CN112469842A - 表面硬化材料的制造方法 - Google Patents

表面硬化材料的制造方法 Download PDF

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CN112469842A
CN112469842A CN201980040442.XA CN201980040442A CN112469842A CN 112469842 A CN112469842 A CN 112469842A CN 201980040442 A CN201980040442 A CN 201980040442A CN 112469842 A CN112469842 A CN 112469842A
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nitrogen
steel material
less
producing
temperature
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中岛隆
伊藤太郎
松川龙也
别府正昭
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Japan Pakase Seiki Co ltd
Nihon Parkerizing Co Ltd
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Japan Pakase Seiki Co ltd
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Abstract

表面硬化材料的制造方法，包括：将表面固溶有氮的钢铁材料在包含氯化物的熔融物中在650℃～900℃的范围内进行浸渍的浸渍步骤，和将浸渍了的上述钢铁材料以马氏体相变开始的下部临界冷却速度以上的冷却速度冷却至马氏体相变开始温度以下的冷却步骤。

Description

表面硬化材料的制造方法
技术领域
本发明涉及通过对表面固溶有氮的钢铁材料实施规定的处理从而使其硬化至深的位置的表面硬化材料的制造方法。
背景技术
作为钢铁材料的表面硬化处理法，以往，开发了各种方法。例如，在专利文献1中，公开了以下方法：对钢实施软氮化处理，在表面形成规定厚度的氮化物层，接着在1000～1200℃加热30～120分钟。另外，在专利文献2中，公开了以下方法：在对金属型材进行氮化处理后进行表面的加热，以马氏体相变的临界冷却速度以上且30℃/秒以下的冷却速度冷却至马氏体相变开始温度以下，使表面的氮化合物减少或消失并且使氮扩散·固溶至内部，与单独氮化处理相比使表面硬化层更深。
现有技术文献
专利文献
专利文献1：日本特开2015-59248号公报
专利文献2：日本特开平7-138733号公报
发明内容
发明所要解决的课题
但是，在专利文献1和2所记载的方法中，有时对于表面固溶有氮的钢铁材料，不能使大量的氮渗透至深处，或者表面氧化从而不能形成硬质的表面直至深的位置。因此，本发明的目的解决上述问题，提供一种制造具有硬质的表面直至深的位置的表面硬化材料的方法。
用于解决课题的手段
即，本发明包含以下方案。
(1)表面硬化材料的制造方法，包括：将表面固溶有氮的钢铁材料在包含氯化物的熔融物中在650℃～900℃的范围内进行浸渍的浸渍步骤，和
将浸渍了的上述钢铁材料以马氏体相变开始的下部临界冷却速度以上的冷却速度冷却至马氏体相变开始温度以下的冷却步骤；
(2)上述(1)中所述的表面硬化材料的制造方法，其中，表面固溶有氮的钢铁材料还包含铁氮化合物层作为表层；
(3)上述(1)或(2)所述的表面硬化材料的制造方法，其中，表面固溶有氮的钢铁材料在表面还固溶有碳；
(4)上述(1)或(2)所述的表面硬化材料的制造方法，还包括：对钢铁材料进行氮化处理从而将氮固溶于表面的氮化处理步骤；
(5)上述(4)所述的表面硬化材料的制造方法，其中，上述氮化处理为气体氮化处理、气体软氮化处理、等离子体氮化处理或盐浴软氮化处理；
(6)上述(4)或(5)所述的表面硬化材料的制造方法，其中，在上述氮化处理步骤前，还包括：对钢铁材料实施渗碳处理的渗碳处理步骤。
(7)上述(1)～(6)的任一项所述的表面硬化材料的制造方法，其中，将氮固溶于表面(进行上述氮化处理)的钢铁材料以质量％计包含
0.01％以上且1.5％以下的C、
3％以下的Si、
2％以下的Mn、
合计5％以下的Cr、Mo、Cu和Ni、
合计1％以下的Nb、Ti、V和B、
0.1％以下的P、
0.05％以下的S、
70.0％以上且99.5％以下的Fe；
(8)上述(1)～(6)的任一项所述的表面硬化材料的制造方法，其中，将氮固溶于表面(进行上述氮化处理)的钢铁材料以质量％计包含
0.01％以上且1.5％以下的C、
3％以下的Si、
2％以下的Mn、
合计5％以下的Cr、Mo、Cu和Ni、
合计1％以下的Nb、Ti、V和B、
0.1％以下的P、
0.05％以下的S，
还包含Fe和不可避免的杂质作为余量。
发明效果
根据本发明，能够提供一种制造具有硬质的表面直至深的位置的表面硬化材料的方法。
具体实施方式
本发明涉及的表面硬化材料的制造方法包括：将表面固溶有氮的钢铁材料在包含氯化物的熔融物中在650℃～900℃的范围内进行浸渍的浸渍步骤，和将浸渍了的上述钢铁材料以马氏体相变开始的下部临界冷却速度以上的冷却速度冷却至马氏体相变开始温度以下的冷却步骤。以下，进行具体说明。
所谓表面固溶有氮的钢铁材料，是指在钢铁材料的表面氮处于固溶状态。作为用于将氮固溶于表面的钢铁材料，只要至少包含铁和碳且包含70质量％以上(优选80质量％以上)的铁就没有特别限制，具体可举出一般结构用轧制钢材、冷轧钢材和钢带、机械结构用碳素钢钢材、机械结构用合金钢钢材、碳素工具钢钢材、高速工具钢钢材、弹簧钢钢材、高碳铬轴承钢钢材等。予以说明，由与钢铁材料同样的组成构成的具有镀膜的钢铁材料也可成为对象。该情况下，钢铁材料和镀膜可以包含同一组成，也可以包含不同组成。另外，钢铁材料除了铁和碳以外可以包含其它元素。作为其它元素，例如可举出Si、Mn、Cr、Mo、Cu、Ni、Nb、Ti、V、B、P、S、O等。这些之中，钢铁材料可以包含一种或两种以上，钢铁材料也可以包含全部。
对钢铁材料中包含的各元素的含量进行说明。C(碳)的含量通常在0.01质量％以上且1.5质量％以下的范围内，优选在0.4质量％以上且1.0质量％以下的范围内。Si(硅)的含量通常为3质量％以下，优选为1质量％以下。Mn(锰)的含量通常为2质量％以下，优选为0.6质量％以下。Cr(铬)、钼(Mo)、Cu(铜)、镍(Ni)等的合计含量通常为5质量％以下。Nb(铌)、Ti(钛)、V(钒)、B(硼)等的合计含量可以为1质量％以下，优选为杂质水平。P(磷)的含量通常为0.1质量％以下，优选为0.05质量％以下。S(硫)的含量通常为0.05质量％以下，优选为0.03质量％以下。O(氧)的含量优选为杂质水平。
在本实施方式中，作为优选的钢铁材料，包含：0.01质量％以上且1.5质量％以下的范围内的C；3质量％以下的Si；2质量％以下的Mn；合计5质量％以下的Cr、Mo、Cu和Ni；合计1质量％以下的Nb、Ti、V和B；0.1质量％以下的P；0.05质量％以下的S；和70.0质量％以上且99.5质量％以下的Fe，或者作为余量的Fe和不可避免的杂质。具体地，说到JIS钢种，可举出SPCC、S10C、S45C、S55C、SK65(SK7)、SK105(SK3)、SUJ2、SCM420、SCM440等。这些钢铁材料可以为实施了预退火或球化退火的钢铁材料。
作为将氮固溶于钢铁材料的表面的方法，例如可举出对于钢铁材料的氮化处理。本发明涉及的表面硬化材料的制造方法可以进一步包含“在浸渍步骤前，对钢铁材料实施氮化处理，从而将氮固溶于表面的氮化处理步骤”。另外，在氮化处理步骤后且后述的浸渍步骤前，可以将表面固溶有氮的钢铁材料冷却，或者在将表面固溶有氮的钢铁材料冷却后进行清洗。作为对于钢铁材料的氮化处理，只要为以往已知的方法就没有特别限制，例如可举出气体氮化处理、气体软氮化处理、等离子体氮化处理或盐浴软氮化处理等。另外，在进行后述的渗碳处理步骤的情况下，可以进行渗碳氮化处理作为氮化处理。通过进行这些氮化处理，在钢铁材料的表面形成固溶有氮的氮扩散层、或者该氮扩散层与在该氮扩散层上形成的铁氮化合物层的复合层。
上述氮扩散层中的氮通常为0.05质量％以上，但不限定于该值。另外，铁氮化合物层中的铁氮化合物例如为ε-Fe2-3N；γ’-Fe4N；Fex(N,C)[x为任意数值。]；CrN、Cr2N、TiN、Si3N4、VN等MxN[M：钢铁材料中包含的金属材料，例如Cr、Ti、Si、V等，x为任意数值。]等。铁氮化合物层的厚度通常以1μm以上且50μm以下的范围内形成。氮化处理的温度和时间等条件根据钢铁材料的种类、处理的方法等而不同，通常在A1相变点以下的温度进行规定时间，例如在300℃以上且600℃以下的范围内且5分钟以上且120分钟以下的范围内进行。更具体地，在盐浴软氮化处理的情况下，温度优选为550℃以上且600℃以下的范围内，更优选为570℃以上且590℃以下的范围内。处理时间优选为60分钟以上且120分钟以下的范围内。
铁氮化合物层的厚度可利用光学显微镜或扫描型电子显微镜对通过将钢铁材料进行氮化处理而得到的、表面固溶有氮的钢铁材料的剖面进行测定。铁氮化合物层的组成可利用EPMA(电子束显微分析仪)分析来测定。氮扩散层的厚度可利用EPMA(电子束显微分析仪)分析作为在铁中仅固溶有氮的层、或者在固溶了氮的母相中使合金元素(Cr、V、Nb、Ti、Al)的氮化物分散析出而成的复合层的厚度来测定。
本发明涉及的表面硬化材料的制造方法在浸渍步骤前，更具体地，在上述氮化处理步骤前，可进一步包括：“对钢铁材料实施渗碳处理的渗碳处理步骤”。通过进行该渗碳处理步骤，可将碳固溶于钢铁材料的表面。另外，通过进行该渗碳处理步骤和氮化处理步骤，能够得到在表面固溶化有碳和氮的钢铁材料。在此，作为渗碳处理，例如可举出固体渗碳处理；盐浴渗碳处理等液体渗碳处理；气体渗碳处理；真空渗碳处理(真空气体渗碳处理)；等离子体渗碳处理(离子渗碳处理)等，但不限定于这些。渗碳处理的温度和时间等条件根据钢铁材料的种类、处理的方法、使碳渗透的深度等而不同，以将碳固溶于钢铁材料的表面的方式适当设定。予以说明，本发明涉及的表面硬化材料的制造方法在进行了渗透处理步骤后、氮化处理步骤前，为了提高钢铁材料的表面硬度，可进一步在适宜的条件下进行淬火、回火等处理。
浸渍步骤
将表面固溶有氮的钢铁材料接着浸渍在包含氯化物的熔融物中。通过该浸渍步骤，能够使更多的在表面固溶了的氮渗透至深处，并且能够防止表面发生氧化，因此，通过后述的冷却步骤，也能够使表面强度提高直至深的位置。作为熔融物中包含的氯化物，例如可举出NaCl、KCl、BaCl2等，但不限于这些。这些氯化物可以单独使用一种，也可以将两种以上混合使用。熔融物可以包含Na、K、Ba等的硝酸金属盐和/或碳酸金属盐，也可以不包含。浸渍在熔融物中的温度(浸渍温度)通常为650℃以上且900℃以下的范围内。限定于该温度范围的理由是因为，若不在该温度范围浸渍，则不能将表面硬化材料的表面硬度充分地提高至深的位置。浸渍在熔融物中的时间根据用于将氮固溶于表面的钢铁材料的种类、浸渍温度等而不同，通常为5分钟以上且60分钟以下，优选为5分钟以上且30分钟以下。
冷却步骤
通过将在浸渍步骤中浸渍了的上述钢铁材料进行急冷，使表面部发生马氏体相变，能够制造具有硬质的表面直至深的位置的表面硬化材料。作为冷却(急冷)的条件，只要是马氏体相变开始(发生)的下部临界冷却速度以上的冷却速度就没有特别限制，优选为上部临界冷却速度以上的冷却速度。下部临界冷却速度和上部临界冷却速度根据浸渍的上述钢铁材料的组成而不同，一般为20℃/秒～30℃/秒以上。予以说明，作为进行冷却的温度，只要为马氏体相变开始温度以下就没有特别限制。另外，冷却(急冷)方法没有特别限制，优选浸渍于水、盐水、聚合物分散水溶液、油、盐浴、铅浴等冷却介质。在进行了冷却步骤后，对于冷却了的上述钢铁材料，可以进行水洗或者在水洗后进一步进行回火。通过进行回火，可制造使韧性得到提高的表面硬化材料。回火可在通常所进行的条件下进行。回火的温度和时间等条件根据冷却了的上述钢铁材料的组成、使用用途而不同，例如可举出150℃以上且180℃以下的范围内的温度和60分钟以上且90分钟以下的范围内的时间等。
实施例
为了确认根据本发明的制造方法的效果，制作了7种试验片。予以说明，将用于试验片制作的各JIS钢种的成分组成示于表1。余量为铁和杂质，单位为质量％。
(1)试验片1
对机械结构用碳素钢钢材S45C在850℃进行4小时退火，通过机械加工，成型为直径20mm×长50mm，制作了试验片1。
(2)试验片2
将板厚1mm的汽车用极软钢薄钢板SPCC切断成70mm×150mm，制作了试验片2。
(3)试验片3
将S10C在900℃进行4小时的退火，通过机械加工，成型为直径20mm×长50mm，制作了试验片3。
(4)试验片4
将S55C在850℃进行4小时的退火，通过机械加工，成型为直径20mm×长50mm，制作了试验片4。
(5)试验片5和试验片6
将SCM420在850℃进行4小时的退火，通过机械加工，成型为直径20mm×长50mm，制作了试验片5。将该试验片一边注入丙烷改性气体(RX气体)和富丙烷气体一边在渗碳炉内在930℃进行180分钟渗碳处理。其后，将温度下降至850℃后进行油冷(淬火)，以有效硬化层深度(550HV)成为0.8mm的方式进行回火，对表面进行机械研磨，成型为直径20mm×长50mm，制作了在表面具备渗碳层的试验片6。予以说明，有效硬化层深度基于JIS G 0557：2006中的“钢的渗碳硬化层深度测定方法”来测定。
(6)试验片7
将SCM440球化退火，通过机械研磨，成型为直径20mm×长50mm，制作了试验片。
表1
JIS钢种 C Si Mn Cr Mo Ni P S
S45C 0.42-0.48 0.15-0.35 0.60-0.90 - - - ≤0.030 ≤0.035
SPC 0.15以下 - ≤0.60 - - - ≤0.100 ≤0.050
S10C 0.08-0.13 0.15-0.35 0.30-0.60 - - - ≤0.030 ≤0.035
S55C 0.52-0.58 0.15-0.35 0.60-0.90 - - - ≤0.030 ≤0.035
SCM420 0.18-0.23 0.15-0.35 0.60-0.90 0.90-1.20 0.15-0.25 ≤0.25 ≤0.030 ≤0.030
SCM440 0.38-0.43 0.15-0.35 0.60-0.90 0.90-1.20 0.15-0.30 ≤0.25 ≤0.030 ≤0.030
No.1～5的评价材料的制作
将试验片1浸渍于盐浴软氮化剂(パ一カ一热处理工业制；NS-2)，在570℃进行120分钟的盐浴软氮化处理。将进行了盐浴软氮化处理的试验片1利用光学显微镜和EPMA分析进行观察，可确认以距表面约15μm的厚度形成铁氮化合物层、在铁氮化合物层下以约200μm的厚度形成氮扩散层而形成复合层。将进行了盐浴软氮化处理的试验片1浸渍于包含氯化物金属盐的盐浴剂，在600℃～1000℃进行了30分钟盐浴加热。作为盐浴剂，在600℃或650℃进行加热的情况下，使用パ一カ一热处理工业制GS540(熔点540℃)，在800℃～1000℃进行加热的情况下，使用パーカー热处理工业制GS660(熔点660℃)。进行了盐浴加热后，将试验片1浸渍于20～30℃的5％NaCl水溶液中进行冷却(以下称作“水冷”)，制作了No.1～5的评价材料。此时的冷却速度为约170℃/秒。
No.6～10的评价材料的制作
对试验片1进行等离子体氮化处理，将进行了等离子体氮化处理的试验片1利用光学显微镜和EPMA分析进行观察。予以说明，就等离体子氮化处理而言，以炉内的N2气体和H2气体的体积比成为1∶4的方式进行调整，减压至3torr，在570℃进行6小时。光学显微镜的观察的结果，可确认铁氮化合物层在表面不连续地形成，另外，以距铁氮化合物层的下方或表面约200μm的厚度形成氮扩散层。对进行了等离子体氮化处理的试验片1的表面进行机械研磨，除去在表面不连续地形成的稍许铁氮化合物层，与上述同样，进行在盐浴剂中的浸渍和水冷，制作了No.6～10的评价材料。
特性评价
评价了No.1～10的评价材料的特性(表面氧化、剖面硬度)。表面氧化确认水冷时有无氧化物等从试验片1的表面的剥离、脱落、和采用金相显微镜对各评价材料进行剖面观察(观察倍率500倍)时的表面氧化皮的厚度来评价。在没有剥离、脱落、氧化皮的厚度不到2μm的情况下，判断为实用化水平，表面氧化评价为“无”。其他情况下即在确认到剥离、脱落的情况下、或者氧化皮的厚度为2μm以上的情况下，表面硬化评价为“有”。
表面硬度将各评价材料切断后，采用机械研磨将剖面镜面抛光，接着使用显微硬度试验机(微型维氏)，以测定负载0.3kgf，测定了从表面至深度300μm的位置处的显微硬度(HV)。
将这些结果示于表2。
表2
Figure BDA0002839060870000091
No.11～18的评价材料的制作
利用光学显微镜和EPMA分析观察了与上述同样地进行了盐浴软氮化处理的试验片1或6。光学显微镜的观察的结果，可确认以距表面约15μm的厚度形成铁氮化合物层，在铁氮化合物层的下方以约200μm的厚度形成氮扩散层。
对于进行了盐浴软氮化处理的试验片6，在800℃进行5分钟或30分钟的盐浴加热后，浸渍在30～40℃的冷淬油(出光制，ダフニーマスタークエンチA)中冷却(以下称作“油冷”)，制作了No.11和12的评价材料。此时的冷却速度大概为约100℃/秒。
另外，对于进行了盐浴软氮化处理的试验片1或6，在电炉内在800℃进行5分钟或30分钟的加热(电炉加热)。加热后，将试验片1或6水冷或油冷，制作了No.13～15的评价材料。
对于进行了盐浴软氮化处理的试验片6，使用高频电源装置(最大输出功率：30kW；频率：70kHz)在800℃加热0.5～5分钟(IH)。加热后，将试验片6油冷，制作了No.16～18的评价材料。
对于No.11～18的评价材料，与上述同样地进行了特性的评价。将其结果示于表3。
表3
Figure BDA0002839060870000101
No.19～26的评价材料的制作
与上述同样地，将进行了盐浴软氮化处理的试验片1～7利用光学显微镜和EPMA分析进行观察。光学显微镜的观察的结果，可确认以距表面约15μm的厚度形成铁氮化合物层，在铁氮化合物层的下方以约200μm的厚度形成氮扩散层。对于进行了盐浴软氮化处理的试验片1～7，在850℃进行5分钟的盐浴加热后，进行水冷或油冷，制作了No.19和No.21～26的评价材料。另外，对于进行了盐浴软氮化材料的试验片6，在850℃进行5分钟的盐浴加热后，放置于20℃的房间，冷却至20℃，制作了No.20的评价材料。此时的冷却速度大概为约10℃/秒。对于No.19～26的评价材料，与上述同样地进行了特性的评价。将其结果示于表4。
表4
Figure BDA0002839060870000111

Claims (5)

1.表面硬化材料的制造方法，包括：
将表面固溶有氮的钢铁材料在包含氯化物的熔融物中在650℃～900℃的范围内进行浸渍的浸渍步骤，和
将浸渍了的上述钢铁材料以马氏体相变开始的下部临界冷却速度以上的冷却速度冷却至马氏体相变开始温度以下的冷却步骤。
2.权利要求1所述的表面硬化材料的制造方法，其中，表面固溶有氮的钢铁材料还包含铁氮化合物层作为表层。
3.权利要求1或2所述的表面硬化材料的制造方法，还包括：对钢铁材料进行氮化处理从而将氮固溶于表面的氮化处理步骤。
4.权利要求1或2所述的表面硬化材料的制造方法，其中，表面固溶有氮的钢铁材料在表面还固溶有碳。
5.权利要求3所述的表面硬化材料的制造方法，其中，在上述氮化处理步骤前，还包括：对钢铁材料实施渗碳处理的渗碳处理步骤。
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