CN116855902B - Low-aluminum-content titanium-based target material and preparation method thereof - Google Patents
Low-aluminum-content titanium-based target material and preparation method thereof Download PDFInfo
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- CN116855902B CN116855902B CN202310904370.7A CN202310904370A CN116855902B CN 116855902 B CN116855902 B CN 116855902B CN 202310904370 A CN202310904370 A CN 202310904370A CN 116855902 B CN116855902 B CN 116855902B
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- 239000010936 titanium Substances 0.000 title claims abstract description 42
- 239000013077 target material Substances 0.000 title claims abstract description 31
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 86
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 68
- 238000011282 treatment Methods 0.000 claims abstract description 64
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 239000011812 mixed powder Substances 0.000 claims abstract description 23
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000011049 filling Methods 0.000 claims abstract description 6
- 238000004321 preservation Methods 0.000 claims description 24
- 238000007872 degassing Methods 0.000 claims description 18
- 238000009849 vacuum degassing Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 239000010935 stainless steel Substances 0.000 claims description 11
- 229910001220 stainless steel Inorganic materials 0.000 claims description 11
- 238000011068 loading method Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 7
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 description 15
- 239000011248 coating agent Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 11
- 229910010037 TiAlN Inorganic materials 0.000 description 8
- 239000011863 silicon-based powder Substances 0.000 description 8
- 229910010038 TiAl Inorganic materials 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- 238000000280 densification Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000005240 physical vapour deposition Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 238000005275 alloying Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000007596 consolidation process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- 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
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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)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The application relates to a low aluminum content titanium-based target material and a preparation method thereof in the field of target material manufacture, comprising the following steps of mechanically mixing Al powder, ti powder and Me powder according to a proportion to form mixed powder, wherein the content of the Al powder in the mixed powder is 1-30 at%, the content of the Ti powder is 70-99% and the content of the Me powder is 0-20at%; filling the mixed powder into a sheath, and performing two times of hot isostatic pressing, wherein the heat treatment temperature of the first hot isostatic pressing treatment is T1, and the heat treatment temperature of the second hot isostatic pressing treatment is T2, and the conditions are satisfied: t2-t1=250 to 800 ℃. The application has the effects of improving the density of the aluminum-titanium-based target material and reducing the preparation cost of the target material.
Description
Technical Field
The application relates to the field of target manufacturing, in particular to a low-aluminum-content titanium-based target and a preparation method thereof.
Background
With the improvement of industrial materials and machine tool performance, the cutting requirements of cutters arranged on machine tools or equipment are also improved, and coated cutters are developed for the cutting requirements. The coated cutter is characterized in that a layer of metal compound with excellent performance is coated on the surface of the cutter by a chemical or physical method, so that the cutter has the novel characteristics of high hardness, friction and abrasion resistance, small heat transfer coefficient and the like, the reliability of the cutter in high-speed, high-temperature, high-pressure, heavy-load and corrosive medium environments is improved, and the service life of the cutter is prolonged.
At present, the common coating of the coated tool is TiAlN coating, the TiAlN coating can enable the nano hardness of the tool to be up to 37GPa, the oxidation temperature is increased to 800 ℃, and the friction coefficient with steel is also reduced. TiAlN coating can also be used for mobile phones, watches, glasses, some ornaments and the like, so that the TiAlN coating keeps longer-lasting brightness and is deeply favored by customers.
The main ways to obtain TiAlN coating are Physical Vapor Deposition (PVD) and Chemical Vapor Deposition (CVD). In the process of preparing the TiAlN coating by the PVD coating technology, a target material is used as a direct raw material, and the quality of the TiAlN coating directly influences the performance of a final coating.
The density performance of the target material not only affects the sputtering rate in the sputtering coating process, but also affects the electrical and optical properties of the film, and the higher the density of the target material, the better the performance of the film. At present, the Al content in most targets for preparing TiAlN coating is above 30%, al is used as a matrix, and Hot Isostatic Pressing (HIP) is carried out at a lower temperature (400-500 ℃) by mixing simple substance powder, so that the target bulk material with the density of more than 99% is finally obtained.
And for the target material, when the Ti content is higher, the PVD coating technology utilizes the electric and optical properties of the film formed by the target material on the body to be coated to be better. However, when the Al content in the target is less than 30at%, ti in the target corresponds to the matrix, and a high-density (99%) target cannot be obtained by molding at the same HIP temperature, and it is necessary to further raise the HIP temperature to solve the problem. And because the melting point of Al is relatively low, the HIP temperature is raised to easily cause melting of Al powder and the sheath, and when the temperature is higher than 500 ℃, the Al and Ti can generate alloying reaction to emit heat, so that the Al and the sheath in the target are further caused to be melted, and the target is difficult to form.
In order to solve the problem that when preparing a high-density low-aluminum target material, the target material is difficult to form due to the fact that Al and a sheath are melted caused by the fact that the HIP temperature is increased, the prior art proposes to prepare TiAl alloy by smelting firstly, then prepare TiAl alloy powder in an atomization powder preparation mode, and take the TiAl alloy powder as a raw material of Al element in the target material, so that Al is not easy to flow due to melting caused by overhigh temperature, and the high-density target material can be prepared by a powder metallurgy high-temperature forming method. However, the process for preparing the TiAl alloy by smelting and preparing the TiAl alloy powder by atomizing and pulverizing is relatively complex, the cost is high, and the mass production is difficult.
Disclosure of Invention
In order to improve the density of an aluminum-titanium-based target and reduce the preparation cost of the target, the application provides a low-aluminum-content titanium-based target and a preparation method thereof.
The application provides a low-aluminum-content titanium-based target material and a preparation method thereof, which adopts the following technical scheme:
The low-aluminum-content titanium-based target and the preparation method thereof are characterized by comprising the following steps:
Mechanically mixing Al powder, ti powder and Me powder according to a proportion to form mixed powder, wherein the content of the Al powder in the mixed powder is 1-30at%, the content of the Ti powder is 70-99%, and the content of the Me powder is 0-20at%;
Filling the powder into a sheath, and performing two times of hot isostatic pressing, wherein the heat treatment temperature of the first time of hot isostatic pressing is T 1, and the heat treatment temperature of the second time of hot isostatic pressing is T 2, and the requirements are met: t 2-T1 = 250-800 ℃.
When the Al content in the target is less than 30at%, ti in the target corresponds to the matrix, and a high-density (99%) target cannot be obtained by molding at the same HIP temperature, and the HIP temperature needs to be further raised to solve the problem. The melting point of Al is low, the high temperature in the hot isostatic pressing treatment process can cause alloying reaction of Ti and Al to emit heat, the high heat of the high-temperature hot isostatic pressing treatment and the heat emitted by alloying can cause Al to be melted, and a high-density target material is difficult to obtain.
According to the technical scheme, the mixed powder of the Al powder, the Ti powder and the Me powder is filled into the sheath and then subjected to hot isostatic pressing twice, and as the temperature of T 2-T1 =250-800 ℃, the Al powder, the Ti powder and the Me powder can be solidified together by the first hot isostatic pressing treatment to form an initial TiAlMe target ingot blank with low density, and the initial TiAlMe target ingot blank is further densified by the second hot isostatic pressing treatment and the like. Since Al is already consolidated in the original TiAlMe target ingot after the first hiping, the melted Al does not flow, so that the original TiAlMe target ingot can be shaped into a high-density target material after the second hiping. The target is preformed through the first hot isostatic pressing, then the target is compactly formed through the second hot isostatic pressing, the TiAl alloy powder does not need to be prepared through smelting and atomizing powder preparation, the situation that the target cannot be formed due to the fact that the Al is melted due to the fact that the HIP temperature is too high can be reduced, the process difficulty is reduced, and the preparation cost of the target is greatly reduced.
Optionally, the step of twice hot isostatic pressing comprises:
Filling the powder into a first sheath, reserving a degassing port in the first sheath, heating, vacuum degassing, performing first hot isostatic pressing, and removing the first sheath to obtain an initial TiAlMe target ingot blank with the density of more than or equal to 85%;
and loading the initial TiAlMe target ingot blank into a second sheath, heating, vacuum degassing, performing second hot isostatic pressing, and removing the sheath to obtain a TiAlMe target ingot blank finished product with the density of more than or equal to 99%.
By adopting the technical scheme, the first sheath and the second sheath are respectively vacuumized through heating and vacuum degassing, and water or gas impurities which are physically adsorbed and weakly bonded in the mixed powder and the initial TiAlMe target ingot blank are desorbed and extracted, so that the gas impurities such as N, O in the target are effectively reduced, and the purity of the target product is improved.
Optionally, the treatment temperature of the first hot isostatic pressing treatment is 400-600 ℃, the pressure is 100-150 MPa, and the heat preservation and pressure maintaining time is 2-6h.
By adopting the technical scheme, the processing temperature of 400-600 ℃ ensures that the target ingot blank formed by hot pressing does not leave more gaps so as to achieve certain density, and simultaneously, al and the first sheath are not melted to be difficult to mold. If the pressure is lower than 100-150 MPa, the consolidation fastness among Ti powder, al powder and Me powder in the original TiAlMe target ingot blank is insufficient, so that Al flows after being melted in a high-temperature hot isostatic pressing stage and is difficult to form; if the pressure setting is too great, the cost of the hot isostatic pressing process will increase.
Optionally, the treatment temperature of the second hot isostatic pressing treatment is 850-1200 ℃, the pressure is 100-150 MPa, and the heat preservation and pressure maintaining time is 2-6 h.
By adopting the technical scheme, the processing temperature of 850-1200 ℃ can enable the initial TiAlMe target ingot blank to be further densified, so that certain compactness can be achieved, HIP cost is not too high due to too high temperature, and the condition that the target is difficult to be molded due to melting of a second cladding caused by too high temperature is not easy to occur.
Optionally, the first sheath is an aluminum sheath, and the second sheath is a stainless steel sheath.
By adopting the technical scheme, the aluminum sheath cannot be melted at the processing temperature in the second hot isostatic pressing process, so that the mixed powder in the aluminum sheath can be preformed in the hot isostatic pressing process. The heat-bearing range of the stainless steel is generally between 1000 ℃ and 1300 ℃, wherein the heat-bearing temperature of the stainless steel of the model 316 can reach 1300 ℃, so that the stainless steel sheath is heat-resistant and not molten in the second hot isostatic pressing treatment, and the low-density TiAlMe target ingot blank is easier to compact in the high-temperature hot isostatic pressing treatment.
Optionally, the degassing temperature of the heating vacuum degassing treatment is 400-600 ℃ for two times, the degassing heat preservation vacuum degree is less than or equal to 2 x 10 -2 Pa, and the heat preservation time is 4-8h.
By adopting the technical scheme, the limited degassing temperature, heat preservation vacuum degree and time can enable the water or gas impurities which are physically adsorbed and weakly bonded adsorbed in the mixed powder and the initial TiAlMe target ingot blank to be more thoroughly desorbed and extracted, and meanwhile, the heating vacuum degassing treatment cost is not greatly increased, so that the preparation cost is reduced.
Optionally, the granularity of the Ti powder is-80 to-500 meshes; the granularity of the Al powder is-200 to-500 meshes; the Me powder is-200 to-500 meshes.
By adopting the technical scheme, the granularity range of-80 to-500 meshes means that Ti can pass through a screen with the granularity range of 80 to 500 meshes, and the Al powder and the Me powder are the same. The grain size of the target is mainly controlled by the grain size of the single powder, and the smaller the grain size of the single powder is, the smaller the grain size of the target is. However, if the simple substance powder is too small, the mixing is not uniform, and the grain sizes of different parts of the prepared target material are large; and when the Al powder is unevenly mixed with the other two, the consolidation fastness of the Al in the initial TiAlMe target material is insufficient, so that the condition that the density of the target material product is reduced due to Al flowing occurs in the second hot isostatic pressing treatment. The target material prepared from the Ti powder, the Al powder and the Me powder in the granularity range has higher density due to smaller grain size, and the density of the target material product is not reduced due to uneven mixing.
Optionally, by adopting the above technical scheme, me is an added element material, specifically may be the above elements, so that oxidation resistance, wear resistance, cracking resistance of the formed coating film and other performances of the target material can be respectively improved, and loosening and shrinkage cavity phenomena of the target material can be effectively avoided, so that compactness of the TiAlMe target material is further improved.
Optionally, the purity of the Al powder, the Ti powder and the Me powder is more than or equal to 99.8 percent.
By adopting the technical scheme, the purities of the Al powder, the Ti powder and the Me powder are all more than or equal to 99.8%, and the purity of the finally formed target can be improved, so that the performance and the quality of a sputtering film formed after the sputtering coating of the target are improved.
Optionally, the aluminum content of the titanium-based target is 1-30at%. The density is more than or equal to 99 percent.
In summary, the present application includes at least one of the following beneficial technical effects:
1. The target is preformed through the first hot isostatic pressing, and then the target is subjected to compact forming through the second hot isostatic pressing, so that the high-density target can be obtained, the TiAl alloy powder is not required to be prepared through smelting and atomizing powder preparation, the situation that the target cannot be formed due to the fact that Al is melted due to the fact that the HIP temperature is too high can be reduced, the process difficulty is reduced, and the preparation cost of the target is greatly reduced;
Drawings
FIG. 1 is a process flow diagram of an embodiment of the present application.
Detailed Description
The application is described in further detail below with reference to fig. 1 and the examples.
1. Examples
Example 1:
The low-aluminum-content titanium-based target and the preparation method thereof are characterized by comprising the following steps:
S1, selecting Ti powder with the granularity of-80 meshes, al powder with the granularity of-200 meshes and Me powder with the granularity of-200 meshes, wherein the purities of the Al powder, the Ti powder and the Si powder are all 99.8%, and mechanically mixing the Al powder, the Ti powder and the Me powder according to a proportion to form mixed powder, wherein the content of the Ti powder in the mixed powder is 80at%, the content of the Al powder is 16at% and the content of the Si powder is 4at%.
S2, filling the mixed powder into a first sheath, reserving a degassing port in the first sheath, and carrying out heating and vacuum degassing to obtain a first blank, wherein the temperature of heating and vacuum degassing treatment is 400 ℃, the degassing and heat preservation vacuum degree is 2 x 10 -2 Pa, and the heat preservation time is 4 hours;
S3, performing first hot isostatic pressing treatment on the first blank, wherein the treatment temperature of the first hot isostatic pressing treatment is 400 ℃, the pressure is 100MPa, the heat preservation and pressure maintaining time is 2 hours, and removing the first sheath to obtain an initial TiAlMe target ingot blank with the density of more than or equal to 85%;
S4, loading the initial TiAlMe target ingot blank into a stainless steel sleeve, reserving a degassing port in the stainless steel sleeve, and carrying out heating vacuum degassing treatment again to obtain a second blank, wherein the temperature of the heating vacuum degassing treatment is 400 ℃, the degassing heat preservation vacuum degree is 2 x 10 -2 Pa, and the heat preservation time is 4 hours;
S5, performing second hot isostatic pressing treatment on the second blank, wherein the treatment temperature of the second hot isostatic pressing treatment is 850 ℃, the pressure is 100MPa, and the heat preservation and pressure maintaining time is 2 hours; removing the stainless steel sheath to obtain TiAlMe target ingot blank finished product with density more than or equal to 99%, and performing linear cutting processing to obtain target product meeting the drawing requirement.
Example 2:
the difference from example 1 is that: selecting Ti powder with the granularity of-325 meshes, al powder with the granularity of-325 meshes and Si powder with the granularity of-325 meshes.
Example 3:
The difference from example 1 is that: selecting Ti powder with the granularity of-500 meshes, al powder with the granularity of-500 meshes and Si powder with the granularity of-500 meshes.
Example 4:
the difference from example 2 is that: the treatment temperature of the first hot isostatic pressing treatment is 470 ℃, the pressure is 140MPa, and the heat preservation and pressure maintaining time is 3 hours;
example 5:
the difference from example 2 is that: the treatment temperature of the first hot isostatic pressing treatment is 600 ℃, the pressure is 150MPa, and the heat preservation and pressure maintaining time is 6 hours;
example 6:
The difference from example 4 is that: the treatment temperature of the second hot isostatic pressing treatment is 950 ℃, the pressure is 130MPa, and the heat preservation and pressure maintaining time is 3 hours;
Example 7:
The difference from example 4 is that: the treatment temperature of the second hot isostatic pressing treatment is 1200 ℃, the pressure is 150MPa, and the heat preservation and pressure maintaining time is 3 hours;
example 8;
The difference from example 6 is that: the degassing temperature of the two heating vacuum degassing treatments is 450 ℃, the degassing heat preservation vacuum degree is less than or equal to 2 x 10 -3 Pa, and the heat preservation time is 6h;
example 9;
The difference from example 6 is that: the degassing temperature of the two heating vacuum degassing treatments is 600 ℃, the degassing heat preservation vacuum degree is less than or equal to 2 x 10 -4 Pa, and the heat preservation time is 8 hours;
Example 10:
The difference from example 8 is that: the content of Ti powder is 99at%, the content of Al powder is 1at%, and the content of Si powder is 0at%;
Example 11:
The difference from example 8 is that: the content of Ti powder is 70at%, the content of Al powder is 1at%, and the content of Si powder is 19at%;
2. Comparative example
Comparative example 1:
the difference from example 1 is that: carrying out first hot isostatic pressing forming treatment on the first blank body subjected to heating vacuum degassing treatment, wherein the heat preservation and pressure maintaining time is 6 hours;
Comparative example 2:
The difference from example 1 is that: directly filling the mixed powder into a stainless steel sleeve, reserving a degassing port on the stainless steel sleeve, heating and vacuum degassing to obtain a third blank, and performing second hot isostatic pressing on the third blank for 6 hours.
Comparative example 3
The difference from example 1 is that: the treatment temperature of the first hot isostatic pressing treatment was 700 ℃, and the treatment temperature of the first hot isostatic pressing treatment was 900 ℃.
3. Performance test:
1) The average grain size of the target products prepared in examples 1-11 and comparative examples 1-3 was evaluated according to the method for measuring the average grain size of the metal material of GB/T6394-2002;
2) The initial TiAlMe target ingot blanks prepared in examples 1-11 were subjected to a weighing method to determine the relative density of the initial TiAlMe target ingot blank;
3) The target products prepared in examples 1 to 11 and comparative examples 1 to 3 were subjected to measurement of the relative densities of the target products according to the archimedes' drainage method;
4) The target products prepared in examples 1 to 11 and comparative examples 1 to 3 were subjected to spectral energy measurement to determine the purity of the target products.
The above performance test results are shown in table 1:
4. analysis and summary of results:
As can be seen by combining examples 1-11 and comparative examples 1-3 and by combining table 1, example 1 produced a target product having a relative density of 99.1%, whereas comparative example 1 only subjected the first hiping treatment of the first green body of the mixed powder, while maintaining the temperature and pressure for the same time as example 1, produced a target product having a relative density much lower than example 1; in comparative example 2, the mixed powder was directly charged into the stainless steel sheath to prepare a third green body, and the third green body was subjected to only the second hot isostatic pressing treatment, and the relative density of the prepared target product was lower than that of example 1, although the holding time was the same as that of example 1.
As can be seen from Table 1, the relative density of the target product of comparative example 3 was 89.9%, which is much lower than that of example 1. It is clear from this that when the treatment temperature of the first HIP'd treatment is too high and the temperature of the second HIP'd treatment is too low, i.e., the temperature difference between the first HIP'd treatment and the second HIP'd treatment is too small, the relative densities of the obtained target products meet.
From the above, the mixed powder is preformed by the first hot isostatic pressing treatment, and then is further densified by the second hot isostatic pressing treatment, and when the temperature difference between the first hot isostatic pressing treatment and the second hot isostatic pressing treatment is=250-800 ℃, the target material with the relative density more than or equal to 99% can be obtained.
As can be seen from Table 1, the relative density of the target products of example 4 was 99.5%, and the relative densities of the target products of examples 6-7 were all 99.9%. From the above, the treatment temperature, pressure and holding time of the second hiping treatment in example 6 were better for densification of the target product than in example 4. Example 7 does not improve the densification of the target product over example 6 and would increase HIP costs and be detrimental to production.
The grain sizes of the Ti powder, the Al powder and the Si powder selected in examples 1-3 are ordered as follows: example 1 > example 2 > example 3. As is clear from Table 1, the average grain size of example 1 was 90 to 105. Mu.m, the relative density was 99.1%, the average grain size of example 2 was 50 to 60. Mu.m, the relative density was 99.4%, and the average grain size of example 3 was 45 to 65. Mu.m, the relative density was 99.3%.
From the above, example 1 resulted in a larger average grain size of the target product due to the larger grain size, and example 2 resulted in a smaller grain size resulting in a larger average grain size of the target product, such that the relative density of the target product of example 2 was greater than that of example 1; however, in example 3, the particle size was too small, so that the uniformity of the mixed powder was insufficient, the difference in average grain size of the target product was increased, and the relative density of the target was decreased. Therefore, when the grain sizes of Ti powder, al powder and Si powder are 325 meshes, the parallel grain size of the target product can be smaller and more uniform, the relative density of the target product is larger, and the quality of the target product is better.
As can be seen from table 1, the initial TiAlMe target ingot of example 2 had a relative density of 86%, the target product had a relative density of 99.4%, the initial TiAlMe target ingot of example 4 had a relative density of 89%, the target product had a relative density of 99.5%, the initial TiAlMe target ingot of example 5 had a relative density of 89%, and the target product had a relative density of 99.5%.
From the above, compared with example 2, the treatment temperature, pressure and holding time of the first hot isostatic pressing treatment in example 4 have better preforming effect on the mixed powder, and the corresponding densification effect on the target product is also improved. Example 5 does not improve the preforming effect on the mixed powder and densification effect on the target product compared to example 4, and would increase HIP cost, which is disadvantageous for production.
As can be seen from Table 1, the purity of the target product of example 6 was 99.91%, and the purity of the target products of examples 7 to 8 was 99.96%. From the above, compared with example 6, the degassing temperature, the degassing heat-preserving vacuum degree and the heat-preserving time of the heating vacuum degassing treatment in example 7 can desorb and extract the water or gas impurities which are physically adsorbed and weakly bonded in the mixed powder and the initial TiAlMe target ingot blank more thoroughly, so that the purity of the target product is better. Example 8 does not improve the purity enhancement effect of the target product compared to example 6, and increases the cost of the heating vacuum degassing treatment, which is disadvantageous for production.
The above embodiments are not intended to limit the scope of the present application, so: all equivalent changes in structure, shape and principle of the application should be covered in the scope of protection of the application.
Claims (6)
1. The preparation method of the low-aluminum-content titanium-based target material is characterized by comprising the following steps of:
Mechanically mixing Al powder, ti powder and Me powder according to a proportion to form mixed powder, wherein the content of the Al powder in the mixed powder is 1-30at%, the content of the Ti powder is 70-99at%, and the content of the Me powder is 0-20at%;
The mixed powder is filled into a sheath, and twice hot isostatic pressing is carried out, wherein the heat treatment temperature of the first hot isostatic pressing treatment is T1, the heat treatment temperature of the second hot isostatic pressing treatment is T2, and the conditions are satisfied: t2-t1=250-800 ℃;
Filling the powder into a first sheath, reserving a degassing port in the first sheath, heating, vacuum degassing, performing first hot isostatic pressing, and removing the first sheath to obtain an initial TiAlMe target ingot blank with the density of more than or equal to 85%;
Loading the initial TiAlMe target ingot blank into a second sheath, heating, vacuum degassing, performing second hot isostatic pressing, and removing the sheath to obtain a TiAlMe target ingot blank finished product with the density of more than or equal to 99%;
The treatment temperature of the first hot isostatic pressing treatment is 400-600 ℃, the pressure is 100-150 MPa, and the heat preservation and pressure maintaining time is 2-6h;
The degassing temperature of the heating vacuum degassing treatment is 400-600 ℃ for two times, the degassing heat preservation vacuum degree is less than or equal to 2x10 - 2 Pa, and the heat preservation time is 4-8h;
the granularity of the Ti powder is-80 to-500 meshes; the granularity of the Al powder is-200 to-500 meshes; the Me powder is-200 to-500 meshes.
2. The method for preparing a low aluminum content titanium-based target material according to claim 1, wherein the method comprises the following steps: the treatment temperature of the second hot isostatic pressing treatment is 850-1200 ℃, the pressure is 100-150 MPa, and the heat preservation and pressure maintaining time is 2-6 h.
3. The method for preparing a low aluminum content titanium-based target material according to claim 2, wherein the method comprises the following steps: the first sheath is an aluminum sheath; the second sheath is a stainless steel sheath.
4. A method for producing a low aluminum content titanium-based target according to any one of claims 1 to 3, characterized in that: and Me is at least one selected from Si, B, zr, W, co, mo, cr, ta, nb, V and La elements.
5. A method for producing a low aluminum content titanium-based target according to any one of claims 1 to 3, characterized in that: the purity of the Al powder, the Ti powder and the Me powder is more than or equal to 99.8 percent.
6. A low aluminum content titanium-based target produced by the production method of any one of claims 1 to 5, characterized in that: the aluminum content of the titanium-based target material is 1-30at% and the density is more than or equal to 99%.
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