CN113736312A - Preparation process of slurry for sintered neodymium iron boron screen printing - Google Patents

Preparation process of slurry for sintered neodymium iron boron screen printing Download PDF

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Publication number
CN113736312A
CN113736312A CN202110881290.5A CN202110881290A CN113736312A CN 113736312 A CN113736312 A CN 113736312A CN 202110881290 A CN202110881290 A CN 202110881290A CN 113736312 A CN113736312 A CN 113736312A
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CN
China
Prior art keywords
parts
screen printing
slurry
rare earth
hydride
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Pending
Application number
CN202110881290.5A
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Chinese (zh)
Inventor
张震
刘竞成
徐娟
陈翔
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Anhui Hanhai New Material Co ltd
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Anhui Hanhai New Material Co ltd
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Priority to CN202110881290.5A priority Critical patent/CN113736312A/en
Publication of CN113736312A publication Critical patent/CN113736312A/en
Priority to PCT/CN2022/109682 priority patent/WO2023011462A1/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/10Printing inks based on artificial resins
    • C09D11/106Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C09D11/107Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder

Abstract

The invention provides a paste manufacturing process for sintered neodymium iron boron screen printing, and relates to the technical field of screen printing. The method comprises the following steps: reacting fluoride R1F3And hydride R2H3Crushing into powder, uniformly mixing to obtain a powder mixture, dissolving the powder mixture in a solvent, and then sequentially adding a defoaming agent and a high polymer resin to prepare the heavy rare earth suspension slurry. The slurry prepared by the process has strong adhesive force, short drying time after printing, no screen blockage during printing, greatly improved coercive force of the neodymium iron boron, low equipment cost and suitability for industrial batch production, and simultaneously achieves the effects of magnetron sputtering and coating.

Description

Preparation process of slurry for sintered neodymium iron boron screen printing
Technical Field
The invention relates to the technical field of screen printing, in particular to a preparation process of paste for screen printing of sintered neodymium iron boron.
Background
The silk screen printing belongs to orifice plate printing, wherein screen glue is utilized to seal redundant screen gauze areas, required figures or characters are reserved, and printing ink is printed on a printing stock through holes of an orifice plate through certain pressure to form the required figures or characters. The screen printing is cheap, has relatively long retention period, is accepted by more and more industries, and has wide application.
The printing stock commonly used in the prior art comprises base materials such as glass, paper, plastics, metal and the like, and mainly adopts solvent type ink, wherein the ink is mainly prepared by mixing resin, pigment, solvent, auxiliary agent and the like, and then various patterns and characters are printed on the printing stock through a silk screen.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a slurry manufacturing process for screen printing of sintered neodymium iron boron, which takes the sintered neodymium iron boron as a printing stock, carbon cannot enter a neodymium iron boron magnet to cause product deterioration, the adhesive force of the slurry is strong, the drying time after printing is short, a screen printing plate is not blocked during printing, the coercive force of the neodymium iron boron can be greatly improved, the effects of magnetron sputtering and coating are achieved, the equipment cost is low, and the process is suitable for industrial batch production.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a manufacturing process of slurry for screen printing of sintered neodymium iron boron comprises the following steps:
(1) reacting fluoride R1F3And hydride R2H3Crushing into powder, uniformly mixing to obtain a powder mixture, dissolving the powder mixture in a solvent, and then sequentially adding a defoaming agent and a high polymer resin to prepare the heavy rare earth suspension slurry.
R1 is one of Tb, Dy and Ho;
r2 is one of Tb, Dy and Ho;
preferably, the defoaming agent is propylene glycol block polyether, the polymer resin is acrylic resin, and the solvent is absolute ethyl alcohol.
Preferably, the heavy rare earth suspension slurry is prepared from the following raw materials in parts by weight: fluoride R1F32-6 parts of hydride R2H32-6 parts of propylene glycol block polyether, 5-10 parts of propylene glycol block polyether, 8-20 parts of acrylic resin and 50-80 parts of absolute ethyl alcohol.
Preferably, the solid content of the heavy rare earth suspension slurry is 50-95%.
Preferably, fluoride R1F3And hydridesR2H3The particle size of the powder of (2) is 1.5 to 5 μm.
According to the invention, by adding the acrylic resin and the fluoride and hydride containing the heavy rare earth element, the adhesive force of the heavy rare earth suspension slurry to the sintered neodymium iron boron of the printing stock can be improved, and the effects of magnetron sputtering and coating on the sintered neodymium iron boron can be achieved. The fluoride and the hydride can also change the dispersion degree and the surface activity of a system, increase the specific surface area, refine crystal grains and further improve the coercive force of the sintered neodymium iron boron magnetic steel. The addition of the acrylic resin has the advantages of high curing speed and high hardness of a formed film, and is also a connecting material in the whole system. The addition of the defoaming agent propylene glycol block polyether can effectively inhibit and eliminate the foam generated in the preparation of heavy rare earth suspension slurry and printing, so that the whole operation is smoothly carried out.
Compared with the prior art, the invention has the following beneficial effects:
(1) the heavy rare earth suspension slurry provided by the invention has the advantages that the drying time after printing is short, a screen printing plate is not blocked during printing, and the adhesive force of the slurry is strong;
(2) after the heavy rare earth suspension slurry prepared by the invention is used for screen printing, carbon cannot enter the neodymium iron boron magnet to cause product deterioration through high-temperature diffusion and tempering treatment, the coercive force of the neodymium iron boron magnet can be greatly improved, the effects of magnetron sputtering and coating are achieved, and the heavy rare earth suspension slurry is suitable for industrial mass production and application.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further clarified with the specific embodiments.
A manufacturing process of slurry for screen printing of sintered neodymium iron boron comprises the following steps:
(1) reacting fluoride R1F3And hydride R2H3Pulverizing into powder, mixing to obtain powder mixture, dissolving the powder mixture in defoamer, polymer resin and solvent in sequence, and making into tabletRare earth suspension slurry;
r1 is one of Tb, Dy and Ho;
r2 is one of Tb, Dy and Ho;
according to the invention, by adding the acrylic resin, the fluoride containing the heavy rare earth element and the hydride into the system, the adhesive force of the heavy rare earth suspension slurry to the sintered neodymium iron boron of the printing stock can be improved, and the effects of magnetron sputtering and coating on the sintered neodymium iron boron can be achieved. The fluoride and the hydride can also change the dispersion degree and the surface activity of the system, increase the specific surface area and refine grains. The addition of the acrylic resin has the advantages of high curing speed and high hardness of a formed film, and is also a connecting material in the whole system. The addition of the defoaming agent propylene glycol block polyether can effectively inhibit and eliminate the foam generated in the preparation of heavy rare earth suspension slurry and printing, so that the whole operation is smoothly carried out.
In the invention, the high polymer resin is acrylic resin, the weight part of the acrylic resin in the heavy rare earth suspension slurry is 8-20 parts, in the embodiment of the invention, the weight part of the acrylic resin is 8 parts, 12 parts, 16 parts or 20 parts, and the acrylic resin is purchased from a new Weifang Fule material CFW 313.
In the invention, the solvent is 50-80 parts by weight of absolute ethyl alcohol, and in the embodiment, the weight parts of the absolute ethyl alcohol are 55 parts, 60 parts, 66 parts or 70 parts.
In the invention, fluoride R1F containing heavy rare earth element and hydride are used as components to prepare heavy rare earth suspension slurry3And hydride R2H3Pulverizing to powder with particle diameter of 1.5-5 μm, wherein the fluoride R1F32-6 parts of hydride R2H32-6 parts, in the embodiment of the invention, the particle size is crushed to 1.8 μm, the selected fluoride is terbium fluoride, dysprosium fluoride and holmium fluoride, the selected hydride is terbium hydride, dysprosium hydride and holmium hydride, the weight parts of the fluoride are 2 parts, 4 parts or 6 parts, and the weight parts of the hydride are 2 parts, 4 parts or 6 parts.
In the invention, the defoaming agent is propylene glycol block polyether, which is mainly used for eliminating foam in a system and is 5-10 parts by weight, and in the embodiment, the propylene glycol block polyether is 6 parts by weight.
In the invention, the fixed pattern can be selected according to actual requirements, and characters or figures can be selected.
According to the invention, after the heavy rare earth suspension slurry is printed on the surface of the sintered neodymium iron boron magnetic steel through the fixed pattern, high-temperature diffusion and tempering treatment are carried out, so that the coercive force of the sintered neodymium iron boron is improved, and no residual carbon exists after high-temperature diffusion, so that carbon cannot enter the neodymium iron boron magnet to cause product deterioration; in the embodiment, the high-temperature diffusion temperature is 800 ℃, 850 ℃ or 900 ℃, the diffusion time is 3 hours, and the tempering temperature is 450 ℃, 480 ℃ or 500 ℃, and the treatment time is 4 hours.
In the following examples terbium fluoride (TbF)3) Dysprosium fluoride (DyF)3) Holmium fluoride (HoF)3) And terbium hydride (TbH)3) Dysprosium hydride (DyH)3) Holmium hydride (HoH)3) Supplied by alatin reagent limited; the propylene glycol block polyether is L61 of Lin Yi national mechanical and chemical industries, Co; acrylic resin is a novel Weifang Fule material CFW313, and the sintered neodymium iron boron magnetic steel is N35 and is provided by Shanghai Emhao magnetic material Co.
Example 1
(1) Crushing 2 parts of dysprosium fluoride and 2 parts of terbium hydride into powder, uniformly mixing to obtain a powder mixture, dissolving the powder mixture in 55 parts of absolute ethyl alcohol, and then adding 6 parts of propylene glycol block polyether and 8 parts of acrylic resin to prepare heavy rare earth suspension slurry;
(2) and printing the heavy rare earth suspension slurry on the surface of the sintered neodymium-iron-boron magnetic steel through a fixed pattern, diffusing for 3h at 800 ℃, and then tempering for 4h at 450 ℃.
Example 2
(1) Crushing 2 parts of dysprosium fluoride and 4 parts of terbium hydride into powder, uniformly mixing to obtain a powder mixture, dissolving the powder mixture in 60 parts of absolute ethyl alcohol, and then adding 6 parts of propylene glycol block polyether and 12 parts of acrylic resin to prepare heavy rare earth suspension slurry;
(2) and printing the heavy rare earth suspension slurry on the surface of the sintered neodymium-iron-boron magnetic steel through a fixed pattern, diffusing for 3h at 850 ℃, and then tempering for 4h at 480 ℃.
Example 3
(1) Crushing 4 parts of dysprosium fluoride and 4 parts of terbium hydride into powder, uniformly mixing to obtain a powder mixture, dissolving the powder mixture in 66 parts of absolute ethyl alcohol, and then adding 6 parts of propylene glycol block polyether and 16 parts of acrylic resin to prepare heavy rare earth suspension slurry;
(2) and printing the heavy rare earth suspension slurry on the surface of the sintered neodymium-iron-boron magnetic steel through a fixed pattern, diffusing for 3h at 850 ℃, and then tempering for 4h at 480 ℃.
Example 4
(1) Crushing 6 parts of dysprosium fluoride and 4 parts of terbium hydride into powder, uniformly mixing to obtain a powder mixture, dissolving the powder mixture in 70 parts of absolute ethyl alcohol, and then adding 6 parts of propylene glycol block polyether and 20 parts of acrylic resin to prepare heavy rare earth suspension slurry;
(2) and printing the heavy rare earth suspension slurry on the surface of the sintered neodymium-iron-boron magnetic steel through a fixed pattern, diffusing for 3h at 900 ℃, and then tempering for 4h at 500 ℃.
Example 5
(1) Crushing 4 parts of dysprosium fluoride and 6 parts of terbium hydride into powder, uniformly mixing to obtain a powder mixture, dissolving the powder mixture in 70 parts of absolute ethyl alcohol, and then adding 6 parts of propylene glycol block polyether and 20 parts of acrylic resin to prepare heavy rare earth suspension slurry;
(2) and printing the heavy rare earth suspension slurry on the surface of the sintered neodymium-iron-boron magnetic steel through a fixed pattern, diffusing for 3h at 900 ℃, and then tempering for 4h at 500 ℃.
Comparative example 1
(1) Crushing 0.5 part of dysprosium fluoride and 0.5 part of terbium hydride into powder, uniformly mixing to obtain a powder mixture, dissolving the powder mixture in 70 parts of absolute ethyl alcohol, and then adding 6 parts of propylene glycol block polyether and 20 parts of acrylic resin to prepare heavy rare earth suspension slurry;
(2) and printing the heavy rare earth suspension slurry on the surface of the sintered neodymium-iron-boron magnetic steel through a fixed pattern, diffusing for 3h at 900 ℃, and then tempering for 4h at 500 ℃.
Comparative example 2
The comparative example was prepared substantially identically to example 1 except that in step (1) no fluoride and hydride were added and the remaining preparation was unchanged.
In the above examples 1 to 5 and comparative examples 1 to 2, the obtained sintered nd-fe-b with patterns printed thereon, which was subjected to high temperature diffusion and tempering, was subjected to magnetic property test, and the test results are shown in table 1:
TABLE 1 test results of examples 1-5 and comparative examples 1-2
Group of Coercive force (KOe)
Commercial brand N35 11.95
Example 1 13.62
Example 2 15.21
Example 3 16.52
Example 4 17.35
Example 5 17.34
Comparative example 1 13.14
Comparative example 2 12.01
The results show that the coercive force of the sintered neodymium iron boron magnetic steel is really obviously improved after the heavy rare earth suspension slurry prepared by the invention is printed on the sintered neodymium iron boron magnetic steel through a fixed pattern and is subjected to high-temperature diffusion and tempering treatment.
The foregoing shows and describes the general principles, essential features, and inventive features of this invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (5)

1. A manufacturing process of slurry for screen printing of sintered neodymium iron boron is characterized by comprising the following steps: reacting fluoride R1F3And hydride R2H3Crushing into powder, uniformly mixing to obtain a powder mixture, dissolving the powder mixture in a solvent, and then sequentially adding a defoaming agent and a high polymer resin to prepare heavy rare earth suspension slurry;
r1 is one of Tb, Dy and Ho;
r2 is one of Tb, Dy and Ho.
2. The manufacturing process of the paste for screen printing of the sintered neodymium-iron-boron according to claim 1, wherein the defoaming agent is propylene glycol block polyether, the polymer resin is acrylic resin, and the solvent is absolute ethyl alcohol.
3. The sintered NdFeB screen printing of claim 2The slurry preparation process is characterized in that the heavy rare earth suspension slurry comprises the following raw materials in parts by weight: fluoride R1F32-6 parts of hydride R2H32-6 parts of propylene glycol block polyether, 7-10 parts of propylene glycol block polyether, 8-20 parts of acrylic resin and 50-80 parts of absolute ethyl alcohol.
4. The manufacturing process of the paste for screen printing of sintered neodymium-iron-boron according to claim 1, wherein the solid content of the heavy rare earth suspension paste is 50-95%.
5. The manufacturing process of the paste for screen printing of sintered NdFeB as claimed in claim 1, wherein the fluoride R1F3And hydride R2H3The particle size of the powder of (2) is 1.5 to 5 μm.
CN202110881290.5A 2021-08-02 2021-08-02 Preparation process of slurry for sintered neodymium iron boron screen printing Pending CN113736312A (en)

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PCT/CN2022/109682 WO2023011462A1 (en) 2021-08-02 2022-08-02 Preparation process of slurry for sintered neodymium-iron-boron silk-screen printing

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023011462A1 (en) * 2021-08-02 2023-02-09 安徽省瀚海新材料股份有限公司 Preparation process of slurry for sintered neodymium-iron-boron silk-screen printing
CN116504437A (en) * 2023-04-28 2023-07-28 有研稀土新材料股份有限公司 Organic slurry for neodymium-iron-boron screen printing and preparation method thereof

Citations (1)

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Publication number Priority date Publication date Assignee Title
JP2021040010A (en) * 2019-09-02 2021-03-11 Tdk株式会社 Manufacturing method of rare-earth permanent magnet and manufacturing installation of rare-earth permanent magnet

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Publication number Priority date Publication date Assignee Title
CN105472791A (en) * 2015-12-23 2016-04-06 东莞珂洛赫慕电子材料科技有限公司 Rare earth-doped semiconductor infrared radiation thick-film electronic paste and preparation method therefor
CN108630368B (en) * 2018-06-11 2020-09-11 安徽大地熊新材料股份有限公司 Surface coating slurry for high-coercivity neodymium-iron-boron magnet and preparation method of neodymium-iron-boron magnet
CN113736312A (en) * 2021-08-02 2021-12-03 安徽省瀚海新材料股份有限公司 Preparation process of slurry for sintered neodymium iron boron screen printing

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2021040010A (en) * 2019-09-02 2021-03-11 Tdk株式会社 Manufacturing method of rare-earth permanent magnet and manufacturing installation of rare-earth permanent magnet

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023011462A1 (en) * 2021-08-02 2023-02-09 安徽省瀚海新材料股份有限公司 Preparation process of slurry for sintered neodymium-iron-boron silk-screen printing
CN116504437A (en) * 2023-04-28 2023-07-28 有研稀土新材料股份有限公司 Organic slurry for neodymium-iron-boron screen printing and preparation method thereof

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