GB2615397A - Preparation method of copper nitride powder - Google Patents

Preparation method of copper nitride powder Download PDF

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Publication number
GB2615397A
GB2615397A GB2218222.4A GB202218222A GB2615397A GB 2615397 A GB2615397 A GB 2615397A GB 202218222 A GB202218222 A GB 202218222A GB 2615397 A GB2615397 A GB 2615397A
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copper nitride
sacrificial layer
nitride powder
preparation
film
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GB202218222D0 (en
Inventor
Yang Chengtao
Xing Mengjiang
Yang Xiaodong
Dai Chuanxiang
Xing Mengdao
Liu Yonghong
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Yangtze River Delta Research Institute of UESTC Huzhou
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Yangtze River Delta Research Institute of UESTC Huzhou
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    • 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

Abstract

A preparation method of a copper nitride powder, comprises the steps of: constructing a sacrificial layer disposed on a support layer, for example a silica sacrificial layer on a silicon wafer or a photoresist sacrificial layer on glass; growing a copper nitride film on the sacrificial layer; changing the external conditions to modify the sacrificial layer and obtain a separate copper nitride film; and cleaning, drying, grinding, and sieving the separate film to obtain the copper nitride powder. Changing the external conditions, e.g. by soaking in a liquid, heating or cooling, can change the humidity, pH or temperature to cause the sacrificial layer to lose the original connectivity thereof. Suitably, the sacrificial layer is an oxide or an organic viscous substance, and the external conditions are changed by etching or losing the viscous substance. The sacrificial layer may be constructed by plasma-enhanced chemical vapour deposition (PECVD), oxidation reaction or spin coating. The separate film may be cleaned by rinsing with deionised water and an organic solvent 3-5 times successively and repeatedly, and finally rinsing with deionised water. The cleaned film may be dried under vacuum or in a nitrogen atmosphere for 3-10 hours at a temperature of 50-80°C.

Description

PREPARATION METHOD OF COPPER NITRIDE POWDER
TECHNICAL FIELD
[0001] The present disclosure relates to the technical field of materials, in particular to a preparation method of a copper nitride powder.
BACKGROUND
[0002] Not only can copper nitride be used as a novel semiconductor material with excellent photoelectric properties, copper nitride will react to form high-quality copper after heat treatment. This high-quality copper has excellent electrical conductivity and density. In the integrated circuit printing process, the copper nitride paste can be used to form circuit electrodes and wire structures in the form of copper conductor precursors, which can be used for integrated circuit chip manufacturing and packaging. Printing copper electrode precursors by means of copper nitride paste can reduce the oxidation effect of air on copper, enhance the oxidation resistance of copper conductor electrodes, and provide high-quality copper conductors. Herein, it is necessary to possess the manufacturing technology of copper nitride powder to manufacture the copper nitride paste.
[0003] Chinese Patent Publication No. CN 102491290A proposes a method for preparing copper nitride powder, including the following steps: adding copper oxide and copper salt as raw materials into a high pressure resistant reactor, exhausting air in the reactor, add adding a solvent medium and a nitridisine agent into the reactor, heat the reactor to 50-350°C, keeping the pressure of the reactor at 0.1-35.0 MPa, and reacting for 0.5-5.0 h in this state, in the heating state; and reducing the pressure in the reactor to be 0-0.5 MPa in a heating state, and separating a solid powder to obtain the copper nitride powder. The copper nitride powder is prepared in a supercritical or near-critical system, the preparation method is simple and has high applicability to the raw materials, and the prepared copper nitride is pure. However, the above method requires a lot of energy and pressure, and the preparation process has certain risks.
SUMMARY
[0004] In order to overcome the defects in the prior art, an objective of the present disclosure is to provide a preparation method of a copper nitride powder featuring a simple preparation method and low energy consumption.
[0005] Technical solution: A preparation method of a copper nitride powder was provided, including: [0006] constructing a substrate, where the substrate comprises at least one support layer and at least one sacrificial layer disposed on the support layer, and the sacrificial layer is configured to be modifiable by changing external conditions; [0007] growing a film on the sacrificial layer; [0008] changing the external conditions to modify the sacrificial layer and obtain a separate film; and [0009] cleaning, drying, grinding, and sieving the separate film obtained to obtain the copper nitride powder.
[0010] Further, the following steps may further be included: [0011] conducting a secondary drying on a sieved copper nitride powder, where the secondary drying is conducted under vacuum or in a nitrogen atmosphere at a temperature of 50-80°C for 3-10 h. [0012] Further, the substrate is cleaned after constructing the substrate, including the following step: [0013] rinsing the substrate with deionised water and an organic solvent 3-5 times repeatedly, and finally rinsing with the deionised water.
[0014] Further, the cleaning may be implemented by rinsing or ultrasonic cleaning.
[0015] Further, changing the external conditions may be intended to change humidity, pll, or temperature to cause the saciificial layer to lose original connectivity thereof, and the external conditions may be changed by soaking in a liquid, heating, or cooling.
[0016] Further, the sacrificial layer may be an oxide or an organic viscous substance, and the external conditions may be changed by etching or losing the viscous substance.
[0017] Further, the sacrificial layer may be constructed by plasma-enhanced chemical vapour deposition (PECVD), oxidation reaction, or spin coating.
[0018] Further, a separate film obtained after separation is cleaned, including the following step: [0019] rinsing the separate film with deionised water and an organic solvent 3-5 times successively and repeatedly, and finally rinsing with the deionised water.
[0020] Further, a cleaned film is dried, including the following step: [0021] drying the cleaned film under vacuum or in a nitrogen atmosphere for 3-10 h, and holding at a temperature of 50-80°C.
[0022] Further, the organic solvent used for rinsing may be ethanol, acetone, or isopropanol. [0023] The present disclosure has the following beneficial effects: In the present disclosure, according to the foregoing method, a freestanding film is obtained, and the film is ground and sieved to obtain the copper nitride powder. Compared with the existing methods, the method has very high application prospects because of the advantages of low heating temperature, no demand for pressurisation, low energy consumption, better environment friendliness, convenient operation strong practicality, and optimal production.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0024] In order to make the objectives, technical solutions, and advantages of the present disclosure clearer, the present disclosure will be further described in detail below in conjunction with examples. It should be understood that the specific examples described herein are merely intended to explain the present disclosure, but not to limit the present disclosure. Based on the examples of the present disclosure, all other examples obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present disclosure.
[0025] The present disclosure provides a preparation method of a copper nitride powder, including: [0026] step S100: constructing at least one support layer and at least one sacrificial layer disposed on the support layer, where the sacrificial layer is configured to be modifiable by changing external conditions; [0027] step S200: growing a film on the sacrificial layer; [0028] step 5300: changing the external conditions to modify the sacrificial layer and obtain a separate film; and [0029] step 5400: cleaning, drying, grinding, and sieving the separate film obtained to obtain the copper nitride powder.
[0030] According to the foregoing method, a freestanding film is obtained, and the film is ground and sieved to obtain the copper nitride powder. Compared with the existing methods, the method has very high application prospects because of the advantages of low heating temperature, no demand for pressurisation, low energy consumption, better environment friendliness, convenient operation, strong practicality, and optimal production.
[0031] Preferably, step S400 may further be followed by step S401: conducting a secondary drying on a sieved copper nitride powder, where the secondary drying may be conducted under vacuum or in a nitrogen atmosphere at a temperature of 50-80°C for 3-10 h. [0032] Specifically, step S100 may further be followed by step S101: the substrate is cleaned to keep the substrate clean after constructing the substrate, including the following step: [0033] rinsing the substrate with deionised water and an organic solvent 3-5 times repeatedly, and finally rinsing with the deionised water. Preferably, the cleaning may be implemented by rinsing or ultrasonic cleaning.
[0034] In step S300, step 5300 may further be followed by step 5301: cleaning a separate film obtained after separation, rinsing the separate film with deionised water and an organic solvent 3-5 times successively and repeatedly, and finally rinsing the separate film with the deionised water. Herein, the organic solvent used for rinsing may be ethanol, acetone, or isopropanol. [0035] Further, step S301 may further be followed by step S302: a cleaned film is dried, including the following step: [0036] drying the cleaned film under vacuum or in a nitrogen atmosphere for 3-10 h, and holding at a temperature of 50-80°C.
[0037] In S200, a film growth method may be one selected from the group consisting of atomic layer deposition (ALD), PECVD, magnetron sputtering, evaporation, and spin coating.
[0038] A functional layer may further be provided between the sacrificial layer and the support layer to achieve heat dissipation and/or high resistance performance.
[0039] In a preferred example, the support layer may be made of semiconductor, ceramic, or glass.
[0040] In a preferred example, in step S100, changing the external conditions may be intended to change humidity, pH, or temperature to cause the sacrificial layer to lose original connectivity thereof, and the external conditions may be changed by soaking in a liquid, heating, or cooling. [0041] In a preferred example, the sacrificial layer may be an oxide or an organic viscous substance, and the external conditions may be changed by etching or losing the viscous substance [0042] In a preferred example, the sacrificial layer may be constructed by PECVD, oxidation reaction, or spin coating.
[0043] In a preferred example, a film growth thickness may be not less than 5 nm, and the film may be made of one material selected from the group consisting of semiconductors, ceramics, polymers, and other organic or inorganic materials.
[0044] The preparation method of a copper nitride powder provided by the present disclosure will be described in detail below with reference to specific examples:
[0045] Example 1:
[0046] This example provided a preparation method of a copper nitride powder, specifically a preparation method for converting a copper nitride film into a copper nitride powder. The substrate contains two layers, a support layer and a sacrificial layer. A commercially available 500 pm silicon wafer was used as the support layer, and 1 pm silica was used as the sacrificial layer. The sacrificial layer was disposed on the top layer, and the support layer was disposed on the bottom layer. Herein, the silica sacrificial layer was obtained after high temperature treatment of the silicon wafer. The copper nitride film was deposited and grown on this substrate by PECVD process, and the film thickness was 0.5 gm. Before the growth of the copper nitride film, the substrate was repeatedly rinsed with ethanol and deionised water three times successively, and finally rinsed with deionised water.
[0047] The substrate on which the copper nitride film was grown was soaked in a hydrofluoric acid solution for 1 h. The silica sacrificial layer was etched and dissolved, and thc copper nitride film was separated from thc support layer. A separate freestanding copper nitride film was obtained. The film was removed with a hydrofluoric acid-resistant Teflon utensil. The film was repeatedly rinsed with deionised water and ethanol solvent three times, and finally rinsed with deionised water. After that, the film was dried in the vacuum environment of an oven for 3 h, and the temperature was held at 50°C. The dried film was mechanically ground using a ball mill, mill balls and the copper nitride film were put into the ball mill at a ratio of 8:1, the grinding aid was put in a mass ratio of 1% of the total mass, and the rotational speed was set to 500 rpm for grinding for 1 h. Herein, every 30 min of grinding, the ball mill was halted for 10 min to dissipate heat, and the temperature was held at not higher than 200°C. After grinding, the mixture was sieved through a 500-mesh sieve to remove the mill balls. Subsequently, the ground copper nitride powder was rinsed with ethanol and deionised water three times successively, placed in a vacuum drying oven and dried at 50°C for 3 h to obtain a finished product of copper nitride powder.
[0048] Example 2:
[0049] This example provided a preparation method of a copper nitride powder, specifically a preparation method for converting a copper nitride film into a copper nitride powder. The substrate contains two layers, a support layer and a sacrificial layer. A piece of commercially available 175 pm glass was used as the support layer, and 1 pm photoresist was used as the sacrificial layer. The sacrificial layer was disposed on the top layer, and the support layer was disposed on the bottom layer. Herein, the photoresist sacrificial layer was obtained by a spin coating process. The copper nitride film was deposited and grown on this substrate by reactive magnetron sputtering process, and the film thickness was 10 pm. Before the growth of the copper nitride film, the substrate was repeatedly rinsed with acetone, isopropanol, and deionised water five times successively, and finally rinsed with deionised water.
[0050] The substrate on which the copper nitride film was grown was soaked in an acetone solution for 0.5 h. The photoresist sacrificial layer was dissolved, and the copper nitride film was separated from the support layer. A separate freestanding copper nitride film was obtained. The film was removed with a Teflon utensil. The film was repeatedly rinsed with acetone, isopropanol, and deionised water five times. After that, the film was dried in the vacuum environment of an oven for 5 h, and the temperature was held at 60°C. Grinding was carried out using a mortar mill, the rotational speed was set to 100 rpm, and the time was set to 0.5 h. After grinding, the mixture was sieved through a 500-mesh sieve to remove the unevenly ground large-sized copper nitride film. Subsequently, the ground copper nitride powder was rinsed with acetone, isopropanol, and deionised water five times successively, placed in a vacuum drying oven and dried at 60°C for 5 h to obtain a finished product of copper nitride powder.
[0051] The above is only the preferred implementation of the present disclosure. It should be noted that: those skilled in the art may make several improvements and modifications departing from the principle of the present disclosure, and these improvements and modifications should also be deemed as falling within the protection scope of the present disclosure.

Claims (10)

  1. CLAIMSI. A preparation method of a copper nitride powder, comprising the following steps: constructing a substrate, wherein the substrate comprises at least one support layer and at least one sacrificial layer disposed on the support layer, and the sacrificial layer is configured to be modifiable by chat-wing external conditions; growing a film on the sacrificial layer; changing the external conditions to modify the sacrificial layer and obtain a separate film; and cleaning, drying, grinding, and sieving the separate film obtained to obtain the copper nitride powder.
  2. 2. The preparation method of a copper nitride powder according to claim 1, further comprising the following steps: conducting a secondary drying on a sieved copper nitride powder, wherein the secondary drying is conducted under vacuum or in a nitrogen atmosphere at a temperature of 50-80°C for 3-10 h.
  3. 3. The preparation method of a copper nitride powder according to claim 1, wherein the substrate is cleaned after constructing the substrate, comprising the following step: rinsing the substrate with deionised water and an organic solvent 3-5 limes repeatedly, and finally rinsing with the deionised water.
  4. 4. The preparation method of a copper nitride powder according to claim 3, wherein the cleaning is implemented by rinsing or ultrasonic cleaning.
  5. 5. The preparation method of a copper nitride powder according to claim 1, wherein changing the external conditions are intended to change humidity, pH, or temperature to cause the sacrificial layer to lose original connectivity thereof, and the external conditions are changed by soaking in a liquid, heating, or cooling.
  6. 6. The preparation method of a copper nitride powder according to claim 5, wherein the sacrificial layer is an oxide or an organic viscous substance, and the external conditions are changed by etching or losing the viscous substance.
  7. 7. The preparation method of a copper nitride powder according to claim 6, wherein the sacrificial layer is constructed by plasma-enhanced chemical vapour deposition (PECVD), oxidation reaction, or spin coating.
  8. 8. The preparation method of a copper nitride powder according to claim 1, wherein a separate film obtained after separation is cleaned, comprising the following step: rinsing the separate film with deionised water and an organic solvent 3-5 titnes successively and repeatedly, and finally rinsing with the deionised water.
  9. 9. The preparation method of a copper nitride powder according to claim 8, wherein: a cleaned film is dried, comprising the following step: drying the cleaned film under vacuum or in a nitrogen atmosphere for 3-10 h, and holding at a temperature of 50-80°C.
  10. 10. The preparation method of a copper nitride powder according to claim 8, wherein the organic solvent used for rinsing is ethanol, acetone, or isopropanol.
GB2218222.4A 2021-12-06 2022-12-05 Preparation method of copper nitride powder Pending GB2615397A (en)

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Publication number Priority date Publication date Assignee Title
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
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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US6270840B1 (en) * 1998-09-28 2001-08-07 Weinert Vakuum Verfahrenstechnik Gmbh Apparatus and method for producing plane-parallel flakes
US20040076819A1 (en) * 2001-03-13 2004-04-22 Pitt Andrew Martin 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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US5135812A (en) * 1979-12-28 1992-08-04 Flex Products, Inc. Optically variable thin film flake and collection of the same
US6270840B1 (en) * 1998-09-28 2001-08-07 Weinert Vakuum Verfahrenstechnik Gmbh Apparatus and method for producing plane-parallel flakes
US20040076819A1 (en) * 2001-03-13 2004-04-22 Pitt Andrew Martin 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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