CN114807875A - Preparation method of amorphous alloy thick film of immiscible metal - Google Patents

Preparation method of amorphous alloy thick film of immiscible metal Download PDF

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CN114807875A
CN114807875A CN202210424640.XA CN202210424640A CN114807875A CN 114807875 A CN114807875 A CN 114807875A CN 202210424640 A CN202210424640 A CN 202210424640A CN 114807875 A CN114807875 A CN 114807875A
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immiscible
alloy
ion source
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易军
贾生伟
黄波
卞西磊
贾延东
王刚
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University of Shanghai for Science and Technology
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    • 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
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    • 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
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    • C23C14/3442—Applying energy to the substrate during sputtering using an ion beam
    • C—CHEMISTRY; METALLURGY
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
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    • C22C45/04—Amorphous alloys with nickel or cobalt as the major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
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    • 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
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    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
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    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
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    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
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    • 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
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    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • 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
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Abstract

The invention discloses a preparation method of an amorphous alloy thick film of immiscible metal, which is characterized in that immiscible metal is spliced into a target material, a focusing ion source bombards the target material with certain energy, atoms which are originally immiscible are sputtered and deposited on a rotating substrate, and the rotation of the substrate enables alloy components to be uniform. Due to the very high cooling rate, immiscible atoms have no time to phase separate to form an amorphous alloy. While sputtering and depositing, the surface of the growing alloy film is bombarded by an auxiliary ion source with smaller energy and beam current, so that the compactness of the film in the deposition process is improved, and the preparation of the amorphous immiscible alloy thick film is realized. The method can obviously improve the amorphous forming capability of the alloy, and the thickness of the prepared alloy film difficult to dissolve in each other can even reach more than 100 microns, and the prepared alloy film has large size and high density.

Description

Preparation method of amorphous alloy thick film of immiscible metal
Technical Field
The invention relates to a preparation method of an amorphous alloy thick film, belonging to the field of material science and condensed state physics.
Background
The amorphous alloy has unique mechanical properties such as ultrahigh strength, fracture toughness, high hardness, low elastic modulus, high fatigue performance and the like due to the long-range disordered short-range ordered structure; the amorphous alloy also has unique functional characteristics, such as high magnetic permeability, low coercive force, low iron loss, excellent catalytic performance, corrosion resistance, excellent catalytic performance and the like. Has attracted extensive research interest in basic research and engineering applications. However, due to the limitations of glass forming ability, most of the conventional alloy compositions cannot be made into amorphous alloys. Since Duwez prepared AuSi amorphous alloy by rapid solidification in 1961 (reference 1, W.Klement, R.H.Willens, P.Duwez, Non-crystalline structure in solid gold-silicon alloys, Nature 187869-.
Years of research experience shows that the formation of amorphous alloy generally satisfies the following conditions:
firstly, the number of alloy components is more than 3;
secondly, the atomic size difference between the constituent elements is larger than 12 percent;
and thirdly, the main components have larger negative mixing enthalpy (document 2, A. Inoue, Stabilization of metallic supercooled liquid and bulk Amorphous alloys, Acta Materialia 48279-306 (2000)).
Satisfying these conditions at the same time allows the alloy to have a greater glass forming ability. Based on this composition design criteria, a number of composition systems with large glass forming capabilities have been explored. However, this criterion is not valid for immiscible alloy systems, since the enthalpy of mixing of immiscible alloy systems is positive. Cu-W (document 3, T.Xie, J.Zhu, L.Fu, et al, The evaluation of hard in Cu-W alloy films, Materials Science and Engineering A729170-. However, the immiscible amorphous alloy thin film prepared by the method cannot be characterized in certain properties and structures due to the limitation of the thickness, such as performance tests of stretching, breaking and fatigue, and structural characterization of high-energy X-ray, and the like, and limits scientific understanding and engineering application of the materials to a certain extent. Therefore, a new process for preparing an amorphous immiscible alloy with sufficient thickness is urgently needed, so that the application space of the amorphous immiscible alloy is opened.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defect of insufficient thickness of the amorphous immiscible alloy prepared in the prior art, and provides a preparation method of the amorphous immiscible metal thick film.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
a method for preparing an amorphous alloy thick film of immiscible metal comprises the following steps:
splicing immiscible metals into a target material, and bombarding the target material by using a focused ion source; sputtering out immiscible metal atoms which are immiscible originally and depositing the immiscible metal atoms on a rotating substrate; rotation of the substrate table makes the alloy composition uniform; because the cooling speed of the metal atoms is very high, the immiscible metal atoms cannot be separated in time to form amorphous alloy; while sputtering and depositing, bombarding the growing alloy film surface with auxiliary ion source and smaller energy and beam current than the focused ion source to densify the alloy film during deposition and to prepare thick amorphous immiscible alloy film.
Preferably, the target material is a wafer spliced by at least two immiscible metals.
Preferably, the immiscible alloy is at least one of an X-Cu alloy, a Y-Al alloy, a Ni-Ag alloy and Bi-Ga; wherein X is at least one of Nb, Mo, Ta, W, Sn, Pb, Co, Cr, Zr, Bi and Fe, and Y is at least one of Sn, Bi, In and Pb.
Preferably, the energy of the focusing ion source is 300-1500eV, and the beam current is 30-150 mA; preferably, the energy of the auxiliary ion source is not higher than 600eV, and the beam current is not higher than 80 mA.
Preferably, the substrate is made of Si, glass, SiC, SiN and a base made of metal materials.
Preferably, the deposition rate of the alloy film is 1-20 nm/min.
Preferably, during said alloy film deposition, the substrate table is rotated at a speed not higher than 60 rmp.
Preferably, the working gas pressure during the deposition of the alloy film is 1.0X 10 -2 Pa-5.0×10 -2 Pa。
Preferably, the thickness of the prepared amorphous alloy thick film of immiscible metal is not less than 10 μm, even up to not less than 100 μm.
Preferably, the mass percentages of various metals required by the target are calculated according to the components of the prepared target amorphous alloy thick film, the angle of a sector part required by each metal on the circular target is calculated according to the mass percentages, and the immiscible metals are spliced into the target.
Preferably, the process method for preparing the immiscible amorphous alloy thick film provided by the invention comprises the design and preparation of a target material before ion beam sputtering, wherein the used target material is a wafer formed by splicing immiscible sector metals together. Calculating the mass percentages of various metals required by the target according to the components of the prepared alloy film, and calculating the fan-shaped angle required by each metal on the circular target according to the mass percentages.
Preferably, the system to be vacuumized is vacuumized to a high vacuum state, argon is introduced to adjust the working pressure, the substrate table rotates at a constant speed, the focusing ion source bombards the target material with high energy and beam current, a cascade collision effect is generated in a few atomic layers on the outermost surface of the target material, a large number of target material particles are sputtered, atoms which are difficult to mix originally are sputtered out and deposited on a rotating substrate, the rotation of the substrate enables the alloy components to be uniform, and the deposited particles are solidified into amorphous alloy without phase separation. Meanwhile, the auxiliary ion source bombards the growing alloy film with lower energy and beam current, so that the defects on the surface of the alloy film are reduced, the compactness of the alloy film is increased, and the alloy film with larger thickness is prepared. The method specifically comprises the following steps:
1) designing a target according to the components of an alloy film, calculating the mass percentages of various metals of the required target, calculating the required fan-shaped angles of the various metals on the circular target according to the mass percentages, and splicing the various metals into a circular target;
the alloy film prepared by the invention has the composition A a B b Where A and B are immiscible, it is possible for both to be alloys consisting of a plurality of elements, the atomic percentages by weight of metal A and metal B being set to wt A % and wt B % atomic set as at A % and at B % by mole of A metal and B metal, M being the molar mass of the metals A And M B The densities of the A metal and the B metal are set to rho A And ρ B The required volumes of metal A and metal B are set to V A And V B The desired fan central angle is set to n A And n B (ii) a The specific calculation formula is as follows:
the required mass percentage ratio of A to B is as follows:
Figure BDA0003607982530000031
desired volume percent ratio of A to B:
Figure BDA0003607982530000032
required target segment angles of a and B:
n A ＝360×V A ％
n B ＝360×V B ％
2) after designing the target material according to the above mode, the substrate is arranged on the substrate table of the vacuum cavity, the alloy target material is arranged on the target table, the vacuum cavity is closed, the baffle plate is opened, and the air pressure in the vacuum cavity is pumped to be lower than 6 multiplied by 10 by the vacuum pumping system -4 Pa; introducing argon gas into the focusing ion source and the auxiliary ion source to stabilize the working pressure in the cavity at 1.0 × 10 -2 Pa to 5.0X 10 -2 Pa; before depositing the alloy film, closing the baffle, starting the auxiliary ion source and bombarding the substrate by the energy of not less than 100eV and the beam current of not less than 10mA for pre-cleaning; then closing the auxiliary ion source and opening the baffle; starting a focusing ion source, bombarding the surface of the target by using energy not less than 300eV and beam current not less than 30mA to remove an oxide layer, and closing the focusing ion source;
3) opening a substrate table driving motor to enable the substrate table to rotate at 0-60 rmp, closing a baffle, opening a focusing ion source to bombard a target at high energy of 150-1500eV and beam current of 0-100mA, and sputtering a large amount of target particles to enable immiscible atoms to be mixed together forcibly and deposited on the surface of the substrate; because of the very high cooling rate, the deposited particles solidify to form amorphous alloys without having to phase separate; meanwhile, the auxiliary ion source is started to bombard the growing alloy film with lower energy of 0-600eV and beam current of 0-80mA, so that the defects on the surface of the alloy film are reduced, the compactness of the alloy film is increased, and the alloy film with larger thickness is prepared.
The invention provides a preparation method of an immiscible amorphous alloy thick film, which is characterized in that immiscible metal is spliced into a target material, a focusing ion source is used for bombarding the target material with certain energy, atoms of different components which are originally immiscible are mixed together forcibly, then the mixture is deposited on a rotating alloy film substrate, and due to the very high cooling speed, the amorphous alloy is formed in time of phase separation. When the focused ion source sputters, the auxiliary ion source bombards the surface of the alloy film which is growing with certain energy, the binding force between the alloy film and the substrate is improved, the compactness of the alloy film in the deposition process is improved, and the preparation of the amorphous immiscible alloy thick film is realized.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the thickness of the immiscible alloy film prepared by the process method is not less than 10 micrometers, even can reach more than 100 micrometers, which cannot be reached by the prior art;
2. in the preparation process, the auxiliary ion source bombards the growing alloy film, the energy carried by the bombardment is transferred to the deposited atoms, and the atoms transversely and longitudinally migrate after obtaining the energy, so that the alloy film cavity is filled, and meanwhile, the atoms with low adhesion capability can be sputtered away from the surface of the alloy film to finally form a compact alloy film;
3. when the preparation is started, the auxiliary ion source bombards the substrate on which the alloy film is growing, part of ions penetrate into the surface of the substrate to form a transition layer, so that the film and the substrate atoms are mutually combined, and the binding force between the alloy film and the substrate is obviously improved;
4. the process method of the invention can mix the atoms which are difficult to be mixed together by force, thus realizing the preparation of the amorphous alloy which is difficult to be mixed;
5. the method can use the high-purity immiscible alloy target material, and avoids the impurity problem caused by the target material prepared by powder metallurgy and other methods, thereby improving the amorphous forming capability of the alloy and enabling more component systems to be prepared into amorphous alloy.
Drawings
FIG. 1 is a schematic view of an apparatus for preparing an immiscible amorphous alloy thick film according to a preferred embodiment of the present invention. The ion source system comprises a focusing ion source 1, an auxiliary ion source 2, a substrate table 3, a target table 4, a focusing ion source ion beam 5, an auxiliary ion source ion beam 6, a sample ion beam 7, a substrate 8, a target 9, a baffle 10 and a vacuum cavity 11.
FIG. 2 shows Cu in example 1 60 W 40 Schematic diagram of target design. Wherein 1 '-Cu, 2' -W.
FIG. 3 is a graph representing Cu in example 1 60 W 40 And (3) a high-resolution transmission electron microscope picture of the amorphous thick film, wherein the inset is a picture after Fourier transformation.
Figure 4 is an X-ray diffraction (XRD) picture characterizing the NbMoTaWCu amorphous thick film in example 2.
FIG. 5 is a high resolution TEM image of the NbMoTaWCu amorphous thick film of example 2, with the inset being a selected area electron diffraction image.
FIG. 6 is a 12 inch diameter 20 micron thick Mo prepared in example 9 55 Cu 45 Photo of amorphous alloy thick film.
Detailed Description
The invention discloses a process method for preparing an immiscible amorphous alloy thick film, which comprises the steps of splicing immiscible metal into a target material, bombarding the target material by a focusing ion source with certain energy, sputtering atoms which are originally immiscible and depositing the atoms onto a rotating substrate, and rotating the substrate to ensure that alloy components are uniform. Due to the very high cooling rate, immiscible atoms have no time to phase separate to form an amorphous alloy. While sputtering and depositing, bombarding the surface of the growing alloy film with small energy and beam current by using an auxiliary ion source, and improving the compactness of the film in the deposition process, thereby realizing the preparation of the amorphous immiscible alloy thick film; the method specifically comprises the following steps:
1) designing a target according to the components of an alloy film, calculating the mass percentages of various metals of the required target, calculating the required fan-shaped angles of the various metals on the circular target according to the mass percentages, and splicing into a circular target;
the alloy film prepared by the invention has the composition A a B b Where A and B are immiscible, it is possible for both to be alloys consisting of a plurality of elements, the atomic percentages by weight of metal A and metal B being set to wt A % and wt B % atomic set as at A % and at B % by mole of A metal and B metal, M being the molar mass of the metals A And M B The densities of the A metal and the B metal are set to rho A And ρ B The required volume of the A metal and the B metal is set as V A And V B The desired fan central angle is set to n A And n B (ii) a The specific calculation formula is as follows:
the required mass percentage ratio of A to B is as follows:
Figure BDA0003607982530000051
desired volume percent ratio of A to B:
Figure BDA0003607982530000052
required target segment angles of a and B:
n A ＝360×V A ％
n B ＝360×V B ％
2) referring to fig. 1, after the target 9 is designed according to the step 1), the substrate 8 is mounted on the substrate stage 3 of the vacuum chamber 11, the alloy target 9 is mounted on the target stage 4, the vacuum chamber 11 is closed, and the air pressure in the vacuum chamber 11 is pumped to be lower than 6 × 10 by using a vacuum pumping system -4 Pa; then introducing argon into the focusing ion source 1 and the auxiliary ion source 2 until the vacuum chamber 11 is stabilized at the working pressure of 1.0 × 10 -2 Pa to 5.0X 10 -2 Pa, closing the baffle 10, firstly opening the auxiliary ion source 2 and bombarding the substrate 8 with energy not less than 100eV and beam current not less than 10mA for pre-cleaning; the auxiliary ion source 2 is then turned off and the shutter 10 is opened. The focusing ion source 1 is turned on and the beam is irradiated at an energy of not less than 300eV and a beam intensity of not less than 30mAClosing the focusing ion source 1 after the oxide layer on the surface of the target 9 is removed by flow bombardment;
3) closing the baffle 10, opening the substrate table driving motor to rotate the substrate table at 0 to 60rmp, bombarding the target 9 by the focused ion source 1 at the higher energy of 150-1500eV and the beam current of 0-100mA, sputtering a large amount of target particles, and forcibly mixing immiscible atoms together to deposit on the surface of the substrate 8, wherein the deposited particles are solidified into amorphous alloy without being separated in time due to the very high cooling speed. Meanwhile, the auxiliary ion source is started to bombard the growing alloy film with lower energy of 0-600eV and ion beam current of 0-80mA, so that the defects on the surface of the alloy film are reduced, the compactness of the alloy film is increased, and the alloy film with larger thickness is prepared.
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
example 1
In this example, a method for preparing an amorphous alloy thick film of immiscible metal, Cu, was used 60 W 40 The immiscible amorphous alloy thick film comprises the following steps:
1) firstly, designing a target material according to atomic percentages required by experiments, wherein the specific design mode is as follows:
the mass percentage ratio of Cu to W required in this embodiment:
Figure BDA0003607982530000061
the volume percentage ratio of Cu to W required in this example:
Figure BDA0003607982530000062
the sector angle of the Cu and W target required in this embodiment:
n Cu ＝360×V Cu ％＝189.1°
n W ＝360×V W ％＝170.9°
according to the design mode, cutting 189.1-degree sector Cu, cutting 170.9-degree sector W with the same thickness and radius as Cu, and splicing the two into a complete wafer target, wherein the schematic diagram of the target is shown in FIG. 2;
2) mounting a wafer target on a target table of a vacuum chamber, mounting a 4-inch silicon wafer substrate on a substrate table of the vacuum chamber, closing the vacuum chamber, and vacuumizing to 4 x 10 by using a vacuumizing system -4 Pa, then introducing argon into the ion source, maintaining 2.8X 10 - 2 A working air pressure of Pa; before depositing an alloy film, closing the baffle, starting an auxiliary ion source to bombard the substrate for 5min with 500eV energy and 50mA beam current for pre-cleaning, and then closing the auxiliary ion source; opening a baffle, starting a focusing ion source to bombard the target for 20min by 700eV energy and 70mA beam current, and closing the focusing ion source after removing an oxide layer on the surface of the target;
3) closing the baffle, opening a substrate table driving motor, rotating the substrate table at 30rmp, and starting coating at room temperature; starting a focusing ion source, bombarding the target with 700eV energy and 70mA beam current, sputtering a large amount of target particles, and forcibly mixing immiscible atoms together to deposit on the surface of the substrate; meanwhile, the auxiliary ion source is started and the growing alloy film is bombarded by 100eV energy and 20mA beam current, so that the defects on the surface of the alloy film are reduced, and the compactness of the alloy film is increased; depositing for 48 hours continuously to prepare Cu with the thickness of 10 microns 60 W 40 Immiscible amorphous alloy thick film.
Experimental test analysis:
cu prepared in this example 60 W 40 The high-resolution transmission electron microscope picture and the inset after Fourier transformation of the immiscible amorphous alloy thick film are shown in figure 3, and it can be seen that the atomic arrangement is disordered in a long range and has no periodicity, and a diffraction ring appears in the picture after Fourier transformation, which fully proves that the picture is a typical amorphous structure.
Example 2
This embodiment is substantially the same as embodiment 1, and is characterized in that:
in this embodiment, a method for preparing an amorphous alloy thick film of immiscible metal includes the following steps:
1) calculating the volume percent of the NbMoTaW target material and the Cu target material prepared by the powder metallurgy method according to the atomic percent in the embodiment 1, calculating the fan-shaped angle required by the NbMoTaW and the Cu, and splicing the NbMoTaW target material and the Cu target material into a complete wafer target material;
2) mounting a wafer target on a target table of a vacuum chamber, mounting a 12-inch silicon wafer substrate on a substrate table of the vacuum chamber, closing the vacuum chamber, and vacuumizing to 3 × 10 by using a vacuumizing system -4 Pa, then introducing argon into the ion source, and keeping the pressure at 2.7X 10 - 2 A working air pressure of Pa; before depositing an alloy film, closing the baffle, starting an auxiliary ion source to bombard the substrate for 6min with 500eV energy and 50mA beam current for pre-cleaning, and then closing the auxiliary ion source; opening a baffle, starting a focusing ion source to bombard the target for 25min by 700eV energy and 70mA beam current, and closing the focusing ion source after removing an oxide layer on the surface of the target;
3) closing the shutter, opening the substrate table drive motor, and rotating the substrate table at 35 rmp; starting a focusing ion source, bombarding the target with 700eV energy and 70mA beam current, sputtering a large amount of target particles, and forcibly mixing immiscible atoms together to deposit on the surface of the substrate; simultaneously, starting an auxiliary ion source and bombarding the growing alloy film by 100eV energy and 18mA beam current, so that the defects on the surface of the alloy film are reduced, and the compactness of the alloy film is increased; continuously depositing for 48h to prepare the NbMoTaWCu immiscible amorphous alloy thick film with the thickness of 12 mu m.
Experimental test analysis:
the X-ray diffraction (XRD) of the NbMoTaWCu immiscible amorphous alloy thick film prepared in this example is shown in fig. 4, and it can be seen that there is no sharp bragg peak corresponding to the crystal on the XRD diffraction pattern except for the broad diffuse peak, so the prepared NbMoTaWCu immiscible amorphous alloy thick film with 12 μm thickness is a single amorphous phase. As shown in fig. 5, in order to further characterize the high resolution transmission electron microscope picture and the selected area electron diffraction picture of the NbMoTaWCu immiscible amorphous thick film, it can be seen that the atomic arrangement is disordered in long range and has no periodicity, and the selected area electron diffraction pattern has a diffraction ring, which is fully proved to be a complete amorphous structure.
Example 3
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, a method for preparing an amorphous alloy thick film of immiscible metal, Cu, was used 55 Ta 45 The immiscible amorphous alloy thick film comprises the following steps:
1) calculating the volume percentage of the high-purity Cu and Ta target materials according to the atomic percentage in the embodiment 1, calculating the fan-shaped angle required by each Cu and Ta, and splicing the high-purity Cu and Ta target materials into a complete wafer target material;
2) mounting the target material on the target platform of the vacuum chamber, mounting the 12-inch silicon wafer substrate on the substrate table of the vacuum chamber, closing the vacuum chamber, and vacuumizing to 4 × 10 with a vacuumizing system -4 Pa, then argon gas was introduced into the ion source, and 2.7X 10 was maintained -2 A working air pressure of Pa; before depositing an alloy film, closing the baffle, starting an auxiliary ion source to bombard the substrate for 6min with 500eV energy and 50mA beam current for pre-cleaning, and then closing the auxiliary ion source; opening a baffle, starting a focusing ion source to bombard the target for 30min by 700eV energy and 70mA beam current, and closing the focusing ion source after removing an oxide layer on the surface of the target;
3) closing the shutter, opening the substrate table drive motor, and rotating the substrate table at 35 rmp; starting a focusing ion source, bombarding the target with 800eV energy and 85mA beam current, sputtering a large amount of target particles, and forcibly mixing immiscible atoms together to deposit on the surface of the substrate; meanwhile, the auxiliary ion source is started and the growing alloy film is bombarded by 100eV energy and 20mA beam current, so that the defects on the surface of the alloy film are reduced, and the compactness of the alloy film is increased; depositing for 60 hours continuously to prepare Cu with the thickness of 12 mu m 55 Ta 45 Immiscible amorphous alloy thick film.
Example 4
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, a method for preparing an amorphous alloy thick film of immiscible metal, Nb 25 Ta 25 Cu 50 The immiscible amorphous alloy thick film comprises the following steps:
1) calculating the volume percentage of the high-purity NbTa target material and the Cu target material according to the atomic percentage in the embodiment 1, calculating the fan-shaped angles required by the three target materials, and splicing the three target materials into a complete wafer target material;
2) mounting the target material on a target table of a vacuum chamber, mounting a 12-inch silicon wafer substrate on a substrate table of the vacuum chamber, closing the vacuum chamber, and vacuumizing to 5 x 10 by using a vacuumizing system -4 Pa, then argon gas was introduced into the ion source, and 2.7X 10 was maintained -2 A working air pressure of Pa; before depositing an alloy film, closing the baffle, starting an auxiliary ion source to bombard the substrate for 6min with 500eV energy and 50mA beam current for pre-cleaning, and then closing the auxiliary ion source; opening a baffle, starting a focusing ion source to bombard the target for 20min by 700eV energy and 70mA beam current, and closing the focusing ion source after removing an oxide layer on the surface of the target;
3) closing the shutter, opening the substrate table drive motor, and rotating the substrate table at 40 rmp; starting a focusing ion source, bombarding the target with 700eV energy and 70mA beam current, sputtering a large amount of target particles, and forcibly mixing immiscible atoms together to deposit on the surface of the substrate; meanwhile, the auxiliary ion source is started and the growing alloy film is bombarded by 100eV energy and 20mA beam current, so that the defects on the surface of the alloy film are reduced, and the compactness of the alloy film is increased; depositing for 75h continuously to prepare Nb with the thickness of 12 mu m 25 Ta 25 Cu 50 Immiscible amorphous alloy thick film.
Example 5
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, a method for preparing an amorphous alloy thick film of immiscible metal, Co 50 Cu 50 The immiscible amorphous alloy thick film comprises the following steps:
1) calculating the volume percentage of the Co target material and the Nb target material according to the atomic percentage in the embodiment 1, calculating the fan-shaped angle required by each Cu and Nb, and splicing into a complete wafer target material;
2) mounting the target on the target table of a vacuum chamber, 4 inches of siliconThe sheet substrate is mounted on a substrate stage of a vacuum chamber, the vacuum chamber is closed, and a vacuum system is used to evacuate air to 4 × 10 -4 Pa, then introducing argon into the ion source, and keeping the pressure at 2.7X 10 -2 A working air pressure of Pa; before depositing an alloy film, closing the baffle, starting an auxiliary ion source to bombard the substrate for 4min at the energy of 500eV and the beam current of 50mA for pre-cleaning, and then closing the auxiliary ion source; opening a baffle, starting a focusing ion source to bombard the target for 25min by 700eV energy and 70mA beam current, and closing the focusing ion source after removing an oxide layer on the surface of the target;
3) closing the shutter, opening the substrate table drive motor, and rotating the substrate table at 25 rmp; starting a focusing ion source, bombarding the target with 900eV energy and 85mA beam current, sputtering a large amount of target particles, and forcibly mixing immiscible atoms together to deposit on the surface of the substrate; meanwhile, the auxiliary ion source is started and the growing alloy film is bombarded by 100eV energy and 20mA beam current, so that the defects on the surface of the alloy film are reduced, and the compactness of the alloy film is increased; depositing for 70h continuously to prepare Co with the thickness of 17 mu m 50 Cu 50 Immiscible amorphous alloy thick film.
Example 6
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, a method for preparing an amorphous alloy thick film of immiscible metal, Nb 20 Mo 30 Cu 50 The immiscible amorphous alloy thick film comprises the following steps:
1) nb prepared by powder metallurgy 2 Mo 3 Calculating the volume percentage of the target material and the Cu target material according to the atomic percentage in the embodiment 1, calculating the fan-shaped angle required by the two target materials, and splicing the two target materials into a complete wafer target material;
2) mounting the target material on the target table of the vacuum chamber, mounting the 18-inch silicon wafer substrate on the substrate table of the vacuum chamber, closing the vacuum chamber, and vacuumizing to 4 × 10 by using a vacuumizing system -4 Pa, then argon gas was introduced into the ion source and maintained at 2.7X 10 - 2 Working air pressure of Pa level; before depositing the alloy film, the baffle is closed, and the auxiliary ion source is started to carry out deposition at 500eV energy and 50mA beam currentBombarding the substrate for 4min for pre-cleaning, and then closing the auxiliary ion source; opening a baffle, starting a focusing ion source to bombard the target for 25min by 700eV energy and 70mA beam current, and closing the focusing ion source after removing an oxide layer on the surface of the target;
3) closing the shutter, opening the substrate table drive motor, and rotating the substrate table at 60 rmp; starting a focusing ion source, bombarding the target with 700eV energy and 70mA beam current, sputtering a large amount of target particles, and forcibly mixing immiscible atoms together to deposit on the surface of the substrate; meanwhile, the auxiliary ion source is started and the growing alloy film is bombarded by 90eV energy and 15mA beam current, so that the defects on the surface of the alloy film are reduced, and the compactness of the alloy film is increased; the continuous deposition is carried out for 65 hours, and Nb with the thickness of 15 mu m is prepared 20 Mo 30 Cu 50 Immiscible amorphous alloy thick film.
Example 7
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, a method for preparing an amorphous alloy thick film of immiscible metal, Ta 20 Mo 20 Cu 60 The immiscible amorphous alloy thick film comprises the following steps:
1) calculating the volume percent of TaMo target material and Cu target material prepared by powder metallurgy according to the atomic percent in the embodiment 1, calculating the fan-shaped angles required by the two target materials, and splicing the two target materials into a complete wafer target material;
2) mounting the target material on a target table of a vacuum chamber, mounting a 2-inch silicon wafer substrate on a substrate table of the vacuum chamber, closing the vacuum chamber, and vacuumizing to 2 x 10 by using a vacuumizing system -4 Pa, then argon gas was introduced into the ion source, and 2.7X 10 was maintained -2 A working air pressure of Pa; before depositing an alloy film, closing the baffle, starting an auxiliary ion source to bombard the substrate for 4min at the energy of 500eV and the beam current of 50mA for pre-cleaning, and then closing the auxiliary ion source; opening a baffle, starting a focusing ion source to bombard the target for 25min by 700eV energy and 70mA beam current, and closing the focusing ion source after removing an oxide layer on the surface of the target;
3) close shutter, open substrate table drive motor, make substrate table go on at 35rmpRotating; starting a focusing ion source, bombarding the target with 800eV energy and 80mA beam current, sputtering a large amount of target particles, and forcibly mixing immiscible atoms together to deposit on the surface of the substrate; meanwhile, the auxiliary ion source is started and the growing alloy film is bombarded by 90eV energy and 17mA beam current, so that the defects on the surface of the alloy film are reduced, and the compactness of the alloy film is increased; the Ta with the thickness of 15 mu m is prepared by continuous deposition for 65h 20 Mo 20 Cu 60 Immiscible amorphous alloy thick film.
Example 8
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, a method for preparing an amorphous alloy thick film of immiscible metal, Nb 30 W 20 Cu 50 The immiscible amorphous alloy thick film comprises the following steps:
1) nb to 3 W 2 Calculating the volume percentage of the target material and the Cu target material according to the atomic percentage in the embodiment 1, calculating the fan-shaped angles required by the three target materials, and splicing the three target materials into a complete wafer target material;
2) mounting the target material on a target table of a vacuum chamber, mounting a 4-inch silicon wafer substrate on a substrate table of the vacuum chamber, closing the vacuum chamber, and vacuumizing to 2 x 10 by using a vacuumizing system -4 Pa, then introducing argon into the ion source, and keeping the pressure at 2.7X 10 -2 A working air pressure of Pa; before depositing an alloy film, closing the baffle, starting an auxiliary ion source to bombard the substrate for 4min at the energy of 500eV and the beam current of 50mA for pre-cleaning, and then closing the auxiliary ion source; opening a baffle, starting a focusing ion source to bombard the target for 25min by 700eV energy and 70mA beam current, and closing the focusing ion source after removing an oxide layer on the surface of the target;
3) closing the shutter, opening the substrate table drive motor, and rotating the substrate table at 35 rmp; starting a focusing ion source, bombarding the target with 900eV energy and 90mA beam current, sputtering a large amount of target particles, and forcibly mixing immiscible atoms together to deposit on the surface of the substrate; simultaneously starting the auxiliary ion source and bombarding the growing alloy film with 100eV energy and 17mA beam current, reducing the defects on the surface of the alloy film and increasing the defects on the alloy filmTightness; the continuous deposition is carried out for 65 hours, and Nb with the thickness of 15 mu m is prepared 30 W 20 Cu 50 Immiscible amorphous alloy thick film.
Example 9
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, a method for preparing an amorphous alloy thick film of immiscible metal, Mo 55 Cu 45 The immiscible amorphous alloy thick film comprises the following steps:
1) calculating the volume percentage of the Mo target material and the Cu target material according to the atomic percentage in the embodiment 1, calculating the fan-shaped angle required by the two target materials, and splicing the two target materials into a complete wafer target material;
2) mounting the target material on a target table of a vacuum chamber, mounting a 4-inch silicon wafer substrate on a substrate table of the vacuum chamber, closing the vacuum chamber, and vacuumizing to 2 x 10 by using a vacuumizing system -4 Pa, then argon gas was introduced into the ion source and maintained at 2.7X 10 -2 Working air pressure of Pa level; before depositing an alloy film, closing the baffle, starting an auxiliary ion source to bombard the substrate for 4min at the energy of 500eV and the beam current of 50mA for pre-cleaning, and then closing the auxiliary ion source; opening a baffle, starting a focusing ion source to bombard the target for 25min by 700eV energy and 70mA beam current, and closing the focusing ion source after removing an oxide layer on the surface of the target;
3) closing the shutter, opening the substrate table drive motor, and rotating the substrate table at 35 rmp; starting a focusing ion source, bombarding the target with 700eV energy and 70mA beam current, sputtering a large amount of target particles, and forcibly mixing immiscible atoms together to deposit on the surface of the substrate; meanwhile, the auxiliary ion source is started and the growing alloy film is bombarded by 100eV energy and 17mA beam current, so that the defects on the surface of the alloy film are reduced, and the compactness of the alloy film is increased; continuously depositing for 80h to prepare Mo with the thickness of 20 mu m 55 Cu 45 Immiscible amorphous alloy thick film.
Experimental test analysis:
as shown in FIG. 6, 12-inch 20-micron-thick Mo prepared in this example 55 Cu 45 Photograph of thick film cross section of immiscible amorphous alloy can be seenThe alloy film bonds well to the substrate.
Example 10
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, a method for preparing an amorphous alloy thick film of immiscible metal, Mo 20 W 25 Cu 55 The immiscible amorphous alloy thick film comprises the following steps:
1) mo prepared by powder metallurgy method 2 W 2.5 Calculating the volume percentage of the target material and the Cu target material according to the atomic percentage in the embodiment 1, calculating the fan-shaped angle required by the two target materials, and splicing the two target materials into a complete wafer target material;
2) mounting the target material on a target table of a vacuum chamber, mounting a 4-inch silicon wafer substrate on a substrate table of the vacuum chamber, closing the vacuum chamber, and vacuumizing to 2 x 10 by using a vacuumizing system -4 Pa, then argon gas was introduced into the ion source, and 2.7X 10 was maintained -2 A working air pressure of Pa; before depositing an alloy film, closing the baffle, starting an auxiliary ion source to bombard the substrate for 4min at the energy of 500eV and the beam current of 50mA for pre-cleaning, and then closing the auxiliary ion source; opening a baffle, starting a focusing ion source to bombard the target for 25min by 700eV energy and 70mA beam current, and closing the focusing ion source after removing an oxide layer on the surface of the target;
3) closing the shutter, opening the substrate table drive motor, and rotating the substrate table at 35 rmp; starting a focusing ion source, bombarding the target with 800eV energy and 80mA beam current, sputtering a large amount of target particles, and forcibly mixing immiscible atoms together to deposit on the surface of the substrate; meanwhile, the auxiliary ion source is started and the growing alloy film is bombarded by 90eV energy and 17mA beam current, so that the defects on the surface of the alloy film are reduced, and the compactness of the alloy film is increased; continuously depositing for 80h to prepare Mo with the thickness of 20 mu m 20 W 25 Cu 55 Immiscible amorphous alloy thick film.
Example 11
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, a method for preparing an amorphous alloy thick film of immiscible metal is disclosed, wherein the immiscible alloy is at least one of Sn-Al alloy, Bi-Al alloy, In-Al alloy, Pb-Al alloy, Ni-Ag alloy, and Bi-Ga.
The method for preparing the immiscible amorphous thick film in the embodiment of the invention comprises the steps of splicing immiscible metals into a target material, bombarding the target material by using a focused ion source with certain energy, sputtering atoms which are originally immiscible and depositing the atoms onto a rotating substrate, and rotating the substrate to ensure that the alloy components are uniform. Due to the very high cooling rate, immiscible atoms have no time to phase separate to form an amorphous alloy. While sputtering and depositing, the surface of the growing alloy film is bombarded by an auxiliary ion source with smaller energy and beam current, so that the compactness of the film in the deposition process is improved, and the preparation of the amorphous immiscible alloy thick film is realized. The method of the embodiment can obviously improve the amorphous forming capability of the alloy, and the thickness of the prepared alloy film difficult to dissolve mutually can even reach more than 100 microns, and has large size and high density.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitutions, as long as the purpose of the present invention is met, and the present invention shall fall within the protection scope of the present invention without departing from the technical principle and inventive concept of the present invention.

Claims (10)

1. A method for preparing an amorphous alloy thick film of immiscible metal is characterized by comprising the following steps:
splicing immiscible metals into a target material, and bombarding the target material by using a focused ion source; sputtering out immiscible metal atoms which are immiscible originally and depositing the immiscible metal atoms on a rotating substrate; rotation of the substrate table makes the alloy composition uniform; because the cooling speed of the metal atoms is very high, the immiscible metal atoms cannot be separated in time to form amorphous alloy; while sputtering and depositing, bombarding the growing alloy film surface with auxiliary ion source and smaller energy and beam current than the focused ion source to densify the alloy film during deposition and to prepare thick amorphous immiscible alloy film.
2. The method of claim 1, wherein the thick amorphous alloy film of immiscible metal is prepared by: the target material is a wafer spliced by at least two immiscible metals.
3. The method of claim 1, wherein the thick amorphous alloy film of immiscible metal is prepared by: the immiscible alloy is at least one of X-Cu alloy, Y-Al alloy, Ni-Ag alloy and Bi-Ga; wherein X is at least one of Nb, Mo, Ta, W, Sn, Pb, Co, Cr, Zr, Bi and Fe, and Y is at least one of Sn, Bi, In and Pb.
4. The method of claim 1, wherein the thick amorphous alloy film of immiscible metal is prepared by: the energy of the focusing ion source is 300-1500eV, and the beam current is 30-150 mA; the energy of the auxiliary ion source is not higher than 600eV, and the beam current is not higher than 80 mA.
5. The method of claim 1, wherein the thick amorphous alloy film of immiscible metal is prepared by: the substrate is made of Si, glass, SiC, SiN and a base made of metal materials.
6. The method of claim 1, wherein the thick amorphous alloy film of immiscible metal is prepared by: the deposition rate of the alloy film is 1-20 nm/min.
7. The method of claim 1, wherein the thick amorphous alloy film of immiscible metal is prepared by: during the deposition of the alloy film, the substrate stage is rotated at a speed not higher than 60 rmp.
8. Of immiscible metals according to claim 1The preparation method of the amorphous alloy thick film is characterized by comprising the following steps: in the alloy film deposition process, the working gas pressure is 1.0 x 10 -2 Pa-5.0×10 -2 Pa。
9. The method of claim 1, wherein the thick amorphous alloy film of immiscible metal is prepared by: the thickness of the prepared amorphous alloy thick film of the immiscible metal is not less than 10 mu m.
10. The method of claim 1, wherein the thick amorphous alloy film of immiscible metal is prepared by: calculating the mass percentages of various metals required by the target according to the components of the prepared target amorphous alloy thick film, calculating the angle of a fan-shaped part required by each metal on the circular target according to the mass percentages, and splicing the immiscible metals into the target.
CN202210424640.XA 2022-04-21 2022-04-21 Preparation method of amorphous alloy thick film of immiscible metal Pending CN114807875A (en)

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