CN110303141A - A kind of effective single crystal Cu fixed anode target of X-ray and preparation method thereof - Google Patents

A kind of effective single crystal Cu fixed anode target of X-ray and preparation method thereof Download PDF

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Publication number
CN110303141A
CN110303141A CN201910620310.6A CN201910620310A CN110303141A CN 110303141 A CN110303141 A CN 110303141A CN 201910620310 A CN201910620310 A CN 201910620310A CN 110303141 A CN110303141 A CN 110303141A
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CN
China
Prior art keywords
mold
tungsten
fixed anode
ray
anode target
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Pending
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CN201910620310.6A
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Chinese (zh)
Inventor
张明鸣
邹远振
周文强
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Zhuzhou Weirhenium New Material Technology Co Ltd
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Zhuzhou Weirhenium New Material Technology Co Ltd
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Priority to CN201910620310.6A priority Critical patent/CN110303141A/en
Publication of CN110303141A publication Critical patent/CN110303141A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D19/00Casting in, on, or around objects which form part of the product
    • B22D19/16Casting in, on, or around objects which form part of the product for making compound objects cast of two or more different metals, e.g. for making rolls for rolling mills
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04Alloys based on tungsten or molybdenum
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J35/00X-ray tubes
    • H01J35/02Details
    • H01J35/04Electrodes ; Mutual position thereof; Constructional adaptations therefor
    • H01J35/08Anodes; Anti cathodes

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
  • X-Ray Techniques (AREA)

Abstract

The invention proposes a kind of effective single crystal Cu fixed anode targets of X-ray, including Copper substrate and tungsten-rhenium alloy piece target surface.Tungsten-rhenium alloy piece and high-purity copper powders, Slow cooling after two-part heating heating is added in a kind of preparation method of the effective single crystal Cu fixed anode target of above-mentioned X-ray in a mold.Design of the present invention to mold and technological temperature makes the fixed anode target matrix copper of preparation have mono-crystalline structures.There is no thermal expansion coefficient caused by crystal boundary and pyroconductivity anisotropy, to solve the problems, such as X-ray fixed anode target caused grain boundary separation under the action of thermal stress at work, and there is higher heat dissipation performance, service life is more long.

Description

A kind of effective single crystal Cu fixed anode target of X-ray and preparation method thereof
Technical field
The present invention relates to metal working technical areas, and in particular to a kind of effective single crystal Cu fixed anode target of X-ray and Preparation method.
Background technique
When X-ray tube works, high pressure is applied to cathode and generates electron beam, high velocity bombardment anode target material, so that anode target material Generate X-ray.Only have 1% energy to be converted to X-ray energy when beam bombardment, remaining energy is then all converted to thermal energy, because This target body temperature can sharply rise to 1000 DEG C or more.In order to obtain stronger X-ray output power, generallys use and pass through increase Electron beam current rated value.Focus point area requirement also results in target surface overheat even local melting while more concentration.
X-ray tube fixed anode target is usually made of oxygen-free copper matrix and tungsten plate target surface, and customary preparation methods are by tungsten It is weldingly fixed on Copper substrate, or non-oxygen copper bar and tungsten plate is placed in graphite jig, founding combination tungsten plate and Copper substrate.
Application No. is a kind of anode head components of anode target of 201020263396.6 disclosure of the invention, and the anode head is by sun Cartridge, tungsten board group by tungsten plate at being weldingly fixed on anode head and be prepared.Application No. is 201310604629.2 to disclose one The casting method and device of the fixed oxygen-free copper anode target of kind closed glass X ray, are placed in quartz for anode tungsten and oxygen-free copper It in bell jar, is heated using medium frequency induction power supply, until the anode tungsten is melted with the oxygen-free copper and combined closely.Above method system Standby fixed anode target is all polycrystalline structure, there is the dendroid crystal boundary being made of oxide or impurity.During the work time, Under the action of thermal stress, crystal grain occurs recrystallization and becomes coarse crystal grain, and thermal conductivity is caused to decline.Coarse crystal grain is further broken It is broken into tiny particle, the defects of migration, recombination result in hole, surface hole defect.It is easier at grain boundaries and tiny crystal grain By the bombardment of electron beam, mechanical performance is weaker.Therefore it easily causes and cracks along grain boundaries, to influence vacuum degree, make the service life Shorten.
Single crystal Cu is face-centered cubic (FCC) structure, therefore the anisotropic problem of heat transfer and thermal expansion coefficient is not present. Therefore the fixed anode target by single crystal Cu as matrix has excellent heat-conductive characteristic.Moreover, because caused by thermal stress Intercrystalline cracking problem is fully solved.Therefore, single crystal Cu fixed anode target is compared to anode target material prepared by traditional approach With higher performance and longer service life.
Summary of the invention
In order to solve the above technical problems, the present invention provide a kind of effective single crystal Cu fixed anode target of X-ray and its Preparation method is prepared it is intended that providing a kind of effective single crystal Cu fixed anode target of X-ray using the present invention The Copper substrate of fixed anode target has single crystal organization structure feature.Uniform, tungsten target material and Copper substrate bond strength with ingredient Advantage that height, thermal diffusivity are good, the service life waits so long.
The present invention provides a kind of effective single crystal Cu fixed anode target of X-ray, including Copper substrate and tungsten-rhenium alloy piece target surface.
As further improvement of the invention, by tungsten-rhenium alloy sheet material and copper powders, cast in a mold.
As further improvement of the invention, which is characterized in that the Copper substrate is mono-crystalline structures, and target surface is rolling state tungsten Rhenium alloys piece, rhenium content are 1-5wt%.
As further improvement of the invention, the mold is the mold that reeded cylindrical graphite is opened in side.
The present invention further protects a kind of preparation method of effective single crystal Cu fixed anode target of above-mentioned X-ray, in mold Middle addition tungsten-rhenium alloy piece and high-purity copper powders, Slow cooling after two-part heating heating.
As further improvement of the invention, specific steps include:
S1. the preparation of mold: the graphite jig that preparation is matched with fixed anode target size, in mold flank hole, hole Angle is consistent with mold inclined-plane;
S2. pre-reduction: rolling piece for tungsten-rhenium alloy and high-purity copper powder be placed in mold, and hydrogen heating is led in heating furnace Reduction, temperature are controlled at 900-1000 DEG C, control hydrogen flowing quantity to play cleaning and go back the impurity of original mould and raw material surface Effect;Meanwhile binder course is formed between this stage, tungsten-rhenium alloy piece and copper powder, it can accelerate to form copper list in cast sections Brilliant rate.
S3. it casts: increasing temperature, be passed through non-oxidizing gas, maintain the temperature at 1100-1200 DEG C, raw material are complete It restores, after 10-15min, air pressure is to 1Pa hereinafter, heat preservation 30min in reduction furnace;
S4. it cools down: according to certain rate slow cooling.
As further improvement of the invention, cooling rate described in step S4 is 5-6 DEG C/min.
The present invention further protects a kind of graphite jig, including graphite base (1), graphite circumferential wall (1a), the graphite Circumferential wall (1a) and graphite base (1) are in conjunction with monoblock type, and side inner hole (2) is parallel with graphite base (1) upper surface.
The invention has the following beneficial effects:
The method for preparing fixed anode target of the invention, which abandons, existing is brazed or is placed in stone for tungsten target face and Copper substrate The method of founding in black mold, and by the graphite jig in design special construction, raw material are using tungsten-rhenium alloy piece and high-purity Copper powder.Copper powder is used to replace traditional copper rod as raw material, the bond strength of target surface and matrix is higher, while can reduce casting Temperature.Tungsten plate is replaced with rolling state tungsten-rhenium alloy piece, the high-temperature behavior of target surface can be improved, to can be improved using power and longevity Life.
Design of the present invention to mold and technological temperature makes the fixed anode target matrix copper of manufacture have mono-crystalline structures. There is no thermal expansion coefficient caused by crystal boundary and pyroconductivity anisotropy, to solve X-ray fixed anode target Caused grain boundary separation problem under the action of thermal stress at work.And there is higher heat dissipation performance, service life is more Long.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of 1 mold of the embodiment of the present invention;
Fig. 2 is that the temperature of the embodiment of the present invention 1 changes over time figure;
Wherein, 1. graphite base;1a. graphite circumferential wall;2. side inner hole;3. tungsten-rhenium alloy sheet material;4. high-purity copper powder.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the invention is clearly and completely described, Obviously, the embodiment described is the embodiment of part of representative of the invention, rather than whole embodiments, this field are general Other all embodiments obtained belong to protection of the invention to logical technical staff without making creative work Range.
The technical scheme is that a kind of effective copper single crystal fixed anode target of X-ray, including monocrystalline Copper substrate and tungsten Rhenium alloys target surface.The effective single crystal Cu fixed anode target raw material of X-ray is tungsten-rhenium alloy sheet material and high-purity copper powders, in mould It is cast in tool.
The preparation method of the effective copper single crystal fixed anode target of the X-ray, specific steps include:
Step 1, the preparation of mold, the graphite jig that preparation is matched with fixed anode target size, in mold flank hole, The angle in hole is consistent with mold inclined-plane.
Tungsten-rhenium alloy is rolled piece and high-purity copper powder is placed in mold by step 2, pre-reduction, and hydrogen is led in heating furnace Heating reduction.Temperature is controlled at 900-1000 DEG C, controls hydrogen flowing quantity to play cleaning and go back original mould and raw material surface Impurity.In this step, nucleus is initially formed above die hole.Tungsten-rhenium alloy piece and copper powders form certain knot simultaneously It closes, accelerates the rate that copper single crystal is grown in step 3.
Step 3: casting increases temperature, maintains the temperature at copper fusing point or more, and 1100-1200 DEG C.It is passed through non-oxidizing gas Body restores raw material completely.After 10-15min, air pressure is to 1Pa hereinafter, heat preservation 30min in reduction furnace.
Step 4: it is cooling, according to the rate slow cooling of 5-6 DEG C/min.In this step, it should be noted that supercooling is avoided to be produced The formation of raw nucleus, and promote the growth of copper single crystal.When mold temperature decline, due to the temperature above graphite side openings It is faster than center portion decline, while die edge part thermal capacitance is smaller, therefore starts to crystallize above mold cavity.With Temperature further decreases, and copper crystallization process is from the edge above aperture to tungsten-rhenium alloy target surface, then diffuses to entire anode, with Form copper single crystal structure.
Embodiment 1
A kind of graphite jig structure of the effective single crystal Cu fixed anode target of X-ray as shown in Figure 1, including graphite base 1, stone Black circumferential wall 1a, with graphite base 1 be monoblock type in conjunction with.Side inner hole 2 is parallel with graphite base upper surface 1, can promote crystalline substance Karyomorphism at.Tungsten-rhenium alloy sheet material 3, high-purity copper powder 4.
Embodiment 2
It is proportionally put into the tungsten-rhenium alloy piece 3 and high-purity copper powder 4 processed in graphite jig in embodiment 1, then is placed in In heating furnace, heated according to the technique of Fig. 2 temperature curve.
In stage A, it is passed through hydrogen, keeping temperature is 800-900 DEG C, in the process, graphite in reduction and cleaning furnace The impurity on 1 surface of boat.Heating and logical hydrogen time need the impurity in long enough to removal furnace on boat and raw material surface.Pass through The step can inhibit to form nucleus in the other parts except the inner hole upper section of graphite jig side, and can accelerate Core forming speed in cooling step.Meanwhile binder course is formed between this stage, tungsten-rhenium alloy piece and copper powder, it can accelerate connecing The rate of B-stage of getting off formation copper single crystal.
In stage B, it is passed through non-oxidizing gas, since raw material use high-purity copper powder, casting temperature is compared to use The casting temperature of copper rod is lower, raises the temperature to 1100-1200 DEG C.After 10-15min, reduce furnace in air pressure to 1Pa hereinafter, Keep the temperature 30min.
In stage C, the solidification and crystallization temperature (1083 DEG C) of slow cooling to copper, speed is 5-6 DEG C/min, in this rank Section, formation and promotion crystallization process in order to avoid nucleus, it should be noted that avoid being subcooled.Due to being communicated in side inner hole and furnace, Thermal capacitance is smaller, therefore upon a drop in temperature, the decline of temperature above the inner hole of side faster to provide nucleus.So in side Start to crystallize above hole, then reaches near tungsten-rhenium alloy target surface, then diffuse to entire anode.The X-ray tube prepared by this method With the single crystal Cu anode substrate diameter 36mm of single crystal Cu fixed anode target, length 50mm, 20 ° of cone angles are (relative to horizontal angle Degree), target surface is tungsten-rhenium alloy, diameter 16mm, thickness 3mm.
Compared with prior art, the method for preparing fixed anode target of the invention abandons existing by tungsten target face and copper The method that matrix is brazed or is placed in founding in graphite jig, and by the graphite jig in design special construction, raw material are adopted With tungsten-rhenium alloy piece and high-purity copper powder.Copper powder is used to replace traditional copper rod as raw material, the bond strength of target surface and matrix is more Height, while casting temperature can be reduced.Leaf is replaced with tungsten-rhenium alloy piece, the high-temperature behavior of target surface can be improved, so as to mention Height uses power and service life.
Design of the present invention to mold and technological temperature makes the fixed anode target matrix copper of manufacture have mono-crystalline structures. There is no thermal expansion coefficient caused by crystal boundary and pyroconductivity anisotropy, to relieve X-ray fixed anode target Caused grain boundary separation problem under the action of thermal stress at work.And there is higher heat dissipation performance, service life is more Long.
Those skilled in the art is not under conditions of departing from the spirit and scope of the present invention that claims determine, also Various modifications can be carried out to the above content.Therefore the scope of the present invention is not limited in above explanation, but by The range of claims determines.

Claims (8)

1. a kind of effective single crystal Cu fixed anode target of X-ray, which is characterized in that including Copper substrate and tungsten-rhenium alloy piece target surface.
2. the effective single crystal Cu fixed anode target of a kind of X-ray according to claim 1, which is characterized in that by tungsten-rhenium alloy Sheet material and copper powders, cast in a mold.
3. the effective single crystal Cu fixed anode target of a kind of X-ray according to claim 1, which is characterized in that described copper-based Body is mono-crystalline structures, and the target surface is rolling state tungsten-rhenium alloy piece, and rhenium content is 1-5wt%.
4. the effective single crystal Cu fixed anode target of a kind of X-ray according to claim 2, which is characterized in that the mold The graphite jig of reeded cylinder is opened for side.
5. a kind of preparation side of the effective single crystal Cu fixed anode target of the X-ray as described in any one of claim 1-4 claim Method, which is characterized in that tungsten-rhenium alloy piece and high-purity copper powders, Slow cooling after two-part heating heating are added in a mold.
6. preparation method according to claim 5, characterized in that specific steps include:
S1. the preparation of mold: the graphite jig that preparation is matched with fixed anode target size, in mold flank hole, hole Angle is consistent with mold inclined-plane;
S2. pre-reduction: rolling piece for tungsten-rhenium alloy and high-purity copper powder be placed in mold, and hydrogen heating is led in heating furnace Reduction, temperature are controlled at 900-1000 DEG C;
S3. it casts: increasing temperature, continue to be passed through hydrogen, maintain the temperature at 1100-1200 DEG C, raw material are restored completely, 10- After 15min, air pressure is to 1Pa hereinafter, heat preservation 30min in reduction furnace;
S4. it cools down: according to certain rate slow cooling.
7. preparation method according to claim 6, which is characterized in that cooling rate described in step S4 is 5-6 DEG C/min.
8. a kind of graphite jig, which is characterized in that including graphite base (1), graphite circumferential wall (1a), the graphite circumferential wall (1a) and graphite base (1) are in conjunction with monoblock type, and side inner hole (2) is parallel with graphite base (1) upper surface.
CN201910620310.6A 2019-07-10 2019-07-10 A kind of effective single crystal Cu fixed anode target of X-ray and preparation method thereof Pending CN110303141A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112563092A (en) * 2020-12-08 2021-03-26 佛山宁宇科技股份有限公司 Manufacturing process of single-crystallization evaporation-resistant X-ray bulb tube anode target
WO2023150983A1 (en) * 2022-02-10 2023-08-17 上海超群检测科技股份有限公司 Method for manufacturing tungsten target material of x-ray tube

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DE3213571C1 (en) * 1982-04-13 1983-10-06 Siemens Ag Solid X-ray tube anode and process for producing it
JPH02165548A (en) * 1988-12-19 1990-06-26 Toshiba Corp Fixed anode type x-ray tube
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CN106711002A (en) * 2015-08-12 2017-05-24 湖北省大冶市探伤机厂 Integrated anode target for X-ray circumferential flat-target ceramic tube
CN108977777A (en) * 2018-08-06 2018-12-11 株洲佳邦难熔金属股份有限公司 A kind of effective W-Re of X-ray-Mo alloy composite anode target and preparation method thereof
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US4400824A (en) * 1980-02-12 1983-08-23 Tokyo Shibaura Denki Kabushiki Kaisha X-Ray tube with single crystalline copper target member
DE3213571C1 (en) * 1982-04-13 1983-10-06 Siemens Ag Solid X-ray tube anode and process for producing it
JPH02165548A (en) * 1988-12-19 1990-06-26 Toshiba Corp Fixed anode type x-ray tube
CN1121638A (en) * 1994-10-28 1996-05-01 株式会社岛津制作所 Anode for an X-ray tube, a method of manufacturing the anode, and a fixed anode X-ray tube
CN201796852U (en) * 2010-07-19 2011-04-13 杭州凯龙医疗器械有限公司 Anode head component of anode target
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112563092A (en) * 2020-12-08 2021-03-26 佛山宁宇科技股份有限公司 Manufacturing process of single-crystallization evaporation-resistant X-ray bulb tube anode target
WO2022120961A1 (en) * 2020-12-08 2022-06-16 朱惠冲 Fabrication process for single-crystallization anti-evaporation x-ray tube anode target
GB2617028A (en) * 2020-12-08 2023-09-27 Zhu Huichong Fabrication process for single-crystallization anti-evaporation X-ray tube anode target
WO2023150983A1 (en) * 2022-02-10 2023-08-17 上海超群检测科技股份有限公司 Method for manufacturing tungsten target material of x-ray tube

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Application publication date: 20191008