CN110904389B - Multifunctional integrated Fe-Al-Ta eutectic composite material and preparation method thereof - Google Patents

Multifunctional integrated Fe-Al-Ta eutectic composite material and preparation method thereof Download PDF

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CN110904389B
CN110904389B CN201911221058.8A CN201911221058A CN110904389B CN 110904389 B CN110904389 B CN 110904389B CN 201911221058 A CN201911221058 A CN 201911221058A CN 110904389 B CN110904389 B CN 110904389B
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eutectic
solidification
composite material
area
solidification rate
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CN110904389A (en
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来园园
崔春娟
任驰强
邓力
刘艳云
王丛
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Xian University of Architecture and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/04—Influencing the temperature of the metal, e.g. by heating or cooling the mould
    • B22D27/045—Directionally solidified castings
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/24—Deposition of silicon only
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/305—Sulfides, selenides, or tellurides
    • C23C16/306—AII BVI compounds, where A is Zn, Cd or Hg and B is S, Se or Te
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C23C16/345—Silicon nitride
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/401—Oxides containing silicon
    • C23C16/402—Silicon dioxide
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/48—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation
    • C23C16/483—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation using coherent light, UV to IR, e.g. lasers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2202/00—Metallic substrate
    • B05D2202/10—Metallic substrate based on Fe

Abstract

A multifunctional integrated Fe-Al-Ta eutectic composite material and a preparation method thereof are disclosed, wherein an electron beam suspension area melting technology, a spraying technology, a photochemical deposition technology and other process technologies are combined, the solidification rate of the Fe-Al-Ta eutectic composite material is changed in the material preparation process, and a certain area of the material is specially processed by the spraying technology, the photochemical deposition technology and other process technologies, and the area can be in any shape or pattern, so that the prepared material has required specific performance in the patterned area, and the material with multiple functions integrated into a whole is prepared. Therefore, by a method combining the three technologies, firstly, the solidification rate of different areas is changed to change the solidification structure of the material, and then, according to actual needs, a certain specific area is subjected to specific processing by adopting the spraying and photochemical deposition technologies, so that the prepared sample integrates multiple functions. The material performance is centralized, simplified and diversified, and the comprehensive performance is improved.

Description

Multifunctional integrated Fe-Al-Ta eutectic composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of metallurgy, relates to a specific processing technology for a specific area of a Fe-Al-Ta eutectic composite material, and particularly relates to process technologies such as electron beam area melting, spraying, photochemical deposition and the like.
Background
With the rapid development of modern science and technology, elements are continuously developed in the direction of miniaturization, centralization and large storage capacity. Although composites with excellent properties can be prepared by various preparation techniques, many problems arise in practical applications. Therefore, in practical application, materials with good comprehensive properties are mostly needed, which puts higher requirements on the processing and preparation of the materials. In practical application, the invention concentrates the material performance, not only can integrate the element with multiple functions, but also can show multiple performances on the surface of the element.
At present, few materials with single performance can meet the use requirements, so most of the materials adopt composite materials, but the composite materials prepared by some current methods cannot show multiple performances on the same material, and the process stability, the long-term high temperature resistance, the environmental aging resistance and the like of most of the composite materials are poor. This results in relatively low material utilization and short service life.
Disclosure of Invention
In order to overcome the defects of low utilization rate, poor stability and the like of the existing material, improve the performance of the material and enable a device to have multiple functions, the invention aims to provide a multifunctional integrated Fe-Al-Ta eutectic composite material and a preparation method thereof. The material can enable different areas to have different performances according to different service requirements, the internal structure of the material prepared by the method can meet different performances, and the material surface can also have different characteristics according to requirements, so that the prepared material has different performances in different areas. Thereby effectively overcoming the defects and shortcomings of short service life and poor performance of common materials, improving the performance of the materials and simultaneously expanding the application of the materials.
In order to achieve the purpose, the invention adopts the technical scheme that:
a multifunctional Fe-Al-Ta eutectic composition is prepared from Fe2Ta (Al) as a reinforcing phase and Fe (Al, Ta) as a matrix phase. The reinforcing phase Fe2Ta (Al) grows directionally along with heat flow, is uniformly distributed in the matrix phase Fe (Al, Ta), and has obvious anisotropy.
And coating and/or depositing a thin film on a designated area of the surface of the eutectic composite material.
The invention provides a preparation method of the multifunctional integrated Fe-Al-Ta eutectic composite material, which is used for preparing eutectic alloy according to the eutectic point of a Fe-Al-Ta phase diagram. Performing directional solidification on the alloy by an electron beam suspension zone melting technology to obtain Fe (Al, Ta)/Fe2In the solidification process of the Ta (Al) eutectic composite material, the solidification rate of directional solidification is changed, so that the microstructure of the material is changed, different parts of the component generate different solidification structure forms, sizes and distributions, and the different parts have different performances, thereby realizing multifunction integration.
When the solidification rate is 0-6 mu m/s, the structure of the material is a lamellar eutectic structure. With the increase of the solidification rate, the eutectic structure is converted from a lamellar structure to a rod-shaped structure, and when the solidification rate is 200-600 mu m/s, the structure of the material is the rod-shaped eutectic structure. When the solidification rate is further increased, the eutectic structure is gradually converted into a spherical shape from a rod shape, and when the solidification rate is 600-900 mu m/s, the structure of the material is a spherical eutectic structure.
The smelting temperature is 1580-1680 ℃, the temperature gradient is 350-450K/cm, the rated power of an electron gun is 500KW, the conduction ratio is 30%, the accelerating voltage is 8.5-9.2 KV, the emission current is 11-13 mA, and the vacuum degree is 1.4-1.6 x 10- 4mbar。
And carrying out semiconductor film formation on the designated area on the surface of the eutectic composite material by using a chemical deposition method, and depositing to form films meeting different requirements by controlling process conditions.
The chemical deposition method is thermal deposition, plasma deposition or photochemical vapor deposition, and a metal film, a dielectric film, an insulator film or a compound semiconductor film, or an amorphous semiconductor film or an alloy semiconductor film is deposited on the eutectic composite material according to requirements.
The photochemical vapor deposition method is carried out in a low-pressure deposition chamber, Hg vapor is introduced into the deposition chamber, and Hg in the deposition chamber is excited to be in an activated state by using 254nm ultraviolet light, and the reaction formula is as follows:
Hg(hv,254nm)―→Hg'
hg in an activated state decomposes molecules of the reaction gas;
if ZnS is to be deposited, two reaction gases, i.e., COS and Zn (CH), are required3)2The reaction formula is as follows:
COS+Hg―→CO+S
S+Zn(CH3)2(hv,254nm, Hg) → ZnS + gas
If Si is to be deposited3N4Then SiH is required4And NH3Two reaction gases, the reaction formula of which is:
SiH4+NH3(hv,254nm,Hg)―→Si3N4+ qi (qi)Body
If SO is to be deposited2Then SiH is required4And N2O two reaction gases, the reaction formula of which is:
SiH4+N2O(hv,254nm,Hg)―→SiO2+ gas
ZnS, Si formed during the reaction3N4And SiO2A film is formed on the surface of the heated sample, and residual gas and Hg steam are filtered and then pumped away by a vacuum pump.
The method utilizes a spraying method to spray the appointed area on the surface of the eutectic composite material so as to cover the surface metal performance of the area and have the performance of a coating material.
The coating material may be plastic.
Compared with the prior art, the invention adopts the electron beam suspension area melting directional solidification technology to prepare the material, and utilizes the technologies of spraying, photochemical deposition and the like to prepare the device with specific performance in a specific area, and simultaneously prepare the performance required by the area at different positions in the same device. The solidification rate is changed by utilizing an electron beam suspension area melting directional solidification technology, a microstructure of a material structure is changed, and a required coating is added to a specific area on the surface of the material according to requirements by utilizing technologies such as spraying, photochemical deposition and the like, so that the surface performance of the material is changed, and the composite material with various integrated performances is prepared. The invention can improve the utilization rate of materials and prolong the service life of devices. And can be applied in large scale in industrial production, thereby expanding the application of materials.
The invention not only provides a theoretical basis for the research and development of material area patterning, but also has important guiding significance for expanding the application of the electron beam zone-melting directional solidification technology, the spraying technology and the photochemical deposition technology.
Drawings
FIG. 1 is a schematic diagram of the electron beam levitation zone melting principle.
Fig. 2 is a schematic diagram of an electron gun.
FIG. 3 illustrates spray coating to produce a composite material having specific properties in the patterned region (H).
FIG. 4 is a schematic diagram of an experimental apparatus for LCVD deposition of amorphous silicon.
FIG. 5 is a schematic view of a multifunctional integrated Fe-Al-Ta eutectic composite material.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the drawings and examples.
The invention provides a preparation method of the multifunctional integrated Fe-Al-Ta eutectic composite material, which comprises the steps of preparing eutectic alloy according to the eutectic point of a Fe-Al-Ta phase diagram, and directionally solidifying the alloy by an electron beam suspension zone melting technology to obtain Fe (Al, Ta)/Fe2Ta (Al) eutectic composite material changes the microstructure of the material by changing the solidification rate of directional solidification in the solidification process, so that different parts of the component generate different solidification structure forms, sizes and distributions, and the specific part has a specific microstructure, so that the parts have different functions, different parts have different performances, and multiple functions are integrated. The method comprises the following steps of smelting an eutectic alloy in a vacuum induction furnace in a high-purity Ar atmosphere to generate an eutectic alloy ingot, then carrying out electron beam suspension area smelting and directional solidification on the eutectic alloy ingot, and carrying out eutectic reaction in the liquid-solid phase change process.
One feasible process parameter of the electron beam suspension zone melting directional solidification of the invention is as follows:
melting temperature: 1580-1680 ℃, temperature gradient: 350-450K/cm, electron gun rated power: 500KW, conduction ratio: 30%, acceleration voltage: 8.5-9.2 KV, emission current: 11-13 mA, vacuum degree: 1.4-1.6 multiplied by 10-4mbar, and a smelting zone of 5-10 mm. The principle is shown in fig. 1 and fig. 2. Among them, the electron beam zone melting furnace is a very complicated system. The working principle is as follows: the electron gun 11 emits electrons, the electrons are accelerated under the action of an electric field, electric energy is converted into kinetic energy, a large number of electrons bombard and heat the surface of the metal material, the kinetic energy of the high-speed moving electrons is converted into heat energy, and the material area is melted. The electron gun 11 moves up and down along the electron gun moving direction 12. The raw material 14 is vertically mounted in the holding structure and the modified zone 13 is a narrow zone above it. The lower clamp can adjust the sample left, right, up and down in a certain range, and the annular cathode can move up and down along the sample at the speed of 0 to +/-23 mm/min by means of the transmission mechanism. When the high-voltage power supply is switched on, electrons emitted by the electron gun are accelerated under the action of an electric field to bombard the sample, and the kinetic energy of the electrons is converted into heat energy. And 15 is a bar frame.
Fig. 2 is a schematic diagram of an electron gun, which is the most critical device in a vacuum electron beam zone melting furnace. The working principle of the electron gun is as follows: the filament is electrified to emit a large number of hot electrons after being heated to a white thermalization state, the accelerating electric field adopts negative high voltage, the anode is grounded, and the electrons are accelerated under the action of the high-voltage electric field. Due to the action of the accelerating electric field and the shielding, electrons can be gathered to the anode.
The annular electron gun mainly comprises an electron gun body 24, an upper auxiliary electrode 21, a lower auxiliary electrode 23, a filament and a bunching electrode 25, wherein the electron gun body is of a water-cooling structure and is divided into an upper part and a lower part, the upper auxiliary electrode 21, the bunching electrode 25 and the filament (cathode 22) are arranged at the upper part of the gun body, and the lower auxiliary electrode 23 is arranged at the lower part of the gun body. In this electron gun, the gun body, the upper and lower auxiliary electrodes, and the auxiliary electrode are connected to a negative high voltage, and the bar material in the region to be grounded is used as the anode 26.
On the basis, process technologies such as spraying and/or photochemical deposition are combined, so that the material can enable different areas to have different properties according to requirements. The surface of a specific area of the material is modified by process technologies such as spraying and/or photochemical deposition, so that the performance of the specific area can be changed. The material may exhibit different or different properties in each of the different regions of the device material.
Specifically, in the directionally solidified eutectic composite material, in order to enable the device to be used normally and efficiently in practice, a specific part of the device material needs to be processed, so that the utilization rate of the material is improved. The performance of a specific part of the composite material can be improved by a spraying method, the moving path of a spraying gun head is accurately controlled, the gun head is enabled to move and spray in an area needing to be improved, the surface metal performance of the area is covered, the performance of the area is improved, and the composite material with excellent performance is prepared. The plastic coating method includes many methods, such as flame spraying, fluidized spraying, powder electrostatic spraying, thermal deposition, suspension coating, etc., and the basic process flow is workpiece pretreatment (degreasing, sand blasting, dust removal, preheating, etc.) → coating (spray dipping, pouring, brushing, etc.) → curing (sintering, drying, crosslinking, etc.) → coating product. FIG. 3 is a composite material having specific properties for patterned regions (H) prepared by spray coating. The H-shaped area, which represents the modified area, is machined on the raw material by means of a spray gun. The modified regions may be in any pattern and may be modified in any region, represented here by H. 31 is a spray gun, 32 is a modified region, and 33 is a sample.
And carrying out semiconductor film formation on the designated area on the surface of the eutectic composite material by using a chemical deposition method, and depositing to form films meeting different requirements by controlling process conditions. There are several methods available to decompose the reaction gas: heating (thermal deposition); plasma or radio frequency discharge (plasma deposition); and ultraviolet light irradiation (light deposition).
In the chemical vapor deposition process, a reaction gas such as silane, ammonia gas, an organozinc compound, etc. is introduced into a reaction chamber and decomposed, and then a desired thin film is formed on the surface of a heated sample. Chemical Vapor Deposition (CVD) and vacuum thermal evaporation and sputtering are currently common thin film deposition techniques. The technique of photochemical deposition (PVD) is an important branch of the chemical vapor deposition technique, and is relatively new thin film deposition technique. The main characteristic of the technology is that the whole CVD process is completed by utilizing the assistance of ultraviolet light. The method has the characteristics of low deposition temperature (50-250 ℃), small probability of charged ions impacting a sample, uniform film layer coverage and the like.
Currently, photochemical vapor deposition is performed in a low pressure deposition chamber at about 133 Pa. A small amount of Hg vapor was introduced into the deposition chamber and the Hg therein was excited in an activated state with 254nm uv light. The reaction formula is as follows:
Hg(hv,254nm)―→Hg'
the Hg in the activated state decomposes the molecules of the reaction gas.
If ZnS is to be deposited, two reaction gases, i.e., COS and Zn (CH), are required3)2The reaction formula is as follows:
COS+Hg―→CO+S
S+Zn(CH3)2(hv,254nm, Hg) → ZnS + gas
If Si is to be deposited3N4Then SiH is required4And NH3Two reaction gases, the reaction formula of which is:
SiH4+NH3(hv,254nm,Hg)―→Si3N4+ gas
If SO is to be deposited2Then SiH is required4And N2O two reaction gases, the reaction formula of which is:
SiH4+N2O(hv,254nm,Hg)―→SiO2+ gas
ZnS, Si formed during the above reaction3N4And SiO2A film is formed on the surface of the heated sample, and residual gas and Hg steam are filtered and then pumped away by a vacuum pump.
Laser Chemical Vapor Deposition (LCVD) is a new technique for applying laser light to conventional Chemical Vapor Deposition (CVD). The LCVD technique is a technique in which a reaction gas enclosed in a gas chamber is irradiated with a laser beam to induce a chemical reaction, and the resultant is deposited on a substrate placed in the gas chamber. The LCVD has the greatest advantage that the whole substrate is not directly heated in the deposition process, and the deposition can be carried out as required; the space selectivity is good, and the film generation can be limited on any micro area of the substrate; the deposition rate is faster than CVD. There are many examples of LCVD, such as American scientific household CO2Laser induced SiH4Gas (or SiH)4Mixed gas of/Ar) as a silicon source, a 3mm quartz plate as a substrate, SiH4The pyrolysis causes silicon to be deposited on the quartz wafer.
FIG. 4 is a schematic diagram of an experimental apparatus for LCVD deposition of amorphous silicon, 41 is a laser beam, 42 is a gas chamber, 43, 45 are outer windows, and 44 is a substrate.
The principle of laser chemical film formation: e.g. using CO2Laser induced SiH4The reaction gas is enclosed in a stainless steel gas chamber, and the laser beam enters the gas chamber through an infrared window, passes through the gas chamber in a direction parallel to the surface of the substrate and in a direction very close to the substrate, and is positioned in the stainless steel gas chamberThe reactive gas near the substrate surface is induced by the laser to decompose as follows, i.e.
SiH4―→Si+2H2(gas)
The Si produced by the reaction is deposited on the substrate in the form of an amorphous film. Different types of amorphous silicon films can be deposited by adopting different laser irradiation modes and substrate placement modes. If the laser beam is focused and irradiated perpendicularly to the substrate, a small-sized amorphous silicon thin film can be deposited on the substrate.
In order to improve the overall performance of the material, a combination of a plurality of preparation methods can be adopted, and the corresponding performance is reflected in the corresponding area, so that different parts of the material have different functions.
The eutectic composite material prepared by the invention has the most remarkable characteristics of directional solidification and a series of excellent characteristics, such as good orientation, uniform distribution and grain refinement of a reinforcing phase, firm interface bonding of the reinforcing phase and a matrix phase, good physicochemical compatibility and the like. In addition, the material with specific performance in a specific area can be freely prepared by utilizing the process technologies such as spraying and/or photochemical deposition, and the performance required by the area can be prepared at different positions in the same device.
The multifunctional integrated Fe-Al-Ta eutectic composite material is prepared from Fe2Ta (Al) as a reinforcing phase, Fe (Al, Ta) as a matrix phase, Fe as a reinforcing phase2Ta (Al) grows directionally along with heat flow, is uniformly distributed in the matrix phase Fe (Al, Ta), and has obvious anisotropy. The mechanical property is greatly improved, and particularly the high-temperature strength and the high-temperature creep resistance are obviously improved. When the solidification rate is low, the texture of the material is a lamellar eutectic texture, and as the solidification rate is increased, the solidification texture is subjected to lamellar-rod-shaped-spheroidizing evolution.
The microstructure of the metal determines the macroscopic mechanical property, so that the microstructure of different areas of the material can be changed by controlling the solidification rate in directional solidification. The properties exhibited by different rates of coagulated tissue are slightly different: when the solidification rate is low (0-6 mu m/s), the Fe-Al-Ta eutectic structure is lamellar, and the lamellar structure has the advantages of good high-temperature creep resistance, good fracture resistance and good room-temperature plasticity. When the solidification rate is further increased (200-600 mu m/s), the eutectic structure is converted from a lamellar structure to a rod-shaped structure, and the rod-shaped structure has the advantages of excellent plasticity, toughness and fatigue resistance. The rod-shaped eutectic structure has good normal-temperature mechanical property, and the lamellar eutectic structure has good high-temperature mechanical property; when the solidification rate is further increased (600-900 mu m/s), the eutectic structure is converted from a rod shape to a spherical shape, and the spherical eutectic structure has the characteristics of good wear resistance and high strength.
After the surface of the metal part is coated with a layer of plastic by a coating method, the original characteristics of the metal can be maintained, and the metal part can have certain characteristics of the plastic, such as corrosion resistance, wear resistance, electrical insulation, self lubrication, organic matter hand feeling and the like. Device coating applications have become very common. There are also many types of plastics that can be used as coating materials for device coatings, and the most common plastics for coating the surfaces of metal devices are polyvinyl chloride, polyethylene, ultra-high molecular weight polyethylene, nylon, and the like. The choice of the device coating method and the type of plastic to be coated depends on the device material and its requirements for coating properties.
By utilizing the photochemical vapor deposition, a high-quality and nondestructive film can be obtained, and the film has many practical applications. The advantages of this thin film deposition technique are that the deposition is performed at low temperature, the deposition rate is fast, metastable phases can grow and abrupt junctions can be formed. Compared with plasma chemical vapor deposition, photochemical vapor deposition has no energetic particles to bombard the surface of the growing film, and the photons for exciting the decomposition of reactant molecules have insufficient energy to initiate ionization, so that the high-quality film can be obtained by using the technology, and the film is well combined with the substrate. In the photochemical vapor deposition process, when high-energy photons selectively excite surface adsorbed molecules or gas molecules, the molecular bonds are broken to generate free chemical particles, and further a thin film or a compound is formed on a substrate, the photochemical deposition process is performed, and the process is strongly dependent on the wavelength of incident photons. The high energy light source required for photochemical deposition can typically be achieved by a laser source or an ultraviolet lamp. Many different thin film materials such as various metal films, dielectric films, insulator films and compound semiconductor films have been obtained using photochemical vapor deposition, and high quality thin films can be obtained by mercury-sensitized photochemical vapor deposition in addition to a direct photodecomposition process. Amorphous Si (a-Si) and other alloy semiconductors (such as a-SiGe, a-SiGe: H, etc.) are semiconductor films with broad optoelectronic application prospects. The high-quality a-Si film can be prepared by utilizing mercury sensitization and a direct photochemical vapor deposition method.
Laser chemical vapor deposition essentially consists of two mechanisms for laser-triggered chemical reactions, one being a photo-chemical reaction and the other being a thermo-chemical reaction. During the photochemical reaction, photons of sufficiently high energy are used to break down molecules and form a film, or react with other chemicals present in the reactive gas and form a compound film on an adjacent substrate. In another type of process, a laser beam is used as a heat source to effect thermally-induced decomposition, and the resulting temperature increase on the substrate controls the deposition reaction. Since the heating in laser chemical vapor deposition is very localized, the reaction temperature can be very high. Al, Ni, Au, Si, SiC, poly Si, and Al/Au films have been obtained using laser chemical vapor deposition.
The following are several specific embodiments of the present invention.
Example 1:
1) vertically installing the wire-cut material in a clamping structure with a clamp in a vacuum degree of 1.4-1.6 × 10-4mbar, conduction ratio of 30%, acceleration voltage of 8.7KV and emission current of 11mA, and carrying out directional solidification experiment in electron beam suspension zone melting equipment (1600 deg.C) to melt the material zone.
2) When the material is in service and the high-temperature creep resistance, the fracture resistance and the room-temperature plasticity of the material are required to be good, the material is directionally solidified from bottom to top at a low solidification rate by controlling the drawing rate, namely the solidification rate is 0-6 mu m/s. Therefore, the block material with lamellar eutectic microstructure can be obtained, and has high-temperature creep resistance. As shown in fig. 5 (a).
3) When the surface of the material part does not need the metal property, as shown in the square area on the front surface of fig. 5(a) (the shape of the area can be arbitrary), the surface spraying treatment is carried out according to the requirement, so that the surface metal property is covered.
Example 2:
1) vertically installing the wire-cut material in a clamping structure with a clamp in a vacuum degree of 1.4-1.6 × 10-4mbar, conduction ratio of 30%, acceleration voltage of 8.7KV and emission current of 11mA, and carrying out directional solidification experiment in electron beam suspension zone melting equipment (1600 deg.C) to melt the material zone.
2) When the material is in service, one part of the material is required to have good high-temperature creep resistance, fracture resistance and room-temperature plasticity, and the other part of the material is required to have good plasticity, toughness, fatigue resistance and the like, the material is directionally solidified from bottom to top by controlling the drawing speed. The low-speed solidification is carried out on the part which requires good high-temperature creep resistance, fracture resistance and room-temperature plasticity, and the higher-speed solidification is carried out on the part which requires good plasticity, toughness and fatigue resistance. If the lower half part of the material is solidified at a low speed, and the upper half part of the material is solidified at a higher speed, namely the solidification rate of the lower half part of the material is 0-6 mu m/s, and the solidification rate of the upper half part of the material is 200-600 mu m/s, so that the lower half part of the microstructure of the material is a lamellar eutectic structure, has higher high-temperature creep resistance, fracture resistance and room-temperature plasticity, and the upper half part of the microstructure is a rod-shaped eutectic structure, and has good plasticity, toughness and fatigue resistance. As shown in fig. 5 (b).
3) When the surface of the material part does not need the metal property, as shown in fig. 5(b) the front irregular area (the shape of the area can be arbitrary), the surface spraying treatment is performed according to the requirement, so that the surface metal property is covered.
Example 3:
1) vertically installing the wire-cut material in a clamping structure with a clamp in a vacuum degree of 1.4-1.6 × 10-4mbar, conduction ratio of 30%, acceleration voltage of 8.7KV and emission current of 11mA, and carrying out directional solidification experiment in electron beam suspension zone melting equipment (1600 deg.C) to melt the material zone.
2) When the material is in service, if the material is required to have three different performances and more diversified performances, the sample is zone-melted and directionally solidified from bottom to top by moving the electron gun. Higher rate (200-; the part with good high-temperature creep resistance, fracture resistance and room-temperature plasticity is required to be solidified at a low speed (less than or equal to 6 mu m/s); the portion where the wear resistance and strength are high is required to undergo high-rate (600-900 μm/s) solidification. For example, the material is divided into four zones, with the lowest portion of the material undergoing higher rate solidification, the middle lower portion undergoing high rate solidification, the middle upper portion undergoing low rate solidification, and the uppermost portion undergoing high rate solidification. The microstructure of the obtained material has the advantages that the lowest part of the microstructure is a rod-shaped eutectic structure, the plasticity, the toughness and the fatigue resistance are good, the middle-lower part is a spherical eutectic structure, the wear resistance and the strength are high, the middle-upper part is a lamellar eutectic structure, the high-temperature creep resistance, the fracture resistance and the room-temperature plasticity are good, and the uppermost part is a spherical eutectic structure, the wear resistance and the strength are good. This results in a monolithic material divided into four regions with three different properties. As shown in fig. 5 (c).
3) When the partial surface of the material does not need the performance of metal, as shown in a front trapezoidal area and a side semi-elliptical area (the shape of the area can be arbitrary) in fig. 5(c), surface spraying treatment is carried out according to the requirement, for example, after a layer of plastic is coated on the surface of a metal part, the original characteristics of the metal can be kept, and the metal part can have certain characteristics of the plastic. Such as corrosion resistance, wear resistance, electrical insulation, self-lubrication, organic hand feeling and the like.
Example 4:
1) vertically installing the wire-cut material in a clamping structure with a clamp in a vacuum degree of 1.4-1.6 × 10-4mbar, conduction ratio of 30%, acceleration voltage of 8.7KV and emission current of 11mA, and carrying out directional solidification experiment in electron beam suspension zone melting equipment (1600 deg.C) to melt the material zone.
2) When the material is in service and the material is required to have excellent plasticity, toughness, fatigue resistance and other properties, the material is directionally solidified from bottom to top at a higher solidification rate by controlling the drawing rate, namely the solidification rate is 200-600 mu m/s. Therefore, the block material with the microstructure of the rod-shaped eutectic crystal is obtained, and has good plasticity, toughness and fatigue resistance. As shown in fig. 5 (d).
3) When a thin film, such as an amorphous silicon thin film, needs to be added on the surface of the material, a laser chemical vapor deposition technique can be used to deposit a micro-sized amorphous silicon thin film on the surface of the material, as shown in fig. 5(d) a front S-shaped area (the shape of the area can be arbitrary), and the micro-sized amorphous silicon can be used to manufacture a large-scale integrated circuit or other microelectronic devices. Therefore, the material integrating multiple functions can be manufactured by utilizing a directional solidification technology and a laser chemical vapor deposition technology.
Example 5:
1) vertically installing the wire-cut material in a clamping structure with a clamp in a vacuum degree of 1.4-1.6 × 10-4mbar, conduction ratio of 30%, acceleration voltage of 8.7KV and emission current of 11mA, and carrying out directional solidification experiment in electron beam suspension zone melting equipment (1600 deg.C) to melt the material zone.
2) When the material is in service, one part of the material is required to have good high-temperature creep resistance, fracture resistance and room-temperature plasticity, and when the other part of the material has high wear resistance and high strength, the material is directionally solidified from bottom to top by controlling the drawing rate. The low-speed solidification is carried out on the part which requires high-temperature creep resistance, fracture resistance and good room-temperature plasticity, and the high-speed solidification is carried out on the part which requires high wear resistance and high strength. If the lower half part of the material is solidified at a low speed, and the upper half part of the material is solidified at a high speed, namely the solidification rate of the lower half part is 0-6 mu m/s, and the solidification rate of the upper half part is 600-900 mu m/s, so that the lower half part of the microstructure of the material is a lamellar eutectic structure, has high-temperature creep resistance, fracture resistance and room-temperature plasticity, and the upper half part of the microstructure is a spherical eutectic structure, and has good wear resistance and strength. As shown in fig. 5 (e).
3) When a thin film, such as an amorphous silicon thin film, needs to be added on the surface of the material, a laser chemical vapor deposition technique can be used to deposit a micro-sized amorphous silicon thin film or a large-area amorphous silicon thin film on the surface of the material, as shown in fig. 5(e) a square area and an S-shaped area on the front surface (the shape of the area can be arbitrary), the micro-sized amorphous silicon can be used to manufacture large-scale integrated circuits or other microelectronic devices, and the large-area amorphous silicon can be used to manufacture solar cells. By combining the above, the multifunctional integrated material is manufactured by utilizing a directional solidification technology and a laser chemical vapor deposition technology according to requirements.
Example 6:
1) vertically installing the wire-cut material in a clamping structure with a clamp in a vacuum degree of 1.4-1.6 × 10-4mbar, conduction ratio of 30%, acceleration voltage of 8.7KV and emission current of 11mA, and carrying out directional solidification experiment in electron beam suspension zone melting equipment (1600 deg.C) to melt the material zone.
2) When the material is in service and is required to have three different performances, the material is directionally solidified from bottom to top by controlling the drawing speed. The high-speed solidification is carried out on the part which requires good performances such as plasticity, toughness and fatigue resistance, the low-speed solidification is carried out on the part which requires good performances such as high-temperature creep resistance, fracture resistance and room-temperature plasticity, and the high-speed solidification is carried out on the part which requires high wear resistance and high strength. For example, the lower half of the material is solidified at a higher rate, the middle part is solidified at a higher rate, and the upper half is solidified at a lower rate, i.e., the lower half of the material is solidified at a rate of 200 μm/s to 600 μm/s, the middle part is solidified at a rate of 600 μm/s to 900 μm/s, and the upper half is solidified at a rate of 0 to 6 μm/s. The lower half part of the microstructure of the obtained material is a rod-shaped eutectic structure, and has good plasticity, toughness and fatigue resistance, the middle part is a spherical eutectic structure, and has good wear resistance and strength, and the upper half part is a lamellar eutectic structure, and has good high-temperature creep resistance, fracture resistance and room-temperature plasticity. As shown in fig. 5(f).
3) When a thin film, such as an amorphous silicon thin film, needs to be added on the surface of the material, a laser chemical vapor deposition technique can be used to deposit a micro-sized amorphous silicon thin film or a large-area amorphous silicon thin film on the surface of the material, as shown in fig. 5(f) by a rectangular area on the right side of the front surface and a semi-oval area on the side surface (the shape of the area can be arbitrary), the micro-sized amorphous silicon can be used to manufacture large-scale integrated circuits or other microelectronic devices, and the large-area amorphous silicon can be used to manufacture solar cells. Meanwhile, if other properties are partially required, as shown in fig. 5(f) a rectangular area on the left side of the front surface (the shape of the area can be arbitrary), for example, corrosion resistance, etc., a plastic film can be added to the surface of the material by a spraying method. The three techniques are combined to manufacture the multifunctional integrated material.
Example 7:
1) vertically installing the wire-cut material in a clamping structure with a clamp in a vacuum degree of 1.4-1.6 × 10-4mbar, conduction ratio of 30%, acceleration voltage of 8.7KV and emission current of 11mA, and carrying out directional solidification experiment in electron beam suspension zone melting equipment (1600 deg.C) to melt the material zone.
2) When the material is in service and the wear resistance and the strength of the material are required to be excellent, the material is directionally solidified from bottom to top at a high solidification rate by controlling the drawing rate, namely the solidification rate is 600-900 mu m/s. Therefore, the obtained block material with spherical eutectic microstructure has high wear resistance and strength. As shown in fig. 5(g). As in fig. 5(g).
3) When the material surface needs large-area changing performance, as shown in fig. 5(g) the surface net covering area, the surface spraying treatment can be carried out according to the requirement (such as increasing the wear resistance of the material) to cover the metal surface. Meanwhile, if other properties are needed in another part, as shown in the front surface H region (the shape of the region can be arbitrary) in fig. 5(g), if an amorphous silicon film is needed to manufacture a microelectronic device, the surface is modified by using the laser chemical vapor deposition technology. The three techniques are combined to manufacture the multifunctional integrated material.
Example 8:
1) vertically installing the wire-cut material in a clamping structure with a clamp in a vacuum degree of 1.4-1.6 × 10-4mbar, conduction ratio of 30%, acceleration voltage of 8.7KV and emission current of 11mA, and carrying out directional solidification experiment in electron beam suspension zone melting equipment (1600 deg.C) to melt the material zone.
2) When the material is in service, one part of the material is required to have good plasticity, toughness and fatigue resistance, and the other part of the material is required to have high wear resistance and strength, and the material is directionally solidified from bottom to top by controlling the drawing rate. The high-speed solidification is carried out on the part which requires good performances such as plasticity, toughness and fatigue resistance, and the high-speed solidification is carried out on the part which requires high wear resistance and strength. For example, the lower half of the material is solidified at a higher speed, and the upper half is solidified at a higher speed, that is, the solidification rate of the lower half of the material is 200 μm/s to 600 μm/s, and the solidification rate of the upper half is 600 μm/s to 900 μm/s. The lower half part of the microstructure of the obtained material is a rod-shaped eutectic structure, and the obtained material has good plasticity, toughness and fatigue resistance, and the upper half part is a spherical eutectic structure, so that the wear resistance and the strength are good. As shown in fig. 5 (h).
3) When the material surface needs large-area changing performance, as shown by the right oblique line coverage area of the surface in fig. 5(h), if a large-area amorphous silicon film is needed, the surface is deposited by using the chemical vapor deposition technology. If other properties are required, the surface coating treatment can be performed according to the requirements (such as increasing the wear resistance of the material), as shown in the H-shaped area (the shape of the area can be any) in fig. 5(H), so that the metal surface is covered by the area. The three techniques are combined to manufacture the multifunctional integrated material.
Description of the product properties:
the Fe-Al-Ta eutectic composite material with multiple functions integrated is prepared by an electron beam suspension zone melting technology, the structure of the alloy is changed by changing the solidification rate, and the material with multiple functions integrated is prepared by adopting spraying and photochemical deposition technologies in a certain specific zone according to actual needs, so that the comprehensive performance of the material is improved.
Therefore, the invention greatly improves the utilization rate of materials and reduces the preparation cost of devices. The material performance is centralized, simplified and diversified by the method of combining the three modes, and the material with multiple functions integrated can be prepared, so that the comprehensive performance of the material is improved.
The above description is only one material embodiment of the present invention, and not all or only one embodiment, and any equivalent changes to the technical solution of the present invention by a person of ordinary skill in the art through reading the present specification are covered by the claims of the present invention.

Claims (3)

1. A preparation method of a multifunctional integrated Fe-Al-Ta eutectic composite material is provided, and the multifunctional integrated Fe-Al-Ta eutectic composite material is made of Fe2Ta (Al) as a reinforcing phase, Fe (Al, Ta) as a matrix phase, the reinforcing phase Fe2Ta (Al) grows directionally along heat flow, is uniformly distributed in a matrix phase Fe (Al, Ta), has obvious anisotropy, prepares eutectic alloy according to the eutectic point of a Fe-Al-Ta phase diagram, carries out electron beam suspension zone melting directional solidification on the eutectic alloy, and obtains Fe (Al, Ta)/Fe2Ta (Al) eutectic composite material, in the process, the solidification rate of different areas in the directional solidification process is changed, so that the microstructure of the material is changed, different parts of a component generate different solidification structure forms, sizes and distributions, and the different parts of the material have different performances, so that the multifunctional integration is realized, the Ta (Al) eutectic composite material is characterized in that a photochemical vapor deposition method is used for carrying out semiconductor film formation on a designated area on the surface of the eutectic composite material, films meeting different requirements are formed by deposition through controlling process conditions, the photochemical vapor deposition method is carried out in a low-pressure deposition chamber, Hg vapor is introduced into the deposition chamber, and Hg in the deposition chamber is in an activated state by using 254nm ultraviolet light, and the reaction formula is as follows:
Hg(hv,254nm)―→Hg'
hg in an activated state decomposes molecules of the reaction gas;
if ZnS is to be deposited, two reaction gases, i.e., COS and Zn (CH), are required3)2The reaction formula is as follows:
COS+Hg―→CO+S
S+Zn(CH3)2(hv,254nm, Hg) → ZnS + gas
If Si is to be deposited3N4Then SiH is required4And NH3Two reaction gases, the reaction formula of which is:
SiH4+NH3(hv,254nm,Hg)―→Si3N4+ gas
If Si O is to be deposited2Then SiH is required4And N2O two reaction gases, the reaction formula of which is:
SiH4+N2O(hv,254nm,Hg)―→SiO2+ gas
ZnS, Si formed during the reaction3N4And SiO2A film is formed on the surface of the heated sample, and residual gas and Hg steam are filtered and then pumped away by a vacuum pump.
2. The preparation method of the multifunctional integrated Fe-Al-Ta eutectic composite material as claimed in claim 1, wherein when the solidification rate is 0-6 μm/s, the texture of the material is lamellar eutectic texture; with the increase of the solidification rate, the eutectic structure is converted from a lamellar structure to a rod-shaped structure, and when the solidification rate is 200-600 mu m/s, the structure of the material is the rod-shaped eutectic structure; when the solidification rate is further increased, the eutectic structure is gradually converted into a spherical shape from a rod shape, and when the solidification rate is 600-900 mu m/s, the structure of the material is a spherical eutectic structure.
3. The preparation method of the multifunctional integrated Fe-Al-Ta eutectic composite material as claimed in claim 1, wherein the smelting temperature is 1580-1680 ℃, the temperature gradient is 350-450K/cm, the rated power of an electron gun is 500KW, the conduction ratio is 30%, the acceleration voltage is 8.5-9.2 KV, the emission current is 11-13 mA, and the vacuum degree is 1.4-1.6 x 10-4mbar。
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