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JP2745065B2 - Bonding wire for semiconductor device - Google Patents

Bonding wire for semiconductor device

Info

Publication number
JP2745065B2
JP2745065B2 JP1112579A JP11257989A JP2745065B2 JP 2745065 B2 JP2745065 B2 JP 2745065B2 JP 1112579 A JP1112579 A JP 1112579A JP 11257989 A JP11257989 A JP 11257989A JP 2745065 B2 JP2745065 B2 JP 2745065B2
Authority
JP
Japan
Prior art keywords
wire
bonding wire
less
bonding
strength
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
Application number
JP1112579A
Other languages
Japanese (ja)
Other versions
JPH02119148A (en
Inventor
恭秀 大野
芳雄 大関
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Steel Corp
Original Assignee
Nippon Steel Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nippon Steel Corp filed Critical Nippon Steel Corp
Publication of JPH02119148A publication Critical patent/JPH02119148A/en
Application granted granted Critical
Publication of JP2745065B2 publication Critical patent/JP2745065B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B5/00—Turning-machines or devices specially adapted for particular work; Accessories specially adapted therefor
    • B23B5/08—Turning-machines or devices specially adapted for particular work; Accessories specially adapted therefor for turning axles, bars, rods, tubes, rolls, i.e. shaft-turning lathes, roll lathes; Centreless turning
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H01B1/026—Alloys based on copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/02—Alloys based on gold
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
    • H01L21/60—Attaching or detaching leads or other conductive members, to be used for carrying current to or from the device in operation
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Landscapes

  • Engineering & Computer Science (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Wire Bonding (AREA)

Description

【発明の詳細な説明】 （産業上の利用分野） 本発明は半導体素子の電極と外部リードを接続するた
めに使用するボンディングワイヤに関するものである。Description: TECHNICAL FIELD The present invention relates to a bonding wire used for connecting an electrode of a semiconductor element to an external lead.

（従来の技術） 従来、半導体素子の電極を外部リードに接続するため
に、Auに微量のCa,Be,Geなどを含有させたAu合金の線径
25〜50μｍのワイヤ、すなわちボンディングワイヤが用
いられている。(Prior art) Conventionally, in order to connect the electrode of the semiconductor element to the external lead, the wire diameter of Au alloy containing a small amount of Ca, Be, Ge, etc. in Au
A wire of 25 to 50 μm, that is, a bonding wire is used.

このワイヤを用いて半導体素子とリードフレームを接
続する際に、両者とも超音波による圧接か、半導体素子
の電極については、アークで先端をボールアップした後
熱圧着する方法がとられている。When a semiconductor element and a lead frame are connected by using these wires, either a method of pressing by ultrasonic waves or a method of thermocompression bonding the electrodes of the semiconductor element after ball-up of the tip with an arc.

しかしながら、近年ICのより一層の小型化、集積化が
おこなわれ、電極数の増加のため、現状ワイヤ径では、
電極の占める面積が大きくなりすぎることが問題視され
るようになってきた。この問題を解決するためには、ワ
イヤ径を細くすることが必要であるが、現状のワイヤを
細くしたのでは、配線時及び使用中の断線の割合が高く
実用に供しえない。However, in recent years, further miniaturization and integration of ICs have been performed, and the number of electrodes has increased.
It has become a problem that the area occupied by the electrodes becomes too large. In order to solve this problem, it is necessary to reduce the diameter of the wire. However, if the current wire is reduced, the rate of disconnection during wiring and during use is high and cannot be put to practical use.

そのため現状ワイヤでは、ボンディングワイヤの特性
としては線径20μｍ程度が限界であるとされていた。Therefore, it has been considered that the current wire has a limit of about 20 μm in wire diameter as a characteristic of the bonding wire.

特開昭56−49534号公報および特開昭56−49535号公報
ではPtを30wt％まで、あるいはPdを40wt％までAuに加え
ることによりワイヤの高強度化をはかり、細線化を可能
にするという提案もあるが、合金元素の含有量がある限
界を越えると接合時に形成するボールの硬さが増し、熱
圧着に必要な荷重が大きくなり、ICのシリコンチップに
損傷を与える等の問題が起きる。特開昭60−15958号公
報では、Alに異種元素を混入した電極配線に対して良好
な熱圧着性を有するボンディングワイヤとして、Au基の
合金ワイヤが提案されているが、これも同様の問題があ
り、従来から採用されているIC,及び接合方法を特別に
変更することなく、ICの小型化、高密度化がはかれる新
しいボンディングワイヤが求められている。In JP-A-56-49534 and JP-A-56-49535, it is said that by adding Pt up to 30 wt% or Pd up to 40 wt% to Au, the strength of the wire can be increased and the wire can be thinned. Although there are proposals, if the alloy element content exceeds a certain limit, the hardness of the ball formed at the time of joining increases, the load required for thermocompression bonding increases, and problems such as damaging the silicon chip of the IC occur . Japanese Patent Application Laid-Open No. 60-15958 proposes an Au-based alloy wire as a bonding wire having good thermocompression bonding property for electrode wiring in which a different element is mixed into Al. Therefore, there is a demand for a new bonding wire that can reduce the size and density of the IC without specially changing the conventionally used IC and the bonding method.

（発明が解決しようとする課題） そこで、本発明は、ボンディングワイヤの線径をこれ
までよりも細くしても従来のワイヤと同じ信頼性を持っ
たワイヤを提供することを目的とする。また、本発明の
他の目的としては、製造時においても強度がつよくて極
細線にすることが可能で、接合時の破断強度に優れた断
線の極めて少ない半導体素子用ボンディングワイヤを提
供しようとするものである。(Problems to be Solved by the Invention) Accordingly, an object of the present invention is to provide a wire having the same reliability as a conventional wire even if the wire diameter of a bonding wire is made smaller than before. Another object of the present invention is to provide a bonding wire for a semiconductor element which has high strength during production and can be formed into a fine wire, and has excellent breaking strength at the time of bonding and extremely few disconnections. Things.

（課題を解決するための手段） 本発明の要旨は下記のとおりである。(Means for Solving the Problems) The gist of the present invention is as follows.

（１） Cuを１〜5wt％未満含有し、残部はAuからなる
半導体素子用ボンディングワイヤ。(1) A bonding wire for a semiconductor element which contains Cu in an amount of less than 1 to 5 wt% and the balance is made of Au.

（２） Cuを１〜5wt％未満と、Ca,Ge,Be,La,Inの１種
または２種以上を合計で0.0003〜0.01wt％含有し、残部
はAuからなる半導体素子用ボンディングワイヤ。(2) A bonding wire for a semiconductor element containing 1 to 5% by weight of Cu and one or more of Ca, Ge, Be, La, and In in a total of 0.0003 to 0.01% by weight, with the balance being Au.

（３） Cuを１〜5wt％未満と、Ptを１〜5wt％未満含有
し、残部はAuからなる半導体素子用ボンディングワイ
ヤ。(3) A bonding wire for a semiconductor element containing Cu of less than 1 to 5 wt% and Pt of less than 1 to 5 wt%, with the balance being Au.

（４） Cuを１〜5wt％未満と、Ptを１〜5wt％未満と、
Ca,Ge,Be,La,Inの１種または２種以上を合計で0.0003〜
0.01wt％含有し、残部はAuからなる半導体素子用ボンデ
ィングワイヤ。(4) Cu less than 1-5 wt%, Pt less than 1-5 wt%,
One or more of Ca, Ge, Be, La, In and 0.0003 or more in total
A bonding wire for semiconductor devices consisting of 0.01 wt% and the balance Au.

本発明の半導体素子用ボンディングワイヤにおいて、
AuにCuを１〜5wt％未満含有させた理由は、CuがAuに完
全に固溶することにより、母線の強度が向上するばかり
か接合強度も高くなるからで、これまでのワイヤではな
かなか難しかった線径20μｍ以下の細線にしても、Cuが
１％以上含有されていれば、破断強度4gr以上を満足す
ることが出来る。この特徴は、Cuの含有量の増加ととも
に強度の上昇が認められるが、５％を越えると耐食性に
問題を生じ、長時間を経た後での信頼性を損なう。ま
た、Cuの含有量が５％に達すると接合時に形成するボー
ルの硬さが増加し、熱圧着に必要な荷重が大きくなるこ
とからシリコンチップに損傷を与えるためである。In the semiconductor device bonding wire of the present invention,
The reason why Cu contained less than 1 to 5 wt% in Au is that the complete solid solution of Cu not only improves the strength of the bus bar, but also increases the bonding strength. Even with a thin wire having a wire diameter of 20 μm or less, a breaking strength of 4 gr or more can be satisfied if Cu is contained at 1% or more. With this feature, an increase in strength is observed with an increase in the content of Cu, but if it exceeds 5%, a problem occurs in corrosion resistance and reliability after a long time is impaired. Further, when the Cu content reaches 5%, the hardness of the ball formed at the time of joining increases, and the load required for thermocompression bonding increases, thereby damaging the silicon chip.

なお、原料となるAu、Cuは不純物の含有量が多いと製
品の特性が不安定となることと、細線化や接合時に破断
の原因となるので、99.9％以上の高純度とすることが好
ましい。In addition, since Au and Cu as raw materials have a high impurity content, the characteristics of the product become unstable, and the wire may be broken at the time of thinning or joining, it is preferable to have a high purity of 99.9% or more. .

Cuの含有によってこのような効果が得られるのは、固
溶体強化と規則格子の生成によっていると推察される。
なお、Ptは、この効果を助長する働きをする。その含有
量は、１〜5wt％未満の範囲で、それ未満では効果がな
く、上限を越えると延性の減少やボールの硬さの増加と
いう不都合が生ずる。It is presumed that such effects are obtained by the inclusion of Cu due to solid solution strengthening and formation of ordered lattices.
Pt works to promote this effect. If the content is less than 1 to 5 wt%, there is no effect if less than 5 wt%, and if it exceeds the upper limit, disadvantages such as decrease in ductility and increase in hardness of the ball occur.

伸線時に導入された加工歪を除き、適度な延性と十分
な強度を保持するために、200〜600℃の温度と適切な時
間の熱処理を行うことが望ましい。It is desirable to perform a heat treatment at a temperature of 200 to 600 ° C. and an appropriate time in order to maintain appropriate ductility and sufficient strength, excluding processing strain introduced during wire drawing.

伸線ままの細線は延性（伸び）がなく、また加工歪の
ためカールが強く、使用に供せないことがあるので通常
は焼なまし熱処理を行う。熱処理の温度が高いほど、長
時間であるほど強度が低下し、延性が大きくなるのが一
般的であるが、その程度は合金成分の含有量によって異
なるので、線径と成分に応じた熱処理条件を選ぶ必要が
ある。また、この熱処理によって組織の再結晶、粒成長
が進行するが、結晶粒径が線径に近づくと、強度，延性
とも著しく低下するため、熱処理条件の選定は細線ワイ
ヤの場合は特に重要である。The as-drawn fine wire does not have ductility (elongation), and has a strong curl due to processing distortion, so that it may not be usable, so that it is usually subjected to annealing heat treatment. In general, the higher the heat treatment temperature and the longer the heat treatment, the lower the strength and the higher the ductility.However, the degree depends on the content of the alloy components, so the heat treatment conditions according to the wire diameter and the components You need to choose In addition, the heat treatment promotes recrystallization and grain growth of the structure, but when the crystal grain size approaches the wire diameter, both the strength and ductility are significantly reduced. Therefore, the selection of the heat treatment condition is particularly important in the case of a fine wire. .

第１図は、Cuを含有した線径10μｍのワイヤで4gr以
上の破断強度を確保する熱処理条件を示したグラフであ
る。実線は400℃、破線は200℃で処理した場合を示して
いる。FIG. 1 is a graph showing heat treatment conditions for securing a breaking strength of 4 gr or more with a wire containing Cu and having a wire diameter of 10 μm. The solid line indicates the case where the treatment was performed at 400 ° C, and the broken line indicates the case where the treatment was performed at 200 ° C.

また、特に、従来の金ボンディングワイヤの添加にも
用いられているCa,Be,Ge,La,Inの添加は、本発明のボン
ディングワイヤの接合強度を向上させる。この目的のた
めに、これらの元素の１種または２種以上を合計で0.00
03〜0.01wt％の範囲で添加することができる。In particular, the addition of Ca, Be, Ge, La, and In, which is also used for the conventional addition of a gold bonding wire, improves the bonding strength of the bonding wire of the present invention. For this purpose, one or more of these elements may be added in a total of 0.00
It can be added in the range of 03 to 0.01 wt%.

本発明のボンディングワイヤは、真空溶解炉等を用い
て本発明にしたがった化学成分のAu合金を溶解し鋳造し
た後、線引、熱処理等を行って所望の線径のワイヤに製
造される。The bonding wire of the present invention is manufactured into a wire having a desired wire diameter by melting and casting an Au alloy of a chemical component according to the present invention using a vacuum melting furnace or the like, and then performing drawing and heat treatment.

（実施例） つぎに、本発明の効果を明瞭にする実施例を説明す
る。(Example) Next, an example for clarifying the effects of the present invention will be described.

純度99.99％の高純度Auと純度99.9％の高純度Cuを用
い、第１表のような元素を添加した材料を真空溶解炉で
溶製し、線引、熱処理をおこなった。線径は、10μm,一
部は、12μm,15μm,19μm,25μm,30μｍである。Using high-purity Au of 99.99% purity and high-purity Cu of 99.9% purity, materials added with the elements shown in Table 1 were melted in a vacuum melting furnace, drawn, and heat-treated. The wire diameter is 10 μm, and partly 12 μm, 15 μm, 19 μm, 25 μm, and 30 μm.

引っ張り試験はゲージ長100mmの試験片を用いた。接
合強度は第２図に示すようにSiチップ１とリードフレー
ム２に接合したボンディングワイヤ３を図に示すように
矢印方向に引っ張り、そのときの破断強度を測定した。
ワイヤの破断荷重、伸びと接合後の破断強度を比較材と
対比して第１表に示す。For the tensile test, a test piece having a gauge length of 100 mm was used. As shown in FIG. 2, the bonding wire 3 bonded to the Si chip 1 and the lead frame 2 was pulled in the direction of the arrow as shown in FIG. 2, and the breaking strength was measured.
The breaking load and elongation of the wire and the breaking strength after joining are shown in Table 1 in comparison with comparative materials.

第１表から明らかなように、本発明ワイヤは、細径に
もかかわらず破断強度及び接合強度が優れていることが
わかる。また、従来のボンディングワイヤと同様の線径
で使用すれば、より強度の高いワイヤが得られる。As is clear from Table 1, the wire of the present invention has excellent breaking strength and bonding strength despite its small diameter. Also, if the wire diameter is the same as that of a conventional bonding wire, a wire having higher strength can be obtained.

（発明の効果） 以上説明したように、本発明ワイヤは、破断強度及び
接合強度に優れ、特に、従来のワイヤに対して、10μｍ
のような細径にしても従来のワイヤ以上に信頼性の高い
ワイヤとして高集積化したLSIの小型化に役立つもので
ある。 (Effects of the Invention) As described above, the wire of the present invention is excellent in breaking strength and bonding strength, and in particular, is 10 μm
Even with such a small diameter, it is useful for reducing the size of highly integrated LSIs as wires having higher reliability than conventional wires.

【図面の簡単な説明】[Brief description of the drawings]

第１図は、Cuを含有した線径10μｍのワイヤで4gr以上
の破断強度を確保する熱処理条件を示したグラフであ
る。実線は400℃、破線は200℃で処理した場合を示して
いる。 第２図は、接合強度測定法の説明図である。 1;Siチップ、2;リードフレーム、3;ボンディングワイ
ヤ、↑；引っ張り方向FIG. 1 is a graph showing heat treatment conditions for securing a breaking strength of 4 gr or more with a wire containing Cu and having a wire diameter of 10 μm. The solid line indicates the case where the treatment was performed at 400 ° C, and the broken line indicates the case where the treatment was performed at 200 ° C. FIG. 2 is an explanatory view of a bonding strength measuring method. 1; Si chip, 2; Lead frame, 3; Bonding wire, ↑; Pull direction

───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭56−76556（ＪＰ，Ａ) 特開 昭56−49534（ＪＰ，Ａ) 特開 昭56−88329（ＪＰ，Ａ) 特開 昭56−115544（ＪＰ，Ａ) 特開 昭56−122140（ＪＰ，Ａ) 特開 平１−110741（ＪＰ，Ａ) ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-56-76556 (JP, A) JP-A-56-49534 (JP, A) JP-A-56-88329 (JP, A) JP-A-56-88329 115544 (JP, A) JP-A-56-122140 (JP, A) JP-A 1-110741 (JP, A)

Claims (7)

(57)【特許請求の範囲】(57) [Claims] 【請求項１】Cuを１〜5wt％未満含有し、残部はAuから
なる半導体素子用ボンディングワイヤ。1. A bonding wire for a semiconductor element, comprising 1 to less than 5% by weight of Cu and the balance of Au. 【請求項２】Cuを１〜5wt％未満と、Ca,Ge,Be,La,Inの
１種または２種以上を合計で0.0003〜0.01wt％含有し、
残部はAuからなる半導体素子用ボンディングワイヤ。2. The composition contains Cu in an amount of 1 to less than 5 wt% and one or more of Ca, Ge, Be, La and In in a total amount of 0.0003 to 0.01 wt%.
The remainder is a semiconductor element bonding wire made of Au. 【請求項３】Cuを１〜5wt％未満と、Ptを１〜5wt％未満
含有し、残部はAuからなる半導体素子用ボンディングワ
イヤ。3. A bonding wire for a semiconductor element comprising Cu of less than 1 to 5% by weight and Pt of less than 1 to 5% by weight, with the balance being Au. 【請求項４】Cuを１〜5wt％未満と、Ptを１〜5wt％未満
と、Ca,Ge,Be,La,Inの１種または２種以上を合計で0.00
03〜0.01wt％含有し、残部はAuからなる半導体素子用ボ
ンディングワイヤ。4. The method according to claim 1, wherein the content of Cu is less than 1 to 5 wt%, the content of Pt is less than 1 to 5 wt%, and at least one of Ca, Ge, Be, La, and In is 0.00%.
A bonding wire for semiconductor devices containing 03-0.01wt%, the balance being Au. 【請求項５】線径が20μｍ以下である請求項１〜４のい
ずれかに記載の半導体素子用ボンディングワイヤ。5. The bonding wire for a semiconductor device according to claim 1, wherein the wire diameter is 20 μm or less. 【請求項６】破断強さが4gr以上である請求項１〜４の
いずれかに記載の半導体素子用ボンディングワイヤ。6. The bonding wire for a semiconductor element according to claim 1, which has a breaking strength of 4 gr or more. 【請求項７】線径が15μｍ以下で破断強さが4gr以上で
ある請求項１〜４のいずれかに記載の半導体素子用ボン
ディングワイヤ。7. The bonding wire for a semiconductor device according to claim 1, wherein the wire diameter is 15 μm or less and the breaking strength is 4 gr or more.
JP1112579A 1988-05-02 1989-05-01 Bonding wire for semiconductor device Expired - Fee Related JP2745065B2 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP10958788 1988-05-02
JP63-109587 1988-05-02

Publications (2)

Publication Number Publication Date
JPH02119148A JPH02119148A (en) 1990-05-07
JP2745065B2 true JP2745065B2 (en) 1998-04-28

Family

ID=14514045

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JP (1) JP2745065B2 (en)
KR (1) KR930001265B1 (en)
DE (1) DE3990432C1 (en)
GB (1) GB2229859B (en)
WO (1) WO1989011161A1 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10233408A (en) * 1997-02-21 1998-09-02 Nec Corp Metal junction structure and semiconductor device
JP3426473B2 (en) * 1997-07-01 2003-07-14 新日本製鐵株式会社 Gold alloy wires for semiconductor devices
DE19740004A1 (en) * 1997-09-11 1998-11-19 Siemens Ag Bond wire for semiconductor device contact terminal
DE19753055B4 (en) * 1997-11-29 2005-09-15 W.C. Heraeus Gmbh Fine wire of a gold alloy, process for its preparation and its use

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3769006A (en) * 1972-01-27 1973-10-30 Gold Refining W Co Bright cast alloy, and composition
JPS53112060A (en) * 1977-03-11 1978-09-30 Tanaka Electronics Ind Gold wire for bonding semiconductor
JPS55127041A (en) * 1979-03-26 1980-10-01 Hitachi Ltd Resin-sealed semiconductor device
JPS5649534A (en) * 1979-09-28 1981-05-06 Tanaka Kikinzoku Kogyo Kk Bonding wire for semiconductor device
JPS5676556A (en) * 1979-11-28 1981-06-24 Tanaka Denshi Kogyo Kk Bonding gold wire for semiconductor element
DE3153395C2 (en) * 1981-02-12 1987-11-19 W.C. Heraeus Gmbh, 6450 Hanau, De Use of a very fine wire made of a copper/tin alloy
DD201156A1 (en) * 1981-10-02 1983-07-06 Daut Hans Heiner Precious metal alloys for micro-wire materials
US4490504A (en) * 1983-08-15 1984-12-25 General Electric Company Flame retardant non-dripping polycarbonate compositions
JPS6049534A (en) * 1983-08-26 1985-03-18 三菱電機株式会社 Circuit breaker
EP0288776A3 (en) * 1987-04-28 1989-03-22 Texas Instruments Incorporated Gold alloy wire connection to copper doped aluminum semiconductor circuit interconnection bonding pad
JPH0221201A (en) * 1988-08-25 1990-01-24 Amada Co Ltd Distance detector for processing machine

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WO1989011161A1 (en) 1989-11-16
GB2229859B (en) 1993-01-06
JPH02119148A (en) 1990-05-07
KR900700217A (en) 1990-08-11
DE3990432C1 (en) 1994-06-23
GB8928848D0 (en) 1990-06-13
GB2229859A (en) 1990-10-03
KR930001265B1 (en) 1993-02-22

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