CN1810717A - Ytterbium oxide and yttrium oxide co-stabilized zirconia ceramic material and its prepn process - Google Patents
Ytterbium oxide and yttrium oxide co-stabilized zirconia ceramic material and its prepn process Download PDFInfo
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- CN1810717A CN1810717A CN 200610024361 CN200610024361A CN1810717A CN 1810717 A CN1810717 A CN 1810717A CN 200610024361 CN200610024361 CN 200610024361 CN 200610024361 A CN200610024361 A CN 200610024361A CN 1810717 A CN1810717 A CN 1810717A
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- 229910002076 stabilized zirconia Inorganic materials 0.000 title claims abstract description 12
- 229910010293 ceramic material Inorganic materials 0.000 title claims description 20
- 238000000034 method Methods 0.000 title claims description 19
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 title abstract description 29
- 229910003454 ytterbium oxide Inorganic materials 0.000 title abstract description 23
- 229940075624 ytterbium oxide Drugs 0.000 title abstract description 21
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 title abstract description 15
- 230000008569 process Effects 0.000 title description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000000843 powder Substances 0.000 claims abstract description 32
- 239000003381 stabilizer Substances 0.000 claims abstract description 30
- 238000002360 preparation method Methods 0.000 claims abstract description 23
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims abstract description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 13
- 238000013461 design Methods 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- 238000001272 pressureless sintering Methods 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 239000011858 nanopowder Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims 10
- 239000002243 precursor Substances 0.000 claims 6
- 238000005538 encapsulation Methods 0.000 claims 3
- 238000009694 cold isostatic pressing Methods 0.000 claims 2
- 239000002245 particle Substances 0.000 claims 2
- 238000005979 thermal decomposition reaction Methods 0.000 claims 2
- 239000000919 ceramic Substances 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000010987 cubic zirconia Substances 0.000 abstract description 2
- 229910002082 tetragonal zirconia polycrystal Inorganic materials 0.000 description 35
- 229910002078 fully stabilized zirconia Inorganic materials 0.000 description 25
- 239000000463 material Substances 0.000 description 10
- 238000005245 sintering Methods 0.000 description 9
- 229910001928 zirconium oxide Inorganic materials 0.000 description 7
- 229910052727 yttrium Inorganic materials 0.000 description 6
- 229910052769 Ytterbium Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 238000005056 compaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000011224 oxide ceramic Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910007746 Zr—O Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
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Abstract
本发明涉及一种氧化镱和氧化钇共稳定氧化锆陶瓷及制备方法，其特征在于：同时使用氧化镱和氧化钇两种氧化物作为稳定剂，采用包裹技术制备两种稳定剂共同包裹的纳米氧化锆粉体，所得粉体于空气中无压烧结，在低稳定剂含量下分别获得四方氧化锆多晶(TZP)和全稳定立方氧化锆陶瓷(FSZ)。采用的原料是纯度(质量百分比)不小于99.9的氧化镱(Yb2O3)、氧化钇(Y2O3)和单斜氧化锆粉(平均晶粒尺寸小于100纳米)，最终获得的TZP陶瓷中氧化镱(Yb2O3)的摩尔百分比在1.0－2.0％范围内，氧化钇(Y2O3)的摩尔百分比在1.0－2.0％范围内；FSZ陶瓷中氧化镱(Yb2O3)的摩尔百分比在3.0－4.0％范围内，氧化钇(Y2O3)的摩尔百分比在1.0－2.0％范围内。
The invention relates to a co-stabilized zirconia ceramic made of ytterbium oxide and yttrium oxide and a preparation method thereof. Zirconia powder, the obtained powder is sintered in air without pressure, and tetragonal zirconia polycrystalline (TZP) and fully stable cubic zirconia ceramics (FSZ) are respectively obtained under low stabilizer content. The raw materials used are ytterbium oxide (Yb 2 O 3 ), yttrium oxide (Y 2 O 3 ) and monoclinic zirconia powder (average grain size less than 100 nanometers) with a purity (mass percentage) of not less than 99.9. The final TZP The molar percentage of ytterbium oxide (Yb 2 O 3 ) in ceramics is in the range of 1.0-2.0%, and the molar percentage of ytterbium oxide (Y 2 O 3 ) is in the range of 1.0-2.0%; ytterbium oxide (Yb 2 O 3 ) in FSZ ceramics ) in the range of 3.0-4.0% by mole, and the mole percentage of yttrium oxide (Y 2 O 3 ) in the range of 1.0-2.0%.
Description
Technical field
That the present invention relates to is ytterbium oxide and yttrium oxide co-stabilized tetragonal zirconia polycrystal (TZP) and fully stabilized zirconia pottery (FSZ) and preparation method.More precisely provide a kind of with ytterbium oxide (Yb
2O
3), yittrium oxide (Y
2O
3) and the monoclinic zirconia powder be raw material, adopt technique for packing to prepare powder, under low stabiliser content, reach densified acquisition by pressureless sintering and have the TZP pottery of good mechanical property and have fully stabilized zirconia pottery (FSZ) of electric property and preparation method thereof, belong to zirconia-based ceramics product and preparation method field.
Background technology
Zirconium white is a kind of multiduty stupalith, can be divided into tetragonal zirconia polycrystal pottery (TZP), partial stabilization zirconium oxide ceramic (PSZ) and fully stabilized zirconia pottery (FSZ) according to constitutional features.Wherein tetragonal zirconia polycrystal pottery and partial stabilization zirconium oxide ceramic have excellent mechanical property, have obtained important application in fields such as machinery, biology, medical science; The fully stabilized zirconia pottery has good electric property, exists wide application prospect at energy field.
Studies show that the phase transformation of four directions → monocline can take place in cooling procedure zirconia, this phase transition process is accompanied by the Volume Changes of 3-5%, can cause porcelain body seriously to ftracture, and therefore, the pure zirconia pottery can not be used.In order at room temperature to obtain stable four directions or cubic zirconia, usually adopt the mode of adding some metal oxide to avoid the phase transformation of four directions → monocline.These metal oxides and zirconia generate solid solution, stablize Tetragonal and Emission in Cubic.The most frequently used stabilizing agent is CaO, MgO, CeO
2, Y
2O
3Deng, wherein with Y
2O
3For the research of stabilizing agent the most extensive.The tetragonal zirconia polycrystal of stabilized with yttrium oxide (Y-TZP) pottery particularly adds 3mol%Y
2O
3The 3Y-TZP pottery, have good mechanical property.Yet, when the 3Y-TZP pottery was exposed in humidity or the thermal and hydric environment for a long time, the phase transformation that the monocline phase is arrived in spontaneous four directions mutually can take place, cause material property sharply to descend thus, even catastrophic failure, i.e. low temperature aging phenomenon take place.Research is found, the easiest generation in the 3Y-TZP pottery of low temperature aging phenomenon, Y in material
2O
3Content when increasing or reducing, this aging phenomenon all can be inhibited.But, reduce Y
2O
3Content usually can cause undergoing phase transition in the cooling procedure and can not obtain the TZP pottery; Increase Y
2O
3Content can affect its mechanical property to a certain extent.This shows, only use Y
2O
3As the TZP ceramic material of stabilizing agent, its mechanical performance has certain limitation.By in matrix, introducing the second stabilizing agent, can adjust the performance of Y-TZP pottery, can obtain to compare single Y in some situation
2O
3Stablize and have the more ZrO of superior function
2Material [1, M.M.R.Boutz, A.J.A.Winnubst, B.Van Langerak, et al, J.Mater.Sci.30 (1995) 1854.].
For the fully stabilized zirconia pottery, when adopting single oxide as stabilizing agent, usually need to add a large amount of stabilizing agents, and need higher sintering temperature and long heat treatment time could obtain Emission in Cubic.Even like this, the distribution of stabilizing agent in each crystal grain is still inhomogeneous, is segregated on the crystal boundary in a large number.With Y
2O
3Stable FSZ pottery is example, and the content of stabilizing agent is usually above 8.0mol%.There are some researches show, introduce the second stabilizing agent and can greatly promote its solid solution in zirconia crystal grain, make its distribution in each crystal grain be tending towards even.Therefore, by to the selection of another stabilizing agent and preparation technology's control, not only there is the possibility of optimizing the TZP ceramic material property, and exists the possibility that under low stabiliser content, obtains the fully stabilized zirconia pottery.
In addition because Yb
3+Ionic radius in all rare earth elements near the size of Zr-O octahedral voids, infer that thus Yb is to ZrO
2Has stronger stabilization.By in matrix, introducing Yb
2O
3, utilize the synergy of compound stabilizer, can reduce the consumption of stabilizing agent, under low stabiliser content, obtain tetragonal zirconia polycrystal and fully stabilized zirconia pottery, thereby optimize the performance of material.In addition, except that stabilizer type and components selection, the preparation technology of powder and performance thereof also have great influence to the final performance of sintered ceramic.Therefore, the inventor attempts selecting Yb
2O
3And Y
2O
3In the time of as stabilizing agent, utilize technique for packing to prepare Yb
2O
3And Y
2O
3The ZrO of common parcel
2Nano-powder obtains fine and close ZrO by pressureless sintering
2Ceramic material.
Summary of the invention
The object of the present invention is to provide by Yb
2O
3And Y
2O
3Be total to stable zirconia ceramics, that is comply with as co-stabilizer Yb
2O
3And Y
2O
3Amount and prepare TZP or FSZ zirconia ceramics.Obtain that a kind of stabiliser content is low, the ytterbium oxide of good mechanical properties and yttrium oxide co-stabilized tetragonal zirconia ceramics material (TZP) and fully stabilized zirconia ceramic material (FSZ).
The objective of the invention is to implement by following manner: be not less than 99.9% ytterbium oxide (Yb with purity (mass percent)
2O
3), yittrium oxide (Y
2O
3) and average grain size be initiation material less than the monoclinic zirconia powder of 100 nanometers, adopt the nm-class powder of zirconium oxide of the synthetic ytterbium oxide of technique for packing and the common parcel of yittrium oxide, under low stabiliser content, obtain fine and close ytterbium oxide and yttrium oxide co-stabilized tetragonal zirconia polycrystal (TZP) and fully stabilized zirconia pottery (FSZ) material by pressureless sintering.
Concrete processing step is:
(1) for tetragonal zirconia ceramics material (TEP), as co-stabilizer as stabilizing agent Yb
2O
3And Y
2O
3Mole percent be divided into 1.0-2.0% and 1.0-2.0%; For fully stabilized zirconia ceramic material (FSZ), be 3.0-4.0% according to the ytterbium oxide molar percentage respectively as ytterbium oxide and the yittrium oxide of stabilizing agent, the yittrium oxide molar percentage is design component in the 1.0-2.0% scope.
(2) raw material: comprise that purity is not less than 99.9% ytterbium oxide (Yb
2O
3), yittrium oxide (Y
2O
3) and average grain size less than the monoclinic zirconia powder of 100 nanometers.Composition proportioning according to above-mentioned (1) is selected an amount of corresponding compounds.
(3) powder is synthetic: ytterbium oxide and yttrium oxide are dissolved in the nitric acid that concentration is 0.5-1.5mol/L, cubic polycrystal zirconia ball with stabilized with yttrium oxide in container is a ball-milling medium, with nm-class powder of zirconium oxide in dehydrated alcohol mixing and ball milling 20-30 hour, use the Rotary Evaporators dry suspension then, obtain the presoma of coated powder, presoma obtains the nm-class powder of zirconium oxide of the common parcel of ytterbium oxide and yttrium oxide in 100-400 ℃ of calcining thermolysis in 0.5-2.0 hour in air.
(4) nm-class powder of zirconium oxide of the common parcel of ytterbium oxide and yttrium oxide is through cold isostatic compaction or dry-pressing formed, forming pressure is 100-300MPa, in air in 1400-1500 ℃ of pressureless sintering, soaking time is controlled in 1-5 hour scope, obtains fine and close ytterbium oxide and yttrium oxide co-stabilized tetragonal zirconia polycrystal (TZP) or fully stabilized zirconia pottery (FSZ).
Advantage of the present invention is:
(1) synthesis technique of powder is simple, and cost is low, does not need complex apparatus, enlarges scale production easily.
(2) replace rare earth nitrades as initiation material take rare earth oxide, reduce consumption, reduced preparation cost.
(3) carry out pyrolysis under lower temperature, avoided powder granule in the calcination process to grow up and the generation of hard aggregation, the powder after the pyrolysis can directly use, and does not need secondary ball milling, has further simplified preparation technology.
(4) can under low stabiliser content, obtain ytterbium oxide and yttrium oxide co-stabilized tetragonal zirconia polycrystal (TZP) and fully stabilized zirconia pottery (FSZ) by regulating component.By optimizing sintering condition, it is best that the mechanical property of tetragonal zirconia polycrystal (TZP) reaches.Particularly, as stabilizing agent Y
2O
3And Yb
2O
3Mole percent be TZP when being respectively 1.0-2.0% and 1.0-2.0%; As stabilizing agent Y
2O
3And Yb
2O
3Molal quantity be FSZ when being respectively 1.0-2.0% and 3.0-4.0%.
Description of drawings
The concrete process flow sheet of Fig. 1
Fig. 2 consists of 1.0mol%Yb
2O
3-1.0mol%Y
2O
3-ZrO
2, the XRD collection of illustrative plates of the TZP pottery that obtains under the different sintering conditions and corresponding 1400 ℃/1h of SEM photo (a), (b) 1450 ℃/1h, (d) 1450 ℃/4h
Fig. 3 consists of xmol%Yb
2O
3-1.0mol%Y
2O
3-ZrO
2(x=1.0,2.0,3.0,4.0) are HV at mechanical property (a) figure of 1450 ℃ of potteries of 1 hour of pressureless sintering in air
10(10 kilograms load under Vickers' hardness), unit is GPa, (b) figure is K
IC(fracture toughness property), unit is MPam
1/2
Fig. 4 consists of 4.0mol%Yb
2O
3-1.0mol%Y
2O
3-ZrO
2, at XRD collection of illustrative plates and the SEM photo of 1450 ℃ of FSZ potteries of 2 hours of sintering in air
Fig. 5 consists of 1.0mol%Yb
2O
3-2.0mol%Y
2O
3-ZrO
2XRD collection of illustrative plates and SEM photo at 1450 ℃ of TZP potteries that sintering obtained in 1 hour in air
Embodiment
Embodiment 1 is not less than 99.9% ytterbium oxide (Yb with purity
2O
3), yittrium oxide (Y
2O
3) and monoclinic zirconia powder (average grain size is less than 100 nanometers) be raw material, design is final to obtain ytterbium oxide (Yb in the TZP pottery
2O
3) molar percentage is 1.0%, yittrium oxide (Y
2O
3) molar percentage is 1.0%.Select an amount of corresponding compound according to above-mentioned composition and ratio, with ytterbium oxide (Yb
2O
3) and yittrium oxide (Y
2O
3) be dissolved in an amount of nitric acid and obtain settled solution, take the Y-TZP ball as ball-milling medium, in absolute ethyl alcohol, mix less than the monoclinic zirconia powder of 100 nanometers with average grain size and ball milling 24 hours.Use the rotary evaporator dry suspension behind the ball milling, obtain the presoma of coated powder.Presoma was calcined 1 hour in air in 300 ℃, obtained the nm-class powder of zirconium oxide of the common parcel of ytterbium oxide and yittrium oxide.Coated powder in 1450 ℃ of sintering, obtains that (Yb, Y)-the TZP pottery, its prepared step as shown in Figure 1 in air behind cold isostatic compaction.The XRD collection of illustrative plates of the TZP pottery of preparation, microstructure and mechanical property are respectively as shown in Figures 2 and 3.
The final ZrO that obtains of embodiment 2 designs
2Ytterbium oxide (Yb in the pottery
2O
3) molar percentage is 2.0%, yittrium oxide (Y
2O
3) molar percentage is 1.0%, according to the method synthetic powder of embodiment 1, the preparation pottery, sintering time is 1 hour.The ZrO of preparation
2The mechanical property of pottery as shown in Figure 3.
The final ZrO that obtains of embodiment 3 designs
2Ytterbium oxide (Yb in the pottery
2O
3) molar percentage is 3.0%, yittrium oxide (Y
2O
3) molar percentage is 1.0%, according to the method synthetic powder of embodiment 1, the preparation pottery, sintering time is 1 hour.The ZrO of preparation
2The mechanical property of pottery respectively as shown in Figure 3.
Ytterbium oxide (Yb in the final acquisition of the embodiment 4 designs FSZ pottery
2O
3) molar percentage is 4.0%, yittrium oxide (Y
2O
3) molar percentage is 1.0%, according to the method synthetic powder of embodiment 1, the preparation pottery, sintering time is 2 hours.The XRD collection of illustrative plates of the FSZ pottery of preparation and microstructure are as shown in Figure 4.
Ytterbium oxide (Yb in the final acquisition of the embodiment 5 designs TZP pottery
2O
3) molar percentage is 1.0%, yittrium oxide (Y
2O
3) molar percentage is 2.0%, according to the method synthetic powder of embodiment 1, the preparation pottery.The XRD collection of illustrative plates of the TZP pottery of preparation and microstructure are as shown in Figure 5.
Claims (10)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013003990A1 (en) * | 2011-07-04 | 2013-01-10 | 辽宁爱尔创生物材料有限公司 | Method for changing light transmittance of dental zirconia material |
| CN112159228A (en) * | 2020-09-27 | 2021-01-01 | 中国科学院上海光学精密机械研究所 | Preparation of Y by filling nano powder2O3Method for producing-MgO composite powder |
| CN114829304A (en) * | 2019-12-24 | 2022-07-29 | 关东电化工业株式会社 | Coated zirconia fine particles and method for producing same |
| CN115124343A (en) * | 2022-06-01 | 2022-09-30 | 上海大学 | A kind of zirconia solid solution yttrium oxide ceramic, its preparation method and application |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3034132B2 (en) * | 1992-09-29 | 2000-04-17 | 京セラ株式会社 | Zirconia solid electrolyte |
| JPH07215758A (en) * | 1994-01-28 | 1995-08-15 | Shinagawa Refract Co Ltd | Zirconia sintered compact |
| CN1170787C (en) * | 2002-03-22 | 2004-10-13 | 中国科学院上海硅酸盐研究所 | Magnesium oxide and yttrium oxide co-stabilized tetragonal zirconia polycrystalline ceramics and preparation method thereof |
| CN1251992C (en) * | 2004-06-25 | 2006-04-19 | 中国科学院上海硅酸盐研究所 | Neodymia and yttrium oxide co-stabilized cubic zirconia polycrystalline ceramic and its preparation method |
-
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- 2006-03-03 CN CNB2006100243615A patent/CN100347130C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013003990A1 (en) * | 2011-07-04 | 2013-01-10 | 辽宁爱尔创生物材料有限公司 | Method for changing light transmittance of dental zirconia material |
| US8697176B2 (en) | 2011-07-04 | 2014-04-15 | Liaoning Upcera Co., Ltd. | Method of changing translucent properties of zirconia dental materials |
| CN114829304A (en) * | 2019-12-24 | 2022-07-29 | 关东电化工业株式会社 | Coated zirconia fine particles and method for producing same |
| CN112159228A (en) * | 2020-09-27 | 2021-01-01 | 中国科学院上海光学精密机械研究所 | Preparation of Y by filling nano powder2O3Method for producing-MgO composite powder |
| CN112159228B (en) * | 2020-09-27 | 2023-02-14 | 中国科学院上海光学精密机械研究所 | Preparation of Y by filling nano powder 2 O 3 Method for producing-MgO composite powder |
| CN115124343A (en) * | 2022-06-01 | 2022-09-30 | 上海大学 | A kind of zirconia solid solution yttrium oxide ceramic, its preparation method and application |
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