CN114717555A - Method for forming rare earth oxyfluoride film - Google Patents
Method for forming rare earth oxyfluoride film Download PDFInfo
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- CN114717555A CN114717555A CN202210504745.6A CN202210504745A CN114717555A CN 114717555 A CN114717555 A CN 114717555A CN 202210504745 A CN202210504745 A CN 202210504745A CN 114717555 A CN114717555 A CN 114717555A
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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
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
- C01F17/259—Oxyhalides
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Abstract
The invention discloses a method for forming a rare earth oxyfluoride film, which belongs to the technical field of semiconductor coating preparation and comprises the following steps: providing a gas comprising F ions or C ions or S ions; heating the gas to generate free F ions, and reacting with Y ions in a low-pressure reaction chamber2O3And (3) coating reaction, wherein the pressure of the low-pressure reaction cavity is less than or equal to 101kPa, and the gas temperature after heating pretreatment is 200-1000 ℃. Mixing the pretreated gas with Y2O3The coating reacts to generate the yttrium oxyfluoride film. The yttrium oxyfluoride film prepared by the method has more sufficient reaction, the purity of the obtained yttrium oxyfluoride film is higher, the content of impurities such as heterogeneous yttrium fluoride is less, and the plasma-resistant anticorrosion capability can be enhanced.
Description
Technical Field
The invention belongs to the technical field of semiconductor coating preparation, and particularly relates to a method for forming a rare earth oxyfluoride film.
Background
Currently for reinforcing semiconductor chipsThe capability of the manufacturing equipment for absorbing film and the capability of the manufacturing equipment for resisting plasma corrosion are carried out by adopting a mode of carrying out plasma fusion on an equipment metal base material or a base material anodic oxidation layer to manufacture a rare earth oxide coating. A common coating species is Y2O3、Al2O3And so on. Yttrium oxyfluoride has also been proposed as a material superior to the common rare earth oxides in several patents. But current patents all use YF3And Y2O3Plasma melting is carried out on the mixed powder to prepare the yttrium oxyfluoride coating. The method can be influenced by various factors such as powder proportion, spraying conditions and the like, because the temperature in the process of spraying is high, the inside of the method is easy to react, the purity of the coating is maintained to be low, impurities such as heterogeneous yttrium fluoride and the like can be contained, the heterogeneous yttrium fluoride can be converted into orthorhombic yttrium fluoride by heating in the use environment of plasma etching, and the microcracks on the coating can be increased along with the generation of internal stress in the conversion process, so that the protective performance of the coating is reduced.
Disclosure of Invention
In view of the above, the present invention provides a method for forming a rare earth oxyfluoride thin film, which can improve the purity of a high-purity yttrium oxyfluoride coating, so that the high-purity yttrium oxyfluoride coating has better performance in resisting plasma corrosion.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention discloses a method for forming a rare earth oxyfluoride film, which is characterized by comprising the following steps of:
providing a gas comprising F ions or C ions or S ions;
heating the gas to generate free F ions, and reacting with Y ions in a low-pressure reaction chamber2O3The coating reacts, the pressure of the low-pressure reaction cavity is less than or equal to 101kPa, and the temperature of the gas after heating pretreatment is 200-1000 ℃;
mixing the pretreated gas with Y2O3The coating reacts to generate the yttrium oxyfluoride film.
Further, the gas comprises F2、CF4And SF6Or a mixed gas of a plurality of kinds.
Further, the gas comprises SF6The pressure of the low-pressure reaction cavity is 101kPa, and the temperature of the gas after the heating pretreatment is 400 ℃.
Further, the gas comprises SF6The pressure of the low-pressure reaction cavity is 0.001-0.1 kPa, and the gas temperature after the heating pretreatment is 200 ℃.
Further, the gas comprises SF6The pressure of the low-pressure reaction cavity is 0.001-0.1 kPa, and the temperature of the gas after the heating pretreatment is 400 ℃.
Further, the mixed gas includes CF4And SF6The composition ratio of the mixed gas is CF4：SF6＝3:7。
Further, heating pretreatment is being gone on with the heating intracavity, through set up inert gas pusher in heating chamber rear end, inert gas pusher passes through inert gas with the mist propelling movement to low pressure reaction chamber.
Further, the flow rate of the mixed gas during the pushing was 50 sccm.
Furthermore, the hardness of the yttrium oxyfluoride film is 710-730 HV, and the porosity is 3.0% -3.2%.
The invention has the beneficial effects that:
the invention provides a method for forming rare earth oxyfluoride film, which provides gas containing F ions, C ions or S ions, and free F ions and Y ions can be combined after high-temperature heating2O3The coating reacts to generate a high-purity yttrium oxyfluoride film, free C ions or S ions can be combined with O ions, so that the reaction is more sufficient, the purity of the obtained yttrium oxyfluoride film is higher, the content of impurities such as heterogeneous yttrium fluoride is lower, and the plasma-resistant anti-corrosion capability can be enhanced.
Additional advantages, objects, and features of the invention will be set forth in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
FIG. 1 is a diagram of an apparatus used in the method of the present invention;
FIG. 2 is a graph comparing purity-related physical property data of thin films of oxyfluoride under various conditions of examples of the present invention;
FIG. 3 is a comparison of the crystal structure uniformity of thin oxyfluoride films under the conditions of the examples of the present invention.
The drawings are numbered as follows: nitrogen gas generator 1, gas loading device 2, gas heating device 3, test piece carrying platform 4, reaction chamber 5 and vacuum pump 6.
Detailed Description
Comparative example YF direct use3And Y2O3The mixed powder was subjected to plasma fusion to produce an yttria coating having a hardness of 550HV, a porosity of 6.0% and a purity of YOF of 51%.
Example 1, providing SF6A gas; heating the gas to generate free F ions, and reacting with Y ions in a low-pressure reaction chamber2O3The coating reacts, the pressure of the low-pressure reaction cavity is 101kPa, and the temperature of the gas after the heating pretreatment is 400 ℃; mixing the pretreated gas with Y2O3The coating reacts to generate the yttrium oxyfluoride film. Heating preliminary treatment is going on in order to heat the intracavity, through set up inert gas pusher in heating chamber rear end, inert gas pusher passes through inert gas with the mist propelling movement extremely low pressure reaction chamber, the mist flow during propelling movement is 50 sccm.
Example 2, providing SF6A gas; heating the gas to generate free F ions, and reacting with Y ions in a low-pressure reaction chamber2O3The coating reacts, the pressure of the low-pressure reaction cavity is 0.001-0.1 kPa, and the coating reactsThe gas temperature after the heating pretreatment is 200 ℃; mixing the pretreated gas with Y2O3The coating reacts to generate the yttrium oxyfluoride film. Heating preliminary treatment is going on in order to heat the intracavity, through set up inert gas pusher in heating chamber rear end, inert gas pusher passes through inert gas with the mist propelling movement extremely low pressure reaction chamber, the mist flow during propelling movement is 50 sccm.
Example 3 providing SF6A gas; heating the gas to generate free F ions, and reacting with Y ions in a low-pressure reaction chamber2O3The coating reacts, the pressure of the low-pressure reaction cavity is 0.001-0.1 kPa, and the temperature of the gas after heating pretreatment is 400 ℃; mixing the pretreated gas with Y2O3The coating reacts to generate the yttrium oxyfluoride film. Heating preliminary treatment is going on in order to heat the intracavity, through set up inert gas pusher in heating chamber rear end, inert gas pusher passes through inert gas with the mist propelling movement extremely low pressure reaction chamber, the mist flow during propelling movement is 50 sccm.
Example 4, providing CF4And SF6The mixed gas has the composition ratio of CF4：SF63: 7; heating the gas to generate free F ions, and reacting with Y ions in a low-pressure reaction chamber2O3The coating reacts, the pressure of the low-pressure reaction cavity is 0.001-0.1 kPa, and the temperature of the gas after heating pretreatment is 1000 ℃; mixing the pretreated gas with Y2O3The coating reacts to generate the yttrium oxyfluoride film. Heating preliminary treatment is going on in order to heat the intracavity, through set up inert gas pusher in heating chamber rear end, inert gas pusher passes through inert gas with the mist propelling movement extremely low pressure reaction chamber, the mist flow during propelling movement is 50 sccm.
TABLE 1
The above is a YOF purity contrast diagram under the conditions of the above examples, XRD is called X-ray diffraction, and the features of the X-ray signal after diffraction are obtained by utilizing the diffraction phenomenon of X-rays in crystals, and the diffraction pattern is obtained by processing. The spectrogram information can be used for determining the phase of a conventional microscope, and obtaining whether defects (dislocation), lattice defects and the like exist in the crystal. The evaluation was performed by XRD peak intensity, and the ratio of peaks belonging to YOF was defined as 100% in total of main peak intensities of the respective components.
As can be seen from Table 1, the most significant effect on the purity of the yttrium oxyfluoride coating is the gas composition used, using SF6The gas is subjected to ion reaction treatment, so that the purity of the yttrium oxyfluoride coating can be greatly improved. The gas has the best effect at 400 ℃, the low pressure has great influence on the purity of the yttrium oxyfluoride coating, but the preparation cost in the low-pressure environment is high, and the best cost performance can be obtained by controlling the pressure between 0.001-0.1 kPa. For F2The control of the gas is also costly and has a limited effect on the purity.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (9)
1. A method for forming a rare earth oxyfluoride film, comprising the steps of:
providing a gas comprising F ions or C ions or S ions;
heating the gas to generate free F ions, and reacting with Y ions in a low-pressure reaction chamber2O3The coating reacts, the pressure of the low-pressure reaction cavity is less than or equal to 101kPa, and the temperature of the gas after heating pretreatment is 200-1000 ℃;
mixing the pretreated gas with Y2O3The coating reacts to generate the yttrium oxyfluoride film.
2. The method for forming a rare earth oxyfluoride film according to claim 1, wherein: the gas comprises F2、CF4And SF6Or a mixed gas of a plurality of kinds.
3. The method for forming a rare earth oxyfluoride thin film according to claim 2, wherein: the gas comprising SF6The pressure of the low-pressure reaction cavity is 101kPa, and the temperature of the gas after the heating pretreatment is 400 ℃.
4. The method for forming a rare earth oxyfluoride thin film according to claim 2, wherein: the gas comprising SF6The pressure of the low-pressure reaction cavity is 0.001-0.1 kPa, and the temperature of the gas after the heating pretreatment is 200 ℃.
5. The method for forming a rare earth oxyfluoride thin film according to claim 2, wherein: the gas comprising SF6The pressure of the low-pressure reaction cavity is 0.001-0.1 kPa, and the temperature of the gas after the heating pretreatment is 400 ℃.
6. The method for forming a rare earth oxyfluoride thin film according to claim 2, wherein: the mixed gas comprises CF4And SF6The composition ratio of the mixed gas is CF4：SF6＝3:7。
7. The method for forming a rare earth oxyfluoride thin film according to any one of claims 2 to 6, wherein: the heating pretreatment is carried out in order to heat the intracavity, through set up inert gas pusher in heating chamber rear end, inert gas pusher passes through inert gas with the mist propelling movement extremely low pressure reaction chamber.
8. The method for forming a rare earth oxyfluoride thin film according to claim 7, wherein: the flow rate of the mixed gas during pushing was 50 sccm.
9. The method for forming a rare earth oxyfluoride thin film according to claim 8, wherein: the yttrium oxyfluoride film has a hardness of 710-730 HV and a porosity of 3.0% -3.2%.
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| CN202210504745.6A CN114717555B (en) | 2022-05-10 | 2022-05-10 | Method for forming rare earth oxyfluoride film |
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| CN202210504745.6A CN114717555B (en) | 2022-05-10 | 2022-05-10 | Method for forming rare earth oxyfluoride film |
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| CN114717555B CN114717555B (en) | 2023-06-13 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003151963A (en) * | 2001-11-16 | 2003-05-23 | Matsushita Electric Ind Co Ltd | Dry-etching method and apparatus |
| CN107532283A (en) * | 2015-03-18 | 2018-01-02 | 恩特格里斯公司 | Object coated with fluorine annealed film |
| JPWO2021124996A1 (en) * | 2019-12-18 | 2021-06-24 |
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- 2022-05-10 CN CN202210504745.6A patent/CN114717555B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003151963A (en) * | 2001-11-16 | 2003-05-23 | Matsushita Electric Ind Co Ltd | Dry-etching method and apparatus |
| CN107532283A (en) * | 2015-03-18 | 2018-01-02 | 恩特格里斯公司 | Object coated with fluorine annealed film |
| JPWO2021124996A1 (en) * | 2019-12-18 | 2021-06-24 |
Non-Patent Citations (1)
| Title |
|---|
| WEI-KAI WANG等: "Plasma Etching Behavior of SF6 Plasma Pre-Treatment Sputter-Deposited Yttrium Oxide Films", 《COATINGS》 * |
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