Summary of the invention
The purpose of this invention is to provide a kind of heavy duty x-ray tube preparation method, can prepare that the X spool is used in the high-power Medical CT machine, have good heat radiating, anode target material that radiating efficiency is high with WMo graphite composite anode target.
The technical solution adopted in the present invention is, a kind of heavy duty x-ray tube carries out according to the following steps with the preparation method of WMo graphite composite anode target:
Step 1: calculate respectively require the quality of tungsten powder and molybdenum powder in the target
Target size as requested, by formula m=ρ π r
2H calculates the quality of tungsten powder and molybdenum powder respectively, in the formula: m for the quality of the tungsten powder of asking or molybdenum powder, ρ is the density of tungsten or molybdenum, h is the height of tungsten layer or molybdenum layer, r is the target radius;
Step 2: prepare tungsten powder material and molybdenum powder material respectively
1 quality that calculates is got tungsten powder set by step, and tungsten powder purity is 99.5%~99.9%, particle diameter is 1 μ m~6 μ m, is the glycerol that 5ml/kg gets purity assay by the tungsten powder mass volume ratio, put into batch mixer, mixed 6 hours~10 hours, then with 40 orders~60 purpose sieves screening, obtain the tungsten powder material
1 quality that calculates is got molybdenum powder set by step, and molybdenum powder purity is 99.5%~99.9%, particle diameter is 1 μ m~6 μ m, is the glycerol that 5ml/kg gets purity assay by the molybdenum powder mass volume ratio, put into batch mixer, mixed 6 hours~10 hours, and with 40 orders~60 mesh sieves screening, obtained the molybdenum powder material then;
Step 3: the quality of determining each component in the binding agent
M by formula
1=ρ π r
2H calculates the quality of binding agent, in the formula, and m
1Be the quality of binding agent, h gets 0.1mm, and ρ is the mixed solid density of titanium nickel zirconium, gets 6.148 gram per centimeters
3, r is the radius of made target,
Determine the quality of Ti, Ni and Zr according to 1/3 of the quality of above-mentioned binding agent,
According to the quality of above-mentioned binding agent, press mass volume ratio 50ml/kg, determine the volume of absolute ethyl alcohol;
Step 4: preparation binding agent
Draw the quality of Ti, Ni, Zr and the volume of absolute ethyl alcohol according to step 3, the absolute ethyl alcohol that get purity respectively and be 99.5%~99.8%, particle diameter is not more than titanium valve, nickel powder, zirconium powder and the purity assay of 10 μ m, and put into batch mixer, and mixed 2 hours~4 hours, obtain binding agent;
Step 5: spread stacked pressure
Requirement for height by each layer, layering bonding agent that step 4 is obtained, molybdenum powder material and the tungsten powder material that step 2 makes are spread in the steel mold successively, under the pressure of 500MPa~800MPa, suppress 2min~4min, deviate from from mould with the pressing pressure of 200MPa~300MPa then, obtain the composite green compact that forms successively by fixed tack coat, molybdenum powder layer and tungsten powder layer;
Step 6: sinter molding
The composite green compact that graphite and step 5 make is put into graphite jig successively, and the tack coat of composite green compact contacts with graphite, and it is that 50MPa~100MPa, vacuum degree are 2.8 * 10 that this graphite jig is placed pressure
-3Pa~6.6 * 10
-3Pa, temperature are that sintering 1 hour~2 hours obtains the target blank in 2200 ± 10 ℃ the vacuum heating-press sintering stove;
Step 8: grinding
The target blank that the last step was obtained is installed on the dynamic equilibrium machine, and grinding promptly makes heavy duty x-ray tube WMo graphite composite anode target.
The invention has the beneficial effects as follows:
1. the tungsten that fusing point is the highest in the selection metal is as the target surface material, and tungsten fusing point height, steam force down, density reaches the atomic number height greatly, can produce a large amount of X ray under beam bombardment.The molybdenum of selecting Heat stability is good is as transition zone, by very high heat capacity and heat-sinking capability are strong, density is little graphite as carriage.Not only reduced the volume and weight of CT machine anode target material, and solved well the heat dissipation problem of anode target material, the useful life of having improved target.
2. the leading indicator of the target for preparing near or surpass external like product.Broken external monopolization to this technology, the inspection fee when having reduced health check-up simultaneously has obvious practical significance to the reform of China's medical system from now on.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
The inventive method adopts powder metallurgy technology, with purity be 99.5%~99.9%, particle diameter is tungsten powder and the molybdenum powder of 1 μ m~6 μ m, adopt a certain amount of binding agent (mass ratio Ti of each component: Ni: Zr=1: 1: 1) spread layer bonding with high-purity, high-strength, highly dense graphite, the shop layer structure of each component is followed successively by tungsten powder layer 1, molybdenum powder layer 2, adhesive layer 3 and graphite linings 4 as shown in Figure 1 from top to bottom.Then, under the pressing pressure of 500MPa~800MPa, be cold-pressed into the green compact of certain diameter.It is 2.8 * 10 that these green compact are placed vacuum degree
-3Pa~6.6 * 10
-3Pa, temperature are that 2200 ℃ ± 10 ℃, pressure are sintering 1 hour~2 hours in the vacuum hotpressing stove of 50MPa~100MPa, and grinding then promptly makes heavy duty x-ray tube with WMo graphite composite anode target.
Above-mentioned high-power be that the maximum power of Medical CT machine is above 100 kilowatts.
The inventive method, carry out according to the following steps:
Step 1: the quality that calculates tungsten powder and molybdenum powder respectively
According to the size of customer requirements target, m=ρ π r by formula
2H calculates the quality of tungsten powder and molybdenum powder, in the formula, m for the quality of the tungsten powder of asking or molybdenum powder, ρ is that the density of tungsten or molybdenum (is respectively 19.3 gram per centimeters
3, 10.3 gram per centimeters
3), h is the height of tungsten layer or molybdenum layer, r is the target radius,
Step 2: prepare tungsten powder material and molybdenum powder material respectively
1 quality that calculates is got tungsten powder set by step, the purity of tungsten powder is 99.5%~99.9%, particle diameter is 1 μ m~6 μ m, mass volume ratio by tungsten powder is the glycerol that 5ml/kg gets purity assay, put into batch mixer in the lump, mixed 6 hours~10 hours, sieve with 40 orders~60 purpose sieves then, obtain the tungsten powder material
1 quality that calculates is got molybdenum powder set by step, the purity of molybdenum powder is 99.5%~99.9%, particle diameter is 1 μ m~6 μ m, mass volume ratio by molybdenum powder is the glycerol that 5ml/kg gets purity assay, put into batch mixer in the lump, mixed 6 hours~10 hours, sieve with 40 orders~60 mesh sieve then, obtain the molybdenum powder material;
Step 3: the quality of determining each component in the binding agent
M by formula
1=ρ π r
2H calculates the quality of binding agent, in the formula, and m
1Be the quality of asking binding agent, h gets 0.1mm, and ρ is the mixed solid density of titanium valve, nickel powder and zirconium powder, gets 6.148 grams per cubic centimters, and r is the radius of made target,
According to the quality of above-mentioned binding agent, press the mass ratio of each component: Ti: Ni: Zr=1 again: 1: 1, determine the quality of Ti, Ni and Zr,
According to the quality of above-mentioned binding agent, press the mass volume ratio of 50ml/kg, determine the volume of absolute ethyl alcohol;
Step 4: preparation binding agent
The quality of 3 Ti that draw, Ni, Zr and the volume of absolute ethyl alcohol set by step, the absolute ethyl alcohol that get purity respectively and be 99.5%~99.8%, particle diameter is not more than titanium valve, nickel powder, zirconium powder and the purity assay of 10 μ m, above-mentioned raw materials is put into batch mixer, mixed 2 hours~4 hours, and obtained binding agent;
Step 5: spread stacked pressure
The binding agent that step 4 is obtained, the molybdenum powder material that step 2 makes and tungsten powder material are packed in the steel mold successively, control the height composite demand of each layer, under the pressure of 500MPa~800MPa, suppress, keep this pressure 2min~4min, deviate from from mould with the pressing pressure of 200MPa~300MPa then, obtaining the lower end is tack coat, and middle is that molybdenum layer, upper end are the composite green compact of tungsten layer;
Step 6: sinter molding
The composite green compact that graphite and step 5 make is put into graphite jig successively, and the tack coat of composite green compact contacts with graphite, and it is that 50MPa~100MPa, vacuum degree are 2.8 * 10 that this graphite jig is placed pressure
-3Pa~6.6 * 10
-3Pa, temperature are in 2200 ± 10 ℃ the vacuum heating-press sintering stove, sintering 1 hour~2 hours, and sinter molding obtains the target blank;
Step 7: grinding
The target blank that the last step was obtained is installed on the dynamic equilibrium machine, adjusts balance, and it is carried out grinding, until satisfying the drawing dimensional requirement, promptly makes heavy duty x-ray tube WMo graphite composite anode target.
Embodiment 1
Producing diameter is 20mm, highly is the W/Mo/ graphite composite target material of 48mm, and wherein tungsten layer thickness is 2mm, and molybdenum layer thickness is 6mm, and graphite linings thickness is 40mm (containing adhesive layer thickness 0.1mm).
According to formula m=ρ π r
2H calculates the quality of tungsten powder and molybdenum powder respectively.Get purity and be 99.5%, particle diameter is tungsten powder 16.16 grams of 1 μ m~6 μ m, press mass volume ratio 5ml/kg with tungsten powder, calculate and get the glycerol 0.10ml of purity assay, above-mentioned raw materials is put into batch mixer, mixed 6 hours, after evenly mixing, sieve, obtain the tungsten powder material with 40 purpose sieves.Get purity and be 99.5%, particle diameter is molybdenum powder 19.26 grams of 1 μ m~6 μ m, by with the mass volume ratio 5ml/kg of molybdenum powder, calculate and get the glycerol 0.08ml of purity assay, molybdenum powder and glycerol are put into batch mixer, mix after 6 hours, sieve, obtain the molybdenum powder material with 40 purpose sieves.According to m
1=ρ π r
2H calculates the quality of required binding agent, in the formula, and h=0.1mm, ρ=6.148 gram per centimeters
3R=20mm, press the mass ratio Ti of each component of binding agent: Ni: Zr=1: 1: 1 again, calculate the quality of Ti, Ni, Zr, titanium valve 0.64 gram, nickel powder 0.64 gram, zirconium powder 0.64 gram that get purity respectively and be 99.5%, particle diameter are not more than 10 μ m according to the volume mass percentage of 50ml/kg, calculate and get absolute ethyl alcohol 0.097ml then, titanium valve, nickel powder, zirconium powder and absolute ethyl alcohol are put into batch mixer mixed 2 hours, make binding agent.The binding agent, molybdenum powder material and the tungsten powder material that obtain are packed in the steel pressing mold tool successively, under the pressing pressure of 500MPa, pressurize 2min moulding, the pressing pressure with 200MPa is deviate from from mould then, obtains the composite green compact that is formed by fixed successively tack coat, molybdenum powder layer and tungsten powder layer.With diameter is 20mm, and thickness is that graphite and this composite green compact of 40mm put into graphite jig successively, and the tack coat of composite green compact is contacted with graphite, and it is that 50MPa, vacuum degree are 2.8 * 10 that this graphite jig is placed pressure
-3Pa, temperature are in 2190 ℃ the vacuum heating-press sintering stove, to be incubated 1 hour sinter molding.Make diameter and be 20mm, highly be the W/Mo/ graphite composite target material blank of 48mm, this composite target material blank is installed in the dynamic equilibrium machine raises the leveling weighing apparatus, and grinding promptly makes heavy duty x-ray tube WMo graphite composite anode target to satisfying the drawing dimensional requirement.
Embodiment 2
Producing diameter is 60mm, highly is the W/Mo/ graphite composite anode target of 40mm, and wherein, tungsten layer thickness is 1.5mm, and molybdenum layer thickness is 5.5mm, and graphite linings thickness is 33mm (containing adhesive layer thickness 0.1mm).
According to formula m=ρ π r
2H calculates the quality of tungsten powder and molybdenum powder respectively.Get purity and be 99.7%, particle diameter is tungsten powder 81.86 grams of 1 μ m~6 μ m, by with the mass volume ratio 5ml/kg of tungsten powder, calculate and get the glycerol 0.41ml of purity assay, above-mentioned raw materials is put into batch mixer, mix after 8 hours, sieve, obtain the tungsten powder material with 50 purpose sieves.Get purity and be 99.7%, particle diameter is molybdenum powder 158.93 grams of 1 μ m~6 μ m, press mass volume ratio 5ml/kg with molybdenum powder, calculate and get the glycerol 0.80ml of purity assay, molybdenum powder and glycerol are put into batch mixer, mix after 8 hours, sieve with 50 purpose sieves, obtain the molybdenum powder compound.Press m
1=ρ π r
2H calculates the quality of required binding agent, in the formula, and h=0.1mm, ρ=6.148 gram per centimeters
3R=60mm, press the mass ratio Ti of each component of binding agent: Ni: Zr=1: 1: 1 again, calculate the quality of Ti, Ni, Zr, titanium valve 5.79 grams, nickel powder 5.79 grams and zirconium powder 5.79 grams that get purity respectively and be 99.6%, particle diameter are not more than 10 μ m than 50ml/kg, calculate and get the absolute ethyl alcohol 0.87ml of purity assay according to volume mass, titanium valve, nickel powder, zirconium powder and absolute ethyl alcohol are put into batch mixer mixed 3 hours, make binding agent.The binding agent, molybdenum powder material and the tungsten powder material that obtain are packed in the steel pressing mold tool successively, under the pressing pressure of 600MPa, pressurize 3min moulding, the pressing pressure with 250MPa is deviate from from mould then, obtains the composite green compact that is formed by fixed successively tack coat, molybdenum powder layer and tungsten powder layer.With diameter is 60mm, and thickness is that three high graphite and this composite green compact of 33mm put into graphite jig successively, and the tack coat of composite green compact is contacted with three high graphite, and it is that 75MPa, vacuum degree are 4.7 * 10 that this graphite jig is placed pressure
-3Pa, temperature are in 2200 ℃ the vacuum heating-press sintering stove, to be incubated 1.5 hours and to carry out sinter molding.Make diameter and be 60mm, highly be the W/Mo/ graphite composite target material blank of 40mm, this composite target material blank is installed in high speed rotating on the dynamic equilibrium machine, adjust balance, and grinding promptly makes heavy duty x-ray tube W/Mo/ graphite composite anode target to satisfying the drawing dimensional requirement.
Embodiment 3
Producing diameter is 100mm, highly is the W/Mo/ graphite composite anode target of 60mm, and wherein, tungsten layer thickness is 2mm, and molybdenum layer thickness is 6mm, and graphite linings thickness is 52mm (containing adhesive layer thickness 0.1mm).
According to formula m=ρ π r
2H calculates the quality of tungsten powder and molybdenum powder respectively.Get purity and be 99.8%, particle diameter is tungsten powder 303.17 grams of 1 μ m~6 μ m, press mass volume ratio 5ml/kg with tungsten powder, calculate and get the glycerol 1.51ml of purity assay, above-mentioned raw materials is put into batch mixer, mixed 9 hours, after evenly mixing, sieve, obtain the tungsten powder material with 55 purpose sieves.Get purity and be 99.8%, particle diameter is molybdenum powder 481.61 grams of 1 μ m~6 μ m, press mass volume ratio 5ml/kg with molybdenum powder, calculate and get the glycerol 2.4ml of purity assay, molybdenum powder and glycerol are put into batch mixer, mixed 9 hours, after evenly mixing, sieve, obtain the molybdenum powder material with 55 purpose sieves.Press m
1=ρ π r
2H calculates the quality of required binding agent, in the formula, and h=0.1mm, ρ=6.148 gram per centimeters
3R=100mm, press the mass ratio Ti of each component of binding agent: Ni: Zr=1: 1: 1 again, calculate the quality of Ti, Ni, Zr, titanium valve 16.10 grams, nickel powder 16.10 grams and zirconium powder 16.10 grams that get purity respectively and be 99.7%, particle diameter are not more than 10 μ m according to the volume mass ratio of 50ml/kg, calculate and get the absolute ethyl alcohol 2.415ml of purity assay then, titanium valve, nickel powder, zirconium powder and absolute ethyl alcohol are put into batch mixer mixed 3.5 hours, make bonding agent.The binding agent, molybdenum powder material and the tungsten powder material that obtain are packed in the steel pressing mold tool successively, under the pressing pressure of 700MPa, pressurize 3.5min moulding, the pressing pressure with 270MPa is deviate from from mould then, obtains the composite green compact that is formed by fixed successively tack coat, molybdenum powder layer and tungsten powder layer.With diameter is 100mm, and thickness is that three high graphite and the composite green compact of 52mm put into graphite jig, and the tack coat of composite green compact is contacted with three high graphite, and it is that 90MPa, vacuum degree are 5.8 * 10 that this graphite jig is placed pressure
-3Pa, temperature are in 2205 ℃ the vacuum heating-press sintering stove, be incubated 1.8 hours sinter moldings, making diameter is 100mm, it highly is the W/Mo/ graphite composite target material blank of 60mm, this composite target material blank is installed in high speed rotating on the dynamic equilibrium machine, adjust balance, and grinding promptly makes heavy duty x-ray tube WMo graphite composite anode target to satisfying the drawing dimensional requirement.
Embodiment 4
Producing diameter is 120mm, highly is the W/Mo/ graphite composite anode target of 57mm, and wherein, tungsten layer thickness is 2.5mm, and molybdenum layer thickness is 6.5mm, and graphite linings thickness is 48mm (containing adhesive layer thickness 0.1mm).
According to formula m=ρ π r
2H calculates the quality of tungsten powder and molybdenum powder respectively.Get purity and be 99.9%, particle diameter is tungsten powder 545.70 grams of 1 μ m~6 μ m, press mass volume ratio 5ml/kg with tungsten powder, calculate and get the glycerol 2.73ml of purity assay, above-mentioned raw materials is put into batch mixer, mixed 10 hours, after evenly mixing, sieve, obtain the tungsten powder material with 60 purpose sieves.Get purity and be 99.9%, particle diameter is molybdenum powder 751.31 grams of 1 μ m~6 μ m, press mass volume ratio 5ml/kg with molybdenum powder, calculate and get the glycerol 3.76ml of purity assay, molybdenum powder and glycerol are put into batch mixer, mixed 10 hours, after evenly mixing, sieve, obtain the molybdenum powder material with 60 purpose sieves.Press m
1=ρ π r
2H calculates the quality of required binding agent, in the formula, and h=0.1mm, ρ=6.148 gram per centimeters
3R=120mm, press the mass ratio Ti of each component of binding agent: Ni: Zr=1: 1: 1 again, calculate the quality of Ti, Ni, Zr, titanium valve 23.18 grams, nickel powder 23.18 grams, zirconium powder 23.18 grams that get purity respectively and be 99.8%, particle diameter are not more than 10 μ m according to the volume mass ratio of 50ml/kg, calculate and get the absolute ethyl alcohol 3.48ml of purity assay then, titanium valve, nickel powder, zirconium powder and absolute ethyl alcohol are put into batch mixer mixed 4 hours, make bonding agent.The binding agent, molybdenum powder material and the tungsten powder material that obtain are packed in the steel pressing mold tool successively, under the pressing pressure of 800MPa, pressurize 4min moulding, the pressing pressure with 300MPa is deviate from from mould then, obtains the composite green compact that is formed by fixed successively tack coat, molybdenum powder layer and tungsten powder layer.With diameter is 120mm, and thickness is that three high graphite and this composite green compact of 48mm put into graphite jig, and the tack coat of composite green compact is contacted with three high graphite, is that 100MPa, vacuum degree are 6.6 * 10 at pressure
-3Pa, temperature are in 2210 ℃ the vacuum heating-press sintering stove, to be incubated 2 hours sinter moldings.Make diameter and be 120mm, highly be the W/Mo/ graphite composite target material blank of 57mm, this composite target material blank is installed in high speed rotating on the dynamic equilibrium machine, adjust balance, and grinding promptly makes heavy duty x-ray tube WMo graphite composite anode target to satisfying the drawing dimensional requirement.
The heavy duty x-ray tube that adopts the inventive method to make WMo graphite composite anode target, through actual detected, the anode target material that rate of heat dissipation is made than prior art improves 10%~20%.
Adopt the stacked pressure technology in shop to obtain the W/Mo composite bed of thin W bed thickness Mo layer density distribution uniformity; By adding transition zone, soldering and Pervasion Weld Technology combined obtain being connected of metal molybdenum and high-performance graphite, can satisfy 1300 ℃ and not ftracture the requirement of stable performance when descending military service.It is fixed that the concrete size of WMo graphite target is come according to the concrete requirement of user.