JPH03155483A - Method for joining graphite to titanium or titanium alloy - Google Patents
Method for joining graphite to titanium or titanium alloyInfo
- Publication number
- JPH03155483A JPH03155483A JP29102189A JP29102189A JPH03155483A JP H03155483 A JPH03155483 A JP H03155483A JP 29102189 A JP29102189 A JP 29102189A JP 29102189 A JP29102189 A JP 29102189A JP H03155483 A JPH03155483 A JP H03155483A
- Authority
- JP
- Japan
- Prior art keywords
- titanium
- graphite
- joining
- alloy
- bonding
- 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.)
- Granted
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 30
- 239000010439 graphite Substances 0.000 title claims abstract description 30
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000010936 titanium Substances 0.000 title claims abstract description 23
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 22
- 238000005304 joining Methods 0.000 title abstract description 16
- 238000000034 method Methods 0.000 title description 18
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 abstract description 19
- 238000005219 brazing Methods 0.000 abstract description 13
- 229910045601 alloy Inorganic materials 0.000 abstract description 5
- 239000000956 alloy Substances 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 abstract description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 abstract description 2
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 2
- 239000011733 molybdenum Substances 0.000 abstract description 2
- 229910052718 tin Inorganic materials 0.000 abstract description 2
- 239000011135 tin Substances 0.000 abstract description 2
- 229910052720 vanadium Inorganic materials 0.000 abstract description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 description 6
- 238000009864 tensile test Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 229910001651 emery Inorganic materials 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000003353 gold alloy Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Pressure Welding/Diffusion-Bonding (AREA)
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
この発明は、黒鉛（石墨、グラファイト）と、チタンま
たはチタン合金との接合方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a method for joining graphite (graphite, graphite) and titanium or a titanium alloy.
更に詳しくは黒鉛とチタンまたはチタン合金とを、高温
かつ真空（または不活性気体の存在）下において、接着
面を加圧保持することによって、両者な固相（固体）の
まま極めて強固に接合させることができるようにした黒
鉛とチタンまたはチタン合金との接合方法に関するもの
である。More specifically, graphite and titanium or titanium alloys are bonded extremely firmly while both remain in a solid state by pressurizing and holding the adhesive surfaces under high temperature and vacuum (or in the presence of an inert gas). The present invention relates to a method for joining graphite and titanium or a titanium alloy, which makes it possible to bond graphite to titanium or titanium alloy.
〈従来の技術と発明が解決しようとする問題点〉黒鉛は
熱、及び電気の良導体で、高い融点（３５００℃）と優
れた耐熱衝撃性を有することから、各種電極材料、炉の
内張材、モーターブラシ、鋳造用モウルド（ｍｏｕｌｄ
）材等に広（使用されている。また、原子炉内壁材（中
性子減速材）としての特性が優れていることから、近年
その適用が検討されており、このため金属と強固に接合
させる技術の開発が望まれている。<Problems to be solved by conventional technology and invention> Graphite is a good conductor of heat and electricity, and has a high melting point (3500°C) and excellent thermal shock resistance, so it is used as various electrode materials and furnace lining materials. , motor brush, casting mold
) materials, etc. Also, due to its excellent properties as a nuclear reactor inner wall material (neutron moderator), its application has been considered in recent years, and for this reason, technology to firmly bond it with metal is being considered. development is desired.
さて、黒鉛とチタンまたはチタン合金との接合は、従来
両者の接合面にロウ材（主成分としてチタン、ジルコニ
ウムを含む）を挾む（介する）と共に、高温真空下に一
定時間保持する真空ロウ付法により行われてきた（特開
昭６３−１１２０９５号公報（日本原子力研究所）、及
び日本金属学会：金属セラミック接合研究会資料（平成
元年２月２日）参照）。Conventionally, graphite and titanium or titanium alloys are bonded by sandwiching a brazing material (containing titanium and zirconium as main components) on the bonding surfaces of the two, and by vacuum brazing, which is held under high-temperature vacuum for a certain period of time. (Refer to Japanese Unexamined Patent Application Publication No. 112095/1989 (Japan Atomic Energy Research Institute) and Japan Institute of Metals: Metal Ceramic Bonding Study Group Materials (February 2, 1989)).
しかしながら従来法は、接着面にロウ材を介する（挾む
）溶融接合であるため、ロウ材の性質が、互いに接合し
て形成された接合素材の品質に大きく影響し、次のよう
な欠点を有している。However, since the conventional method uses fusion bonding with a brazing material interposed between the bonding surfaces, the properties of the brazing material greatly affect the quality of the bonded materials formed by bonding them together, resulting in the following drawbacks: have.
（イ）ロウ材の融点が高いと、接合時に金属材料（チタ
ンまたはチタン合金）が変質してしまう、また黒鉛と金
属両者の熱膨張率の差により割れが生じ易（なる。(a) If the melting point of the brazing material is high, the metal material (titanium or titanium alloy) will change in quality during joining, and cracks will easily occur due to the difference in thermal expansion coefficient between graphite and the metal.
（ロ）ロウ材の融点が低いと、接合時は問題は生じない
ものの、できた接合素材はロウ材の融点以下でしか使用
できない。(b) If the melting point of the brazing material is low, no problems will occur during joining, but the resulting joining material can only be used at temperatures below the melting point of the brazing material.
（ハ）ロウ材そのものの強度が問題となる場合がある。(c) The strength of the brazing material itself may be a problem.
そこで発明者は、接着面にロウ材を使用しないでも、黒
鉛とチタンまたはチタン合金とを強固に接合（接着）さ
せる方法（固相状態での接合）について鋭意研究した結
果、両者の接合面を無酸素の雰囲気下に、加圧状態で一
定以上の高温に保持すれば、驚くべきことに、黒鉛とチ
タンまたはチタン合金とを極めて強固に接合（接着）さ
せることができることを知り本願発明を完成した。Therefore, the inventor conducted intensive research on a method of firmly bonding (adhering) graphite and titanium or titanium alloy without using a brazing material on the bonding surface (solid state bonding). Surprisingly, he discovered that graphite and titanium or titanium alloys could be extremely strongly bonded (adhered) by keeping them under pressure and at a high temperature above a certain level in an oxygen-free atmosphere, and completed the present invention. did.
く問題を解決するための手段〉 すなわち、本願発明は次の構成を有すものである。Means to solve problems〉 That is, the present invention has the following configuration.
ｒ黒鉛と、チタンまたはチタン合金とを接合（接着）さ
せるに際し、両者の接合面を下記に記載する（Ａ）、（
Ｂ）、及び（Ｃ）の条件下に保持することを特徴とする
黒鉛とチタンまたはチタン合金との接合方法。r When bonding (adhering) graphite and titanium or titanium alloy, the bonding surfaces of both are described below (A), (
A method for joining graphite and titanium or a titanium alloy, characterized by holding the material under the conditions of B) and (C).
（Ａ）真空下または不活性気体の存在下に保持すること
。(A) Maintaining under vacuum or in the presence of an inert gas.
（Ｂ）加圧すること。(B) Apply pressure.
（Ｃ）８５０℃以上の温度に保持すること、１この発明
において使用される黒鉛は、天然、または人造のいずれ
の黒鉛（石墨、グラファイト）であっても使用できる０
本願発明の方法を実施すると、黒鉛によっては接合し難
いか、または接合不完全な場合が生ずることがある。し
かし、この場合には、理由は必ずしも明らかではないが
、黒鉛を予め接合温度以上に空焼きしておけばよい。(C) Maintaining the temperature at 850°C or higher; 1. The graphite used in this invention can be either natural or artificial graphite (graphite, graphite).
When the method of the present invention is carried out, some graphites may be difficult to bond or may be incompletely bonded. However, in this case, although the reason is not necessarily clear, the graphite may be preheated to a temperature higher than the bonding temperature.
この発明において使用されるチタン合金とは、チタンと
アルミニウム、バナジウム、モリブデン、マンガン、錫
、ジルコニウム等との合金をいう（例 Ｔｉ−６ＡＩ−
４Ｖ合金、Ｔｊ−８ＡＩ−Ｉ Ｍ ｏ −ＩＶ金合金Ｔ
ｌ−８Ｍｎ−合金、ＴｉＴｉ−６ＡＩ−２Ｓｎ−４２ｒ
−２合金等）。The titanium alloy used in this invention refers to an alloy of titanium with aluminum, vanadium, molybdenum, manganese, tin, zirconium, etc. (Example: Ti-6AI-
4V alloy, Tj-8AI-IM o -IV gold alloy T
l-8Mn-alloy, TiTi-6AI-2Sn-42r
-2 alloy, etc.).
この発明において、黒鉛とチタンまたはチタン合金との
接合面を真空下または不活性気体の存在下に保持する理
由は、黒鉛及びチタン合金が高温で着火しない（酸化さ
れない）ためである。In this invention, the reason why the bonding surface between graphite and titanium or titanium alloy is maintained under vacuum or in the presence of an inert gas is that graphite and titanium alloy do not ignite (do not oxidize) at high temperatures.
この発明において、黒鉛とチタンまたはチタン合金との
接合面には、通常研磨処理、有機溶媒での洗浄等の前処
理を施す、そして、この接合面に対して１通常数ｋｇ／
ｃｍ”以上に加圧した状態のままで接合処理を行う。In this invention, the bonding surface between graphite and titanium or titanium alloy is usually subjected to a pretreatment such as polishing or cleaning with an organic solvent, and the bonding surface is usually subjected to several kg/
The bonding process is performed while the pressure is still applied to a pressure of 1.5 cm or more.
従来、本願発明に係る接合方法のような、−見非常に簡
単な接合方法が知られていなかったのは、次の（イ）及
び（ロ）の理由によるものと思われる。The reason why a very simple joining method such as the joining method according to the present invention has not been known so far is probably due to the following reasons (a) and (b).
（イ）黒鉛とチタンまたはチタン合金との接合は、他の
金属と同様にロウ材の使用が不可欠であるとの固定観念
が広く存在したこと。(a) There was a widespread fixed idea that the use of brazing metal was essential for joining graphite with titanium or titanium alloys, just as with other metals.
（ロ）ロウ材を使用して接着面を加圧すると、はとんど
全てのログ材が接着面から排除されてしまうため、加圧
処理が全くされないか、または極めて不十分な加圧処理
しかされたことがなかったこと。(b) When applying pressure to the bonding surface using brazing wood, almost all of the log material is removed from the bonding surface, resulting in either no pressure treatment or extremely insufficient pressure treatment. But it had never happened before.
〈実施例〉
（１）接合装置として、市販のホットプレス装置（第１
図）を用い、接合試料は第２図に示すようにａ、ｂの２
種類の形状とした。<Example> (1) As a bonding device, a commercially available hot press device (first
2), and the bonded sample is 2 parts a and b as shown in Fig. 2.
It has a variety of shapes.
種々の接合条件により接合処理を施した後、ａタイプの
試料は、第３図の形状に加工後第４図の方法で、またｂ
タイプの試料は第５図に示す方法で引張り試験を行った
。After performing bonding processing under various bonding conditions, the sample of type a was processed into the shape shown in Fig. 3, and then processed by the method shown in Fig. 4, and b
A tensile test was carried out on a sample of the type according to the method shown in FIG.
なお、接合前処理として、接合面は＄１ＯＯＯのエメリ
ー紙で研磨した後、アセトン中で洗浄し接合装置（第１
図）にセットした。雰囲気が１０−’ Ｔｏｒｒ以下
に達した後、第６図に示すように、所定の温度、加圧力
、時間で接合処理を行った。As a pre-bonding treatment, the bonding surfaces were polished with $100 emery paper, washed in acetone, and placed in the bonding device (No. 1).
(Figure). After the atmosphere reached 10-' Torr or less, a bonding process was performed at a predetermined temperature, pressure, and time, as shown in FIG.
（２）作製した接合試料に対し、前項の方法で弓張り試
験を行い接合部の強度を調べた。引張り試験は室温で行
い、引張り速度は０．５ｍｍ／ｍｉｎとした。(2) The produced bonded sample was subjected to a bow tension test using the method described in the previous section to examine the strength of the bonded portion. The tensile test was conducted at room temperature, and the tensile speed was 0.5 mm/min.
なお、用いた黒鉛素材は、■ニスイージーのＭＧ−Ｙ、
及びＭＧ−３の２種類、チタン素材は工業用純チタン第
３種（ＣＰＴｉ）及びＴｉ−６Ａ １−４Ｖ合金（６−
４Ｔｉ）（７）２種類でその引張り強さを第１表（巻末
以下同じ）に示す、また、第２表及び第３表に各接合条
件で作成した試料の引張り試験結果を示す。In addition, the graphite material used was ■Ni-Easy's MG-Y,
and MG-3, and the titanium materials are industrially pure titanium type 3 (CPTi) and Ti-6A 1-4V alloy (6-
4Ti) (7) The tensile strengths of the two types are shown in Table 1 (same at the end of the book), and Tables 2 and 3 show the tensile test results of samples prepared under each bonding condition.
第２表及び第３表の結果によれば、本願発明の方法によ
り黒鉛とチタンまたはチタン合金を接合した後、両者を
分離（分割）しようとすれば黒鉛部分に破壊（破断）が
起こることが分かる（第７図）、すなわち、黒鉛とチタ
ンまたはチタン合金は、極めて強固に接合し、接合部分
の強度は素材以上の強度に達していることが分かる。According to the results in Tables 2 and 3, after graphite and titanium or titanium alloy are joined by the method of the present invention, if an attempt is made to separate (split) the two, destruction (rupture) will occur in the graphite part. As can be seen (Fig. 7), it can be seen that graphite and titanium or titanium alloy are extremely strongly bonded, and the strength of the bonded portion exceeds that of the raw material.
〈発明の効果〉
以上のようにこの発明に係る黒鉛とチタンまたはチタン
合金との接合方法によれば、ロウ材を全く使用すること
なく両者を固体（固相）状のままで極めて強固に接着さ
せることができるという効果を有し、その応用範囲は極
めて広い。<Effects of the Invention> As described above, according to the method for joining graphite and titanium or titanium alloy according to the present invention, the two can be bonded extremely firmly while remaining in a solid state without using any brazing material. The range of applications is extremely wide.
第１図は接合装置（ホットプレス装置）を示す図（断面
図）、第２図は接合試料ａ及びｂの形状を示す図（正面
図）、第３図は接合試料ａの引張試験片の形状を示す図
（正面図）、第４図は接合試料ａの引張り試験方法を示
す図（正面図）、第５図は接合試料すの引張り試験方法
を示す図（断面図）、第６図は接合プロセスを示す図、
第７図は接合試料すの試験片の破断形態を示す図（正面
図）である。
１・・・油圧シリンダー
２・・・ヒーター
３・・・熱電対
４・・・接合試料
５・・・黒鉛
６・・・チタンまたはチタン合金
７・・・真空ポンプ
８・・・ロードセル
９・・・破断面
なお、第７図中のＴは接合温度を示し、ＦＣは炉冷の略
号である。Fig. 1 is a cross-sectional view showing the bonding device (hot press device), Fig. 2 is a front view showing the shapes of bonded samples a and b, and Fig. 3 is a tensile test piece of bonded sample a. Figure 4 is a diagram showing the tensile test method for bonded sample a (front view), Figure 5 is a diagram showing the tensile test method for bonded sample A (cross-sectional view), and Figure 6 is a diagram showing the shape (front view). is a diagram showing the joining process,
FIG. 7 is a diagram (front view) showing the fracture form of a test piece of a bonded sample. 1... Hydraulic cylinder 2... Heater 3... Thermocouple 4... Bonded sample 5... Graphite 6... Titanium or titanium alloy 7... Vacuum pump 8... Load cell 9... - Fractured surface Note that T in FIG. 7 indicates the joining temperature, and FC is an abbreviation for furnace cooling.
Claims (1)
）させるに際し、両者の接合面を下記に記載する（Ａ）
、（Ｂ）、及び（Ｃ）の条件下に保持することを特徴と
する黒鉛とチタンまたはチタン合金との接合方法。 （Ａ）真空下または不活性気体の存在下に保持すること
。 （Ｂ）加圧すること。 （Ｃ）８５０℃以上の温度に保持すること。(1) When bonding (adhering) graphite and titanium or titanium alloy, the bonding surfaces of both are described below (A)
, (B), and (C). (A) Maintaining under vacuum or in the presence of an inert gas. (B) Apply pressure. (C) Maintain the temperature at 850°C or higher.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1291021A JP2676413B2 (en) | 1989-11-10 | 1989-11-10 | Method for joining graphite and titanium or titanium alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1291021A JP2676413B2 (en) | 1989-11-10 | 1989-11-10 | Method for joining graphite and titanium or titanium alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03155483A true JPH03155483A (en) | 1991-07-03 |
| JP2676413B2 JP2676413B2 (en) | 1997-11-17 |
Family
ID=17763429
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1291021A Expired - Fee Related JP2676413B2 (en) | 1989-11-10 | 1989-11-10 | Method for joining graphite and titanium or titanium alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2676413B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008081362A (en) * | 2006-09-27 | 2008-04-10 | Kwansei Gakuin | Method for producing bonded material of tantalum and carbon, gradient composition structure of tantalum and carbon, method for producing tantalum tube and pit carbon core, tantalum tube and pit carbon core, method for producing tantalum carbide wire, and tantalum carbide wire |
| CN114178638A (en) * | 2021-12-03 | 2022-03-15 | 湘潭大学 | Welding method for high-strength graphite pipe and titanium alloy pipe sleeved composite component |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61111979A (en) * | 1984-11-07 | 1986-05-30 | 科学技術庁金属材料技術研究所長 | Manufacture of bonded material of graphite and high melting point metal |
| JPH01111783A (en) * | 1987-05-13 | 1989-04-28 | Shin Meiwa Ind Co Ltd | Joined structure of carbon and ceramics, carbon or metal |
-
1989
- 1989-11-10 JP JP1291021A patent/JP2676413B2/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61111979A (en) * | 1984-11-07 | 1986-05-30 | 科学技術庁金属材料技術研究所長 | Manufacture of bonded material of graphite and high melting point metal |
| JPH01111783A (en) * | 1987-05-13 | 1989-04-28 | Shin Meiwa Ind Co Ltd | Joined structure of carbon and ceramics, carbon or metal |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008081362A (en) * | 2006-09-27 | 2008-04-10 | Kwansei Gakuin | Method for producing bonded material of tantalum and carbon, gradient composition structure of tantalum and carbon, method for producing tantalum tube and pit carbon core, tantalum tube and pit carbon core, method for producing tantalum carbide wire, and tantalum carbide wire |
| CN114178638A (en) * | 2021-12-03 | 2022-03-15 | 湘潭大学 | Welding method for high-strength graphite pipe and titanium alloy pipe sleeved composite component |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2676413B2 (en) | 1997-11-17 |
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