CN117721425A - CrAlO composite target material and preparation method and application thereof - Google Patents
CrAlO composite target material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 239000013077 target material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 54
- 239000000956 alloy Substances 0.000 claims abstract description 54
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000010935 stainless steel Substances 0.000 claims abstract description 20
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims description 51
- 238000001513 hot isostatic pressing Methods 0.000 claims description 34
- 238000000576 coating method Methods 0.000 claims description 18
- 238000007872 degassing Methods 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
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Abstract
The application relates to the technical field of powder metallurgy materials, and particularly discloses a CrAlO composite target material, a preparation method and application thereof. The CrAlO composite target disclosed by the application is of a double-layer structure, wherein the CrAlO alloy target is used as the upper layer of the target, and the stainless steel is used as the bottom layer of the targetThe method comprises the steps of carrying out a first treatment on the surface of the The CrAlO alloy target material comprises the following components in percentage by atom: cr=50-95 at%, α -Al 2 O 3 =5-50at%. The application also discloses a preparation method and application of the CrAlO composite target. By utilizing the technical scheme, the CrAlO alloy target with high density, less impurity element content and high bending strength can be obtained, and the target is uniform in structure, free of segregation and good in film performance.
Description
Technical Field
The application relates to the technical field of powder metallurgy materials, in particular to a CrAlO composite target material, a preparation method and application thereof.
Background
With the development of cutting technology and the requirements of processed materials, more severe requirements are put on the coating of cutting tools. The traditional nitride coating generally has obvious oxidation phenomenon at 800-1000 ℃, and the high-temperature service performance of the coated cutting tool is restricted from being further improved. Due to alpha-Al 2 O 3 Has the characteristics of high-temperature hardness and good oxidation resistance, and simultaneously, the addition of Cr element can induce and promote the formation of alpha phase of the corundum structure, and is more favorable for the coating to obtain Cr with the corundum structure when the content of Cr element in the coating is increased to a higher level 2 O 3 Alpha-phase oxides of the same structure are widely used in the field of PVD coated cutting tools.
Currently, most CrAlO targets are produced by adding alpha-Al to a CrAl target 2 O 3 Is prepared by the method. The Cr content in the target material prepared by the process is generally below 50at percent, so that Al can be used as a matrix and pure Cr powder, pure Al powder and alpha-Al can be used as the matrix 2 O 3 Mixing the powder, hot pressing or hot isostatic pressing sintering at a lower temperature (400-600 ℃) to obtain a bulk material with the density of more than 98%, and finally machining to obtain the target material with the corresponding size. However, with the continued development of coating applications, the use of CrAlO targets with high Cr content is increasing. When the Cr content is more than or equal to 50at%, the corresponding Al content is reduced, and when hot pressing or hot isostatic pressing sintering is carried out at a lower temperature (400-600 ℃), the target material density is low, and the use requirement of the coating film cannot be met.
Disclosure of Invention
In order to improve the compactness of the CrAlO target, the application provides a CrAlO composite target, and a preparation method and application thereof.
The application provides a CrAlO composite target material, which adopts the following technical scheme:
the CrAlO composite target is of a double-layer structure, wherein a CrAlO alloy target is used as a target upper layer, and stainless steel is used as a target bottom layer; the CrAlO alloy target material comprises the following components in percentage by atom: cr=50-95 at%, α -Al 2 O 3 ＝5-50at％。
In order to improve the defect of non-compact CrAlO target material, the sintering temperature needs to be further increased; in the process, the applicant finds that because the melting point of Al is relatively low, the hot pressing or hot isostatic pressing temperature is further increased, aluminum powder or HIP is easily caused to be molten in a sheath, and the hot pressing or hot isostatic pressing sintering is not facilitated due to the liquid phase; meanwhile, when the hot pressing or hot isostatic pressing temperature exceeds 600 ℃, cr and Al alloying reaction, violent heat release, can further cause aluminum and sheath to melt.
The method adopts Cr as a matrix, and only alpha-Al is added into pure Cr 2 O 3 The introduction of pure Al with low melting point elements is avoided, the hot isostatic pressing temperature is further raised to be higher than 800 ℃, and the CrAlO alloy target with the density of more than or equal to 99.2% can be obtained, and the CrAlO alloy target has uniform structure, no segregation and excellent coating performance.
Meanwhile, the stainless steel is used as a target bottom layer, so that the problems that a CrAlO single-layer target is large in brittleness, difficult to machine and easy to crack and break in clamping positions (such as ears, steps and the like) in the using process are solved.
Preferably, the CrAlO alloy target material comprises the following components in percentage by atom: cr=60-90 at%, α -al2o3=10-40 at%.
In a specific embodiment, the CrAlO alloy target consists of the following components in atomic percent: cr=50at%, α -Al 2 O 3 ＝50at％；Cr＝60at％，α-Al 2 O 3 ＝40at％；Cr＝70at％，α-Al 2 O 3 ＝30at％；
Cr＝80at％，α-Al 2 O 3 ＝20at％；Cr＝90at％，α-Al 2 O 3 ＝10at％；Cr＝95at％，α-Al 2 O 3 ＝5at％。
In some specific embodiments, the CrAlO alloy target consists of the following components in atomic percent: cr=50-60 at%, α -Al 2 O 3 ＝40-50at％；Cr＝60-70at％，α-Al 2 O 3 ＝30-40at％；Cr＝70-80at％，α-Al 2 O 3 ＝20-30at％；Cr＝80-90at％，α-Al 2 O 3 ＝10-20at％；Cr＝90-95at％，α-Al 2 O 3 ＝5-10at％；Cr＝80-95at％，α-Al 2 O 3 ＝5-20at％。
Preferably, the relative density of the CrAlO alloy target is more than or equal to 99.2%.
In a second aspect, the present application provides a method for preparing the CrAlO composite target, which specifically includes the following steps:
weighing Cr powder and alpha-Al 2O3 powder according to the component proportion of the CrAlO composite target material, and uniformly mixing to obtain alloy powder;
respectively carrying out compression molding treatment on the alloy powder and the stainless steel powder to obtain an alloy semi-compact pressed compact and a stainless steel semi-compact pressed compact with the relative density of 67-90%;
overlapping the alloy semi-compact pressed compact and the stainless steel semi-compact pressed compact into a sheath, and sequentially carrying out degassing treatment and hot isostatic pressing treatment to obtain a composite blank;
and removing the sheath from the composite blank, and then machining and cleaning to obtain the CrAlO composite target.
Preferably, the specification parameters of each raw material powder are specifically: the purity is more than 99.8wt percent, the granularity of Cr powder is-300 meshes, the purity is more than 99.5wt percent, and the alpha-Al 2 O 3 The powder particle size was-270 mesh.
Preferably, the parameter conditions of the mixing process are: adding 0.5-5wt% of absolute ethyl alcohol according to the weight percentage of the mixed powder, and mixing for 4-8h under the condition of 500-800r/min of rotating speed.
The mixing process in this application is semi-wet mixing, which ensures that Cr powders (7.2 g/cm 3 ) And alpha-Al 2 O 3 (3.95g/cm 3 ) Uniformly mixing, and no component segregation; meanwhile, the filling property of powder during mould pressing is improved, and the problem of edge and corner falling is reduced.
In a specific embodiment, the alloy powder semi-compact has a size of (D110-D220) ×6-40 mm and a compaction pressure of 300-800t.
In a specific embodiment, the stainless steel semi-compact has a size of (D110-D220) ×6-20 mm and a pressing pressure of 200-600t.
The purpose of the degassing is to remove alcohol and gas impurity elements such as oxygen, nitrogen, water vapor and the like which are introduced into the pressed compact, reduce the content of the gas impurity elements in the target material and ensure the purity of the target material; meanwhile, certain negative vacuum is achieved in the sheath, so that the ingot blank is fully densified during hot isostatic pressing.
Preferably, the conditions of the degassing treatment are: at 170-270 deg.C and 3×10 vacuum degree -2 -8×10 -2 Preserving heat for 2-8h under the condition of Pa; then at 400-600deg.C and vacuum degree of 2×10 -2 -2×10 -3 Preserving heat for 6-16h under the condition of Pa.
Experimental analysis shows that the two-stage degassing treatment is selected, so that the low content of the gas impurity elements C and H in the target material is ensured. This is because if alcohol is introduced to wet mix during the powder mixing process, if the degassing time is short or the degassing temperature is low, the alcohol is not completely volatilized, so that the content of C and H in the target material is high.
The sintering temperature, pressure and time of the hot isostatic pressing are matched; the temperature is too high, and the problem of brittle cracking of the target material exists; when the temperature is too low, the density of the target material is low, and the coating performance is affected.
Preferably, the conditions of the hot isostatic pressing are: the temperature is 850-1300 ℃, the pressure is 100-140MPa, and the heat preservation and pressure maintaining time is 2-8h.
Preferably, the conditions of the hot isostatic pressing are: the temperature is 950-1200 ℃, the pressure is 110-130MPa, and the heat preservation and pressure maintaining time is 2-8h.
In a specific embodiment, the temperature of the hot isostatic pressing may be 850 ℃, 950 ℃, 1060 ℃, 1200 ℃, 1300 ℃.
In some specific embodiments, the temperature of the hot isostatic pressing may also be 850-950 ℃, 850-1060 ℃, 850-1200 ℃, 950-1060 ℃, 950-1300 ℃, 1060-1200 ℃, 1060-1300 ℃, 1200-1300 ℃.
Test analysis shows that when the hot isostatic pressing treatment temperature is lower or higher in the process of preparing the alloy target, the density of the target is low, the coating performance is affected, and the bending strength of the target is poor. Therefore, the application controls the hot isostatic pressing treatment to the conditions, so that the comprehensive performance of the alloy target material is ensured.
In a third aspect, the application provides an application of the CrAlO composite target in preparing a cutter coating.
In summary, the technical scheme of the application has the following effects:
the method adopts Cr as a matrix, and only alpha-Al is added into pure Cr 2 O 3 The introduction of pure Al with low melting point elements is avoided, and meanwhile, stainless steel is used as a target material bottom layer; and further, the hot isostatic pressing temperature is raised to be higher than 800 ℃, so that the CrAlO alloy target with the density of more than or equal to 99.2 percent can be obtained, and the CrAlO alloy target has uniform structure, no segregation and excellent coating performance.
Drawings
FIG. 1 is a microstructure of CrAlO composite targets prepared in example 4 of the present application.
Detailed Description
The present application is described in further detail below in conjunction with examples, comparative examples, and performance test runs, which should not be construed as limiting the scope of the claimed application.
Examples
Examples 1 to 6
Examples 1-6 provide a CrAlO composite target, respectively.
The above-described embodiments differ in that: the composition of the CrAlO alloy target is shown in Table 1.
The preparation method of the CrAlO composite target in the embodiment specifically comprises the following steps:
s1: according to Table 1, cr powder and alpha-Al 2 O 3 Weighing the powder according to a proportion, adding the powder into a three-dimensional mixer, adding 2% absolute ethyl alcohol, mixing for 6 hours at the rotating speed of 650r/min, and uniformly mixing to obtain alloy powder; wherein the purity of Cr powder is 99.8wt%, the granularity is 300 mesh, and alpha-Al 2 O 3 The powder purity was 99.5wt% and the powder particle size was-270 mesh.
S2: and (3) filling the alloy powder and the stainless steel powder into a mould respectively for cold press molding to obtain an alloy semi-compact pressed compact and a stainless steel semi-compact pressed compact with the relative density of 70%.
S3: the alloy semi-compact pressed compact and the stainless steel semi-compact pressed compact are stacked and put into a packaging sleeve, and then degassing treatment is carried out, wherein the conditions of the degassing treatment are as follows: at 200 deg.C and 5×10 vacuum degree -2 Preserving heat for 4h under the condition of Pa; then at 500 ℃ and a vacuum degree of 8 multiplied by 10 -3 Preserving heat for 10h under the condition of Pa.
S4: placing the degassed ingot blank into a hot isostatic pressing furnace for hot isostatic pressing treatment, wherein the hot isostatic pressing conditions are as follows: the temperature is 1060 ℃, the pressure is 130MPa, and the heat preservation and pressure maintaining time is 5h.
S5: removing a sheath from the composite blank subjected to hot isostatic pressing through turning, obtaining a CrAlO composite target blank through linear cutting, and obtaining a CrAlO composite target with the required external dimension through common turning or numerical control turning; the dimensions were D164×15mm.
TABLE 1 composition of CrAlO alloy targets in examples 1-6
Examples 7 to 12
Examples 7-12 provide a CrAlO composite target, respectively.
The above embodiment differs from embodiment 4 in that: the specific process parameters for the degassing treatment and the hot isostatic pressing are different and are shown in table 2.
Table 2 specific process parameters for degassing and hot isostatic pressing in examples 4, 7-12
The above examples are identical in composition to the CrAlO alloy target of example 4.
Comparative example
Comparative example 1
This comparative example provides a CrAlO composite target.
This comparative example differs from example 4 in that: step S1 is to add Al powder.
The preparation method of the CrAlO composite target in the comparative example specifically comprises the following steps:
s1: cr powder, alpha-Al 2 O 3 Weighing the powder and the Al powder according to the proportion of 80at%, 10at% and 10at%, adding into a three-dimensional mixer, adding 2% absolute ethyl alcohol, mixing for 6 hours under the condition of the rotating speed of 650r/min, and uniformly mixing to obtain alloy powder; wherein the purity of Cr powder is 99.8wt%, the granularity is 300 mesh, and alpha-Al 2 O 3 The powder purity was 99.5wt% and the powder particle size was-270 mesh.
S2: and (3) filling the alloy powder and the stainless steel powder into a mould respectively for cold press molding to obtain an alloy semi-compact pressed compact and a stainless steel semi-compact pressed compact with the relative density of 70%.
S3: the alloy semi-compact pressed compact and the stainless steel semi-compact pressed compact are stacked and put into a packaging sleeve, and then degassing treatment is carried out, wherein the conditions of the degassing treatment are as follows: at 200 deg.C and 5×10 vacuum degree -2 Preserving heat for 4h under the condition of Pa; then at 500 ℃ and a vacuum degree of 8 multiplied by 10 -3 Preserving heat for 10h under the condition of Pa.
S4: placing the degassed ingot blank into a hot isostatic pressing furnace for hot isostatic pressing treatment, wherein the hot isostatic pressing conditions are as follows: the temperature is 1060 ℃, the pressure is 130MPa, and the heat preservation and pressure maintaining time is 5h.
In this comparative example, al powder was melted due to the excessively high temperature during hot isostatic pressing. Because the Al content is less than or equal to 15at%, the stainless steel sheath is not melted. However, when the ingot blank after HIP is peeled off, many cracks exist on the large surface and the outer circle of the CrAlO target layer, and a finished product cannot be processed. This is due to the fact that Al and Cr undergo alloying reactions, producing brittle and hard AlCr master alloys, resulting in very high internal stresses in the HIP ingots.
Comparative example 2
This comparative example provides a CrAlO monolayer target.
The preparation method of the CrAlO monolayer target in the comparative example specifically comprises the following steps:
this comparative example differs from example 4 in that: the CrAlO composite target is a single-layer CrAlO alloy target and does not contain a bottom layer.
The preparation method of the CrAlO monolayer target in the comparative example specifically comprises the following steps:
s1: cr powder and alpha-Al 2 O 3 Weighing the powder according to the proportion of 80at% and 20at%, adding the powder into a three-dimensional mixer, adding 2% absolute ethyl alcohol, mixing for 6 hours by using the three-dimensional mixer with the rotating speed of 650r/min, and uniformly mixing to obtain alloy powder; wherein the purity of Cr powder is 99.8wt%, the granularity is 300 mesh, and alpha-Al 2 O 3 The purity of the powder is 99.5wt% and the granularity of the powder is 270 meshes;
s2: the alloy powder is filled into a packaging sleeve and then is subjected to degassing treatment, wherein the conditions of the degassing treatment are as follows: 500 ℃ and 8 x 10 vacuum degree -3 Pa, and keeping the temperature for 10h;
s3: placing the degassed ingot blank into a hot isostatic pressing furnace for hot isostatic pressing treatment, wherein the hot isostatic pressing conditions are as follows: the temperature is 1100 ℃, the pressure is 130MPa, and the heat preservation and pressure maintaining time is 5h.
S4: removing the sheath from the single-layer blank subjected to hot isostatic pressing through turning, and obtaining the CrAlO composite target with the required external dimension through linear cutting, turning, milling and other processing modes; the dimensions were D164×15mm.
When PVD coating experiments are carried out on the target material prepared in the comparative example, cracks appear at the step position due to the problem of brittleness of the material; after the finished product is processed, obvious segregation exists on the surface of the finished product.
Comparative example 3
This comparative example provides a CrAlO composite target.
This comparative example differs from example 4 in that: the composition of the CrAlO alloy target material is Cr=45at%, and alpha-Al 2 O 3 ＝55at％。
The preparation method of the CrAlO composite target material in the comparative example is the same as that of example 4.
Performance test
1. Microstructure of microstructure
FIG. 1 is a microstructure of a CrAlO alloy target in a CrAlO composite target prepared in example 4 of the application, and it can be seen that the target has a uniform structure without obvious holes, and the average grain size is about 48 μm.
(2) Relative density: the measured density is measured by an archimedes drainage method according to the measured density value divided by the theoretical density value of the target.
(3) The method for detecting the brittleness (bending strength) of the target comprises the following steps: the mechanical properties are measured by an Instron 3369 universal material tester, and according to the industry standard YB/T5349-2014, test method for bending mechanical properties of metallic materials.
(4) Non-metallic impurity element content: the C content is measured by a high-frequency combustion infrared absorption method, and the H content is measured by an inert gas melting infrared absorption method.
(5) Position reliability of the mounting card in the coating process: and continuously carrying out a coating experiment for 12 hours under the condition that the target bears 10kg of water pressure, and observing whether cracks exist at the step position.
Detection result: as shown in table 3.
TABLE 3 results of Performance test of CrAlO alloy targets in CrAlO composite targets of examples 1-13 and comparative examples 1-3
In combination with Table 3, the results of the tests of comparative examples 1 to 13 and comparative examples 1 to 3 were shown to be Cr=50 to 95at%, α -Al 2 O 3 The CrAlO alloy target material with the composition of 5-50at% is taken as the upper layer of the target material, stainless steel is taken as the bottom layer of the target material, so that the CrAlO alloy target material with the density of more than or equal to 99.2% can be obtained, the impurity element content of the target material is low, the bending strength is high, the target material structure is uniform, and the segregation is avoided; when the target material is subjected to PVD coating experiments, the coating experiments are continuously carried out for 12 hours, no crack exists at the step of the target material, and the performance of the film layer is good (the surface of the film layer is smooth and flat, and no large liquid drop and large particle exist).
According to the detection results of comparative examples 1-6 and comparative example 3, the Cr content in comparative example 3 is 45at%, and the compactness and bending strength of the target material, the appearance of the product and the reliability of the coating film are poor; the higher the Cr content in the CrAlO alloy target material, the higher the compactness and bending strength of the target material, therefore, the alloy uses 50-95at% Cr and 5-50at% alpha-Al 2 O 3 And forming a CrAlO alloy target. Further, in order to reduce the content of impurity C in the target, the CrAlO alloy target comprises the following components in atomic percent: cr=60-90 at%, α -Al 2 O 3 ＝10-40at％。
According to the detection results of comparative examples 4 and 7-9, in example 7, one-stage degassing treatment process is adopted, and the content of impurity elements in the target is high, so that the alloy target is treated by adopting two-stage degassing treatment processes, and the temperature, the vacuum degree and the treatment time of the two-stage processes are matched.
According to the detection results of comparative examples 4 and 10-13, the hot isostatic pressing treatment condition is controlled to be 850-1300 ℃, the pressure is 100-140MPa, the heat preservation and pressure maintaining time is 2-8 hours, the compactness and the bending strength of the alloy target can be further improved, the reliability of steps in film plating is further ensured, and the film plating process is continuous and stable.
While the invention has been described in detail in the foregoing general description and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (10)
1. The CrAlO composite target is characterized in that the CrAlO composite target has a double-layer structure, wherein a CrAlO alloy target is used as a target upper layer, and stainless steel is used as a target bottom layer; the CrAlO alloy target material comprises the following components in percentage by atom: cr=50-95 at%, α -Al 2 O 3 =5-50at%。
2. The CrAlO composite target according to claim 1, wherein the CrAlO alloy target consists of the following components in atomic percent: cr=60-90 at%, α -Al 2 O 3 =10-40at%。
3. The CrAlO composite target according to claim 1, wherein the relative density of the CrAlO alloy target is not less than 99.2%.
4. A method for preparing a CrAlO composite target according to any one of claims 1 to 3, comprising the steps of:
according to the component proportion of the CrAlO composite target, cr powder and alpha-Al are mixed 2 O 3 Weighing the powder according to a proportion, and uniformly mixing to obtain alloy powder;
respectively carrying out compression molding treatment on the alloy powder and the stainless steel powder to obtain an alloy semi-compact pressed compact and a stainless steel semi-compact pressed compact with the relative density of 67-90%;
overlapping the alloy semi-compact pressed compact and the stainless steel semi-compact pressed compact into a sheath, and sequentially carrying out degassing treatment and hot isostatic pressing treatment to obtain a composite blank;
and removing the sheath from the composite blank, and then machining and cleaning to obtain the CrAlO composite target.
5. The preparation method of the CrAlO composite target material according to claim 4, wherein specification parameters of each raw material powder are specifically as follows: the purity is more than 99.8wt percent, the granularity of Cr powder is-300 meshes, the purity is more than 99.5wt percent, and the alpha-Al 2 O 3 The powder particle size was-270 mesh.
6. The preparation method of the CrAlO composite target material according to claim 4, wherein the parameter conditions of the mixing treatment are as follows: adding 0.5-5wt% of absolute ethyl alcohol according to the weight percentage of the mixed powder, and mixing for 4-8h under the condition of 500-800r/min of rotating speed.
7. The method for preparing a CrAlO composite target according to claim 4, wherein the degassing treatment conditions are as follows: at 170-270 deg.C and 3×10 vacuum degree -2 -8×10 -2 Preserving heat for 2-8h under the condition of Pa; then at 400-600deg.C and vacuum degree of 2×10 -2 -2×10 -3 Preserving heat for 6-16h under the condition of Pa.
8. The method for preparing a CrAlO composite target according to claim 4, wherein the conditions of hot isostatic pressing are: the temperature is 850-1300 ℃, the pressure is 100-140MPa, and the heat preservation and pressure maintaining time is 2-8h.
9. The method for preparing a CrAlO composite target according to claim 8, wherein the conditions of the hot isostatic pressing are: the temperature is 950-1200 ℃, the pressure is 110-130MPa, and the heat preservation and pressure maintaining time is 2-8h.
10. Use of a CrAlO composite target as defined in any one of claims 1 to 3 for the preparation of a tool coating.
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| CN202311783774.1A CN117721425A (en) | 2023-12-22 | 2023-12-22 | CrAlO composite target material and preparation method and application thereof |
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| CN202311783774.1A CN117721425A (en) | 2023-12-22 | 2023-12-22 | CrAlO composite target material and preparation method and application thereof |
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| CN202311783774.1A Pending CN117721425A (en) | 2023-12-22 | 2023-12-22 | CrAlO composite target material and preparation method and application thereof |
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| CN116804265A (en) * | 2023-07-21 | 2023-09-26 | 苏州六九新材料科技有限公司 | CrAlCuFe alloy target and preparation method thereof |
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