CN114275745A - Preparation method of copper nitride powder - Google Patents
Preparation method of copper nitride powder Download PDFInfo
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- CN114275745A CN114275745A CN202111472062.9A CN202111472062A CN114275745A CN 114275745 A CN114275745 A CN 114275745A CN 202111472062 A CN202111472062 A CN 202111472062A CN 114275745 A CN114275745 A CN 114275745A
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- copper nitride
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- 229910052802 copper Inorganic materials 0.000 title claims abstract description 64
- 239000010949 copper Substances 0.000 title claims abstract description 64
- -1 copper nitride Chemical class 0.000 title claims abstract description 57
- 239000000843 powder Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000010408 film Substances 0.000 claims abstract description 39
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000004140 cleaning Methods 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000010409 thin film Substances 0.000 claims abstract description 9
- 238000007873 sieving Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000000758 substrate Substances 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000004528 spin coating Methods 0.000 claims description 4
- 239000011345 viscous material Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 25
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 45
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920002120 photoresistant polymer Polymers 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 150000001879 copper Chemical class 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000000231 atomic layer deposition Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/0625—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with copper
-
- 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
- C23C14/0005—Separation of the coating from the substrate
-
- 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
- C23C14/0641—Nitrides
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
-
- 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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive 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
- C23C14/22—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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of copper nitride powder, which comprises the following steps: constructing at least one support layer and at least one sacrificial layer disposed on the support layer, the sacrificial layer configured to be modifiable by a change in an external condition; growing a thin film on the sacrificial layer and growing the thin film; changing the external conditions to modify the sacrificial layer and obtain an independent film; and cleaning and drying the obtained single film, and grinding and sieving to obtain the copper nitride powder. Compared with the prior art, the method has the advantages of low heating temperature, no need of pressurization, low energy consumption, environmental friendliness, simplicity and convenience in operation, strong practicability, high yield and the like, and has a very high application prospect.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a method for preparing copper nitride powder.
Background
The copper nitride not only can be used as a novel semiconductor material and has good photoelectric characteristics, but also can react to generate high-quality copper after heat treatment, the high-quality copper has better conductivity and density, and the copper nitride slurry can form a circuit electrode and a lead structure in the form of a copper conductor precursor by matching with an integrated circuit printing process, so that the copper nitride slurry can be used for manufacturing, packaging and the like of integrated circuit chips. The copper electrode precursor is printed in a copper nitride slurry mode, so that the oxidation effect of air on copper can be reduced, the oxidation resistance of the copper conductor electrode is enhanced, and a high-quality copper conductor is provided. Among them, the copper nitride slurry must have a manufacturing technique of copper nitride powder.
The patent publication of Chinese invention with publication number CN102491290A proposes a method for preparing copper nitride powder, which comprises the following steps: adding copper oxide and copper salt serving as raw materials into a high-pressure-resistant reactor, discharging air in the reactor, simultaneously adding a solvent medium and a nitriding agent into the reactor, heating the reactor to 50-350 ℃, keeping the pressure of the reactor at 0.1-35.0 MPa, reacting for 0.5-5.0 h in the state, reducing the pressure of the reactor to 0-0.5 MPa in the heating state, and separating solid powder to obtain powdery copper nitride. The method is used for preparing the copper nitride powder in a supercritical (near-critical) system, the preparation process is simple, the preparation method has strong applicability to raw materials, and the obtained copper nitride is relatively pure. However, the above method requires a lot of energy and pressurization, and the production process has a certain risk.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention provides a preparation method of copper nitride powder, which is simple in preparation method and low in energy consumption.
The technical scheme is as follows: a method for preparing a nitrided copper powder, comprising:
building a substrate, wherein the substrate comprises at least one supporting layer and at least one sacrificial layer arranged on the supporting layer, and the sacrificial layer is configured to be modified through change of external conditions;
growing a thin film on the sacrificial layer and growing the thin film;
changing the external conditions to modify the sacrificial layer and obtain an independent film;
and cleaning and drying the obtained single film, and grinding and sieving to obtain the copper nitride powder.
Further, the method also comprises the following steps:
and carrying out secondary drying on the sieved copper nitride powder, wherein the secondary drying is carried out in a vacuum or nitrogen environment at the temperature of 50-80 ℃ for 3-10 h.
Further, cleaning the substrate after the substrate is built, comprising the steps of:
and repeatedly washing the deionized water and the organic solvent for 3-5 times, wherein the last washing is deionized water cleaning.
Further, the cleaning mode is flushing or ultrasonic cleaning.
Further, the change of the external conditions includes changing the humidity, the acidity or the alkalinity, or the temperature so that the sacrificial layer loses the original connectivity, and the change of the external conditions includes liquid soaking, heating or cooling.
Further, the sacrificial layer is an oxide or an organic adhesive material, and the change of the external condition includes corrosion or loss of the adhesive material.
Further, the sacrificial layer is constructed by PECVD, oxidation reaction, or spin coating.
Further, the cleaning of the separated individual thin film comprises the following steps:
and repeatedly washing with deionized water and an organic solvent for 3-5 times in sequence, wherein the last washing is deionized water washing.
Further, the method for drying the washed film comprises the following steps:
drying for 3-10h in vacuum or nitrogen environment, and keeping the temperature at 50-80 ℃.
Further, the organic solvent used for washing is an organic solvent such as ethanol, acetone or isopropanol.
Has the advantages that: compared with the prior art, the method has the advantages of low heating temperature, no need of pressurization, low energy consumption, environmental friendliness, simplicity and convenience in operation, strong practicability, high yield and the like, and has a very high application prospect.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the 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.
The invention provides a preparation method of copper nitride powder, which comprises the following steps:
s100, constructing at least one supporting layer and at least one sacrificial layer arranged on the supporting layer, wherein the sacrificial layer is configured to be modified through the change of external conditions;
s200, cultivating a film on the sacrificial layer and growing the film;
s300, changing external conditions to modify the sacrificial layer and obtain an independent film;
s400: and cleaning and drying the obtained single film, and grinding and sieving to obtain the copper nitride powder.
Compared with the prior art, the method has the advantages of low heating temperature, no need of pressurization, low energy consumption, environmental friendliness, simplicity and convenience in operation, strong practicability, high yield and the like, and has a very high application prospect.
Preferably, after step S400, the method further comprises step S401: and carrying out secondary drying on the sieved copper nitride powder, wherein the secondary drying is carried out in a vacuum or nitrogen environment at the temperature of 50-80 ℃ for 3-10 h.
Specifically, the method also comprises a step S101 after the step S100, wherein the substrate is cleaned after being constructed so as to keep the substrate clean, and the method comprises the following steps:
and repeatedly washing the deionized water and the organic solvent for 3-5 times, wherein the last washing is deionized water cleaning. Preferably, the cleaning manner is flushing or ultrasonic cleaning.
In S300, step S301 is further included after step S300: and cleaning the separated single film, repeatedly washing the film for 3-5 times by using deionized water and an organic solvent in sequence, wherein the last washing is deionized water washing. Wherein the organic solvent used for washing is ethanol, acetone or isopropanol.
Further, step S302 is further included after step S301: drying the washed film, comprising the following steps:
drying for 3-10h in vacuum or nitrogen environment, and keeping the temperature at 50-80 ℃.
In S200, the thin film growth method is one of ALD, PECVD, magnetron sputtering, evaporation, spin coating, and other thin film growth methods.
And a functional layer is arranged between the sacrificial layer and the supporting layer and used for realizing heat dissipation and/or high resistance performance.
In a preferred embodiment, the support layer is made of a semiconductor, ceramic or glass.
In a preferred embodiment, the change of the external condition includes changing the humidity, the acidity or the alkalinity or the temperature so that the sacrificial layer loses its original connectivity, and changing the external condition includes soaking in a liquid, heating or cooling in S100.
In a preferred embodiment, the sacrificial layer is an oxide or an organic viscous substance, and the change in external conditions includes corrosion or loss of the viscous substance.
In a preferred embodiment, the sacrificial layer is constructed by PECVD, oxidation reaction or spin-on coating.
In a preferred embodiment, the thickness of the film is not less than 5 nm, and the film material is one of organic or inorganic materials such as semiconductor, ceramic, polymer, etc.
The following will specifically explain the preparation method of copper nitride powder according to the present invention by referring to specific examples:
example 1:
the embodiment provides a method for manufacturing copper nitride powder, in particular to a method for converting a copper nitride film into copper nitride powder. The substrate comprises two layers, a support layer and a sacrificial layer. A commercially available silicon wafer with the thickness of 500 mu m is selected as a supporting layer, silicon oxide with the thickness of 1 mu m is selected as a sacrificial layer, the sacrificial layer is positioned on a top layer, and the supporting layer is positioned on a bottom layer. Wherein the silicon oxide sacrificial layer is obtained after the high-temperature heat treatment of the silicon wafer. The copper nitride film is deposited and grown on the substrate by using a PECVD process, and the film thickness is 0.5 mu m. Before the growth of the copper nitride film, the substrate is repeatedly washed by ethanol and deionized water for 3 times, and the last washing is the washing by the deionized water.
And (3) soaking the substrate with the copper nitride film in hydrofluoric acid solution for 1 h. The sacrificial layer of silicon oxide will be etched away and the copper nitride film will be separated from the support layer. Thus obtaining the separated independent copper nitride film. And fishing out the film by using a hydrofluoric acid resistant Teflon utensil. And repeatedly washing the film with deionized water and an ethanol solvent for 3 times, wherein the last washing is deionized water washing. And then drying the mixture in a vacuum environment of an oven for 3 hours, and keeping the temperature at 50 ℃. The dried film was mechanically ground using a ball mill, and then the grinding balls were mixed with the copper nitride film at a ratio of 8: 1 percent of the grinding aid is put into a ball mill, the mass ratio of the grinding aid is 1 percent of the total mass, the rotating speed is set to be 500rpm, and the grinding is carried out for 1 hour. And stopping the machine for 10 minutes to dissipate heat every 30 minutes of grinding, and keeping the temperature not to exceed 200 ℃. And (3) after grinding, sieving by a 500-mesh sieve to remove grinding balls, then washing the ground copper nitride powder by ethanol and deionized water for 3 times, putting the washed copper nitride powder into a vacuum drying oven for drying at the temperature of 50 ℃ for 3 hours to obtain the finished product of copper nitride powder.
Example 2:
the embodiment provides a method for manufacturing copper nitride powder, in particular to a method for converting a copper nitride film into copper nitride powder. The substrate comprises two layers, a support layer and a sacrificial layer. The method comprises the steps of selecting 175-micron commercially available glass as a supporting layer, selecting 1-micron photoresist as a sacrificial layer, wherein the sacrificial layer is positioned on a top layer, and the supporting layer is positioned on a bottom layer. The photoresist sacrificial layer is obtained through a spin coating process. The copper nitride film is deposited and grown on the substrate by a reactive magnetron sputtering process, and the thickness of the film is 10 mu m. Before the growth of the copper nitride film, the substrate is repeatedly washed by acetone, isopropanol and deionized water for 5 times, and the last washing is deionized water cleaning.
And (3) soaking the substrate with the copper nitride film in an acetone solution for 0.5 h. The sacrificial photoresist layer will be dissolved and the copper nitride film will be separated from the support layer. Thus obtaining the separated independent copper nitride film. Fishing out the film by using a Teflon utensil. The film was repeatedly rinsed 5 times with acetone, isopropanol, deionized water solvent. And drying the mixture in a vacuum environment of an oven for 5 hours, and keeping the temperature at 60 ℃. The mixture was ground by a mortar machine at a set rotation speed of 100rpm for 0.5 hour. After grinding, sieving by a 500-mesh sieve to remove the large-size copper nitride film which is not uniformly ground. And then washing the ground copper nitride powder with acetone, isopropanol and deionized water for 5 times, and drying in a vacuum drying oven at 60 ℃ for 5 hours to obtain the finished product of copper nitride powder.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (10)
1. The preparation method of the copper nitride powder is characterized by comprising the following steps of:
building a substrate, wherein the substrate comprises at least one supporting layer and at least one sacrificial layer arranged on the supporting layer, and the sacrificial layer is configured to be modified through change of external conditions;
growing a thin film on the sacrificial layer and growing the thin film;
changing the external conditions to modify the sacrificial layer and obtain an independent film;
and cleaning and drying the obtained single film, and grinding and sieving to obtain the copper nitride powder.
2. The method for producing copper nitride powder according to claim 1, further comprising the steps of:
and carrying out secondary drying on the sieved copper nitride powder, wherein the secondary drying is carried out in a vacuum or nitrogen environment at the temperature of 50-80 ℃ for 3-10 h.
3. The method for producing copper nitride powder according to claim 1, wherein: cleaning the substrate after the substrate is constructed, comprising the steps of:
and repeatedly washing the deionized water and the organic solvent for 3-5 times, wherein the last washing is deionized water cleaning.
4. The method for producing copper nitride powder according to claim 3, wherein: the cleaning mode is flushing or ultrasonic cleaning.
5. The method for producing copper nitride powder according to claim 1, wherein: the external condition change comprises changing the humidity, the acidity or the alkalinity or the temperature to cause the sacrificial layer to lose the original connectivity, and the external condition change comprises liquid soaking, heating or cooling.
6. The method for producing copper nitride powder according to claim 5, wherein: the sacrificial layer is an oxide or an organic viscous substance, and the change of the external condition includes corrosion or loss of the viscous substance.
7. The method for producing copper nitride powder according to claim 6, wherein: the sacrificial layer is constructed by PECVD, oxidation reaction or spin-coating.
8. The method for producing copper nitride powder according to claim 1, wherein: cleaning the separated single film, comprising the following steps:
and repeatedly washing with deionized water and an organic solvent for 3-5 times in sequence, wherein the last washing is deionized water washing.
9. The method for producing copper nitride powder according to claim 8, wherein: drying the washed film, comprising the following steps:
drying for 3-10h in vacuum or nitrogen environment, and keeping the temperature at 50-80 ℃.
10. The method for producing copper nitride powder according to claim 8, wherein: wherein the organic solvent used for washing is ethanol, acetone or isopropanol.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111472062.9A CN114275745A (en) | 2021-12-06 | 2021-12-06 | Preparation method of copper nitride powder |
| GB2218222.4A GB2615397A (en) | 2021-12-06 | 2022-12-05 | Preparation method of copper nitride powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111472062.9A CN114275745A (en) | 2021-12-06 | 2021-12-06 | Preparation method of copper nitride powder |
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| CN114275745A true CN114275745A (en) | 2022-04-05 |
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| CN202111472062.9A Pending CN114275745A (en) | 2021-12-06 | 2021-12-06 | Preparation method of copper nitride powder |
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| CN116062712A (en) * | 2023-04-04 | 2023-05-05 | 南京邮电大学 | Sodium battery current collector based on thorn-shaped copper nitride and preparation method and application thereof |
| GB2615397A (en) * | 2021-12-06 | 2023-08-09 | Yangtze Delta Region Institute Of Univ Of Electronic Science And Technology Of China Huzhou | Preparation method of copper nitride powder |
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| JP2017135329A (en) * | 2016-01-29 | 2017-08-03 | 国立大学法人東京工業大学 | Copper nitride semiconductor and manufacturing method of the same |
| CN107068607A (en) * | 2017-04-24 | 2017-08-18 | 西安电子科技大学 | Electrode material transfer method based on sacrifice layer |
| CN111009589A (en) * | 2019-11-13 | 2020-04-14 | 浙江师范大学 | Copper nitride thin film solar cell and preparation method thereof |
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| US5135812A (en) * | 1979-12-28 | 1992-08-04 | Flex Products, Inc. | Optically variable thin film flake and collection of the same |
| DE19844357C2 (en) * | 1998-09-28 | 2001-04-05 | Hilmar Weinert | Belt steaming system and process for the production of plane-parallel platelets |
| GB0106059D0 (en) * | 2001-03-13 | 2001-05-02 | Secr Defence | Release films |
| CN114212760A (en) * | 2021-12-06 | 2022-03-22 | 电子科技大学长三角研究院(湖州) | Preparation method of superfine copper nitride powder |
| CN114275745A (en) * | 2021-12-06 | 2022-04-05 | 电子科技大学长三角研究院(湖州) | Preparation method of copper nitride powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2017135329A (en) * | 2016-01-29 | 2017-08-03 | 国立大学法人東京工業大学 | Copper nitride semiconductor and manufacturing method of the same |
| CN107068607A (en) * | 2017-04-24 | 2017-08-18 | 西安电子科技大学 | Electrode material transfer method based on sacrifice layer |
| CN111009589A (en) * | 2019-11-13 | 2020-04-14 | 浙江师范大学 | Copper nitride thin film solar cell and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2615397A (en) * | 2021-12-06 | 2023-08-09 | Yangtze Delta Region Institute Of Univ Of Electronic Science And Technology Of China Huzhou | Preparation method of copper nitride powder |
| CN116062712A (en) * | 2023-04-04 | 2023-05-05 | 南京邮电大学 | Sodium battery current collector based on thorn-shaped copper nitride and preparation method and application thereof |
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| GB202218222D0 (en) | 2023-01-18 |
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