JP2725027B2 - Embedding material for calcium phosphate glass crystallization - Google Patents
Embedding material for calcium phosphate glass crystallizationInfo
- Publication number
- JP2725027B2 JP2725027B2 JP63191280A JP19128088A JP2725027B2 JP 2725027 B2 JP2725027 B2 JP 2725027B2 JP 63191280 A JP63191280 A JP 63191280A JP 19128088 A JP19128088 A JP 19128088A JP 2725027 B2 JP2725027 B2 JP 2725027B2
- Authority
- JP
- Japan
- Prior art keywords
- glass
- calcium phosphate
- embedding material
- weight
- heat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000011521 glass Substances 0.000 title claims description 41
- 239000001506 calcium phosphate Substances 0.000 title claims description 26
- 229910000389 calcium phosphate Inorganic materials 0.000 title claims description 26
- 235000011010 calcium phosphates Nutrition 0.000 title claims description 26
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 title claims description 26
- 239000000463 material Substances 0.000 title claims description 22
- 238000002425 crystallisation Methods 0.000 title description 8
- 230000008025 crystallization Effects 0.000 title description 7
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 17
- 239000003779 heat-resistant material Substances 0.000 claims description 9
- 239000013078 crystal Substances 0.000 description 14
- 239000002245 particle Substances 0.000 description 7
- 230000007547 defect Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 5
- 238000005266 casting Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000007527 glass casting Methods 0.000 description 4
- 230000001939 inductive effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000009863 impact test Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- ROPDWRCJTIRLTR-UHFFFAOYSA-L calcium metaphosphate Chemical compound [Ca+2].[O-]P(=O)=O.[O-]P(=O)=O ROPDWRCJTIRLTR-UHFFFAOYSA-L 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- GEIAQOFPUVMAGM-UHFFFAOYSA-N ZrO Inorganic materials [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- DHAHRLDIUIPTCJ-UHFFFAOYSA-K aluminium metaphosphate Chemical compound [Al+3].[O-]P(=O)=O.[O-]P(=O)=O.[O-]P(=O)=O DHAHRLDIUIPTCJ-UHFFFAOYSA-K 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000005548 dental material Substances 0.000 description 1
- 238000004031 devitrification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は歯科用材料などに有用なリン酸カルシウム系
ガラスを結晶化して結晶化ガラスを製造する際に使用さ
れる包埋材に関するものである。Description: TECHNICAL FIELD The present invention relates to an embedding material used for producing crystallized glass by crystallizing calcium phosphate glass useful for dental materials and the like.
リン酸カルシウム系結晶化ガラスは生体の骨や歯と組
成が類似しており、生体とのなじみのよさから注目され
ている歯科用あるいは人工骨材料である。このリン酸カ
ルシウム系結晶化ガラスは原料を溶融し、ロストワック
ス法などで鋳造してガラス鋳造体を製造した後、熱処理
により結晶化することによって製造される。Calcium phosphate crystallized glass has a similar composition to bones and teeth of living organisms, and is a dental or artificial bone material that has attracted attention because of its good compatibility with living organisms. This calcium phosphate crystallized glass is produced by melting a raw material, casting it by a lost wax method or the like to produce a glass casting, and then crystallizing it by heat treatment.
リン酸カルシウム系ガラスを結晶化するには鋳造成形
されたガラスを鋳型のまゝ熱処理して結晶化させる方法
と、鋳型からガラス鋳造体を分離した後処理して結晶化
させる方法とがある。There are a method of crystallizing the calcium phosphate glass, a method of crystallizing the glass formed by casting and heat-treating the glass in a mold, and a method of crystallizing the glass by separating the glass casting from the mold and then treating it.
上記２種の結晶化法のうち前者においては鋳型材の成
分であるSiO2,Al2O3,MgO,ZrO2などがガラス鋳造体の表
面に接触しているため、その接触点の成分によって結晶
核の生成状態が異なったり異常な結晶核の生成や成長が
起こり勝ちであった。このように結晶核の生成や成長に
ムラがあると、リン酸カルシウム系ガラスは表面失透機
構によって結晶化が進行するため、一旦結晶核の生成に
ムラが生じると結晶全体が均一とはならず、外観的に劣
ったり、内部に欠陥を生じやすい欠点がある。In the former of the above two types of crystallization methods, since the components of the mold material such as SiO 2 , Al 2 O 3 , MgO, and ZrO 2 are in contact with the surface of the glass casting, Crystal nucleus formation state was different or abnormal crystal nucleus formation and growth were likely to occur. If there is unevenness in the generation and growth of crystal nuclei as described above, the crystallization of the calcium phosphate glass proceeds by the surface devitrification mechanism, so once the generation of the crystal nuclei becomes uneven, the entire crystal will not be uniform, There are drawbacks such as poor appearance and easy occurrence of defects inside.
また、後者においてはガラス表面の状態、即ち表面粗
さ、水分や油脂分等の吸着、付着の程度によって結晶化
は微妙に影響を受け、結果として前者ほどではないにし
ても不均一な結晶体となる。更に、ガラスの結晶化はそ
の軟化点付近の温度領域で行われるため、後者には軟化
変形によって鋳造体が歪み易い欠点もある。In the latter, the crystallization is slightly affected by the state of the glass surface, that is, the surface roughness, the degree of adsorption and adhesion of moisture and oils and the like, and as a result, the non-uniform crystals are not as good as the former. Becomes Furthermore, since the crystallization of glass is performed in a temperature region near its softening point, the latter has a disadvantage that the casting is easily distorted by softening deformation.
これらの欠点が解消されて、均一な結晶化ガラスが得
られれば高強度のリン酸カルシウム系結晶化ガラスが製
造できるのである。If these drawbacks are eliminated and a uniform crystallized glass can be obtained, a high-strength calcium phosphate crystallized glass can be manufactured.
本発明者らはリン酸カルシウム系結晶化ガラスの表面
がリン酸アルミニウムと接触していると均一な結晶化ガ
ラスができるとを見出し本発明を完成させたものであ
る。すなわち、本発明は結晶質あるいは無定形のリン酸
アルミニウムを５重量％以上含有し、残部が耐熱材料ま
たは結晶質あるいは無定形のリン酸カルシウムを10重量
％以上含有する耐熱材料であるリン酸カルシウム系ガラ
ス結晶化用包埋材であり、結晶化をこの包埋材中に埋め
込んで結晶化すれば、外観的には極めて優れており、か
つ内部欠陥のないリン酸カルシウム系結晶化ガラスが得
られるものである。The present inventors have found that a uniform crystallized glass can be obtained when the surface of the calcium phosphate crystallized glass is in contact with aluminum phosphate, and have completed the present invention. That is, the present invention provides a calcium phosphate-based glass crystallization which is a heat-resistant material containing 5% by weight or more of crystalline or amorphous aluminum phosphate and the remainder being 10% by weight or more of heat-resistant material or crystalline or amorphous calcium phosphate. By embedding the crystallization in this embedding material and crystallizing it, a calcium phosphate crystallized glass having extremely excellent appearance and free from internal defects can be obtained.
リン酸アルミニウム粒子がリン酸カルシウム系ガラス
表面と接触し、ガラス表面に多数の均一な結晶核を誘起
するため結果としてガラス全体がムラ無く一定の結晶化
度合に制御することが可能となる。このリン酸アルミニ
ウム粒子の結晶核を誘起する作用は他のSiO2やAl2O3な
どと比較して速く、リン酸アルミニウムが他の成分と接
触していても、リン酸アルミニウム粒子がある程度以上
存在すれば、その結晶核を誘起する作用は生ずる。Since the aluminum phosphate particles come into contact with the surface of the calcium phosphate-based glass and induce a large number of uniform crystal nuclei on the glass surface, the entire glass can be controlled to have a uniform crystallinity without unevenness. The action of inducing the crystal nuclei of the aluminum phosphate particles is faster than other SiO 2 or Al 2 O 3 etc., and even when the aluminum phosphate is in contact with other components, the aluminum phosphate particles If present, the action of inducing the crystal nucleus occurs.
また、リン酸カルシウムをリン酸アルミニウムと併用
することにより、更にその作用を強めることができる。
この理由については不明な点もあるが、リン酸カルシウ
ム自体には均一結晶核誘起作用は見られないので、リン
酸アルミニウムの持つ均一結晶核誘起作用に対する一種
の触媒効果を持つものと考えられる。Further, by using calcium phosphate in combination with aluminum phosphate, its action can be further enhanced.
Although the reason for this is not clear, calcium phosphate itself does not show a uniform crystal nucleus inducing action, and is considered to have a kind of catalytic effect on the uniform crystal nucleus inducing action of aluminum phosphate.
本発明の包埋材の主体であるリン酸アルミニウムとし
てはオルトリン酸アルミニウム（Al2O3・P2O5）、メタ
リン酸アルミニウム（Al2O3・3P2O5）などが使用可能で
ある。これらのリン酸アルミニウムが主体であれば、他
の成分が多少入ることはさしつかえない。また、その結
晶形態は無定形（ガラスを含む、以下同様）であっても
結晶質であってもあるいはそれらの混合物であっても構
わない。その使用量は包埋材全体の５重量％以上である
ことが必要である。５重量％未満では他の耐熱材料の影
響を受け結晶核の生成が均一とならない。Aluminum orthophosphate (Al 2 O 3 · P 2 O 5 ), aluminum metaphosphate (Al 2 O 3 · 3P 2 O 5 ) or the like can be used as the aluminum phosphate which is the main component of the embedding material of the present invention. . If these aluminum phosphates are the main components, some other components may not enter. The crystal form may be amorphous (including glass, the same applies hereinafter), crystalline, or a mixture thereof. It is necessary that the amount used is not less than 5% by weight of the whole embedding material. If it is less than 5% by weight, the generation of crystal nuclei is not uniform due to the influence of other heat-resistant materials.
本発明の包埋材の残部の耐熱材料は結晶化する温度で
軟化や溶融せず、かつ結晶化する材料と反応などの悪影
響を及ぼさないものであればよく、シリカ、アルミナ、
チタニア、ジルコニアなどの耐火材料やその他のガラ
ス、セラミックスなどが使用可能である。特にその耐熱
材料の一部をリン酸カルシウムとすることにより、既述
したようにその作用を一層高めることができる。このリ
ン酸カルシウムも各種のものが使用でき、CaO・P2O5,2C
aO・P2O5,3CaO・P2O5あるいは4CaO・3P2O5など、あるい
はそれら混合物であって、これ以外の成分が多少混入す
ることは構わない。この場合も結晶形態は無定形であっ
ても結晶質であってもあるいはそれらの混合物であって
もよい。リン酸カルシウムを使用する場合には耐熱材料
中の10重量％以上ないとリン酸カルシウムの効果が発揮
されにくい。The remaining heat-resistant material of the embedding material of the present invention does not soften or melt at the temperature at which it crystallizes, and may be any material that does not adversely affect the material to be crystallized and the reaction, such as silica, alumina,
Refractory materials such as titania and zirconia, and other glasses and ceramics can be used. In particular, by using calcium phosphate as a part of the heat-resistant material, the action can be further enhanced as described above. Various types of calcium phosphate can be used, and CaO · P 2 O 5 , 2C
aO.P 2 O 5 , 3CaO.P 2 O 5 or 4CaO.3P 2 O 5 , or a mixture thereof, and other components may be slightly mixed. Also in this case, the crystalline form may be amorphous, crystalline, or a mixture thereof. When calcium phosphate is used, the effect of calcium phosphate is difficult to exert unless it is at least 10% by weight in the heat-resistant material.
この包埋材の粒度は100μｍ以下が好ましい。大きい
粒子が入ると包埋材とガラス体との接触が悪くなり、本
発明の効果が発揮できない。The particle size of the embedding material is preferably 100 μm or less. When large particles enter, the contact between the embedding material and the glass body becomes poor, and the effect of the present invention cannot be exhibited.
本発明の包埋材の使用方法は、適当な耐熱容器に本包
埋材を入れ、鋳造形成したガラスを包埋材中に埋め込ん
で熱処理する。場合によっては鋳造体の周囲数mm以下を
本発明の包埋材とし、その外側は任意の耐熱材料粉末と
してもよい。また、包埋材を水，アルコールなどの適当
な溶媒でスラリー化した後、流し込んで包埋してもよ
い。更に、その際包埋材の硬化を助ける適当なバインダ
ーを加えてもよい。In the method of using the embedding material of the present invention, the embedding material is placed in an appropriate heat-resistant container, and the glass formed by casting is embedded in the embedding material and heat-treated. In some cases, the embedding material of the present invention may be several mm or less around the casting, and the outside thereof may be any heat-resistant material powder. Alternatively, the embedding material may be slurried with an appropriate solvent such as water or alcohol, and then poured and embedded. Further, at that time, a suitable binder for assisting the curing of the embedding material may be added.
実施例 １ リン酸カルシウム系ガラス（CaO38.5mol％,P2O548.1m
ol％,Al2O39.1mol％,Li2O4.3mol％）ロストワックス法
により歯冠形状に鋳造した。鋳型からガラスを分離した
後、粒径１〜68μｍのリン酸アルミニウム粉末（結晶質
70重量％中）に包埋し、650℃で10hr熱処理した。Example 1 Calcium phosphate glass (CaO 38.5 mol%, P 2 O 5 48.1 m
ol%, Al 2 O 3 9.1mol %, was cast in the crown shape by Li 2 O4.3mol%) lost wax process. After separating the glass from the mold, an aluminum phosphate powder having a particle size of 1 to 68 μm (crystalline
(At 70% by weight) and heat-treated at 650 ° C. for 10 hours.
調製した結晶化ガラスは半透明の象牙色で外観も内部
にも欠陥は見られなかった。1m上から鉄板上に落下させ
る衝撃試験でも壊れなかった。The prepared crystallized glass had a translucent ivory color, and no defects were observed in the appearance and the inside. It did not break even in an impact test in which it was dropped onto an iron plate from 1m above.
実施例 ２ 実施例１で得られた歯冠形状のリン酸カルシウム系ガ
ラスをリン酸アルミニウム（結晶質70重量％）65重量
％、アルミナ25重量％、シリカ10重量％で構成される粒
径１〜68μｍの粉末中に包埋し、650℃で10hr熱処理し
た。Example 2 The crown-shaped calcium phosphate-based glass obtained in Example 1 was made of 65% by weight of aluminum phosphate (crystalline 70% by weight), 25% by weight of alumina, and 10% by weight of silica. And heat-treated at 650 ° C. for 10 hours.
この結晶化ガラスも半透明の象牙色で外観も内部にも
欠陥は見られず、衝撃試験もクリアした。This crystallized glass was also translucent ivory with no defects in appearance or inside, and passed the impact test.
実施例 ３ 実施例１と同じ歯冠形状のリン酸カルシウム系ガラス
をリン酸アルミニウム（結晶質70重量％）50重量％、メ
タリン酸カルシウムガラス50重量％で構成される粒径１
〜68μｍの粉末中に包埋し、650℃で10hr熱処理した。Example 3 The same crown-shaped calcium phosphate glass as in Example 1 was composed of 50% by weight of aluminum phosphate (crystalline 70% by weight) and 50% by weight of calcium metaphosphate glass.
It was embedded in 〜68 μm powder and heat-treated at 650 ° C. for 10 hours.
この結晶化ガラスも半透明の象牙色で外観も内部にも
欠陥は見られず、衝撃試験での破壊もなかった。This crystallized glass was also translucent ivory, had no defects in appearance or inside, and did not break in the impact test.
比較例 １ 実施例１で得られた歯冠形状のリン酸カルシウム系ガ
ラスを鋳型（SiO290重量％、MgO5重量％、その他５重量
％）のまゝ650℃で10hr熱処理した。Comparative Example 1 The crown-shaped calcium phosphate glass obtained in Example 1 was heat-treated at 650 ° C. for 10 hours in a mold (90% by weight of SiO 2 , 5% by weight of MgO, and 5% by weight of others).
得られた結晶化ガラスは不透明の白色で審美性が悪
く、中心部には微細な気孔が生成していた。そのためか
落下試験では破壊してしまった。The crystallized glass obtained was opaque white and poor in aesthetics, and fine pores were formed at the center. For that reason, it was destroyed in the drop test.
比較例 ２ 実施例１で得られた歯冠形状のリン酸カルシウム系ガ
ラスを粒径１〜68μｍのアルミナ粉末およびメタリン酸
カルシウムガラス中にそれぞれ包埋し、650℃で10hr熱
処理した。Comparative Example 2 The crown-shaped calcium phosphate glass obtained in Example 1 was embedded in alumina powder having a particle size of 1 to 68 μm and calcium metaphosphate glass, respectively, and heat-treated at 650 ° C. for 10 hours.
得られた結晶化ガラスはいずれも半透明の象牙色中に
白色不透明部分の混った外観で、中心部には微細な気孔
が生成しており、落下試験により破壊した。Each of the resulting crystallized glasses had a translucent ivory color with white opaque portions mixed therein, and had fine pores formed in the center, and was broken by a drop test.
本発明のリン酸アルミニウムを含む包埋材を使用する
と均一な結晶となるため、実施例に見られるように審美
性に優れて、内部欠陥もなく、強度的にも優れた結晶化
ガラスが得られた。When the embedding material containing aluminum phosphate of the present invention is used, uniform crystals are obtained, so that a crystallized glass having excellent aesthetics, no internal defects, and excellent strength can be obtained as shown in Examples. Was done.
しかし、ガラス鋳造体を鋳型のまゝ結晶化（比較例
１）したり、リン酸アルミニウムを含まない包埋材中で
結晶化（比較例２）とすると、均一な結晶化の生成と成
長が行われないため、内部に気泡が生成し、そのため外
観も悪く、強度も低下してしまうのである。However, when the glass casting is crystallized as a mold (Comparative Example 1) or crystallized in an embedding material containing no aluminum phosphate (Comparative Example 2), uniform crystallization is generated and grown. Since it is not performed, air bubbles are generated inside, so that the appearance is poor and the strength is reduced.
───────────────────────────────────────────────────── フロントページの続き 審査官 徳永 英男 (56)参考文献 特開 昭62−87427（ＪＰ，Ａ) ──────────────────────────────────────────────────続 き Continuation of the front page Examiner Hideo Tokunaga (56) References JP-A-62-87427 (JP, A)
Claims (2)
ムを５重量％以上含有し残部が耐熱材料であることを特
徴とするリン酸カルシウム系ガラス結晶化用包埋材。1. An embedding material for crystallizing a calcium phosphate glass, comprising 5% by weight or more of crystalline or amorphous aluminum phosphate and the balance being a heat-resistant material.
カルシウムを10重量％以上含有することを特徴とする特
許請求の範囲第１項記載のリン酸カルシウム系ガラス結
晶化用包埋材。2. The embedding material for crystallizing a calcium phosphate glass according to claim 1, wherein the heat-resistant material contains at least 10% by weight of crystalline or amorphous calcium phosphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63191280A JP2725027B2 (en) | 1988-07-30 | 1988-07-30 | Embedding material for calcium phosphate glass crystallization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63191280A JP2725027B2 (en) | 1988-07-30 | 1988-07-30 | Embedding material for calcium phosphate glass crystallization |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0244038A JPH0244038A (en) | 1990-02-14 |
| JP2725027B2 true JP2725027B2 (en) | 1998-03-09 |
Family
ID=16271933
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63191280A Expired - Fee Related JP2725027B2 (en) | 1988-07-30 | 1988-07-30 | Embedding material for calcium phosphate glass crystallization |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2725027B2 (en) |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6287427A (en) * | 1985-10-11 | 1987-04-21 | Asahi Glass Co Ltd | Mold material |
-
1988
- 1988-07-30 JP JP63191280A patent/JP2725027B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0244038A (en) | 1990-02-14 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |