JP4479321B2 - Roll for rolling plate material made of molten glass and manufacturing method thereof - Google Patents
Roll for rolling plate material made of molten glass and manufacturing method thereof Download PDFInfo
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- JP4479321B2 JP4479321B2 JP2004119947A JP2004119947A JP4479321B2 JP 4479321 B2 JP4479321 B2 JP 4479321B2 JP 2004119947 A JP2004119947 A JP 2004119947A JP 2004119947 A JP2004119947 A JP 2004119947A JP 4479321 B2 JP4479321 B2 JP 4479321B2
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- 239000000463 material Substances 0.000 title claims description 26
- 238000005096 rolling process Methods 0.000 title claims description 19
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000006060 molten glass Substances 0.000 title claims 3
- 239000000956 alloy Substances 0.000 claims description 24
- 229910045601 alloy Inorganic materials 0.000 claims description 24
- 238000005242 forging Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 238000000137 annealing Methods 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 2
- 239000006104 solid solution Substances 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 150000001247 metal acetylides Chemical class 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 5
- 230000006872 improvement Effects 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000009864 tensile test Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 238000005452 bending Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
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Description
本発明は、ケイ素を主体とする板材の圧延用ロールと、その製造方法に関する。本発明により、過酷な条件で使用しても、長期にわたって高品質の製品板材を与えることのできるロールが提供される。 The present invention relates to a roll for rolling a plate material mainly composed of silicon, and a method for producing the roll. The present invention provides a roll capable of providing a high-quality product plate material over a long period of time even when used under severe conditions.
ケイ素を主体とする板材の製造に当たってはさまざまな方法が可能であるが、その中に、溶融した板素材を２本の成形ロールで圧延し、成形して製品を得る、という方法がある。このとき使用する圧延用ロールは、とくに鉛などを含有する板材を製造する場合は、その材質特性により溶融温度が高いから、ロールにかかる熱負荷は非常に高く、ロール寿命は長くない。ロールが湾曲すると、製品板厚が不均一になるし、ロール表面に微細なクラックが入ると、それが製品板材の表面に転写され、製品の品質を低下させる。これが、この種の板材圧延用ロールの製造に当たって解決すべき問題であった。 Various methods are possible for manufacturing a plate material mainly composed of silicon. Among them, there is a method in which a molten plate material is rolled with two forming rolls and molded to obtain a product. The rolling roll used at this time, particularly when producing a plate material containing lead or the like, has a high melting temperature due to its material characteristics, so the heat load applied to the roll is very high and the roll life is not long. When the roll is curved, the product plate thickness becomes non-uniform, and when a fine crack enters the roll surface, it is transferred to the surface of the product plate material and the product quality is lowered. This is a problem to be solved in manufacturing this kind of roll for rolling sheet materials.
ケイ素を主体とする板材に用いる圧延用ロールの材料としては、Ｃｏ基合金が好適であるとされ、実際にほとんどのものがＣｏ基合金で製造されている。出願人もその開発に努力し、適切な合金組成のＣｏ基合金を見出して、すでに開示した（特許文献１）。その合金は、重量％で、Ｃ：０．０３〜０．６０％、Ｓｉ：１．０％以下、Ｍｎ：３．０％以下、Ｎｉ：２〜４０％、Ｃｒ：１５〜２５％、Ｆｅ：１５％以下、Ｗおよび（または）Ｍｏ：５〜２０％を含有し、残部が実質的にＣｏからなる合金組成をもつものであり、ロール表面の耐熱損傷性を高くするためには、表面がＪＩＳ結晶粒度番号にして８以上の細粒であって、析出炭化物の面積率（％）が、２０箇所測定したときの最大値と最小値との差が５％以下であるという均質さをもつことが要求される。 As a material for a rolling roll used for a plate material mainly composed of silicon, a Co-based alloy is considered suitable, and most of them are actually manufactured from a Co-based alloy. The applicant also made efforts to develop it, and found a Co-based alloy having an appropriate alloy composition, which has already been disclosed (Patent Document 1). The alloy is, by weight, C: 0.03 to 0.60%, Si: 1.0% or less, Mn: 3.0% or less, Ni: 2 to 40%, Cr: 15 to 25%, Fe : 15% or less, W and / or Mo: 5 to 20%, with the balance being substantially composed of Co, and in order to increase the heat damage resistance of the roll surface, Is a fine grain having a JIS grain size number of 8 or more, and the area ratio (%) of the precipitated carbide has a homogeneity that the difference between the maximum value and the minimum value when measured at 20 locations is 5% or less. It is required to have.
出願人はまた、上記の合金組成を有するＣｏ基合金を材料としてケイ素を主体とする板材の圧延用ロールを製造する方法も開発し、上記合金と同時に開示した（特許文献２）。その方法は、上記合金組成を有するＣｏ基合金のインゴットから出発し、まずインゴットに温度１１６０〜１２２０℃で均熱処理を施したのち、１１６０〜１２２０℃の温度で鍛錬比２以上の熱間加工を施し、続いて１１６０〜１２２０℃の温度で均熱処理を施したのち、１０５０〜１１６０℃の温度で鍛錬比２以上の仕上げ加工を施すことからなる。仕上げ加工における均熱処理は、析出した炭化物を固溶させるため行なうものである。
こうした技術の改良にもかかわらず、圧延用ロールの寿命という点では、前記した問題が完全に解決したわけではなかった。問題のひとつは圧延用ロールのマクロ的な曲がりであり、いまひとつはロール表面に生じる微細なクラックが引き起こす、製品板材表面の凹凸である。この凹凸に対する制約はきわめてきびしく、クラック生じた圧延用ロールは、もはや使用に耐えない。 Despite these technical improvements, the above-mentioned problems have not been completely solved in terms of the life of the rolling roll. One of the problems is macro bending of the roll for rolling, and the other is unevenness on the surface of the product plate caused by fine cracks generated on the roll surface. The restrictions on the unevenness are extremely severe, and the cracked rolling roll can no longer withstand use.
本発明の目的は、きびしい使用条件のもとで長期間使用しても、ロール全体に湾曲が生じないのはもちろんのこと、ロール表面に微細なクラックが入らず、したがってより長期にわたって使用できる、ケイ素を主体とする板材の圧延用ロールと、その製造方法を提供することにある。 The object of the present invention is that, even if it is used for a long time under harsh usage conditions, the entire roll does not bend, and fine cracks do not enter the roll surface, so it can be used for a longer period of time. An object of the present invention is to provide a roll for rolling a plate material mainly composed of silicon and a method for producing the roll.
上記の目的を達成する本発明のケイ素を主体とする板材の圧延用ロールの製造方法は、重量％で、Ｃ：０．０３〜０．６０％、Ｓｉ：１．０％以下、Ｍｎ：３．０％以下、Ｎｉ：２〜４０％、Ｃｒ：１５〜２５％、Ｆｅ：１５％以下、Ｗおよび／またはＭｏ：５〜２０％を含有し、残部がＣｏおよび不可避な不純物からなる合金組成のＣｏ基合金を材料とし、熱間鍛造によりロール形状に成形してロール素材を得、このロール素材を温度１０００〜１１６０℃において固溶化処理したのち、温度８８０〜９８０℃において焼鈍処理し、最後に表面を鏡面に仕上げることからなる。
The method for producing a roll for rolling a sheet material mainly composed of silicon according to the present invention that achieves the above object is as follows: C: 0.03 to 0.60%, Si: 1.0% or less, Mn: 3 Alloy composition containing 0.0% or less, Ni: 2 to 40%, Cr: 15 to 25%, Fe: 15% or less, W and / or Mo: 5 to 20%, with the balance being Co and inevitable impurities A Co-base alloy is used as a material, and is formed into a roll shape by hot forging to obtain a roll material. The roll material is subjected to a solution treatment at a temperature of 1000 to 1160 ° C , and then annealed at a temperature of 880 to 980 ° C. And finishing the mirror surface.
本発明の方法に従って製造した圧延用ロールは、従来の製造方法によるロールにくらべて、過酷な条件下に使用しても、ロール全体の湾曲などが生じないことはむろん、ロール表面に生じた微細クラックにより製品板材の品質が低下するまでの、使用寿命が著しく改善されている。これは、とくに製品品質に対する要求がきびしい、鉛などを含有するケイ素を主体とする板材の製造に有利に作用し、かつ、製造コストの低減に寄与する。 The roll for rolling produced according to the method of the present invention does not cause the entire roll to bend even if it is used under severe conditions as compared with the roll produced by the conventional production method. The service life is significantly improved until the quality of the product plate is deteriorated due to the crack. This has an advantageous effect on the production of a plate mainly composed of silicon containing lead or the like, which is particularly demanding for product quality, and contributes to a reduction in production cost.
本発明の製造方法は、Ｃｏ基合金の熱間鍛造によるロール素材の成形を、さきに開示した発明の方法に従って実施することが好ましい。すなわち、Ｃｏ基合金のインゴットを温度１１６０〜１２２０℃に加熱する均熱処理を施し、温度１１６０〜１２２０℃において鍛錬比１．８以上の荒鍛造を行ない、それに続いて、温度１１６０〜１２２０℃に加熱する均熱処理を施したのち、温度１０５０〜１１６０℃において鍛錬比１．８以上の仕上げ鍛造を行なうという工程である。 In the production method of the present invention, it is preferable that the roll material is formed by hot forging of a Co-based alloy according to the method of the invention disclosed above. That is, a soaking process is performed in which a Co-based alloy ingot is heated to a temperature of 1160 to 1220 ° C., and rough forging with a forging ratio of 1.8 or more is performed at a temperature of 1160 to 1220 ° C., followed by heating to a temperature of 1160 to 1220 ° C. This is a step of performing finish forging with a forging ratio of 1.8 or more at a temperature of 1050 to 1160 ° C. after performing soaking.
このようにして製造される本発明の圧延用ロールは、これも前記したさきの発明において見出されたところに従って、表面がＪＩＳ結晶粒度番号にして８以上の細粒であって、析出炭化物の面積率（％）が、２０箇所測定したときの最大値と最小値との差が５％以下であるような、均質なものとすることが望ましい。 The rolling roll of the present invention produced in this way is a fine grain having a surface having a JIS crystal grain size number of 8 or more in accordance with the findings of the invention described above. It is desirable that the area ratio (%) be uniform so that the difference between the maximum value and the minimum value when measured at 20 locations is 5% or less.
上記のＣｏ基合金の合金組成は、前述した、出願人がかつて開示した発明（前掲特許文献１）のそれと同じものであり、合金組成の限定理由は、すでに述べたとおりである。表面の結晶粒度番号の限定および析出炭化物の面積率がもつべき均質さもまた、すでに開示した発明で必要としたものと同じである。この合金のインゴットから成形ロールを製造する好ましい工程も、さきに開示（前掲特許文献２）した発明の工程と異ならない。 The alloy composition of the Co-based alloy is the same as that of the invention previously disclosed by the applicant (Patent Document 1), and the reasons for limiting the alloy composition are as described above. The surface grain size number limitation and the homogeneity that the precipitated carbide area ratio should have are also the same as those required for the previously disclosed invention. A preferable process for producing a forming roll from the ingot of this alloy is not different from the process of the invention disclosed above (Patent Document 2).
本発明において、ガラス板成形ロールに関する上述した既知の技術と異なる点は、固溶化処理に続いて、表面を鏡面に仕上げることに先だって、温度８８０〜９８０℃における焼鈍処理を行なうことにある。焼鈍のための加熱時間は、均熱後、数時間が適切である。上記した焼鈍温度の範囲は、後記する実施例にみるように、さまざまな温度で焼鈍を実施した結果を、種々の観点から総合的に判断して決定したものである。
In the present invention, known techniques different from the above relates to a glass plate forming roll is had continued to solution treatment, prior to finish the surface mirror is to perform an annealing process at temperature 880-980 ° C.. The heating time for annealing is appropriate for several hours after soaking. The range of the annealing temperature described above is determined by comprehensively judging the results of annealing at various temperatures from various viewpoints as seen in the examples described later.
焼鈍処理の意義は、Ｃｏ基合金のマトリクス中に析出した炭化物を、適度に凝集させて、延性を改善することにある。析出炭化物は、引っ張り応力が作用したときに、破断の起点となると考えられ、凝集が生じていない、つまり微細な炭化物が多数分散しているときは、マトリクス金属は細かい網目のようにそれら炭化物粒子を囲んでおり、極度に凝集が進み、巨大化した炭化物が小数存在するようになると、マトリクスが形成する網目は、粗くなる。どちらも極端な場合は延性が低く、中間の、炭化物の凝集が適度に進んだ状態において、延性が高く得られる。この機構は、後記する実施データの延性の値、および破断面の顕微鏡写真によって裏付けられる。焼鈍温度が低すぎると、上記した炭化物の凝集が進行しないし、高すぎると、粗大化した炭化物によってロールの表面が荒れ、製品板材の品質が低下する。 The significance of the annealing treatment is to improve the ductility by appropriately agglomerating carbides precipitated in the matrix of the Co-based alloy. Precipitation carbide is considered to be the starting point of fracture when tensile stress is applied, and when agglomeration does not occur, that is, when a large number of fine carbides are dispersed, the matrix metal is in the form of a fine mesh. When the agglomeration progresses extremely and a small number of enlarged carbides exist, the mesh formed by the matrix becomes rough. In both extreme cases, the ductility is low, and high ductility can be obtained in an intermediate state where the agglomeration of carbides has progressed moderately. This mechanism is supported by the ductility values in the implementation data described below and micrographs of the fracture surface. If the annealing temperature is too low, the above-described agglomeration of carbides does not proceed, and if it is too high, the roll surface is roughened by coarsened carbides, and the quality of the product plate is lowered.
このようなわけで、高温における延性、ロール寿命および製品品質を総合的に考慮し、適切な焼鈍温度として選んだのが、前記した８８０〜９８０℃の範囲である。下の表１は、考慮した諸因子を示す。
For this reason, the range of 880 to 980 ° C. is selected as an appropriate annealing temperature in consideration of ductility at high temperatures, roll life, and product quality. Table 1 below shows the factors considered.
表１
Table 1
つぎの組成（質量％）のＣｏ基合金を、真空誘導炉溶解−再溶解法により製造し、２ｔインゴットに鋳造した。
０．１０％Ｃ−０．１％Ｓｉ−１．５％Ｍｎ−１１％Ｎｉ−２０％Ｃｒ−１５％Ｗ−２％Ｆｅ−残部Ｃｏ
A Co-based alloy having the following composition (mass%) was produced by a vacuum induction furnace melting-remelting method and cast into a 2t ingot.
0.10% C-0.1% Si-1.5% Mn-11% Ni-20% Cr-15% W-2% Fe-balance Co
分塊鍛造−仕上げ鍛造を経て、固溶化処理ののち、焼鈍（８３０℃または９３０℃）を行ない、機械加工により成形ロールの形状にした。表面の結晶粒度を調査したところ、どちらも、ＪＩＳ結晶粒度番号にして８以上の細粒であって、析出炭化物の面積率（％）が、２０箇所測定したときの最大値と最小値との差にして５％以下という、好ましい圧延用ロールの条件を満たしていた。 After forging and finishing forging, after solid solution treatment, annealing (830 ° C. or 930 ° C.) was performed, and the shape of the forming roll was formed by machining. When the crystal grain size of the surface was investigated, both were fine grains having a JIS grain size number of 8 or more, and the area ratio (%) of the precipitated carbide was the maximum value and the minimum value when measured at 20 locations. A preferable rolling roll condition of 5% or less was satisfied.
上記の焼鈍温度８３０℃および９３０℃の熱処理品から試験片を採取し、それらについて常温および高温（７５０℃）における引張り試験を行なった。その結果を対比すると、下記の表２に掲げるとおりである。 Test pieces were collected from the heat-treated products having the annealing temperatures of 830 ° C. and 930 ° C., and subjected to a tensile test at normal temperature and high temperature (750 ° C.). The results are compared as shown in Table 2 below.
表２
表２に示した引張り試験の結果を対比すると、常温の引張りではほとんど差がないが、高温の引張りでは、絞り値の向上とともに、とくに伸びと絞りとの値の比が、９３０℃焼鈍では１．０を越えることが注目される。すなわち、本発明に従って９３０℃で焼鈍したものは、よく伸び、しかも高度に絞れた後に破断しており、延性の向上が顕著である。破断面を顕微鏡で観察すると、図１（９３０℃焼鈍）および図２（８３０℃）のとおりであって、前者はマトリクスの網目が適度に大きくなっていること、換言すれば、前述した、破断の起点となる炭化物の凝集度合いが適度に進んでいることがうかがわれる。
Comparing the results of the tensile test shown in Table 2, there is almost no difference in the normal temperature tension, but in the high temperature tension, with the improvement of the drawing value, the ratio between the elongation and the drawing value is particularly 1 when the annealing at 930 ° C. It is noted that the value exceeds .0. That is, those annealed to the present invention therefore at 930 ° C. may stretch, yet are broken after highly juicing, improvement of ductility is remarkable. When the fracture surface is observed with a microscope, it is as shown in FIG. 1 (annealed at 930 ° C.) and FIG. 2 (830 ° C.), and the former shows that the matrix network is appropriately large. It can be seen that the degree of agglomeration of the carbide that is the starting point of the process proceeds moderately.
この圧延用ロールは、発明の範囲外である７５０℃の焼鈍処理をしたものよりも寿命が長く、表１に示したように、とくに好ましい温度の焼鈍をしたものは、最大５倍に達する寿命を享受することができる。従来の、固溶化処理をしただけのものと比較すれば、さらに長寿命である。圧延用ロールの寿命を左右するものは、ロール全体の湾曲が問題にならない場合は、ロール表面に微細クラックが入って、製品板材の品質が低下するという劣化であるが、本発明による高温延性の改善が、過酷な条件下の使用が引き起こす微細クラックの発生を遅れさせる。 This rolling roll has a longer life than the one subjected to annealing at 750 ° C., which is outside the scope of the invention, and as shown in Table 1, the one that has been annealed at a particularly preferable temperature reaches a maximum of five times the life. Can be enjoyed. Compared to the conventional solution-treated one, the life is even longer. What affects the life of the roll for rolling is a deterioration in which the quality of the product plate material is deteriorated due to microcracking on the roll surface when the entire roll is not curved. Improvements delay the generation of microcracks caused by use under harsh conditions.
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| CN105414219B (en) * | 2015-12-31 | 2018-06-01 | 中国航空工业集团公司北京航空制造工程研究所 | A kind of preparation method of metal/intermetallic compound laminar composite |
| CN114182153B (en) * | 2021-11-26 | 2022-11-18 | 北冶功能材料(江苏)有限公司 | Nickel-based alloy and preparation method and application thereof |
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