CN102366833B - Production method of tungsten-titanium target blank - Google Patents
Production method of tungsten-titanium target blank Download PDFInfo
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- CN102366833B CN102366833B CN201110372337.1A CN201110372337A CN102366833B CN 102366833 B CN102366833 B CN 102366833B CN 201110372337 A CN201110372337 A CN 201110372337A CN 102366833 B CN102366833 B CN 102366833B
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Abstract
The invention relates to a production method of a tungsten-titanium target blank. The production method comprises the following steps of: firstly, providing tungsten-titanium powder; secondly, putting the tungsten-titanium powder into a vacuum sheath and vacuumizing; thirdly, carrying out sinter molding by using a hot isostatic pressing technology; and after the sinter molding is completed, cooling and taking out the tungsten-titanium target blank by removing the vacuum sheath. With the adoption of the production method of the tungsten-titanium target blank, provided by the invention, a die is avoided being used; meanwhile, compared with the tungsten-titanium target blank which is prepared by hot-pressing, the tungsten-titanium target blank which is prepared by adopting the production method has the advantages of better density and uniformity of the internal organization structure.
Description
Technical field
The present invention relates to field of semiconductor manufacture, relate in particular to a kind of preparation method of tungsten-titanium target blank.
Background technology
Vacuum splashing and plating is that the plasma that produces under abnormal glow discharge condition of low density gas is under electric field action; target material surface is bombarded; the molecule of target material surface, atom, ion and electronics etc. are sputtered out; the particle being sputtered is with certain kinetic energy, and directive matrix surface forms coating in a certain direction.
In vacuum splashing and plating process, often can use tungsten-titanium target blank.Early stage tungsten-titanium target blank obtains by fusion casting, yet, because the fusing point of tungsten and the fusing point of titanium differ greatly, be respectively 3400 ℃, 1660 ℃, and both also differ greatly by proportion, be respectively 19.35 grams/cubic centimeter, 4.5 grams/cubic centimeter, therefore, when carrying out founding, difficult control of temperature, and tungsten titanium is after fusing, can form solid solution, easily there is segregation phenomena, cause the tungsten titanium target material uneven components forming.In order to overcome this problem, in industry, occurred adopting the method for powder metallurgy to realize processing tungsten-titanium target blank, this powder metallurgical technique is by producing metal dust (adding or do not add non-metal powder), implement to be shaped and sintering, making the processing method of material or goods.Powder metallurgy is because it has unique machinery, physical property, and these performances can realize porous, half fine and close or fully dense material and goods that traditional casting method cannot be made.
In concrete powder metallurgy process, generally by ready powder is contained in speciality mould, then be placed in vacuum hotpressing stove, first with certain pressure by powder pressing, then be evacuated down to setting value, then intensification limit, limit pressurization, until pressure and temperature all reaches setting value, heat-insulation pressure keeping is cooling with stove after a period of time, comes out of the stove.Said process also claims hot pressing (Hot Pressing, HP).The principle of this hot pressing is: under high temperature, the lattice of powder and crystal boundary can spread and Plastic Flow to a certain degree.
Yet, in realizing hot pressing, the mould that need to match according to the size design of tungsten-titanium target blank, the more expensive and easier loss of this mould, in addition, adopt the uniformity of internal organizational structure of the tungsten-titanium target blank of this method processing more and more higher sputtering technology that cannot meet the demands.
In view of this, be necessary to propose in fact a kind of preparation method of new tungsten-titanium target blank, to overcome the defect of prior art.
Summary of the invention
The problem that the present invention solves is the preparation method that proposes a kind of new tungsten-titanium target blank, to solve existing realization in hot pressing, due to the mould that need to match according to the size design of tungsten-titanium target blank, and the more expensive and easier loss of this mould, and adopt cannot the meet the demands problem of more and more higher sputtering technology of the uniformity of internal organizational structure of the tungsten-titanium target blank of this method processing.
For addressing the above problem, the invention provides a kind of preparation method of tungsten-titanium target blank, comprising:
Tungsten titanium powder is provided;
Tungsten titanium powder is placed into vacuum canning and vacuumizes;
Adopt heat and other static pressuring processes to carry out sinter molding;
Complete after sinter molding, carry out cooling and remove vacuum canning and take out tungsten-titanium target blank.
Alternatively, tungsten titanium powder is placed into after vacuum canning, also shuts described jacket, the step of the deaeration pipe on reserved described jacket, described in vacuumize step and complete by described deaeration pipe.
Alternatively, the vacuum vacuumizing described in step at least reaches 2 * 10
-3pa.
Alternatively, the vacuum vacuumizing described in step at least reaches 2 * 10
-3after Pa, also carry out the step to described vacuum canning heating.
Alternatively, described heating steps proceeds to temperature and reaches after 250 ℃~500 ℃, carries out incubation step, in described heating and insulating process, continues to vacuumize the vacuum making in vacuum canning and is at least 2 * 10
-3pa, carries out described sinter molding step afterwards.
Alternatively, the described insulating process duration is 3-4 hour.
Alternatively, described heat and other static pressuring processes design parameter is: 800 ℃~1400 ℃ of temperature, and environmental stress 150Mpa~200Mpa, and be incubated 3 hours under this temperature pressure~6 hours, cooling 4 hours~6 hours to 600 ℃ afterwards.
Alternatively, described vacuum canning adopts the mild steel welding fabrication that thickness is 1.0mm~2.0mm.
Alternatively, in described sinter molding step, the vacuum of described vacuum canning is at least 2 * 10
-3pa, and in being closed state.
Alternatively, described tungsten titanium powder is placed into after vacuum canning, tungsten titanium powder is carried out to cold pressing treatment, shut afterwards described jacket step.
Alternatively, the purity of described tungsten titanium powder is at least 99.9%.
Alternatively, the purity of described tungsten titanium powder is at least 99.9%, and the density of described tungsten-titanium target blank is at least 99%.
Compared with prior art, the present invention has the following advantages: adopt vacuum canning sealing tungsten titanium powder; Adopt afterwards heat and other static pressuring processes to carry out sinter molding; Complete after sinter molding, carry out cooling and remove vacuum canning and take out tungsten-titanium target blank, said method forms in tungsten-titanium target blank process, avoided use mould, meanwhile, the density of the tungsten-titanium target blank of formation is, the uniformity of internal organizational structure is better than adopting the density of tungsten-titanium target blank of hot pressing formation, the uniformity of internal organizational structure.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of tungsten-titanium target blank provided by the invention.
The specific embodiment
As stated in the Background Art, the uniformity of the internal organizational structure of the tungsten-titanium target blank of the existing heat pressing process processing more and more higher sputtering technology that cannot meet the demands, the inventor analyzes, this is for example, because hot pressing is exert pressure in single shaft direction (vertical direction), this makes the crystal grain of powder when being molded into target, all directions discontinuity.Thereby the inventor proposes to adopt hot isostatic pressing method in sinter molding process.Particularly, the preparation method of tungsten-titanium target blank provided by the invention comprises: first adopt vacuum canning sealing tungsten titanium powder; Adopt afterwards heat and other static pressuring processes to carry out sinter molding; Complete after sinter molding, carry out cooling and remove vacuum canning and take out tungsten-titanium target blank, said method forms in tungsten-titanium target blank process, avoided use mould, meanwhile, the density of the tungsten-titanium target blank of formation is, the uniformity of internal organizational structure is better than adopting the density of tungsten-titanium target blank of hot pressing formation, the uniformity of internal organizational structure.
For above-mentioned purpose of the present invention, feature and advantage can more be become apparent, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.
Figure 1 shows that the flow chart of the preparation method of tungsten-titanium target blank provided by the invention, below in conjunction with Fig. 1, introduce in detail the specific embodiment of the present invention.
First, execution step S11, provides tungsten titanium powder.
In concrete manufacturing process, the purity of the tungsten-titanium target blank forming after considering, preferably provides purity to be at least 99.9% tungsten titanium powder in this step.
Then, execution step S12, is placed into vacuum canning by tungsten titanium powder, vacuumizes.
In the present embodiment, vacuum canning adopts the mild steel welding fabrication that thickness is 1.0mm~2.0mm.It should be noted that, the material of vacuum canning is selected need meet fusing point higher than the temperature in heating process.In addition, it is generally acknowledged, the thickness of vacuum canning need to be enough thick, guarantee vacuumize and heating process in, weld can not split, and the inventor finds to adopt mild steel, the jacket thickness that is 1.0mm~2.0mm in conjunction with thickness, can realize pressure conduction effect good, also there will not be weld easily to split, cause the phenomenon of gas leakage.This vacuum canning can be by Machine Design, and CAD for example makes its shape meet the shape of target, afterwards by seamless tubular goods or sheet material through splicing formation welded together.This vacuum canning generally comprises jacket body and lid, this deaeration pipe is arranged on this lid, particularly, tungsten titanium powder is placed into after vacuum canning, use press to carry out cold pressing treatment to tungsten titanium powder, afterwards this lid is welded on this jacket body and forms complete jacket, this step also claims to shut jacket step.It should be noted that, shut in jacket step, this deaeration pipe is not shut, and deaeration pipe is connected with vaccum-pumping equipment, can also be to vacuumizing in jacket.The technique of welding can realize by argon arc welding.The cold pressing treatment of this step can be avoided powder to be drawn out of in vacuum and waste.
Then start to vacuumize, to a certain extent, for example vacuum reaches 2 * 10
-3during Pa, start jacket to heat.Until be heated to uniform temperature, for example reach after 250 ℃~500 ℃, carry out incubation step, in described heating and insulating process, continue to vacuumize, keep the vacuum in vacuum canning to be at least 2 * 10
-3pa.The object that above-mentioned limit heating edge vacuumizes is that heating makes the impurity in tungsten titanium powder become gaseous state, is evacuated equipment discharge jacket, the tungsten titanium powder of having purified.Tungsten titanium powder is after above-mentioned heating and incubation step, and baseset is formed bulk, but now density is still very poor.Because the fusing point of tungsten, titanium is very high, reach respectively 3400 ℃, more than 1660 ℃, the inventor has analyzed the impurity in tungsten titanium powder, preferably adopts 250 ℃~500 ℃, substantially can remove most impurity, can not cause excessive power consumption again.Secondly, in vacuum, the vacuum that vacuum canning keeps, if too small, can cause caking weak effect, the cost of heat and other static pressuring processes after increasing; If excessive, can cause tungsten titanium powder to be evacuated equipment and extract out, wasted material.The inventor finds, when temperature retention time is 3~4 hours, can realizes and allow the internal temperature of whole material can reach uniformly design temperature, can guarantee to remove the object of lower boiling impurity simultaneously.
Then, execution step S13, adopts heat and other static pressuring processes to carry out sinter molding.
After insulation in step S12 finishes, take out jacket, under the state that continues its inner vacuum of maintenance, hold one's breath (be about to the duct occlusion of holding one's breath, make an airtight vacuum environment of the inner formation of jacket), now the vacuum of described vacuum canning is at least 2 * 10
-3pa.Afterwards, the jacket of holding one's breath is placed in high temperature insostatic pressing (HIP) (Hot Isostatic Pressing, HIP) stove and carries out high temperature insostatic pressing (HIP) step.
High temperature insostatic pressing (HIP) is the process that a kind of static pressure of at high temperature utilizing every equalization is suppressed.The static pressure of this every equalization is generally by inert gas, and for example argon gas as passing, realize by piezodielectric.The inventor finds, tungsten titanium powder is adopted to high temperature insostatic pressing (HIP) method, can avoid ingot casting method to make the grainiess generation gross segregation of material, thereby can improve processing performance and the mechanical performance of the tungsten-titanium target blank after moulding.Hot isostatic pressing method have assemble hot pressing, etc. the plurality of advantages such as static pressure, yet the concrete technology parameter that will obtain adopting this method to process the target that meets standard but and be not easy.
Above-mentioned parameter mainly comprises: temperature, the disproportionate relation of environmental stress and temperature retention time and three, in existing heat and other static pressuring processes, general temperature is greatly between 200 ℃~500 ℃, pressure can complete the caking of common metal powder at 50~150Mpa, yet, for tungsten titanium powder, in conjunction with vacuum condition, the inventor finds, this heat and other static pressuring processes design parameter adopts 800 ℃ to 1400 ℃ of temperature, in high temperature insostatic pressing (HIP) stove, rush argon gas or nitrogen, the environmental stress 150Mpa to 200Mpa that keeps jacket place, and be incubated 3 hours under this temperature pressure~6 hours, control afterwards cooldown rate, while making in cooling 4 hours~6 hours high temperature insostatic pressing (HIP) stoves temperature to 600 ℃, pressure in this process in high temperature insostatic pressing (HIP) stove is at 150Mpa to 200Mpa, the density of gained tungsten-titanium target blank, the uniformity of internal organizational structure all more existing tungsten-titanium target blank will be well and percent defective low, workability can be poor, add and be difficult for falling material man-hour, and manufacturing cost is lower.
Vacuum in existing heat and other static pressuring processes in general jacket need to be greater than 10
-2pa, and the inventor finds that vacuum reaches 2 * 10
-3during Pa, can start sintering process, the simultaneously requirement of vacuum reduces, and also makes the heating-up temperature of sintering reduce, saved energy consumption, and has reached the object that preparation density is at least 99% tungsten-titanium target blank.
Complete after sinter molding, execution step S14, carries out cooling and removes vacuum canning and take out tungsten-titanium target blank.
In this step, after temperature to 600 ℃, turn off high temperature insostatic pressing (HIP) stove in high temperature insostatic pressing (HIP) stove, when this stove is cooled to 200 ℃ below, jacket is taken out, remove afterwards vacuum canning taking-up tungsten-titanium target blank.The dismounting of this step can realize by chemical method or mechanical means.The tungsten-titanium target blank taking out also needs through methods such as turning, line cuttings afterwards, thereby makes the tungsten titanium target material of final needs.Through detecting, adopt the density of the tungsten-titanium target blank of above-mentioned steps making to be at least 99%, and internal organizational structure is even, grain size meets the requirement of sputtering target material.
In sum, the present invention has the following advantages: (1) adopts vacuum canning sealing tungsten titanium powder; Adopt afterwards heat and other static pressuring processes to carry out sinter molding; Complete after sinter molding, carry out cooling and remove vacuum canning and take out tungsten-titanium target blank, said method forms in tungsten-titanium target blank process, avoided use mould, meanwhile, the density of the tungsten-titanium target blank of formation is, the uniformity of internal organizational structure is better than adopting the density of tungsten-titanium target blank of hot pressing formation, the uniformity of internal organizational structure;
(2) it is generally acknowledged, the thickness of vacuum canning need to be enough thick, guarantee vacuumize and heating process in, weld can not split, and the inventor finds to adopt mild steel, the jacket thickness that is 1.0mm~2.0mm in conjunction with thickness, can realize pressure conduction effect good, also there will not be weld easily to split, cause the phenomenon of gas leakage;
(3), before heat and other static pressuring processes starts, the vacuum vacuumizing in step at least reaches 2 * 10
-3after Pa, also carry out the step to described vacuum canning heating, the object that limit heating edge vacuumizes is that heating makes the impurity in tungsten titanium powder become gaseous state, is evacuated equipment discharge jacket, the tungsten titanium powder of having purified;
(4) in addition, the inventor has analyzed the impurity in tungsten titanium powder, preferably adopts 250 ℃~500 ℃, substantially can remove most impurity, can not cause excessive power consumption again.Secondly, in vacuum, the vacuum that vacuum canning remains on, if too small, can cause caking weak effect, the cost of heat and other static pressuring processes after increasing; If excessive, can cause tungsten titanium powder to be evacuated equipment and extract out, wasted material.The inventor finds, when temperature retention time is 3~4 hours, can realizes and allow the internal temperature of whole material can reach uniformly design temperature, can guarantee to remove the object of lower boiling impurity simultaneously;
(5) in existing heat and other static pressuring processes, the vacuum in general jacket need to be greater than 10
-2pa, and the inventor finds that vacuum reaches 2 * 10
-3during Pa, can start sintering process, the simultaneously requirement of vacuum reduces, and also makes the heating-up temperature of sintering reduce, saved energy consumption, and has reached the object that preparation density is at least 99% tungsten-titanium target blank.
Although the present invention with preferred embodiment openly as above; but it is not for limiting the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; can utilize method and the technology contents of above-mentioned announcement to make possible change and modification to technical solution of the present invention; therefore; every content that does not depart from technical solution of the present invention; any simple modification, equivalent variations and the modification above embodiment done according to technical spirit of the present invention, all belong to the protection domain of technical solution of the present invention.
Claims (8)
1. a preparation method for tungsten-titanium target blank, is characterized in that, comprising:
Tungsten titanium powder is provided;
Tungsten titanium powder is placed into vacuum canning, vacuumizes, described in the vacuum that vacuumizes in step at least reach 2 * 10
-3pa, reaches 2 * 10
-3after Pa, also carry out described vacuum canning heating steps, described heating steps proceeds to temperature and reaches after 250 ℃~500 ℃, carries out incubation step, in described heating and insulating process, continues to vacuumize the vacuum making in vacuum canning and is at least 2 * 10
-3pa;
Adopt heat and other static pressuring processes to carry out sinter molding, described heat and other static pressuring processes design parameter is: 800 ℃~1400 ℃ of temperature, environmental stress 150Mpa~200Mpa, and be incubated 3 hours under this temperature pressure~6 hours, cooling 4 hours~6 hours to 600 ℃ afterwards, after temperature to 600 ℃, turn off high temperature insostatic pressing (HIP) stove in high temperature insostatic pressing (HIP) stove;
Complete after sinter molding, carry out cooling and remove vacuum canning and take out tungsten-titanium target blank.
2. the preparation method of tungsten-titanium target blank according to claim 1, it is characterized in that, tungsten titanium powder is placed into after vacuum canning, also shut described jacket, the step of the deaeration pipe on reserved described jacket, described in vacuumize step and complete by described deaeration pipe.
3. the preparation method of tungsten-titanium target blank according to claim 1, is characterized in that, described in vacuumize insulating process in step and continue 3~4 hours.
4. the preparation method of tungsten-titanium target blank according to claim 1, is characterized in that, described vacuum canning adopts the mild steel welding fabrication that thickness is 1.0mm~2.0mm.
5. the preparation method of tungsten-titanium target blank according to claim 1, is characterized in that, in described sinter molding step, the vacuum of described vacuum canning is at least 2 * 10
-3pa, and in being closed state.
6. the preparation method of tungsten-titanium target blank according to claim 2, is characterized in that, described tungsten titanium powder is placed into after vacuum canning, and tungsten titanium powder is carried out to cold pressing treatment, shuts described jacket step described in carrying out afterwards.
7. the preparation method of tungsten-titanium target blank according to claim 1, is characterized in that, the purity of described tungsten titanium powder is at least 99.9%.
8. the preparation method of tungsten-titanium target blank according to claim 7, is characterized in that, the density of the described tungsten-titanium target blank of making is at least 99%.
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CN103447535B (en) * | 2012-05-30 | 2015-09-09 | 宁波江丰电子材料股份有限公司 | The preparation method of target |
CN102699325A (en) * | 2012-06-20 | 2012-10-03 | 江苏美特林科特殊合金有限公司 | Preparing method for Ti-Si alloy target materials |
CN104694895B (en) * | 2013-12-05 | 2017-05-10 | 有研亿金新材料股份有限公司 | W-Ti alloy target material and manufacturing method thereof |
CN105642899B (en) * | 2014-11-20 | 2018-11-27 | 宁波江丰电子材料股份有限公司 | The manufacturing method of molybdenum silicon target |
CN105695832A (en) * | 2014-11-26 | 2016-06-22 | 宁波江丰电子材料股份有限公司 | CrMo alloy molding method |
CN106270556A (en) * | 2015-06-10 | 2017-01-04 | 宁波江丰电子材料股份有限公司 | The method for turning of tungsten titanium target material |
CN107971485B (en) * | 2017-11-28 | 2020-06-05 | 宁波市鄞州隆茂冲压件厂 | Sintering process of tungsten-titanium alloy |
TWI641697B (en) | 2017-12-26 | 2018-11-21 | 國家中山科學研究院 | Preparation method for preparing high-purity and dense tungsten-titanium metal |
CN113579233B (en) * | 2021-07-14 | 2023-08-11 | 先导薄膜材料(安徽)有限公司 | Tungsten-titanium alloy target material and preparation method and application thereof |
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US5993734A (en) * | 1998-03-25 | 1999-11-30 | Sony Corporation | Method for making W/Ti sputtering targets and products in an inert atmosphere |
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