CN114635063B - Preparation method of aluminum-based alloy target material for hard coating without original powder grain boundary - Google Patents
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention provides a preparation method of an aluminum-based alloy target material for a hard coating without an original powder grain boundary. The method comprises the steps of taking aluminum powder and one or more other element powders as raw materials, performing ball milling mixing pretreatment on the raw material powders, performing cold isostatic pressing treatment, loading the cold isostatic pressed compact into a sheath, performing vacuum thermal degassing treatment, performing hot rolling on the degassed sheath to realize densification and forming of the powder, controlling the microstructure of a target through thermal treatment, and finally performing mechanical processing to obtain a target finished product. The aluminum-based alloy target material for the hard coating, which is prepared by the invention, has the following advantages: (1) The alloy composition has a wide proportion range, and other element powders can be one or more of powders of titanium, chromium, silicon, tungsten, vanadium, boron, tantalum, yttrium, niobium, molybdenum, zirconium, hafnium and the like; (2) the target material has high density, and the relative density reaches more than 99 percent; (3) the target material has high purity and can be freely adjusted; (4) the target microstructure has no primary powder grain boundaries.
Description
Technical Field
The invention relates to the technical field of test systems, in particular to an aluminum-based alloy target, and specifically relates to a preparation method of an aluminum-based alloy target for hard coating in the fields of cutters, dies and the like without original powder grain boundaries. .
Background
The hard coating is mainly applied to coating of cutters and dies. The film plating cutter has the advantages of high hardness, gao Moji binding force, high-temperature oxidation resistance, low friction coefficient and the like. The use of the film plating cutter can realize high feed depth, high feed speed, high cutting precision and hard cutting, and greatly improve the processing quality and efficiency. The use of the film coating die can greatly prolong the service life of the die, reduce the surface roughness of the product and improve the quality of the product.
Targets as key consumables are one of the important factors for preparing high-performance hard coatings. The main component system of the aluminum-based alloy target material for the hard coating at present comprises two types of aluminum-titanium base and aluminum-chromium base. The basic components of the alloy are aluminum+titanium and aluminum+chromium, which gradually develop into aluminum+X+Y and aluminum+X+Y+Z, wherein the element X is titanium or chromium, the element Y is silicon, and the element Z is one or more of tungsten, vanadium, boron, tantalum, yttrium, niobium, molybdenum, zirconium, hafnium and the like. At present, an aluminum-based alloy target material for a hard coating is mainly prepared by adopting a hot isostatic pressing process. However, the hot isostatic pressing process has the defects of high equipment, high pressing cost and the like, and the hot isostatic pressing aluminum-based alloy target material has obvious original powder grain boundaries. When in coating, larger molten pools are easy to form at the boundary of original powder particles in the target material, and liquid drops are formed to splash on the film layer, so that large particles with larger size and larger quantity exist in the film, the composition, hardness and roughness of the film layer are affected, and the performance of the film layer is reduced. Therefore, it is necessary to invent a method for preparing an aluminum-based alloy target for hard coating with high performance, low cost and no primary powder grain boundary.
Disclosure of Invention
The invention aims at: aiming at the defects and shortcomings of the prior art, the invention aims to provide a preparation method of an aluminum-based alloy target material for a hard coating, which has high performance, low cost and no primary grain boundary. The aluminum-based alloy target material for the hard coating, which has the advantages of wide proportion range of alloy components, high purity, high density, no original powder grain boundary of a microstructure, fine and uniform grain size and good matching property with coating equipment and a coating process, can be obtained without using hot isostatic pressing equipment, and meets the preparation requirements of the hard coating in different application fields such as cutters, dies and the like.
The technical scheme of the invention is as follows:
1. raw material powder selection and ball milling mixing pretreatment
The raw material powder of the invention consists of aluminum powder and other element powder. The other element powder can be one or more of titanium, chromium, silicon, tungsten, vanadium, boron, tantalum, yttrium, niobium, molybdenum, zirconium, hafnium and other powder, the total content of other elements is 1-50at%, and the balance is aluminum. The purity and the oxygen content of the raw material powder are controlled, so that the purity and the oxygen content of the target finished product are controlled, and a foundation is laid for eliminating the grain boundaries of the original powder in the target subsequently. The purity of the raw aluminum powder is 99.9 percent, and the oxygen content is less than 500ppm; the purity of other element powder is 99.8-99.95%, and the oxygen content is less than 1500ppm.
Through ball milling mixing pretreatment, on one hand, the discrete segregation resistance of the mixed powder can be improved; on the other hand, the method can primarily destroy the oxide film on the surface of the aluminum powder, and lays a foundation for eliminating the original powder grain boundary in the target material subsequently. The ball milling and mixing pretreatment process comprises the steps of mixing and ball milling raw material powder in a V-shaped mixer, a biconical mixer or a three-dimensional mixer protected by argon according to the component proportion, wherein the specific process comprises the ball milling time of 2-16 h and the ball material weight ratio of 1:3-10:1.
2. Cold isostatic pressing treatment
The raw material powder is subjected to ball milling mixing pretreatment and then is subjected to cold isostatic pressing treatment. The cold isostatic pressing treatment can obtain a compact with high density, and the relative density of the compact is 75-85%. The cold isostatic pressing effect is three, firstly, the shrinkage during densification is reduced, and the risk of the sheath being pulled apart is reduced; secondly, the diffusion capacity of the original powder is improved, and a foundation is laid for realizing powder densification through a hot rolling process in the follow-up process; thirdly, the raw material powder is subjected to plastic deformation, so that an oxide film on the surface of the raw material powder is further damaged, and a foundation is laid for eliminating the original powder grain boundary in the target material subsequently. The cold isostatic pressing treatment process is carried out under the pressure of 180-240 MPa and the pressure maintaining time of 15-30 min.
3. Vacuum thermal degassing treatment
In the invention, the cold isostatic pressed compact is filled into a sheath and then subjected to vacuum thermal degassing treatment. The vacuum heat degassing treatment has two main effects, namely, the residual gas in the cold isostatic pressing compact is pumped out, so that the resistance in the follow-up powder densification through a hot rolling process is reduced; secondly, the oxygen content in the cold isostatic pressing compact is reduced, and a foundation is laid for eliminating the original powder grain boundary in the target material subsequently. The book is provided withThe vacuum thermal degassing treatment process is that the final degassing temperature is 300-500 ℃, and the final vacuum degree is more than 1 multiplied by 10 -3 Pa, and preserving heat for 60-300 min on the basis.
4. Hot rolling treatment
In the invention, the degassed sheath is subjected to hot rolling treatment. The hot rolling treatment has three main effects, namely, the densification and formation of the powder are realized through a hot rolling process; secondly, the densification forming of the powder is realized, meanwhile, the powder is subjected to plastic deformation, oxide films on the surfaces of powder particles are destroyed, and the boundaries of original powder particles are eliminated; thirdly, the microstructure of the target material is controlled, and a foundation is laid for subsequent heat treatment. The hot rolling process of the invention has the rolling temperature of 400-550 ℃ at the beginning and the rolling temperature of more than 300 ℃ at the end, the rolling reduction of 30-90%, the rolling passes of 1-7 times and the rolling rate of 0.2-1.5 m/s.
5. Heat treatment of
In the invention, the target material after hot rolling treatment is subjected to heat treatment. The heat treatment has two main effects, namely, the control of the internal microstructure and grain size of the target material; and secondly, the internal stress of the target material is eliminated, and the subsequent machining is facilitated. The heat treatment process is carried out at 350-500 ℃, the temperature is kept for 30-60 min, and the air is cooled.
The invention has the remarkable effects that:
(1) The aluminum-based alloy target prepared in the invention has no original powder grain boundary. The selection of the raw material powder controls the oxygen content in the raw material powder; ball milling mixing and cold isostatic pressing treatment to primarily destroy oxide films on the surfaces of the raw material powder particles; the vacuum heat degassing treatment further reduces the oxygen content in the cold isostatic pressed compact; on the basis of the previous steps, the hot rolling treatment realizes the densification and shaping of the powder, and simultaneously, the powder is subjected to plastic deformation, so that oxide films on the surfaces of powder particles are destroyed, and finally, the original powder particle boundaries are eliminated.
(2) While the microstructure in the traditional hot isostatic pressing aluminum-based alloy target is isotropic, the aluminum-based alloy target prepared by the invention can control the anisotropy and the grain size of the microstructure through hot rolling and heat treatment processes, and the average grain size of an aluminum substrate is smaller than 10 mu m, so that the target is well matched with coating equipment and a coating process.
(3) The densification of the aluminum-based alloy target can be realized without using expensive hot isostatic pressing equipment, and the production cost is reduced.
Drawings
Fig. 1 is a microstructure view of a conventional hot isostatic pressing aluminum-titanium alloy target.
Fig. 2 is a microstructure of an aluminum-titanium alloy target in example 1 according to the present invention.
FIG. 3 is a microstructure of an aluminum matrix of an aluminum-titanium alloy target in accordance with example 1 of the present invention
Detailed Description
The present invention will be further described below by way of specific examples, but is not limited thereto.
Example 1
The purity of the aluminum powder of the raw material powder is 99.9%, the oxygen content is 400ppm, the purity of the titanium powder is 99.8%, and the oxygen content is 1200ppm. And (3) ball-milling and mixing the aluminum powder and the titanium powder in a V-shaped mixer according to the component proportion Ti33Al67at percent. The ball milling and mixing process is carried out for 4 hours, and the ball-material ratio is 1:1.
And (5) carrying out cold isostatic pressing treatment on the mixed powder. The cold isostatic pressing process is 200MPa and the dwell time is 20min.
And loading the cold isostatic pressing pressed compact into a pure aluminum sheath for vacuum thermal degassing treatment. The vacuum thermal degassing process has final degassing temperature of 400 deg.C and final vacuum degree of more than 1×10 -3 Pa, and preserving heat for 180min on the basis.
And carrying out hot rolling and heat treatment on the degassed sheath. The hot rolling treatment process is that the initial rolling temperature is 450 ℃, the final rolling temperature is more than 300 ℃, the rolling reduction is 40%, the rolling passes are 3 times, and the rolling speed is 1m/s.
And (3) carrying out heat treatment on the target material after the hot rolling treatment, wherein the heat treatment process is 400 ℃, preserving the heat for 30min and cooling the target material in air. Through detection, the relative density of the aluminum-titanium target material is 99.3%, and the average grain size of the aluminum matrix is 4.8 mu m.
As can be seen from fig. 1, 2 and 3, according to the process of the present invention, example 1 eliminates the original powder grain boundaries while achieving the densification of the powder, while controlling the average grain size of the aluminum matrix in the target to be less than 10 μm.
Example 2
The purity of the aluminum powder of the raw material powder is 99.9%, the oxygen content is 400ppm, the purity of the chromium powder is 99.9%, and the oxygen content is 500ppm. And (3) ball-milling and mixing the aluminum powder and the chromium powder in a three-dimensional mixer according to the component proportion Cr30Al70at percent. The ball milling and mixing process is carried out for 8 hours, and the ball-material ratio is 3:1. And (5) carrying out cold isostatic pressing treatment on the mixed powder. The cold isostatic pressing process is 220MPa and the dwell time is 15min. And loading the cold isostatic pressing pressed compact into a pure aluminum sheath for vacuum thermal degassing treatment. The vacuum thermal degassing process has final degassing temperature of 500 deg.C and final vacuum degree of more than 1×10 -3 Pa, and incubating for 120min on this basis. And carrying out hot rolling and heat treatment on the degassed sheath. The hot rolling treatment process is that the initial rolling temperature is 500 ℃, the final rolling temperature is more than 300 ℃, the rolling reduction is 60%, the rolling passes are 3 times, and the rolling speed is 0.8m/s. The heat treatment process is 450 ℃, the temperature is kept for 40min, and the air is cooled. Through detection, the relative density of the aluminum-chromium target material is 99.5%, and the average grain size of the aluminum matrix is 8.3 mu m.
Example 3
The purity of the aluminum powder of the raw material powder is 99.9%, the oxygen content is 400ppm, the purity of the chromium powder is 99.9%, the oxygen content is 500ppm, the purity of the vanadium powder is 99.9%, and the oxygen content is 1000ppm. And ball-milling and mixing the aluminum powder, the chromium powder and the vanadium powder in a three-dimensional mixer according to the component proportion Cr45Al45V10at percent. The ball milling and mixing process is carried out for 10 hours, and the ball-material ratio is 4:1. And (5) carrying out cold isostatic pressing treatment on the mixed powder. The cold isostatic pressing process is 240MPa and the dwell time is 20min. And loading the cold isostatic pressing pressed compact into a pure aluminum sheath for vacuum thermal degassing treatment. The vacuum thermal degassing process has final degassing temperature of 500 deg.C and final vacuum degree of more than 1×10 -3 Pa, and incubating for 120min on this basis. And carrying out hot rolling and heat treatment on the degassed sheath. The hot rolling treatment process is that the initial rolling temperature is 520 ℃, the final rolling temperature is more than 300 ℃, the rolling reduction is 50%, the rolling passes are performed for 4 times, and the rolling speed is 0.5m/s. The heat treatment process is 480 ℃, the temperature is kept for 60min, and the air is cooled. Through detection, the relative density of the aluminum-chromium-vanadium target material is 99.2%, and the average grain size of the aluminum matrix is 7.2 mu m.
Example 4
The purity of the raw powder aluminum powder is 99.9%, the oxygen content is 400ppm, the purity of the titanium powder is 99.8%, the oxygen content is 1200ppm, the purity of the silicon powder is 99.9%, and the oxygen content is 800ppm. And (3) ball-milling and mixing aluminum powder, chromium powder and silicon powder in a biconical mixer according to the component proportion Ti30Al60Si10 at%. The ball milling and mixing process is carried out for 6 hours, and the ball-material ratio is 2:1. And (5) carrying out cold isostatic pressing treatment on the mixed powder. The cold isostatic pressing process is 210MPa and the dwell time is 25min. And loading the cold isostatic pressing pressed compact into a pure aluminum sheath for vacuum thermal degassing treatment. The vacuum thermal degassing process has final degassing temperature of 420 deg.C and final vacuum degree of more than 1×10 -3 Pa, and preserving heat for 180min on the basis. And carrying out hot rolling and heat treatment on the degassed sheath. The hot rolling treatment process is that the initial rolling temperature is 480 ℃, the final rolling temperature is more than 300 ℃, the rolling reduction is 30%, the rolling passes are performed for 4 times, and the rolling speed is 0.4m/s. The heat treatment process is 420 ℃, the temperature is kept for 20min, and the air is cooled. Through detection, the relative density of the aluminum titanium silicon target material is 99.4%, and the average grain size of the aluminum matrix is 5.5 mu m.
The preparation method of the aluminum-based alloy target material for the hard coating without the original powder grain boundary comprises the following steps:
s1: raw material powder selection and ball milling mixing pretreatment; selecting raw material powder aluminum powder with the purity of 99.9%, the oxygen content of less than 500ppm, and other element powder with the purity of 99.8% -99.95% and the oxygen content of less than 1500ppm; ball milling and mixing time is 2-16 h, and ball material ratio is 1:3-10:1;
s2: cold isostatic pressing treatment;
cold isostatic pressing the mixed powder;
s3: vacuum thermal degassing treatment;
loading the cold isostatic pressing compact into a sheath, and then carrying out vacuum thermal degassing treatment;
s4: carrying out hot rolling treatment;
carrying out hot rolling treatment on the degassed sheath; the method comprises the steps of carrying out a first treatment on the surface of the
S5: heat treatment of
And carrying out heat treatment on the target after the hot rolling treatment.
In the step S1, mixing and ball milling are carried out in a V-shaped mixer, a biconical mixer or a three-dimensional mixer which are protected by argon.
In the step S1, other element powder is one or more of titanium, chromium, silicon, tungsten, vanadium, boron, tantalum, yttrium, niobium, molybdenum, zirconium, hafnium and other powder.
In the step S2, the pressure is 180-240 MPa, and the pressure maintaining time is 15-30 min.
In the step S3, the degassing temperature is 300-500 ℃, and the final vacuum degree is more than 1 multiplied by 10 -3 Pa, and preserving heat for 60-300 min on the basis.
In the step S4, the rolling temperature is 400-550 ℃, the rolling temperature is more than 300 ℃, the rolling reduction is 30-90%, the rolling passes are 1-7 times, and the rolling speed is 0.2-1.5 m/S.
In the step S5, the heat treatment process is carried out at 350-500 ℃, the temperature is kept for 30-60 min, and the air is cooled.
Claims (3)
1. A preparation method of an aluminum-based alloy target material for a hard coating without an original powder grain boundary is characterized by comprising the following steps: the method comprises the following steps:
s1: raw material powder selection and ball milling mixing pretreatment; the raw material powder consists of aluminum powder and other element powder, wherein the total content of other elements is 1-50at%, and the balance is aluminum; the purity of the aluminum powder is 99.9%, the oxygen content is less than 500ppm, the purity of other element powder is 99.8-99.95%, and the oxygen content is less than 1500ppm; ball milling and mixing time is 2-16 h, and ball material ratio is 1:1-10:1;
s2: cold isostatic pressing treatment;
cold isostatic pressing the mixed powder; the pressure is 180-240 MPa, and the pressure maintaining time is 15-30 min;
s3: vacuum thermal degassing treatment;
loading the cold isostatic pressing compact into a sheath, and then carrying out vacuum thermal degassing treatment; final degassing temperature of 300-500 deg.c and final vacuum degree of greater than 1 x 10 -3 Pa, and preserving heat for 60-300 min on the basis;
s4: carrying out hot rolling treatment;
carrying out hot rolling treatment on the degassed sheath; the rolling temperature is 400-550 ℃ at the beginning, the rolling temperature is more than 300 ℃, the rolling reduction is 30-90%, the rolling passes are 1-7 times, and the rolling speed is 0.2-1.5 m/s;
s5: heat treatment of
And (3) performing heat treatment on the target material after the hot rolling treatment, wherein the heat treatment process is that the temperature is 350-500 ℃, the heat is preserved for 30-60 min, and the air is cooled.
2. The method for preparing an aluminum-based alloy target for hard coating without original powder grain boundaries according to claim 1, wherein the method comprises the following steps: in the step S1, mixing and ball milling are carried out in a V-shaped mixer, a biconical mixer or a three-dimensional mixer which are protected by argon.
3. The method for preparing an aluminum-based alloy target for hard coating without original powder grain boundaries according to claim 1, wherein the method comprises the following steps: in the step S1, the other element powder is one or more of titanium, chromium, silicon, tungsten, vanadium, boron, tantalum, yttrium, niobium, molybdenum, zirconium and hafnium powder.
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