JP2764085B2 - Molybdenum tray and its manufacturing method - Google Patents
Molybdenum tray and its manufacturing methodInfo
- Publication number
- JP2764085B2 JP2764085B2 JP1018830A JP1883089A JP2764085B2 JP 2764085 B2 JP2764085 B2 JP 2764085B2 JP 1018830 A JP1018830 A JP 1018830A JP 1883089 A JP1883089 A JP 1883089A JP 2764085 B2 JP2764085 B2 JP 2764085B2
- Authority
- JP
- Japan
- Prior art keywords
- molybdenum
- tray
- layer
- coating layer
- microns
- 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
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims description 49
- 229910052750 molybdenum Inorganic materials 0.000 title claims description 47
- 239000011733 molybdenum Substances 0.000 title claims description 47
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 239000011247 coating layer Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- 239000010410 layer Substances 0.000 claims description 12
- 239000000919 ceramic Substances 0.000 claims description 10
- 238000007750 plasma spraying Methods 0.000 claims description 10
- 239000000956 alloy Substances 0.000 claims description 9
- 229910045601 alloy Inorganic materials 0.000 claims description 9
- 239000002344 surface layer Substances 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 11
- 238000000034 method Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 239000008188 pellet Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000003758 nuclear fuel Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000003979 granulating agent Substances 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- OOAWCECZEHPMBX-UHFFFAOYSA-N oxygen(2-);uranium(4+) Chemical compound [O-2].[O-2].[U+4] OOAWCECZEHPMBX-UHFFFAOYSA-N 0.000 description 1
- UTDLAEPMVCFGRJ-UHFFFAOYSA-N plutonium dihydrate Chemical compound O.O.[Pu] UTDLAEPMVCFGRJ-UHFFFAOYSA-N 0.000 description 1
- FLDALJIYKQCYHH-UHFFFAOYSA-N plutonium(IV) oxide Inorganic materials [O-2].[O-2].[Pu+4] FLDALJIYKQCYHH-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- FCTBKIHDJGHPPO-UHFFFAOYSA-N uranium dioxide Inorganic materials O=[U]=O FCTBKIHDJGHPPO-UHFFFAOYSA-N 0.000 description 1
- 229920002554 vinyl polymer Polymers 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
- Coating By Spraying Or Casting (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は原子炉燃料等の焼結に使用されるモリブデン
トレイに関する。Description: TECHNICAL FIELD The present invention relates to a molybdenum tray used for sintering of nuclear fuel and the like.
［従来の技術］ 原子炉用燃料である二酸化ウランや二酸化プルトニウ
ム等のペレットの焼結は、耐熱性にすぐれたモリブデン
トレイにペレットを載せたものを複数枚積み重ねて加熱
炉に入れ加熱することにより行なわれている。この場
合、ペレットを直接トレイに載せることもあるが、モリ
ブデン又はモリブデン基合金の敷板をトレイに載せ、そ
の上にペレットを載せることが多い。[Prior art] Sintering of pellets such as uranium dioxide and plutonium dioxide, which are fuels for nuclear reactors, is performed by stacking a plurality of pellets on a molybdenum tray having excellent heat resistance, heating the pellets in a heating furnace, and heating. Is being done. In this case, the pellets may be placed directly on the tray. However, in many cases, a bed plate made of molybdenum or a molybdenum-based alloy is placed on the tray, and the pellets are placed on the tray.
［発明が解決しようとする課題］ 上記原子炉燃料の焼結温度は1700〜1750℃ときわめて
高温であり、しかも積み重ねられたトレイの総重量は30
〜40kgにも達するため、モリブデントレイや敷板その他
の部品が互いに接着し、引剥し時に損傷するという問題
があった。[Problems to be Solved by the Invention] The sintering temperature of the above reactor fuel is extremely high at 1700 to 1750 ° C, and the total weight of the stacked trays is 30
Since it reaches ~ 40 kg, there is a problem that molybdenum trays, floor boards and other parts adhere to each other and are damaged when peeled off.
これを防止するため、トレイや敷板等の部品の互いに
接触する部分にホーニング処理を施こし表面粗さを粗く
して接着を防止する方法がとられているが、この方法は
初めのうちは接着が起こりにくいが数回の使用で効果が
なくなるという問題があった。To prevent this, a method has been adopted in which parts that come into contact with each other, such as trays and floorboards, are subjected to honing treatment to reduce the surface roughness and prevent adhesion. However, there is a problem that the effect is lost after several uses.
本発明は上記従来のモリブデントレイにおける接着の
問題を解決することを目的としている。An object of the present invention is to solve the problem of adhesion in the above-mentioned conventional molybdenum tray.
［課題を解決するための手段］ 上記課題を解決するため、本発明は次のようなモリブ
デントレイとその製法を提供する。[Means for Solving the Problems] In order to solve the above problems, the present invention provides the following molybdenum tray and a method for manufacturing the same.
すなわち、本発明にかかるモリブデントレイは、モリ
ブデン又はモリブデン基合金を基材とするトレイであっ
て、その表面にモリブデンと耐熱性セラミックスからな
るコーティング層が形成されていることを特徴としてい
る。That is, the molybdenum tray according to the present invention is a tray based on molybdenum or a molybdenum-based alloy, and is characterized in that a coating layer made of molybdenum and a heat-resistant ceramic is formed on the surface thereof.
また、本発明にかかるモリブデントレイの製法は、ト
レイを形成するモリブデン又はモリブデン基合金の基材
の表面にプラズマ溶射法によりモリブデンに富む下地層
を形成し、さらにその上からプラズマ溶射法により耐熱
性セラミックスに富む表面層を形成したのち、1500℃以
上の高温で焼成することを特徴としている。In addition, the method for manufacturing a molybdenum tray according to the present invention includes forming a molybdenum-rich underlayer by plasma spraying on the surface of a substrate of molybdenum or a molybdenum-based alloy forming the tray, and further heat-resistant by plasma spraying from above. After forming a surface layer rich in ceramics, it is characterized by firing at a high temperature of 1500 ° C or higher.
以下、具体例を挙げつつ詳細に説明する。 Hereinafter, a detailed example will be described with reference to specific examples.
先ず、モリブデントレイの基材としては純モリブデン
又はモリブデン基合金の板材が使用される。モリブデン
基合金としては例えばモリブデンにSiO2,K2O,Al2O3等を
添加したものであり、適度の加工性と耐熱性を有するも
のであればよい。使用上不都合を生じない範囲であれば
少量の他の元素を含有してもよい。モリブデン又はモリ
ブデン基合金の板材は通常の粉末冶金法によって製造す
ることができる。また、トレイの形状は、被加熱材を載
せることができるものであればよく、例えば単なる平板
板のものであってもよく、箱状のものであってもよい。First, a plate material of pure molybdenum or a molybdenum-based alloy is used as a base material of the molybdenum tray. The molybdenum-based alloy may be, for example, molybdenum to which SiO 2 , K 2 O, Al 2 O 3, or the like is added, as long as it has appropriate workability and heat resistance. A small amount of other elements may be contained within a range that does not cause inconvenience in use. The plate material of molybdenum or a molybdenum-based alloy can be manufactured by a usual powder metallurgy method. The shape of the tray may be any shape as long as the material to be heated can be placed thereon. For example, the shape may be a simple flat plate or a box.
この基材の表面にコーティング層を形成するが、この
コーティング層は接着を防止するためのものであるか
ら、基材の全表面に形成する必要はなく、少なくとも使
用時に他のトレイその他の物品に接触する部分のみに形
成しておけばよい。A coating layer is formed on the surface of the base material, but since this coating layer is for preventing adhesion, it is not necessary to form the coating layer on the entire surface of the base material. What is necessary is just to form only in the part which contacts.
コーティング層は大別してモリブデンに富んだ下地層
と実質的に耐熱性セラミックスからなる表面層からな
る。これら下地層と表面層とは明確に境界づけられる必
要はなく、理想的には最下部すなわち基材に接する部分
が純モリブデン（又はモリブデン基合金）で、表層にな
るほど耐熱性セラミックスの濃度が高くなるよう濃度勾
配があり、最上層部が実質的に耐熱性セラミックスの層
となっているのが望ましい。耐熱性セラミックスとして
は、例えばアルミナ、マグネシヤ、ジルコニヤ等の酸化
物が最も普通であるが、他に窒化物や硼化物等公知の耐
熱性セラミックスを使用することができる。The coating layer is roughly divided into a molybdenum-rich underlayer and a surface layer substantially made of a heat-resistant ceramic. The underlayer and the surface layer do not need to be clearly bounded. Ideally, the lowermost part, that is, the part in contact with the base material is pure molybdenum (or a molybdenum-based alloy), and the higher the surface layer, the higher the concentration of the heat-resistant ceramic. It is desirable that there is a concentration gradient so that the uppermost layer is substantially a layer of a heat-resistant ceramic. As the heat-resistant ceramics, for example, oxides such as alumina, magnesium, and zirconia are the most common, but other known heat-resistant ceramics such as nitrides and borides can be used.
このようなコーティング層は、例えばプラズマ溶射法
によって形成することができる。この場合、例えば平均
粒度３〜５ミクロン程度のモリブデン粉末を用い、流動
性を改良するため例えばポリビニール系の造粒剤を用い
て10〜100ミクロン程度、より好ましくは30〜80ミクロ
ン程度の球状の顆粒に造粒して使用する。また、耐熱性
セラミックスも例えば10〜40ミクロン程度の粒状のもの
を使用する。これらを市販のプラズマ溶射機に入れ、両
者の配合比を調節しながら基材表面に吹き付けてゆけば
よい。なお、密着性を向上させるため基材表面は予め30
〜60ミクロンの表面粗さに荒らしておくのが好ましい。
プラズマ溶射により所望のコーティング層を形成した
ら、その密着性を向上するため、例えば水素気流中又は
不活性雰囲気中で1500〜1800℃に加熱して焼成を行な
う。これにより接合強度のすぐれたコーティング層が形
成されるのである。Such a coating layer can be formed by, for example, a plasma spraying method. In this case, for example, a molybdenum powder having an average particle size of about 3 to 5 microns is used. In order to improve fluidity, for example, a polyvinyl-based granulating agent is used to form a spherical particle of about 10 to 100 microns, more preferably about 30 to 80 microns. Granulated into granules for use. Also, heat-resistant ceramics having a granular shape of, for example, about 10 to 40 microns are used. These may be put into a commercially available plasma spraying machine and sprayed onto the surface of the base material while adjusting the mixing ratio of the two. In addition, in order to improve the adhesion,
It is preferable to roughen to a surface roughness of ~ 60 microns.
After forming a desired coating layer by plasma spraying, in order to improve the adhesion, baking is performed, for example, by heating to 1500 to 1800 ° C. in a hydrogen stream or an inert atmosphere. As a result, a coating layer having excellent bonding strength is formed.
［実施例］ 通常の粉末冶金法によって製造した純モリブデン板製
トレイの表面にプラズマ溶射法によりモリブデンとアル
ミナの複合層を形成した。その手順は次の通りであっ
た。[Example] A composite layer of molybdenum and alumina was formed by plasma spraying on the surface of a tray made of a pure molybdenum plate manufactured by a usual powder metallurgy method. The procedure was as follows.
先ず、平均粒度3.5ミクロンの純モリブデン粉末を平
均粒度約50ミクロンの顆粒に造粒した。また、アルミナ
粒としては純度99.6％以上で粒度約30ミクロンの市販の
アルミナ粉末を使用した。これら両原料粒をプラズマ溶
射機の２つのポットに別々に入れ、両原料の配合比を変
化させながら前記トレイの表面に溶射を行ない、第１表
に示すようなコーティング槽を形成した。同表におい
て、実施例１はモリブデン50％（重量％、以下同じ）と
アルミナ50％の混合物からなる複合層一層のみを形成し
たものである。実施例２は基材表面に先ずモリブデン10
0％の下地層を形成し、その上からモリブデン50％とア
ルミナ50％の複合層を形成した概略二層構造のものであ
る。また実施例３は、先ずモリブデン100％の下地層を
形成し、その上にモリブデン50％とアルミナ50％の複合
層を形成したのち、さらにその上にアルミナ100％の表
面層を形成したものである。この構造を模式的に表わせ
ば第１図のようになる。図中Ａはモリブデン基材、Ｂは
コーティング層で、B1は純モリブデン下地層、B2はモリ
ブデンとアルミナの複合層、B3は純アルミナ表面層であ
る。プラズマ溶射によるコーティング層の厚みは100〜1
50ミクロンとした。このうち、実施例2,3のモリブデン1
00％の下地層の厚さは10〜50ミクロン、好ましくは30〜
50ミクロンであった。焼成温度は1500〜1800℃であり、
雰囲気は水素気流中、保持時間は３〜５時間であった。
なお、第１表には比較例として基材表面にアルミナ層の
みを200ミクロンの厚みで形成したものを併記してい
る。First, pure molybdenum powder having an average particle size of 3.5 microns was granulated into granules having an average particle size of about 50 microns. As the alumina particles, commercially available alumina powder having a purity of 99.6% or more and a particle size of about 30 microns was used. These two raw material particles were separately placed in two pots of a plasma spraying machine, and sprayed on the surface of the tray while changing the mixing ratio of the two raw materials to form a coating tank as shown in Table 1. In the table, in Example 1, only one composite layer made of a mixture of 50% molybdenum (% by weight, hereinafter the same) and 50% alumina was formed. In Example 2, molybdenum 10 was first applied to the substrate surface.
It has a roughly two-layer structure in which a 0% underlayer is formed, and a composite layer of 50% molybdenum and 50% alumina is formed thereon. In Example 3, a base layer of 100% molybdenum was first formed, a composite layer of 50% molybdenum and 50% alumina was formed thereon, and then a surface layer of 100% alumina was further formed thereon. is there. FIG. 1 schematically shows this structure. In the figure, A is a molybdenum base material, B is a coating layer, B1 is a pure molybdenum base layer, B2 is a composite layer of molybdenum and alumina, and B3 is a pure alumina surface layer. The thickness of the coating layer by plasma spraying is 100-1
It was 50 microns. Of these, molybdenum 1 of Examples 2 and 3
The underlayer thickness of 00% is 10 to 50 microns, preferably 30 to
It was 50 microns. Firing temperature is 1500-1800 ℃,
The atmosphere was a hydrogen stream, and the retention time was 3 to 5 hours.
Table 1 also shows a comparative example in which only an alumina layer was formed to a thickness of 200 microns on the substrate surface.
上記各実施例と比較例についてコーティング層の剥離
強度を調べた結果は第１表に示す通りであった。この剥
離強度は、コーティング層の表面に接着剤で鋼材を接合
し、引張り荷重を負荷してコーティング層が剥離する荷
重を調べたものである。同表からわかる通り、実施例の
ものは比較例のものに較べ４〜５倍の強度を有し、長時
間の使用に充分耐えるものであった。また、これら実施
例の構造を有するモリブデントレイを実際に原子炉燃料
の焼結に使用した結果、いずれも問題となる接着現象は
生じなかった。The results of examining the peel strength of the coating layer for each of the above Examples and Comparative Examples are as shown in Table 1. The peel strength is obtained by joining a steel material to the surface of the coating layer with an adhesive, applying a tensile load, and examining a load at which the coating layer peels. As can be seen from the table, the example had 4 to 5 times the strength of the comparative example and was sufficiently resistant to long-term use. Further, as a result of actually using the molybdenum trays having the structures of these examples for sintering of nuclear reactor fuel, no problematic adhesion phenomenon occurred.
［発明の効果］ 以上の説明から明らかなように、本発明によれば高温
で長時間使用しても問題となる接着現象が生じないすぐ
れたモリブデントレイを得ることが可能となった。 [Effects of the Invention] As is apparent from the above description, according to the present invention, it has become possible to obtain an excellent molybdenum tray which does not cause a problem of adhesive phenomenon even when used at a high temperature for a long time.
第１図は本発明の一実施例の構造を模式的にあらわす断
面図である。 Ａ……基材、Ｂ……コーティング層FIG. 1 is a sectional view schematically showing the structure of one embodiment of the present invention. A: Base material, B: Coating layer
Claims (2)
するトレイであって、その表面にモリブデンと耐熱性セ
ラミックスからなるコーティング層が形成されているこ
とを特徴とするモリブデントレイ。1. A molybdenum tray comprising molybdenum or a molybdenum-based alloy as a base material, the surface of which is provided with a coating layer made of molybdenum and heat-resistant ceramics.
ン基合金の基材の表面にプラズマ溶射法によりモリブデ
ンに富む下地層を形成し、さらにその上からプラズマ溶
射法により耐熱性セラミックスに富む表面層を形成した
のち、1500℃以上の高温で焼成することを特徴とするモ
リブデントレイの製法。2. A molybdenum-rich base layer is formed on the surface of a molybdenum or molybdenum-based alloy base material forming a tray by plasma spraying, and a heat-resistant ceramic-rich surface layer is formed thereon by plasma spraying. After that, it is fired at a high temperature of 1500 ° C. or more, a method for producing a molybdenum tray.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1018830A JP2764085B2 (en) | 1989-01-27 | 1989-01-27 | Molybdenum tray and its manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1018830A JP2764085B2 (en) | 1989-01-27 | 1989-01-27 | Molybdenum tray and its manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02200766A JPH02200766A (en) | 1990-08-09 |
| JP2764085B2 true JP2764085B2 (en) | 1998-06-11 |
Family
ID=11982483
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1018830A Expired - Fee Related JP2764085B2 (en) | 1989-01-27 | 1989-01-27 | Molybdenum tray and its manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2764085B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7332228B2 (en) | 2003-02-25 | 2008-02-19 | A.L.M.T. Corporation | Coated refractory metal plate having oxide surface layer, and setter which uses the same and which is used in sintering |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006046181A1 (en) * | 2004-10-26 | 2006-05-04 | Koninklijke Philips Electronics N.V. | Molybdenum-molybdenum brazing and rotary-anode x-ray tube comprising such a brazing |
| JP6360245B1 (en) * | 2017-11-08 | 2018-07-18 | 新和工業株式会社 | Sintering setter and method for producing the same |
-
1989
- 1989-01-27 JP JP1018830A patent/JP2764085B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7332228B2 (en) | 2003-02-25 | 2008-02-19 | A.L.M.T. Corporation | Coated refractory metal plate having oxide surface layer, and setter which uses the same and which is used in sintering |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02200766A (en) | 1990-08-09 |
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