阅读说明：本技术 一种陶瓷增强合金中纳米陶瓷相的高通量优选方法 (High-flux optimization method for nano ceramic phase in ceramic reinforced alloy ) 是由 罗晋如 龚星宇 董武梅 王长浩 邓林 于 2021-05-24 设计创作，主要内容包括：本发明公开一种陶瓷增强合金中纳米陶瓷相的高通量优选方法,包括以下步骤：S1：将不锈钢基底粉末分别与不同成分和配比的纳米粉体机械混合制备多种混合粉末；S2：采用激光熔覆法将多种混合粉末按成分梯度分区打印成板状单臂样品；S3：将单臂样品切割成楔形结构,经高温保温处理后使用普通热辊轧机进行单道次平轧,获得不同变形量条件下的厚度一致的轧制板材；S4：采用网格逐点打硬度的方法对样品不同成分部分在不同变形量处的强化程度进行评估；通过制备具有梯度成分的坯料,并联用楔形轧制法制备同时具有成分和变形量梯度的样品板材,采用逐点硬度法筛选维氏硬度值最高的合金成分与变形量,有助于陶瓷相增强合金中增强相的快速优选。(The invention discloses a high-flux optimization method of a nano ceramic phase in a ceramic reinforced alloy, which comprises the following steps: s1: mechanically mixing stainless steel base powder with nano-powder with different components and proportions to prepare various mixed powders; s2: printing a plurality of mixed powders into a plate-shaped single-arm sample according to component gradient partitions by adopting a laser cladding method; s3: cutting a single-arm sample into a wedge-shaped structure, carrying out high-temperature heat preservation treatment, and then carrying out single-pass flat rolling by using a common hot rolling mill to obtain rolled plates with consistent thickness under the conditions of different deformation amounts; s4: evaluating the strengthening degree of different component parts of the sample at different deformation positions by adopting a method of punching hardness point by a grid; the method is characterized in that a blank with gradient components is prepared, a wedge rolling method is used for preparing a sample plate with gradient components and deformation, and the alloy component with the highest Vickers hardness value and the deformation are screened by a point-by-point hardness method, so that the rapid optimization of the reinforced phase in the ceramic phase reinforced alloy is facilitated.)

1. A high flux optimization method for a nanoceramic phase in a ceramic reinforced alloy, comprising the steps of:

s1: mechanically mixing stainless steel base powder with nano-powder with different components and proportions to prepare various mixed powders;

s2: printing a plurality of mixed powders into a plate-shaped single-arm sample according to component gradient partitions by adopting a laser cladding method;

s3: cutting a single-arm sample into a wedge-shaped structure, carrying out high-temperature heat preservation treatment, and then carrying out single-pass flat rolling by using a common hot rolling mill to obtain rolled plates with consistent thickness under the conditions of different deformation amounts;

s4: and evaluating the strengthening degree of different component parts of the sample at different deformation positions by adopting a method of punching hardness point by using a grid.

2. The high throughput optimization method for nano ceramic phases in ceramic reinforced alloy according to claim 1, wherein the rolling direction is vertical in step S3In the direction of component gradient, the rolling temperature is 1100-1200 ℃, and the rolling strain rate is 1-10s^-1。

3. The high throughput optimization method for nano ceramic phases in ceramic reinforced alloy according to claim 1, wherein hardness grid points are distributed along the gradient direction of deformation amount at the center of the composition in step S4, and the strengthening effect is evaluated by using hardness method.

4. High throughput optimization method of nanoceramic phases in ceramic reinforced alloys according to claim 1, characterized in that in step S1 stainless steel base powder is prepared by gas atomization powdering.

5. The high-flux optimization method for the nano-ceramic phase in the ceramic-reinforced alloy according to claim 1, wherein in step S1, 4 kinds of nano-powders with different component ratios are selected to prepare 4 kinds of different mixed powders, which are respectively: fe powder, Fe powder + 0.5% Y nano powder, Fe powder + 0.5% Y2O3 nano powder, Fe powder + 0.5% Y nano powder and 2% TiC nano powder.

6. The high-flux optimization method for the nano-ceramic phase in the ceramic-reinforced alloy as claimed in claim 1, wherein in step S2, a 1070nm wavelength yttrium-doped fiber laser is used as a heat source, a synchronous powder-feeding laser additive manufacturing system is used to feed powder through a coaxial three-way powder-feeding nozzle under the protection of high-purity argon, a plate-shaped single arm member is laser-clad and printed layer by layer under the parameter conditions of laser power of 600-.

7. The high throughput optimization method for nano ceramic phase in ceramic reinforced alloy according to claim 1, wherein in step S3, the single arm sample is cut into wedge shaped plate with 5-10 ° top angle.

8. The high throughput optimization method for the nanoceramic phase in the ceramic-reinforced alloy according to claim 1, wherein in step S4, the surface of the rolled sample is divided into grids with deformation, wherein the grids are divided into 10%, 20%, 30%, 40%, 50%, 60%, 70% deformation along the gradient direction of the deformation at the center of the composition, and each grid is printed with 5 hardness points, i.e. top, middle, bottom, left, and right, by using a vickers hardness tester, and then the average hardness is determined.

Technical Field

The invention relates to the field of ceramic reinforced alloy structure design, laser cladding and rolling processing, in particular to a high-flux optimization method for a nano ceramic phase in a ceramic reinforced alloy.

Background

The introduction of high-melting-point nano ceramic phase in the alloy to pin the grain boundary is an important idea for improving the high-temperature structure stability of the material, improving the high-temperature service performance and designing the structure of a novel high-temperature service structure material. The type, content, size, density and distribution of the ceramic reinforcing phase are key factors influencing the mechanical performance of the material, so that in the ceramic reinforced alloy, the influence of different reinforcing phases on the mechanical performance of the ceramic reinforcing material is determined to be one of the most important problems in designing the ceramic phase according to different mechanical performance requirements of the material under different service environments.

Carbides, nitrides and oxides are the most common three types of ceramic phases in the current ceramic reinforced alloy, and different ceramic phases can make the material obtain different performance performances due to different melting points, matching of a second phase and a substrate interface and the like. Carbides are generally of the two types M23C6 and MX in steel. M23C6 is easy to age and grow at high temperature, and coarse M23C6 carbide induces creep holes, so that creep rupture and irradiation ductile-brittle transition temperature (DBTT) are increased sharply. Compared with carbide, the thermal stability of the nanometer MX-type nitride is generally higher than that of the carbide, the nanometer MX-type nitride has better matrix wettability than that of oxide, and the coarsening rate at high temperature is lower, so that the steel has higher high-temperature structure stability and better high-temperature mechanical performance. When the nitrogen content in the steel is too high, coarse spherical CrVTiN composite nitrides and coarse Z-phase precipitates with CrNbN as a main component are easily formed, and simultaneously, the precipitation of XM type nitrides is reduced, and the two coarse complex nitrides are easy to coarsen in the service process and have small effect on stable structures. The thermal stability of XM type nitrides such as NbN, TaN, VN and the like is high, and three elements of Nb, Ta and V are often added into steel to fix nitrogen so as to reduce the reduction of impact toughness caused by easily segregated solid solution nitrogen. TiN in XM-type nitrides is likely to form coarse inclusions, and thus serves as a crack source during impact and reduces impact toughness, and therefore, it is also necessary to avoid the formation thereof. The free energy of formation of the oxide is larger than that of carbide and nitride, and the steel has higher thermodynamic stability compared with a main precipitation strengthening phase in the traditional steel melting process, and oxide particles with stable chemical structures and high melting points are introduced into a steel matrix in a large amount of ultrafine nano particles in a dispersing way through a special process, so that the high-temperature service capacity of the steel can be greatly improved, namely the nano oxide dispersion strengthened steel (ODS steel). The rare earth oxides such as Y2O3 and the like have stable physicochemical properties, have larger neutron absorption cross sections, still can stabilize pinning dislocation motion when being used in high-temperature, long-time and stress environments, improve the high-temperature tissue stability of the material, and Oxide Dispersion Strengthened (ODS) steel has excellent tissue stability when being aged at medium and low temperature (below 800 ℃) for a long time and at high temperature for a short time, has higher mechanical properties, is more stable in simulated irradiation of neutrons or heavy ions and electrons, and particularly has excellent radiation swelling resistance in a high He environment, so that Y2O3 is a better nano ceramic phase selection in the steel. However, the number density of the reinforcing phase is difficult to be increased to more than 1023 by adopting single type ceramic phase reinforcement, and further improvement of material performance is restricted, so that various types of nano ceramic phases are introduced to further improve the number density, increase the pinning mass point and carry out synergistic reinforcement, and the method becomes a new organizational design idea for further improving the reinforcement effect; therefore, there is a need for a high throughput optimization method for nanoceramic phases in ceramic-reinforced alloys that addresses the above-mentioned problems.

Disclosure of Invention

The invention aims to provide a high-flux optimization method of a nano ceramic phase in a ceramic reinforced alloy, which is characterized in that a blank with gradient components is prepared by a powder feeding laser cladding method, a sample plate with gradient components and deformation is prepared by a wedge rolling method in parallel, and an alloy component with the highest Vickers hardness value and deformation are screened by a point-by-point hardness method to predict the plate component with the best reinforcement effect and a rolling deformation process, so that the rapid optimization of the reinforced phase in the ceramic phase reinforced alloy is facilitated, the double reduction of research and development period and cost is realized, and the problems of complex component regulation and control, more preparation process parameters, long research and development period and high research and development cost of a ceramic reinforced composite material are solved.

The embodiment of the invention is realized by the following steps:

a high throughput optimization method for a nanoceramic phase in a ceramic reinforced alloy, comprising the steps of:

s1: mechanically mixing stainless steel base powder with nano-powder with different components and proportions to prepare various mixed powders;

s2: printing a plurality of mixed powders into a plate-shaped single-arm sample according to component gradient partitions by adopting a laser cladding method;

s3: cutting a single-arm sample into a wedge-shaped structure, carrying out high-temperature heat preservation treatment, and then carrying out single-pass flat rolling by using a common hot rolling mill to obtain rolled plates with consistent thickness under the conditions of different deformation amounts;

s4: and evaluating the strengthening degree of different component parts of the sample at different deformation positions by adopting a method of punching hardness point by using a grid. The method comprises the steps of preparing a blank with gradient components by a powder feeding laser cladding method, preparing a sample plate with gradient components and deformation by a wedge rolling method in parallel, screening an alloy component with the highest Vickers hardness value and deformation by a point-by-point hardness method to estimate the plate component with the best strengthening effect and a rolling deformation process, facilitating the rapid optimization of a strengthening phase in the ceramic phase strengthened alloy, realizing the dual reduction of research and development period and cost, and solving the problems of complex regulation and control of the components of the ceramic strengthened composite material, more preparation process parameters, long research and development period and high research and development cost.

Preferably, the rolling direction is perpendicular to the direction of the composition gradient in step S3, the rolling temperature is 1100-1200 ℃, and the rolling strain rate is 1-10S^-1。

Preferably, in step S4, the hardness grid points are distributed along the gradient direction of the deformation amount at the center of the composition, and the strengthening effect is evaluated by the hardness method.

Preferably, in step S1, the stainless steel base powder is prepared by a gas atomization powdering method.

Preferably, in step S1, 4 kinds of nanopowders with different composition ratios are selected to prepare 4 kinds of different mixed powders, which are: fe powder, Fe powder + 0.5% Y nano powder, Fe powder + 0.5% Y2O3 nano powder, Fe powder + 0.5% Y nano powder + 2% TiC nano powder.

Preferably, in step S2, a 1070nm wavelength yttrium-doped fiber laser is used as a heat source, a synchronous powder feeding laser additive manufacturing system is used to feed powder through a coaxial three-way powder feeding nozzle under the protection of high-purity argon gas, a laser power of 600-1000W, a spot diameter of 1.8mm, a scanning rate of 400mm/min, a lifting amount of 0.3mm, and a chamber water oxygen content of less than 10 × 10-6 are used to perform laser cladding layer by layer to print a plate-shaped single arm piece, and the plate-shaped single arm piece is printed layer by layer until a partitioned plate-shaped single arm sample is prepared.

Preferably, in step S3, the single-arm sample is cut into wedge-shaped boards having an apex angle of 5 to 10 °.

Preferably, in step S4, the surface of the rolled sample is divided into meshes of deformation amounts, and it is required to divide the meshes into 10%, 20%, 30%, 40%, 50%, 60%, 70% deformation amounts in the gradient direction of the deformation amount at the center of the composition, print 5 hardness points of upper, middle, lower, left, and right sides on each mesh by dot-by-dot printing using a vickers hardness tester, and then find the average hardness.

Due to the adoption of the technical scheme, the invention has the beneficial effects that: the invention discloses a high-flux optimization method of a nano ceramic phase in a ceramic reinforced alloy, which comprises the following steps of: s1: mechanically mixing stainless steel base powder with nano-powder with different components and proportions to prepare various mixed powders; s2: printing a plurality of mixed powders into a plate-shaped single-arm sample according to component gradient partitions by adopting a laser cladding method; s3: cutting a single-arm sample into a wedge-shaped structure, carrying out high-temperature heat preservation treatment, and then carrying out single-pass flat rolling by using a common hot roller mill to obtain rolled plates with consistent thickness under the conditions of different deformation amounts; s4: and evaluating the strengthening degree of different component parts of the sample at different deformation positions by adopting a method of punching hardness point by using a grid. The method comprises the steps of preparing a blank with gradient components by a powder feeding laser cladding method, preparing a sample plate with gradient components and deformation by a wedge rolling method in parallel, screening an alloy component with the highest Vickers hardness value and deformation by a point-by-point hardness method to pre-estimate the plate component with the best strengthening effect and a rolling deformation process, facilitating the rapid optimization of a strengthening phase in the ceramic phase strengthened alloy, realizing the dual reduction of research and development period and cost, and solving the problems of complex regulation and control of the components of the ceramic strengthened composite material, more preparation process parameters, long research and development period and high research and development cost.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and that for a person skilled in the art, other related drawings may be obtained from these drawings without inventive effort.

FIG. 1 is a schematic illustration of the composition distribution of a laser clad sample according to the present invention;

FIG. 2 is a schematic view of the wedge rolling mode of the present invention;

FIG. 3 is a graph showing the results of (a) hardness distribution and (b) phase structure analysis of samples having different compositions and different deformation amounts according to the present invention;

FIG. 4 is a flow chart of the steps in the present invention.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.

The following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without any inventive step, are within the scope of the present invention.

It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.

In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or the orientations or positional relationships that the products of the present invention usually place when in use, and are only used for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements referred to must have specific orientations, be constructed in specific orientations, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.

Furthermore, the terms "horizontal", "vertical", "suspended", and the like do not imply that the components are required to be absolutely horizontal or suspended, but may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.

In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.

Example 1: referring to fig. 1 to 4, the high flux optimization method for nano ceramic phase in ceramic reinforced alloy of the present embodiment includes the following steps: s1: mechanically mixing stainless steel base powder with nano-powder with different components and proportions to prepare various mixed powders; s2: adopting a laser cladding method to print various mixed powders into a plate-shaped single-arm sample according to component gradient partitions; s3: cutting a single-arm sample into a wedge-shaped structure, carrying out high-temperature heat preservation treatment, and then carrying out single-pass flat rolling by using a common hot rolling mill to obtain rolled plates with consistent thickness under the conditions of different deformation amounts; s4: and evaluating the strengthening degree of different component parts of the sample at different deformation positions by adopting a method of punching hardness point by using a grid. The method comprises the steps of preparing a blank with gradient components by a powder feeding laser cladding method, preparing a sample plate with gradient components and deformation by a wedge rolling method in parallel, screening an alloy component with the highest Vickers hardness value and deformation by a point-by-point hardness method to pre-estimate the plate component with the best strengthening effect and a rolling deformation process, facilitating the rapid optimization of a strengthening phase in the ceramic phase strengthened alloy, realizing the dual reduction of research and development period and cost, and solving the problems of complex component regulation and control, more preparation process parameters, long research and development period and high research and development cost of the ceramic reinforced composite material.

Example 2: in the present embodiment, the rolling direction is perpendicular to the direction of the composition gradient in step S3, the rolling temperature is 1150 ℃, and the rolling strain rate is 1-10S^-1. In this example, the hardness grid points are distributed along the gradient direction of the deformation amount at the center of the component in step S4, and the strengthening effect is evaluated by the hardness method. In step S1 of the present example, a stainless steel base powder prepared by a gas atomization powdering method. In step S1 of this embodiment, 4 kinds of nanopowders with different composition ratios are selected to prepare 4 different mixed powders, which respectively are: fe powder, Fe powder + 0.5% Y nano powder, Fe powder + 0.5% Y2O3 nano powder, Fe powder + 0.5% Y nano powder and 2% TiC nano powder.

Example 3: in step S2 of this embodiment, an yttrium-doped fiber laser with a wavelength of 1070nm is used as a heat source, a synchronous powder feeding laser additive manufacturing system is used to feed powder through a coaxial three-way powder feeding nozzle under the protection of high-purity argon gas, a laser power of 600 + 1000W, a spot diameter of 1.8mm, a scanning rate of 400mm/min, a lifting amount of 0.3mm, and a chamber water oxygen content of less than 10 × 10-6 are used to perform laser cladding layer by layer to print a plate-shaped single arm member, and the plate-shaped single arm member is printed layer by layer until a partitioned plate-shaped single arm sample is prepared. In step S3 of this example, a single arm sample was cut into a wedge-shaped plate having an apex angle of 5 to 10 °. In step S4 of the present embodiment, the mesh of the deformation amount is divided on the surface of the sample after rolling, the deformation amount is divided by 10%, 20%, 30%, 40%, 50%, 60%, 70% in the gradient direction of the deformation amount at the center position of the composition, and the upper, middle, lower, left, right 5 hardness points are printed on each mesh by using the point-by-point printing with the vickers hardness tester, and then the average hardness is determined.

Example 4: in the present embodiment, the study of the present case shows that the deformation does not greatly affect the hardening effect of the alloy when the ceramic material is deformed at a high temperature of 1100 ℃, and the analysis result of the alloy phase shows that the base of the 4-class alloy is a softer ferrite structure, and the reinforcing phase is the main factor affecting the hardness. The region B having the composition Fe + 0.5% Y + 2% TiC has the highest hardness, and the composite reinforcing phase is evaluated to have the best reinforcing effect in this example. The invention relates to a high-flux tissue optimization method of a nano ceramic phase reinforced alloy, which selects 3 nano ceramic phases with different components to be respectively added independently and mixed, carries out the research on the reinforcing effect of adding 0.5 percent of Y, 0.5 percent of Y2O3 and 0.5 percent of Y +2 percent of TiC on a base alloy through layer-by-layer powder feeding laser cladding comparison, obtains the deformation with gradient change through wedge-shaped binding, discusses the influence of the alloy components and the thermal deformation on the reinforcing effect of different combined ceramic phase reinforced alloys, and can optimize the components of the alloy or the deformation process at high flux by adopting the method.

The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.