CN1352313A - Method for producing sputtered aluminium alloy target material by using gas jet powder - Google Patents

Method for producing sputtered aluminium alloy target material by using gas jet powder Download PDF

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Publication number
CN1352313A
CN1352313A CN 01134646 CN01134646A CN1352313A CN 1352313 A CN1352313 A CN 1352313A CN 01134646 CN01134646 CN 01134646 CN 01134646 A CN01134646 A CN 01134646A CN 1352313 A CN1352313 A CN 1352313A
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CN
China
Prior art keywords
aluminium
target material
powder
sputtered
aluminium alloy
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CN 01134646
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CN1133753C (en
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赖明雄
邱思议
郑楚丕
温志中
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Industrial Technology Research Institute ITRI
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Industrial Technology Research Institute ITRI
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Abstract

The pneumatic powder blasting process of producing sputtered aluminium alloy target material is suitable for making various aluminum alloy, such as Al-Cr, Al-Si-Cu and Al-Ti, target. The preferable practical steps include melting the metal material for the puttered aluminium alloy target into melt; pneumatic blasting to produce metal powder; and vacuum hot pressing metal powder to form sputtered aluminium alloy target in protective inert gas. Through the said process, high quality sputtered target without material segregation and micro particle may be produced fast and in low cost.

Description

Make the method for sputtered aluminium alloy target material with gas jet powder
Invention field
The present invention relates to make the method for sputtered aluminium alloy target material with gas jet powder, especially refer to a kind of raw material powder of making sputtered target material with the gas blowout method according to the alloying constituent proportioning, again this powdered alloy is sieved, obtain suitable powder diameter, carry out vacuum hotpressing with this powder at last and be shaped to make sputtered aluminium alloy target material.
Background technology
In read-write repeatedly type laser disc (CD-RW, DVD-RAM and DVD-RW etc.) manufacturing processed, must use aluminium alloy (as aluminium-titanium, aluminium-Chrome metal powder) film as the reflecting layer; And in flat-panel screens (as TFT-LCD, PDP, OLED etc.) manufacturing processed, also must use aluminium alloy (as aluminium-tantalum, aluminum-neodymium alloys etc.) to make conductive film, and then make electrode (Electrode).Therefore, sputtered aluminium alloy target material just becomes indispensable material in laser disc and the flat-panel screens industry processing procedure.
At present in each big sputtered target material manufactory of the whole world, all adopt two kinds of different methods for the manufacturing of sputtered aluminium alloy target, a kind of is to adopt casting to make ingot casting, carries out that forging process makes again; Another kind is made in Spray Forming mode, Japan Kobe company is unique company that makes the sputtered aluminium alloy target with Spray Forming method, it is described to see also United States Patent (USP) word the 5514909th and No. 6096438, it is to sweep stack with the melting alloy in the high pressure gas spray to form ingot casting, carries out heat afterwards and all presses (HIP) or forging method to make.With regard to known casting/forging method, when making sputtered aluminium alloy target material, often make sputtered aluminium alloy target material produce segregation phenomena (Segregation) because of adding alloying element, and then make that the membrane quality of sputter gained is relatively poor, and sputter target surface easily produces microparticle (Particle), also can influence the homogeneity of property of thin film; And if when using known SprayForming mode to make sputtered aluminium alloy target material, though can avoid above-mentioned disadvantages associated, but the sputter target cost of manufacture will significantly be improved, when especially some are difficult for adopting the sputter target of hot all pressures in the forging mode in making, its cost more will improve because of using heat all to press.
Clearly, the sputtered aluminium alloy target that uses known technology to make, not to be easy to generate segregation phenomena, and then make the membrane quality variation of sputter gained, or sputter target surface easily produces microparticle (Particle), be exactly that cost of manufacture is too high, the preparation method is too complicated, and the making quality is wayward.
Summary of the invention
An object of the present invention is to avoid producing the phenomenon of material segregation for a kind of method of making sputtered aluminium alloy target material with gas jet powder is provided.
A further object of the present invention can be made the raw material powder of sputtered target material according to the alloying constituent proportioning for a kind of method of making sputtered aluminium alloy target material with gas jet powder is provided.
A further object of the present invention is in order to provide a kind of method of making sputtered aluminium alloy target material with gas jet powder, and its making processes is simple and easy, and with low cost.
The present invention is for reaching above-mentioned purpose, so propose a kind of method of making sputtered aluminium alloy target material with gas jet powder, it comprises that the raw metal that will make sputtered aluminium alloy target material earlier is melt into molten metal; Then, with the gas blowout method this molten metal is made metal-powder; At last, this metal-powder is made sputtered aluminium alloy target material, and feed rare gas element as shielding gas with the vacuum hotpressing shaping.
The gas blowout method as the term suggests promptly be to utilize gas when the spraying media, be dispersed as small droplets with the melt metal liquation or utilize centrifugal force that it is fallen and loose into small droplets, becomes the method for metal-powder again through cooled and solidified.Its gas commonly used has air and rare gas element, and as nitrogen, argon gas etc., and required gas blowout stove can be divided into horizontal and rectilinear two kinds.The empirical formula that concerns of the size of the particle diameter of made powder and spray condition is: D = c V [ γ / ρ m ] 0.22 [ U m / ρ m ] 0.57 Wherein, D: powder diameter
C: nozzle geometric constant
V: the speed of spray gas
U m: the viscosity of metal melting body
ρ m: the density of metal melting body
γ: the surface tension of metal melting body
By in the formula as can be known, the size of made powder particle and the inversely proportional relation of the speed of spray gas, that is the speed of spray gas is faster, made powder diameter is littler; Also can use different controlled variable, control the chemical ingredients of powder diameter size and powder.The present invention adopts the gas blowout legal system to make Al alloy powder, can accurately grasp the particle diameter and the chemical ingredients of aluminium alloy, and uses the powder process of rare gas element fast spraying, can guarantee not have the segregation phenomena generation that alloying element causes.
Hot compacting as the term suggests promptly be to use hot pressing furnace, is exerted pressure to the metal-powder of desiring press molding, and under certain temperature, keeps for some time, the gap between metal-powder is disappeared, thereby obtain required density and shape.It is broadly divided into three steps: in (1) initial stage sintering stage, metal-powder is via diffusion process or viscous deformation, and constriction growth rapidly causes the particle contact area to increase, and makes that the gap between metal-powder becomes cylindric hole; (2) the sintering stage in mid-term, in this stage, these cylindric holes will be shrunk to less cylindric hole again, and any gas all can be extruded and sink in the hole, then, roundlet column hole becomes utmost point destabilization, and is subjected under the energy of surface and crystal boundary, forms sealing and coarse spherical hole; (3) in the last sintering stage, independently spherical hole disappears, and reaches complete densification, obtains required density and shape.
Domestic manufacturing in CD and LCD flat-panel screens has accounted for global space of top prominence in producing, therefore the also certain quantity of tool on the usage quantity of the sputtered target material of relevant film.As only on the industrial market making method of employed import sputter target forge processing procedure and (2) Spray forming adds follow-up HIP processing procedure nothing more than adding based on (1) casting; The innovation part of this patent promptly is to avoid the easy material segregation of casting and produces the shortcoming of microparticle and make high-quality sputtered target material than the quicker and cheap processing procedure of Spray Forming method.
Method of making sputtered aluminium alloy target material with gas jet powder of the present invention all can be used for making various sputtered aluminium alloy target material (aluminium-chromium, aluminium-silicon-copper, aluminium-titanium or the like).
The preferably, the method with gas jet powder making aluminum-titanium alloy sputtered target material of the present invention comprises: metallic aluminium and aluminium-titanium mother alloy are heated between 1100 ℃ to 1300 ℃ simultaneously, make it be melt into aluminium-titanium liquation; With the gas blowout method this aluminium-titanium liquation is made aluminium-ti powder; Use vacuum hotpressing is shaped, and in 500 ℃ to 650 ℃ of temperature, pressure 20MPa to 50MPa, continue 80 to 100 minutes, this aluminium-ti powder is made the aluminum-titanium alloy sputtered target material, and feed argon gas as shielding gas, and hydrogen is as reducing gas.
Further the present invention is done more deep explanation below in conjunction with drawings and Examples.
Description of drawings
Wherein, accompanying drawing 1 is made the schema of sputtered aluminium alloy target material with gas jet powder for the present invention.
Accompanying drawing 2 is the synoptic diagram of the employed gas blowout stove of gas blowout method of the present invention.
Accompanying drawing 3 is the synoptic diagram of the employed hot pressing furnace of hot compacting of the present invention.
Accompanying drawing 4 is made the schema of aluminum-titanium alloy sputtered target material with gas jet powder for the present invention.
Accompanying drawing 5 is made the schema of aluminium-Chrome metal powder sputtered target material with gas jet powder for the present invention.
Accompanying drawing 6 is made the schema of al-si-cu alloy sputtered target material with gas jet powder for the present invention.
Wherein number in the figure is expressed as respectively:
1 is the raw material preparation;
1a is aluminium and aluminium-titanium mother alloy;
1b is aluminium and aluminium-chromium mother alloy;
1c is aluminium and aluminium-silicon mother alloy and Solder for Al-Cu Joint Welding mother alloy;
2 are the powder process of gas blowout method;
2a is for being aluminium-titanium liquation with aluminium and aluminium-titanium mother alloy fusion, with the powder process of gas blowout method;
2b is for being aluminium-molten chromium with aluminium and aluminium-chromium mother alloy fusion, with the powder process of gas blowout method;
2c is for being aluminium-silicon-copper melt with aluminium and aluminium-silicon mother alloy and the fusion of Solder for Al-Cu Joint Welding mother alloy, with the powder process of gas blowout method;
3 for powder is collected, screening;
3a is for collecting screening aluminium-ti powder;
3b is for collecting screening aluminium-chromium powder end;
3c is for collecting screening aluminium-silicon-copper powder;
4 is powder sintering, is shaped;
4a is aluminium-ti powder sintering, is shaped;
4b is aluminium-chromium powder end sintering, is shaped;
4c is aluminium-silicon-copper powder sintering, is shaped;
5 for finishing sputtered aluminium alloy target material;
5a is for finishing the aluminum-titanium alloy sputtered target material;
5b is for finishing aluminium-Chrome metal powder sputtered target material;
5c is for finishing the al-si-cu alloy sputtered target material;
6 is rectilinear gas blowout stove;
60 is process furnace;
600 is crucible;
601 is well heater;
61 is nozzle;
62 are the spraying storehouse;
63 is the powder collection storehouse;
7 is molten aluminium alloy;
70 is the hollow form cone;
71 is Al alloy powder;
8 is rare gas element;
9 is hot pressing furnace;
90 is graphite jig;
91 is outer casing base;
92 is oil gear;
920 is pedestal;
921 is the oil pressure rod;
922 is cushion block;
923 is punching pin;
93 is well heater.
A kind of method of making sputtered aluminium alloy target material with gas jet powder, its preferable implementation step, as shown in Figure 1:
(a) raw material prepares 1: according to the different sputtered aluminium alloy target material of desire to make, for example: different sputtered aluminium alloy target materials such as aluminium-chromium, aluminium-silicon-copper, aluminium-titanium, prepare required different metal raw material, certainly, also sputtered aluminium alloy target material remaining behind the sputter (sputtered target material is used remaining certain thickness and just needed to change) can be reclaimed, confirm after the composition, after the sputtered aluminium alloy target material that reclaims is broken into pieces, again as required different metal raw material.
(b) gas blowout legal system powder 2: the raw metal that step (a) is prepared is inserted in the process furnace of gas blowout stove, this raw metal is melt into after the molten metal, carry out gas blowout manufactured Al alloy powder, to avoid the Al alloy powder oxidation with rare gas element.
(c) powder is collected, sieved 3: after the prepared Al alloy powder of step (b) is collected, sieve the powder that meets required particle diameter to stay, it amounts to material output capacity (Yield) more than 85%.
(d) powder sintering, shaping 4: the Al alloy powder that screening is good in the step (c) is put into hot pressing furnace,, impose the hot compacting of different time, temperature and pressure, and the feeding rare gas element is as shielding gas according to different demands.
(e) finish sputtered aluminium alloy target material 5: the vacuum hotpressing through step (d) is shaped, and has made that the gap between Al alloy powder disappears, and has made required sputtered aluminium alloy target material.
Be example explanation gas blowout process with rectilinear gas blowout stove below.
The synoptic diagram of the employed gas blowout stove of gas blowout method of the present invention as shown in Figure 2.Rectilinear gas blowout stove 6, be to put into the crucible 600 of process furnace 60 with making the required raw metal of sputtered aluminium alloy target material, utilize well heater 601 heating of process furnace 60, make raw metal be melt into molten aluminium alloy 7, and the rare gas element 8 of utilization feeding, molten aluminium alloy 7 is sprayed fast by nozzle 61, because molten aluminium alloy 7 is subjected to the effect of rare gas element 8 rapid expansion in nozzle 61 exits, make molten aluminium alloy 7 in nozzle 61 exits, promptly spray and form hollow form cone 70 in the storehouse 62 and outwards disperse, if molten aluminium alloy 7 has sufficient superheating temperature and is subjected to the effect of shearing stress and accelerating force again, at first form tough band shape, then form spheric Al alloy powder 71 subsequently and concentrate in the powder collection storehouse 63.
The synoptic diagram of the employed hot pressing furnace of hot compacting of the present invention as shown in Figure 3, the Al alloy powder 71 (shown in Figure 2) that has soon sieved is put into the graphite jig 90 of hot pressing furnace 9, and graphite jig 90 is supported by outer casing base 91; Exert pressure by 92 pairs of Al alloy powders 71 of oil gear, 71 heating of 93 pairs of Al alloy powders of well heater so, after continuing for some time, just can make required sputtered aluminium alloy target material.Wherein oil gear 92 includes: pedestal 920, oil pressure rod 921, cushion block 922 and punching pin 923.When oil gear 92 activates, the oil pressure rod 921 generation displacement that is under pressure, the cushion block 922 and the punching pin 923 that drive its front end simultaneously and connected are applied to pressure on the Al alloy powder 71.
The present invention as shown in Figure 4 is with the schema of gas jet powder making aluminum-titanium alloy sputtered target material, and its step is as follows:
(a) aluminium and aluminium-titanium mother alloy 1a: fine aluminium and aluminium-titanium mother alloy are ready to complete according to component proportions (Al-2.3wt%Ti).
(b) be aluminium-titanium liquation with aluminium and aluminium-titanium mother alloy fusion, with gas blowout legal system powder 2a: with the raw material that step (a) is ready to complete, insert and carry out the powder process of gas blowout method in the gas blowout stove, the employed nozzle material of this gas blowout stove is a stupalith, bore is 2.5-4.0mm, and it is material that crucible then adopts zirconium white.Place crucible to be heated to 1100-1300 ℃ metallic aluminium and aluminium-titanium mother alloy, making metallic aluminium and aluminium-titanium mother alloy fusion is the aluminum-titanium alloy liquation, and nozzle cools off so that current are logical, and sprays with common argon gas (Ar).The atomization process of this gas blowout manufactured aluminum-titanium alloy powder lasts about 2-4 minute altogether, and owing to utilize protective atmosphere-argon gas fast spraying powder process, does not take place so prepared aluminum-titanium alloy powder does not have the phenomenon of segregation.
(c) collect, sieve aluminium-ti powder 3a: aluminium-ti powder is collected and sieved, and amounting to material output capacity (Yield) is 90.5%, and powder diameter is distributed in 40-100 μ m.Analysis part aluminium-ti powder composition as can be known, its composition is identical with the raw material composition of preparation, is Al-2.3wt%Ti.
(d) aluminium-ti powder sintering, shaping 4a: in the graphite jig that step (c) aluminium-ti powder finished of sieving is inserted hot pressing furnace; feed the mixed gas of argon gas and hydrogen; wherein argon gas is as the shielding gas of heat pressure forming process; and hydrogen is as reducing gas, and sintering temperature is that 550 ℃~650 ℃, sintering pressure are that 20Mpa~50MPa, sintering time are 80~100 minutes.Behind the present embodiment sintering 90 minutes, the aluminum-titanium alloy sputtered target material is shaped.
(e) finish aluminum-titanium alloy sputtered target material 5a: after the sintering of process step (d), the shaping, the Al-2.3wt%Ti sputter target is taken out by hot pressing furnace, measuring its density value is 2.71g/cm 3(density of aluminium is 2.7g/cm 3The density of titanium is 4.5g/cm 3), the compactness of prepared as can be known Al-2.3wt%Ti sputter target is very good.
The present invention as shown in Figure 5 makes the schema of aluminium-Chrome metal powder sputtered target material with gas jet powder, and the present invention as shown in Figure 6 makes the schema of al-si-cu alloy sputtered target material with gas jet powder, the flow process that is adopted is all similar with the step of front, the sputtered target material difference that the just raw material difference that adopts, and desire is made.Also express the method that the present invention makes sputtered aluminium alloy target material with gas jet powder, all can use for making various sputtered aluminium alloy target material, and can avoid the known casting/sputtered aluminium alloy target material of forging made can produce the phenomenon of material segregation; And not only processing procedure is simple for it, and it is with low cost many that more known again Spray Forming mode is made sputtered aluminium alloy target material, can say thorough all shortcomings of having improved known technology.
Of the present invention graphic with describe as above with the preferred embodiment explanation, association obtains easily, such as: use other gas jet powder to make sputtered aluminium alloy target material, or adopt horizontal gas blowout stove to carry out gas blowout method powder process or the like, be familiar with this field skill person after comprehension spirit of the present invention, all can expect changing enforcement, so the explanation of preferred embodiment of the present invention only is used for helping to understand the present invention, non-in order to limit spirit of the present invention, in not breaking away from spiritual scope of the present invention, replace when doing a little change retouching and equal variation, it does not also break away from the spirit and scope of the present invention.

Claims (10)

1, a kind of method of making sputtered aluminium alloy target material with gas jet powder is characterized in that may further comprise the steps:
A, will provide the raw metal of making sputtered aluminium alloy target material to be melt into a molten metal earlier;
B, this molten metal is made metal-powder with the gas blowout method;
C, this metal-powder is made a sputtered aluminium alloy target material with hot compacting.
2, method of making sputtered aluminium alloy target material with gas jet powder as claimed in claim 1 is characterized in that wherein the described raw metal of step a is selected from aluminium and aluminium-chromium mother alloy, aluminium and aluminium-silicon mother alloy and wherein a kind of combination of Solder for Al-Cu Joint Welding mother alloy, aluminium and aluminium-titanium mother alloy.
3, method of making sputtered aluminium alloy target material with gas jet powder as claimed in claim 1 is characterized in that wherein the described sputtered aluminium alloy target material of step c is selected from aluminium-Chrome metal powder sputtered target material, al-si-cu alloy sputtered target material, wherein a kind of combination of aluminum-titanium alloy sputtered target material.
4, method of making sputtered aluminium alloy target material with gas jet powder as claimed in claim 1 is characterized in that wherein feeding rare gas element as shielding gas in the described heat pressure forming process of step c.
5, method of making sputtered aluminium alloy target material with gas jet powder as claimed in claim 1 is characterized in that described rare gas element is an argon gas.
6, a kind of method of making sputtered aluminium alloy target material with gas jet powder is characterized in that its step comprises:
A, with metallic aluminium and aluminium-titanium mother alloy simultaneously heating and melting become aluminium-titanium mixed molten liquid;
B, this aluminium-titanium mixed molten liquid is made aluminium-ti powder with the gas blowout method;
C, this aluminium-ti powder is made the aluminum-titanium alloy sputtered target material with hot compacting.
7, method of making sputtered aluminium alloy target material with gas jet powder as claimed in claim 6 is characterized in that wherein the described Heating temperature of step a is between 1100 ℃-1300 ℃.
8, method of making sputtered aluminium alloy target material with gas jet powder as claimed in claim 6 is characterized in that wherein the temperature of the described hot compacting of step c is 500 ℃-650 ℃.
9, method of making sputtered aluminium alloy target material with gas jet powder as claimed in claim 6 is characterized in that wherein the described hot compacting required time of step c is 80-100 minute.
10, method of making sputtered aluminium alloy target material with gas jet powder as claimed in claim 6 is characterized in that wherein the pressure of the described hot compacting of step c is 20Mpa-50MPa.
CNB011346469A 2001-11-08 2001-11-08 Method for producing sputtered aluminium alloy target material by using gas jet powder Expired - Lifetime CN1133753C (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100409980C (en) * 2006-09-01 2008-08-13 鞍钢实业微细铝粉有限公司 Production technology of two-nozzle atomization aluminium powder
CN101224496B (en) * 2007-01-18 2010-05-19 光洋应用材料科技股份有限公司 Manufacture method of sputtering targets
CN102363215A (en) * 2011-11-04 2012-02-29 中南大学 Method for preparing chromium aluminum alloy target by powder vacuum hot pressed sintering
CN103981487A (en) * 2014-05-28 2014-08-13 厦门建霖工业有限公司 Chromium-aluminum alloy target as well as preparation method and application thereof
CN109628897A (en) * 2018-12-06 2019-04-16 新疆众和股份有限公司 A kind of high-purity alusil alloy sputtering target material blank and preparation method thereof
CN112517917A (en) * 2020-11-25 2021-03-19 河南东微电子材料有限公司 Preparation method of CrTiLa alloy powder for chromium-titanium target material

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100409980C (en) * 2006-09-01 2008-08-13 鞍钢实业微细铝粉有限公司 Production technology of two-nozzle atomization aluminium powder
CN101224496B (en) * 2007-01-18 2010-05-19 光洋应用材料科技股份有限公司 Manufacture method of sputtering targets
CN102363215A (en) * 2011-11-04 2012-02-29 中南大学 Method for preparing chromium aluminum alloy target by powder vacuum hot pressed sintering
CN103981487A (en) * 2014-05-28 2014-08-13 厦门建霖工业有限公司 Chromium-aluminum alloy target as well as preparation method and application thereof
CN103981487B (en) * 2014-05-28 2016-04-27 厦门建霖工业有限公司 A kind of chromium-aluminum alloy target material its preparation method and application
CN109628897A (en) * 2018-12-06 2019-04-16 新疆众和股份有限公司 A kind of high-purity alusil alloy sputtering target material blank and preparation method thereof
CN112517917A (en) * 2020-11-25 2021-03-19 河南东微电子材料有限公司 Preparation method of CrTiLa alloy powder for chromium-titanium target material

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