CN104878244B - A kind of titanium almag target and preparation method thereof - Google Patents

A kind of titanium almag target and preparation method thereof Download PDF

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CN104878244B
CN104878244B CN201410069676.6A CN201410069676A CN104878244B CN 104878244 B CN104878244 B CN 104878244B CN 201410069676 A CN201410069676 A CN 201410069676A CN 104878244 B CN104878244 B CN 104878244B
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titanium
target
almag
powder
magnesium
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CN104878244A (en
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吕宏
谢元锋
李屹民
夏扬
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GRIMN Engineering Technology Research Institute Co Ltd
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Beijing General Research Institute for Non Ferrous Metals
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Abstract

The present invention relates to a kind of titanium almag target and preparation method thereof.The mass percent of the titanium almag target forms:Titanium 73%~97%, aluminium 0.1%~20%, magnesium 1%~26.9%.Present invention additionally comprises the hot pressed sintering preparation method of titanium almag target.The titanium almag target and its hot pressed sintering preparation method of the present invention, alloying component is uniform, and alloy target material consistency is high, steady quality.

Description

A kind of titanium almag target and preparation method thereof
Technical field
The present invention relates to a kind of target that surface coating is carried out to material and preparation method thereof, more particularly, to a kind of titanium Almag target and preparation method thereof.
Background technology
It is the important method of widening materials application field that incrustation is carried out to material, various metals, alloy, inorganic material Material, high polymer material, by surface coating, can improve case hardness, wearability, corrosion resistance, and can change material Surface color, improve the decoration performance of material.Target is critical material used in plated film, hits target table by high energy beam current Face, the composition of target is transferred to plated material surface, obtain various film layers of different nature.
Titanium magnalium target medically has application value by spatter film forming, because titanium has bio-compatibility, simultaneously The addition of magnalium can allow in human body it is calcareous be easy in titanium magnalium film superficial growth, therefore be coated with synthetic bone material surface Titanium magnalium film, the using effect of synthetic bone material can be improved.
Last layer TiAlMg (N) film layer is plated on the surface of the materials such as metal, plastics, glass, to improve the wearability of material Can, and there is decorative effect very attractive in appearance.At present, generally with the Coating Materials such as pure titanium or titanium-aluminium alloy and magnesium metal come Prepare this film layer.This method has that technique is cumbersome, and plated film colour consistency is poor, does not reach industrial requirement.In order to Meet plated film requirement and used, it is necessary to which titanium magnalium is prepared into alloy and is used as target.
At present, the preparation generally use fusion casting of titanium almag and normal pressure-sintered technique.
(1)Fusion casting
It is main to consider that Mg differs larger with Ti fusing point using this method, and Mg vapour pressure is higher, it usually needs 1000 DEG C~1600 DEG C meltings.Metal Mg volatilizations are serious, and titanium almag uneven components prepared by this method, casting There is the defects of stomata, coarse grains in part, yield rate is relatively low.
(2)Normal pressure-sintered method
Titanium almag uses normal pressure-sintered technique, i.e., first titanium valve, aluminium powder, magnesium powder is cold-pressed to definite shape, Ran Houfang Enter in atmosphere furnace and sinter, this technological process length, loss of the cold pressure procedure to mould is larger, and the equipment that technique needs is more.Due to Mg fusing point is relatively low, and general sintering temperature can be relatively low, and Ti is not easy phase counterdiffusion with Mg, Al, so as to cause product consistency low, production Product porosity is too high so that coating process is unstable, and the problems such as obtained film layer out-of-flatness, therefore this technique is not suitable for preparing The TiAlMg targets of high quality.
Process above, it is difficult to the titanium almag target of high quality is prepared, but the application of titanium almag is very valuable, It is especially important to develop a kind of method for preparing titanium almag target.
The content of the invention
The technical problem to be solved in the present invention is to overcome the shortcomings of normal pressure-sintered technology, there is provided a kind of technological process Short, production cost is low, the titanium almag target hot pressed sintering preparation method of steady quality.
Technical scheme is used by the present invention solves the technical problem:
A kind of titanium almag target, its alloy component range(Mass percent)For:Titanium 73%~97%, aluminium 0.1%~ 20%, magnesium 1%~26.9%;The target is prepared by hot-pressing sintering method.
The preparation method of above-mentioned titanium almag target, using hot pressed sintering preparation method, comprises the following steps:
(1) purity for weighing -200 mesh is more than 99%(w%)Titanium valve or Ti3Al alloyed powders and aluminium powder and magnesium powder, in batch mixing It is well mixed in machine;
(2) by Ti3Al alloyed powders, aluminium powder, the mixed-powder of titanium valve and magnesium powder put mould in the mould of sintering Enter in vacuum hotpressing stove, vacuumize, vacuum is less than 1Pa, then heat up, temperature is from room temperature(25℃)When being warming up to 400 DEG C, Heating rate is maintained at 3~10 DEG C/min, and the pressure of hot pressing furnace pressure head is maintained at 5~10MPa;Then proceed to be warming up to 500~ 640 DEG C, while hot pressing furnace ram pressures are increased to 15~20MPa, heat-insulation pressure keeping 30~120 minutes, then start to cool, unload Pressure, naturally cools to room temperature;
(3) vacuum is removed, is stripped, obtains the titanium aluminum magnesium ternary alloy target blank of sinter molding, then by machining, Obtain satisfactory titanium almag target.
The above-mentioned titanium almag target preparation method the step of(1)In, in powder mixed process, it is filled with mixing machine Hydrogen or argon gas, to reduce oxidation of the material powder in mixing process;Powder incorporation time in batch mixer is 12~48 small When.
Advantages of the present invention:
1)The titanium aluminum magnesium ternary alloy target each group distribution ratio of the present invention, can according to the performance requirement of plated film film layer, Regulated and controled in larger scope.
2)The present invention titanium almag target and its hot pressed sintering preparation method, titanium aluminum magnesium ternary alloy target alloy into Divide uniformly, alloy target material consistency is high, steady quality, and it is low to prepare difficulty.
3)The titanium almag target and its hot pressed sintering preparation method of the present invention, titanium aluminum magnesium ternary alloy target hot pressing Cheng Caiyong two-parts heat up and pressurization, and two-part heating can ensure that target material blank body is heated evenly, and two stage pressurization can ensure Target consistency is evenly distributed.
Brief description of the drawings
Fig. 1 is that composition prepared by embodiment 1 is Ti:73%, Al:0.1%, Mg:Outside 26.9% titanium almag target See.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment.
Embodiment 1
(1) composition is Ti:73%, Al:0.1%, Mg:26.9%, the purity for weighing -200 mesh is more than 99% 1000 grams of powder, Match and be:730 grams of titanium valve, 1 gram of Al powder, 269 grams of magnesium powder, argon gas is filled with batch mixer and is mixed 24 hours;
(2) mixed-powder of well mixed titanium valve, aluminium powder, magnesium powder is mounted in the mould of sintering, mould is put into In vacuum hotpressing stove, vacuumizing, vacuum starts to warm up after being less than 1Pa, when temperature is from room temperature to 400 DEG C, heating rate 5 DEG C/min are maintained at, the pressure of hot pressing furnace pressure head is maintained at 5MPa;Then proceed to be warming up to 580 DEG C.Hot pressing furnace pressure head simultaneously Pressure rise is to 15MPa.Heat-insulation pressure keeping 120 minutes, then start to cool, release, naturally cool to room temperature;
(4) vacuum is removed, the demoulding, the titanium aluminum magnesium ternary alloy target blank of sinter molding is obtained, is then added by machinery Work, obtain satisfactory titanium almag target.Target consistency reaches 97%, and target intensity is high, outward appearance silvery white, such as Fig. 1 It is shown.
Embodiment 2
(1) composition is:Ti:97%, Al:1%, Mg:2%, the purity for weighing -200 mesh is more than 99% 1000 grams of powder, proportioning For:970 grams of titanium valve, 10 grams of Al powder, 20 grams of magnesium powder, argon gas is filled with batch mixer and is mixed 48 hours;
(2) mixed-powder of well mixed titanium valve, aluminium powder, magnesium powder is mounted in the mould of sintering, mould is put into In vacuum hotpressing stove, vacuumizing, vacuum starts to warm up after being less than 1Pa, when temperature is from room temperature to 400 DEG C, heating rate 5 DEG C/min are maintained at, the pressure of hot pressing furnace pressure head is maintained at 5MPa;Then proceed to be warming up to 630 DEG C.Hot pressing furnace pressure head simultaneously Pressure rise is to 20MPa.Heat-insulation pressure keeping 120 minutes, then start to cool, release, naturally cool to room temperature;
(4) vacuum is removed, the demoulding, the titanium aluminum magnesium ternary alloy target blank of sinter molding is obtained, is then added by machinery Work, obtain satisfactory titanium almag target.Target consistency reaches 99.2%, and target intensity is high, outward appearance silvery white.
Embodiment 3
(1) composition is:Ti:79%, Al:20%, Mg:1%, the purity for weighing -200 mesh is more than 99% 1000 grams of powder, matches somebody with somebody Than for:Ti3938 grams of Al alloyed powders, 52 grams of Al powder, 10 grams of magnesium powder, hydrogen is filled with batch mixer and is mixed 12 hours;
(2) by well mixed Ti3Al alloyed powders, aluminium powder, the mixed-powder of magnesium powder are in the mould of sintering, by mould Tool is put into vacuum hotpressing stove, is vacuumized, and vacuum starts to warm up after being less than 1Pa, when temperature is from room temperature to 400 DEG C, is risen Warm speed is maintained at 3 DEG C/min, and the pressure of hot pressing furnace pressure head is maintained at 5MPa;Then proceed to be warming up to 640 DEG C.Hot pressing simultaneously The pressure rise of furnace pressure head is to 15MPa.Heat-insulation pressure keeping 30 minutes, then start to cool, release, naturally cool to room temperature;
(4) vacuum is removed, the demoulding, the titanium aluminum magnesium ternary alloy target blank of sinter molding is obtained, is then added by machinery Work, obtain satisfactory titanium almag target.Target consistency reaches 96%, and target intensity is high, outward appearance silvery white.
Embodiment 4
(1) composition is:Ti:73%, Al:1%, Mg:26%, the purity for weighing -200 mesh is more than 99% 1000 grams of powder, matches somebody with somebody Than for:730 grams of Ti powder, 10 grams of Al powder, 260 grams of magnesium powder, hydrogen is filled with batch mixer and is mixed 20 hours;
(2) mixed-powder of well mixed titanium valve, aluminium powder, magnesium powder is mounted in the mould of sintering, mould is put into In vacuum hotpressing stove, vacuumizing, vacuum starts to warm up after being less than 1Pa, when temperature is from room temperature to 400 DEG C, heating rate 10 DEG C/min are maintained at, the pressure of hot pressing furnace pressure head is maintained at 10MPa;Then proceed to be warming up to 620 DEG C.Hot pressing furnace pressure simultaneously Head pressure rise is to 20MPa.Heat-insulation pressure keeping 60 minutes, then start to cool, release, naturally cool to room temperature;
(4) vacuum is removed, the demoulding, the titanium aluminum magnesium ternary alloy target blank of sinter molding is obtained, is then added by machinery Work, obtain satisfactory titanium almag target.Target consistency reaches 99.1%, and target intensity is high, outward appearance silvery white.
Embodiment 5
(1) composition is:Ti:87%, Al:1%, Mg:12%, the purity for weighing -200 mesh is more than 99% 1000 grams of powder, matches somebody with somebody Than for:870 grams of Ti powder, 10 grams of Al powder, 120 grams of magnesium powder, hydrogen is filled with batch mixer and is mixed 12 hours;
(2) mixed-powder of well mixed titanium valve, aluminium powder, magnesium powder is mounted in the mould of sintering, mould is put into In vacuum hotpressing stove, vacuumizing, vacuum starts to warm up after being less than 1Pa, when temperature is from room temperature to 400 DEG C, heating rate 6 DEG C/min are maintained at, the pressure of hot pressing furnace pressure head is maintained at 5MPa;Then proceed to be warming up to 630 DEG C.Hot pressing furnace pressure head simultaneously Pressure rise is to 15MPa.Heat-insulation pressure keeping 120 minutes, then start to cool, release, naturally cool to room temperature;
(4) vacuum is removed, the demoulding, the titanium aluminum magnesium ternary alloy blank of sinter molding is obtained, then by machining, obtains Satisfactory titanium aluminum magnesium ternary alloy target.Target consistency reaches 98%, and target intensity is high, outward appearance silvery white.
The technological process of the inventive method is short, and production cost is low, and obtained titanium almag target material composition is uniform, alloys target Material consistency is high, and steady quality.

Claims (4)

  1. A kind of 1. titanium almag target, it is characterised in that:Its mass percent forms:Titanium 73%~97%, aluminium 0.1% ~1%, magnesium 2%~26.9%.
  2. 2. a kind of preparation method of titanium almag target, comprises the following steps:
    (1) it is according to the mass percent composition of titanium almag target:Titanium 73%~97%, aluminium 0.1%~20%, magnesium 1% ~26.9%, the purity for weighing -200 mesh is more than 99% titanium valve or Ti3Al alloyed powders and aluminium powder and magnesium powder, in batch mixer It is well mixed;
    (2) by titanium valve or Ti3Mould is put into by Al alloyed powders and aluminium powder and the mixed-powder of magnesium powder in the mould of sintering In vacuum hotpressing stove, vacuumize, vacuum is less than 1Pa, then heat up, when temperature is from room temperature to 400 DEG C, heating rate 3~10 DEG C/min are maintained at, the pressure of hot pressing furnace pressure head is maintained at 5~10MPa;Then proceed to be warming up to 500~640 DEG C, together When hot pressing furnace ram pressures be increased to 15~20MPa, heat-insulation pressure keeping 30~120 minutes, then start to cool, release is naturally cold But room temperature is arrived;
    (3) vacuum is removed, the demoulding, the titanium aluminum magnesium ternary alloy target blank of sinter molding is obtained, then by machining, obtains Titanium almag target.
  3. 3. the preparation method of titanium almag target as claimed in claim 2, it is characterised in that:In powder mixed process, Hydrogen or argon gas are filled with mixing machine.
  4. 4. the preparation method of titanium almag target as claimed in claim 3, it is characterised in that:The incorporation time of powder is 12 ~48 hours.
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Publication number Priority date Publication date Assignee Title
CN106001547A (en) * 2016-07-22 2016-10-12 马建剑 Anti-corrosion titanium-magnesium alloy material and preparing method thereof
CN109371371A (en) * 2018-12-10 2019-02-22 有研工程技术研究院有限公司 A kind of preparation method of selenium arsenic germanium multi-component Alloy Sputtering target
CN112779506A (en) * 2019-11-08 2021-05-11 有研工程技术研究院有限公司 Titanium-aluminum-magnesium-silicon alloy target material and preparation method thereof
CN112144023B (en) * 2020-08-27 2022-11-29 有研工程技术研究院有限公司 Preparation method of high-density osmium target material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1535326A (en) * 2000-10-24 2004-10-06 ����Τ�����ʹ�˾ Methods of forming titanium-based and zirconium-based mixed-metal materials and sputtering targets
CN101348895A (en) * 2008-06-27 2009-01-21 贵州振华云科电子有限公司 Preparation of porous stack metal or alloy sputtering target material
CN102321833A (en) * 2011-09-29 2012-01-18 余鹏 Al-Ti-Si alloy target material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
JP2901049B2 (en) * 1994-11-15 1999-06-02 株式会社神戸製鋼所 Al-Ti alloy target material for arc ion plating

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1535326A (en) * 2000-10-24 2004-10-06 ����Τ�����ʹ�˾ Methods of forming titanium-based and zirconium-based mixed-metal materials and sputtering targets
CN101348895A (en) * 2008-06-27 2009-01-21 贵州振华云科电子有限公司 Preparation of porous stack metal or alloy sputtering target material
CN102321833A (en) * 2011-09-29 2012-01-18 余鹏 Al-Ti-Si alloy target material and preparation method thereof

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