33 33, with a relatively high electromechanical coupling factor Kp, are required. Known substances do not meet (see Table 1) these requirements.

The purpose of the invention is to overcome the above mentioned drawbacks.

SUMMARY OF THE INVENTION It is an object of the present invention to provide a novel piezoceramic substance with more efficient electrophysical parameters by introducing into the known substance the fourth component and, in some cases, subsequently modifying the substance obtained.

197 406

TABLE 1

PbB ¹ 1 Λ B ¹¹ * 03 in triple system Electrophysical parameters pore. C. Literature dielectr. constant E ^T 33 elektrome chán. binding factor Kp mechan. quality Q dielektric. losses (in weak field) w, »% 1 ^Pbm> 2/3 Za, / 3 ⁰ 3 1570-3120 0,568-0,714 - '- 2 ^{PbHbg /} ₃ Μβ ^ ^{/ 3} O ³ H. Ouchi: J. Am. Segan? Rn ^ 5 ¹ · 2137 0.638 65 1.87 3 ^{PbNb 2 /} ° ^{C / 3} ° ³ 1360-2030 0.64-0.73 305-420 - 4 PbNbg / ^ Mn «| 630-1000 0,35-0,61 1900-2030 1,1-2,3 5 ^{PbNbg / 3 Ni 1/3 03} me p. U.S. Pat. 45-14465 720-3200 0.4-0.61 Λ 95-161 - 6 ^{Pbw 1/2 Z} » ^{1/2 03} franc. U.S. Pat. 1554 730 1500-2500 0.52-0.59 72-80 - 7 ^PbW 1/2 “1/2 1/2 ° ³ franc. U.S. Pat. 1551 975 - 0,25-0,5 295-300 - β ^{PbW 1/2 Ni 1/2} ° ³ franc. U.S. Pat. 1554 730 1090-1800 0.4-0.6 15-80 - 9 ^PbW 1/2 ^Co l / 2 ⁰ 3 me p. U.S. Pat. 46-2354 1130-1980 0.42-0.63 ee

A piezoceramic substance according to the invention, comprising lead titanate PbTiO4, lead zirconate PbZrO4 and, as a third component, lead metabonate PbHbg / iMe2O4 or lead metal tungstate PbWi / gee / 2o0 *, in which Me is a divalent metal selected from magnesium, cobalt, manganese, and nickel are therefore in that they contain a fourth component of lead metalborate or metal tungstate. of the above formulas wherein Me 'is a divalent metal selected from the group of zinc, magnesium, cobalt, magnan and nickel, wherein when the third and fourth components are lead metallobioate of the above formula and the metal in the third nickel component is Me in the fourth component magnesium or cobalt, and if the third and fourth components are lead metallobate of the above formula and the metal Me in the third component magnesium, the metal in the fourth component is zinc, cobalt or nickel, said components being in the following molar percentages:

lead titanate 30.0 to 52.5 lead zirconate 25.0 to 47.6 the third component 1.5 to 28.4 the fourth component 2.3 to 29.4

The following molar ratios are preferred:

lead titanate 37.5 to 42.5 lead zirconate '33.0 to 42.0 the third component 5.0 to 15.0 fourth component 5.0 to 15.0

The third and fourth components can be expressed as follows:

197 40β where

B a BIU denotes Eb ³⁺ or W ⁶⁺ В ¹¹ a denotes Zn ²⁺ , Mg ²⁺ , С <5 ²⁺ , tin ^{2+ or} Ni ²⁺ QC - 1/2 for W ⁶ * and 1/3 ^for Mb ⁵ * Acquisition of consumption ^{em p} f ^j e ^- where B ¹ - B ¹¹¹ »Nb ^{5+ and} B ^{11 -} Ni ² * is B ¹⁷ » Mg ²⁺ or C ²⁺ and if В ¹ »B ¹¹¹ = Nb ⁵⁺ and B ¹¹ = Mg ² * is ^B17 = Zn ²⁺ C ^{2+ no} b ^o · Ni ²⁺ .

The following are piezoceramic substances, which are called as systems and whose content of components is given in mole percent:

System 1 PbTÍO ₃ 32.5 - 45.0 PbZrO ₃ 26.0 - 44.5 PbNbg2Zn3 / 303 1.9 - 18.6 BNB ^{P 2 /} 3mg ^{1/3 O} ₃ 2.5 - 21.8

Mentioned ^and substance mfóe ^Comprise I ^to the MO ^difik AČN YSL ^{i K i s} Cn alkyl from 3.6 to 3.9 mol. % Mn0 ₂ , resp. 0.83-0.86 mol. % CoO.

System 2

PbT10 ₃ 35,0 · - 42.5 PbZrOj 27,0 - 39.3 PbNbg / jZn1 / 3O3 2 - 17.8 PbNbg / ^ Co ^ / тру 2.9 - 26.5

(2)

To this substance, 3.5-3.7 moles are additionally added as modifying oxygen. % MnOg, resp. 2.03 mol. % FegOj ·

System 3

PbTiO ₃

PbZrOj ^PbNb 2 / ^3Me 1/3 ^O 3

PbNbg4Ce1 / 3 ° 3

35.0 - 45.0

- 42,55

2.4 - 21.6

2.8 - 27.6 (3)

This substance may also contain 1.9-3.0 moles as modifying oxygen. % 'MhOg.

System 4

PbTi0 ₃

PbZr0 ₃

PbNbg / ^ Zni / ^

PbN ^ g ^ ^ ^ ^ ^ 3/10 ^

System 5

PbTiO,

35.0 - 47.5

36.22 - 44.94

1.73 - 15.15

4.3 - 12.29

37.5 - 45.0 (4)

PbZrOj 34.7 - 44.6 ^PbHb 2/3 ^{Co _1/3} ° 3 3.5 - 21,4 (5) PbNb _J g _/ lfci ₁ / 3З3 4.3 - 10.5 System 6 PbTiOj 30.0 - 42,5 PbZrOj 23.1 - 44.3 (6) PbN ^{b2 / 3MgI} 8.3 - 22,7 ^{PWNb clay} 2/3 1/3 3 ° 4.3 - 29,4

Said substance may contain 0.76-3.8 mol ·% MnOg as modifying oxide.

System 7

PbTiO ₃ 30.0 - 45.0 PbZrO ₃ 25.4 - 47.6 (7) ^Pb N ^{b2 / 3} »i ^{_1/3 0} · 3 2.3 - 22.7 ^PbNb 2/3 ^Co 1/3 4.1 - 29.4

1.9-3.8 moles can be added to the substances as modifying oxygen. % MnOg.

System 8

PbTi0 ₃ 32.5 - 42,5 PbZr0 ₃ 32.8 - 42.8 (8) ^pbW 1/2 ^Zn 1/2 ° 3 6.1 - 17,8 Pb ^ bg (^ Zni) 3O3 5.7 - 15,0

0.76-1.9 moles can be added as modifying oxide. % MnOg.

System 9

PbTiOj

PbZr0j ^PbW1 / 2 ^Zn1 / 2 ° 3 PbNbgy ₃ Co ^ / 3Ο3

32.5 - 45.0

30.0 - 46.4

6.1 - 16.2

8.0 - 21.8 (9)

Modifying oxygen 0.77-3.8 moles can be additionally added to this material. % MnOg.

System 10

PbTiO3

PbZrO3 ^PbW 1/2 ^Mg 1/2 ° 3

Pblbbg / zZa ^ / 3О3

32.5 - 45.0

33.4 - 42.5

6.1 - 15.0

5.4 - 15.0

Suitably 0.76-3.8 moles are added as modifying oxygen. % MnOg.

(10)

197 406

System 11 PbTiOj 35.0 - 45.0 PbZrOj 30.6 - 44.5 ^PbW 1/2 ^Mg 1/2 ° 3 6.1 - 14.0 Italy (11) PbNbg / jCo2 / jOj 6.9 - 17.2

System 12 PbTiOj 35.0 - 45.0 PbZrOj 32.3 - 44.6 ^{PbW1 / 2} "gl ^{/ 2} ° ³ 6.1 - 16.2 (12) ^ 2 ^ / 3¾ 4.1 - H, 7 As mod ^and f and ^{also N NU IIc} with ^{alkyl Cart l} of n additionally add 0.76-1 1.9 mol ·% lbiO

System 13

PbTiOj 35.0 - 52,5 PbZr-j 33.58 - 44.2 ^{PbWi /} 2j ^ 1 ^ 4.48 - 11,37 PbNbgyjMn /// Oj - U1I9 System 14 PbTiOj 37.5 - 42,5 PbZrOj 32.8 - 39,4 ^{PbWi /} 2 ^M 2 ^{i /} 2 ^{O3 6.4} - 16,2 ^PbW 1/2 ^Zn 1/2 ° 3 6.4 - 15,5 System 15 PbTi03 37.5 - 45,0 PbZrO3 34.7 - 44.9 ^PbWi / 2 ^{Hii / 2} ° ^{3 4,} 3 - H, 4 PbNb2y3Zn // 303 5.7 - 14,4 ^D Uve ene ^{and beginnings} and can contain as modifier System 16 PbTi03 37.5 - 4 ^^, 5 PbZrO3 30.0 - 42.0 1.5 - 13-, 5 2.3 - 22,0 As the modifier oxide only e ^ ^Prior el.ně ¹

(13) (14) (15) oxygen additional 0.76-1.9 mol. % MnOg.

(16)

1.76-3.8 mol. % IbiOg.

System 17

PbTiOj

PbZrOj ^pbw 1.2 ^Ni 1.2 ^O 3 Pb bg ^ / ^ oo / 3О3

35.0 - 42.5

22.9 - 45.6

5.32 - 14.1

3.6 - 21.8 (17)

System 18

PbTiO ₃

PbZrO ^

Pb «, _{/ 2} » 1, _{/ 2} O ₃

PbNb _2/3 Mn ^ / 3θ3

37.5 - 45.0

36.8 - 45.3

5.12 - 13.54

4.48 - 11.37 (18)

System 19

PbTiOj

PbZrO ^ ^PhNb 2/3 ^H1 / 3 ° 3 PbWi _{/ 2} Nii / ₂ ° 3

32.5 - 45.0

38.4 - 42.5

4.1 - 28.4

5.8 - 13.6 (19)

Said substance may contain 0.76-1.9 mol% MnOg as modifying oxygen

System 20 PbTiOj 37.5 - 45.0 PbZrOj 32.5 - 42.0 øWW _1/2 Mg _1/2 0 ₃ 6.7 - 16.2 tbwl / 2 * il / 2 ° 3 5.1 - 13.6 System 21 PbTÍO ₃ 35.0 - 45.0 PbZrO ₃ 32.2 - 44.7 PbW _1/2 Co _1/2 0 ₃ 4.1 10.0 PbNbg ^ Co ^ 8.1 - 21.8 System 22 PbTiO ₃ 37.5 - 45.0 PbZrO ₃ 36.2 - 42.8 _Γ ™ _{ι / 2} 1Ιβ, / ₂ 0 ₃ 6.1 - 16.0 ^pbW 1/2 ^{Co 1/2/2} ° 3 4.3 12.8 System 23 PbTiO ₃ 37.5 45.0 PbZrO ₃ 35.7 - 43.9 ^ 1/2 ^ 1 / 2¾ 4.1 * 11.0 ^rbW 1/2 ^{Co 1/2/2} ° 3 5.4 - 13.0 System 24 PbT10 ₃ 30.0 - 45.0 PbZrO ₃ 25.0 - 47.6 ^PbW 1/2 ^Zn 1/2 ° 3 1.5 - 28.4 PBIN> 2 / jMgi / ₃ 0j 2.3 - 29.4

(21) (22) (23)

197

406

System 25 PbTiO ₃ 30.0 - 45.0 PbZrOj 25.0 47.6 PbW _1/2 Co _1/2 0 ₃ 1.5 28.4 Italy (25) PbNb _2/3 Zn ^ / 3θ3 2.3 - 29.4 System 26 PbTiO ₃ 30.0 - 45.0 PbZrO ₃ 25.0 - 47.6 ™ _1/2 ^W , / 2 ° ₃ 1.5 - 28.4 Italy (26) гьт _2/3 ш, _л о ₃ 2.3 - 29.4 System 27 PbTiO ₃ 30.0 - 45.0 PbZrO ₃ 25.0 - 47.6 РЬНЪ2 / з ^ * Ц / 3θ3 1.5 - 28.4 Italy (27) PbW _1/2 Co _1/2 0 ₃ 2.3 - 29.4 System 28 PbT10 ₃ 30.0 - 45.0 PbZrO ₃ 25.0 - 47.6 (28) ^р » ^1/1 °« 1 / г ° з 1.5 - 28.4 ΓΜ _»2/3» ^ / ₃ <^ 2.3 • 29.4 System 29 PbTiO ₃ 37.5 - 42.5 PbZrO ₃ 40.5 - 37.26 PbW _1/2 Ni _{/ 2} ° ₃ 5.34 - 5.82 (29) PW _1/2 Zn _1/2 0 ₃ 14.9 - 16.18 System 30 PbTiO ₃ 37.5 - 45.0 PbZrO ₃ 36.85 - 46.69 ^PbI 1/2 ^0o 1/2 ° 3 4.12 - 10.94 (30) PbNbgy ₃ MH + / ₂ 0 ₃ 4.30 - 10.92 System 31 PbTiO ₃ 37.5 - 45.0 PbZrO ₃ 36.25 - 42.42 Pb * 1/2 ^Z »1/2 ⁰ 3 6.1 - 16.38 (31) Pblíb _2/3 Mn ^ _{/ 3} O ₃ 4.68 - 11.37

System 32 PbTiO ₃ 35,0 - 42.5 PbZrOj 38,29 - 43.29 ^PbW 1/2 ^Zn 1/2 ⁰ 3 14,9 - 16.83 (32) ^PbW 1/2 ^Co 1/2 ⁰ 3 4,31 - 4.88 System 33 PbTiO ₃ 35,0 - 42.5 PbZrOj 28,18 - 35.82 United Kingdom (33) ^Pb * V ^ 2 ^Mg 1/2 ⁰ 3 12,9 - 15.54 (nb ^{) 2 /} 3M ^{gi / 3} 03 8.28 - 18.56

Most of these systems have high piezoelectric parameters ·

Piezokeramioké compounds according to the invention can be obtained with different combinations of values which are required in various fields of use · can for example be obtained highly conducting substance with a high portion ^to tr ^{i c} ou constant £ 33 »in ^{yšší h} o ^d no ^T ou electro ^ ch ^ CKE in ^those wasps ^di (Kp) and in the ^y SSIM piezoelectric modulus d ^ which is used in audio engineering, the seismograph and other occasions where the piezoelectric materials require a high piezoelectric properties ·

Substances according to the invention were also obtained with low dielectric loss values (tg <5) in weak fields (E = 10 to 30 v / cm) and strong fields (E = qv / cm) and in higher quality (Kp ad ^). substances can be used in hydroacoustic equipment.

Have also been developed látky.podle invention with a low dielectric value at a relatively higher value · electromechanical conductivity of such substances are used in ultrasound of the ^{p ZD} ovacíc ^h under ^RI zen ^Ch · Among j ^by unique ^and sku ^ nand materials ^{for Star} ter exhibit ^{also learning} nky ^p ccording to the ^invention can point to the e factor greater mechanical strength and a sufficient value of the frequency stability · such substances are used in filtration systems · Next, a description is given effect, having all of the system according to the invention substances ·

Table 2 shows the parameters of the best compositions of these highly efficient systems.

TABLE 2

System serial number Composition, mol ·% Electrophysical parameters PbTiO ₃ PbZr0 ₃ ^Β 4 λ ⁰ 3 ^p ' ^{1 0} c ^bI 1 ° 3 t 33 ^k p d ^ · 10 ⁶ CGSE 1 42.5 40.7 PbNb2 / Zn ^ _3/3 O ₃ 4.3 ^{PbNb2 /} 3M ^g1 / 30 ₃ 12.5 2260 0.67 6.6 ^^ 2/3 ^ 1/3 ^ 3 РЫП ^^ Со ^ / 3/3 3 42.50 42.55 7.18 7.77 2210 0.67 6.03 ^{pbNb2 /} ₃ Mg ^ / 3О3 ^{HER PbNb} 2.3 1/3 3 ° 6 42.50 39.16 8.29 10,05 3130 0,677 7.8 ^PbKb 2y3 ^Hi 1/3 ° 3 PbNb2 / ₃ 0o1 / i0 ₃ 7 35,00 28.34 27.30 9.36 2699 0,656 6.44 ^PbW 1/2 ^For 1/2 ⁰ 3 PblTbg ^ Zn ^ ^{/ 3} θ ³ 8 40.00 39.48 6.66 13.86 2655 0,658 6.72

197 40В

10 40.00 39.48 Pbw _1/2 Mg _1/2 o ₃ 6.66 PbNb ₂ y ₃ 2n ₁ ^ ³ θ ³ 13.86 ! 2762 0,703 7.65 9 42.50 42.66 ^PbW 102 ^Zn 102 ° 3 6.38 PbLib2O ₃ Co3y30 ₃ 8, 46 2159 0.65 5.67 15 Dec 42.50 39.73 ^ 2 ^ / 2 ° ³ 4.48 ^ ЬШ> 2у ₃ 2п ^ ^ ³ θ ³ 13.29 2480 0,613 5.92 11 42.50 37.37 ^ 1/2 ³ ^ ² ½ 12.88 PbNbg ^ Co ^ ^ ³ θ ³ 7.25 2973 * 0,618 6.23 12 40.00 36.60 Pb _{Wl /} og _1/2 O3 13.10 1 ^{PbNb2O3Ni O3} 10.30 ° ³ 3166 0,652 7.33 14 40.00 37.80 ^ 1/2 ^ 1 ⁰² ° ³ 6.66 ^{PbW 1O2 Zn 1O2 0} 3 15.54 2634 0,675 7.06 16 40.00 35.40 9.84 ^3,132 ° ³³¹⁰ ^ 14.76 3860 0,722 9.38 17 40.00 34.26 ръ ^ ⁰² ^ ⁰²⁰³ 5.58 ^pb ° rb ^2o ₃ C ^o1O3 ° ³ 20.16 2730 0,645 6.42 19 Dec 35,00 31.65 PbNb20 ^з N / 10 ° ^{з з} 27.30 ^рь * ¹⁰² * ^{/ 102} ° ³ 6.05 4441 0.608 7.66 20 May 37.50 30.44 26.25 ^PbW 1 ^O2Ni1O2 ° ³ 5.81 2360 0,655 6.14 21 37.50 35,00 ^{PbW 1O2 Co 1O2 0} 3 9.62 PbNb ² O ³ Co ³ γ ³ 17.88 3368 0,622 ^6.65 22nd 42.50 38.29 ^ръ > / 02 ' ^/ / 02 ° 3 14.89 ^ 102 ^ 102 ⁰³ 4.32 2390 0.605 5.42 23 42.50 40.71 ^рь ^ ^1О2 ^ ^{// О20} 3 4.31 12.48 2387 0,633 5.84

Thus they exhibit the best systems of high efficiency systems

- 2159 - 4441 Kp 0.605 - 0.722 d ₃₁ - (5.42 - 9.38). 10 ⁶ , CGS - jodziotelc.

These substances can be used in acoustics, seismographs and in other cases where piezoelectric substances with maximum piezoelectric properties are required.

In systems containing cobalt, in addition to having high piezoelectric mechanism to the increased fourth ^{(Q 260-6 0} °).

For systems containing manganese, most systems have lower dielectric losses in the weak and strong field: tg (weak field) 0.2 - 1.0%; tg 8 (strong pol) at. E kV / crn)

1.0 to 3.4% and a high mechanical quality Q 400 - 2 500 at sufficiently high přezolllk ^t ri / cal / ^hr paramltrec ^{h What} is valuable ^e u ^ flow tzterýk the ^p ou ^fo is hy ^ ca ^ a ^^ The parameters of some compositions of these systems are given in Table 3 ·

£ 8

0h b- Φ

IA M- O what O XO CA b- CM b- AND «» 4 » • «» CA M IA LD IA

O O P O P T ~ ’Ф b- IA b- CA CA Ch iA CM in- in- IN" CM CM

b- Ф CM b * Ch b ~ M · LD M · CA IA LD LD iD LD "to 4k » "to SKK O O O O O

Ο ΙΛ O Ch r- * AND AND AND * r- »- cm CM CA

ME oo IA CA m · CM CM CA CA •to <k • • 4k O O O O O

o řW

W

H I

CA Ch O O CA CA > 4 X r- 1 00 Φ in 1 ch * Ch 'x ’Ф X CM CM

CA O CA Ch CA About CM Хч O CM> 4 04 CM. «К CA in- ^ 4 r * л $ bcm «K b 40 IA * ’Ф <- U o CA X «I co and C CM * x X £ вГ вГ δ fi

CM

P ch <* \

u> O O Μ- IA CA CA ΙΑ SKK * « "to M CM t- O M ’Ф CA M-

IA

SKK

CM

IA *

CM

IA £ * * «(.CM

VW

Φ ΙΛ

Ch

WHAT

197. 406

Some of the compounds of the invention (Table 4) have a low dielectric constant at a relatively high electromechanical coupling factor, allowing the use of ultrasound in ^p lines oždovac ^Ch ·

TABLE 4

System number Composition, mol ·% Bletrophysical parameters PbTiO3 PbZrO3 ^Pb L ^aBlI < ⁰ 3 ph-iii beers _o 43 Kp PbNb2 / 3Mni / ₃ O ₃ 13 42.50 36.86 19.14 1.5 434 0.509 ^PbW 1/2 ^Ni 1/2 ⁰ 3 i 1 ^PbNb 2/3 ^MW 1/3 ^O 3 18 40.0 43.5 5.58 10.92 500 0.518 ‘PbNb2 / з1Ь11 / з ° з 5 40.0 45.72 3.78 ¹⁰ , 5 510 0.532 1.2 ^{pbw Mg 1/20} 3 PWn> 2 / -jMnj / 3 ° 3 13 45,00 30.26 14.84 9.9 518 0.536 ^RBW 1 / ^{2Mg 1/20} 3 PbHbg / ^ Zn ^ / ^ Oj 10 42.50 46,00 5.75 5.75 845 0.610

Saxon systems listed in Table 5, ^{characterized} in caries ^l ^ me high mecha CBROM quality ^BC and ^p MLM high electromechanical coupling factor Kp ·

Some of these systems are listed in Table 5 ·

TABLE 5

^{Whose l} with the alimentary canal Composition, mol ·% Bletrophysical parameters · PbTiO3 PbZrO3 PbB ¹ _ ^(I0 CB-03 PbB1-CcB CCO3 Q Kp 4 35.0 40.95 PbNb _2/3 Zi ^ / 303 15,15 PbNb ₂ / 3Mn // 30 ₃ 8.9 2120 0.49 4 37.5 43.18 PbNb2 / 3Zn // 3О3 14.44 PbNb ₂ / 3M & 1/303 4.88 1910 0.52 5 42.5 38.58 PbNbg / ₃ C0H3O3 8.45 PbNb ₂ / 3Mn1 / 3O ₃ 10.47 2370 0.52

18 37.5 45.31 PbWi _{/ 2} Ni _V2 0 ₃ 5.82 11.37 2360 * 0.52 30 42.50 38.52 ^rbW _1/2 ^Co 1/2 1/2 9.1 9.88 2440 0.51

Some systems exhibit, at sufficiently high mechanical quality and electromechanical coupling factors, the stability of the resonance frequency fr in the temperature range from - 40 ° C to + 80 ° C (Table 6), allowing the use of these substances in filtration technology.

TABLES 6

number show- conditions Composition, mol. % Electrophysical parameters PbT10 ₃ PbZr0 ₃ PbB ^ B ¹ ^ Q Kp fr _t o - fr ₂₀ o _ fr ₂₀ o $ 13 52.5 33.58 øWW _1/2 Mg _1/2 0 ₃ 5.28 PbNb ₂ y ₃ Mn 2 y ₃ O ₃ 8.64 1150 0.33 <0.15 5 45.0 38.5 Kiss ₂ y ₃ Co ^ ^ ₃ θ ₃ 7.26 ^PbNb 2/3 ^Mn 1/3 ° 3 9.24 1300 0.44 <0.2 5 45.0 36.9 PbNb ₂ Y ₃ Co ^ © у ₃ 8.08 ₃ PbNb _2/3 Mn ^ / 3θ3 10.02 1480 0.43 0.2 4 47.5 38.48 PbNbg / jZn ^ ^ ₃ 0 ₃ 1.73 PbNbg / JMn4 / ₃ 0 ₃ 12.29 890 0.46 <± 0.2

The modification of the piezoceramic compound according to the invention makes it possible in some cases to obtain even more effective dielectric and piezoceramic indicators.

For example, the addition of 0.76-3 mol% MnOg, or 0.83-0.86 mol ·% OoO to some systems, greatly reduces weak and strong field dielectric losses, increases meohanic quality, allows systems with low dielectric losses to be obtained at relatively high piezoelectric parameters Kp & d1 and results in a combination of low electrical constant and relatively high electromechanical coupling factor, which is important for ultrasonic delay lines. are listed in Table 7 ·

The addition of 2.03 molar% PegO ^ allows to obtain a substance with low dielectric losses in both weak and strong fields at high dielectric and piezoelectric parameters (Table 8).

197 40В

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197 406

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197 408

TABLE 8

о 100 ALIGN! о сл о 48 IN 180 ь v> Η О 4> о ш 04 / 4> г- О сл σ> г · ΙΛ in • Мн ▼ * со * С (Лс5 ф От » • к • к «К хг ш м · эд МВ СЛ мв д W СМ ь- 4I 48 40 1Л ш .Μ  · » «К • к «К Ч о о о о Й й 4 » 518 со ОЧ t— м · > 1 «К «К «К • к Ф СМ Г 00 г · 40 й * * <Э ьо 4 г- см 4 » i я Д (0 1L 48 ча со СО -cfr рн ^ ф о • к «К « £ »in fi л г · о о О сл о о о о ЕН сл ча 04 / СЛ см сл см со 04 / е— см т · е— й О 1 4 » сл СЛ сл СЛ 13 1 о см ф о «К см 1 о СМ ф О • к см йм эд эд СЛ О СЛ СЛ О О СЛ СЛ гО τ- Ο ΙΛ о о О 04 / НЙ (Л • к с СЛ «К 8 \ СЛ СМ Н 1 СМ см Η V- J * РЬВ and сл сл • СЛ о о no о СЛ СЛ о -ч. а и * V 0 СМ т- СО «К я ЬЗ 4к 8 ьЗ • к 8 м X СЛ со СЛ t— А * 4, г · ч. т ^- 3 1 см СМ * 8 § in § й £ н з Lq СО эд СЛ о Г СЛ й «К 8 ' 8 IS3 о 04 / £ 4fr СЛ сл о СО О й «К СО с • к О 8 £ СЛ О, в h А 1 1> ®Ρ (ΰ см 8 М 0 4 * ю »m

197 406

The piezo-ceramic according to the invention is produced as follows:

Starting materials> such as oxides, carbonates and metal hydroxides are taken, for example:

PbOOj Ti0 ₂ Zr0 ₂ кь ₂ о ₅ wo ₃

ZnO

MnCO ₃ MnOg

Co (OH) ₂

Pe ₂ ° ₃

Mg (OH) ₂

The starting materials of this composition are blended in a ball mill for 10 hours wet. The synthesis is then carried out according to the usual PbO ceramic technology. Synthesis conditions: temperature 750-850 ° C, duration of the first synthesis 4 hours, duration of the second synthesis 10 hours ·

To obtain quality piezoceramics, the synthesized substance is sintered using hot pressing · Hot pressing conditions: temperature 1100-1250 ° C, pressure 20 MPa, holding time 40 min ·

After sintering the samples are sanded ·

For the polarization required for ceramics to have piezoelectric properties and for the measurement of electrophysical parameters, electrodes must be formed on the specimens. · To this end, the specimens are coated with a silver paste and maintained at 800 ° C.

The polarization is carried out in a silicone oil, which is an organosilicic liquid, at a temperature of from 90 to 185 ° C for a period of from 25 to 45 minutes, in an electric field of 16.0 to 50.0 kV / cm ·

Sample testing is performed 24 hours after polarization.

In order to better understand the invention, the following examples of the preparation of the piezoceramic agent according to the invention are given

Example 1

Production of piezoceramics, which contains in molar percentages:

PbTiO ₃ - 42.5 PbNb _2/3 Zn _1/3 0 ₃ - 4.3

PbZrO ₃ - 40.7 PbMb _2/3 Mg _1/3 0 ₃ - 12.5

Disposal of the substance, in accordance with the above composition as oxides, carbonates and metal hydroxides PbCO ₃ , TiO ₂ , ZrO ₂ , HbgOg · Mg (OH) ₂ is taken and wet mixed in a ball mill for 10 hours. substance synthesis · Synthesis is carried out according to common ceramic technology, in a protective atmosphere PbO ·

Synthesis conditions: temperature 850 ° C, duration of first synthesis 4 hours, second synthesis 10 hours · Synthesized substance is sintered using hot pressing · Hot pressing conditions: temperature 1200 ° C, pressure 20 MPa, holding time 40 min · Polarization is performed in silicone oil at 100 ° C for 30 minutes in el. field of 25.0 kV / om.

The electrical parameters of the substance of the composition have the following values:

2260 d ₃₁

Kp - 0.67, Q - 75

10 ⁶ CaSB units tg (in weak el · field) 1.5% ·

Example 2

Production of a piezoceramics under the conditions as in Example 1, which contains in mole%:

PbTiO ₃

PbZrO ₃

32.5

32.4

PbHbg / zZn 15.45

PbNb _2/3 Mg _1/3 0 ₃ - 19.65

197 40V ^{and £ £} ₃ 2500, d. ^ = ^5, 97 · ¹⁰ “$ CGiSB - one ^ k

Kp 0,6, tg Ó (in weak field) in 1,6%, Q «83.

Example 3

Production of piezoceramic substance containing molar%,

PbT10 ₃ - 40.0 PbmigjjZiuty.jO. ³ - 5,0

PbZrOj - 48.6 Pblbj ₂ / 31®i / ³ 0 ₃ - 6.4 as the modifying oxide and contains 3.7 mol. % MnOg.

The following raw materials were chosen:

°° ^Pb ₃ TiCg, ZrO ^{g g} O ^g Nb, Zn ^ ^M g ^{(OH) g, g} Mn °.

These components selected by said assembly is mixed in a wet ball mill for 10 hours. It is then twice · Synthesis of Synthesis was carried out according ^to conventional eramické technol ^{g s} IE in protective atmos ^FER e PbO. Cond ^{s y} s ^y nk ntézy: temperature 850 ° C, duration of the synthesis of the first four hours ,. duration of the second synthesis was 10 hours. Sintering seprovede pressing TE ^beta la from Wohto ^p o ^d misses ^{to: p t} e lota 1200 ° C, ^t varnish ^{20 MPa,} the time ^from an otter 4 ^{0 inches}

Polarization ^P Roveda silicone oil ^P s ^{of 100} ° C for 3 ⁰ min. in el. field of 30 kV / cm. Electrophysical parameters of this system have the following values:

£ ® ³ . D ^ 405 - ¹ 52nd 10 “ ⁶ CGSE - ^ dnotek, Kp« 0.478,

Q 5 ^{218 tg <(L} in meters and ^BE EL. ^P ol ⁱ⁾ 0.3% ^P s E 2 kV / cm, T ^g dT ^«1.6%.

Example 4

Preparation of a piezoceramic agent under the same conditions as in Example 3, which contained in% by weight:

PbTiO ₃ - 42.5 PbNb _{2 /} 3Zn1 _{/ 3} 0 ₃ - 4.3

PbZrOj - 40.7 PbJb> 2/3 ^{1 |} g1 / 303 - 12.5 and contains 0.83 mol% Co0 as the modifying oxide. The additive is added in the form of Co (OH) 2 during mixing of all starting components.

Electrophysical parameters have the following values:

^£ 3 ^3-2240 d ^31-6, 75 · 10 "$ CGSE ^{- j} ednot ^Kp · ^e k 0.69 ^{g ot} t ⁽ⁱⁿ a weak electric. ^{P oli)« 0,} $ 5, ^P s E - 2kV / ^{cm g} t g ^T - Q 9.2 ^- 222 _in

The following production process examples (from No. 5 to No. 75) are summarized in the table

9, in which the relative ratios of the main components, concentration, are given. added modifiers, conditions for synthesis, sintering and polarization, as well as values of electrophysical parameters.

TABLE 9

1β7 40β

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187 408

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197 406

15 Dec ф Р Ьча £ ф 574 оо ф см Ь- см ф Φ 1Л 40 СО г · 40 ф г * » • » • «К «К сл Ь- г- ф сл 40 34 СМ ь · ш 40 СЛ СМ Ф C- 40 1X4 г- ш 40 40 LC4 40 40 • «К м SKK «К О о О О о О СМ (О 1 1 СО 1 г- г · * «К г— 00 СО я— ь · Р 00 IN- СМ СО ф LC4 04 / г · ш «» • к • к • к «К О Г " № О о я— о о 04 / о о о 04 / IN- о Р СЛ ф сл 04 / ш т— с * - 00 40 IN сл СЛ г- СМ О о 1Г4 о о О О ш о 04 / 8 ф ф сл 8 о гл Ф ф см СЛ 8 ▼ - г · Г о СЛ О о сл О о сл о со 8 04 / О 8 40 о со о 8 г ^- СМ см я— см см см см Г я— О о О о О о t— 8 LT4 Я— 8 LC4 г · ш я— 8 СО + СО and 00 + ф ф ф СМ 04 / 40 1 1 1 о • к 1 1 Й г- сл сл сл сл СЛ сл о о О о О о СЛ сл СЛ ГЛ СЛ сл X, > ч г- 04 / Г IN" I4 г · я— см г- 40 1 Ф н сл • н О • н СЛ О 40 о СЛ ц> «К Ф К % «К О 4к ť- О СЛ • к сл о сл • 04 / СМ IN" см см СМ см см СМ см gí> £ £ £ к I д Й * К WITH й й й £ £ й сл сл сл СЛ СЛ СЛ о о о О О о Г ' сл сл сл сл сл > ч > ч τ- г- я— in- AND т · Ф ’ Ο О ГЛ £ • к * 40 СЛ * 04 СМ 40 сл • к 40 о «К ^ Л сл «К * ч 04 / 04 / СО 04 / X. о ь · см £ IN- см £ СМ £ см хз 2 см £ я— СМ £ см й й й Й й 04 / ф 40 Ф см ф СЛ СМ СЛ г- СЛ 00 сл • • к • к • к «К «К СЛ СО 04 / СО СЛ 00 СЛ см СЛ см ф см I4 о Ш о 1А о см «К «К «К «К • к см LT4 СМ 1X4 см ш ф СЛ ф СЛ ф сл г · 1Г4 40 г- СО 04 / о г- IN· г · г- г · см

197 406

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197 40В

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197 40b

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197 406

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197 406

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197 406

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197 406

Claims (17)

BACKGROUND OF THE INVENTION 1 · Piezo-ceramics containing lead titanate PbTiOj, lead zirconate PbZrOj and, as a third component, lead metallobonate PbNbg / jMe ^ / з ° з or lead metal tungstate PbW-ygMe ^ gO ^, in which Me is selected from bivalent zinc , cobalt, manganese and nickel, characterized in that the fourth component comprises lead metal borate or lead metal tungstate of the above formulas, in which Me is a bivalent metal selected from the group of zinc, magnesium, cobalt, manganese and nickel, and the fourth component of the lead metallobioate of the above formula and the metal Me in the third component of nickel is Me metal in the fourth component of magnesium or cobalt, and if the third and fourth component is lead metallobioate of the above formula and the metal Me in the third component of magnesium in the fourth folder zinc, cobalt or nickel, said components being contained in the following molar: nich prooenteoh: lead titanate 30.0 to 52.5 lead zirconate 25.0 to 47.6 the third component 1.5 to 26.4 fourth component 2.3 to 29.4. A piezo-ceramics according to claim 1, characterized in that it contains components in molar prooents: lead titanate 32.5 to 45.0 lead zirconate 26.0 to 44.5 lead zinconiobate 1.9 to 18.6 lead magnesium borate 2.5 to 21.8. 3. Piezoceramic agent according to claim 2, characterized in that it contains from 3.6 to 3.9 mol% of manganese dioxide or from 0.63 to 0.66 mol% of cobalt oxide as modifying oxides. 4. A piezo-ceramics according to claim 1, characterized in that it contains a molar prooenteoht lead titanate 35.0 to 42.5 lead zirconate 27.0 to 39.3 lead zinconiobate 2,0 to 17.8 lead cobalt 2.9 to 26.5. 5. The piezo-ceramics according to claim 4, characterized in that it contains from 3.5 to 3.7 mol% of manganese dioxide or 2.03 mol% of iron oxide as modifying oxides. 6. The piezo-ceramics according to claim 1, characterized in that it contains in molar proo lead titanate 35.0 to 45.0 lead zirconate 25.0 to 42.55 lead magnesium borate 2.4 to 21.6 Lead cobalt 2.8 to 27.6. 7. The piezo-ceramics according to claim 6, characterized in that it contains from 1.9 to 3.8 mol% of manganese dioxide as modifying oxide. 197 406 8. Piezoceramic substance according to claim 1, characterized in that it contains in molar percentages: lead titanate 35.0 to 47.5 lead zirconate 36.22 to 44.94 lead zinconiobate . 1.73 to 15.15 lead manganese 4.3 to 12.29. Piezoceranic substance according to 9. point 1, exacerbated by the fact that they contained them in percentages of percentages: lead titanate 37.5 to 45.0 lead zirconate 34.7 az 44.6 Lead cobalt 3.5 to 21.4 lead manganese 4.3 to 10.5. 10. The piezo-cereal substance according to claim 1, characterized in that it contains in molar percentages: lead titanate 30.0 az 42.5 lead zirconate 23.1 to 44.3 lead magnesium borate 8.3 to 22.7 Lead nickel 4.3 to 29.4. 11. The piezo ceramic according to claim 10, characterized in that it contains 0.76 to 3.8 mole percent of manganese dioxide as modifying oxides. 12. Piezoceramic substance according to claim 1, characterized in that it contains in molar percentages: lead titanate 30.0 az 45.0 lead zirconate 25,4 * to 47.6 Lead nickel 2.3 at to 22.7 Lead cobalt 4.1 to 29.4. 13. A piezoceramic substance according to claim 12, characterized in that as modifying oxide it contains 1.9 to 3.8 mole percent of manganese dioxide. 14. Piezoceramic substance according to claim 1, characterized in that it contains in molar percentages: lead titanate 32.5 to 42.5 lead zirconate 32.8 to 42.8 lead zinc tungstate 6.1 az 17.8 Lead zinc borate 5.7 az 15.0. 15. The piezoceramic substance of claim 14, wherein the modifying oxide comprises from about 0.76 to about 1.9 mole percent of manganese dioxide. 16. Piezoceramic substance according to claim 1, characterized in that it contains in molar percentages: lead titanate 32.5 to 45.0 lead zirconate 30.0 to 45.4 lead zinc tungstate 6.1 to 16.2 Lead cobalt 8.0 az 21.8. 17. The piezo ceramic according to claim 16, wherein the modifying oxide comprises from about 0.77 to about 3.8 mole percent manganese dioxide. 406 Piezoceramic substance according to claim 1, characterized in that it contains in molar percentages: lead titanate 32.5 to 45.0 lead zirconate 33.4 to 42.8 niagnesiuwolřraman lead 6.1 to 15.0 Lead zinc borate 5.4 to 15.0. Piezoceramic substance according to Claim 18, characterized in that it contains from 0.76 to 3.8 mol% of manganese dioxide as modifying oxide. Piezoceramic substance according to claim 1, characterized in that it contains in molar percentages: lead titanate 35.0 V az 45.0 lead zirconate 30.6 to 44.5 lead magnesium tungstate 6.1 to 14.0 Lead cobalt 6.9 to 17.2. Piezoceramic substance according to claim 1, characterized in that it contains in molar percentages: lead titanate 35.0 to 45.0 lead zirconate 32.3 to 44.6 lead magnesium tungstate 6.1 v az 16.2 Lead nickel 4.1 in az 11.7. The piezo-ceramic according to claim 21, characterized in that it contains 0.76 to 1.9 mole percent of manganese dioxide as modifying oxide. Piezoceramic substance by percentage point: characterized in that it contains in molar lead titanate 35.0 to 52.5 lead zirconate 33.58 to 44.2 lead magnesium tungstate 4.48 to 11.37 lead manganese 6.1 to 16.19. Piezoceramic substance according to item 1 percent: lead titanate lead zirconate lead magnesium tungstate lead zinc tungstate Piezoceramic substance according to item 1, percentage: characterized in that it contains in molar 37.5 to 42.5 32.8 to 39.4 6.4 to 16.2 6.4 to 15.5. characterized in that it contains in molar lead titanate 37.5 to 45.0 lead zirconate 34.7 to 44.9 lead nickel tungstate 4.3 to 11.4 lead zinconiobate 5.7 to 14.4. The piezoceramic substance according to claim 25, characterized in that it contains from 0.76 to 1.9 molar prooents of manganese dioxide as modifying oxide. Piezoceramic substance according to claim 1, characterized in that it contains in molar percentages: 197 406 lead titanate 37.5 to 42.5 lead zirconate 30.0 to 42.0 lead nickel tungstate 1.5 to 13.5 lead magnesium borate 2.3 to 22,0 · 28 · 29 · 30. 31 · 32 · 33 · 34 · 35 · Piezoceramic substance according to claim 27, characterized in that it contains from 0.76 to 3.0 mol% of manganese dioxide as modifying oxide. Piezoceramic substance according to claim 1, characterized in that it contains in mole percent: lead titanate 35.0 to 42.5 lead zirconate 22.9 to 45.6 lead nickel tungstate 5.32 to 14.1 Lead cobalt 3.6 to 21.8 · Piezoceramic substance according to claim 1, characterized in that it contains in molar percentages: lead titanate 37.5 to 45.0 lead zirconate 36.8 to 45.3 lead nickel tungstate 5.12 to 13.54 lead manganese 4.48 at to 11,37 · Piezoceramic substance according to claim 1, characterized in that it contains in molar percentages: lead titanate 32.5 to 45.0 lead zirconate 38.4 to 42.5 Lead nickel 4 ^, 1 to 28.4 lead nickel tungstate 5.8 to 13,6 · Piezoceramic substance according to claim 31, characterized in that it contains from 0.76 to 1.9 mol% of manganese dioxide as modifying oxide. Piezoceramic Substance according to Item 1, Percent: characterized in that it contains in molar lead titanate 37.5 to 45.0 lead zirconate 32.5 to 42.0 lead magnesium chloride ^6, 7 to 16.2 lead nickel tungstate 5.1 to 13,6 · Piezocerami substance according to item 1, percentage: characterized in that it contains in molar lead titanate 35.0 to 45.0 lead zirconate 32.2 to 44.7 kobaltwolf: ^^ jan lead 4.1 to 10.0 Lead cobalt 8.1 to 21.8 · Piezoceramic substance by percentage point: characterized in that it contains in molar lead titanate 37.5 to 45.0 lead zirconate 36.2 to 42.8 Bagnesiumwolfra ^^ leaded 6.1 to 16.0 kobaltwolfra ^ m leaded 4.3 to 12,8, 197 Зб. 37. 38. 39. 40. 41. 42. 409 Piezoceramic substance according to point 1, characterized by by that contains in molar percentages: lead titanate 37.5 to 45.0 lead zirconate 35,7 to 43.9 lead nickel tungstate 4.1 to 11.0 lead cobalt tungstate 5,4 to 13.0. Piezoceramic substance according to point 1, indicate ící se team. that contains in molar percentages: lead titanate 30.0 to 45.0 lead zirconate 25.0 to 47.6 lead zinc tungstate 1,5 to 28.4 lead magnesium borate 2,3 to 29.4. Piezoceramic substance according to point 1, characterized by by that contains in molar percentages: lead titanate 30.0 to 45.0 lead zirconate 25.0 to 47.6 lead cobalt tungstate 1,5 to 28.4 lead zinconiobate 2,3 to 29.4. Piezo - ceramics according to point 1, characterized by by that contains in molar percenteoh: lead titanate 30.0 to 45.0 lead zirconate 25.0 to 47.6 lead zinc tungstate 1,5 to 28.4 Lead nickel 2,3 to 29.4. Piezoceramic substance according to point 1, indicate ící se by that contains in molar percentages: lead titanate 30.0 to 45.0 lead zirconate 25.0 to 47.6 Lead nickel 1,5 to 28.4 lead cobalt tungstate 2,3 to 29.4. Piezoceramic substance according to point 1, characterized by by that contains in molar prooentech: lead titanate 30.0 to 45.0 lead zirconate 25.0 to 47.6 lead cobalt tungstate 1,5 to 28.4 lead magnesium borate 2,3 to 29.4. Piezoceramic substance according to point 1, characterized by by that contains in molar percentages: lead titanate 37.5 to 42.5 lead zirconate 40,5 až 37.26 lead nickel tungstate 5.34 to 5.82 lead zinc tungstate 14,9 to 16.18. > Piezoceramic substance according to point 1, characterized by by that contains in molar percentages: lead titanate 37.5 to 45.0 43. 197 406 36.85 to 46.69 4.12 to 10.94 4.30 to 10.92. 44. lead zirconate lead cobalt tungstate lead manganese lead Piezoceramic substance according to claim 1, characterized in that it contains in molar prooenthal: lead titanate 37.5 to 45.0 lead zirconate 36.25 to 42.42 lead zinc tungstate 6.1 to 16.38 lead manganese 4.68 to 11.37. 45. Piezoceramic substance according to claim 1, characterized in that it contains in molar percentages: lead titanate 35.0 V az 42.5 lead zirconate 38.29 to 43.29 lead zinc tungstate 14.9 to 16.83 lead cobalt tungstate 4.31 to 4.88. 46 · Piezocerami substance according to claim 1, characterized in that it contains in molar percentages: lead titanate 35.0 to 42.5 lead zirconate 28.18 to 35.82 lead magnesium tungstate 12.9 to 15.54 lead magnesium borate 6.28 to 18.56.