CN116926484A - Processing technology of zirconium yttrium chromium alloy sputtering target material - Google Patents
Processing technology of zirconium yttrium chromium alloy sputtering target material Download PDFInfo
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- 238000005477 sputtering target Methods 0.000 title claims abstract description 70
- 229910000599 Cr alloy Inorganic materials 0.000 title claims abstract description 63
- XKIPKUMKVHOMGV-UHFFFAOYSA-N [Y].[Cr].[Zr] Chemical compound [Y].[Cr].[Zr] XKIPKUMKVHOMGV-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000000788 chromium alloy Substances 0.000 title claims abstract description 63
- 239000013077 target material Substances 0.000 title claims abstract description 46
- 238000012545 processing Methods 0.000 title claims abstract description 45
- 238000005516 engineering process Methods 0.000 title claims abstract description 22
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 52
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000001816 cooling Methods 0.000 claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 24
- 239000002184 metal Substances 0.000 claims abstract description 24
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 22
- 239000000956 alloy Substances 0.000 claims abstract description 22
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 17
- 239000011651 chromium Substances 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910002804 graphite Inorganic materials 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 230000003064 anti-oxidating effect Effects 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 5
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical group O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 9
- 238000005204 segregation Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 9
- 238000009413 insulation Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 229910000946 Y alloy Inorganic materials 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- GNKHOVDJZALMGA-UHFFFAOYSA-N [Y].[Zr] Chemical compound [Y].[Zr] GNKHOVDJZALMGA-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910001093 Zr alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 1
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
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C16/00—Alloys based on zirconium
-
- 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
- C22F1/186—High-melting or refractory metals or alloys based thereon of zirconium or alloys based thereon
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The application relates to the technical field of sputtering target material processing, and particularly discloses a processing technology of a zirconium yttrium chromium alloy sputtering target material. The processing technology comprises the following steps: mixing 72.5-79 parts by weight of zirconium blocks, 16-22 parts by weight of yttrium blocks and 2.5-7.5 parts by weight of chromium blocks to obtain a mixture; under the protection of inert gas and electromagnetic stirring, heating and melting the mixture to obtain a metal mixed solution; pouring the metal mixed solution in an ingot mould, removing the ingot mould, and cooling to room temperature to obtain an alloy ingot; and carrying out heat treatment on the alloy ingot to obtain the zirconium yttrium chromium alloy sputtering target material. The zirconium yttrium chromium alloy sputtering target material obtained by the processing technology has the advantages of average grain size less than 50 mu m and yttrium processing loss rate less than 5%, ensures the yttrium content in the zirconium yttrium chromium alloy sputtering target material, reduces yttrium resource waste, has the advantages of high compactness, no air hole, no segregation, no crack, uniform structure and easy processing, and meets the market demand.
Description
Technical Field
The application relates to the technical field of sputtering target material processing, in particular to a processing technology of a zirconium yttrium chromium alloy sputtering target material.
Background
The engine is used as a power machine and is widely applied to the fields of aviation, power generation, transportation and the like. Turbine blades of an engine often handle high temperature environments during operation, where the turbine blades are subjected not only to significant mechanical loads, but also to high temperature oxidation and hot corrosion. In order to increase the service life of the turbine blade and ensure the normal operation of the engine, a thermal insulation coating is often coated on the surface of the turbine blade. The yttria-stabilized zirconia thermal insulation coating has the characteristics of good stability, low heat conductivity coefficient, good oxidation resistance and excellent wear resistance at high temperature, and has been applied to turbine blades. The heat-insulating coating is generally processed by adopting a zirconium yttrium alloy sputtering target material, and the heat-insulating coating is sprayed on the surface of the turbine blade in a sputtering mode, so that the quality of the zirconium yttrium alloy sputtering target material is the basis for ensuring the heat-insulating coating.
Zirconium and yttrium alloy sputtering target materials are generally obtained by mixing zirconium blocks and yttrium blocks, melting and casting. However, the applicant finds that in practical processing, the melting temperature of the zirconium block and the yttrium block is high, and at high temperature, metal yttrium is easy to volatilize, so that yttrium resource is wasted, and the content of yttrium in the zirconium yttrium alloy sputtering target material is influenced.
Disclosure of Invention
In order to reduce volatilization of yttrium in the zirconium yttrium alloy sputtering target processing process, the application provides a processing technology of a zirconium yttrium chromium alloy sputtering target, which adopts the following technical scheme:
a processing technology of a zirconium yttrium chromium alloy sputtering target material comprises the following steps:
s1, mixing 72.5-79 parts by weight of zirconium blocks, 16-22 parts by weight of yttrium blocks and 2.5-7.5 parts by weight of chromium blocks to obtain a mixture;
s2, under the protection of inert gas and electromagnetic stirring, heating and melting the mixture to obtain a metal mixed solution;
s3, pouring the metal mixed solution in an ingot mould, removing the ingot mould, and cooling to room temperature to obtain an alloy ingot;
and S4, performing heat treatment on the alloy ingot to obtain the zirconium yttrium chromium alloy sputtering target material.
By adopting the technical scheme, the obtained zirconium yttrium chromium alloy sputtering target material has the average grain size smaller than 50 mu m, and has the advantages of high density, no air hole, no segregation, no crack, uniform structure and easy processing, and meets the market demand.
In the zirconium yttrium chromium alloy sputtering target material processing, chromium blocks are added into zirconium blocks and yttrium blocks to obtain a mixture, and further a metal mixed solution is obtained. Chromium in the metal mixed solution can play a role in stabilizing yttrium, reduce the oxidation and volatilization of yttrium, and reduce the volatilization of yttrium by being matched with the inert gas protection in the step S2. According to the processing technology, through mutual matching of the steps, the yttrium processing loss rate is reduced and is less than 5%, so that the yttrium content in the zirconium yttrium chromium alloy sputtering target material is ensured, the yttrium resource waste is reduced, and the processing stability of the zirconium yttrium chromium alloy sputtering target material is improved.
Meanwhile, the application also limits the addition amount of the chromium blocks, thereby realizing the limit of the chromium element content in the zirconium yttrium chromium alloy sputtering target material, reducing the influence of the chromium element content on the stabilization of yttrium, and reducing the influence of the chromium element content on the performance of the thermal insulation coating. And when the addition amount of the chromium blocks is 2.5-7.5 parts by weight, the yttrium can play a good role in stabilizing yttrium, the performance of the thermal insulation coating cannot be influenced, and the market demand is met.
Optionally, in step S2, the temperature is raised to 1750-1900 ℃ and the temperature is raised to melt for 45-60min.
By adopting the technical scheme, the temperature rise and melting temperature and the temperature rise and melting time are optimized, so that the zirconium block, the yttrium block and the chromium block can form a metal mixed solution conveniently.
Optionally, the inert gas is argon, and the pressure of the argon is 0.03-0.09MPa.
By adopting the technical scheme, the pressure of argon is optimized, volatilization of yttrium in the metal mixed solution is reduced, yttrium content in the zirconium yttrium chromium alloy sputtering target material is ensured, and processing stability of the zirconium yttrium chromium alloy sputtering target material is improved.
In various embodiments, the pressure of the argon gas is 0.06MPa, which may also be set to 0.03MPa, 0.04MPa, 0.05MPa, 0.07MPa, 0.08MPa, 0.09MPa, etc., as desired.
Optionally, in step S2, the frequency of the electromagnetic stirring is 8-12Hz.
By adopting the technical scheme, the zirconium block, the yttrium block and the chromium block can increase the uniformity of raw material mixing and improve the uniformity of yttrium in the zirconium yttrium chromium alloy sputtering target material through electromagnetic stirring.
In various embodiments, the frequency of the electromagnetic stirring is 10Hz, which may also be set to 8Hz, 9Hz, 11Hz, 12Hz, etc., as desired.
Optionally, the temperature of the ingot mould is 890-910 ℃.
By adopting the technical scheme, the ingot mould is preheated to 890-910 ℃, so that the moisture and volatile matters in the ingot mould can be effectively removed, and the influence of sundries is reduced. And when the metal mixed solution is poured and cooled, the temperature of the ingot mould is firstly reduced and then reduced to the room temperature, so that the cooling gradient of the metal mixed solution is effectively reduced, the metal mixed solution can be fed better, the utilization rate is increased, the situation that an alloy ingot is cracked due to the fact that the metal mixed solution is rapidly cooled to the room temperature is reduced, and the performance of the zirconium-yttrium-chromium alloy sputtering target is also improved.
In various embodiments, the temperature of the ingot mold is 900 ℃, which may also be set to 890 ℃, 895 ℃, 905 ℃, 910 ℃, etc., as desired.
In step S3, the metal mixed solution is poured into an ingot mould, and then is subjected to heat preservation treatment for 10-30min, and then the ingot mould is removed. In various embodiments, the incubation time is 20 minutes, which may also be set to 10 minutes, 15 minutes, 25 minutes, 30 minutes, etc., as desired.
Optionally, the ingot mould is a graphite crucible, and an antioxidation layer is arranged on the surface of the graphite crucible.
Optionally, the antioxidation layer is a yttrium oxide layer.
When the metal mixture is poured in the graphite crucible, if the metal mixture is in direct contact with the graphite crucible, a reaction may occur, thereby corroding the graphite crucible and forming metal carbide. Therefore, an oxidation-resistant layer is provided on the surface of the graphite crucible. The oxidation resistant layer is arranged as an yttrium oxide layer, so that the corrosion of the metal mixed liquid to the graphite crucible can be reduced, the temperature of the metal mixed liquid can be adapted, and the casting of the metal mixed liquid is facilitated.
Optionally, in step S4, the heat treatment of the alloy ingot specifically includes: and heating the alloy ingot to 840-850 ℃, carrying out heat preservation treatment for 2-4h, quickly cooling to 290-310 ℃, and then cooling to room temperature, thereby obtaining the zirconium yttrium chromium alloy sputtering target.
By adopting the technical scheme, the alloy ingot is heated to 840-850 ℃ so that the crystal grains of the alloy ingot are enlarged, and the uniformity of yttrium in the alloy ingot can be effectively improved. And the grains become larger, the performance of the zirconium yttrium chromium alloy sputtering target is reduced, and the preparation of the thermal insulation coating is not facilitated. Therefore, the alloy ingot is further cooled rapidly from 840-850 ℃ to 290-310 ℃ by rapid cooling, the quenching effect is achieved, the grains are effectively refined, the grains are reduced, the performance of the zirconium yttrium chromium alloy sputtering target is improved, and the preparation of the thermal insulation coating is facilitated.
Optionally, in step S4, the cooling rate of the cooling is 550-560 ℃/min.
When the cooling rate is too slow, the effect of refining the crystal grains of the alloy ingot is affected, and even the effect of refining the crystal grains cannot be achieved; when the cooling rate is too fast, the alloy ingot may have larger internal stress, causing cracking of the alloy ingot. And when the cooling rate is 550-560 ℃/min, the zirconium yttrium chromium alloy sputtering target material can be cooled rapidly, grains can be effectively refined, the average grain size is less than 15 mu m, and the performance of the zirconium yttrium chromium alloy sputtering target material is improved.
In various embodiments, the cooling rate is 555 ℃/min, which may also be set to 550 ℃/min, 560 ℃/min, etc., as desired.
Optionally, in step S4, the temperature rising rate of the temperature rising is 8-12 ℃/min.
By adopting the technical scheme, the heating rate is optimized, the equipment investment cost is reduced because the heating rate is too fast, and the processing efficiency is also reduced because the heating rate is too slow.
In various embodiments, the heating rate is 10deg.C/min, which may also be set to 8deg.C/min, 9deg.C/min, 11deg.C/min, 12deg.C/min, etc., as desired.
In summary, the application has the following beneficial effects:
the zirconium yttrium chromium alloy sputtering target material obtained by the processing technology has the average grain size of less than 50 mu m, has the advantages of high compactness, no air holes, no segregation, no cracks, uniform structure and easy processing, ensures the yttrium content in the zirconium yttrium chromium alloy sputtering target material, reduces the yttrium resource waste, and improves the processing stability of the zirconium yttrium chromium alloy sputtering target material in the processing process, wherein the yttrium processing loss rate is less than 5%.
Detailed Description
In order that the application may be more readily understood, the application will be further described in detail with reference to the following examples, which are given by way of illustration only and are not limiting in scope of application. The starting materials or components used in the present application may be prepared by commercial or conventional methods unless specifically indicated.
Examples
Table 1 content of each raw material of the mixture (unit: 10 g)
| Examples | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Zirconium block | 75 | 79 | 77 | 73 | 77.5 | 72.5 |
| Yttrium block | 20 | 16 | 18 | 22 | 20 | 20 |
| Chromium block | 5 | 5 | 5 | 5 | 2.5 | 7.5 |
| Totals to | 100 | 100 | 100 | 100 | 100 | 100 |
Example 1
A processing technology of a zirconium yttrium chromium alloy sputtering target material comprises the following steps:
s1, adding yttrium blocks and chromium blocks into zirconium blocks, and stirring for 10min to obtain a mixture.
The proportions of the raw materials of the zirconium block, the yttrium block and the chromium block are shown in table 1.
S2, adding the mixture into a vacuum induction melting furnace, starting electromagnetic stirring, wherein the frequency of the electromagnetic stirring is 10Hz, vacuumizing and introducing argon to ensure that the pressure of the argon is 0.06MPa, and then heating to 1800 ℃ for melting treatment for 45min to obtain a metal mixed solution.
And S3, pouring the metal mixed solution in an ingot mould with the temperature of 900 ℃, carrying out heat preservation treatment for 20min, removing the ingot mould, and cooling to 25 ℃ to obtain an alloy ingot which is a cylinder with the diameter of 165mm.
The ingot mould is a graphite crucible, an antioxidation layer is arranged on the surface of the graphite crucible, and the antioxidation layer is an yttrium oxide layer.
S4, heating the alloy ingot to 845 ℃ at a heating rate of 10 ℃/min, and carrying out heat preservation treatment for 3 hours. Then rapidly cooling to 300 ℃ at a cooling rate of 555 ℃/min. And then cooling to 25 ℃ to obtain the zirconium yttrium chromium alloy sputtering target.
Examples 2 to 6
The difference between the processing technology of the zirconium yttrium chromium alloy sputtering target material and the embodiment 1 is that in the step S1, the raw material proportions of the zirconium block, the yttrium block and the chromium block are different, and the raw material proportions of the zirconium block, the yttrium block and the chromium block are shown in the table 1.
Example 7
The processing technology of the zirconium yttrium chromium alloy sputtering target material is different from that of the embodiment 1 in that in the step S2, the temperature rise and melting temperature are 1750 ℃.
Example 8
The processing technology of the zirconium yttrium chromium alloy sputtering target material is different from that of the embodiment 1 in that in the step S2, the temperature rise and melting temperature is 1900 ℃.
Example 9
The processing technology of the zirconium yttrium chromium alloy sputtering target material is different from that of the embodiment 1 in that in the step S2, the temperature rising and melting time is 60min.
Example 10
The processing technology of the zirconium yttrium chromium alloy sputtering target material is different from that of the embodiment 1 in that in the step S3, the temperature of the ingot mould is 800 ℃.
Example 11
The processing technology of the zirconium yttrium chromium alloy sputtering target material is different from that of the embodiment 1 in that in the step S4, the temperature of heating is 800 ℃.
Example 12
The processing technology of the zirconium yttrium chromium alloy sputtering target material is different from that of the embodiment 1 in that in the step S4, the cooling rate of cooling is 400 ℃/min.
Example 13
The processing technology of the zirconium yttrium chromium alloy sputtering target material is different from that of the embodiment 1 in that in the step S4, the cooling rate of cooling is 300 ℃/min.
Comparative example
Comparative example 1
The processing technology of the zirconium yttrium chromium alloy sputtering target material is different from that of the embodiment 1 in that in the step S1, the raw material proportions of the zirconium block, the yttrium block and the chromium block are different, and the weight proportions of the zirconium block, the yttrium block and the chromium block are 80:20:0, namely, the chromium block is not added.
Performance detection
(1) Zirconium yttrium chromium alloy sputtering targets obtained in examples 1 to 9 and comparative example 1 were taken as test samples, and yttrium content in the test samples was detected, and the detection results are shown in table 2.
Wherein the yttrium addition amount is the yttrium addition amount in the mixture; the yttrium content is the yttrium content in the zirconium yttrium chromium alloy sputtering target material; the yttrium processing loss rate is the loss rate in the process of processing yttrium blocks into zirconium yttrium chromium alloy sputtering targets, and the yttrium processing loss rate=yttrium addition amount-yttrium content.
(1) The zirconium yttrium chromium alloy sputtering targets obtained in examples 1 to 13 and comparative example 1 were each taken as a sample, and the average grain size of the samples was examined, and the examination results are shown in table 2.
TABLE 2 detection results
Note that: "/" indicates undetected.
As can be seen from Table 2, the zirconium yttrium chromium alloy sputtering target material obtained by the processing technology has lower yttrium processing loss rate in the processing process, and the yttrium processing loss rate is 4.28-4.56%, so that the yttrium content in the zirconium yttrium chromium alloy sputtering target material is ensured, the yttrium resource waste is reduced, and the processing stability of the zirconium yttrium chromium alloy sputtering target material is improved. Meanwhile, the zirconium yttrium chromium alloy sputtering target material also has good average grain size which is 13.24-47.49 mu m, especially in examples 1-9, and the average grain size is 13.24-13.52 mu m, so that the zirconium yttrium chromium alloy sputtering target material has the advantages of high compactness, no air holes, no segregation and uniform structure, and meets the market demand.
Comparing example 1 with example 10, it can be seen that the temperature of the ingot mold in step S3 has a certain effect on the average grain size of the zirconium yttrium chromium alloy sputtering target, and the average grain size is smaller when the temperature of the ingot mold is 890-910 ℃. By combining with example 11, it can be seen that the temperature of the alloy ingot in step S4 also has a certain effect on the average grain size of the zirconium yttrium chromium alloy sputtering target, and the temperature of the alloy ingot is 840-850 ℃, so that the zirconium yttrium chromium alloy sputtering target exhibits better performance.
Comparing example 1 with examples 12-13, it can be seen that the average grain size of the zirconium yttrium chromium alloy sputtering target increases with decreasing cooling rate, and the average grain size is less than 15 μm at a cooling rate of 550-560 ℃/min, which shows better performance.
It should be noted that the above-described embodiments are only for explaining the present application and do not constitute any limitation of the present application. The application has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. Modifications may be made to the application as defined in the appended claims, and the application may be modified without departing from the scope and spirit of the application. Although the application is described herein with reference to particular means, materials and embodiments, the application is not intended to be limited to the particulars disclosed herein, as the application extends to all other means and applications which perform the same function.
Claims (10)
1. A processing technology of a zirconium yttrium chromium alloy sputtering target material is characterized in that: the method comprises the following steps:
s1, mixing 72.5-79 parts by weight of zirconium blocks, 16-22 parts by weight of yttrium blocks and 2.5-7.5 parts by weight of chromium blocks to obtain a mixture;
s2, under the protection of inert gas and electromagnetic stirring, heating and melting the mixture to obtain a metal mixed solution;
s3, pouring the metal mixed solution in an ingot mould, removing the ingot mould, and cooling to room temperature to obtain an alloy ingot;
and S4, performing heat treatment on the alloy ingot to obtain the zirconium yttrium chromium alloy sputtering target material.
2. The process for manufacturing a zirconium yttrium chromium alloy sputtering target according to claim 1, wherein the process comprises the following steps: in the step S2, the temperature is raised to be between 1750 and 1900 ℃ and the temperature is raised to be between 45 and 60 minutes.
3. The process for manufacturing a zirconium yttrium chromium alloy sputtering target according to claim 1, wherein the process comprises the following steps: the inert gas is argon, and the pressure of the argon is 0.03-0.09MPa.
4. The process for manufacturing a zirconium yttrium chromium alloy sputtering target according to claim 1, wherein the process comprises the following steps: in step S2, the frequency of electromagnetic stirring is 8-12Hz.
5. The process for manufacturing a zirconium yttrium chromium alloy sputtering target according to claim 1, wherein the process comprises the following steps: the temperature of the ingot mould is 890-910 ℃.
6. The process for manufacturing a zirconium yttrium chromium alloy sputtering target according to claim 1, wherein the process comprises the following steps: the ingot mould is a graphite crucible, and an antioxidation layer is arranged on the surface of the graphite crucible.
7. The process for manufacturing a zirconium yttrium chromium alloy sputtering target according to claim 6, wherein the process comprises the following steps: the antioxidation layer is a yttrium oxide layer.
8. The process for manufacturing a zirconium yttrium chromium alloy sputtering target according to claim 1, wherein the process comprises the following steps: in step S4, the heat treatment of the alloy ingot specifically includes: and heating the alloy ingot to 840-850 ℃, carrying out heat preservation treatment for 2-4h, quickly cooling to 290-310 ℃, and then cooling to room temperature, thereby obtaining the zirconium yttrium chromium alloy sputtering target.
9. The process for manufacturing a zirconium yttrium chromium alloy sputtering target according to claim 8, wherein the process comprises the following steps: in the step S4, the cooling rate of cooling is 550-560 ℃/min.
10. The process for manufacturing a zirconium yttrium chromium alloy sputtering target according to claim 8, wherein the process comprises the following steps: in the step S4, the temperature rising rate of the temperature rising is 8-12 ℃/min.
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