CN107385386A - A kind of high rigidity, high infiltration rate and big infiltration layer salt bath B-V co-penetrant and co-penetration technology - Google Patents
A kind of high rigidity, high infiltration rate and big infiltration layer salt bath B-V co-penetrant and co-penetration technology Download PDFInfo
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- 238000001764 infiltration Methods 0.000 title claims abstract description 73
- 150000003839 salts Chemical class 0.000 title claims abstract description 56
- 230000008595 infiltration Effects 0.000 title abstract description 24
- AUVPWTYQZMLSKY-UHFFFAOYSA-N boron;vanadium Chemical compound [V]#B AUVPWTYQZMLSKY-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 47
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 10
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 9
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910001626 barium chloride Inorganic materials 0.000 claims abstract description 8
- 229910021538 borax Inorganic materials 0.000 claims abstract description 8
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 8
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 8
- 229910000831 Steel Inorganic materials 0.000 claims description 17
- 239000010959 steel Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000002474 experimental method Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000956 alloy Substances 0.000 claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 239000010431 corundum Substances 0.000 claims description 5
- 238000010791 quenching Methods 0.000 claims description 5
- 230000000171 quenching effect Effects 0.000 claims description 5
- 239000000565 sealant Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052796 boron Inorganic materials 0.000 abstract description 6
- 229910052720 vanadium Inorganic materials 0.000 abstract description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 5
- 230000003670 easy-to-clean Effects 0.000 abstract description 4
- 239000013040 bath agent Substances 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- 229910052810 boron oxide Inorganic materials 0.000 abstract description 2
- 229910052580 B4C Inorganic materials 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 235000013024 sodium fluoride Nutrition 0.000 abstract 1
- 239000011775 sodium fluoride Substances 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 238000005496 tempering Methods 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 238000005271 boronizing Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces
- C23C12/02—Diffusion in one step
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Abstract
一种高硬度、高渗速及大渗层盐浴硼钒共渗剂及工艺，其特征是所述的共渗剂是以氧化硼为基盐的盐浴硼钒共渗剂，主要由氧化硼、氟化钠、碳化硼、氯化钡、五氧化二钒按一定的质量百分比组成。工艺是把工件表面抛光、清洗后放入装有盐浴剂的坩埚中，在950℃环境中，保温4h，进行硼钒共渗。本发明得到的共渗层厚度为167µm～182µm，平均渗速可达到41.75～45.5μm/h，其渗速是传统共渗剂的2～3倍。表面显微硬度可达到2481.9～2849.5HV之间，是以硼砂为基盐的2～3倍，是基体硬度的6～7倍。渗层与基体的呈冶金结合，其结合力可达到63N。摩擦系数可降至0.13，耐磨性得到大幅度提升。并且渗处理后的工件的残盐极易清理。可广泛应用表面需要高耐磨、高硬度的零部件，有很大的经济效益。
A salt-bath boron-vanadium co-penetration agent with high hardness, high permeation speed and large permeation layer and its technology is characterized in that the co-penetration agent is a salt bath boron-vanadium co-penetration agent with boron oxide as the base salt, mainly composed of oxidation Boron, sodium fluoride, boron carbide, barium chloride and vanadium pentoxide are composed according to a certain mass percentage. The process is to polish and clean the surface of the workpiece, put it into a crucible with salt bath agent, keep it warm for 4 hours in an environment of 950 ° C, and carry out co-infiltration of boron and vanadium. The co-infiltration layer obtained by the invention has a thickness of 167µm to 182µm, and an average infiltration rate of 41.75 to 45.5µm/h, which is 2 to 3 times that of traditional co-infiltration agents. The surface microhardness can reach between 2481.9 and 2849.5HV, which is 2 to 3 times that of borax as the base salt and 6 to 7 times that of the matrix. The metallurgical bond between the infiltrated layer and the substrate can reach 63N. The coefficient of friction can be reduced to 0.13, and the wear resistance is greatly improved. And the residual salt of the workpiece after infiltration treatment is very easy to clean. It can be widely used in parts that require high wear resistance and high hardness on the surface, and has great economic benefits.
Description
技术领域technical field
本发明涉及化学热处理领域，尤其是一种硼钒共渗剂的配方及共渗工艺，具体来说是一种通过化学热扩散反应沉积的方法在合金模具钢表面制备高硬度、高渗速及大渗层及其他优异性能的硼钒共渗层。The present invention relates to the field of chemical heat treatment, especially a formula of boron-vanadium co-infiltration agent and a co-infiltration process, specifically a method of chemical thermal diffusion reaction deposition to prepare high hardness, high infiltration rate and Large infiltration layer and other boron vanadium co-infiltration layer with excellent performance.
背景技术Background technique
合金模具钢由于其优异的综合性能广泛用于汽车零部件及模具制造。但在实际工作环境下，大部分的合金模具钢仍会因为表面过渡磨损发生失效。因此模具表面处理技术会直接涉及到模具制造性能、使用寿命等。其中TD盐浴渗金属技术由于具备设备简单、操作方便、生产成本低以及形成的渗层具有优异的性能而受到各国学者的青睐。盐浴渗钒和渗硼都能提高材料表面硬度和耐磨性，但是单一渗硼由于产生硼脆而使渗硼技术在应用上受到一定限制, 而单一渗钒又因渗层薄约10μm，不能呈受大负荷。盐浴硼钒共渗新工艺能够克服硼脆钒薄，而又具有比单渗层更高的硬度及低的摩擦系数和良好的耐磨性。应用于模具、汽车零件等领域上可以取得明显的技术经济效益。所谓硼钒共渗就是同时向钢表面渗入金属钒和硼原子的工艺过程。Alloy die steel is widely used in auto parts and die manufacturing due to its excellent comprehensive properties. However, in the actual working environment, most alloy die steels will still fail due to excessive surface wear. Therefore, the mold surface treatment technology will directly relate to the mold manufacturing performance and service life. Among them, the TD salt bath infiltration technology is favored by scholars from all over the world because of its simple equipment, convenient operation, low production cost and excellent performance of the formed infiltration layer. Both salt bath vanadium and boronizing can improve the surface hardness and wear resistance of the material, but the single boronizing technology is limited in application due to boron brittleness, and the single vanadiumizing is about 10μm thinner, Cannot be subjected to heavy loads. The new process of boron-vanadium co-infiltration in salt bath can overcome boron brittleness and vanadium thinness, and has higher hardness, low friction coefficient and good wear resistance than single infiltration layer. Applied in molds, auto parts and other fields can obtain obvious technical and economic benefits. The so-called co-infiltration of boron and vanadium is the process of infiltrating metal vanadium and boron atoms into the steel surface at the same time.
当前的TD盐浴渗金属技术在单渗中能获得比较理想的硬度及厚度，但是在共渗领域其效果就有明显的下降。而且以硼砂为基盐，虽然得到广泛应用但是其存在着所渗元素种类少、被渗工件材质种类少、渗温高、渗层薄、盐浴粘度大、工件粘盐多清洗残盐困难、设备（坩埚等）腐蚀严重等问题，严重限制了应用。为了解决传统TD处理中存在的问题本发明提出了一种以B2O3 为基盐的新型盐浴硼钒共渗剂。相比于传统盐浴剂通过新型硼钒共渗盐浴剂所置得的渗层拥有更高的硬度，渗速和渗层厚度得到很大提高，并且粘盐度降低工件易清理。对相关仪器设备的腐蚀性明显降低。而且具有很好的可操作性和巨大的经济价值。The current TD salt bath infiltration metal technology can obtain ideal hardness and thickness in single infiltration, but its effect is significantly reduced in the field of co-infiltration. Moreover, borax is used as the base salt, although it is widely used, but it has few types of elements to be infiltrated, few types of materials to be infiltrated, high infiltration temperature, thin infiltration layer, high viscosity of salt bath, and difficulty in cleaning residual salt due to sticky salt in the workpiece. Problems such as serious corrosion of equipment (crucible, etc.) seriously limit the application. In order to solve the problems existing in the traditional TD treatment, the present invention proposes a new salt bath boron vanadium co-penetration agent with B 2 O 3 as the base salt. Compared with the traditional salt bath agent, the infiltration layer prepared by the new boron-vanadium co-infiltration salt bath agent has higher hardness, the penetration rate and the thickness of the infiltration layer are greatly improved, and the viscosity and salinity are reduced, and the workpiece is easy to clean. Corrosion to related instruments and equipment is significantly reduced. And it has good operability and huge economic value.
发明内容Contents of the invention
本发明的目的是针对当前合金模具钢耐磨性不够的缺陷，提供了一种以B2O3为基盐的新型盐浴硼钒共渗剂及其共渗方法，新型共渗剂可极大的提高共渗层的硬度、厚度及渗速，且渗后工件残盐易于清理，对相关仪器设备的腐蚀性明显降低。具有很好的可操作性和巨大的经济价值。The purpose of the present invention is to provide a new salt bath boron-vanadium co-infiltration agent and its co-infiltration method with B 2 O 3 as the base salt for the defect that the current alloy mold steel has insufficient wear resistance. The new co-infiltration agent can be extremely Greatly improve the hardness, thickness and penetration rate of the co-infiltration layer, and the residual salt of the workpiece after infiltration is easy to clean, and the corrosion to related instruments and equipment is significantly reduced. It has good operability and great economic value.
本发明的技术方案之一是：One of technical solutions of the present invention is:
一种高硬度、高渗速及大渗层盐浴硼钒共渗剂，其特征在于：它是以氧化硼（B2O3）为基盐的盐浴硼钒共渗剂，主要由氧化硼（B2O3）、氟化钠（NaF）、碳化硼（B4C）、氯化钡（BaCl2）、五氧化二钒（V2O5）组成，其中，氧化硼（B2O3）的质量百分比为44~53.8%、氟化钠（NaF）的质量百分比为22.2~27.5%、五氧化二钒（V2O5）的质量百分比为4.4~4.5%、氯化钡（BaCl2）的质量百分比为4.4~5.3%、碳化硼（B4C）的质量百分比为8.4~25%；各组份的质量百分比之和为100%。A salt-bath boron-vanadium co-penetration agent with high hardness, high permeation rate and large permeation layer, characterized in that it is a salt bath boron-vanadium co-penetration agent based on boron oxide (B 2 O 3 ), mainly composed of oxidized Boron (B 2 O 3 ), sodium fluoride (NaF), boron carbide (B 4 C), barium chloride (BaCl 2 ), vanadium pentoxide (V 2 O 5 ), among which boron oxide (B 2 The mass percentage of O 3 ) is 44~53.8%, the mass percentage of sodium fluoride (NaF) is 22.2~27.5%, the mass percentage of vanadium pentoxide (V 2 O 5 ) is 4.4~4.5%, barium chloride ( The mass percentage of BaCl 2 ) is 4.4-5.3%, and the mass percentage of boron carbide (B 4 C) is 8.4-25%; the sum of the mass percentages of each component is 100%.
用B2O3取代传统的硼砂，因B2O3在高温条件下具有很好的溶解碱性金属氧化物的性质，且相比于硼砂，B2O3在反应中腐蚀性不强能制备出表面质量更好的渗层；所述B2O3为分析纯，其含量大于90%；B4C为化学纯，其含量大于99%；V2O5 为分析纯，其含量为99.9%。Use B 2 O 3 to replace traditional borax, because B 2 O 3 has good properties of dissolving alkaline metal oxides under high temperature conditions, and compared with borax, B 2 O 3 is less corrosive in the reaction. A better surface quality infiltration layer is prepared; the B 2 O 3 is analytically pure, and its content is greater than 90%; B 4 C is chemically pure, and its content is greater than 99%; V 2 O 5 is analytically pure, and its content is 99.9%.
本发明的技术方案之二是：The second technical scheme of the present invention is:
一种基于高硬度、高渗速及大渗层盐浴硼钒共渗剂的合金模具钢表面盐浴硼钒共渗方法，其特征在于它包括以下步骤：A salt-bath boron-vanadium co-penetration method on the surface of alloy die steel based on high hardness, high permeation rate and large permeation layer salt bath boron-vanadium co-penetration agent is characterized in that it comprises the following steps:
（1）按照上述盐浴硼钒共渗剂配方中的质量百分比称量原料并机械混合均匀后放入坩埚中备用；(1) Weigh the raw materials according to the mass percentage in the formula of the above-mentioned salt-bath boron-vanadium co-infiltration agent, mix them uniformly and put them into the crucible for later use;
（2）基体材料预处理：基体材料选用42CrMo钢，首先将原材料线切割成10×10×3mm大小的试样，表面经除油、去离子水清洗后进行砂纸打磨和机械抛光，将表面抛至粗糙度为Ra1μm，然后丙酮超声波清洗至注10min、乙醇冲洗吹干，制得试样；(2) Base material pretreatment: 42CrMo steel is selected as the base material. Firstly, the raw material is wire-cut into 10×10×3mm samples. Raw to a roughness of Ra 1 μm, then ultrasonically cleaned with acetone for 10 minutes, rinsed with ethanol and dried to obtain a sample;
（3）硼钒共渗处理：将装有盐浴硼钒共剂的坩埚放入箱式电阻炉中，加热至1000±50℃，保温15±5 min使盐浴硼钒共剂融解均匀，然后降温至共渗温度950℃，制得硼钒共渗剂；将试样放入配备好的硼钒共渗盐浴内，并使试样的主要工作面尽量保持与盐浴流动方向垂直，保温一定时间4±0.5h取出油淬，即在42CrMo钢表面制得硼钒层；(3) Boron-vanadium co-infiltration treatment: put the crucible containing the salt bath boron-vanadium co-agent into a box-type resistance furnace, heat it to 1000±50°C, and keep it warm for 15±5 minutes to melt the salt-bath boron-vanadium co-agent evenly. Then lower the temperature to a co-infiltration temperature of 950°C to prepare a boron-vanadium co-infiltration agent; put the sample into the prepared boron-vanadium co-infiltration salt bath, and keep the main working surface of the sample perpendicular to the flow direction of the salt bath as much as possible. After holding for a certain time of 4±0.5h, take out the oil quenching, that is, a boron-vanadium layer is made on the surface of 42CrMo steel;
（4）清洗试样：轻轻敲击试样，使其表面残盐脱落，若仍有残盐粘附，可用水浴箱加热至100℃煮1±0.5h左右即可；(4) Clean the sample: gently tap the sample to make the residual salt off the surface, if there is still residual salt adhered, it can be heated to 100°C in a water bath and boiled for about 1±0.5h;
实验前将配好的硼钒共渗剂混合均匀置于刚玉坩埚中加盖，再用高温密封胶密封放入烘箱中于100℃保温45min烘干。试验后将取出的试样进行油淬，试样表面清洗干净后在180℃下回火2h。Before the experiment, mix the prepared boron-vanadium co-infiltration agent evenly, place it in a corundum crucible and cover it, then seal it with high-temperature sealant and put it in an oven at 100°C for 45 minutes to dry. After the test, the sample taken out was oil quenched, the surface of the sample was cleaned and tempered at 180°C for 2 hours.
本发明的有益效果是：The beneficial effects of the present invention are:
（1）本发明提供了一种高硬度、高渗速及大渗层的新型盐浴硼钒共渗剂配方。在以42CrMo钢为基体、950℃保温4h条件下，渗层外表层显微硬度200gf压力下可达到2481.9～2849.5HV之间，是以硼砂为基盐得到渗层的的1.5～2倍，是基体硬度的6～7倍。(1) The present invention provides a new formula of salt bath boron-vanadium co-penetration agent with high hardness, high permeation rate and large permeation layer. Under the conditions of 42CrMo steel as the substrate and 950°C for 4 hours, the microhardness of the outer layer of the infiltrated layer can reach between 2481.9 and 2849.5HV under the pressure of 200gf, which is 1.5 to 2 times that of the infiltrated layer obtained with borax as the base salt. 6 to 7 times the hardness of the matrix.
（2）采用该法在工件上得到的渗层厚度大、渗速快，在以42CrMo钢为基体、950℃保温4h条件下，其渗层最大厚度可达到167～182μm,平均渗速可达到41.75～45.5μm/h。其渗速是传统共渗剂的2～3倍。(2) The thickness of the infiltration layer obtained on the workpiece by this method is large and the infiltration rate is fast. Under the condition of using 42CrMo steel as the substrate and holding at 950°C for 4 hours, the maximum thickness of the infiltration layer can reach 167-182 μm, and the average infiltration rate can reach 41.75～45.5μm/h. Its permeation rate is 2 to 3 times that of traditional permeation agents.
（3）并且在本共渗剂下得到的渗层界面结合较好，与基体呈冶金结合，在实施例一种其渗层与基体的结合力可达到63N，摩擦磨损系数降至0.13，耐磨性得到很大的提高。(3) In addition, the interfacial bonding of the infiltrated layer obtained under this co-infiltration agent is better, and it is metallurgically bonded to the substrate. In Example 1, the bonding force between the infiltrated layer and the substrate can reach 63N, and the friction and wear coefficient is reduced to 0.13. Grinding has been greatly improved.
（4）本发明提供的硼钒共渗剂，无任何毒性，对周围环境无任何污染。且减少了硼钒共渗剂对坩埚及夹具的腐蚀。(4) The boron-vanadium co-penetration agent provided by the present invention has no toxicity and no pollution to the surrounding environment. Moreover, the corrosion of the crucible and the fixture by the boron-vanadium co-infiltration agent is reduced.
（5）本发明得到的共渗层厚度为167µm～182µm，平均渗速可达到41.75～45.5μm/h，其渗速是传统共渗剂的2～3倍。表面显微硬度可达到2481.9～2849.5HV之间，是以硼砂为基盐的2～3倍，是基体硬度的6～7倍。渗层与基体的呈冶金结合，其结合力可达到63N。摩擦系数可降至0.13，耐磨性得到大幅度提升。并且渗处理后的工件的残盐极易清理。可广泛应用表面需要高耐磨、高硬度的零部件，有很大的经济效益。(5) The thickness of the co-infiltration layer obtained by the present invention is 167µm to 182µm, and the average penetration rate can reach 41.75 to 45.5μm/h, which is 2 to 3 times that of the traditional co-infiltration agent. The surface microhardness can reach between 2481.9 and 2849.5HV, which is 2 to 3 times that of borax as the base salt and 6 to 7 times that of the matrix. The metallurgical bond between the infiltrated layer and the substrate can reach 63N. The coefficient of friction can be reduced to 0.13, and the wear resistance is greatly improved. And the residual salt of the workpiece after infiltration treatment is very easy to clean. It can be widely used in parts that require high wear resistance and high hardness on the surface, and has great economic benefits.
附图说明Description of drawings
图1是实施例一的试样实验后硼钒共渗层的横截面化染SEM形貌图。Fig. 1 is a cross-sectional chemically dyed SEM topography diagram of the boron-vanadium co-infiltrated layer after the sample experiment of Example 1.
图2是实施例一的试样实验后硼钒共渗层表面XRD图谱。Fig. 2 is the XRD spectrum of the surface of the boron-vanadium co-infiltrated layer after the experiment of the sample of Example 1.
图3是实施例一的试样实验后硼钒共渗层与基体的界面结合力图。Fig. 3 is a diagram of the interface bonding force between the boron-vanadium co-infiltrated layer and the substrate after the sample experiment of the first embodiment.
图4是实施例一的试样实验后硼钒共渗层的摩擦系数随摩擦磨损实验进行时间的变化。Fig. 4 is the variation of the friction coefficient of the boron-vanadium co-infiltrated layer with the time of the friction and wear experiment after the sample experiment of the first embodiment.
图5是实施例一的试样实验后硼钒共渗层摩擦磨损SEM图。Fig. 5 is the SEM diagram of the friction and wear of the boron-vanadium co-infiltrated layer after the test of the sample of the first embodiment.
图6是实施例二的试样实验后硼钒共渗层的横截面化染SEM形貌图。Fig. 6 is a cross-sectional chemically dyed SEM topography diagram of the boron-vanadium co-infiltrated layer after the sample experiment of the second embodiment.
图7是实施例三的试样实验后硼钒共渗层的横截面化染SEM形貌图。Fig. 7 is a cross-sectional chemically dyed SEM topography diagram of the boron-vanadium co-infiltrated layer of the sample in Example 3 after the experiment.
具体实施方式：detailed description:
下面结合附图和实例对本发明作进一步的说明。The present invention will be further described below in conjunction with accompanying drawings and examples.
实施例一。Embodiment one.
如图1-5所示As shown in Figure 1-5
本实施例的盐浴硼钒共渗剂由氧化硼（B2O3）53.8g、氟化钠（NaF）27.5g、五氧化二钒（V2O5）5g、氯化钡（BaCl2）5.3g、碳化硼（B4C）8.4g组成，将配好的硼钒共渗剂机械混合均匀后置于刚玉坩埚中加盖，再用高温密封胶密封放入烘箱中于100±10℃保温45±5min烘干。The salt-bath boron-vanadium co-penetration agent of this example is composed of 53.8g of boron oxide (B 2 O 3 ), 27.5g of sodium fluoride (NaF), 5g of vanadium pentoxide (V 2 O 5 ), barium chloride (BaCl 2 ) 5.3g, boron carbide (B 4 C) 8.4g, mechanically mix the prepared boron vanadium co-infiltration agent, put it in a corundum crucible and cover it, then seal it with high temperature sealant and put it in an oven at 100±10 ℃ heat preservation 45±5min drying.
（1）基体材料预处理：本发明基体材料选用42CrMo钢，首先将原材料线切割成10×10×3mm大小的试样，表面经除油、去离子水清洗后进行砂纸打磨和机械抛光，将表面抛至粗糙度为Ra1μm，然后丙酮超声波清洗10min、乙醇冲洗吹干，制得试样；(1) Base material pretreatment: the base material of the present invention selects 42CrMo steel, first the raw material is wire-cut into 10 × 10 × 3mm samples, the surface is degreased and deionized water is cleaned and then sanded and mechanically polished. Polish the surface until the roughness is Ra 1 μm, then ultrasonically clean with acetone for 10 minutes, rinse and dry with ethanol to prepare the sample;
（2）硼钒共渗处理：将装有盐浴硼钒共剂的坩埚放入箱式电阻炉中，加热至1000±50℃，保温15±5 min使盐浴硼钒共剂融解均匀，然后降温至共渗温度950℃，制得硼钒共渗剂；将试样放入配备好的硼钒共渗盐浴内，并使试样的主要工作面尽量保持与盐浴流动方向垂直，保温一定时间4±0.5h取出油淬，即在42CrMo钢表面制得硼钒层；(2) Boron-vanadium co-infiltration treatment: Put the crucible containing the salt bath boron-vanadium co-agent into a box-type resistance furnace, heat it to 1000±50°C, and keep it warm for 15±5 minutes to melt the salt-bath boron-vanadium co-agent evenly. Then lower the temperature to a co-infiltration temperature of 950°C to prepare a boron-vanadium co-infiltration agent; put the sample into the prepared boron-vanadium co-infiltration salt bath, and keep the main working surface of the sample perpendicular to the flow direction of the salt bath as much as possible. After holding for a certain time of 4±0.5h, take out the oil quenching, that is, a boron-vanadium layer is made on the surface of 42CrMo steel;
（4）清洗试样：轻轻敲击试样，使其表面残盐脱落，若仍有残盐粘附，可用水浴箱加热至100℃煮1h左右即可；具体实施时如果在试样表面清洗干净后再进行180℃+ 2h回火，则效果更佳。(4) Clean the sample: gently tap the sample to make the residual salt on the surface fall off. If there is still residual salt adhered, it can be heated to 100°C in a water bath for about 1 hour; After cleaning and tempering at 180°C + 2h, the effect will be better.
取出样品后进行检测：经检测硼钒共渗层的最大厚度为167μm,共渗层外表层显微硬度100gf压力下为2481.9HV。共渗层的物相组成VO、 V4C2.67、 Fe2C、Fe2B、VCXOZ，基体与共渗层的界面结合力为63N，摩擦系数基本保持在0.13且磨损量很小。如图1-5所示。The samples were taken out for testing: the maximum thickness of the boron-vanadium co-infiltration layer was detected to be 167 μm, and the microhardness of the outer layer of the co-infiltration layer was 2481.9HV under a pressure of 100gf. The phase composition of the co-infiltration layer is VO, V 4 C 2.67 , Fe 2 C, Fe 2 B, VC X O Z , the interfacial bonding force between the substrate and the co-infiltration layer is 63N, the friction coefficient is basically maintained at 0.13 and the wear amount is small. As shown in Figure 1-5.
实施例二。Embodiment two.
如图6所示。As shown in Figure 6.
本实施例的盐浴硼钒共渗剂由氧化硼（B2O3）47g、氟化钠（NaF）23.6g、五氧化二钒（V2O5）4.7g、氯化钡（BaCl2）4.7g、碳化硼（B4C）20g组成，将配好的硼钒共渗剂机械混合均匀后置于刚玉坩埚中加盖，再用高温密封胶密封放入烘箱中于100±10℃保温45±5min烘干。The salt-bath boron-vanadium co-penetration agent of this example consists of 47g of boron oxide (B 2 O 3 ), 23.6g of sodium fluoride (NaF), 4.7g of vanadium pentoxide (V 2 O 5 ), barium chloride (BaCl 2 ) 4.7g, boron carbide (B 4 C) 20g, mechanically mix the prepared boron vanadium co-infiltration agent, put it in a corundum crucible and cover it, then seal it with high temperature sealant and put it in an oven at 100±10℃ Keep warm for 45±5min and dry.
（1）基体材料预处理：本发明基体材料选用42CrMo钢，首先将原材料线切割成10×10×3mm大小的试样，表面经除油、去离子水清洗后进行砂纸打磨和机械抛光，将表面抛至粗糙度为Ra1μm，然后丙酮超声波清洗10min、乙醇冲洗吹干，制得试样；(1) Base material pretreatment: the base material of the present invention selects 42CrMo steel, first the raw material is wire-cut into 10 × 10 × 3mm samples, the surface is degreased and deionized water is cleaned and then sanded and mechanically polished. Polish the surface until the roughness is Ra 1 μm, then ultrasonically clean with acetone for 10 minutes, rinse and dry with ethanol to prepare the sample;
（2）硼钒共渗处理：将装有盐浴硼钒共剂的坩埚放入箱式电阻炉中，加热至1000℃，保温15 min使盐浴硼钒共剂融解均匀，然后降温至共渗温度950℃，制得硼钒共渗剂；将试样放入配备好的硼钒共渗盐浴内，并使试样的主要工作面尽量保持与盐浴流动方向垂直，保温一定时间4h取出油淬，即在42CrMo钢表面制得硼钒层；(2) Boron-vanadium co-infiltration treatment: Put the crucible containing the salt bath boron-vanadium co-agent into a box-type resistance furnace, heat it to 1000°C, and keep it warm for 15 minutes to melt the salt-bath boron-vanadium co-agent evenly, and then cool down to a total The infiltration temperature is 950°C to prepare the boron-vanadium co-infiltration agent; put the sample into the prepared boron-vanadium co-infiltration salt bath, and keep the main working surface of the sample perpendicular to the flow direction of the salt bath as far as possible, and keep it for a certain period of time for 4 hours Take out the oil quenching, that is, make a boron vanadium layer on the surface of 42CrMo steel;
（4）清洗试样：轻轻敲击试样，使其表面残盐脱落，若仍有残盐粘附，可用水浴箱加热至100℃煮1h左右即可；具体实施时如果在试样表面清洗干净后再进行180℃+ 2h回火，则效果更佳。(4) Clean the sample: gently tap the sample to make the residual salt on the surface fall off. If there is still residual salt adhered, it can be heated to 100°C in a water bath for about 1 hour; After cleaning and tempering at 180°C + 2h, the effect will be better.
取出样品后进行检测：经检测硼钒共渗层的最大厚度为180μm,共渗层外表层显微硬度100gf压力下为2604.9HV，渗层物相组成及其他性能和实施例一相似。The sample was taken out and tested: the maximum thickness of the boron-vanadium co-infiltrated layer was 180 μm, and the microhardness of the outer layer of the co-infiltrated layer was 2604.9 HV under a pressure of 100 gf. The phase composition and other properties of the infiltrated layer were similar to those in Example 1.
实施例三。Embodiment three.
如图7所示。As shown in Figure 7.
所采用硼钒共渗剂由氧化硼（B2O3）44g、氟化钠（NaF）22.2g、五氧化二钒（V2O5）4.4g、氯化钡（BaCl2）4.4g、碳化硼（B4C）25g组成，将配好的硼钒共渗剂机械混合均匀后置于刚玉坩埚中加盖，再用高温密封胶密封放入烘箱中于100±10℃保温45±5min烘干。The boron-vanadium co-penetration agent used is composed of boron oxide (B 2 O 3 ) 44g, sodium fluoride (NaF) 22.2g, vanadium pentoxide (V 2 O 5 ) 4.4g, barium chloride (BaCl 2 ) 4.4g, Boron carbide (B 4 C) 25g, mechanically mix the prepared boron-vanadium co-infiltration agent, put it in a corundum crucible and cover it, then seal it with high-temperature sealant and put it in an oven at 100±10°C for 45±5min drying.
（1）基体材料预处理：本发明基体材料选用42CrMo钢，首先将原材料线切割成10×10×3mm大小的试样，表面经除油、去离子水清洗后进行砂纸打磨和机械抛光，将表面抛至粗糙度为Ra1μm，然后丙酮超声波清洗10min、乙醇冲洗吹干，制得试样；(1) Base material pretreatment: the base material of the present invention selects 42CrMo steel, first the raw material is wire-cut into 10 × 10 × 3mm samples, the surface is degreased and deionized water is cleaned and then sanded and mechanically polished. Polish the surface until the roughness is Ra 1 μm, then ultrasonically clean with acetone for 10 minutes, rinse and dry with ethanol to prepare the sample;
（2）硼钒共渗处理：将装有盐浴硼钒共剂的坩埚放入箱式电阻炉中，加热至1000℃，保温15 min使盐浴硼钒共剂融解均匀，然后降温至共渗温度950℃，制得硼钒共渗剂；将试样放入配备好的硼钒共渗盐浴内，并使试样的主要工作面尽量保持与盐浴流动方向垂直，保温一定时间4h取出油淬，即在42CrMo钢表面制得硼钒层；(2) Boron-vanadium co-infiltration treatment: Put the crucible containing the salt bath boron-vanadium co-agent into a box-type resistance furnace, heat it to 1000°C, and keep it warm for 15 minutes to melt the salt-bath boron-vanadium co-agent evenly, and then cool down to a total The infiltration temperature is 950°C to prepare the boron-vanadium co-infiltration agent; put the sample into the prepared boron-vanadium co-infiltration salt bath, and keep the main working surface of the sample perpendicular to the flow direction of the salt bath as far as possible, and keep it for a certain period of time for 4 hours Take out the oil quenching, that is, make a boron vanadium layer on the surface of 42CrMo steel;
（4）清洗试样：轻轻敲击试样，使其表面残盐脱落，若仍有残盐粘附，可用水浴箱加热至100℃煮1h左右即可；具体实施时如果在试样表面清洗干净后再进行180℃+ 2h回火，则效果更佳。(4) Clean the sample: gently tap the sample to make the residual salt on the surface fall off. If there is still residual salt adhered, it can be heated to 100°C in a water bath for about 1 hour; After cleaning and tempering at 180°C + 2h, the effect will be better.
取出样品后进行检测：经检测硼钒共渗层的最大厚度为182μm,共渗层外表层显微硬度100gf压力下为2849.5HV，渗层物相组成及其他性能和实施例一相似。The sample was taken out and tested: the maximum thickness of the boron-vanadium co-infiltrated layer was 182 μm, and the microhardness of the outer layer of the co-infiltrated layer was 2849.5 HV under a pressure of 100 gf. The phase composition and other properties of the infiltrated layer were similar to those in Example 1.
本发明未涉及部分均于现有技术相同或可采用现有技术加以实现。The parts not involved in the present invention are the same as the prior art or can be realized by adopting the prior art.
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