CN102337515B - Preparation method for high-temperature high-differential pressure valve of diamond coating - Google Patents
Preparation method for high-temperature high-differential pressure valve of diamond coating Download PDFInfo
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Abstract
The invention discloses a preparation method for the high-temperature high-differential pressure valve of a diamond coating, which belongs to the technical field of diamond manufacture. A preprocessed WC (Wolfram Carbide)-Co hard alloy YG6 or SiC/Si3N4 ceramic serves as a coating substrate material to prepare a diamond coating valve seat with a direct-pull perforation hot-wire method; the preprocessed WC-Co hard alloy YG6 serves as a coating substrate material to prepare a diamond coating valve plug with a step arrangement hot-wire method; finally, the valve plug is clamped by a valve plug clip and is fixedly connected with a valve rod by a thread and a pin; and the valve seat is thermally embedded into a pressing sleeve and passes through a bushing and a restriction orifice to be arranged in the cavity of a valve body to obtain the high-temperature high-differential pressure valve of the diamond coating. In the preparation method, the hot-wire chemical vapor deposition is adopted to realize by two technical schemes of the direct-pull perforation hot-wire method and the step arrangement hot-wire method, thereby greatly prolonging the service life of the original reducing valve, and bringing a significant meaning for guaranteeing the safe operation of the equipment.
Description
Technical field
What the present invention relates to is a kind of method of diamond fabrication technical field, specifically is the preparation method of the big pressure reduction reducing valve of a kind of high temperature high solid content diamond coatings spool, valve seat.
Background technology
The big pressure reduction reducing valve of high temperature high solid content is operated under the extreme operating condition condition of high temperature, solid particle erosion and gas-solid-liquid multiphase medium effect, 420-500 ℃ of its medium temperature, and the front and back pressure reduction of valve reaches as high as 19MPa, solid content 20-60%.Because the envrionment conditions of reducing valve work is extremely harsh, simultaneously requirement can long-term stable operation again, therefore require high temperature resistant, the big pressure reduction of reducing valve energy, anti-washing away and erosion corrosion, and can under high viscosity, there be obstruction, noiselessness, life-span is long, and sealing is reliable, and conventional reducing valve is difficult to satisfy these requirements.Finish program behavior under the High Pressure Difference condition, the work-ing life of valve and reliability just must be guaranteed, and the requirement of spool, seat material selection aspect is very harsh.At present, High Temperature High Pressure difference limen door uses W-Co kind Wimet, sintering metal and nitrogen carbide hard coat thereof as the material of wear resistant appliance more, under the operating mode of the high erosion of High Temperature High Pressure, traditional Wimet reducing valve spool, seat material are very easy to erosive wear, can't meet the demands work-ing life, has a strong impact on the raising of the normal operation of equipment and throughput.Even the WC Wimet that has adopted hardness to reach 23GPa is made spool and valve seat, the erosion resistance effect of valve is also undesirable, therefore under the prerequisite of taking all factors into consideration manufacturing cost and work-ing life, should adopt hardness and wear resistance higher superhard material and superhard coating as far as possible.
As everyone knows, diamond is the hardest material of occurring in nature, adopt high-pressure high-temperature technology (High Pressure and High Temperature, HPHT) He Cheng high quality polycrystalline diamond (Polycrystalline Diamond, abbreviation PCD) had the high rigidity near natural diamond, high Young's modulus, excellent properties such as high thermal conductivity and chemical stability, on this basis, PCD and carbide matrix material be can be made into polycrystalline diamond compacts (PDCs) (Polycrystalline Diamond Compact again by the High Temperature High Pressure sintering, be called for short PDC), further also can adopt low temperature, low-pressure chemical vapor deposition (Chemical Vapor Deposition, abbreviation CVD) method is at carbide matrix material surface-coated diamond thin, above-mentioned two kinds of technological development high performance composite and top coat, both kept diamond hardness and wear-resisting, abrasion-resistance, have Wimet toughness and workability again, therefore, at the high solid High Pressure Difference reducing valve valve material of high temperature, a kind of innovative idea is exactly that research and development are suitable for resistance to wearing under the extreme operating condition condition, erosion resistance, acid gilding hard rock valve material---PCD diamond, PDC diamond composite and CVD diamond film coating layer, satisfy high temperature, high pressure, particular surroundings multiphase mediums such as particle erosion are the service requirements of the extreme wear working condition condition of representative, for the work-ing life that prolongs the valve key part significantly, guarantee that the highly effective and safe reliability service of production unit is significant.
Find through the literature search to prior art, Chinese patent " a kind of high-temperature high-pressure difference pressure-reducing valve " (patent No. ZL200810202758.8) has been put down in writing a kind of structure of high-temperature high-pressure difference pressure-reducing valve, can be to high temperature, the fluid of high solid content reduces pressure, produce desired big pressure reduction, and from the angle of structural design optimization, prevent the medium flow harsh erosive wear that flow at high speed forms material under big pressure reduction condition of high solid content, on this basis, " a kind of manufacture method of polycrystalline diamond complex valve base of pressure reducing valve " (ZL200910047277.9) prepared polycrystalline diamond complex (PDC) valve base of pressure reducing valve by the High Temperature High Pressure in-situ sintering, be applied to the big pressure reduction reducing valve of high temperature high solid content, have wear-resistant, the anti-impact erosion, the long lifetime characteristics, but this method only is applicable to the preparation of valve base of pressure reducing valve, can't use for the spool that erosive wear is even more serious, and the High Temperature High Pressure sintering is made polycrystalline diamond complex, the equipment complexity, the cost height, particularly for the preparation (aperture is greater than 12 millimeters) of wide aperture valve seat, because factors such as price and technology adopt the PCD diamond, the PDC diamond composite is very difficult.
Chemical vapor deposition diamond film has the premium properties of many uniquenesses, it has near the hardness of natural diamond and wear resistance, has low-friction coefficient, low thermal coefficient of expansion, characteristic such as high heat conductance and high chemical stability, successful diamond synthesis film is so far on heterogeneous matrix from the beginning of the eighties in last century, no matter the CVD diamond is from growth theory, the preparation method, preparation quality and performance characterization, still all obtained huge progress from following process technology and applied research aspect, thereby make its as wear-resistant coating at cutting tool, drawing mould and wear-resistant devices field have broad application prospects, and can effectively solve high rigidity, high-wearing feature and thermotolerance problem.Up to the present do not find as yet the CVD diamond thin to be expanded the report that is applied on the big pressure reduction reducing valve of the high temperature high solid content valve material both at home and abroad.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of preparation method of diamond coatings High Temperature High Pressure difference limen is provided, adopt hot filament CVD to realize by perforation vertical pulling heated filament and two kinds of technical schemes of step arrangement heated filament, can increase substantially the work-ing life of original reducing valve, significant to the safe operation that guarantees equipment.
The present invention is achieved by the following technical solutions, the present invention adopt pretreated WC-Co Wimet YG6 or SiC Si
3N
4Pottery is as the coated substrate material, by vertical pulling perforation heated filament preparing diamond coatings by using valve seat; And adopt through pretreated WC-Co Wimet YG6 as the coated substrate material, by step arrangement heated filament preparing diamond coatings by using spool, last spool is by the spool clamping, use screw thread to fixedly connected with valve rod with pin again, valve seat obtains diamond coatings High Temperature High Pressure difference limen by gland, lining, throttling orifice plate and body cavity assembling.
Described pre-treatment refers to: be immersed in as the cemented carbide substrate of valve seat or spool and carry out ultrasonic cleaning in the Murakami solution, again cemented carbide substrate is immersed in and carries out etching in the Caro mixed acid solution to remove the cobalt element (Co) of underlayer surface, grind pre-treatment with the W10 diamond powder at lathe at last.
The composition of described Murakami solution is potassium hydroxide (KOH), the Tripotassium iron hexacyanide (K
3(Fe (CN)
6)) and water (H
2O), its quality proportioning is KOH: K
3(Fe (CN)
6): H
2O=1: 1: 10.
The composition of described Caro mixed acid solution is the vitriol oil (H
2SO
4) and hydrogen peroxide (H
2O
2), its volume proportion is H
2SO
4: H
2O
2=1: 10.
In the described pre-treatment, as the SiC of valve seat Si
3N
4Pottery directly adopts W10 or the W1 diamond powder carries out respectively on lathe slightly, the smooth grinding pre-treatment.
Described vertical pulling perforation hot wire process refers to: with driving source, be that heated filament passes the substrate endoporus and places the shaft core position of substrate endoporus, with the stretching heated filament of high temperature resistant spring, by the temperature distortion of control heated filament, make it be in shaft core position all the time and in the CVD deposition process, remain straight and upright state, obtain valve seat through post precipitation;
Described heated filament can be further along with the increase of valve base aperture replaces single heated filament with many hank knottings, or adopt many filament assemblies of squirrel-cage to substitute single vertical pulling heated filament and hank knotting.
Apply a direct current bias voltage between described heated filament and the substrate endoporus to form DC bias current, in order between filament assembly and substrate bore surface, produce direct-current plasma, accelerate adamantine deposition.
Described vertical pulling perforation hot wire process specifically refers to:
A) at the valve seat of diameter of bore d≤6 millimeter, adopt diameter 0.4～0.8mm, the single vertical pulling heated filament of heater power 500～600W passes endoporus and places shaft core position;
B) at the valve seat of diameter of bore 6＜d≤30 millimeter, the hank knotting that adopts the heated filament of 2-3 root, every diameter 0.3～0.6mm, every power 1000～1400W to form passes endoporus and places shaft core position;
C) at the valve seat of diameter of bore 30＜d≤50 millimeter, the squirrel-cage filament assembly that adopts the heated filament of 3-6 root, every diameter 0.4～0.8mm, every power 2000～2300W to form passes endoporus and places shaft core position;
Adopt reaction gas pressure: 30～35Torr, carbon source concentration: 1～3%, 800～950 ℃ of underlayer temperatures, bias current: 1.0～4.0A is through obtaining having the valve seat of diamond coatings in 4～17 hours after the deposition.
Described step arrangement hot wire process refers to: by to upper and lower two pairs, totally four heated filaments perpendicular with being vertically placed on valve core axis's direction on the water-cooled worktable apply the power of 500～900W, realize optimum depositing temperature field distribution, after deposition, obtain having the spool of diamond coatings.
Diameter 4≤d≤20 of described spool millimeter;
Diameter 0.4～the 0.8mm of described heated filament;
Described deposition refers to: reaction gas pressure: 1.625～3.325KPa, and carbon source concentration: 1～3%, the underlayer temperature of valve core material: 750～950 ℃, bias current: 0～0.1A is through obtaining the conventional diamond layer of 8～12 micron thickness in 5-8 hour after the deposition.
The hot wire structure up and down of described step arrangement hot wire process distributes for the growth of the diamond coatings of major diameter spool solid of revolution provides suitable temperature field.The hot wire structure that level is installed is easy to adjust relative height and spacing between heated filament, need not the spool base portion of coating, away from heated filament, covers with the molybdenum suitcase, is protected effectively.
The diamond coatings valve seat of the present invention's preparation, spool can be used for all kinds of High Temperature High Pressure differences and contain solid material reducing valve.
Description of drawings
Fig. 1 arranges synoptic diagram for the diamond coatings valve seat prepares heated filament;
Fig. 2 diamond coatings spool heated filament is arranged synoptic diagram.
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The first step, valve seat coating are handled
Valve seat is the YG6 carboloy, physical dimension is 78 * 28 millimeters of φ, 48 millimeters of aperture φ, bore surface carries out ultrasonic cleaning in 30 minutes in Murakami solution, make the alligatoring of Wimet endoporus substrate surface, wherein the composition of Murakami solution is potassium hydroxide (KOH), the Tripotassium iron hexacyanide (K
3(Fe (CN)
6)) and water (H
2O), its quality proportioning is KOH: K
3(Fe (CN)
6): H
2O=1: 1: 10.Cemented carbide substrate is immersed in the etching of carrying out 1 minute in the Caro mixed acid solution to remove the cobalt element (Co) of underlayer surface, wherein the composition of Caro mixed acid solution is the vitriol oil (H again
2SO
4) and hydrogen peroxide (H
2O
2), its volume proportion is HCl: H
2O
2=1: 10, clean dry is placed in the reaction chamber.Hot filament adopts the squirrel-cage filament assembly, and total 0.5 millimeter tantalum wire of φ is 4 in the assembly, and evenly separates on the shape molybdenum sheet of the garden of 40 millimeters of φ.Filament assembly links to each other with filament electrode after passing endoporus, and is stretching with high temperature resistant spring, and assembly axis and interior axially bored line are coincided.Reaction chamber vacuumizes the back and feeds reactant gases (hydrogen and acetone), begin the CVD deposition of diamond coatings after adjusting chamber pressure, processing parameter is: pressure 35Torr, 700 millimeters/minute of total gas flow rates, acetone/hydrogen are 1.5% (volume ratio), and the hot filament heating power is 2.1KW, about 2200 ℃ of filament temperature, the about 4A of direct current positive bias, after depositing in 15 hours, the nib surface deposition obtains about 38 microns diamond coatings.
Second step, spool coating are handled
Spool is the YG6 carboloy, and end diameter is φ 12mm, and the leading portion core is long to be 30mm, and the spool length overall is 66 millimeters.Place the Murakami agent to carry out ultrasonic erosion above-mentioned spool leading portion, the prescription of corrosive fluid (weight ratio) Tripotassium iron hexacyanide: potassium hydroxide: water is 1: 1: 10, about 25 minutes of time, after washing, taking-up place the dioxysulfate aqueous solution (volume ratio 1: 10) to corrode for 30 seconds again, place diadust (20 microns of granularities) alcohol suspension sonic oscillation to handle after cleaning again 20 minutes, clean then and dry up, spool is placed on the water cooling platform of heated filament CVD reaction chamber the deposition of beginning diamond coatings.It directly is the tantalum wire of φ 0.8 that heated filament adopts two pairs of lines, 35 millimeters of tantalum wire spacings, and wherein a pair of height is identical with the end of spool, and another is to then low 25 millimeters.Reaction chamber vacuumizes the back and feeds reactant gases (hydrogen and acetone), the deposition of beginning CVD diamond coatings behind the adjustment chamber pressure, processing parameter is: pressure 10-25Torr, total gas flow rate 700 ml/min, acetone/Hydrogen gas (volume ratio) is 2%, the tantalum wire temperature is about 2100 ℃, and after depositing through 3 hours, the end deposition obtains the diamond coatings of about 6-8 micron thickness.Spool position revolved turn 90 degrees, carry out 3 hours depositions again with same processing parameter, obtain the diamond coatings of about 12 micron thickness, and can effectively guarantee coating uniformity.This spool service life as compared Wimet improves more than 8 times.
The 3rd step, spool are by the spool clamping, use screw thread to fixedly connected with valve rod with pin again, filler need be arranged in space between valve rod and the body cavity, the lantern cover, obturators such as metallic O ring, and fix with gland, valve seat carries out temperature difference press fit arrangement and is provided with lining, throttling orifice plate and body cavity assembling in gland inside, bottom.
Embodiment 2
Present embodiment may further comprise the steps:
Valve seat is the silicon carbide ceramics of reaction sintering, and physical dimension is 45 * 25 millimeters of φ, 20 millimeters of aperture φ, and bore surface is placed in the reaction chamber through the grinding of diamond micro mist, clean dry.Hot filament adopts 0.7 millimeter heated filament hank knotting of 2 φ, and the heated filament hank knotting links to each other with filament electrode after passing endoporus, and is stretching with high temperature resistant spring, and assembly axis and interior axially bored line are coincided.Reaction chamber vacuumizes the back and feeds reactant gases (hydrogen and acetone), begin the CVD deposition of diamond coatings after adjusting chamber pressure, processing parameter is: pressure 32Torr, 700 millimeters/minute of total gas flow rates, acetone/hydrogen are 1.5% (volume ratio), and the hot filament heating power is 1.3KW, about 2200 ℃ of filament temperature, the about 3A of direct current positive bias, after depositing in 9 hours, the nib surface deposition obtains about 35 microns diamond coatings.
Plating CVD diamond coatings on spool, spool is the YG6 carboloy, and end diameter is φ 6, and the leading portion core is long to be 20mm, and the spool length overall is 42 millimeters.Pretreatment process is identical with embodiment 1 spool, places on the water cooling platform of heated filament CVD reaction chamber the deposition of beginning diamond coatings.It directly is the tantalum wire of φ 0.6 that heated filament adopts two pairs of lines, 40 millimeters of tantalum wire spacings, and wherein a pair of height is identical with the end of spool, and another is to then low 20 millimeters.Reaction chamber vacuumizes the back and feeds reactant gases (hydrogen and acetone), the deposition of beginning CVD diamond coatings behind the adjustment chamber pressure, processing parameter is: pressure 10-25Torr, total gas flow rate 700 ml/min, acetone/Hydrogen gas (volume ratio) is 2%, the tantalum wire temperature is about 2100 ℃, and after depositing through 3 hours, blade place deposition obtains the diamond coatings of about 4-7 micron thickness.Spool position revolved turn 90 degrees, carry out 3 hours depositions again with same processing parameter, obtain the diamond coatings of about 10 micron thickness, and can effectively guarantee coating uniformity, the service life as compared Wimet improves more than 8 times.
Embodiment 3
Present embodiment may further comprise the steps:
Valve seat is the YG6 carboloy, physical dimension is 20 * 12 millimeters of φ, 6 millimeters of aperture φ, the bore surface pretreatment process is identical with embodiment 1 valve seat, hot filament links to each other with filament electrode after adopting 0.7 millimeter single tantalum wire of φ to pass nib, stretching with high temperature resistant spring, and assembly axis and nib axis are coincided.Reaction chamber vacuumizes the back and feeds reactant gases, begin the CVD deposition of diamond coatings after adjusting chamber pressure, processing parameter is: pressure 30Torr, 700 millimeters/minute of total gas flow rates, acetone/hydrogen are 1.5% (volume ratio), and the hot filament heating power is 0.6KW, about 2200 ℃ of filament temperature, the about 1A of direct current positive bias, after depositing in 5 hours, the nib surface deposition obtains about 28 microns diamond coatings.
Plating CVD diamond coatings on spool, spool is the YG6 carboloy, and end diameter is φ 4, and the leading portion core is long to be 18mm, and the spool length overall is 35 millimeters.Pretreatment process is identical with embodiment 1 spool, places on the water cooling platform of heated filament CVD reaction chamber the deposition of beginning diamond coatings.It directly is the tantalum wire of φ 0.5 that heated filament adopts two pairs of lines, 40 millimeters of tantalum wire spacings, and wherein a pair of height is identical with the end of spool, and another is to then low 16 millimeters.Reaction chamber vacuumizes the back and feeds reactant gases (hydrogen and acetone), the deposition of beginning CVD diamond coatings behind the adjustment chamber pressure, processing parameter is: pressure 10-25Torr, total gas flow rate 700 ml/min, acetone/Hydrogen gas (volume ratio) is 2%, the tantalum wire temperature is about 2100 ℃, and after depositing through 3 hours, blade place deposition obtains the diamond coatings of about 4-5 micron thickness.Spool position revolved turn 90 degrees, carry out 3 hours depositions again with same processing parameter, obtain the diamond coatings of about 9 micron thickness, and can effectively guarantee coating uniformity, the service life as compared Wimet improves more than 6 times.
Claims (1)
1. the preparation method of a diamond coatings High Temperature High Pressure difference limen is characterized in that, adopts pretreated WC-Co Wimet YG6 or SiC Si
3N
4Pottery is as the coated substrate material, by vertical pulling perforation heated filament preparing diamond coatings by using valve seat; And adopt through pretreated WC-Co Wimet YG6 as the coated substrate material, by step arrangement heated filament preparing diamond coatings by using spool, last spool is by the spool clamping, use screw thread to fixedly connected with valve rod with pin again, valve seat obtains diamond coatings High Temperature High Pressure difference limen by gland, lining, throttling orifice plate and body cavity assembling;
In the described pre-treatment: will be immersed in as the WC-Co Wimet YG6 substrate of valve seat or spool and carry out ultrasonic cleaning in the Murakami solution, again cemented carbide substrate is immersed in and carries out etching in the Caro mixed acid solution to remove the cobalt element (Co) of underlayer surface, grind pre-treatment with the W10 diamond powder at lathe at last; The composition of described Murakami solution is KOH, K
3(Fe (CN)
6) and H
2O, its quality proportioning is KOH:K
3(Fe (CN)
6): H
2O=1:1:10; The composition of described Caro mixed acid solution is H
2SO
4And H
2O
2, its volume proportion is H
2SO
4: H
2O
2=1:10;
Will as the SiC of valve seat Si
3N
4Pottery directly adopts W10 or the W1 diamond powder carries out respectively on lathe slightly, the smooth grinding pre-treatment;
Described vertical pulling perforation hot wire process refers to: with driving source, be that single heated filament, many hank knottings or many filament assemblies of squirrel-cage pass the substrate endoporus and place the shaft core position of substrate endoporus, with the stretching heated filament of high temperature resistant spring, by the temperature distortion of control heated filament, make it be in shaft core position all the time and in the CVD deposition process, remain straight and upright state, obtain valve seat through post precipitation;
Between heated filament and substrate endoporus, apply direct-current biasing to form DC bias current, in order between filament assembly and substrate bore surface, produce direct-current plasma, accelerate adamantine deposition;
A) at the valve seat of diameter of bore d≤6 millimeter, adopt diameter 0.4 ~ 0.8mm, the single vertical pulling heated filament of heater power 500 ~ 600W passes endoporus and places shaft core position;
B) at the valve seat of diameter of bore 6＜d≤30 millimeter, the hank knotting that adopts the heated filament of 2-3 root, every diameter 0.3 ~ 0.6mm, every power 1000 ~ 1400W to form passes endoporus and places shaft core position;
C) at the valve seat of diameter of bore 30＜d≤50 millimeter, the squirrel-cage filament assembly that adopts the heated filament of 3-6 root, every diameter 0.4 ~ 0.8mm, every power 2000 ~ 2300W to form passes endoporus and places shaft core position;
Adopt reaction gas pressure: 30 ~ 35Torr, carbon source concentration: 1 ~ 3%, 800 ~ 950 ° of C of underlayer temperature, bias current: 1.0 ~ 4.0A is through obtaining having the valve seat of diamond coatings in 4 ~ 17 hours after the deposition;
Described step arrangement hot wire process refers to: by to upper and lower two pairs, totally four heated filaments perpendicular with being vertically placed on valve core axis's direction on the water-cooled worktable apply the power of 500 ~ 900W, realize optimum depositing temperature field distribution, after deposition, obtain having the spool of diamond coatings; Diameter 4≤d≤20 of spool millimeter; Diameter 0.4 ~ the 0.8mm of heated filament; Reaction gas pressure during deposition: 1.625 ~ 3.325KPa, carbon source concentration: 1 ~ 3%, the underlayer temperature of valve core material: 750 ~ 950 ° of C, bias current: 0 ~ 0.1A is through obtaining the conventional diamond layer of 8 ~ 12 micron thickness in 5-8 hour after the deposition.
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Cited By (1)
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| CN105803419A (en) * | 2016-04-27 | 2016-07-27 | 富耐克超硬材料股份有限公司 | Cobalt leaching solution system, hard alloy cobalt leaching method and blade with diamond coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1060537C (en) * | 1998-06-12 | 2001-01-10 | 上海交通大学 | Diamond-coated wire-drawing die |
| CN101403448B (en) * | 2008-11-14 | 2010-09-01 | 上海化工研究院 | High-temperature high-pressure difference pressure-reducing valve |
| CN102061453B (en) * | 2011-01-27 | 2012-11-21 | 上海交通大学 | Hot-filament chemical vapor deposition batch preparation method of complicated-shape diamond coated cutting tool |
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2011
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| CN105803419A (en) * | 2016-04-27 | 2016-07-27 | 富耐克超硬材料股份有限公司 | Cobalt leaching solution system, hard alloy cobalt leaching method and blade with diamond coating |
| CN105803419B (en) * | 2016-04-27 | 2018-12-21 | 富耐克超硬材料股份有限公司 | De- cobalt liquor system and hard alloy take off cobalt method and diamond coatings blade |
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