JPH11118968A - Composite cladding tube for nuclear fuel - Google Patents
Composite cladding tube for nuclear fuelInfo
- Publication number
- JPH11118968A JPH11118968A JP9276904A JP27690497A JPH11118968A JP H11118968 A JPH11118968 A JP H11118968A JP 9276904 A JP9276904 A JP 9276904A JP 27690497 A JP27690497 A JP 27690497A JP H11118968 A JPH11118968 A JP H11118968A
- Authority
- JP
- Japan
- Prior art keywords
- alloy
- composite
- cladding tube
- inner layer
- weight
- 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.)
- Withdrawn
Links
- 238000005253 cladding Methods 0.000 title claims abstract description 58
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 239000003758 nuclear fuel Substances 0.000 title claims description 10
- 229910001093 Zr alloy Inorganic materials 0.000 claims abstract description 39
- 239000000203 mixture Substances 0.000 claims abstract description 31
- 230000007797 corrosion Effects 0.000 claims abstract description 30
- 238000005260 corrosion Methods 0.000 claims abstract description 30
- 238000009792 diffusion process Methods 0.000 claims abstract description 23
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 16
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 14
- 229910000765 intermetallic Inorganic materials 0.000 claims abstract description 12
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 229910052718 tin Inorganic materials 0.000 claims abstract description 5
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 5
- 229910052758 niobium Inorganic materials 0.000 claims abstract 3
- 238000000034 method Methods 0.000 claims 1
- 239000000446 fuel Substances 0.000 abstract description 10
- 229910052742 iron Inorganic materials 0.000 abstract 2
- 239000000470 constituent Substances 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 description 29
- 229910052739 hydrogen Inorganic materials 0.000 description 29
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 26
- 238000005266 casting Methods 0.000 description 16
- 229910045601 alloy Inorganic materials 0.000 description 9
- 239000000956 alloy Substances 0.000 description 9
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 238000007740 vapor deposition Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000001055 reflectance spectroscopy Methods 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 238000004868 gas analysis Methods 0.000 description 2
- 238000001192 hot extrusion Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical class [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 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Landscapes
- Laminated Bodies (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、長期に亘って優
れた機械的特性および耐食性を維持することのできる原
子炉燃料棒用の被覆複合管に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a clad composite pipe for a fuel rod of a nuclear reactor, which can maintain excellent mechanical properties and corrosion resistance for a long period of time.
【０００２】[0002]
【従来の技術】軽水炉の燃料棒はジルカロイ２（ＪＩＳ
Ｈ４７５１ＺｒＮＴ８０２Ｄ、成分組成−Ｆｅ：０．
０７〜０．２０重量％、Ｃｒ：０．０５〜０．１５重量
％、Ｓｎ：１．２〜１．７重量％、Ｎｉ：０．０３〜
０．０８重量％を含有し、残りがＺｒおよび不可避不純
物）もしくはジルカロイ４（ＪＩＳ Ｈ４７５１ＺｒＮ
Ｔ８０４Ｄ、成分組成−Ｆｅ：０．１８〜０．２４重量
％、Ｃｒ：０．０７〜０．１３重量％、Ｓｎ：１．２〜
１．７重量％を含有し、残りがＺｒおよび不可避不純
物）などのジルコニウム合金からなる被覆管の内部にＵ
Ｏ2 燃料ペレットを積重ねて充填し、スプリングでＵＯ
2 燃料ペレットを押圧するようにして被覆管の両端を端
栓で溶接密封することにより組立てられ、炉心に装入し
て使用されている。2. Description of the Related Art LWR fuel rods are made of Zircaloy-2 (JIS).
H4751ZrNT802D, component composition -Fe: 0.
07 to 0.20% by weight, Cr: 0.05 to 0.15% by weight, Sn: 1.2 to 1.7% by weight, Ni: 0.03 to
0.08% by weight, the balance being Zr and unavoidable impurities) or Zircaloy 4 (JIS H4751ZrN).
T804D, component composition-Fe: 0.18 to 0.24 wt%, Cr: 0.07 to 0.13 wt%, Sn: 1.2 to
In a cladding tube containing 1.7% by weight and the balance being made of a zirconium alloy such as Zr and inevitable impurities), U
O 2 fuel pellets are stacked and filled, and UO is
(2) It is assembled by welding and sealing both ends of the cladding tube with end plugs so as to press the fuel pellets, and is used by being charged into the core.
【０００３】[0003]
【発明が解決しようとする課題】近年、電力供給源とし
て原子力発電の比重が高まり、それにつれて原子力発電
所の効率的な運転が求められている。原子炉を高効率的
に運転するために、燃料を従来よりも長期間に亘り使用
することが要求されている。しかし、従来のジルカロイ
２もしくはジルカロイ４で構成される被覆管では耐食性
が十分でなく、燃料を長期に亘って使用し続けると、金
属部厚さの減少や吸収水素による脆化などに伴う機械的
特性の劣化が促進される可能性があった。In recent years, the specific gravity of nuclear power generation has increased as a power supply source, and accordingly, there has been a demand for efficient operation of nuclear power plants. In order to operate a nuclear reactor with high efficiency, it is required to use fuel for a longer period than before. However, conventional cladding tubes made of Zircaloy 2 or Zircaloy 4 do not have sufficient corrosion resistance, and if the fuel is used for a long period of time, the mechanical properties associated with a decrease in the thickness of the metal part and embrittlement due to absorbed hydrogen are caused. Deterioration of characteristics could be accelerated.
【０００４】この従来の燃料棒を構成するジルカロイ２
もしくはジルカロイ４被覆管が長期に亘って十分な耐食
性および優れた機械的特性が得られない原因の一つとし
て、軽水炉の燃料棒を構成するジルカロイ２もしくはジ
ルカロイ４被覆管は、原子炉内において４００〜５００
℃の高温水もしくは高温水蒸気に高圧でさらされて表面
が酸化し、その酸化によって発生する水素を吸収してさ
らに酸化が促進され、また水素化により脆化して強度が
低下することによることが知られている。この酸化およ
び水素吸収による脆化を防止するために、ジルカロイ２
もしくはジルカロイ４被覆管の表面に耐食性に優れた正
方晶ジルコニア外皮膜および耐水素透過性に優れた単斜
晶ジルコニア内皮膜の二層構造からなる酸化皮膜を形成
し、強度および耐食性を向上させる手段が提供されてい
るが（特開平４−２８５１５１号公報参照）十分な効果
が得られていない。[0004] Zircaloy 2 constituting this conventional fuel rod
Alternatively, one of the reasons that the Zircaloy-4 cladding tube cannot obtain sufficient corrosion resistance and excellent mechanical properties over a long period of time is that the Zircaloy-2 or Zircaloy-4 cladding tube constituting the fuel rod of the light water reactor is 400 kg ~ 500
It is known that the surface is oxidized when exposed to high temperature water or high temperature steam at a high temperature of ℃, and the hydrogen generated by the oxidation is absorbed to further promote the oxidation, and that the strength is reduced by embrittlement due to hydrogenation. Have been. To prevent embrittlement due to oxidation and hydrogen absorption, Zircaloy 2
Alternatively, a means for improving the strength and corrosion resistance by forming an oxide film having a two-layer structure of a tetragonal zirconia outer film having excellent corrosion resistance and a monoclinic zirconia inner film having excellent hydrogen permeation resistance on the surface of a Zircaloy-4 clad tube. (See Japanese Patent Application Laid-Open No. 4-285151), but a sufficient effect has not been obtained.
【０００５】[0005]
【課題を解決するための手段】そこで、本発明者等は水
素吸収による脆化を起こさず、さらに耐食性に優れた被
覆管を得るべく研究を行っていたところ、（ａ）図１に
示されるように、Ｚｒ合金からなる被覆管の外層部１と
内層部２の間に、水素吸蔵合金であるＺｒＭx （ただ
し、Ｍ：Ｃｒ、ＭｎおよびＶの内の１種または２種以
上、ｘ：１．３〜２．５）の成分組成からなる金属間化
合物を２〜１００容量％含む中間拡散層３を介在させて
複合管とし、これを原子炉の燃料棒の被覆管として使用
すると、被覆管の外層部表面から拡散浸透した水素は水
素吸蔵合金を多量に含む中間拡散層でトラップされ、内
層部への拡散が抑えられて内層部の水素吸収による脆化
を抑えることができ、従って、長期に亘って原子炉燃料
被覆管に要求される機械的特性を内層部によって維持す
ることができる、（ｂ）公知のＺｒ合金（例えば、ジル
カロイ４）の成分組成範囲内であっても、外層部１と内
層部２の組成範囲を少し変えて、被覆管の外層部１を内
層部２よりも耐食性に優れた組成とし、内層部２を外層
部１よりも高強度を有する組成とし、この耐食性に優れ
たＺｒ合金で構成した外層部１と高強度を有するＺｒ合
金で構成した内層部２の間に、水素吸蔵合金であるＺｒ
Ｍx （ただし、Ｍ：Ｃｒ、ＭｎおよびＶの内の１種また
は２種以上、ｘ：１．３〜２．５）からなる金属間化合
物を２〜１００容量％含む中間拡散層３を介在させる
と、耐食性は主として外層部１のＺｒ合金で確保され、
一方、強度は主として内層部２のＺｒ合金で確保され、
外層部１のＺｒ合金が水素を吸収しても、吸収した水素
は中間拡散層３でトラップされ、内層部２への拡散が抑
えられて内層部２の水素吸収による脆化を抑えることが
でき、従って、一層長期に亘って優れた耐食性および機
械的特性を維持することができる、（ｃ）前記複合管の
外層部を耐食性に優れたＦｅ：０．１８〜０．２４重量
％、Ｃｒ：０．０７〜０．１３重量％、Ｓｎ：０．０５
〜０．５重量％、Ｎｂ：０．０５〜１．０重量％を含有
し、残りがＺｒおよび不可避不純物からなる組成のＺｒ
合金で構成し、前記複合管の内層部を高強度を有するＦ
ｅ：０．１８〜０．２４重量％、Ｃｒ：０．０７〜０．
１３重量％、Ｓｎ：０．５超〜１．１５重量％、Ｎｂ：
０．０５〜１．０重量％を含有し、残りがＺｒおよび不
可避不純物からなる組成のＺｒ合金で構成し、前記複合
管の外層部１と内層部２の間に、水素吸蔵合金であるＺ
ｒＭx （ただし、Ｍ：Ｃｒ、ＭｎおよびＶの内の１種ま
たは２種以上、ｘ：１．３〜２．５）からなる金属間化
合物を２〜１００容量％含む中間拡散層３を介在させる
ことが一層好ましい、などの研究結果が得られたのであ
る。The inventors of the present invention have conducted research to obtain a cladding tube which does not cause embrittlement due to hydrogen absorption and has excellent corrosion resistance. (A) FIG. As described above, between the outer layer 1 and the inner layer 2 of the cladding tube made of a Zr alloy, one or more of ZrM x (where M: Cr, Mn, and V, x: When a composite pipe is formed by interposing an intermediate diffusion layer 3 containing 2 to 100% by volume of an intermetallic compound having a component composition of 1.3 to 2.5) and this is used as a cladding pipe for a fuel rod of a nuclear reactor, Hydrogen diffused and infiltrated from the outer layer surface of the tube is trapped in the intermediate diffusion layer containing a large amount of the hydrogen storage alloy, diffusion to the inner layer is suppressed, and embrittlement due to hydrogen absorption in the inner layer can be suppressed. Machines required for reactor fuel cladding for a long time (B) Even if it is within the component composition range of a known Zr alloy (for example, Zircaloy 4), the composition range of the outer layer portion 1 and the inner layer portion 2 is slightly changed. The outer layer portion 1 of the cladding tube has a composition more excellent in corrosion resistance than the inner layer portion 2, the inner layer portion 2 has a composition having a higher strength than the outer layer portion 1, and the outer layer portion 1 made of a Zr alloy excellent in the corrosion resistance. Between the inner layer portion 2 made of a strong Zr alloy and Zr which is a hydrogen storage alloy
Intermediate diffusion layer 3 containing 2 to 100% by volume of an intermetallic compound consisting of M x (where M: one or more of Cr, Mn and V, x: 1.3 to 2.5) Then, the corrosion resistance is mainly secured by the Zr alloy of the outer layer portion 1,
On the other hand, the strength is mainly secured by the Zr alloy of the inner layer part 2,
Even if the Zr alloy in the outer layer portion 1 absorbs hydrogen, the absorbed hydrogen is trapped in the intermediate diffusion layer 3 and diffusion into the inner layer portion 2 is suppressed, so that embrittlement due to hydrogen absorption in the inner layer portion 2 can be suppressed. Therefore, it is possible to maintain excellent corrosion resistance and mechanical properties for a longer period of time. (C) The outer layer of the composite pipe has a corrosion resistance of Fe: 0.18 to 0.24% by weight, Cr: 0.07 to 0.13% by weight, Sn: 0.05
0.5% by weight, Nb: 0.05-1.0% by weight, the balance being Zr having a composition comprising Zr and unavoidable impurities.
Alloy, and the inner layer of the composite pipe has a high strength of F
e: 0.18-0.24% by weight, Cr: 0.07-0.
13% by weight, Sn: more than 0.5 to 1.15% by weight, Nb:
The composite pipe is composed of a Zr alloy having a composition of 0.05 to 1.0% by weight, with the balance consisting of Zr and unavoidable impurities, between the outer layer 1 and the inner layer 2 of the composite pipe.
Intermediate diffusion layer 3 containing 2 to 100% by volume of an intermetallic compound consisting of rM x (where M: one or more of Cr, Mn and V, x: 1.3 to 2.5) Research results such as more preferable were obtained.
【０００６】この発明は、この研究結果に基づいて成さ
れたものであって、（１）Ｚｒ合金からなる外層部と内
層部の間に、ＺｒＭx （ただし、Ｍ：Ｃｒ、Ｍｎおよび
Ｖの内の１種または２種以上、ｘ：１．３〜２．５）の
成分組成からなる金属間化合物を２〜１００容量％含む
中間拡散層を介在させてなる原子炉燃料用複合被覆管、
（２）耐食性に優れたＺｒ合金からなる外層部と高強度
を有するＺｒ合金からなる内層部の間に、ＺｒＭx （た
だし、Ｍ：Ｃｒ、ＭｎおよびＶの内の１種または２種以
上、ｘ：１．３〜２．５）の成分組成からなる金属間化
合物を２〜１００容量％含む中間拡散層を介在させてな
る原子炉燃料用複合被覆管、（３）前記耐食性に優れた
Ｚｒ合金からなる外層部は、Ｆｅ：０．１８〜０．２４
重量％、Ｃｒ：０．０７〜０．１３重量％、Ｓｎ：０．
０５〜０．５重量％、Ｎｂ：０．０５〜１．０重量％を
含有し、残りがＺｒおよび不可避不純物からなる組成を
有し、前記高強度を有するＺｒ合金からなる内層部は、
Ｆｅ：０．１８〜０．２４重量％、Ｃｒ：０．０７〜
０．１３重量％、Ｓｎ：０．５超〜１．１５重量％、Ｎ
ｂ：０．０５〜１．０重量％を含有し、残りがＺｒおよ
び不可避不純物からなる組成を有する前記（２）記載の
原子炉燃料用複合被覆管、に特徴を有するものである。The present invention has been made based on the results of this research. (1) Between the outer layer portion and the inner layer portion made of a Zr alloy, ZrM x (where M: Cr, Mn and V One or more of these, x: 1.3 to 2.5) a composite cladding tube for nuclear reactor fuel with an intermediate diffusion layer containing 2 to 100% by volume of an intermetallic compound having a component composition of
(2) Between an outer layer portion made of a Zr alloy having excellent corrosion resistance and an inner layer portion made of a Zr alloy having high strength, ZrM x (however, one or more of M: Cr, Mn and V, x: a composite cladding tube for a nuclear reactor fuel having an intermediate diffusion layer containing 2 to 100% by volume of an intermetallic compound having a component composition of 1.3 to 2.5), (3) Zr excellent in corrosion resistance The outer layer portion made of the alloy has Fe: 0.18 to 0.24.
Wt%, Cr: 0.07 to 0.13 wt%, Sn: 0.
The inner layer portion comprising a high-strength Zr alloy having a composition of 0.5 to 0.5% by weight, Nb: 0.05 to 1.0% by weight, and a balance of Zr and unavoidable impurities,
Fe: 0.18 to 0.24% by weight, Cr: 0.07 to
0.13% by weight, Sn: more than 0.5 to 1.15% by weight, N
b: The composite cladding tube for a nuclear reactor fuel according to the above (2), which has a composition containing 0.05 to 1.0% by weight and a balance of Zr and unavoidable impurities.
【０００７】この発明の原子炉燃料用複合被覆管の中間
拡散層は、水素吸蔵能の高い金属間化合物であるＺｒＭ
x が少なくとも２容量％含まれていれば外層部から拡散
してきた水素をトラップして内層部への拡散を抑えるこ
とができる。しかし、中間拡散層に含まれる金属間化合
物のＺｒＭx のｘの値がｘ＜１．３およびｘ＞２．５で
は水素吸蔵能が少さくなって水素の内層部への拡散を抑
えることができない。従って、ＺｒＭx におけるｘを
１．３〜２．５に限定した。ｘの一層好ましい範囲は
ｘ：１．８〜２．２である。The intermediate diffusion layer of the composite cladding tube for nuclear fuel of the present invention is made of ZrM which is an intermetallic compound having a high hydrogen storage capacity.
If x is contained at least 2% by volume, hydrogen diffused from the outer layer portion can be trapped and diffusion into the inner layer portion can be suppressed. However, when the value of x of ZrM x of the intermetallic compound contained in the intermediate diffusion layer is x <1.3 and x> 2.5, the hydrogen storage capacity is reduced, and the diffusion of hydrogen to the inner layer can be suppressed. Can not. Therefore, x in ZrMx was limited to 1.3 to 2.5. The more preferable range of x is x: 1.8 to 2.2.
【０００８】[0008]
実施例１ 原料として、９９．９％以上の純度を有するＺｒスポン
ジ、いずれも９９．９％以上の純度を有するＳｎ粒、Ｆ
ｅ粒およびＣｒ粒を用意し、これら原料を配合し、混合
した後、圧粉体にプレス成形した。得られた圧粉体を真
空アーク炉にて溶解し、機械加工により表１〜表４に示
される内層部および外層部の成分組成と同じ成分組成を
有する外径：１７６mm、内径：４０mm、肉厚：６８mmの
寸法を有する中空の内層部材鋳造ビレットおよび外径：
２００mm、内径：１７６mm、肉厚：１２mmの寸法を有す
る中空の外層部材鋳造ビレットを製造した。Example 1 As raw materials, Zr sponge having a purity of 99.9% or more, Sn particles having a purity of 99.9% or more, and F
e particles and Cr particles were prepared, and these materials were blended and mixed, and then pressed into a green compact. The obtained green compact is melted in a vacuum arc furnace, and has the same component composition as the inner layer portion and the outer layer portion shown in Tables 1 to 4 by machining to have an outer diameter of 176 mm, an inner diameter of 40 mm, and meat. Thickness: hollow inner member cast billet with dimensions of 68 mm and outer diameter:
A hollow outer layer member cast billet having dimensions of 200 mm, an inner diameter of 176 mm, and a wall thickness of 12 mm was produced.
【０００９】本発明複合被覆管１〜７では内層部材鋳造
ビレットおよび外層部材鋳造ビレットの合金組成はいず
れもジルカロイ−４の成分組成の範囲内に含まれ、ほぼ
同一の組成を有している。本発明複合被覆管８〜１４で
は内層部材鋳造ビレットおよび外層部材鋳造ビレットの
Ｚｒ合金に含まれるＳｎの含有量を少し変えて、内層部
材鋳造ビレットを外層部材鋳造ビレットよりも強度を有
する組成のＺｒ合金で構成し、外層部材鋳造ビレットを
内層部材鋳造ビレットよりも耐食性に優れた組成のＺｒ
合金で構成している。In the composite cladding tubes 1 to 7 of the present invention, the alloy compositions of the inner layer member billet and the outer layer member billet are both within the range of the component composition of Zircaloy-4, and have substantially the same composition. In the composite cladding tubes 8 to 14 of the present invention, the content of Sn contained in the Zr alloy of the inner layer member casting billet and the outer layer member casting billet is slightly changed so that the inner layer member casting billet has a composition having a strength higher than that of the outer layer member casting billet. Zr having a composition composed of an alloy and having an outer layer member cast billet having a higher corrosion resistance than the inner layer member cast billet.
It is composed of an alloy.
【００１０】これら鋳造ビレットの表面研削を行ったの
ち前記内層部材鋳造ビレットの外表面に表１〜表４に示
される厚さのＣｒ蒸着層、Ｍｎ蒸着層、Ｖ蒸着層、Ｃｒ
およびＭｎの複合蒸着層、ＣｒおよびＶの複合蒸着層、
ＭｎおよびＶの複合蒸着層、Ｃｒ、ＭｎおよびＶの複合
蒸着層を形成し、これら蒸着層を有する内層部材鋳造ビ
レットを前記中空の外層部材鋳造ビレットに挿入し、端
部を溶接後、６００〜７００℃の範囲内の所定の温度で
熱間押出しすることにより複合素管を作製した。この複
合素管を用い、ピルガー圧延および真空熱処理（温度：
５８０〜７８０℃）を繰り返すことにより最終的に外
径：９．５ｍｍ、肉厚：０．５ｍｍの寸法を有する外層
部、中間拡散層および内層部からなる本発明複合被覆管
１〜１４を作製し、ついで４５０〜４９０℃の範囲内の
所定の温度で歪み取り焼鈍を行った。After the surface of the cast billet is ground, a Cr-deposited layer, a Mn-deposited layer, a V-deposited layer,
And Mn, a composite deposited layer of Cr and V,
Forming a composite vapor deposition layer of Mn and V, a composite vapor deposition layer of Cr, Mn and V, inserting the inner layer member casting billet having these vapor deposition layers into the hollow outer layer member casting billet, welding the ends, and A composite tube was prepared by hot extrusion at a predetermined temperature in the range of 700 ° C. Pilger rolling and vacuum heat treatment (temperature:
580 to 780 ° C.) to finally produce the composite cladding tubes 1 to 14 of the present invention comprising an outer layer, an intermediate diffusion layer and an inner layer having an outer diameter of 9.5 mm and a thickness of 0.5 mm. Then, strain relief annealing was performed at a predetermined temperature in the range of 450 to 490 ° C.
【００１１】得られた本発明複合被覆管１〜１４を切断
し、断面に現れている中間拡散層について透過電子顕微
鏡観察およびエネルギー分散型Ｘ線解析することにより
中間拡散層に含まれる金属間化合物相の同定およびその
体積率を測定し、その結果を表１〜表４に示した。The obtained composite cladding tubes 1 to 14 of the present invention are cut, and the interdiffusion layer appearing in the cross section is observed by transmission electron microscopy and energy dispersive X-ray analysis to obtain an intermetallic compound contained in the intermediate diffusion layer. The identification of the phase and the volume ratio thereof were measured, and the results are shown in Tables 1 to 4.
【００１２】さらに、比較のために、中間拡散層を有さ
ない外径：９．５mm、肉厚：０．５mmの寸法のジルカロ
イ−４からなる単管を用意し、これら単管の両端を端栓
で閉じたのち、温度：４００℃の大気中に４時間保持
し、管外面に約２μｍ厚さの初期酸化皮膜を形成するこ
とにより耐水素透過特性を有する従来被覆管Ａを製造し
た。また、内層部材鋳造ビレットおよび外層部材鋳造ビ
レットのＺｒ合金に含まれるＳｎの含有量を少し変え
て、内層部材鋳造ビレットを外層部材鋳造ビレットより
も強度を有する組成のＺｒ合金で構成し、外層部材鋳造
ビレットを内層部材鋳造ビレットよりも耐食性に優れた
組成のＺｒ合金で構成した複合管を用意し、この複合管
の両端を端栓で閉じたのち、温度：４００℃の大気中に
４時間保持し、管外面に約２μｍ厚さの初期酸化皮膜を
形成することにより耐水素透過特性を有する従来被覆管
Ｂを製造した。Further, for comparison, single tubes made of Zircaloy-4 having an outer diameter of 9.5 mm and a wall thickness of 0.5 mm without an intermediate diffusion layer were prepared, and both ends of these single tubes were connected. After closing with an end plug, it was kept in the air at a temperature of 400 ° C. for 4 hours, and an initial oxide film having a thickness of about 2 μm was formed on the outer surface of the tube, thereby producing a conventional coated tube A having a hydrogen permeation resistance. Further, the content of Sn contained in the Zr alloy of the inner layer member casting billet and the outer layer member casting billet is slightly changed so that the inner layer member casting billet is made of a Zr alloy having a composition stronger than the outer layer member casting billet. A composite pipe made of a Zr alloy having a composition more excellent in corrosion resistance than the inner layer member cast billet is prepared, and both ends of the composite pipe are closed with end plugs, and then held in the air at a temperature of 400 ° C. for 4 hours. Then, a conventional cladding tube B having hydrogen permeation resistance was manufactured by forming an initial oxide film having a thickness of about 2 μm on the outer surface of the tube.
【００１３】両端をジルカロイ−４製の端栓で閉じた本
発明複合被覆管１〜１４および従来被覆管ＡおよびＢ
を、オートクレーブ装置に装入し、温度：３６０℃、１
９０気圧の高温高圧水中に６００日保持することにより
腐食試験を実施し、腐食試験前後の本発明複合被覆管１
〜１４および従来被覆管ＡおよびＢの表面酸化膜厚さを
ＦＴＩＲ（フーリエ変換赤外反射分光法）により検出
し、その結果を表１〜表４に示した。さらに腐食試験後
の本発明複合被覆管１〜１４の外表面酸化膜および外層
部を機械加工除去し、内層部合金中の水素吸収量をガス
分析により測定し、その結果を表１〜表４に示した。ま
た、同様に従来被覆管Ａの外面側を除去し、内面側の水
素吸収量を測定し、さらに従来被覆管Ｂの外表面酸化膜
および外層部を機械加工除去し、内層部合金中の水素吸
収量を測定し、これらの結果を表２および表４にそれぞ
れ示した。なお、ＦＴＩＲ（フーリエ変換赤外反射分光
法）によるジルコニウム合金の酸化膜厚さの測定につい
ては、文献「Fourier trannsform infrared refriction
（ＦＴＩＲ）spectroscopy ofcorrosion films on irra
diated zirukonium films ］」に詳述されている。The composite cladding tubes 1 to 14 of the present invention and the conventional cladding tubes A and B, both ends of which are closed with end plugs made of Zircaloy-4
Was charged into an autoclave, and the temperature: 360 ° C., 1
A corrosion test was carried out by holding in a high-pressure water at 90 atm for 600 days, and the composite cladding tube 1 of the present invention before and after the corrosion test was performed.
-14 and the surface oxide film thickness of the conventional cladding tubes A and B were detected by FTIR (Fourier transform infrared reflection spectroscopy), and the results are shown in Tables 1 to 4. Further, the outer surface oxide film and the outer layer of the composite cladding tubes 1 to 14 of the present invention after the corrosion test were machined and removed, and the amount of hydrogen absorbed in the inner layer alloy was measured by gas analysis. It was shown to. Similarly, the outer surface side of the conventional cladding tube A is removed, the amount of hydrogen absorbed on the inner surface side is measured, the outer surface oxide film and the outer layer portion of the conventional cladding tube B are further machined and removed, and hydrogen in the inner layer portion alloy is removed. The absorption was measured, and the results are shown in Tables 2 and 4, respectively. The measurement of the oxide film thickness of a zirconium alloy by FTIR (Fourier transform infrared reflection spectroscopy) is described in the literature "Fourier trannsform infrared refriction".
(FTIR) spectroscopy ofcorrosion films on irra
diated zirukonium films]].
【００１４】[0014]
【表１】 [Table 1]
【００１５】[0015]
【表２】 [Table 2]
【００１６】[0016]
【表３】 [Table 3]
【００１７】[0017]
【表４】 [Table 4]
【００１８】表１〜表４に示される結果から、本発明複
合被覆管１〜７は、これらとほぼ同一組成の単管である
従来被覆管Ａに比べて、酸化膜の厚さがほぼ同じ値を示
しているところから腐食増量がほぼ同じであるが、本発
明複合被覆管１〜７の内層部に含まれる吸収水素量は、
従来被覆管Ａの内面に近い部分の吸収水素量に比べて格
段に少ない。同様に本発明複合被覆管８〜１４は、これ
らとほぼ同一組成の複合管である従来被覆管Ｂに比べ
て、酸化膜の厚さがほぼ同じ値を示しているところから
腐食増量がほぼ同じであるが、本発明複合被覆管８〜１
４の内層部に含まれる吸収水素量は、従来被覆管Ｂの内
層部の吸収水素量に比べて格段に少ない。従って、本発
明複合被覆管１〜１４は内層部の水素脆化が抑制され、
優れた機械的特性を長期に亘って維持することが可能で
あることがわかる。From the results shown in Tables 1 to 4, the composite cladding tubes 1 to 7 of the present invention have substantially the same oxide film thickness as the conventional cladding tube A which is a single tube having almost the same composition. Values indicate that the corrosion increase is almost the same, but the amount of absorbed hydrogen contained in the inner layer of the composite cladding tubes 1 to 7 of the present invention is:
Conventionally, the amount of absorbed hydrogen in the portion near the inner surface of the cladding tube A is much smaller. Similarly, the composite cladding tubes 8 to 14 of the present invention have almost the same increase in corrosion since the thickness of the oxide film is almost the same as that of the conventional cladding tube B, which is a composite tube having almost the same composition. However, the composite cladding tube of the present invention 8-1
The amount of absorbed hydrogen contained in the inner layer of No. 4 is much smaller than that of the inner layer of the conventional cladding tube B. Therefore, in the present composite cladding tubes 1 to 14, hydrogen embrittlement of the inner layer portion is suppressed,
It can be seen that excellent mechanical properties can be maintained for a long time.
【００１９】実施例２ 原料として、いずれも９９．９％以上の純度を有するＺ
ｒスポンジ、Ｓｎ粒、Ｆｅ粒、Ｃｒ粒およびＮｂ粒を用
意し、これら原料を配合し、混合した後、圧粉体にプレ
ス成形した。得られた圧粉体を真空アーク炉にて溶解
し、機械加工によって表５〜表８に示される成分組成を
有し、外径：１７６mm、内径：４０mm、肉厚：６８mmの
寸法を有する中空の内層部材鋳造ビレットおよび外径：
２００mm、内径：１７６mm、肉厚：１２mmの寸法を有す
る中空の外層部材鋳造ビレットを製造した。Example 2 As a raw material, Z having a purity of 99.9% or more was used.
r sponge, Sn particles, Fe particles, Cr particles, and Nb particles were prepared, these raw materials were blended, mixed, and then pressed into a green compact. The obtained green compact is melted in a vacuum arc furnace, and has a component composition shown in Tables 5 to 8 by machining, and has a hollow having an outer diameter of 176 mm, an inner diameter of 40 mm, and a wall thickness of 68 mm. Inner layer cast billet and outer diameter:
A hollow outer layer member cast billet having dimensions of 200 mm, an inner diameter of 176 mm, and a wall thickness of 12 mm was produced.
【００２０】内層部材鋳造ビレットおよび外層部材鋳造
ビレットのＺｒ合金の組成は、内層部材鋳造ビレットお
よび外層部材鋳造ビレットのＺｒ合金に含まれるＳｎの
含有量を少し変えて、内層部材鋳造ビレットを外層部材
鋳造ビレットよりも高強度のＺｒ合金で構成し、外層部
材鋳造ビレットを内層部材鋳造ビレットよりも耐食性に
優れたＺｒ合金で構成している。The composition of the Zr alloy of the inner member casting billet and the outer layer member casting billet is changed by slightly changing the content of Sn contained in the Zr alloy of the inner layer member casting billet and the outer layer member casting billet. The outer layer member cast billet is made of a Zr alloy having higher corrosion resistance than the inner layer member cast billet.
【００２１】これら鋳造ビレットの表面研削を行ったの
ち前記内層部材鋳造ビレットの外表面に表５〜表８に示
される厚さのＣｒ蒸着層、Ｍｎ蒸着層、Ｖ蒸着層、Ｃｒ
およびＭｎの複合蒸着層、ＣｒおよびＶの複合蒸着層、
ＭｎおよびＶの複合蒸着層、Ｃｒ、ＭｎおよびＶの複合
蒸着層を形成し、これら蒸着層を有する内層部材鋳造ビ
レットを前記中空の外層部材鋳造ビレットに挿入し、端
部を溶接後、温度：６００〜７００℃の範囲で熱間押出
しすることにより複合素管を作製した。この複合素管を
用い、ピルガー圧延および真空熱処理（温度：５８０〜
７８０℃）を繰り返すことにより最終的に外径：９．５
ｍｍ、肉厚：０．５ｍｍの寸法を有する外層部、中間拡
散層および内層部からなる本発明複合被覆管１５〜２８
を作製し、ついで温度：４５０〜４９０℃で歪み取り焼
鈍を行った。After the surface of the cast billet was ground, a Cr-deposited layer, a Mn-deposited layer, a V-deposited layer, and a Cr-deposited layer having a thickness shown in Tables 5 to 8 were formed on the outer surface of the inner layer member cast billet.
And Mn, a composite deposited layer of Cr and V,
After forming a composite vapor deposition layer of Mn and V and a composite vapor deposition layer of Cr, Mn and V, inserting the inner layer member casting billet having these vapor deposition layers into the hollow outer layer member casting billet, welding the ends, and then heating the billet. A composite shell was produced by hot extrusion in the range of 600 to 700 ° C. Using this composite tube, Pilger rolling and vacuum heat treatment (temperature: 580 to 580)
780 ° C.) to finally obtain an outer diameter of 9.5.
mm, the present composite cladding tube 15-28 comprising an outer layer, an intermediate diffusion layer, and an inner layer having a thickness of 0.5 mm.
Was prepared and then subjected to strain relief annealing at a temperature of 450 to 490 ° C.
【００２２】得られた本発明複合被覆管１５〜２８を切
断し、断面に現れている中間拡散層について透過電子顕
微鏡観察およびエネルギー分散型Ｘ線解析することによ
り中間拡散層に含まれる金属間化合物相の同定およびそ
の体積率を測定し、その結果を表５〜表８に示した。The obtained composite cladding tubes 15 to 28 of the present invention are cut, and the intermediate diffusion layer appearing in the cross section is observed by a transmission electron microscope and energy dispersive X-ray analysis to obtain an intermetallic compound contained in the intermediate diffusion layer. The identification of the phase and the volume ratio thereof were measured, and the results are shown in Tables 5 to 8.
【００２３】一方、比較のために、本発明複合被覆管１
５〜２１とほぼ同じ構成からなる複合管および本発明複
合被覆管２２〜２８とほぼ同じ構成からなる複合管を用
意し、実施例１の従来被覆管ＡおよびＢと同様に複合管
の両端を端栓で閉じたのち、温度：４００℃の大気中に
４時間保持し、管外面に約２μｍ厚さの初期酸化皮膜を
形成することにより耐水素透過特性を有する従来被覆管
ＣおよびＤを製造した。On the other hand, for comparison, the composite cladding tube 1 of the present invention was used.
A composite pipe having substantially the same configuration as the composite pipes 5 to 21 and a composite pipe having the same configuration as the composite cladding pipes 22 to 28 of the present invention are prepared. After closing with an end plug, the tube is kept in the air at a temperature of 400 ° C. for 4 hours, and an initial oxide film having a thickness of about 2 μm is formed on the outer surface of the tube to produce conventional clad tubes C and D having a resistance to hydrogen permeation. did.
【００２４】両端を端栓で閉じた本発明複合被覆管１５
〜２８および従来被覆管ＣおよびＤを、オートクレーブ
装置に装入し、温度：３６０℃、１９０気圧の高温高圧
水中に６００日保持することにより腐食試験を実施し、
腐食試験前後の表面酸化膜厚さをＦＴＩＲ（フーリエ変
換赤外反射分光法）により検出して腐食増量を求め、そ
の結果を表５〜表８に示した。さらに腐食試験後の本発
明複合被覆管１５〜２８および従来被覆管ＣおよびＤの
内層部の吸収水素量をガス分析により測定し、その結果
を表５〜表８に示した。The composite cladding tube 15 of the present invention having both ends closed with end plugs
２８28 and conventional cladding tubes C and D were charged into an autoclave apparatus, and subjected to a corrosion test by maintaining them in high-temperature high-pressure water at a temperature of 360 ° C. and 190 atm for 600 days.
The thickness of the surface oxide film before and after the corrosion test was detected by FTIR (Fourier transform infrared reflection spectroscopy) to determine the increase in corrosion, and the results are shown in Tables 5 to 8. Further, the amount of hydrogen absorbed in the inner layers of the composite cladding tubes 15 to 28 of the present invention and the conventional cladding tubes C and D after the corrosion test was measured by gas analysis, and the results are shown in Tables 5 to 8.
【００２５】[0025]
【表５】 [Table 5]
【００２６】[0026]
【表６】 [Table 6]
【００２７】[0027]
【表７】 [Table 7]
【００２８】[0028]
【表８】 [Table 8]
【００２９】表５〜表８に示される結果から、本発明複
合被覆管１５〜２８は、表６および表８に示した従来被
覆管ＣおよびＤに比べて酸化膜の厚さがほぼ同じ値を示
しているところから腐食増量がほぼ同じであるが、本発
明複合被覆管１５〜２８の内層部に含まれる吸収水素量
は、従来被覆管ＣおよびＤの内層部に含まれる吸収水素
量に比べて格段に少ないところから、本発明複合被覆管
１５〜２８は優れた機械的特性を内層部によって維持で
きることが分かる。From the results shown in Tables 5 to 8, the composite cladding tubes 15 to 28 of the present invention have substantially the same oxide film thickness as those of the conventional cladding tubes C and D shown in Tables 6 and 8. Shows that the increase in corrosion is almost the same, but the amount of absorbed hydrogen contained in the inner layers of the composite cladding tubes 15 to 28 of the present invention is smaller than the amount of absorbed hydrogen contained in the inner layers of the conventional cladding tubes C and D. Compared to the markedly smaller portions, it is understood that the composite cladding tubes 15 to 28 of the present invention can maintain excellent mechanical properties by the inner layer portion.
【００３０】[0030]
【発明の効果】上述のように、この発明の複合被覆管
は、長期に亘って優れた耐食性および機械的特性を維持
することができるところから、従来よりも信頼性の高い
原子炉燃料棒を提供することができ、さらに原子炉の高
効率運転を長期に亘って行うことのできるなど、原子力
産業の発展に大いに貢献しうるものである。As described above, since the composite cladding tube of the present invention can maintain excellent corrosion resistance and mechanical properties over a long period of time, a more reliable reactor fuel rod than before can be obtained. It can greatly contribute to the development of the nuclear industry, for example, by being able to provide high-efficiency operation of a nuclear reactor over a long period of time.
【図１】この発明の複合被覆管の断面説明図である。FIG. 1 is an explanatory sectional view of a composite cladding tube of the present invention.
１ 外層部 ２ 内層部 ３ 中間拡散層 1 outer layer 2 inner layer 3 intermediate diffusion layer
Claims (3)
に、ＺｒＭx （ただし、Ｍ：Ｃｒ、ＭｎおよびＶの内の
１種または２種以上、ｘ：１．３〜２．５）の成分組成
からなる金属間化合物を２〜１００容量％含む中間拡散
層を介在させてなることを特徴とする原子炉燃料用複合
被覆管。A ZrM x (wherein, one or more of M, Cr, Mn and V, x: 1.3 to 2.5) is provided between an outer layer portion and an inner layer portion made of a Zr alloy. A composite cladding tube for a nuclear reactor fuel comprising an intermediate diffusion layer containing 2 to 100% by volume of an intermetallic compound having the following composition:
と高強度を有するＺｒ合金からなる内層部の間に、Ｚｒ
Ｍx （ただし、Ｍ：Ｃｒ、ＭｎおよびＶの内の１種また
は２種以上、ｘ：１．３〜２．５）の成分組成からなる
金属間化合物を２〜１００容量％含む中間拡散層を介在
させてなることを特徴とする原子炉燃料用複合被覆管。2. The method according to claim 1, wherein a Zr alloy is provided between an outer layer made of a Zr alloy having excellent corrosion resistance and an inner layer made of a Zr alloy having high strength.
An intermediate diffusion layer containing 2 to 100% by volume of an intermetallic compound having a component composition of M x (where M: one or more of Cr, Mn and V, x: 1.3 to 2.5) A composite cladding tube for nuclear reactor fuel, characterized by interposing a cladding.
層部は、Ｆｅ：０．１８〜０．２４重量％、Ｃｒ：０．
０７〜０．１３重量％、Ｓｎ：０．０５〜０．５重量
％、Ｎｂ：０．０５〜１．０重量％を含有し、残りがＺ
ｒおよび不可避不純物からなる組成を有するＺｒ合金で
構成されており、 前記高強度を有するＺｒ合金からなる内層部は、Ｆｅ：
０．１８〜０．２４重量％、Ｃｒ：０．０７〜０．１３
重量％、Ｓｎ：０．５超〜１．１５重量％、Ｎｂ：０．
０５〜１．０重量％を含有し、残りがＺｒおよび不可避
不純物からなる組成を有するＺｒ合金で構成されている
ことを特徴とする請求項２記載の原子炉燃料用複合被覆
管。3. The outer layer portion made of a Zr alloy having excellent corrosion resistance has a Fe content of 0.18 to 0.24% by weight and a Cr content of 0.1%.
07-0.13% by weight, Sn: 0.05-0.5% by weight, Nb: 0.05-1.0% by weight, the balance being Z
and a Zr alloy having a composition consisting of r and unavoidable impurities, and the inner layer portion made of the Zr alloy having high strength includes Fe:
0.18 to 0.24% by weight, Cr: 0.07 to 0.13
Wt%, Sn: more than 0.5 to 1.15 wt%, Nb: 0.
3. The composite cladding tube for a nuclear reactor fuel according to claim 2, wherein the composite cladding tube contains 0.5 to 1.0% by weight and the remainder is made of a Zr alloy having a composition comprising Zr and unavoidable impurities.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9276904A JPH11118968A (en) | 1997-10-09 | 1997-10-09 | Composite cladding tube for nuclear fuel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9276904A JPH11118968A (en) | 1997-10-09 | 1997-10-09 | Composite cladding tube for nuclear fuel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11118968A true JPH11118968A (en) | 1999-04-30 |
Family
ID=17576016
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9276904A Withdrawn JPH11118968A (en) | 1997-10-09 | 1997-10-09 | Composite cladding tube for nuclear fuel |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11118968A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006265725A (en) * | 2005-03-23 | 2006-10-05 | Westinghouse Electric Co Llc | Zirconium alloy improved in corrosion resistance and production method of zirconium alloy improved in corrosion resistance |
| KR100709389B1 (en) | 2003-02-28 | 2007-04-20 | 학교법인 한양학원 | Manufacturing method of high corrosion resistant zirconium alloy fuel cladding tube |
| CN101512671B (en) | 2006-08-24 | 2013-04-10 | 威斯丁豪斯电气瑞典有限公司 | Water reactor fuel cladding tube |
| JPWO2019093370A1 (en) * | 2017-11-10 | 2020-12-03 | 株式会社フェローテックマテリアルテクノロジーズ | Ceramics, probe guide parts, probe cards and sockets for package inspection |
-
1997
- 1997-10-09 JP JP9276904A patent/JPH11118968A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100709389B1 (en) | 2003-02-28 | 2007-04-20 | 학교법인 한양학원 | Manufacturing method of high corrosion resistant zirconium alloy fuel cladding tube |
| JP2006265725A (en) * | 2005-03-23 | 2006-10-05 | Westinghouse Electric Co Llc | Zirconium alloy improved in corrosion resistance and production method of zirconium alloy improved in corrosion resistance |
| CN101512671B (en) | 2006-08-24 | 2013-04-10 | 威斯丁豪斯电气瑞典有限公司 | Water reactor fuel cladding tube |
| JPWO2019093370A1 (en) * | 2017-11-10 | 2020-12-03 | 株式会社フェローテックマテリアルテクノロジーズ | Ceramics, probe guide parts, probe cards and sockets for package inspection |
| US11485686B2 (en) | 2017-11-10 | 2022-11-01 | Ferrotec Material Technologies Corporation | Ceramic, probe guiding member, probe card, and socket for package inspection |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 20050104 |