CN102485378B - Preparation method of ruthenium metal sputtering target material - Google Patents
Preparation method of ruthenium metal sputtering target material Download PDFInfo
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- CN102485378B CN102485378B CN2010105819092A CN201010581909A CN102485378B CN 102485378 B CN102485378 B CN 102485378B CN 2010105819092 A CN2010105819092 A CN 2010105819092A CN 201010581909 A CN201010581909 A CN 201010581909A CN 102485378 B CN102485378 B CN 102485378B
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Abstract
The invention relates to a preparation method of a ruthenium metal sputtering target material. The preparation method prepares the ruthenium metal sputtering target material through a direct hot pressing method, the hot pressing temperature is 1400DEG C to 1700DEG C, the pressure is 35MPa, and the heat and pressure preservation time is 10min to 60min. The density of the ruthenium metal target material which is prepared through the method can reach above 98 percent, the average grain size is below 20mu m, and the oxygen content can reach below 200ppm.
Description
Technical field
The present invention relates to a kind of preparation method of ruthenium metal sputtering target, relate in particular to the preparation method of infusibility noble metal target material, belong to hard disk perpendicular magnetic recording materials field.
Background technology
At present, ruthenium metal sputtering target becomes one of raw material important in the perpendicular magnetic recording multi-layer film structure, be applied in magnetic recording media usually used as intermediate layer, mainly play effects such as reducing lattice mismatch stress between levels, increase heat endurance and reduction noise.
The ruthenium metal targets adopts the method for traditional hot pressing (HP) and high temperature insostatic pressing (HIP) (HIP) to prepare usually., for traditional hot-press method,, owing to adopting heat radiation to heat powder, there are the shortcomings such as manufacturing cycle length, the bad control of uniform crystal particles.For the high temperature insostatic pressing (HIP) method, need to carry out cold moudling and, with the target base jacket of packing into, utilize gas to carry out the target base hot-forming powder, complex process, manufacturing cycle are long, and due to apparatus expensive, operating cost is high.These two kinds of technology of while all can't be carried out dead size and be prepared target, are not suitable for the making of noble metal target material.
Therefore, need to provide a kind of grain refinement, ruthenium sputtering target material preparation method uniformly of making when guaranteeing density.
Summary of the invention
The object of the present invention is to provide a kind of grain refinement, ruthenium sputtering target material preparation method uniformly of making when guaranteeing density.
Above-mentioned purpose of the present invention reaches by the following technical programs:
A kind of preparation method of ruthenium metal sputtering target is characterized in that: prepare ruthenium metal sputtering target by direct hot-press method, and 1400 ℃～1700 ℃ of hot pressing temperatures, pressure is 35MPa, heat-insulation pressure keeping time 10～60min.
A kind of optimal technical scheme is characterized in that: the temperature-rise period of described hot pressing temperature is divided into two stages: room temperature to 1200 ℃, the rate of heat addition are 50 ℃ of min
-11200 ℃ are arrived hot pressing temperature, and the rate of heat addition is 25 ℃ of min
-1
A kind of optimal technical scheme is characterized in that: in described temperature-rise period, and insulation 10min when temperature reaches 1000 ℃.
According to the ruthenium metal sputtering target of the preparation method of above-mentioned ruthenium metal sputtering target preparation, its density reaches more than 98%.
According to the ruthenium metal sputtering target of the preparation method of above-mentioned ruthenium metal sputtering target preparation, its average grain size is below 20 μ m.
According to the ruthenium metal sputtering target of the preparation method of above-mentioned ruthenium metal sputtering target preparation, its oxygen content reaches below 200ppm.
The preparation method of ruthenium metal sputtering target provided by the invention, wherein said ruthenium target, density need to reach more than 95% usually, makes grain refinement, even when guaranteeing density.For the ruthenium metal targets, oxygen content is extremely important, can cause film particles to increase when too high oxygen level, reduce thin film stability, so oxygen content will be controlled at below 200ppm.
The ruthenium alloy target crystalline grains size of DHP method preparation is tiny, good uniformity, and density is high, and whole manufacturing cycle approximately 2 hours, greatly shortens preparation time, has improved production efficiency.In addition, but this technique preparation near net-shape prepares the ruthenium target, and production cost is low.
The invention has the advantages that: the present invention adopts direct hot-pressing technique (Direct Hot Pressing, DHP) carry out the preparation of ruthenium sputtering target material, thereby DHP utilizes the AC electric-heating material to realize a kind of vacuum heating-press sintering method of rapid shaping, be the important way of mass production hot press formed product, Fig. 1 has provided the principle schematic of DHP technology.This technology and discharge plasma sintering (SPS) technology has similar heating mode, and different is that the SPS technology adopts the direct current pulse power source heating, and DHP adopts AC electric-heating.Compare with existing ruthenium metal targets technology of preparing, DHP technology manufacturing cost and operating cost are lower, and production efficiency is high, and equipment price is low, also have advantages of simultaneously " near net-shape " production, are applicable to noble metal target material and make.Utilizing during DHP prepares ruthenium metal targets process, the method can obviously reduce the oxygen content in raw material, and simultaneously because manufacturing cycle is short, it is tiny, even that this preparation method obtains the crystallite dimension of target.
The present invention will be further described below by the drawings and specific embodiments, but and do not mean that limiting the scope of the invention.
Description of drawings
Fig. 1 is the direct hot-press method of the present invention (DHP) principle and method schematic diagram.
Fig. 2 is the temperature-density-oxygen content curve of the direct hot pressing of ruthenium target (DHP) sintering.
Fig. 3 is the optical microscope photograph that embodiment 6 prepares target.
The specific embodiment
3N5 high-purity ruthenium powder metal powder is mixed powder, the size particles of pure ruthenium metal dust is uniformly distributed, make microstructure and the composition of the finished product target that obtains even.
Carry out the direct heat compression technology after packing into powder in mould, the schematic diagram of described mould is seen Fig. 1.Fig. 1 is principle and the method schematic diagram of direct heat platen press, and wherein 1 is copper coin, and 2 is copper electrode, and 3 is graphite electrode, and 4 is the graphite pressure head, and 5 is graphite jig, and 6 is powder.
For the uniformity that improves grain size and avoid target inside lamination to occur, temperature-rise period was divided into for two stages: the first stage is room temperature～1200 ℃, and the rate of heat addition is 50 ℃ of min
-1, be incubated 10min after 1000 ℃, because the adsorb oxygen to ruthenium powder surface after 1000 ℃ starts to separate, the purpose of insulation is to remove the adsorb oxygen of powder surface; Second stage is 1200 ℃～hot pressing temperature, along with temperature rises, starts pressurization, and the rate of heat addition is 25 ℃ of min
-1, it is in order to reduce powder endosexine and heart section thermograde that second stage reduces the rate of heat addition, improves the uniformity of powder internal temperature.
After temperature was elevated to target temperature, pressure namely reached goal pressure, then started heat-insulation pressure keeping, because mould adopts the high purity graphite material, not chipping in order to guarantee pressure mould, pressure is decided to be 35MPa, if adopt the high-strength graphite mould, pressure can be improved.The temperature in heat-insulation pressure keeping stage is 1400 ℃～1700 ℃, and temperature can cause density lower than 95% lower than 1400 ℃, can't meet the requirement of high density sputtering target material, and oxygen content is higher; When temperature can be because excess Temperature causes crystallite dimension too thick during higher than 1700 ℃.The heat-insulation pressure keeping time is 10～60min, and the time can cause target density on the low side lower than 10min, and owing in the insufficient target of gas discharge, a large amount of pores being arranged.Temperature may cause local grain to be grown up after higher than 60min, and, because the time is long, causes manufacturing cost to raise.
Temperature-fall period should be controlled cooling rate, and temperature fall time can not be less than 30min, and too fast cooling rate can cause in target having residual stress, even may cause the cracked of target.
After hot pressing finishes to the target base carry out machining, attrition process obtains the target product to finished size.
Resulting target density can reach more than 98%, and below average grain size 20 μ m, oxygen content can reach below 200ppm.
Embodiment 1～7:
1. 3N5 high-purity ruthenium powder is mixed powder, carry out the direct heat compression technology after packing into powder in the high purity graphite mould.
2. temperature-rise period was divided into for two stages: the first stage is room temperature～1200 ℃, and the rate of heat addition is 50 ℃ of min
-1, be incubated 10min after 1000 ℃; Second stage is 1200 ℃～hot pressing temperature, along with temperature rises, starts pressurization, and the rate of heat addition is 25 ℃ of min
-1
3. after temperature was elevated to target temperature, pressure namely reached 35MPa, then started heat-insulation pressure keeping, and this phase temperature is 1500～1650 ℃, and the heat-insulation pressure keeping time is 10～60min.
4. temperature-fall period should be controlled cooling rate, and temperature fall time can not be less than 30min.
5. after hot pressing finishes to the target base carry out machining, attrition process obtains the target product to finished size.
What obtain the results are shown in Table 1, can find out that the target density that obtains in 1500～1650 ℃ of hot pressing scopes all can reach more than 98%, and below average grain size 20 μ m, oxygen content can reach below 200ppm.The heat-insulation pressure keeping time is under the condition of 60min, and the relation curve of hot pressing temperature and density and oxygen content as shown in Figure 2.Can find out, during lower than 1600 ℃ along with the rising density of temperature raises, during higher than 1600 ℃ along with the rising of temperature because powder cohesion speed is accelerated, pore is not easy to discharge, and causes density to descend a little; Can find out from the relation of temperature and oxygen content, oxygen content raises along with hot pressing temperature and descends.
Comparative example 1～2:
In order to obtain the preparation temperature scope of ruthenium metal targets, carry out respectively the experiment of low temperature and high temperature, compare with embodiment.
1. identical with embodiment 1～7,3N5 high-purity ruthenium powder is mixed powder, carry out the direct heat compression technology after packing into powder in mould.
2. temperature-rise period was divided into for two stages: the first stage is room temperature～1200 ℃, and the rate of heat addition is 50 ℃ of min
-1, be incubated 10min after 1000 ℃; Second stage is 1200 ℃～hot pressing temperature, along with temperature rises, starts pressurization, and the rate of heat addition is 25 ℃ of min
-1
3. after temperature was elevated to target temperature, pressure namely reached goal pressure, then started heat-insulation pressure keeping, and hot pressing temperature is respectively 1400 ℃ and 1700 ℃.
4. should to control cooling rate identical with embodiment 1～7 for temperature-fall period.
5. after hot pressing finishes to the target base carry out machining, attrition process obtains the target product to finished size.
What obtain the results are shown in Table 1, can find out, temperature in the time of 1400 ℃ resulting target density lower than more than 95%, average grain size 4.3 μ m, oxygen content can reach 230ppm.Temperature is in the time of 1700 ℃, more than average grain size reaches 40 μ m, due to the excess Temperature coarse grains.The relation curve of hot pressing temperature and density as shown in Figure 2.Therefore, the preparation temperature of high density ruthenium metal targets can not be lower than 1400 ℃, and can not be higher than 1700 ℃.Fig. 3 is the optical microscope photograph that embodiment 6 prepares target, as can be seen from the figure crystal grain be evenly distributed, without layering, target inside only has the tiny pore of minute quantity.
Table 1.DHP sintering prepares Ru target experimental result
Claims (5)
1. ruthenium metal sputtering target material, preparation method, it is characterized in that: the method by direct hot pressing prepares ruthenium metal sputtering target, and hot pressing temperature is 1400 ℃～1700 ℃, and pressure is 35MPa, and the heat-insulation pressure keeping time is 10～60min; The temperature-rise period of described hot pressing temperature is divided into two stages: room temperature to 1200 ℃, the rate of heat addition are 50 ℃ of min
-11200 ℃ are arrived hot pressing temperature, and the rate of heat addition is 25 ℃ of min
-1
2. the preparation method of ruthenium metal sputtering target as claimed in claim 1, is characterized in that: in described temperature-rise period, be incubated 10min when temperature reaches 1000 ℃.
3. the preparation method of ruthenium metal sputtering target as claimed in claim 1 or 2, it is characterized in that: the density of the ruthenium metal sputtering target of preparation reaches more than 98%.
4. the preparation method of ruthenium metal sputtering target as claimed in claim 3, it is characterized in that: the average grain size of the ruthenium metal sputtering target of preparation is below 20 μ m.
5. the preparation method of ruthenium metal sputtering target as claimed in claim 4, it is characterized in that: the oxygen content of the ruthenium metal sputtering target of preparation reaches below 200ppm.
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| CN102922231A (en) * | 2012-10-25 | 2013-02-13 | 昆明贵金属研究所 | Method for machining ruthenium and ruthenium alloy target |
| CN104032270B (en) * | 2014-06-12 | 2016-05-04 | 贵研铂业股份有限公司 | A kind of large scale ruthenium-base alloy sputtering target material and preparation method thereof |
| CN107805789B (en) * | 2017-11-30 | 2019-09-03 | 清远先导材料有限公司 | Preparation method of ruthenium sputtering target material |
| CN108642464B (en) * | 2018-06-25 | 2020-08-28 | 河南科技大学 | Preparation method of high-purity ruthenium sputtering target material |
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| JPH09249967A (en) * | 1996-03-14 | 1997-09-22 | Mitsubishi Materials Corp | High purity barium-strontium titanate sputtering target material and its production |
| KR20010034218A (en) * | 1998-11-20 | 2001-04-25 | 노미야마 아키히콰 | Co-Ti ALLOY SPUTTERING TARGET AND MANUFACTURING METHOD THEREOF |
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