CN114231915B - Alloy sputtering target material for flat panel display and preparation method thereof - Google Patents
Alloy sputtering target material for flat panel display and preparation method thereof Download PDFInfo
- Publication number
- CN114231915B CN114231915B CN202111350335.2A CN202111350335A CN114231915B CN 114231915 B CN114231915 B CN 114231915B CN 202111350335 A CN202111350335 A CN 202111350335A CN 114231915 B CN114231915 B CN 114231915B
- Authority
- CN
- China
- Prior art keywords
- treatment
- temperature
- refining
- cooling
- sputtering target
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Powder Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses an alloy sputtering target material for a flat panel display, which comprises molybdenum niobium, a grain refining agent, a rare earth element improver and a flowing agent; the mass ratio of the molybdenum to niobium to the refined grain agent to the rare earth element improver to the flowing agent is (9-11): (1-4): (1.5-2.5): 0.5. in the preparation of the alloy sputtering target material, the alloy sputtering target material for the flat panel display, which is prepared by taking molybdenum and niobium as main metal elements, is adopted; the target material has higher density and ductility, thereby ensuring the uniformity of each component in the target material and reducing the generation of air holes and microcracks in the target material.
Description
Technical Field
The invention relates to the technical field of flat panel displays, in particular to an alloy sputtering target material for a flat panel display and a preparation method thereof.
Background
Film-coated flat panel displays have become the mainstream of televisions in the future, but have not been strictly defined internationally, and generally, such display screens have a relatively thin thickness and look like a flat panel, and flat panel displays are of various types, and are classified according to display media and working principles, such as Liquid Crystal Displays (LCD), plasma Displays (PDP), electroluminescence displays (ELD), organic electroluminescence displays (OLED), field Emission Displays (FED), projection displays, and the like. The flat panel display will adopt alloy sputtering target material, which has higher requirements than the traditional material industry, such as size, flatness, purity, impurity content, density, N/O/C/S, grain size and defect control, and higher or special requirements including surface roughness, resistance value, grain size uniformity, composition and structure uniformity, foreign matter (oxide) content and size, magnetic permeability, ultra-high density and ultra-fine grains, etc. The magnetron sputtering film plating is a new physical vapor film plating mode, that is, electron gun system is used to emit and focus electrons onto the material to be plated, so that sputtered atoms are separated from the material with high kinetic energy to fly toward the substrate to deposit film by following the momentum conversion principle. This plated material is called a sputter target. The sputtering target material is metal, alloy, ceramic compound, etc.
In the smelting and preparation process of the existing alloy target, metal segregation can be generated, the grain size of the alloy is increased, and the product performance of the alloy is affected.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an alloy sputtering target material for a flat panel display and a preparation method thereof, so as to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides an alloy sputtering target material for a flat panel display, which comprises molybdenum niobium, a grain refining agent, a rare earth element improver and a flowing agent; the mass ratio of the molybdenum to niobium to the refined grain agent to the rare earth element improver to the flowing agent is (9-11): (1-4): (1.5-2.5): 0.5;
the preparation method of the grain refining agent comprises the following steps:
s1: smelting: te and Mo are mixed according to the weight ratio of 3:1, and then are sent into a smelting furnace for smelting until the raw materials are completely melted;
s2: naturally cooling and molding the smelted raw materials, and then carrying out hot rolling and cold rolling treatment:
s3: finally, homogenizing;
homogenizing at 300-400deg.C for 15-25min, naturally cooling to 200deg.C at a rate of 1-3deg.C/min, keeping the temperature for 10-30min, and naturally cooling to room temperature.
Preferably, the rare earth element modifier is prepared by mixing rare earth lanthanum and TaC according to a weight ratio of 2:1.
Preferably, the flow agent is silicon powder.
Preferably, the hot rolling temperature in the hot rolling and cold rolling treatment is 500-800 ℃, the hot rolling time is 15-25min, the hot rolling deformation rate is 30-50%, and the hot rolling is finished;
then cold rolling is carried out at 0-20 ℃ for 35-45min, and the cold rolling deformation rate is 10-20%.
The preparation method of the alloy sputtering target material for the flat panel display comprises the following steps:
step one, smelting treatment: feeding molybdenum niobium, grain refining agent, rare earth element modifier and flowing agent into an arc melting furnace for treatment until the raw materials are completely melted, and after the raw materials are melted, rotating at a speed of 100-500r/min for 20-30min;
step two, feeding the smelted raw materials into a mould box for pressurizing, cooling and forming, wherein the pressurizing pressure is 5-10MPa, the pressure is maintained for 10-20s, and the cooling temperature is reduced to room temperature at a speed of 1-5 ℃/min, so as to obtain a formed material;
step three, carrying out pre-modification treatment on the molding material:
fourth, rapid air cooling treatment: improving the product subjected to the pre-modification treatment by adopting air cooling treatment, and then performing high-frequency refinement treatment;
step five, carrying out homogenization treatment;
the specific treatment method comprises the following steps:
heating the treated material at 200-400 deg.c for 10-30min, heating to 550 deg.c at the rate of 1-3 deg.c/min, maintaining for 10-30min, cooling to 130-150 deg.c at the rate of 5 deg.c/min, maintaining for 20-30min, and cooling to room temperature;
step six, finally performing aging treatment; the temperature in the aging treatment is 500-700 ℃, the aging time is 10-30min, and finally the temperature is reduced to room temperature at the speed of 1-5 ℃/min.
Preferably, the electric current of the arc melting furnace is 15-25kA, the voltage is 25-35V, and the vacuum degree is 1.5-3.5Pa.
Preferably, the electric arc melting furnace has a current of 20kA, a voltage of 30V and a vacuum degree of 2.0Pa.
Preferably, the specific operation steps of the pre-modification treatment are as follows:
s1: delivering the molding material to 100-300v voltage for bombardment treatment, wherein the bombardment pressure is 10-20min;
s2: then the mixture is sent to be preheated at 500-600 ℃ for 10-30min, after the preheating is finished, the mixture is cooled to 300 ℃ at the speed of 1-3 ℃/min, and the heat preservation is continued for 25-35min;
s3: then, current is conducted for treatment, the current intensity is 1-4A, the current time is 10-20min, then low-pressure sintering is carried out, and the pressure of the low-pressure sintering is 1-4MPa, so that the treated material is obtained.
Preferably, the specific operation steps of the air-cooling treatment are as follows:
firstly, soaking by adopting a sodium dodecyl sulfate solution with the mass fraction of 1-5%, wherein the soaking temperature is 35-45 ℃ and the soaking time is 10-20min;
then blowing and injecting the pre-modified product by adopting low-temperature nitrogen at the temperature of minus 5 ℃ with the blowing and injecting pressure of 1-5Mpa and the blowing and injecting time of 10-20min;
finally, cleaning the mixture in deionized water at 60-80 ℃ for 1-3 times, and then drying the mixture.
The grain refiner adopts Te and Mo for smelting, cooling forming is carried out after the grain refiner is accommodated, hot rolling and cold rolling are carried out, and finally homogenization treatment is carried out, so that the grain refiner after modification treatment can refine grains in target preparation, meanwhile, the added silicon flowing agent is matched with rare earth element modifier of rare earth lanthanum and TaC according to the weight ratio of 2:1, raw material elements are fully reacted, and then the reaction of target raw materials is fully carried out in the pretreatment treatment and the rapid air cooling treatment, so that the reaction degree of products is improved, the generation of pores and microcracks in the target is reduced, and further grains are refined in the reheating homogenization treatment, so that the density and the ductility of the products are improved.
Preferably, the specific operation steps of the high-frequency refinement treatment are as follows:
firstly, carrying out refining treatment at a frequency of 150-180KHz, wherein the refining time is 5-10min, and the refining temperature is 210-240 ℃;
then the refining temperature is adjusted to 160-200 ℃, the frequency is reduced to 120-130KHz, and the refining is continued for 10-20min;
and finally, continuously refining for 20-30min at 120-150 ℃, and naturally cooling to room temperature at a speed of 1-3 ℃/min after finishing refining.
Compared with the prior art, the invention has the following beneficial effects:
in the preparation of the alloy sputtering target material, the alloy sputtering target material for the flat panel display, which is prepared by taking molybdenum and niobium as main metal elements, is adopted; the target material has higher density and ductility, thereby ensuring the uniformity of each component in the target material and reducing the generation of air holes and microcracks in the target material;
in the specific preparation, te and Mo are adopted as grain refiner, cooling forming is carried out after the grain refiner is accommodated, hot rolling and cold rolling are carried out, and finally homogenization treatment is carried out, so that grain refining can be carried out in the preparation of the target material, meanwhile, the added silicon flowing agent is matched with rare earth lanthanum and TaC according to the rare earth element improver with the weight ratio of 2:1, raw material elements are fully reacted, and then the reaction of the target material is fully carried out in the pre-modification treatment and the rapid air cooling treatment, so that the reaction degree of the product is improved, the generation of air holes and microcracks in the target material is reduced, and in the reheating homogenization treatment, further grain refining is carried out, so that the density and the ductility of the product are improved.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The alloy sputtering target material for the flat panel display comprises molybdenum niobium, a grain refining agent, a rare earth element improver and a flowing agent; the mass ratio of the molybdenum to niobium to the refined grain agent to the rare earth element improver to the flowing agent is (9-11): (1-4): (1.5-2.5): 0.5;
the preparation method of the grain refining agent comprises the following steps:
s1: smelting: te and Mo are mixed according to the weight ratio of 3:1, and then are sent into a smelting furnace for smelting until the raw materials are completely melted;
s2: naturally cooling and molding the smelted raw materials, and then carrying out hot rolling and cold rolling treatment:
s3: finally, homogenizing;
homogenizing at 300-400deg.C for 15-25min, naturally cooling to 200deg.C at a rate of 1-3deg.C/min, keeping the temperature for 10-30min, and naturally cooling to room temperature.
The rare earth element modifier is prepared by mixing rare earth lanthanum and TaC according to a weight ratio of 2:1.
The flow agent of this embodiment is silicon powder.
The hot rolling temperature in the hot rolling and cold rolling treatment is 500-800 ℃, the hot rolling time is 15-25min, the hot rolling deformation rate is 30-50%, and the hot rolling is finished;
then cold rolling is carried out at 0-20 ℃ for 35-45min, and the cold rolling deformation rate is 10-20%.
The preparation method of the alloy sputtering target material for the flat panel display comprises the following steps:
step one, smelting treatment: feeding molybdenum niobium, grain refining agent, rare earth element modifier and flowing agent into an arc melting furnace for treatment until the raw materials are completely melted, and after the raw materials are melted, rotating at a speed of 100-500r/min for 20-30min;
step two, feeding the smelted raw materials into a mould box for pressurizing, cooling and forming, wherein the pressurizing pressure is 5-10MPa, the pressure is maintained for 10-20s, and the cooling temperature is reduced to room temperature at a speed of 1-5 ℃/min, so as to obtain a formed material;
step three, carrying out pre-modification treatment on the molding material:
fourth, rapid air cooling treatment: improving the product subjected to the pre-modification treatment by adopting air cooling treatment, and then performing high-frequency refinement treatment;
step five, carrying out homogenization treatment;
the specific treatment method comprises the following steps:
heating the treated material at 200-400 deg.c for 10-30min, heating to 550 deg.c at the rate of 1-3 deg.c/min, maintaining for 10-30min, cooling to 130-150 deg.c at the rate of 5 deg.c/min, maintaining for 20-30min, and cooling to room temperature;
step six, finally performing aging treatment; the temperature in the aging treatment is 500-700 ℃, the aging time is 10-30min, and finally the temperature is reduced to room temperature at the speed of 1-5 ℃/min.
The electric arc melting furnace of this example has a current of 15-25kA, a voltage of 25-35V, and a vacuum of 1.5-3.5Pa.
The electric arc melting furnace of this example had a current of 20kA, a voltage of 30V and a vacuum degree of 2.0Pa.
The specific operation steps of the pre-modification treatment in the embodiment are as follows:
s1: delivering the molding material to 100-300v voltage for bombardment treatment, wherein the bombardment pressure is 10-20min;
s2: then the mixture is sent to be preheated at 500-600 ℃ for 10-30min, after the preheating is finished, the mixture is cooled to 300 ℃ at the speed of 1-3 ℃/min, and the heat preservation is continued for 25-35min;
s3: then, current is conducted for treatment, the current intensity is 1-4A, the current time is 10-20min, then low-pressure sintering is carried out, and the pressure of the low-pressure sintering is 1-4MPa, so that the treated material is obtained.
Preferably, the specific operation steps of the air-cooling treatment are as follows:
firstly, soaking by adopting a sodium dodecyl sulfate solution with the mass fraction of 1-5%, wherein the soaking temperature is 35-45 ℃ and the soaking time is 10-20min;
then blowing and injecting the pre-modified product by adopting low-temperature nitrogen at the temperature of minus 5 ℃ with the blowing and injecting pressure of 1-5Mpa and the blowing and injecting time of 10-20min;
finally, cleaning the mixture in deionized water at 60-80 ℃ for 1-3 times, and then drying the mixture.
The specific operation steps of the high-frequency refinement process of the present embodiment are:
firstly, carrying out refining treatment at a frequency of 150-180KHz, wherein the refining time is 5-10min, and the refining temperature is 210-240 ℃;
then the refining temperature is adjusted to 160-200 ℃, the frequency is reduced to 120-130KHz, and the refining is continued for 10-20min;
and finally, continuously refining for 20-30min at 120-150 ℃, and naturally cooling to room temperature at a speed of 1-3 ℃/min after finishing refining.
Example 1.
The alloy sputtering target material for the flat panel display comprises molybdenum niobium, a grain refining agent, a rare earth element improver and a flowing agent; the mass ratio of the molybdenum to niobium to the refined grain agent to the rare earth element improver to the flowable agent is 9:1:1.5:0.5;
the preparation method of the grain refining agent comprises the following steps:
s1: smelting: te and Mo are mixed according to the weight ratio of 3:1, and then are sent into a smelting furnace for smelting until the raw materials are completely melted;
s2: naturally cooling and molding the smelted raw materials, and then carrying out hot rolling and cold rolling treatment:
s3: finally, homogenizing;
homogenizing at 300deg.C for 15min, naturally cooling to 200deg.C at a rate of 1deg.C/min, keeping the temperature for 10min, and naturally cooling to room temperature.
The rare earth element modifier is prepared by mixing rare earth lanthanum and TaC according to a weight ratio of 2:1.
The flow agent of this embodiment is silicon powder.
The hot rolling temperature in the hot rolling and cold rolling treatment of the embodiment is 500 ℃, the hot rolling time is 15min, the hot rolling deformation rate is 30%, and the hot rolling is finished;
then cold rolling is carried out at 0 ℃ for 35min, and the cold rolling deformation rate is 10%.
The preparation method of the alloy sputtering target material for the flat panel display comprises the following steps:
step one, smelting treatment: feeding molybdenum niobium, a grain refining agent, a rare earth element improver and a flowing agent into an arc melting furnace for treatment until the raw materials are completely melted, and after the raw materials are melted, rotating at 100r/min for 20min;
step two, feeding the smelted raw materials into a mould box for pressurizing, cooling and forming, wherein the pressurizing pressure is 5MPa, the pressure is maintained for 10s, and the cooling temperature is reduced to room temperature at a speed of 1 ℃/min to obtain a formed material;
step three, carrying out pre-modification treatment on the molding material:
fourth, rapid air cooling treatment: improving the product subjected to the pre-modification treatment by adopting air cooling treatment, and then performing high-frequency refinement treatment;
step five, carrying out homogenization treatment;
the specific treatment method comprises the following steps:
heating the treated material to 200 ℃ for 13min, then heating to 550 ℃ at the speed of 1 ℃/min, continuing to keep the temperature for 10-30min, ending the reaction, then cooling to 130 ℃ at the speed of 5 ℃/min, continuing to keep the temperature for 20min, ending the heat preservation, and naturally cooling to room temperature;
step six, finally performing aging treatment; the temperature in the aging treatment is 500 ℃, the aging time is 10min, and finally the temperature is reduced to room temperature at the speed of 1 ℃/min.
The electric arc melting furnace of this example had a current of 15kA, a voltage of 25V and a vacuum of 1.5Pa.
The specific operation steps of the pre-modification treatment in the embodiment are as follows:
s1: delivering the molding material to 100v voltage for bombardment treatment, wherein the bombardment pressure is 10min;
s2: then the mixture is sent to be preheated at 500 ℃ for 10min, after the preheating is finished, the mixture is cooled to 300 ℃ at the speed of 1 ℃/min, and the heat preservation is continued for 25min;
s3: then, current treatment is conducted, the current intensity is 1A, the current time is 10min, and then low-pressure sintering is conducted, wherein the pressure of the low-pressure sintering is 1MPa, so that the treated material is obtained.
Preferably, the specific operation steps of the air-cooling treatment are as follows:
firstly, soaking by adopting a sodium dodecyl sulfate solution with the mass fraction of 1%, wherein the soaking temperature is 35 ℃, and the soaking time is 10min;
then blowing and jetting the pre-modified product with nitrogen at the low temperature of-5 ℃ for 10min, wherein the blowing and jetting pressure is 1 Mpa;
and finally, cleaning for 1 time in deionized water at 60 ℃, and then drying.
The specific operation steps of the high-frequency refinement process of the present embodiment are:
firstly, carrying out thinning treatment at the frequency of 150KHz, wherein the thinning time is 5min, and the thinning temperature is 210 ℃;
then the refining temperature is adjusted to 160 ℃, the frequency is reduced to 120KHz, and the refining is continued for 10min;
and finally, continuously refining for 20min at 120 ℃, and naturally cooling to room temperature at the speed of 1 ℃/min after finishing refining.
Example 2.
The alloy sputtering target material for the flat panel display comprises molybdenum niobium, a grain refining agent, a rare earth element improver and a flowing agent; the mass ratio of the molybdenum to niobium to the refined grain agent to the rare earth element improver to the flowable agent is 11:4:2.5:0.5;
the preparation method of the grain refining agent comprises the following steps:
s1: smelting: te and Mo are mixed according to the weight ratio of 3:1, and then are sent into a smelting furnace for smelting until the raw materials are completely melted;
s2: naturally cooling and molding the smelted raw materials, and then carrying out hot rolling and cold rolling treatment:
s3: finally, homogenizing;
homogenizing at 400deg.C for 25min, naturally cooling to 200deg.C at 3deg.C/min, keeping for 30min, and naturally cooling to room temperature.
The rare earth element modifier is prepared by mixing rare earth lanthanum and TaC according to a weight ratio of 2:1.
The flow agent of this embodiment is silicon powder.
The hot rolling temperature in the hot rolling and cold rolling treatment of the embodiment is 800 ℃, the hot rolling time is 25min, the hot rolling deformation rate is 50%, and the hot rolling is finished;
then cold rolling is carried out at 20 ℃ for 45min, and the cold rolling deformation rate is 20%.
The preparation method of the alloy sputtering target material for the flat panel display comprises the following steps:
step one, smelting treatment: feeding molybdenum niobium, a grain refining agent, a rare earth element improver and a flowing agent into an arc melting furnace for treatment until the raw materials are completely melted, and after the raw materials are melted, rotating at 500r/min for 30min;
step two, feeding the smelted raw materials into a mould box for pressurizing, cooling and forming, wherein the pressurizing pressure is 10MPa, the pressure is maintained for 20s, and the cooling temperature is reduced to room temperature at a speed of 5 ℃/min to obtain a formed material;
step three, carrying out pre-modification treatment on the molding material:
fourth, rapid air cooling treatment: improving the product subjected to the pre-modification treatment by adopting air cooling treatment, and then performing high-frequency refinement treatment;
step five, carrying out homogenization treatment;
the specific treatment method comprises the following steps:
heating the treated material at 400 ℃ for 30min, then heating to 550 ℃ at the speed of 3 ℃/min, continuing to keep the temperature for 30min, ending the reaction, then cooling to 150 ℃ at the speed of 5 ℃/min, continuing to keep the temperature for 30min, ending the heat preservation, and naturally cooling to room temperature;
step six, finally performing aging treatment; the temperature in the aging treatment is 700 ℃, the aging time is 30min, and finally the temperature is reduced to room temperature at the speed of 5 ℃/min.
The electric arc melting furnace of this example had a current of 25kA, a voltage of 35V and a vacuum of 3.5Pa.
The specific operation steps of the pre-modification treatment in the embodiment are as follows:
s1: delivering the molding material to 300v voltage for bombardment treatment, wherein the bombardment pressure is 20min;
s2: then the mixture is sent to be preheated at 600 ℃ for 30min, after the preheating is finished, the mixture is cooled to 300 ℃ at the speed of 3 ℃/min, and the heat preservation is continued for 35min;
s3: then, current treatment is conducted, the current intensity is 4A, the current time is 20min, and then low-pressure sintering is conducted, wherein the pressure of the low-pressure sintering is 4MPa, so that the treated material is obtained.
The specific operation steps of the air cooling treatment in this embodiment are as follows:
firstly, soaking by adopting 5% sodium dodecyl sulfate solution with the soaking temperature of 45 ℃ and the soaking time of 20min;
then blowing and injecting the pre-modified product by adopting low-temperature nitrogen at the temperature of-5 ℃ for 20min, wherein the blowing and injecting pressure is 5 Mpa;
and finally, cleaning the mixture in deionized water at 80 ℃ for 3 times, and then drying the mixture.
The specific operation steps of the high-frequency refinement process of the present embodiment are:
firstly, refining at the frequency of 180KHz for 10min at 240 ℃;
then the refining temperature is adjusted to 200 ℃, the frequency is reduced to 130KHz, and the refining is continued for 20min;
and finally, continuously refining for 30min at 150 ℃, and naturally cooling to room temperature at the speed of 3 ℃/min after finishing refining.
Example 3.
The alloy sputtering target material for the flat panel display comprises molybdenum niobium, a grain refining agent, a rare earth element improver and a flowing agent; the mass ratio of the molybdenum to niobium to the refined grain agent to the rare earth element improver to the flowable agent is 10:2.5:2:0.5;
the preparation method of the grain refining agent comprises the following steps:
s1: smelting: te and Mo are mixed according to the weight ratio of 3:1, and then are sent into a smelting furnace for smelting until the raw materials are completely melted;
s2: naturally cooling and molding the smelted raw materials, and then carrying out hot rolling and cold rolling treatment:
s3: finally, homogenizing;
homogenizing at 350deg.C for 20min, naturally cooling to 200deg.C at a rate of 2deg.C/min, keeping the temperature for 20min, and naturally cooling to room temperature.
The rare earth element modifier is prepared by mixing rare earth lanthanum and TaC according to a weight ratio of 2:1.
The flow agent of this embodiment is silicon powder.
The hot rolling temperature in the hot rolling and cold rolling treatment of the embodiment is 650 ℃, the hot rolling time is 20min, the hot rolling deformation rate is 40%, and the hot rolling is finished;
then cold rolling is carried out at 10 ℃ for 40min, and the cold rolling deformation rate is 15%.
The preparation method of the alloy sputtering target material for the flat panel display comprises the following steps:
step one, smelting treatment: feeding molybdenum niobium, a grain refining agent, a rare earth element improver and a flowing agent into an arc melting furnace for treatment until the raw materials are completely melted, and after the raw materials are melted, rotating at 300r/min for 25min;
step two, feeding the smelted raw materials into a mould box for pressurizing, cooling and forming, wherein the pressurizing pressure is 7.5MPa, the pressure is maintained for 15s, and the cooling temperature is reduced to room temperature at a speed of 3 ℃/min to obtain a formed material;
step three, carrying out pre-modification treatment on the molding material:
fourth, rapid air cooling treatment: improving the product subjected to the pre-modification treatment by adopting air cooling treatment, and then performing high-frequency refinement treatment;
step five, carrying out homogenization treatment;
the specific treatment method comprises the following steps:
heating the treated material at 300 ℃ for 20min, then heating to 550 ℃ at the speed of 2 ℃/min, continuing to keep the temperature for 20min, ending the reaction, then cooling to 140 ℃ at the speed of 5 ℃/min, continuing to keep the temperature for 25min, ending the heat preservation, and naturally cooling to room temperature;
step six, finally performing aging treatment; the temperature in the aging treatment is 600 ℃, the aging time is 20min, and finally the temperature is reduced to room temperature at the speed of 3 ℃/min.
The electric arc melting furnace of this example had a current of 20kA, a voltage of 30V and a vacuum degree of 2.0Pa.
The specific operation steps of the pre-modification treatment in the embodiment are as follows:
s1: delivering the molding material to 200v voltage for bombardment treatment, wherein the bombardment pressure is 15min;
s2: then the mixture is sent to be preheated at 550 ℃ for 20min, after the preheating is finished, the mixture is cooled to 300 ℃ at the speed of 2 ℃/min, and the heat preservation is continued for 30min;
s3: then, current is conducted for treatment, the current intensity is 2.5A, the current time is 15min, and then low-pressure sintering is carried out, wherein the pressure of the low-pressure sintering is 2.5MPa, so that the treated material is obtained.
The specific operation steps of the air cooling treatment in this embodiment are as follows:
firstly, soaking by adopting 3% sodium dodecyl sulfate solution with the soaking temperature of 40 ℃ and the soaking time of 15min;
then blowing and injecting the pre-modified product by adopting low-temperature nitrogen at the temperature of minus 5 ℃ with the blowing and injecting pressure of 3Mpa and the blowing and injecting time of 15min;
and finally, cleaning the mixture in deionized water at 70 ℃ for 2 times, and then drying the mixture.
The specific operation steps of the high-frequency refinement process of the present embodiment are:
firstly, carrying out refining treatment at a frequency of 160KHz, wherein the refining time is 7.5min, and the refining temperature is 220 ℃;
then the refining temperature is adjusted to 170 ℃, the frequency is reduced to 125KHz, and the refining is continued for 15min;
and finally, continuing to refine for 25min at 135 ℃, and naturally cooling to room temperature at the speed of 2 ℃/min after finishing refining.
Comparative example 1.
Unlike example 3, no rapid air cooling treatment was used in the preparation of the alloy sputtering target.
Comparative example 2.
Unlike example 3, no homogenization treatment was performed in the preparation of the alloy sputtering target.
The elongation percentage of the product is measured by using the GB/T228-2010 standard.
The results of the performance measurements of examples 1-3 and comparative examples 1-2 are as follows
From examples 1-3 and comparative examples 1-2, the product of example 3 of the present invention is excellent in both density and elongation, and the properties of the prepared product can be significantly improved.
Fatigue cycle performance was further tested:
the specific operation steps of the pre-modification treatment are further determined:
the specific operation steps of the pre-modification treatment are as follows:
s1: delivering the molding material to 200v voltage for bombardment treatment, wherein the bombardment pressure is 15min;
s2: then the mixture is sent to be preheated at 550 ℃ for 20min, after the preheating is finished, the mixture is cooled to 300 ℃ at the speed of 2 ℃/min, and the heat preservation is continued for 30min;
s3: then, current is conducted for treatment, the current intensity is 2.5A, the current time is 15min, and then low-pressure sintering is carried out, wherein the pressure of the low-pressure sintering is 2.5MPa, so that the treated material is obtained.
The invention further explores the product performance through the pre-modification treatment
Experimental example 1.
The pretreatment was not bombardment-treated.
Experimental example 2.
The preheating treatment is not carried out by adopting the speed of 2 ℃/min to reduce to 300 ℃.
Experimental example 3.
No low pressure sintering treatment was performed.
From experimental examples 1 to 3, it can be seen that the bombardment treatment, the low-pressure sintering treatment and the treatment of lowering the temperature to 300 ℃ at a rate of 2 ℃/min in the pre-modification treatment have a certain influence on the elongation of the product, and based on this, the pre-modification treatment has an improvement effect on the elongation of the product.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (6)
1. An alloy sputtering target material for a flat panel display is characterized by comprising molybdenum niobium, a grain refining agent, a rare earth element improver and a flowing agent; the mass ratio of the molybdenum to niobium to the refined grain agent to the rare earth element improver to the flowing agent is (9-11): (1-4): (1.5-2.5): 0.5;
the preparation method of the grain refining agent comprises the following steps:
s1: smelting: te and Mo are mixed according to the weight ratio of 3:1, and then are sent into a smelting furnace for smelting until the raw materials are completely melted;
s2: naturally cooling and molding the smelted raw materials, and then carrying out hot rolling and cold rolling treatment:
s3: finally, homogenizing;
homogenizing at 300-400deg.C for 15-25min, naturally cooling to 200deg.C at a rate of 1-3deg.C/min, keeping the temperature for 10-30min, and naturally cooling to room temperature; the rare earth element modifier is prepared by mixing rare earth lanthanum and TaC according to a weight ratio of 2:1; the flowing agent is silicon powder; the hot rolling temperature in the hot rolling and cold rolling treatment is 500-800 ℃, the hot rolling time is 15-25min, the hot rolling deformation rate is 30-50%, and the hot rolling is finished;
then cold rolling is carried out at 0-20 ℃ for 35-45min, and the cold rolling deformation rate is 10-20%;
the preparation method of the alloy sputtering target material for the flat panel display comprises the following steps:
step one, smelting treatment: feeding molybdenum niobium, grain refining agent, rare earth element modifier and flowing agent into an arc melting furnace for treatment until the raw materials are completely melted, and after the raw materials are melted, rotating at a speed of 100-500r/min for 20-30min;
step two, feeding the smelted raw materials into a mould box for pressurizing, cooling and forming, wherein the pressurizing pressure is 5-10MPa, the pressure is maintained for 10-20s, and the cooling temperature is reduced to room temperature at a speed of 1-5 ℃/min, so as to obtain a formed material;
step three, carrying out pre-modification treatment on the molding material:
fourth, rapid air cooling treatment: improving the product subjected to the pre-modification treatment by adopting air cooling treatment, and then performing high-frequency refinement treatment;
step five, carrying out homogenization treatment;
the specific treatment method comprises the following steps:
heating the treated material at 200-400 deg.c for 10-30min, heating to 550 deg.c at the rate of 1-3 deg.c/min, maintaining for 10-30min, cooling to 130-150 deg.c at the rate of 5 deg.c/min, maintaining for 20-30min, and cooling to room temperature;
step six, finally performing aging treatment; the temperature in the aging treatment is 500-700 ℃, the aging time is 10-30min, and finally the temperature is reduced to room temperature at the speed of 1-5 ℃/min.
2. The alloy sputtering target for flat panel display according to claim 1, wherein the electric current of the arc melting furnace is 15 to 25kA, the voltage is 25 to 35V, and the vacuum degree is 1.5 to 3.5Pa.
3. The alloy sputtering target for a flat panel display according to claim 1, wherein the arc melting furnace has a current of 20kA, a voltage of 30V, and a vacuum degree of 2.0Pa.
4. The alloy sputtering target for flat panel display according to claim 1, wherein the pre-modification treatment comprises the following specific steps:
s1: delivering the molding material to 100-300v voltage for bombardment treatment, wherein the bombardment pressure is 10-20min;
s2: then the mixture is sent to be preheated at 500-600 ℃ for 10-30min, after the preheating is finished, the mixture is cooled to 300 ℃ at the speed of 1-3 ℃/min, and the heat preservation is continued for 25-35min;
s3: then, current is conducted for treatment, the current intensity is 1-4A, the current time is 10-20min, then low-pressure sintering is carried out, and the pressure of the low-pressure sintering is 1-4MPa, so that the treated material is obtained.
5. The alloy sputtering target for flat panel display according to claim 4, wherein the specific operation steps of the air-cooling treatment are as follows:
firstly, soaking by adopting a sodium dodecyl sulfate solution with the mass fraction of 1-5%, wherein the soaking temperature is 35-45 ℃ and the soaking time is 10-20min;
then blowing and injecting the pre-modified product by adopting low-temperature nitrogen at the temperature of minus 5 ℃ with the blowing and injecting pressure of 1-5Mpa and the blowing and injecting time of 10-20min;
finally, cleaning the mixture in deionized water at 60-80 ℃ for 1-3 times, and then drying the mixture.
6. The alloy sputtering target for flat panel display according to claim 5, wherein the high-frequency refining process comprises the following steps:
firstly, carrying out refining treatment at a frequency of 150-180KHz, wherein the refining time is 5-10min, and the refining temperature is 210-240 ℃;
then the refining temperature is adjusted to 160-200 ℃, the frequency is reduced to 120-130KHz, and the refining is continued for 10-20min;
and finally, continuously refining for 20-30min at 120-150 ℃, and naturally cooling to room temperature at a speed of 1-3 ℃/min after finishing refining.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111350335.2A CN114231915B (en) | 2021-11-15 | 2021-11-15 | Alloy sputtering target material for flat panel display and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111350335.2A CN114231915B (en) | 2021-11-15 | 2021-11-15 | Alloy sputtering target material for flat panel display and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114231915A CN114231915A (en) | 2022-03-25 |
| CN114231915B true CN114231915B (en) | 2023-09-19 |
Family
ID=80749447
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111350335.2A Active CN114231915B (en) | 2021-11-15 | 2021-11-15 | Alloy sputtering target material for flat panel display and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114231915B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321871A (en) * | 2011-09-19 | 2012-01-18 | 基迈克材料科技（苏州）有限公司 | Hot isostatic pressing is produced the method for flat-panel monitor with the molybdenum alloy sputtering target material |
| JP2013083000A (en) * | 2011-09-28 | 2013-05-09 | Hitachi Metals Ltd | METHOD OF MANUFACTURING SINTERED Mo ALLOY SPUTTERING TARGET MATERIAL |
| JP2016188394A (en) * | 2015-03-30 | 2016-11-04 | 日立金属株式会社 | Mo alloy target |
| CN109280892A (en) * | 2018-11-13 | 2019-01-29 | 江苏迪丞光电材料有限公司 | The preparation method and target of flat-panel monitor molybdenum alloy sputtering target |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190161850A1 (en) * | 2017-11-30 | 2019-05-30 | Tosoh Smd, Inc. | Ultra-fine grain size tantalum sputtering targets with improved voltage performance and methods thereby |
-
2021
- 2021-11-15 CN CN202111350335.2A patent/CN114231915B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321871A (en) * | 2011-09-19 | 2012-01-18 | 基迈克材料科技（苏州）有限公司 | Hot isostatic pressing is produced the method for flat-panel monitor with the molybdenum alloy sputtering target material |
| JP2013083000A (en) * | 2011-09-28 | 2013-05-09 | Hitachi Metals Ltd | METHOD OF MANUFACTURING SINTERED Mo ALLOY SPUTTERING TARGET MATERIAL |
| JP2016188394A (en) * | 2015-03-30 | 2016-11-04 | 日立金属株式会社 | Mo alloy target |
| CN109280892A (en) * | 2018-11-13 | 2019-01-29 | 江苏迪丞光电材料有限公司 | The preparation method and target of flat-panel monitor molybdenum alloy sputtering target |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114231915A (en) | 2022-03-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110952064A (en) | Tantalum-silicon alloy sputtering target material and preparation method thereof | |
| CN103572225B (en) | The manufacture method of tantalum target and tantalum target assembly | |
| CN109355632B (en) | Method for improving grain uniformity of molybdenum and molybdenum alloy sputtering target material | |
| CN113073299B (en) | Preparation method of chromium-silicon alloy sputtering target material | |
| CN114892135B (en) | High-purity copper target material and preparation method and application thereof | |
| CN106011738A (en) | Surface plating composite coating process for die | |
| CN104419901A (en) | Method for manufacturing tantalum target material | |
| CN106521434B (en) | A kind of preparation method of the high-purity tantalum target with preferred orientation | |
| CN113737011B (en) | Preparation method of ultra-high purity copper-manganese alloy | |
| WO2023208249A1 (en) | Preparation method for molybdenum alloy tube target material, molybdenum alloy tube target material, and application | |
| WO2023186188A1 (en) | Molybdenum alloy target material, and preparation method and application thereof | |
| CN114231915B (en) | Alloy sputtering target material for flat panel display and preparation method thereof | |
| CN114855131A (en) | Preparation method of molybdenum alloy target, molybdenum alloy target and application | |
| CN106435261A (en) | Long-service-life copper-manganese based alloy target with ultrafine-grained microstructure and processing method thereof | |
| CN114293158B (en) | Preparation method of tungsten-silicon alloy target | |
| CN106567048B (en) | A kind of manufacturing method of large size High-Purity Molybdenum alloy rotary target material | |
| CN114411104A (en) | High-purity silver target and preparation method and application thereof | |
| CN108465700B (en) | Tantalum plate rolling method for obtaining sputtering target material with uniform structure and texture | |
| CN113652658A (en) | La-Zr alloy target and preparation method thereof | |
| CN116804261B (en) | GH738 alloy bar and preparation method thereof | |
| CN114934202B (en) | Tantalum-molybdenum alloy target material and preparation method and application thereof | |
| CN105063540A (en) | Method for preparing Ni-WC coating on surface of low-carbon steel piece | |
| CN114000073A (en) | Process method for improving internal structure of high-purity nickel target material | |
| CN107619972B (en) | Manufacturing method of aluminum-neodymium alloy for magnetron sputtering target material | |
| CN114262874B (en) | Target material for building glass and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |