CN101492830A - Process for producing nano-composite plate of neodymium iron boron material - Google Patents
Process for producing nano-composite plate of neodymium iron boron material Download PDFInfo
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- CN101492830A CN101492830A CNA2008100593730A CN200810059373A CN101492830A CN 101492830 A CN101492830 A CN 101492830A CN A2008100593730 A CNA2008100593730 A CN A2008100593730A CN 200810059373 A CN200810059373 A CN 200810059373A CN 101492830 A CN101492830 A CN 101492830A
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Abstract
The invention provides a method for preparing a nano-composite plating of Nd-Fe-B material. The method is characterized by comprising the following steps: (1) pretreatment of sample surface; (2) preparation of basic plating solution and preparation of composite nano-plating solution by mixing, stirring and ball milling the basic plating solution, nano-powder and a dispersing agent; (3) sealing and plating, namely plating the sample after pretreatment in the basic plating solution; and (4) nano-plating, namely plating the sample after sealing and plating in the composite nano-plating solution while the nano-powder is constantly in a state of excellent dispersion. Compared with the prior art, the method has the advantages that: a two-step plating method is adopted, firstly, the traditional plating solution is used for plating so as to reduce porosity of a plating and improve the bonding force of a basic layer and the plating layer, and then, the composite nano-plating solution is used for plating so as to improve corrosion resistance and abrasion resistance of the composite plating.
Description
Technical field
The present invention relates to a kind of NdFeB material method of coating, relate in particular to a kind of NdFeB material method of coating that has nanometer powder in the plating bath that adopts.
Background technology
Nd-Fe-Bo permanent magnet material with its excellent magnetism energy, high cost performance, has been applied to each industrial circle rapidly since nineteen eighty-three comes out.But, because rear earth element nd standard oxidationreduction potential-2.431V is very easily oxidized.Quicken its corrosion process, thereby seriously influenced the magnetic property of magnet.Therefore the NdFeB permanent magnet exists the shortcoming of corrosion resisting property difference, is seriously influencing its application in every respect.Improve its solidity to corrosion and become one of gordian technique in current NdFeB permanent magnet material and product manufacturing and the exploitation.
Domestic common plant-scale neodymium iron boron surfacecti proteon treatment process is for electroplating and electroless plating methods such as physical vapor deposition at present.Wherein electroplate equipment requirements not highly, processing condition are easier to satisfy, and film forming speed is fast, low price, the advantage that is easy to produce in enormous quantities and obtained using widely in industry member.
At present, electronickelling enjoys favor because of advantage such as high temperature resistant, anti-oxidant, that solidity to corrosion is good.But the standard equilibrium potential of nickel layer is-0.25V, is cathodic electrodeposition coating with respect to neodymium iron boron, only when coating is perfect, could play the effect of mechanical protection to matrix.Referring to " material protection " the 35th volume the 3rd interim " sintering type Nd iron boron electronickelling technology " literary composition; the electronickelling scheme of several routines is disclosed; obtained certain effect; but can also do bigger improvement; to improve every performance of product, similarly can also be with reference to " material protection " the 36th volume the 6th interim " research of surface of Nd-Fe-B permanent magnet nickel plating technology " literary composition.
In recent years, many scientists comprised to nano material that nano-composite coating had produced great interest.Nano combined coating technology is exactly a kind of process for treating surface that grows up on traditional plating basis.By in solution, adding nano powder, prepare nano-composite coating with the method for electrochemical deposition, thereby have the compound coating of sedimentary metal and the dual performance of inert particulate.For example, codeposition Ni and Al on iron and steel
2O
3Nanoparticle, the Ni/Al that obtains
2O
3Composite deposite has not only improved abrasive forces, high temperature resistant and oxidation-resistance, has also improved its corrosion resistance nature significantly.
Also there is on Nd-Fe-B permanent magnet the nano-composite coating of plating can make its performance excellent more, with reference to publication number is CN1924110A, denomination of invention is " a kind of metal-based nano composite plating method that is used for the Nd-Fe-B material antiseptic ", and this application has been added nanometer additive to improve the corrosion resistance nature of material in half light nickel plating.Because this patent is directly carried out compound plating, can influence the bonding force of matrix and coating.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of process for producing nano-composite plate of neodymium iron boron material in addition at the above-mentioned state of the art, this method is by the twice different plating in front and back, has higher hardness, anti-corrosion and wear resisting property preferably to guarantee the gained NdFeB material.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: process for producing nano-composite plate of neodymium iron boron material is characterized in that comprising the steps:
1. the pre-treatment of sample surfaces;
2. distinguish configure base plating bath and composite Nano plating bath, the preparation of composite Nano plating bath is to make through stirring and ball milling after basic plating bath, nanometer powder and the dispersant;
3. sealing of hole plating: get sample plating in basic plating bath that pre-treatment finishes;
4. nanometer plating: get sample that the sealing of hole plating finishes in the composite Nano plating bath and guarantee that nanometer powder is in plating under the state of good distribution all the time.
The basic plating bath of step described in 2. can be the Watts plating bath.Also can adopt several basic plating bath of mentioning in the prior art to dispose.
As preferably, step 2. described in the composite Nano plating bath prepare specific as follows: basic plating bath, nanometer powder and dispersion agent are put into the high speed magnetic stirrer, and stirring velocity is 500～2500rpm, and churning time is 5～30 minutes, ball milling adopts planetary type ball-milling, 4～10 hours ball milling time.
As preferably, step 2. described in its granularity of nanometer powder be 20～100 nanometers, and be selected from following at least a kind of: nano aluminium oxide, nano silicon oxide, nano zircite.
As preferably, step 2. described in nanometer powder mass concentration in the composite Nano plating bath be 10～100g/L.
As preferably, step 2. described in dispersion agent weight be 2%～20% of nanometer powder weight, and be selected from least following a kind of: the polyacrylic acid of modification, polyphosphoric acid salt, poly-organic carboxylate, modification synthetic fat acid amide, polyether polyols with reduced unsaturation, modified polyether.
As preferably, step 3. described in the sealing of hole plating time be 5～30 minutes, plating is 30～120 minutes under the nanometer plating whipped state of step described in 4..
1. step can comprise specifically that tumbling, alkali soak, rust cleaning, microetch and surface are adjusted.
Compared with prior art, the invention has the advantages that: adopt two step plating methods, at first with traditional plating bath plating, help reducing the porosity of coating, improve the bonding force of basic unit and coating, and afterwards with nano combined plating bath plating, help improving the anti-corrosion and wear resisting property of composite deposite; The integrated artistic step is few, is easy to control, and preparation is stable, and solution composition is simple, environment is polluted few; Be uniformly dispersed in the nanometer powder coating, good stability, content height.
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Embodiment: present embodiment is with agglomerating Nd-Fe-B permanent magnet (trade mark is 35M), and circular, external diameter is 9mm, and internal diameter is 4mm, and thickness is 2mm, specifically handles as follows:
1. the pre-treatment of sample surfaces: comprise that tumbling, alkali soak, rust cleaning, microetch and surface adjust;
2. distinguish configure base plating bath and composite Nano plating bath, the preparation of composite Nano plating bath is to make through stirring and ball milling after basic plating bath, nanometer powder and the dispersant;
3. sealing of hole plating: get sample plating in basic plating bath that pre-treatment finishes, the sealing of hole plating time is 5～30 minutes, preferred 20 minutes, matrix is wrapped up fully by nickel dam till;
4. nanometer plating: get sample that the sealing of hole plating finishes in the composite Nano plating bath and guarantee that nanometer powder is in plating under the state of good distribution all the time, cross as under the solution uniform state, executing, plating is 30～120 minutes under the nanometer plating mechanical stirring state, preferred 40 minutes, stirring velocity is 100～1000rpm, is preferably 300rpm.
5. aftertreatment: the samples with water of getting after the nanometer plating is rinsed well, oven dry, and it is stand-by to put into moisture eliminator.
Tumbling: be meant sample is put into the cylinder that fills abrasive material and chemical solution, cylinder is the tetrafluoroethylene ball grinder, is placed on the ball mill of rotating speed 500～1500rpm to rotate 4～12 hours, makes sample and the mutual friction mutually of abrasive material, sample and sample.Remove the oxide skin of sample surfaces, adjust the planeness of sample surfaces, make sample smooth and glossy, particularly edges and corners are level and smooth, evenly.Washing.
That alkali soaks employing is carbonate 10～50g/L, sodium hydroxide 10～30g/L, and tertiary sodium phosphate 10～80g/L, wherein several composite aqueous solution of water glass 1～20g/L, its wash temperature is at 40～1000 ℃, and the time is 2～10 minutes.Remove the grease on surface, ultrasonic washing.
Rust cleaning is to adopt the salpeter solution of 10～100mL/L to come pickling, soaks under the room temperature 1～10 minute, carries out ultrasonic cleaning then.Also can adopt several preferable solution or other modes mentioned in the prior art to eliminate rust.
Microetch: dispose commercial etching solution 50ml/L (the ND ETCHANT K that Hangzhou wild company difficult to understand provides), shared with ultrasonic wave, ultrasonic 2 minutes, washing.
The surface is adjusted: dispose commercial magneticsubstance surface treatment liquid 100ml/L (the ND 150CONDITIONED that Hangzhou wild company difficult to understand provides), soaked washing 2 minutes.
Step 2. in basic plating bath be the Watts plating bath.The specific configuration process is as follows: take by weighing the single nickel salt of 280g/L, the nickelous chloride of 45g/L adds an amount of distilled water, is placed in 40～800 ℃ the water-bath it is dissolved fully.Take by weighing the boric acid solution of 30～60g/L, add an amount of distilled water, being placed in 60～1000 ℃ the water-bath dissolves it fully, then the good solution of these three kinds dissolvings is mixed, add the sodium lauryl sulphate 0.01～0.08g/L for preparing in advance, adjust pH value to 4.0～5.0 with sodium hydroxide.Also can adopt several basic plating bath of mentioning in the prior art to dispose.
Step 2. described in the composite Nano plating bath prepare specific as follows: basic plating bath, nanometer powder and dispersion agent are put into the high speed magnetic stirrer, stirring velocity is 500～2500rpm, churning time is 5～30 minutes, and ball milling adopts planetary type ball-milling, 4～10 hours ball milling time.Wherein, its granularity of nanometer powder is 20～100 nanometers, nanometer powder can be the inorganic nano powder, and specifically can be selected from following at least a kind of: nano aluminium oxide, nano silicon oxide, nano zircite, nanometer powder mass concentration in the composite Nano plating bath is 10～100g/L.Dispersion agent weight is 2%～20% of nanometer powder weight, and is selected from following at least a kind of: the polyacrylic acid of modification, polyphosphoric acid salt, poly-organic carboxylate, modification synthetic fat acid amide, polyether polyols with reduced unsaturation, modified polyether.Dispersion agent adopts and is specifically designed to the agent of preparation water nano dispersion of particles, comes from German enlightening height (Tego) company, and its weight is 2%～20% of nano powder weight.
Dispersion agent is Dispers715W, the Dispers740W of German enlightening height (Tego) company preferably.The aluminum oxide 40g/L that adopts preferred 40 nanometers in the present embodiment is in composite plating bath, and dispersion agent weight is 5% of nanometer powder weight.
The compound weight of nano aluminium oxide is 15.6% in the products obtained therefrom coating, and it is excellent to soak after 400 hours sample surfaces in 3.5% sodium chloride solution.The microhardness mean value of coating reaches 700Hv.
The wear rate of contrast composite deposite and existing nickel coating as can be seen, Ni/Al
2O
3The wear rate of composite deposite is less than the wear rate of nickel coating, i.e. Ni/Al
2O
3The wear resistance of composite deposite is better than nickel coating.
Claims (9)
1, a kind of process for producing nano-composite plate of neodymium iron boron material is characterized in that comprising the steps:
1. the pre-treatment of sample surfaces;
2. distinguish configure base plating bath and composite Nano plating bath, the preparation of composite Nano plating bath is to make through stirring and ball milling after basic plating bath, nanometer powder and the dispersant;
3. sealing of hole plating: get sample plating in basic plating bath that pre-treatment finishes;
4. nanometer plating: get sample plating in the composite Nano plating bath that the sealing of hole plating finishes.
2, process for producing nano-composite plate of neodymium iron boron material according to claim 1 is characterized in that the basic plating bath described in step 2. is the Watts plating bath.
3, process for producing nano-composite plate of neodymium iron boron material according to claim 1, it is characterized in that the composite Nano plating bath prepares specific as follows described in step 2.: basic plating bath, nanometer powder and dispersion agent are put into the high speed magnetic stirrer, stirring velocity is 500～2500rpm, churning time is 5～30 minutes, ball milling adopts planetary type ball-milling, 4～10 hours ball milling time.
4, process for producing nano-composite plate of neodymium iron boron material according to claim 1 is characterized in that its granularity of nanometer powder is 20～100 nanometers described in step 2., and is selected from following at least a kind of: nano aluminium oxide, nano silicon oxide, nano zircite.
5, process for producing nano-composite plate of neodymium iron boron material according to claim 1 is characterized in that nanometer powder mass concentration in the composite Nano plating bath is 10～100g/L described in step 2..
6, process for producing nano-composite plate of neodymium iron boron material according to claim 1, it is characterized in that dispersion agent weight is 2%～20% of nanometer powder weight described in step 2., and be selected from following at least a kind of: the polyacrylic acid of modification, polyphosphoric acid salt, poly-organic carboxylate, modification synthetic fat acid amide, polyether polyols with reduced unsaturation, modified polyether.
7, process for producing nano-composite plate of neodymium iron boron material according to claim 1 is characterized in that the sealing of hole plating time is 5～30 minutes described in step 3..
8, process for producing nano-composite plate of neodymium iron boron material according to claim 1 is characterized in that under the nanometer plating whipped state described in step 4. plating 30～120 minutes.
9, process for producing nano-composite plate of neodymium iron boron material according to claim 1 is characterized in that 1. step comprises that tumbling, alkali soak, rust cleaning, microetch and surface adjust.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100593730A CN101492830A (en) | 2008-01-25 | 2008-01-25 | Process for producing nano-composite plate of neodymium iron boron material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102166873A (en) * | 2010-02-26 | 2011-08-31 | 比亚迪股份有限公司 | Neodymium-iron-boron magnetic steel with coating and preparation methods thereof |
| CN103556208A (en) * | 2013-11-04 | 2014-02-05 | 北京工业大学 | Treating agent and electro-deposition method for forming rare earth hydride particle coating |
| CN105040004A (en) * | 2015-08-28 | 2015-11-11 | 安徽大地熊新材料股份有限公司 | Sintered Nd-Fe-B magnet surface coating technology |
| CN111041541A (en) * | 2019-12-30 | 2020-04-21 | 临沂鑫海新型材料有限公司 | High-performance nickel-based wear-resistant alloy |
| CN113846361A (en) * | 2021-12-01 | 2021-12-28 | 天津三环乐喜新材料有限公司 | Electroplating pretreatment method and equipment for sintered neodymium-iron-boron permanent magnet |
-
2008
- 2008-01-25 CN CNA2008100593730A patent/CN101492830A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102166873A (en) * | 2010-02-26 | 2011-08-31 | 比亚迪股份有限公司 | Neodymium-iron-boron magnetic steel with coating and preparation methods thereof |
| CN103556208A (en) * | 2013-11-04 | 2014-02-05 | 北京工业大学 | Treating agent and electro-deposition method for forming rare earth hydride particle coating |
| CN103556208B (en) * | 2013-11-04 | 2016-02-17 | 北京工业大学 | The electro-deposition method of a kind for the treatment of agent for the formation of rare earth hydride particulate coating and formation coating |
| CN105040004A (en) * | 2015-08-28 | 2015-11-11 | 安徽大地熊新材料股份有限公司 | Sintered Nd-Fe-B magnet surface coating technology |
| CN111041541A (en) * | 2019-12-30 | 2020-04-21 | 临沂鑫海新型材料有限公司 | High-performance nickel-based wear-resistant alloy |
| CN113846361A (en) * | 2021-12-01 | 2021-12-28 | 天津三环乐喜新材料有限公司 | Electroplating pretreatment method and equipment for sintered neodymium-iron-boron permanent magnet |
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Open date: 20090729 |