CN1786274A - Diamond surface titanium coating nickel coating copper coating composite structure and its manufacturing method - Google Patents
Diamond surface titanium coating nickel coating copper coating composite structure and its manufacturing method Download PDFInfo
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- CN1786274A CN1786274A CN 200410096800 CN200410096800A CN1786274A CN 1786274 A CN1786274 A CN 1786274A CN 200410096800 CN200410096800 CN 200410096800 CN 200410096800 A CN200410096800 A CN 200410096800A CN 1786274 A CN1786274 A CN 1786274A
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Abstract
The invention relates to a diamond surface titanizing nickel plating copper plating composite structure and its manufacturing method. Diamond surface has a titanium layer. The titanium has a nickel layer. The nickel layer has a copper layer. Its steps includes the following: titanizing by vacuum micro-evaporating to form TiC at the contact surface of the titanizing layer and the diamond; nickel plating by electroplating method at the titanium layer; copper plating by chemical plating at the nickel layer. The invention improves the bonding strength of the diamond and the bonding agent, and diamond grain strength; endows the coated diamond with high heat conductivity to protect it. It is mainly used in resin bonding agent grinding tool.
Description
Technical field
The present invention relates to a kind of diamond surface titanium coating nickel coating copper coating composite structure and manufacture method.
Background technology
Diamond is very extensive in industrial application, can make multiple instrument such as cutter, emery wheel, grinding tool etc., because the characteristic of diamond itself, combine very difficult with other material, so the matrix from instrument comes off easily, causes the work-ing life of instrument low, production cost increases.
Solution and coating method in the past all is the plating method that adopts single metal basically, adopt single solution and coating method at diamond surface, as: vacuum plating, plating, electroless plating, the single metal or alloy of plating, as: Ni, Cu, Ti, Cr, Ti+Ni, Ni-Co alloy, Cu-Sn-Ti or Cu-Ag-Ti multicomponent alloy, these solution and coating method all exist or such defective, can not obtain satisfied result of use.
Summary of the invention
The objective of the invention is to improve the prior art diamond combines the shortcoming of difficulty and a kind of diamond surface titanium coating nickel coating copper coating composite structure and manufacture method is provided with other material.
For achieving the above object, the present invention takes following design: diamond surface has a titanium layer; One nickel dam is arranged on described titanium layer, a bronze medal layer is arranged on the top layer of described nickel dam.
A kind of diamond surface titanium coating nickel coating copper coating composite structure manufacture method, the step below adopting;
Step 1: the first step adopts the little evaporation titanizing of vacuum, and the one side that the titanizing layer is contacted with diamond forms the titanium carbide TiC by firm chemical bond combination, and the outside surface of titanizing layer then is a metal titanium,
Step 2: adopt electric plating method on the titanium layer face, to plate one deck nickel thorn,
Step 3: adopt the method for electroless plating to plate layer of copper on nickel thorn surface.
Advantage of the present invention mainly is: this diamond interface of the present invention and composite deposite have powerful metallic bond bonded diamond, can improve the bonding strength of diamond and wedding agent; Improve the granule strength of diamond particles; Give the overlay coating diamond higher thermal conductivity; Diamond is played the insulation blocking effect, make it at high temperature sintering and high temperature grinding generation oxidation, greying, solvation or generation carbide.
Diamond with surperficial titanizing and nickel and copper mainly uses in the grinding tool of resinoid bond, also can be used for the metal matrix grinding tool.Use it can make diamond obtain the higher sword that goes out, high abrasive particle bonding strength, diamond surface at first adopts the little evaporation titanizing of vacuum, next adopts electric plating method to plate one deck nickel thorn on the titanium layer face, and the method that adopts electroless plating at last is at the surperficial copper layer that plates one deck high thermal conductivity of nickel thorn.Titanium layer and adamantine bonding surface have generated titanium carbide TiC between being, titanium and diamond are that firm chemical bond combines, and are metallic bond between titanium and nickel, nickel and the copper and combine bonding strength height, coating difficult drop-off.Thereby improve the grinding sharpness of grinding tool, improve working (machining) efficiency, prolong the work-ing life of grinding tool.
Description of drawings
Fig. 1 diamond particles local section of the present invention structural representation.
Embodiment
Embodiment 1: as shown in Figure 1, the present invention by: there is a titanium layer 2 on diamond 1 surface; One nickel dam 3 is arranged on described titanium layer 2, one bronze medal layer 4 is arranged on described nickel dam 3 top layers.
Embodiment 2: diamond 1 is a particulate state, and irregular scraggly type looks surface is arranged, and described titanium layer 2, nickel dam 3 and copper layer 4 form composite bed, parcel diamond 1 according to diamond 1 irregular scraggly type looks surface.
Titanium layer and diamond bonded simultaneously generate the titanium carbide TiC layer of 0.5～0.8 μ m, and it is the titanium layer of thickness 1 μ m that the outside surface of titanium layer has one deck.Electronickelling thorn layer is disregarded thickness, only counts adamantine weightening finish ratio, and the general weightening finish ratio that adopts is: 30%～70%, and copper electroplating layer is disregarded thickness, only counts adamantine weightening finish ratio, and weightening finish is 5%～30%.
Embodiment 3: a kind of diamond surface titanium coating nickel coating copper coating composite structure manufacture method, the step below adopting;
Step 1: adopt the little evaporation titanizing of vacuum, the titanium carbide TiC that one side that the titanizing layer contact with diamond and formation are combined by firm chemical bond, the outside surface of titanizing layer then is a metal titanium, titanizing special use vacuum oven and cover of vacuum unit; In the special-purpose jar of packing into behind diamond and the titanium valve uniform mixing, be placed in the furnace chamber of vacuum unit; Open the vacuum unit and be warming up to the temperature (120 orders are 745 ℃ with thick diamond, and 120 orders are 780 ℃ with thin diamond) of setting, be incubated 1 hour postcooling to 250 and ℃ close the vacuum unit; . treat to cool off fully the back jar is taken out, get product after sifting out diamond; Titanium valve granularity 120 orders with thick diamond with 230 orders with thin titanium valve, 120 orders with thin diamond with 60 orders with thick titanium valve, the per kilogram titanium valve adds the 20ml activation solution, 120 orders are 30g/1000ct with thick diamond titanium valve consumption, 120 orders are 130g/1000ct with thin diamond titanium valve consumption, this technology is as the criterion by coating weightening finish 0.4%, does not calculate thickness of coating;
Step 2: adopt electric plating method to plate one deck nickel on the titanium layer face, the type looks of described one deck nickel are the nickel thorn, use equipment: man-made diamond rolling electroplating machine, at first to carry out electroless plating in the past in electroplated Ni, and its electroless plating step is:
Step " 1 ", diamond is put as in the beaker, pour palladium liquid into, heating also is stirred well to simultaneously boils, then palladium liquid is poured out, again diamond is washed 6-8 all over after pour into separate glue once more heated and stirred diamond is washed 6-8 time again to boiling, the ortho phosphorous acid sodium solution of adding 10% stirs slightly and can carry out electroless plating;
Step " 2 ", prepare electroplate liquid by prescription, the plating bath for preparing in beaker when the water-bath stove is preheated to 80 ℃ is put into the water-bath stove, diamond is poured in the beaker, and stir simultaneously, temperature is controlled at 80-90 ℃, continues about 1 hour, reaction finishes when plating bath no longer includes bubble and emerges, then diamond washing 2 times.
The electroplated Ni step,
Step " 1 ", the diamond that electroless plating is plated are put into and are electroplated bottle, add electroplate liquid, will electroplate bottledly on electroplating machine, put well to electroplate and use negative electrode and anode, and preset gain in weight.Initial voltage is 5V, and electric current is about 1A, through 10-20 minute electric current is transferred to 4A, but voltage can not surpass 10V, and the rotating speed of plating bottle is not as the criterion so that diamond is floating, and the pH value of plating bath is controlled between the 5-5.5, and too high available 10% dilute sulphuric acid is regulated;
Step " 2 ", electroplated Ni step are electroplated and are finished back clean and oven dry the diamond washing, sieved finished product the coating pickling of waste product is fallen, and calculate the substantial proportion of coating; Electroplate composition and the proportioning of plating with plating bath, thickness of coating: chemical plating bath: filling a prescription is: single nickel salt 35g/l; Trisodium Citrate 20g/l; Sodium acetate 20g/l; Inferior sodium phosphate 30g/l; The single nickel salt 270g/l of electroplate liquid; Boric acid 35-41g/l; Sodium lauryl sulphate 0.1-0.5g/l; Sodium-chlor 26g/l; Thickness of coating: this technology is by the requirement processing of nickel plating ratio, as long as the weightening finish of nickel plating is not calculated thickness of coating than qualified, nickel plating is generally 30%～70%;
Step 3: adopt the method for electroless plating to plate layer of copper on nickel thorn surface; Equipment is common water-bath stove, agitator, and beaker, man-made diamond rolling electroplating machine,
Step 1), prepare plating bath by prescription, the plating bath for preparing in beaker when the water-bath stove is preheated to 50 ℃ is put into the water-bath stove, electroplating good diamond finished product pours in the beaker, and stir simultaneously, temperature is controlled at 50-55 ℃, continue about 1 hour, electroless plating reaction finishes when plating bath no longer includes bubble and emerges, then diamond washing 6-8 time;
Step 2), diamond is carried out Passivation Treatment: diamond is placed on electroplates in the bottle, add passivating solution, will electroplate bottledly on electroplating machine, put anode and cathode well, electric current remains on 0.1-0.5A, and passivation is taken off after about 1 hour diamond is cleaned 6-8 time.
Step 3), diamond washing back oven dry have been sieved finished product the coating pickling of waste product have been fallen, and calculate the substantial proportion of coating;
Electroless plating chemical plating bath: disodium ethylene diamine tetraacetate 35g/l; Seignette salt 24g/l; Sodium hydroxide 70g/l; Copper sulfate 20g/l; Formaldehyde 20ml/l; 2-2 dipyridyl 20ml/l; Yellow prussiate of potash 20ml/l; Passivating solution composition: sodium dichromate 99 80-90g/l; Glacial acetic acid is regulated pH value 2.5-3.0; Thickness of coating: coating only calculates copper-plated weightening finish ratio, and does not calculate thickness of coating, generally increases weight 5%～30%.
Claims (8)
1, a kind of diamond surface titanium coating nickel coating copper coating composite structure is characterized in that: diamond surface has a titanium layer; One nickel dam is arranged on described titanium, a bronze medal layer is arranged on the top layer of described nickel dam.
2, a kind of diamond surface titanium coating nickel coating copper coating composite structure according to claim 1 is characterized in that: titanium layer and diamond bonded simultaneously generate the titanium carbide layer of 0.5～0.8 μ m, and it is the titanium layer of thickness 1 μ m that the outside surface of titanium layer has one deck.
3, a kind of diamond surface titanium coating nickel coating copper coating composite structure according to claim 1 and 2 is characterized in that: diamond is a particulate state.
4, a kind of diamond surface titanium coating nickel coating copper coating composite structure manufacture method is characterized in that: the step below adopting;
Step 1: the first step adopts the little evaporation titanizing of vacuum, the titanium carbide that one side that the titanizing layer contacts with diamond and formation are combined by firm chemical bond, and the outside surface of titanizing layer then is a metal titanium,
Step 2: adopt electric plating method on the titanium layer face, to plate one deck nickel thorn,
Step 3: adopt the method for electroless plating to plate layer of copper on nickel thorn surface.
5, a kind of diamond surface titanium coating nickel coating copper coating composite structure manufacture method according to claim 4 is characterized in that: the step below adopting;
In claim 4 step 1: in the special-purpose jar of packing into behind diamond and the titanium valve uniform mixing, be placed in the furnace chamber of vacuum unit; Opening temperature 120 orders that the vacuum unit is warming up to setting is 745 ℃ with thick diamond, and 120 orders are 780 ℃ with thin diamond, is incubated 1 hour postcooling to 250 and ℃ closes the vacuum unit; Treat to cool off fully the back jar is taken out, get product after sifting out diamond;
In claim 4 step 2: at first will carry out electroless plating in the past in electroplated Ni, its electroless plating step is:
Step " 1 ", diamond is put as in the beaker, pour palladium liquid into, heating also is stirred well to simultaneously boils, then palladium liquid is poured out, again diamond is washed 6-8 all over after pour into separate glue once more heated and stirred diamond is washed 6-8 time again to boiling, the ortho phosphorous acid sodium solution of adding 10%, stirring gets final product slightly;
Step " 2 ", prepare electroplate liquid by prescription, the plating bath for preparing in beaker when the water-bath stove is preheated to 80 ℃ is put into the water-bath stove, diamond is poured in the beaker, and stir simultaneously, temperature is controlled at 80-90 ℃, continues about 1 hour, reaction finishes when plating bath no longer includes bubble and emerges, then diamond washing 2 times;
The electroplated Ni step,
Step " 1 ", the diamond that electroless plating is plated are put into and are electroplated bottle, add electroplate liquid, will electroplate bottledly on electroplating machine, put well to electroplate and use negative electrode and anode, and preset gain in weight.Initial voltage is 5V, and electric current is about 1A, through 10-20 minute electric current is transferred to 4A, but voltage can not surpass 10V, and the rotating speed of plating bottle is not as the criterion so that diamond is floating, and the pH value of plating bath is controlled between the 5-5.5, and too high available 10% dilute sulphuric acid is regulated;
Step " 2 ", electroplated Ni step are electroplated and are finished back clean and oven dry the diamond washing, sieved finished product the coating pickling of waste product is fallen;
In claim 4 step 3: the step below adopting;
Step 1), prepare plating bath by prescription, the plating bath for preparing in beaker when the water-bath stove is preheated to 50 ℃ is put into the water-bath stove, electroplating good diamond finished product pours in the beaker, and stir simultaneously, temperature is controlled at 50-55 ℃, continue about 1 hour, electroless plating reaction finishes when plating bath no longer includes bubble and emerges, then diamond washing 6-8 time;
Step 2), diamond is carried out Passivation Treatment: diamond is placed on electroplates in the bottle, add passivating solution, will electroplate bottledly on electroplating machine, put anode and cathode well, electric current remains on 0.1-0.5A, and passivation is taken off after about 1 hour diamond is cleaned 6-8 time;
Step 3), diamond washing back oven dry have been sieved finished product the coating pickling of waste product have been fallen.
6, a kind of diamond surface titanium coating nickel coating copper coating composite structure manufacture method according to claim 5, it is characterized in that: titanium valve granularity 120 orders with thick diamond with 230 orders with thin titanium valve, 120 orders with thin diamond with 60 orders with thick titanium valve, the per kilogram titanium valve adds the 20ml activation solution, 120 orders are 30g/1000ct with thick diamond titanium valve consumption, and 120 orders are 130g/1000ct with thin diamond titanium valve consumption.
7, a kind of diamond surface titanium coating nickel coating copper coating composite structure manufacture method according to claim 5, it is characterized in that: plating solution formula is: single nickel salt 35g/l; Trisodium Citrate 20g/l; Sodium acetate 20g/l; Inferior sodium phosphate 30g/l; The single nickel salt 270g/l of electroplate liquid; Boric acid 35-41g/l; Sodium lauryl sulphate 0.1-0.5g/l; Sodium-chlor 26g/l.
8, a kind of diamond surface titanium coating nickel coating copper coating composite structure manufacture method according to claim 5 is characterized in that: electroless plating chemical plating bath: disodium ethylene diamine tetraacetate 35g/l; Seignette salt 24g/l; Sodium hydroxide 70g/l; Copper sulfate 20g/l; Formaldehyde 20ml/l; 2-2 dipyridyl 20ml/l; Yellow prussiate of potash 20ml/l; Passivating solution composition: sodium dichromate 99 80-90g/l; Glacial acetic acid is regulated pH value 2.5-3.0.
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| CN101941311A (en) * | 2010-07-20 | 2011-01-12 | 华南理工大学 | Copper-diamond composite coating and preparation method thereof |
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| CN106626167A (en) * | 2015-10-30 | 2017-05-10 | 中山联合光电科技股份有限公司 | Long-acting environment-friendly release agent and preparing method thereof |
| CN108517520A (en) * | 2018-06-15 | 2018-09-11 | 北京铂阳顶荣光伏科技有限公司 | A kind of diamond laminated film and its preparation method and application |
| CN108950283A (en) * | 2018-07-13 | 2018-12-07 | 长沙博朗思达新材料科技有限公司 | A kind of preparation method of diamond/copper composite material |
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Owner name: SHANGHAI JINGYAN ABRASIVES CO., LTD. Free format text: FORMER OWNER: SHANGHAI JIANGXIN SUPERHARD MATERIAL CO., LTD. Effective date: 20100108 |
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Effective date of registration: 20100108 Address after: 3 floor, No. 1251, Lane 31, South Road, Shanghai, Pudong Patentee after: Shanghai Fine Abrasives Grinding Tools Co.,Ltd. Address before: 3 floor, No. 1251, Lane 31, South Road, Shanghai, Pudong Patentee before: Shanghai Jiangxin Ultrahard Material Co., Ltd. |