CN114752892A - Platinum film with super-large crystal grains and preparation method thereof - Google Patents

Platinum film with super-large crystal grains and preparation method thereof Download PDF

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Publication number
CN114752892A
CN114752892A CN202210262574.0A CN202210262574A CN114752892A CN 114752892 A CN114752892 A CN 114752892A CN 202210262574 A CN202210262574 A CN 202210262574A CN 114752892 A CN114752892 A CN 114752892A
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oxygen
heat treatment
film
platinum
platinum film
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蒲健
陈茂
冯江涛
池波
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Jiangsu Jingporcelain Intelligent Sensing Technology Research Institute Co ltd
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Jiangsu Jingporcelain Intelligent Sensing Technology Research Institute Co ltd
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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
    • C23C14/06—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
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • 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
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

The invention relates to the technical field of films, in particular to a platinum film with super-large crystal grains and a preparation method thereof. The platinum film is prepared by using a conventional magnetron sputtering method, the mixed gas of argon and oxygen is used as a sputtering carrier gas, the content of the oxygen in the mixed gas of argon and oxygen during sputtering is adjusted, the oxygen content in the deposited platinum film is further adjusted, the subsequent heat treatment temperature and heat treatment atmosphere of the film are matched, and the surface energy and strain energy of the film in the growth process of crystal grains are mainly adjusted, so that the crystal grains with specific orientation have the growth advantages in thermodynamics or kinetics at a certain stage of heat treatment, thereby continuously consuming surrounding small crystal grains and growing abnormally until the abnormally grown crystal grains are contacted with each other, and finally the platinum film with large crystal grain size and uniform crystal grain distribution is obtained. The preparation method is simple, and the prepared platinum film has few structural defects and excellent electrical properties.

Description

Platinum film with super-large crystal grains and preparation method thereof
Technical Field
The invention relates to a film, in particular to a platinum film with super large crystal grains and a preparation method thereof.
Background
Whether for bulk or thin film materials, grain size has a significant impact on the electrical, magnetic, force, optical, etc. properties of the material. The single crystal thin film has important application in the fields of semiconductor industry, integrated circuits and the like. Single crystal thin films typically require the use of a single crystal substrate and are produced using epitaxial techniques, but epitaxial equipment is typically expensive and epitaxial methods have limited choices for substrate materials, typically requiring a difference in lattice size between the film and the substrate of less than 15%, and furthermore, single crystal substrates are typically produced by melt-pulling-cutting-polishing, which is costly to manufacture.
In some applications, the substrate material requirements for single crystal thin films are reduced and it is desirable to obtain thin films with large size grains. For example, in a platinum film resistance temperature sensor, in order to prepare a high-precision sensor, a platinum film with few structural defects such as grain boundaries, dislocations and micro-holes needs to be prepared, and the conventional physical vapor deposition methods such as evaporation, sputtering and the like determine that the prepared deposited film contains a large amount of structural defects such as grain boundaries, dislocations and micro-holes due to the principle limitation of gas-solid phase transition. Although these defects are substantially reduced by suitable heat treatment, a significant number of defects remain, particularly at the grain boundaries, the grain size of the film is generally limited by its thickness, with a maximum grain size having a distribution comparable to and uniform with its thickness. In order to obtain larger size grains, i.e., lower grain boundary density, the thickness of the film may be increased, however, platinum is a noble metal, and increasing the thickness of the platinum film is disadvantageous for reducing material costs.
The driving force for the grain growth of the film comes from the reduction of the total energy of the film-substrate system, and the system energy formed by the film and the substrate mainly comprises the following components: surface energy, interface energy, grain boundary energy, and strain energy. In a thin film having a crystal structure, the above energies all have anisotropy. In face centered cubic, (111) face generally has the lowest surface energy, for body centered cubic and hexagonal close packing, (110) face and (0002) face, respectively; the strain energy depends on the magnitude of the strain and the elastic modulus of the material, which is related to the crystal orientation, with the [100] direction having the smallest elastic modulus in face-centered cubic crystals; the interfacial energy is also related to the substrate, both the substrate orientation and the film orientation if the substrate is crystalline, and mainly to the in-plane orientation of the film if the substrate is amorphous.
In the process of growing the film crystal grains, in order to minimize the total energy, sometimes some crystal grains with specific orientation have thermodynamic or kinetic growth advantages due to external conditions, thereby consuming small crystal grains around the crystal grains to grow abnormally and grow into oversized crystal grains.
Disclosure of Invention
The invention aims to solve the defects and provides a platinum film with super large crystal grains and a preparation method thereof.
In the present invention, a platinum thin film is produced using a conventional magnetron sputtering method, but a mixed gas of argon and oxygen is used as a sputtering carrier gas. After sputtering is complete, oxygen can dissolve in the platinum metal or form platinum oxides and primarily affect the surface energy and strain energy of the as-deposited film. In the subsequent heat treatment process, oxygen dissolved in platinum crystal lattices is desolventized from the platinum film and escapes from the platinum film, the platinum oxide is also subjected to thermal decomposition, and metal platinum is precipitated, and the surface energy and the strain energy of the film are also influenced by the process. The oxygen content of the deposited platinum film is adjusted by adjusting the oxygen content in the mixed gas of argon and oxygen during sputtering, and the oxygen content is matched with subsequent heat treatment, so that the surface energy and the strain energy of the film in the growth process of crystal grains are mainly adjusted, and the crystal grains with specific orientation have the growth advantage in the aspect of thermodynamics or kinetics at a certain stage of the heat treatment, thereby continuously consuming the surrounding small crystal grains and growing abnormally until the abnormally grown crystal grains are contacted with each other, and further the platinum film with large crystal grain size and uniform crystal grain distribution is obtained.
In order to overcome the defects in the background art, the technical scheme adopted by the invention for solving the technical problems is as follows: an oversized-grain platinum film comprises a ceramic substrate; depositing one or more oxygen-containing platinum thin films on the ceramic substrate.
According to another embodiment of the invention, the ceramic substrate is polycrystalline alumina ceramic or single crystal alumina ceramic with the mass percentage of 96% -99%.
According to another embodiment of the invention, the oxygen-containing platinum film is prepared by a magnetron sputtering method, and a sputtering carrier gas is a mixed gas of argon and oxygen.
According to another embodiment of the invention, the mixed gas of argon and oxygen further comprises oxygen with the volume fraction of 0% -100%.
According to another embodiment of the invention, the method further comprises the step of forming an oxygen concentration gradient between two adjacent oxygen-containing platinum films.
The preparation method of the platinum film comprises the following steps:
s1, depositing one or more oxygen-containing platinum films on the alumina substrate;
s2, the oxygen-containing platinum thin film is subjected to heat treatment.
The preparation method of the platinum film comprises the following steps:
s1, depositing a layer of oxygen-containing platinum film on the alumina substrate;
s2, carrying out heat treatment on the oxygen-containing platinum film;
s3, depositing one or more oxygen-containing platinum films on the oxygen-containing platinum films after the heat treatment;
s4, carrying out heat treatment on the oxygen-containing platinum film;
the steps S3, S4 may be repeated.
According to another embodiment of the present invention, further comprising the heat treatment temperature is 0.52Tm ~ 0.72Tm，TmThe heat treatment atmosphere is any one of air, argon and nitrogen, which is the melting point of the metal platinum.
According to another embodiment of the present invention, further comprising the heat treatment comprises: the first stage heat treatment temperature is 0.28Tm ~ 0.45TmThe heat treatment atmosphere is oxygen or airGas; the second stage heat treatment temperature is 0.45Tm ~ 0.72TmThe heat treatment atmosphere is any one of air, argon and nitrogen, wherein TmIs the melting point of platinum metal.
The invention has the beneficial effects that:
(1) the platinum film prepared by the method has compact film layer, large grain size, few structural defects such as grain boundary, dislocation, micropore and the like, and excellent electrical properties;
(2) the method does not need a single crystal substrate, and can be completed by using a polycrystalline substrate, but the method provided by the invention is compatible with the single crystal substrate;
(3) the preparation method is simple, and only the conventional sputtering carrier gas argon is changed into the mixed gas of argon and oxygen by using the conventional magnetron sputtering method; the heat treatment method of the invention is simple, only needs to adjust the conventional heat treatment temperature and heat treatment atmosphere, and can complete all the process flows of the preparation of the required platinum film by using only one device in some sputtering and heat treatment integrated devices.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic view of example 1 of the present invention;
FIG. 2 is a schematic view of embodiment 1 of the present invention;
FIG. 3 is a schematic view of embodiment 2 of the present invention;
FIG. 4 is a schematic view of example 2 of the present invention;
FIG. 5 is a schematic view of example 2 of the present invention;
FIG. 6 is a schematic view of embodiment 2 of the present invention;
FIG. 7 is a schematic view of embodiment 3 of the present invention;
FIG. 8 is a schematic view of embodiment 3 of the present invention;
FIG. 9 is a corresponding low power electron microscope image of FIG. 2;
FIG. 10 is a high power electron microscope image corresponding to FIG. 2;
FIG. 11 is a corresponding low power electron microscope image of FIG. 6;
FIG. 12 is a high power electron micrograph corresponding to FIG. 6.
Wherein: 101 is an alumina substrate, 102 is an oxygen-containing platinum film, 103 is a super-large-grained platinum film prepared in example 1 of the present invention, 201 is an alumina substrate, 202 is a first oxygen-containing platinum film, 203 is a film obtained by heat-treating the first oxygen-containing platinum film 202, 204 is a second oxygen-containing platinum film, 205 is a super-large-grained platinum film prepared in example 2 of the present invention, 301 is an alumina substrate, 302 is a first oxygen-containing platinum film, 303 is a second oxygen-containing platinum film, 304 is a third oxygen-containing platinum film, and 305 is a super-large-grained platinum film prepared in example 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A platinum film with super large crystal grains comprises a ceramic substrate; and depositing one or more oxygen-containing platinum films on the ceramic substrate.
The ceramic substrate is polycrystalline alumina ceramic or single crystal alumina ceramic with the mass percentage of 96-99%.
The oxygen-containing platinum film is prepared by a magnetron sputtering method, and the sputtering carrier gas is a mixed gas of argon and oxygen.
In the mixed gas of argon and oxygen, the volume fraction of the oxygen is 0-100%.
An oxygen concentration gradient exists between two adjacent oxygen-containing platinum films.
A preparation method of a platinum film comprises the following steps:
s1, depositing one or more oxygen-containing platinum films on the alumina substrate;
s2, the oxygen-containing platinum thin film is subjected to heat treatment.
Another platinum film preparation method comprises the following steps:
s1, depositing a layer of oxygen-containing platinum film on the alumina substrate;
s2, carrying out heat treatment on the oxygen-containing platinum film;
s3, depositing one or more oxygen-containing platinum films on the oxygen-containing platinum films after the heat treatment;
s4, carrying out heat treatment on the oxygen-containing platinum film;
wherein the steps S3, S4 can be repeated.
Preferably, the heat treatment temperature is 0.52Tm ~ 0.72Tm，TmThe heat treatment atmosphere is any one of air, argon and nitrogen, which is the melting point of the metal platinum.
In a preferred embodiment, the heat treatment comprises: the first stage heat treatment temperature is 0.28Tm ~ 0.45TmThe heat treatment atmosphere is oxygen or air; the second stage heat treatment temperature is 0.45Tm ~ 0.72TmThe heat treatment atmosphere is any one of air, argon and nitrogen, wherein TmThe melting point of metallic platinum.
Example 1
The embodiment provides a method for preparing a platinum film with an oversized crystal grain, which comprises the following steps:
s1, providing a ceramic substrate 101, and depositing an oxygen-containing platinum film 102 on the ceramic substrate;
s2, carrying out heat treatment on the oxygen-containing platinum film 102 to obtain a platinum film 103 with super large crystal grains.
In step S1, the oxygen-containing platinum film 102 is prepared by a magnetron sputtering method, and the sputtering carrier gas is a mixed gas of argon and oxygen, wherein the volume fraction of the oxygen is 0% to 10%.
In step S2, the heat treatment atmosphere is air, and the heat treatment temperature is 800-1100 ℃.
Example 2
The embodiment provides a method for preparing a platinum film with super-large crystal grains, which comprises the following steps: the method comprises the following steps:
s1, providing a ceramic substrate 201, and depositing an oxygen-containing platinum film 202 on the ceramic substrate;
s2, carrying out heat treatment on the oxygen-containing platinum film 202 to obtain a film 203 after the heat treatment of the film 202;
s3, depositing a layer of oxygen-containing platinum film 204 on the film 203 after the heat treatment;
s4, carrying out heat treatment on the films 203 and 204 to obtain the platinum film 205 with super large crystal grains.
In step S1, the oxygen-containing platinum film 202 is prepared by a magnetron sputtering method, and the sputtering carrier gas is a mixed gas of argon and oxygen, wherein the volume fraction of the oxygen is 30% to 50%.
In step S2, the heat treatment temperature is 900-1100 ℃, and the heat treatment atmosphere is air.
In step S3, the oxygen-containing platinum film 204 is prepared by a magnetron sputtering method, and the sputtering carrier gas is a mixed gas of argon and oxygen, wherein the volume fraction of the oxygen is 0% to 10%.
In step S4, the heat treatment process is divided into two stages, wherein the heat treatment temperature of the first stage is 400-600 ℃, and the heat treatment atmosphere is air; the temperature of the second stage heat treatment is 800-1100 ℃, and the heat treatment atmosphere is air or argon.
Example 3
The embodiment provides a method for preparing a platinum film with super-large crystal grains, which comprises the following steps: the method comprises the following steps:
s1, providing a ceramic substrate 301, depositing a first oxygen-containing platinum film 302 on the ceramic substrate:
s2, depositing a second oxygen-containing platinum film 303 on the first oxygen-containing platinum film 302;
s3, depositing a third oxygen-containing platinum film 304 on the second oxygen-containing platinum film 303;
s4, heat-treating the films 302, 303 and 304 to obtain the platinum film 305 with ultra-large crystal grains.
In step S1, the first oxygen-containing platinum film 302 is prepared by a magnetron sputtering method, and the sputtering carrier gas is a mixed gas of argon and oxygen, wherein the volume fraction of the oxygen is 20% to 40%.
In step S2, the second oxygen-containing platinum film 303 is prepared by a magnetron sputtering method, and the sputtering carrier gas is a mixed gas of argon and oxygen, wherein the volume fraction of the oxygen is 0% to 10%.
In step S3, the third oxygen-containing platinum film 304 is prepared by a magnetron sputtering method, and the sputtering carrier gas is a mixed gas of argon and oxygen, wherein the volume fraction of the oxygen is 20-40%.
In step S4, the heat treatment process is divided into two stages, wherein the heat treatment temperature of the first stage is 400-600 ℃, and the heat treatment atmosphere is oxygen; the temperature of the second stage heat treatment is 800-1000 ℃, and the heat treatment atmosphere is air or argon.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (9)

1. A platinum film with super large crystal grains is characterized by comprising a ceramic substrate; depositing one or more oxygen-containing platinum thin films on the ceramic substrate.
2. The ultra-large grain platinum film of claim 1, wherein the ceramic substrate is a polycrystalline alumina ceramic or a single crystal alumina ceramic in a mass percent of 96-99%.
3. The ultra-large grain platinum film of claim 1, wherein: the oxygen-containing platinum film is prepared by a magnetron sputtering method, and sputtering carrier gas is mixed gas of argon and oxygen.
4. The very large grain platinum film of claim 3, wherein the volume fraction of oxygen in said argon and oxygen mixture is in the range of 0% to 100%.
5. The ultra-large grained platinum film of claim 1, wherein an oxygen concentration gradient exists between two adjacent oxygen-containing platinum films.
6. The method for producing a platinum thin film according to any one of claims 1 to 5, comprising the steps of:
s1, depositing one or more oxygen-containing platinum films on the alumina substrate;
s2, the oxygen-containing platinum thin film is subjected to heat treatment.
7. The method for producing a platinum thin film according to any one of claims 1 to 5, comprising the steps of:
s1, depositing a layer of oxygen-containing platinum film on the alumina substrate;
s2, carrying out heat treatment on the oxygen-containing platinum film;
s3, depositing one or more oxygen-containing platinum films on the oxygen-containing platinum films after the heat treatment;
s4, carrying out heat treatment on the oxygen-containing platinum film;
the steps S3, S4 may be repeated.
8. The method for preparing a platinum thin film according to claim 6 or 7, wherein the heat treatment temperature is 0.52Tm ~ 0.72Tm，TmThe heat treatment atmosphere is any one of air, argon and nitrogen, which is the melting point of the metal platinum.
9. The method for preparing a platinum thin film according to claim 6 or 7, wherein the heat treatment comprises: the first stage heat treatment temperature is 0.28Tm ~ 0.45TmThe heat treatment atmosphere is oxygen or air; the second stage heat treatment temperature is 0.45Tm~ 0.72TmThe heat treatment atmosphere is any one of air, argon and nitrogen, wherein TmIs the melting point of platinum metal.
CN202210262574.0A 2022-03-17 2022-03-17 Platinum film with super-large crystal grains and preparation method thereof Pending CN114752892A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4627902A (en) * 1981-03-24 1986-12-09 Rosemount Engineering Company Limited Method of producing a resistance element for a resistance thermometer
KR19980070383A (en) * 1997-01-07 1998-10-26 이재복 A method for forming a platinum thin film having an antioxidant function on a substrate and an electronic device having a platinum thin film formed by the method
US6498097B1 (en) * 1997-05-06 2002-12-24 Tong Yang Cement Corporation Apparatus and method of forming preferred orientation-controlled platinum film using oxygen

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4627902A (en) * 1981-03-24 1986-12-09 Rosemount Engineering Company Limited Method of producing a resistance element for a resistance thermometer
KR19980070383A (en) * 1997-01-07 1998-10-26 이재복 A method for forming a platinum thin film having an antioxidant function on a substrate and an electronic device having a platinum thin film formed by the method
US6498097B1 (en) * 1997-05-06 2002-12-24 Tong Yang Cement Corporation Apparatus and method of forming preferred orientation-controlled platinum film using oxygen

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