CN100580148C - Process of preparing nano composite sedimentary layer by electroforming - Google Patents

Process of preparing nano composite sedimentary layer by electroforming Download PDF

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Publication number
CN100580148C
CN100580148C CN200610161696A CN200610161696A CN100580148C CN 100580148 C CN100580148 C CN 100580148C CN 200610161696 A CN200610161696 A CN 200610161696A CN 200610161696 A CN200610161696 A CN 200610161696A CN 100580148 C CN100580148 C CN 100580148C
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particle
electromoulding
nanometer
electroforming
nano
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CN101016635A (en
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曲宁松
朱荻
曾永彬
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Shenzhen Hongju Technology Co., Ltd
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Nanjing University of Aeronautics and Astronautics
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Abstract

The invention discloses a preparing craft of nanometer composite sedimentary formation in electromoulding process domain, which comprises the following steps: (a) allocating electromoulding liquid with nanometer particle and inert micrometer particle of diameter at 100-4000 micrometer; setting the mass ratio of micrometer particle total quantity and nanometer particle total quantity at 1:1-20:1; making the total mass of nanometer particle and micrometer particle occupy 1%-30% of casting liquid weight; (b) stirring electromoulding liquid evenly; closing electromoulding electrical source; proceeding nanometer composite layer production; (c) stirring the electromoulding liquid continually in the producing course. This product possesses merits of good compactness, flattening surface and good property. The invention discloses a preparing craft of nanometer composite sedimentary formation in electromoulding process domain, which comprises the following steps: (a) allocating electromoulding liquid with nanometer particle and inert micrometer particle of diameter at 100-4000 micrometer; setting the mass ratio of micrometer particle total quantity and nanometer particle total quantity at 1:1-20:1; making the total mass of nanometer particle and micrometer particle occupy 1%-30% of casting liquid weight; (b) stirring electromoulding liquid evenly; closing electromoulding electrical source; proceeding nanometer composite layer production; (c) stirring the electromoulding liquid continually in the producing course. This product possesses merits of good compactness, flattening surface and good property.

Description

Process of preparing nano composite sedimentary layer by electroforming
Technical field
The technology of the preparing nano composite sedimentary layer by electroforming among the present invention belongs to the electroforming manufacture field.
Background technology
Nano material is made up of superfine crystal grain, and the characteristic dimension size is at the solid material of 0.1~100nm.Nano material has physics and the chemical property different with traditional material such as small-size effect, quantum size effect, macro quanta tunnel effect, surface and interface effect owing to its particular structure.Along with nano material the deepening continuously of aspect researchs such as its development, performance and application, greatly promoted advancing of Materials science research, the appearance of nano particle has simultaneously also brought new opportunity to develop for traditional composite electrodeposition technique.
Nano combined galvanic deposit is in electrodeposition process, and the nano particle of excellent property is joined in the plating bath, makes itself and metal or alloy realize codeposition, and forms the nano-composite plate with some specific function.Nano particle is introduced in the metal plating and given the physics of metal plating with the nano particle uniqueness and the nano combined electro-deposition techniques of chemical property, having opened up the new way of preparation nano composite material, is to have one of research direction of vigor in the nano materials research field.It shows that not only the nano composite material that is prepared by this technology is because the wherein existence of nano particle wild phase, all demonstrate its particular performances at aspects such as hardness, wear resistant friction reducing, internal stress, solidity to corrosion, thermostability, electrocatalysis characteristic and photocatalysis performances, therefore in fields such as machinery, chemical industry, space flight and aviation, automobile, electronics and textile industries extremely wide application prospect is arranged, be embodied in also simultaneously that composite electrodeposition technology tool service temperature is low, less investment, settled layer form advantages such as variation and saving material.
The good performance of nano-composite plate is based upon on the nano particle uniform distribution basis.But nano particle is usually reunited in electroforming solution, normal mechanical stirring, ultrasonic vibration or both the compound alr modes of adopting in the practice, and the method that perhaps adds dispersion agent is come the dispersing nanometer particle.Mechanical stirring is difficult to effective dispersing nanometer particle; Ultrasonic agitation has certain dispersion effect, but in case stop ultrasonic vibration, nano particle is just reunited rapidly, and if in the electroforming process the long-time ultrasonic agitation of using, then can make solution temperature too high, influence the quality of settled layer; Adding dispersion agent in casting liquid can be in the reunion that to a certain degree suppresses nano particle, but dispersion agent constantly consumes in the electroforming process, and its consumption is difficult to calculate, and dispersion agent can be compound to and influences cast layer quality in the cast layer.The reunion how well to solve nano particle in the composite electrodeposition process has become the bottleneck that this technology further develops.
Summary of the invention
The objective of the invention is deficiency, a kind of high-level efficiency, working method that dispersion effect is good and easy and simple to handle are provided at nanoparticulate dispersed method in the existing nano combined deposition technique.
1, a kind of process of preparing nano composite sedimentary layer by electroforming is characterized in that may further comprise the steps:
(a), preparation contains nano particle and diameter is the electroforming solution of the inertia micron particle of 100-4000 micron, and the weight ratio of inertia micron particle total amount and nano particle total amount is 1: 1---20: 1; And nano particle and inertia micron particle gross weight account for 1%~30% of casting liquid weight;
(b), electroforming solution stirred after, connect the electroforming power supply and carry out the manufacturing of nano composite sedimentary layer;
(c), in the electroforming manufacturing processed, constantly stir casting liquid.
It is because can not be compound in the settled layer, thereby the composite deposite that can not form nanometer and micron particle and deposit the performance of reduction coating on the one hand greater than 100 microns particle less than 4000 microns that the inertia micron particle particle diameter of selecting is greater than 100; Large diameter on the other hand particle has big quality, has bigger kinetic energy in the moving process, more can effectively clash into the nano particle of reunion, reaches efficient dispersing nanometer particulate effect.But micron particle can not be greater than 4000 microns, otherwise, because particle remakes into very much the stirring difficulty.Because micron particle compares with nanoparticle, weight is a lot of greatly, and for guaranteeing in the solution enough micron particle quantity is arranged, needing to guarantee to add micron particle total amount in the casting liquid and its weight ratio of total amount of nano particle is 1: 1---20: 1.
Micron particle in the electroforming solution need adopt SiC, Al 2O 3Deng inert particle; Nano particle is used to form nano-composite plate, and the inertia micron particle is used for the dispersing nanometer particle and removes bubble; Under mechanical stirring or ultrasonic vibration or the compound stirring alr mode of both bonded, order about the motion that micron particle does not stop, friction, impact settled layer surface, rapidly, removal is adsorbed bubble and is broken up the nanometer agglomerating particles that is embedded in deposition surface up hill and dale, the nanometer agglomerating particles in their bump casting liquid of not stopping and it is broken up simultaneously, reach effective dispersing nanometer particle, improve nano particle homogeneity in the cast layer, thereby improve the purpose of whole cast layer quality.When micron particle bump nano composite sedimentary layer surface, also play a kind of effect of similar shot peening, make the settled layer surface stress occur, improve the mechanical property of electroformed layer.
Using the present invention can compactness be good to prepare, nanoparticulate dispersed evenly, the electroforming matrix material of surfacing, excellent property.
Description of drawings
Fig. 1 is a preparing nano composite sedimentary layer by electroforming process synoptic diagram.
Label title among Fig. 1: 1, inert particulate particle, 2, nano particle, 3, bubble, 4, nano composite sedimentary layer, 5, negative electrode, 6, the nanometer agglomerating particles on composite sedimentary layer top layer, 7, power supply, 8, anode, 9, the nanometer agglomerating particles in the solution, 10, well heater, 11, temperature controller, 12, temperature sensor, 13, sedimentation tank, 14, electroforming solution.
Embodiment
Implement the present invention---the operating process of " process of preparing nano composite sedimentary layer by electroforming " below in conjunction with Fig. 1 and specific examples explanation.
(1) preparation contains the electroforming solution 14 of nano particle 2 and inertia micron particle 1, and nano particle is used to form nano-composite plate 4, and micron particle is used for the dispersing nanometer particle and removes bubble;
It also can be different types of particle that micron particle and nano particle can be particle of the same race, and the particle diameter of micron particle big (diameter greater than 100 microns less than 4000 microns), and the weight ratio of micron particle total amount and nano particle total amount is 1: 1---20: 1; And nano particle and micron particle gross weight account for 1%~30% of casting liquid weight,
(2) select suitable alr mode (as mechanical stirring, ultrasonic vibration or the compound stirring of both bonded);
(3) by well heater 10, the temperature of the temperature controlling system control electroforming solution 14 that temperature controller 11, temperature sensor 12 are formed;
(4) connect power supply and carry out galvanic deposit, the motion that micron particle 1 does not stop under the ordering about of whipping force, the surface of friction, impact settled layer 4, rapidly, removal is adsorbed bubble 3 and is broken up the nanometer agglomerating particles 6 that is embedded in deposition electricity layer top layer up hill and dale, the nanometer agglomerating particles 9 in their bump casting liquid of not stopping and it is broken up simultaneously, reach effective dispersing nanometer particle, improve nano particle homogeneity in the cast layer, thereby improve the purpose of whole cast layer quality.
Below with deposit N i-ZrO 2Nano-composite plate is an example:
The electroforming solution composition is as follows: nickel sulfamic acid: 400g/L; Nickelous chloride: 15g/L; Boric acid: 30g/L; Nanometer ZrO 2: 20g/L; Micron (particle diameter is 200 microns) SiC:40g/L; Tensio-active agent: an amount of.Select suitable alr mode (as mechanical stirring, ultrasonic vibration or the compound stirring of both bonded) to stir after 1 hour, negative electrode 5, anode 8 are put into electroforming solution, connect power supply 7 beginning galvanic deposit.Proceed to stir the motion that micron SiC 1 is not stopped under the ordering about of whipping force, friction, impact Ni-ZrO in the electrodeposition process 2The surface of nano-composite plate 4 is removed absorption bubble 3 rapidly, up hill and dale and is broken up the nanometer ZrO that is embedded in deposition electricity layer top layer 2Agglomerating particles 6, simultaneously the nanometer ZrO in their bump casting liquid of not stopping 2 Agglomerating particles 9 is also broken up it.Because the particle diameter of micron SiC particle reaches 200 microns, can not be compound in the settled layer, and because its quality is big, the energy that is obtained by stirring is enough big, nano particle and bubble that effective bump is reunited reach efficient dispersing nanometer particle and the effect of removing bubble.Clash into the nano composite sedimentary layer surface at 4 o'clock at micron particle 1, also play a kind of effect of similar shot peening, make the settled layer surface stress occur, improve the mechanical property of electroformed layer.
Whole electroforming process is by well heater 10, the temperature of the temperature controlling system control electroforming solution 14 that temperature controller 11, temperature sensor 12 are formed.

Claims (1)

1, a kind of process of preparing nano composite sedimentary layer by electroforming is characterized in that may further comprise the steps:
(a), preparation contains nano particle and diameter is the electroforming solution of the inertia micron particle of 100-4000 micron, and the weight ratio of inertia micron particle total amount and nano particle total amount is 1: 1---20: 1; And nano particle and inertia micron particle gross weight account for 1%~30% of casting liquid weight;
(b), electroforming solution stirred after, connect the electroforming power supply and carry out the manufacturing of nano composite sedimentary layer;
(c), in the electroforming manufacturing processed, constantly stir casting liquid.
CN200610161696A 2006-12-31 2006-12-31 Process of preparing nano composite sedimentary layer by electroforming Expired - Fee Related CN100580148C (en)

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CN113174622B (en) * 2021-04-29 2023-10-31 北京航空航天大学 Composite coating with micron-sized roughness, preparation method and application

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4039764A1 (en) * 1990-12-13 1992-06-17 Diehl Gmbh & Co Insert for hollow charges - for projectiles produced by chemical or electrolytic deposition
US6660152B2 (en) * 2001-11-15 2003-12-09 The Board Of Trustees Of The University Of Illinois Elemental silicon nanoparticle plating and method for the same
CN1683600A (en) * 2005-02-24 2005-10-19 上海交通大学 Composite electroforming preparing process for nano silicon carbide particle reinforced nickel base composite material
CN1880494A (en) * 2005-06-10 2006-12-20 西安工业学院 High-strength thermal-insulating hybrid particles reinforced aluminum-base composite materials and composite preparation process therefor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4039764A1 (en) * 1990-12-13 1992-06-17 Diehl Gmbh & Co Insert for hollow charges - for projectiles produced by chemical or electrolytic deposition
US6660152B2 (en) * 2001-11-15 2003-12-09 The Board Of Trustees Of The University Of Illinois Elemental silicon nanoparticle plating and method for the same
CN1683600A (en) * 2005-02-24 2005-10-19 上海交通大学 Composite electroforming preparing process for nano silicon carbide particle reinforced nickel base composite material
CN1880494A (en) * 2005-06-10 2006-12-20 西安工业学院 High-strength thermal-insulating hybrid particles reinforced aluminum-base composite materials and composite preparation process therefor

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
复合刷镀纳米Ni-ZrO2高温耐磨性的研究. 张玉峰.电镀与涂饰,第19卷第4期. 2000
复合刷镀纳米Ni-ZrO2高温耐磨性的研究. 张玉峰.电镀与涂饰,第19卷第4期. 2000 *

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