CN105039927B - Large aperture diamond drawing die coating Preparation equipment and preparation method - Google Patents
Large aperture diamond drawing die coating Preparation equipment and preparation method Download PDFInfo
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- CN105039927B CN105039927B CN201510106465.XA CN201510106465A CN105039927B CN 105039927 B CN105039927 B CN 105039927B CN 201510106465 A CN201510106465 A CN 201510106465A CN 105039927 B CN105039927 B CN 105039927B
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Abstract
The invention discloses a kind of large aperture diamond drawing die coating Preparation equipment and preparation methods.It includes CVD deposition equipment, and the drawing mould that can be driven the rotary table of rotation by power-equipment and be vertically installed on rotary table is equipped in CVD deposition equipment, there is the filament assembly of fixed installation in the endoporus of drawing mould；Filament assembly includes the semiorbicular molybdenum sheet of two panels and the multipair vertical heated filament being arranged symmetrically on the semiorbicular molybdenum sheet of two panels, and the end of every vertical heated filament is connected on wherein a piece of semiorbicular molybdenum sheet, and two semi-circular molybdenum sheets are connect respectively with filament electrode.After above-mentioned structure, structure setting is reasonable, and drawing mould has extremely strong wearability, service life is long, greatly reduces cost, improves product quality, drawing die can be used as, for sizing of metal pipe-wall, metal tube etc. to be thinned, can also be used as and press mold.
Description
Technical field
The present invention relates to a kind of chemical gas-phase deposition of diamond coating drawing mould technologies of preparing, specifically a kind of big
Aperture diamond drawing die coating Preparation equipment and preparation method, belong to metallurgical metalloid material coating technology field.
Background technology
The drawing die of large aperture serves many purposes, such as metal wire-drawing, the thinned of metal pipe-wall, sizing etc..It is drawn in tradition
It pulls out in industry, sintered-carbide die is with its cheap and be used widely, and in the drawing of diameter copper pipes, artificial gold
Hard rock drawing mould can not be completed, and hard alloy drawing mould is best selection, but the wearability of sintered carbide die is poor, mould
The service life of tool is short.And diamond thin has hardness, high elasticity modulus, the high heat for being sufficiently close to natural diamond
The excellent properties such as conductance, good self lubricity and chemical stability, so as to make it that there is wide application in tool and mould field
Prospect.With reaching its maturity for chemical CVD method depositing diamond film technology, die cost and using effect are considered, with
It is substrate that hard alloy, which draws molding tool, and one layer of Buddha's warrior attendant uniform, adhesive force can meet requirement is coated in its bore area
Stone film has become a reality, and is a kind of ideal method.
Chinese patent " preparation method of large aperture diamond coatings drawing die " (application number 02136951.8), it is proposed that
Aperture diameter is more than the hard alloy drawing die bore area of 15mm, is sunk using filament assembly instead of single vertical pulling filament CVD
The method of product micron diamond film and nano-diamond composite film.Using large aperture hard alloy drawing die as substrate, endoporus
Surface is added dropwise the cleaning of hydrogen peroxide burn into through dilute hydrochloric acid and is placed in reative cell, is formed and by round molybdenum sheet using by more heated filaments
Uniformly the squirrel-cage filament assembly of isolation distribution substitutes single heated filament, filament assembly pass through after drawing die endoporus with filament electrode
It is connected, is stretched with high temperature resistant spring, and filament assembly axis is made to coincide with die hole axis, by shortening heated filament and bore area
The distance between so that when drawing aperture diameter is more than 15mm, remains to the higher coating quality of holding and growth rate and carry
The uniformity of high coating.By adjusting CVD technological parameters (such as filament temperature, bias current power, reaction gas pressure.Carbon source concentration
With addition inert gas), to obtain micron diamond film or nano-diamond film.Aluminum steel is used for this drawing mould
Cable strand, life of the die can improve 5 times or so.
But in squirrel-cage filament assembly, the coating uniformity of bore area is improved, it can only be by increasing in filament assembly
The radical of heated filament, but heated filament radical is bigger, and the making of filament assembly is more troublesome.And with the increase heated filament radical in aperture
Increase, distance of the heated filament apart from endoporus generally takes 5-7mm, and distance is too small, and the uniformity of coating will be deteriorated, and opposite distance is too
Greatly, although being conducive to coating uniformity raising, coating quality and deposition rate can all decline.This defect causes to get over when aperture
Greatly, the effect of filament assembly is poorer, and it is not too large to limit the mold aperture diameter that can be deposited.And heated filament is laterally put
Putting can also collapse after the heating, disalignment.
Invention content
Can keep very high diamond coatings quality the technical problem to be solved in the present invention is to provide a kind of, coating it is equal
The large aperture diamond drawing die coating Preparation equipment and preparation method of the thickness of even property and coating.
In order to solve the above-mentioned technical problem, large aperture diamond drawing die coating Preparation equipment of the invention, sinks including CVD
Equipment is accumulated, the rotary table of rotation can be driven by power-equipment and be vertically installed at rotation by being equipped in CVD deposition equipment
Drawing mould on revolving worktable has the filament assembly of fixed installation in the endoporus of drawing mould；Filament assembly includes two panels half
The molybdenum sheet and the multipair vertical heated filament being arranged symmetrically on the semiorbicular molybdenum sheet of two panels of annular, the end part of every vertical heated filament
It does not connect on a piece of semiorbicular molybdenum sheet wherein, two semi-circular molybdenum sheets are connect respectively with filament electrode.
The semiorbicular molybdenum sheet of two panels is arranged symmetrically along a wherein symmetry axis for drawing mould, each vertical heat
Silk is circumferentially uniformly distributed in the endoporus of drawing mould and along the isometrical arrangement in drawing mould center.
The lower end of each pair of vertical heated filament is all connected with a horizontal heated filament and forms one group of U-shaped heated filament, and the molybdenum sheet is located at
The endoporus upper end of drawing mould.
The three line weight of axial line of the dotted line of each pair of vertical heated filament, the axial line of drawing mould and rotary table
It closes.
Cooling-water duct is provided in the rotary table.
The lower end of the filament assembly, which is mounted with, can make each vertical heated filament keep vertical weight.
A kind of preparation method based on above-mentioned large aperture diamond drawing die coating Preparation equipment, which is characterized in that including
Following steps：Drawing mould is put on rotary table vertically, and gold is deposited to drawing mould bore area in CVD deposition equipment
Hard rock coating, in deposition process, filament assembly is fixed, and rotary table at the uniform velocity rotates and then drives drawing mould at the uniform velocity
Rotation so that the drawing mould bore area and the distance between filament assembly of rotation are constant, but holding one is opposite at the uniform velocity
Movement, deposition meet following technological parameter requirement：Pressure 5-7KPa, 36 ml/min of methane, 800 ml/min of hydrogen, hot filament
2100-2300 DEG C of temperature, 700-900 DEG C of the base reservoir temperature of drawing mould obtained diamond coatings through 5-10 hours depositions.
After above-mentioned structure, drawing mould is vertically installed on the workbench of rotation, filament assembly is fixedly mounted,
The relative position of drawing mould and filament assembly is uniform, the dotted line of particularly each pair of vertical heated filament, the axial line of drawing mould
It is overlapped with three line of axial line of rotary table, the heated filament arrangement mode of use makes heated filament be uniformly distributed and be done with respect to drawing mould
With respect to uniform speed rotation,
The distance between heated filament and bore area are shortened, to keep higher quality and growth rate, ensure that drawing
The uniformity of the temperature of mold base, while the diamond coatings of the deposition of bore area is made to be uniform again；Molybdenum sheet, which is located at, to be drawn
The endoporus upper end of draft tool does not influence the rotation of drawing mould, and structure setting is reasonable, and drawing mould has extremely strong wearability,
The large aperture drawing mould friction coefficient of preparation is small, and service life is long, greatly reduces cost, improves product quality, can be with
The quality of coating is completely secured；Drawing die can be used as, for sizing of metal pipe-wall, metal tube etc. to be thinned, can also be used as and press
Mold.
Description of the drawings
Fig. 1 is the main structure diagram of large aperture diamond drawing die coating Preparation equipment of the present invention；
Fig. 2 is the drawing mould of large aperture diamond drawing die coating Preparation equipment of the present invention and filament assembly mounting structure
Schematic diagram；
Fig. 3 is the present invention looks up structural representation of Fig. 2.
Specific embodiment
With reference to the accompanying drawings and detailed description, to diamond drawing die coating Preparation equipment in large aperture of the present invention and system
Preparation Method is described in further detail.
As shown in the figure, the large aperture diamond drawing die coating Preparation equipment of the present invention, including CVD deposition equipment 1, CVD
The rotary table 2 of rotation can be driven by power-equipment and be vertically installed at rotary table by being equipped in depositing device 1
On drawing mould 3, preferably using hard alloy drawing mould of the aperture diameter more than 20mm as substrate, the usable city of the present invention
Substrate of the large aperture hard alloy drawing mould as deposition is sold, the trade mark is YG6 or YG8, and aperture diameter is ranging from：20 millis
- 200 millimeters of rice；The tool of drawing mould 3 has the filament assembly 4 of fixed installation there are one endoporus in the endoporus of drawing mould 3；Heated filament
Component 4 includes the semiorbicular molybdenum sheet of two panels and the multipair vertical heated filament being arranged symmetrically on the semiorbicular molybdenum sheet 5 of two panels, also
It is to say that wherein one in each pair of vertical heated filament is arranged on a piece of molybdenum sheet, in addition a vertical heated filament is then arranged in addition a piece of
On molybdenum sheet, the semiorbicular molybdenum sheet 5 of two panels is arranged symmetrically along a wherein symmetry axis for drawing mould, and each vertical heated filament is in drawing
It is circumferentially uniformly distributed in the endoporus of mold and along the isometrical arrangement in drawing mould center, as shown in Fig. 2, axis A is drawing mould
Center, the distance of each vertical heated filament to axis A are equal, the dotted line of each pair of vertical heated filament, the axial line of drawing mould and rotation
Three line of axial line of revolving worktable overlaps；The end of every vertical heated filament is connected on wherein a piece of semiorbicular molybdenum sheet 5,
Two semi-circular molybdenum sheets are connect respectively with filament electrode.
Wherein, the lower end of each pair of vertical heated filament is all connected with a horizontal heated filament and forms one group of U-shaped heated filament, filament assembly 4
Lower end, which is mounted with, can make each vertical heated filament keep vertical weight；Molybdenum sheet 5 is located at the endoporus upper end of drawing mould 3；Rotation
Cooling-water duct 6 is provided in workbench 2.
A kind of preparation method based on above-mentioned large aperture diamond drawing die coating Preparation equipment, includes the following steps：It draws
Draft tool 3 is put on the stent 7 of rotary table 2 vertically, and gold is deposited to 3 bore area of drawing mould in CVD deposition equipment 1
Hard rock coating, in deposition process, filament assembly 4 is fixed, and rotary table 2 at the uniform velocity rotates and then drives drawing mould 3
At the uniform velocity rotate so that the drawing mould bore area and the distance between filament assembly of rotation are constant, but keep one it is opposite
Uniform motion, deposition meet following technological parameter requirement：Pressure 5-7KPa, 36 ml/min of methane, 800 ml/min of hydrogen, heat
2100-2300 DEG C of filament temperature, 700-900 DEG C of the base reservoir temperature of drawing mould obtained diamond coatings through 5-10 hours depositions；
In this manner it is possible to it is deposited in large aperture (a diameter of 20mm-200mm) drawing mould bore area using filament CVD high-quality
The uniform diamond coatings of amount.
Referring to Fig. 2, the present invention equably arranges a plurality of U-shaped heated filament come generation using the heat safe molybdenum sheet of a pair of of semi-circular is parallel
For single heated filament, and overlap three line of axial line of the axial line of filament assembly, the axial line of drawing mould and rotary table；
Two panels semi-circular molybdenum sheet in filament assembly is connected respectively with filament electrode, aggravates in the lower end of U-shaped filament and is made using gravity
Filament keeps vertical, then deposits ultra-smooth diamond coatings with inner surface of the HFCVD methods in drawing mould；Described heated filament
Heated filament in component is tantalum wire or tungsten filament, and number is 2 to 10, and the aperture diameter of drawing die is 20mm to 200mm, heated filament away from
It is 5-7mm from drawing die bore area；Rotary table drives stent and then drawing mould is driven to carry out at the uniform velocity in deposition process
Rotation, filament assembly remains stationary so that heated filament does opposite uniform motion relative to mold, rotating speed 3-5 circles/point；Wherein, in heat
In silk component, the quantity of heated filament needs to change and be increased and decreased according to the size of drawing mould diameter of bore；Drawing mould aperture
Small, the quantity of heated filament can be lacked, and with aperture increases, the quantity of heated filament will also gradually increase.Aperture diameter and heated filament number
Amount can be selected with reference table 1：
1 component heated filament quantity of table and the relationship in drawing mould aperture
Specific implementation process of the present invention is as follows：
Using commercially available YG8 hard alloy drawing mould, aperture is Φ 45, appearance and size Φ 90*54, in drawing mould
The hard alloy on surface is pre-processed, and first with Murakami reagent etch WC phases, the etch time is 15min, then uses acid etch
Co phases are removed, are taken out after 15min, then Liquid Residue is washed away with clear water, supersound washing is cleaned and is placed in reative cell.Filament uses
The filament assembly of the present invention, heated filament are the tantalum wire of 0.6 millimeter of diameter, and radical 3, distribution diameter is 33 millimeters.In filament assembly
Semi-circular molybdenum sheet fix after be connected with filament electrode, aggravate to keep vertical heated filament using gravity in the lower end of filament assembly
Vertical state, and overlap three line of axial line of the axial line of filament assembly, the axial line of drawing mould and rotary table.Instead
Room is answered to be passed through reaction gas (methane and hydrogen) after vacuumizing, puts english and turns to drawing mould after adjustment chamber pressure, rotating speed is
4 circle per minute, then starts CVD deposition diamond coatings, technological parameter is：Pressure 7KPa, 36 ml/min of methane, hydrogen 800
Ml/min, 2200 DEG C of hot filament temperature obtained diamond coatings, it has been proved by practice that using effect of the present invention through 6 hours depositions
Well.
Claims (6)
1. a kind of large aperture diamond drawing die coating Preparation equipment, including CVD deposition equipment（1）, it is characterised in that：It is described
CVD deposition equipment（1）The rotary table of rotation can be driven by power-equipment by being inside equipped with（2）And it is vertically installed at rotation
Drawing mould on workbench（3）, the drawing mould（3）Endoporus in have the filament assembly of fixed installation（4）；The heated filament
Component（4）Including the semiorbicular molybdenum sheet of two panels and multipair in the semiorbicular molybdenum sheet of two panels（5）On the vertical heated filament that is arranged symmetrically,
The end of the every vertical heated filament is connected to wherein a piece of semiorbicular molybdenum sheet（5）On, two semi-circular molybdenum sheet difference
It is connect with filament electrode, dotted line, the axial line of drawing mould and the axial line of rotary table of each pair of vertical heated filament
Three lines overlap.
2. large aperture diamond drawing die coating Preparation equipment described in accordance with the claim 1, it is characterised in that：The two panels half
The molybdenum sheet of annular（5）It is arranged symmetrically along a wherein symmetry axis for drawing mould, each vertical heated filament is in drawing mould
It is circumferentially uniformly distributed in endoporus and along the isometrical arrangement in drawing mould center.
3. large aperture diamond drawing die coating Preparation equipment described in accordance with the claim 1, it is characterised in that：It is each pair of described perpendicular
The lower end of directly-heated silk is all connected with a horizontal heated filament and forms one group of U-shaped heated filament, the molybdenum sheet（5）Positioned at drawing mould（3）It is interior
Hole upper end.
4. large aperture diamond drawing die coating Preparation equipment described in accordance with the claim 1, it is characterised in that：The rotation work
Make platform（2）Inside it is provided with cooling-water duct（6）.
5. large aperture diamond drawing die coating Preparation equipment described in accordance with the claim 1, it is characterised in that：The heated filament group
Part（4）Lower end be mounted with the weight that each vertical heated filament can be made to keep vertical.
6. a kind of preparation method based on large aperture diamond drawing die coating Preparation equipment described in claim 1, feature exist
In including the following steps：Drawing mould（3）It is put in rotary table vertically（2）On, in CVD deposition equipment（1）In to drawing die
Tool（3）Bore area deposition of diamond coatings, in deposition process, filament assembly（4）It is fixed, rotary table（2）It is even
Speed rotates and then drives drawing mould（3）It at the uniform velocity rotates so that between the drawing mould bore area and filament assembly of rotation
Apart from constant, but an opposite uniform motion is kept, deposition meets following technological parameter requirement：Pressure 5-7KPa, methane 36
Ml/min, 800 ml/min of hydrogen, 2100-2300 DEG C of hot filament temperature, 700-900 DEG C of the base reservoir temperature of drawing mould, through 5-
Deposition obtains diamond coatings within 10 hours.
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| CN106119808A (en) * | 2016-08-24 | 2016-11-16 | 张家港合升进出口有限公司 | Cutter diamond coatings preparation facilities |
| CN108570654A (en) * | 2017-03-13 | 2018-09-25 | 深圳先进技术研究院 | A kind of wire-drawing die endoporus prepares the device of diamond coatings |
| US11680310B2 (en) | 2017-05-12 | 2023-06-20 | Continental Reifen Deutschland Gmbh | Systems for depositing coatings on surfaces and associated methods |
| JP7029134B2 (en) * | 2017-08-30 | 2022-03-03 | 一喜 下田 | Diamond manufacturing method |
| CN107937883B (en) * | 2017-12-25 | 2023-07-18 | 深圳先进技术研究院 | Device for depositing diamond coating and preparation method of deposited diamond coating |
| CN108103477A (en) * | 2018-01-29 | 2018-06-01 | 珠海中纳金刚石有限公司 | The automatic center alignment device and method of a kind of HF CVD chemical vapor deposition |
| CN110468386B (en) * | 2018-05-11 | 2024-02-09 | 深圳先进技术研究院 | Hot wire clamp, hot wire deposition equipment, application of hot wire clamp and preparation method of cutter |
| US11590527B2 (en) | 2020-04-24 | 2023-02-28 | Gvd Corporation | Systems, methods, and articles for polymer deposition |
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| CN101280423A (en) * | 2008-04-02 | 2008-10-08 | 中国工程物理研究院总体工程研究所 | Manufacturing method of small aperture diamond coating drawing die |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101560649B (en) * | 2009-06-03 | 2010-11-10 | 中南大学 | Multipurpose industrial equipment for mass production of CVD diamond film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1211635A (en) * | 1998-06-12 | 1999-03-24 | 上海交通大学 | Diamond-coated wire-drawing die |
| CN1327084A (en) * | 2001-05-31 | 2001-12-19 | 上海交通大学 | Method for preparing wire drawing mold with diamond compoiste coating |
| CN1401818A (en) * | 2002-09-12 | 2003-03-12 | 上海交通大学 | Method for mfg. large hole diamond coating drawing die |
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| CN102140627A (en) * | 2011-01-27 | 2011-08-03 | 上海交通大学 | Preparation method of planarized coating layer for diamond with ultra-large-aperture inner holes |
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