CN104233217A - New method for preparing diamond coated cutting tool - Google Patents
New method for preparing diamond coated cutting tool Download PDFInfo
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- CN104233217A CN104233217A CN201410465657.5A CN201410465657A CN104233217A CN 104233217 A CN104233217 A CN 104233217A CN 201410465657 A CN201410465657 A CN 201410465657A CN 104233217 A CN104233217 A CN 104233217A
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- diamond
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- cutting tool
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- coated tools
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Abstract
The invention belongs to the field of a material coating, and particularly provides a new method for preparing a high-quality diamond coated cutting tool by multilayered step-by-step deposition. The new method concretely comprises the following steps: firstly, plating a molybdenum layer on the surface of a hard alloy cutting tool by adopting an electroplating method or a physical vapor deposition method, wherein molybdenum is bound together with cobalt on the surface of a matrix to form a stable compound so as to form a transition layer on the surface of the matrix, so that not only can the influence of cobalt on the surface of the cutting tool to the diamond coating be reduced, but also the dispersion of cobalt towards the surface of the cutting tool from the depth position of the matrix is prevented; and then depositing a diamond coating by two steps through utilizing microwave plasma CVD (MPCVD) method, namely controlling corresponding parameters in diamond nucleation and growth stages to form a nanodiamond thin film with high quality and high stability.
Description
Technical field
The invention belongs to material coating field, be specifically related to a kind of novel method of multilayer stepped depositions diamond-coated tools.
Background technology
Along with automobile, the developing rapidly of aerospace industry, the lightweight of material is quantized, the requirement of high specific strength improves day by day, nonferrous metal and alloy, carbon fiber reinforced plastics, glass filament reinforced plastics, fiber-reinforced metal and the novel material such as graphite, pottery obtain applying more and more widely in the industry, common rapid steel and inserted tool are when carrying out mechanical workout to these materials, and its defect just obviously comes out.Diamond has the performance of many excellences, as ultrahigh hardness, high heat conductance, high optical transmittance and fabulous electrical insulating property, is the ideal material of the manufacture cutter hardly matched in current known materials.Because natural diamond resource is very limited, and expensive, cannot use on a large scale in the industry, therefore carry out the technology development of coating at carbide tool surface, and various diamond-coated tools and coating technology also emerge in an endless stream.
The coating technology be actually used now has a variety of, and comprise CVD, PVD, PCVD, salt bath dip process etc., they can improve the use properties of cutter in certain degree.But the ubiquitous problem of these methods is: the cobalt effectively can not removing tool surface, diamond nucleation difficulty can be caused, promote the formation of graphite-phase, have a strong impact on the bonding force of coating, coating and matrix adhesive force poor, cause diamond particles easily to come off, coating quality is unstable.Preparing diamond-coated tools method at present has in patent, as application number, to be 201010300247.7 publication numbers be that CN102154536A has invented a kind of " carbide tool surface high-current pulsed electron beam treatment process ", high-current pulsed electron beam is utilized to need position to be processed to carry out processing treatment to carbide surface in a vacuum, be the refinement of tool surface homogeneous microstructure, improve surface property and the work-ing life of cutter; " complicated shape cvd diamond/diamond-like composite coating cutter preparation method " as application number to be 201210124337.4 publication numbers be CN102650053A proposes and adopts filament CVD to deposit one deck MCD film at tool surface, adopt floating bias voltage to produce ion bombardment therebetween and ensure its slipperiness, continue deposition one deck DLC film subsequently, obtain the cvd diamond/diamond-like composite coating with excellent film-base adhesion strength, surface abrasion resistance anti-attrition and self-lubricating property.These methods do not solve the cobalt of tool surface, and the existence of cobalt can have a strong impact on the sticking power of diamond coatings, and coating quality is unstable, can reduce performance and the work-ing life of cutter to a certain extent.
Summary of the invention
In order to overcome the defect of aforesaid method, solve the impact of tool surface cobalt existence on cutter, the present invention proposes a kind of novel method of depositing high-quality diamond-coated tools, concrete technical scheme is: first plate one deck molybdenum at carbide tool surface by electrochemical plating or physical vaporous deposition, it can be combined with the cobalt of matrix surface and form stable compound, one deck transition layer is formed at matrix surface, so both reduce the impact of tool surface cobalt in the future on diamond coatings, prevent again cobalt from matrix depths to the diffusion of tool surface; Utilize microwave plasma CVD (MPCVD) method to form one deck diamond coatings in two steps subsequently, namely form at diamond nucleation and growth two corresponding parameters of stage control the nano-diamond film that one deck has high quality and high stability.
Prepare a novel method for diamond-coated tools, its concrete steps are:
(1) put into deionized water ultrasonic wave to inserted tool to clean its surface;
(2) after the cleaning carbide tool surface plating or physical vapor deposition one deck molybdenum, after to be done, with acetone or alcohol washes transition layer;
(3) utilize microwave plasma method MPCVD, the concentration expressed in percentage by volume adopting methane is 1.5%, keeps passing into H
2, deposition 15min, completes the diamond nucleation stage;
(4) inserted tool is put into the diamond powder solution of 0.4 ~ 0.8 μm, utilize microwave plasma method MPCVD, in the diamond film stage, complete the deposition of diamond thin in two steps;
The first step: the concentration expressed in percentage by volume adopting methane is 0.5%, keeps H in step (3)
2flow, air pressure, deposition 15min;
Second step, the concentration expressed in percentage by volume adopting methane is 15%, keeps H in step (3)
2flow, air pressure, deposit more than 8 hours;
(5), after deposition terminates, take out process cutter, obtain high-quality diamond nano film coating.
In step (2), the thickness of described molybdenum layer is: 5 ~ 8 μm.
In step (3), in described microwave plasma method, microwave power is 950 ~ 1000W, temperature 650 ~ 700 DEG C;
Described H
2flow is 90 ~ 110sccm, and air pressure is at 7.5 ~ 8KPa.
In step (4), in the microwave plasma method of the described the first step, microwave power is 1000 ~ 1100W, and temperature is 750 ~ 800 DEG C.
In step (4), in the microwave plasma method of described second step, microwave power is 1100 ~ 1200W, and temperature is 850 ~ 900 DEG C.
Compared with existing Coating Techniques of Cemented Carbide Tools, the invention has the beneficial effects as follows:
1, first on tool matrix, plate a skim, effectively can remove the cobalt of tool surface, and form stable compound coating, can be good at preventing the cobalt of cutter deep layer from spreading to tool surface, ensure that the bonding force between cutter coat and matrix.
2, the diamond nucleation stage, by controlling the concentration of methane and relevant parameter, the high and good diamond coatings of purity of Enhancing Nucleation Density can be obtained.
3, the diamond film stage, the first step, reduces the concentration of methane, changes corresponding parameter, can strengthen the etching action of atomic hydrogen, effectively removes the amorphous component that nucleation of diamond is shown in, ensures the quality of diamond coatings; Second step, raises the concentration of methane, raised temperature and microwave power, extends depositing time, can improve adamantine second nucleation rate, suppresses growing up of crystal grain, can obtain high-quality diamond nano film coating.
4, microwave plasma CVD technique, has that electrodeless pollution, Diamond Thin Film Quality are good, experiment is easy to control and the advantage such as favorable repeatability of sample.
Accompanying drawing explanation
Fig. 1 is the general flow figure preparing diamond-coated tools;
Fig. 2 is the schema in two stages of using MPCVD preparing diamond coatings cutter.
Embodiment
In detail the specific embodiment of the invention is described further below in conjunction with technical scheme, but protection scope of the present invention is not limited to this.
Select YG8 normal granulometry inserted tool to process, this is a kind of typical sintered carbide tool material.
Embodiment 1
1, first ultrasonic cleaning is carried out to YG serial carbide alloy tool surface, remove impurity and the greasy dirt of tool surface.
2, the electroplating surface of inserted tool after the cleaning or physical vapor deposition one deck molybdenum, after to be done, with acetone or alcohol washes transition layer, for deposition of diamond coatings is prepared.
3, on crystal clock bell-type MPCVD equipment, put into by the inserted tool of coating in reaction chamber substrate support table, in the diamond nucleation stage, microwave power is 950W, and the concentration adopting methane is 1.5%, H
2flow be 90sccm, substrate temperature 650 DEG C, air pressure at 7.5KPa, deposition 15min.
4, in the diamond film stage, the deposition of diamond thin is completed in two steps.Inserted tool is put into the diamond powder solution of 0.4 ~ 0.8 μm, the first step, the concentration of methane is reduced to 0.5%, microwave power is 1000W, and temperature is 750 DEG C, H
2flow, air pressure constant, deposition 15min; Second step, rises to 15% by the concentration of methane, and microwave power is 1100W, and temperature is 850 DEG C, H
2flow, air pressure constant, depositing time more than 8 hours.
5, after deposition terminates, take out process cutter, carry out AFM scanning, and carry out particle scale analysis.
Embodiment 2
1, first ultrasonic cleaning is carried out to YG serial carbide alloy tool surface, remove impurity and the greasy dirt of tool surface.
2, the electroplating surface of inserted tool after the cleaning or physical vapor deposition one deck molybdenum, after to be done, with acetone or alcohol washes transition layer, for deposition of diamond coatings is prepared.
3, on crystal clock bell-type MPCVD equipment, put into by the inserted tool of coating in reaction chamber substrate support table, in the diamond nucleation stage, microwave power is 1000W, and the concentration adopting methane is 1.5%, H
2flow be 110sccm, substrate temperature 700 DEG C, air pressure at 8KPa, deposition 15min.
4, in the diamond film stage, the deposition of diamond thin is completed in two steps.Inserted tool is put into the diamond powder solution of 0.4 ~ 0.8 μm, the first step, the concentration of methane is reduced to 0.5%, microwave power is 1100W, and temperature is 800 DEG C, H
2flow, air pressure constant, deposition 15min; Second step, rises to 15% by the concentration of methane, and microwave power is 1200W, and temperature is 900 DEG C, H
2flow, air pressure constant, depositing time more than 8 hours.
After treatment, YG8 carbide tool surface flat smooth, surveying its diamond particles yardstick is tens nanometers, and obtain high-quality diamond nano film coating, cutter wear resistance improves greatly.
Described embodiment is preferred embodiment of the present invention; but the present invention is not limited to above-mentioned embodiment; when not deviating from flesh and blood of the present invention, any apparent improvement that those skilled in the art can make, replacement or modification all belong to protection scope of the present invention.
Claims (5)
1. prepare a novel method for diamond-coated tools, it is characterized in that: comprise following concrete steps:
(1) put into deionized water ultrasonic wave to inserted tool to clean its surface;
(2) after the cleaning carbide tool surface plating or physical vapor deposition one deck molybdenum, after to be done, with acetone or alcohol washes transition layer;
(3) utilize microwave plasma method MPCVD, the concentration expressed in percentage by volume adopting methane is 1.5%, keeps passing into H
2, deposition 15min, completes the diamond nucleation stage;
(4) inserted tool is put into the diamond powder solution of 0.4 ~ 0.8 μm, utilizes microwave plasma method MPCVD, in the diamond film stage, complete the deposition of diamond thin in two steps:
The first step: the concentration expressed in percentage by volume adopting methane is 0.5%, keeps H in step (3)
2flow, air pressure, deposition 15min;
Second step: the concentration expressed in percentage by volume adopting methane is 15%, keeps H in step (3)
2flow, air pressure, deposit more than 8 hours;
(5), after deposition terminates, take out process cutter, obtain high-quality diamond nano film coating.
2. a kind of novel method preparing diamond-coated tools as described in claim 1, it is characterized in that: in step (2), the thickness of described molybdenum layer is: 5 ~ 8 μm.
3. a kind of novel method preparing diamond-coated tools as described in claim 1, is characterized in that:
In step (3), in described microwave plasma method, microwave power is 950 ~ 1000W, temperature 650 ~ 700 DEG C; Described H
2flow is 90 ~ 110sccm, and air pressure is at 7.5 ~ 8KPa.
4. a kind of novel method preparing diamond-coated tools as described in claim 1, is characterized in that:
In step (4), in the microwave plasma method of the described the first step, microwave power is 1000 ~ 1100W, and temperature is 750 ~ 800 DEG C.
5. a kind of novel method preparing diamond-coated tools as described in claim 1, is characterized in that:
In step (4), in the microwave plasma method of described second step, microwave power is 1100 ~ 1200W, and temperature is 850 ~ 900 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410465657.5A CN104233217A (en) | 2014-09-15 | 2014-09-15 | New method for preparing diamond coated cutting tool |
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| CN201410465657.5A CN104233217A (en) | 2014-09-15 | 2014-09-15 | New method for preparing diamond coated cutting tool |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105483644A (en) * | 2016-01-15 | 2016-04-13 | 中国科学院深圳先进技术研究院 | Multilayer diamond coating, manufacturing method thereof and coating tool |
| CN105506574A (en) * | 2015-12-24 | 2016-04-20 | 富耐克超硬材料股份有限公司 | Preparation method of nano-diamond coating and nano-diamond blade |
| CN107699938A (en) * | 2017-10-18 | 2018-02-16 | 上海都为电子有限公司 | A kind of preparation technology of diamond cutting secant |
| CN108277489A (en) * | 2018-03-30 | 2018-07-13 | 镇江东艺机械有限公司 | A kind of crosslinking PVD hard coats high speed cutting tool and manufacturing method |
| CN109811303A (en) * | 2019-01-23 | 2019-05-28 | 上海大学 | Nano-diamond film preparation method based on DLC film middle layer |
| CN110184606A (en) * | 2019-07-10 | 2019-08-30 | 河南富莱格超硬材料有限公司 | Diamond-coated tools and preparation method thereof |
| CN110218974A (en) * | 2019-07-10 | 2019-09-10 | 河南富莱格超硬材料有限公司 | Diamond coatings complex matrix and preparation method thereof |
-
2014
- 2014-09-15 CN CN201410465657.5A patent/CN104233217A/en active Pending
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| 杨仕娥: "硬质合金刀具基体上金刚石涂层的制备及其附着性能的研", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 * |
| 马丙现: "氢的强化刻蚀对金刚石薄膜品质的影响与sp2杂化碳原子的存在形态", 《物理学报》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105506574A (en) * | 2015-12-24 | 2016-04-20 | 富耐克超硬材料股份有限公司 | Preparation method of nano-diamond coating and nano-diamond blade |
| CN105506574B (en) * | 2015-12-24 | 2018-03-06 | 富耐克超硬材料股份有限公司 | The preparation method and Nano diamond blade of nano diamond coating |
| CN105483644A (en) * | 2016-01-15 | 2016-04-13 | 中国科学院深圳先进技术研究院 | Multilayer diamond coating, manufacturing method thereof and coating tool |
| CN107699938A (en) * | 2017-10-18 | 2018-02-16 | 上海都为电子有限公司 | A kind of preparation technology of diamond cutting secant |
| CN107699938B (en) * | 2017-10-18 | 2019-12-20 | 上海都为电子有限公司 | Preparation process of diamond cutting line |
| CN108277489A (en) * | 2018-03-30 | 2018-07-13 | 镇江东艺机械有限公司 | A kind of crosslinking PVD hard coats high speed cutting tool and manufacturing method |
| CN109811303A (en) * | 2019-01-23 | 2019-05-28 | 上海大学 | Nano-diamond film preparation method based on DLC film middle layer |
| CN110184606A (en) * | 2019-07-10 | 2019-08-30 | 河南富莱格超硬材料有限公司 | Diamond-coated tools and preparation method thereof |
| CN110218974A (en) * | 2019-07-10 | 2019-09-10 | 河南富莱格超硬材料有限公司 | Diamond coatings complex matrix and preparation method thereof |
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