CN104416156A - Chromium-aluminum alloy target and preparation method thereof - Google Patents
Chromium-aluminum alloy target and preparation method thereof Download PDFInfo
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- CN104416156A CN104416156A CN201310412674.8A CN201310412674A CN104416156A CN 104416156 A CN104416156 A CN 104416156A CN 201310412674 A CN201310412674 A CN 201310412674A CN 104416156 A CN104416156 A CN 104416156A
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Abstract
The invention provides a chromium-aluminum alloy target and a preparation method thereof. The preparation method comprises the steps of preparing alloy powder, carrying out cold isostatic pressing treatment, carrying out degassing treatment, carrying out hot isostatic pressing treatment and machining. The chromium-aluminum alloy target provided by the invention has the advantages of high density, no air pore and segregation, uniform tissue, small crystal grain and the like and is applicable to the coating sputtering of a variety of cutting tools and dies.
Description
Technical field
The invention belongs to technical field of powder metallurgy material preparation, particularly a kind of preparation method of chromium-aluminum alloy target material.
Background technology
Since the sixties in 20th century, through the development of nearly half a century, tool surface coating technology has become the main method promoting cutting performance.Tool surface coating, mainly through improving tool surface hardness, heat endurance, reducing the methods such as coefficient of friction and promoting cutting speed, improving feed speed, thus improving stock-removing efficiency, and significantly promoting cutter life.
Cutter, tool and mould coating experienced by multiple stage such as TiN, TiAlN, gradate as CrN, CrAlN coating, improve the anti-wear performance of instrument, mould.Pure chromium or chromium-aluminum alloy target material are developed at present to prepare this rete.CrAlN film adopts chromium-aluminum alloy target material to be plated in material surface through vacuum sputtering, and this rete can reach the hardness of more than 2000HV, coefficient of friction 0.3, and serviceability temperature, at 700 DEG C, has the outward appearance of silver color, and application is very extensive.Patent of invention 0113153.9 discloses a kind of production technology of Cr-Al alloy, this technique is after adopting chromium powder and aluminium powder to make alloyed powder, employing cold moudling is suppressed, pressure 120-200MPa, dwell time 2.5-3.5 second, the object of this technique manufactures a kind of additive for aluminum alloy materials, together with being finally melted in aluminium again, but what this cold pressing forming process was produced is chromium, the aluminium powder mixture of a kind of pure mechanical compaction not having metallurgical binding, cannot meet the instructions for use of target.In the application for a patent for invention of publication number CN102363215A, all adopt heat pressing process to prepare chromium-aluminum alloy target material for vacuum splashing and plating.But target size limits by equipment, be difficult to realize target and maximize, and the inner relative density of hot pressing target is uneven, middle exist bigger difference with marginal density, is difficult to obtain the uniform target of high mass density.
Summary of the invention
For the defect of prior art, the object of the present invention is to provide a kind of preparation method of chromium-aluminum alloy target material, the target compactness adopting the method to obtain is good, pore-free, nothing are loosened and segregation, uniform composition, crystal grain is tiny, can realize the chromium-aluminum alloy target material maximized.
To achieve these goals, present invention employs following technical scheme:
A preparation method for chromium-aluminum alloy target material, comprises the following steps:
Step one, the preparation of alloy powder;
Step 2, carries out isostatic cool pressing process to the described alloy powder prepared;
Step 3, carries out degassed process to the material base after described isostatic cool pressing process;
Step 4, carries out hip treatment to the material base after described degassed process;
Step 5, carries out machined to the material base after described hip treatment, obtains required final alloy target after cleaning.
In above-mentioned preparation method, the method for this area routine when the preparation of described alloy powder is not particularly illustrated, can be adopted, namely adopt this area conventional method that raw material is made alloy powder.As a kind of preferred embodiment, in described step one, the preparation of described alloy powder can be directly carried out mixing (i.e. mechanical mix techniques) to prepare alloy powder by satisfactory for average grain diameter raw material in batch mixer.When adopting batch mixer to carry out the mixing of raw material, being more preferably and in V-type batch mixer, mixing 3-5h under vacuum or inert gas (such as high-purity argon gas) protective condition.
In above-mentioned preparation method, as a kind of preferred embodiment, in described step one, the average grain diameter of described alloy powder is 30-150 μm, exemplarily, average grain diameter can be 30-50 μm, 60-70 μm, 120-140 μm, 80-100 μm, 35 μm, 43 μm, 50 μm, 90 μm, 100 μm, 120 μm, 145 μm.The purity preparing described alloy powder feed metal chromium used is preferably more than 99.9%, the purity of metallic aluminium is preferably more than 99.7%.
In above-mentioned preparation method, as a kind of preferred embodiment, in described step 2, under 20-200MPa pressure, carry out isostatic cool pressing process, the dwell time is 10-30min.Exemplarily, pressure during described isostatic cool pressing process can be 22MPa, 30MPa, 40MPa, 50MPa, 65MPa, 75MPa, 100MPa, 120MPa, 140MPa, 155MPa, 168MPa, 180MPa, 190MPa, 195MPa; Dwell time can be 10min, 13min, 15min, 18min, 20min, 25min, 28min.
In above-mentioned preparation method, as a kind of preferred embodiment, in described step 3, the temperature of described degassed process is 300-500 DEG C, and degassing time is 5-30h.Exemplarily, described temperature can be 305 DEG C, 320 DEG C, 350 DEG C, 370 DEG C, 400 DEG C, 425 DEG C, 450 DEG C, 480 DEG C, 495 DEG C; Described degassing time can be 5h, 10h, 20h, 25h, 28h.More preferably, vacuum degree control during described degassed process is 10
-1pa ~ 10
-4pa, exemplarily, vacuum can be 10
-1pa, 10
-2pa, 10
-3pa, 10
-4pa.
In above-mentioned preparation method, as a kind of preferred embodiment, in described step 4, the holding temperature of described hip treatment is 500-1100 DEG C, and temperature retention time is 2-5h, and pressure is 120-140MPa.Exemplarily, described holding temperature can be 502 DEG C, 510 DEG C, 524 DEG C, 580 DEG C, 610 DEG C, 642 DEG C, 670 DEG C, 695 DEG C, 731 DEG C, 767 DEG C, 790 DEG C, 805 DEG C, 850 DEG C, 920 DEG C, 960 DEG C, 980 DEG C, 1020 DEG C, 1070 DEG C, 1095 DEG C; Described temperature retention time can be 2h, 3h, 4.5h, 5h; Described pressure can be 122MPa, 125MPa, 130MPa, 134MPa, 138MPa, 140MPa.
In above-mentioned preparation method, prepare the raw material chromium of described final alloy target, the consumption of aluminium can for this area conventional amount used, as a kind of preferred embodiment, described final alloy target consists of the following composition by atomic percent: the aluminium (namely the atomic percent of aluminium is 20-90%) of chromium 10-80% and surplus; More preferably, above-mentioned chromium-aluminum alloy target material consists of the following composition by atomic percent: chromium 30%, aluminium 70%.
The relative density of chromium-aluminum alloy target material prepared by said method is more than 99%, and average grain size is not more than 100 μm.
In above-mentioned preparation method, various preferred embodiment can independent assortment.
Compared to prior art, the present invention has following beneficial effect:
(1) chromium-aluminum alloy target material that prepared by the inventive method has that density is high, pore-free and segregation, and even tissue, the advantages such as crystal grain is tiny, relative density is more than 99%, and average grain size is not more than 100 μm.And the inventive method can realize the in large size of target product, heat and other static pressuring processes greatly increases powder using efficiency simultaneously, the present invention is by the improvement of technique, achieve the lifting of target quality, meanwhile, the preparation of large scale chromium aluminium target will promote the large-scale industrial application of chromium aluminized coating.This target is applicable to multiple cutter, the sputtering of grinding tool coating uses, this target can improve hardness, the anti-wear performance and high-temperature oxidation resistance etc. of alloy coat, use such target institute production coating, its microhardness can reach HV3250, oxidizing temperature can bring up to 1000 DEG C greatly, coefficient of friction can be reduced to 0.3 ~ 0.35, is more suitable for material high speed, Dry-cutting that the adhesiveness such as aluminium, stainless steel is strong.
Accompanying drawing explanation
Fig. 1 is the micro-organization chart of the target that the embodiment of the present invention 1 obtains.
Fig. 2 is the micro-organization chart of the target that the embodiment of the present invention 2 obtains.
Fig. 3 is the micro-organization chart of the target that the embodiment of the present invention 3 obtains.
Detailed description of the invention
Further describe the present invention below by way of specific embodiment, but the present invention is not limited thereto.
Embodiment 1
The chromium-aluminum alloy target material that the present embodiment provides is grouped into by the one-tenth of following atomic percent: chromium 10%, aluminium 90%.
Its preparation method, comprises the following steps:
Step one; take according to the designing requirement of above-mentioned target material composition average grain diameter is 30 μm, purity is 99.9% crome metal 17.6 parts, purity is 99.7% metallic aluminium 82.4 parts; it is mixed 3h in V-type batch mixer, and vacuumize in mixed process and protect, vacuum degree control is 10
-2about Pa.
Step 2, loaded in cold isostatic compaction mould by gained alloy powder, under the pressure of 20MPa, carry out isostatic cool pressing process, the dwell time is 10min.
Step 3, loaded by the material base after isostatic cool pressing process in the suitable stainless steel jacket of size, be placed on by jacket in degassing equipment and carry out degassed process, heating-up temperature is 300 DEG C, and temperature retention time is 20h, and during insulation, vacuum degree control is 10
-2about Pa, described degassing equipment can be commercially available diffusion pump and well formula resistance furnace.
Step 4, sinter putting into hot isostatic apparatus after degassed complete jacket soldering and sealing, holding temperature is 500 DEG C, and temperature retention time is 2h, and pressure is 120MPa.
Step 5, carries out machined to the ingot blank after described hip treatment, obtains required final alloy target after cleaning, and its maximum length is 1040mm.
The target relative density that this example obtains reaches 99.8%, average grain size about 25 μm.As can be known from Fig. 1, the target pore-free that this embodiment obtains and segregation, even tissue.
The target that the present embodiment obtains is plated in through vacuum sputtering the coating that YG6 carbide tool surface obtains, and microhardness is HV2500, and oxidizing temperature is 800 DEG C, and coefficient of friction is 0.3.
Embodiment 2
The chromium-aluminum alloy target material that the present embodiment provides is grouped into by the one-tenth of following atomic percent, chromium 50%, aluminium 50%.
Its preparation method, comprises the following steps:
Step one, take according to the designing requirement of above-mentioned target material composition average grain diameter is 145 μm, purity is 99.9% chromium powder 65.8 parts, purity be 99.7% aluminium powder 34.2 parts, it is mixed 5h in V-type batch mixer, in mixed process, is filled with high-purity argon gas protection;
Step 2, loaded in cold isostatic compaction mould by the powder mixed and carry out isostatic cool pressing process, isostatic cool pressing pressure is 100MPa, and the dwell time is 15min;
Step 3, loaded by isostatic cool pressing material base in the suitable metal capsule of size, be placed on by jacket in degassing equipment and carry out degassed process, heating-up temperature is 400 DEG C, and temperature retention time is 5h, and during insulation, vacuum degree control is 10
-3about Pa; Described degassing equipment can be commercially available diffusion pump and well formula resistance furnace.
Step 4, sinter putting into hot isostatic apparatus after degassed complete jacket soldering and sealing, holding temperature is 800 DEG C, temperature retention time 3h, pressure 130MPa;
Step 5, carries out machined to the ingot blank after described hip treatment, and obtain required final alloy target after cleaning, its largest diameter is of a size of D355mm.
The target relative density that this example obtains reaches 99.4%, average grain size about 90 μm.As can be known from Fig. 2, the target pore-free that this embodiment obtains and segregation, even tissue.
The target that the present embodiment obtains is plated in through vacuum sputtering the coating that YG6 carbide tool surface obtains, and microhardness is HV3100, oxidizing temperature 950 DEG C, and coefficient of friction is 0.33.
Embodiment 3
The chromium-aluminum alloy target material that the present embodiment provides is grouped into by the one-tenth of following atomic percent, chromium 80%, aluminium 20%.
Its preparation method, comprises the following steps:
Step one; take according to the designing requirement of above-mentioned target material composition average grain diameter is 50 μm, purity is 99.9% chromium powder 88.5 parts, purity be 99.7% aluminium powder 11.5 parts; it is mixed 3h in V-type batch mixer, and vacuumize in mixed process and protect, vacuum degree control is 10
-2about Pa;
Step 2, loaded in cold isostatic compaction mould by the powder mixed and carry out isostatic cool pressing process, isostatic cool pressing pressure is 200MPa, and the dwell time is 20min;
Step 3, loaded by isostatic cool pressing material base in the suitable stainless steel jacket of size, be placed on by jacket in degassing equipment and carry out degassed process, heating-up temperature is 500 DEG C, and temperature retention time is 30h; During insulation, vacuum degree control is 10
-4about Pa; Described degassing equipment can be commercially available diffusion pump and well formula resistance furnace.
Step 4, sinter putting into hot isostatic apparatus after degassed complete jacket soldering and sealing, holding temperature is 1100 DEG C, and temperature retention time is 5h, and pressure is 140MPa;
Step 5, carries out machined to the ingot blank after described hip treatment, obtains required final alloy target after cleaning.
The target relative density that this example obtains reaches 99.0%, average grain size 40 μm.As can be known from Fig. 3, the target pore-free that this embodiment obtains and segregation, even tissue.
The target that the present embodiment obtains is plated in through vacuum sputtering the coating that YG6 carbide tool surface obtains, and microhardness is HV3200, and oxidizing temperature is 900 DEG C, and coefficient of friction is 0.34.
Embodiment 4
The chromium-aluminum alloy target material that the present embodiment provides is grouped into by the one-tenth of following atomic percent, chromium 40%, aluminium 60%.
Its preparation method, comprises the following steps:
Step one; take according to the designing requirement of above-mentioned target material composition average grain diameter is 80 μm, purity is 99.9% chromium powder 56.2 parts, purity be 99.7% aluminium powder 43.8 parts; it is mixed 3.5h in V-type batch mixer, and vacuumize in mixed process and protect, vacuum degree control is 10
-3about Pa;
Step 2, loaded in cold isostatic compaction mould by the powder mixed and carry out isostatic cool pressing process, isostatic cool pressing pressure is 60MPa, and the dwell time is 18min;
Step 3, loaded by isostatic cool pressing material base in the suitable stainless steel jacket of size, be placed on by jacket in degassing equipment and carry out degassed process, heating-up temperature is 350 DEG C, and temperature retention time is 25h; During insulation, vacuum degree control is 10
-4about Pa; Described degassing equipment can be commercially available diffusion pump and well formula resistance furnace.
Step 4, sinter putting into hot isostatic apparatus after degassed complete jacket soldering and sealing, holding temperature is 650 DEG C, and temperature retention time is 4h, and pressure is 125MPa;
Step 5, carries out machined to the ingot blank after described hip treatment, obtains required final alloy target after cleaning.
The target relative density that this example obtains reaches 99.5%, average grain size 60 μm.The target that the present embodiment obtains is plated in through vacuum sputtering the coating that YG6 carbide tool surface obtains, and microhardness is HV3150, and oxidizing temperature is 950 DEG C, and coefficient of friction is 0.32.
Embodiment 5
The chromium-aluminum alloy target material that the present embodiment provides is grouped into by the one-tenth of following atomic percent, chromium 25%, aluminium 75%.
Its preparation method, comprises the following steps:
Step one; take according to the designing requirement of above-mentioned target material composition average grain diameter is 120 μm, purity is 99.9% chromium powder 39.1 parts, purity be 99.7% aluminium powder 60.9 parts; it is mixed 4.5h in V-type batch mixer, and vacuumize in mixed process and protect, vacuum degree control is 10
-3about Pa;
Step 2, loaded in cold isostatic compaction mould by the powder mixed and carry out isostatic cool pressing process, isostatic cool pressing pressure is 160MPa, and the dwell time is 25min;
Step 3, loaded by isostatic cool pressing material base in the suitable stainless steel jacket of size, be placed on by jacket in degassing equipment and carry out degassed process, heating-up temperature is 420 DEG C, and temperature retention time is 15h; During insulation, vacuum degree control is 10
-4about Pa; Described degassing equipment can be commercially available diffusion pump and well formula resistance furnace.
Step 4, sinter putting into hot isostatic apparatus after degassed complete jacket soldering and sealing, holding temperature is 1000 DEG C, and temperature retention time is 3.5h, and pressure is 132MPa;
Step 5, carries out machined to the ingot blank after described hip treatment, obtains required final alloy target after cleaning.
The target relative density that this example obtains reaches 99.7%, average grain size 85 μm.The target that the present embodiment obtains is plated in through vacuum sputtering the coating that YG6 carbide tool surface obtains, and microhardness is HV2500, and oxidizing temperature is 850 DEG C, and coefficient of friction is 0.31.
In above embodiment, the assay method of each parameter is as follows: relative density adopts Archimedes's drainage to measure; By optical metallographic microscope, target crystalline grains size is analyzed; With micro-nano hardometer, cutter coating hardness is detected; Adopt natural thermocouple method to measure Tool in Cutting temperature, and determine coating oxidation temperature, adopt STF-A friction coefficient instrument to measure cutter coat coefficient of friction.
Should be appreciated that the purposes of these embodiments is only not intended to for illustration of the present invention limit the scope of the invention.In addition; also should understand; after having read technology contents of the present invention, those skilled in the art can make various change, amendment and/or modification to the present invention, and these all equivalent form of values fall within the protection domain that the application's appended claims limits equally.
Claims (10)
1. a preparation method for chromium-aluminum alloy target material, is characterized in that, comprises the following steps:
Step one, the preparation of alloy powder;
Step 2, carries out isostatic cool pressing process to the described alloy powder prepared;
Step 3, carries out degassed process to the material base after described isostatic cool pressing process;
Step 4, carries out hip treatment to the material base after described degassed process;
Step 5, carries out machined to the material base after described hip treatment, thus obtains required final alloy target.
2. preparation method according to claim 1, is characterized in that, in described step one, satisfactory for average grain diameter raw material directly carries out mixing preparing by described alloy powder in batch mixer.
3. preparation method according to claim 2, is characterized in that, describedly in batch mixer, directly satisfactory for average grain diameter raw material is carried out mixing refer in V-type batch mixer, mix 3-5h under vacuum or inert gas shielding condition.
4. preparation method according to claim 1, is characterized in that, the average grain diameter of described alloy powder is 30-150 μm.
5. preparation method according to claim 1, is characterized in that, in described step 2, under 20-200MPa pressure, carries out isostatic cool pressing process, and the dwell time is 10-30min.
6. preparation method according to claim 1, is characterized in that, in described step 3, the temperature of described degassed process is 300-500 DEG C, and degassing time is 5-30h; Preferably, vacuum degree control during described degassed process is 10
-1pa ~ 10
-4pa.
7. preparation method according to claim 1, is characterized in that, in described step 4, the holding temperature of described hip treatment is 500-1100 DEG C, and temperature retention time is 2-5h, and pressure is 120-140MPa.
8. preparation method according to claim 1, is characterized in that, described chromium-aluminum alloy target material consists of the following composition by atomic percent: the aluminium of chromium 10-80% and surplus.
9. preparation method according to claim 8, is characterized in that, described chromium-aluminum alloy target material consists of the following composition by atomic percent: chromium 30%, aluminium 70%.
10. chromium alusil alloy target according to claim 1, is characterized in that, the relative density of described alloy target material is more than 99%, and average grain size is not more than 100 μm.
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Cited By (5)
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| CN106312071A (en) * | 2015-06-19 | 2017-01-11 | 宁波江丰电子材料股份有限公司 | A tungsten-titanium tube target manufacture method |
| CN110527957A (en) * | 2019-08-19 | 2019-12-03 | 河北宏靶科技有限公司 | A kind of aluminium chromium-boron alloy target and preparation method thereof |
| CN111636056A (en) * | 2019-03-01 | 2020-09-08 | 宁波江丰电子材料股份有限公司 | Preparation method of target material |
| CN111778487A (en) * | 2020-07-01 | 2020-10-16 | 宁波江丰电子材料股份有限公司 | Chromium-aluminum alloy sputtering target material and preparation method thereof |
| CN114101677A (en) * | 2022-01-26 | 2022-03-01 | 西安赛隆金属材料有限责任公司 | High-chromium aluminum alloy target and preparation method thereof |
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| CN104416156B (en) | 2016-08-17 |
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