CN1121507C - High sputtering-resistant target material containing mixed rare-earth elements - Google Patents
High sputtering-resistant target material containing mixed rare-earth elements Download PDFInfo
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- CN1121507C CN1121507C CN 99113965 CN99113965A CN1121507C CN 1121507 C CN1121507 C CN 1121507C CN 99113965 CN99113965 CN 99113965 CN 99113965 A CN99113965 A CN 99113965A CN 1121507 C CN1121507 C CN 1121507C
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Abstract
The present invention relates to a high-resistance sputtering target material containing mixed rare-earth elements. The rare-earth elements of a lanthanide series and an actinium series are added to an alloy system, which enables a target material to become a Si-Cr-Ni-Re (Re is a rare-earth element) four-component alloy system. The high-resistance sputtering target material comprises the ingredients of Si (35% to 72%), Cr (25% to 50%) and Ni(2% to 20%). The proportion of the sum of the three elements is 100%. Rare earth content accounts for 0.1% to 3.0% of the total weight of the three elements. The accurate cast of a special vacuum induction melting dewaxing investment is used. The high-resistance sputtering target material containing mixed rare-earth elements has the advantages of high accuracy, stability and reliability, and good commonality, can be simultaneously suitable for preparing a metal film and a metal oxide film resistor, so the applicability of the high-resistance sputtering target material is widened, and the production cost is reduced.
Description
Technical field:
The present invention relates to a kind of high sputtering-resistant target material and production technique thereof that contains rare earth element, target is mainly used in preparation metallic membrane or metal oxide film high resistance resistor, and integrated circuit wiring and transmitter etc. belong to electronics, microelectronics and technical field of semiconductors.
Background technology:
The sputter target material that preparation metallic membrane or metal-oxide film resistor are commonly used in electronics industry is Cr-Ni-Si (chromium-nickel-silicon), Cr-Ni (chromium-nickel), Cr-Si (chromium-silicon) Cr-SiOx (X=1,2) (chromium-silicon oxide) is alloy and compound, there is two large problems usually in the resistor that is prepared from this class alloy and the sputter of compound institute, the accuracy and the stability that are resistor are not good enough not high with versatility sputtering target material, the high resistance measurement device from tens of kilohms to tens of megohms for resistance value particularly, it is particularly outstanding that these problems seem.
In electronic industry and semi-conductor industry, because raising and the miniaturization of devices and the microminiaturization of device integrated level, the accuracy of components and parts, stability, reliability and long lifetime just become of paramount importance performance index.For the resistor of high value, this quasi-resistance device is needed as precision resistor usually, and promptly the performance of resistor fluctuates little and stable with the variation (comprising temperature and humidity etc.) of device Service Environment.Under this prerequisite, new requirement and standard have been proposed the material and the technology of making resistance element.To the resistor starting material is sputtering target material, hope can have high reliability, stability and accuracy by the components and parts that this material makes, comprise low resistance temperature coefficient, excellent durability temperature, Steadydamp-heat, higher anti-environmental change performance and versatility, can prepare the resistor of precision.Yet used alloy system and compound-material can not reach above-mentioned requirements.At present the sputter that selected being used to manufactures the high resistance resistor in electronics industry is Cr-Si and Cr-SiO with high resistant target alloy and compound
xThe alloy and the compound of series, the resistor temperature factor prepared big (usually ± 100ppm/ ℃) with this alloy system and compound, the finished product resistor passes through upper category temperature endurance test in 125 ℃, 1000 hours; Added the load endurance test in 70 ℃, 1000 hours ,-55 ℃ of-125 ℃ of climate cycle tests, the success ratio of 56 days Steadydamp-heat performance tests is low, is not suitable for making accurate resistance element.United States Patent (USP) (patent No. 4392992) has reported that the Cr-Si alloy adds people N in sputter
2The time resistor that obtained performance perameter, when Cr is 25-29 at.% (39.5-46.0wt%), Si is 55-69at.% (47.1-57.1wt%) and N
2The square resistance of film is between 400-700 ohm in 8-16at% (3.4-6.8wt%) scope time, and the temperature coefficient of resistance scope is ± 200ppm/ ℃.This electrical property can not satisfy the requirement of high resistivity, low resistance temperature coefficient.The versatility of such target is poor on the other hand, makes metalster and metal-oxide film resistor and must use different types of sputtering target material, makes metalster Cr-Si alloy, makes metal-oxide film resistor Cr-SiO
xCompound can't reach with a kind of sputtering target material and can be suitable for preparing metalster and metal-oxide film resistor simultaneously, has increased the complicacy and the production cost of manufacturing process." Chinese Appropriate technology achievement 94211123 " reported the Ni-Cr series alloy high-resistance metal film resistor sputtering target material of high Si content, and this target can only be used for metalster, does not see the argumentation that can be used for metal-oxide film resistor simultaneously.
Summary of the invention:
The objective of the invention is to the problems referred to above at prior art, a kind of new prescription and production technique thereof of high sputtering-resistant target material are provided, make the novel target that obtains have high-accuracy property, stability, reliability and good versatility, can be applicable to preparation metalster and metal-oxide film resistor simultaneously, the scope of application of expansion target also reduces production costs.
For realizing such goal of the invention, high sputtering-resistant target material of the present invention has adopted new prescription, adding group of the lanthanides and actinium series lucium are hotchpotch in alloy system, the physicals and the chemical property of the uniqueness of utilizing the special outer electronic structure of rare earth element and producing, make high sputtering-resistant target material become a Si-Cr-Ni-Re (Re is a rare earth element) quad alloy system, reach the performance of regulating and improving target with this.
The concrete composition of Si-Cr-Ni-Re quad alloy that the present invention adopts is Si (35%-72%), Cr (25%-50%), Ni (2%-20%), more than is all weight percent (wt%), and Si, Cr and Ni element summation per-cent are 100%.Content of rare earth is the 0.1%-3.0% (weight percent) of Si, Cr and Ni element gross weight, and rare earth element is group of the lanthanides and actinium series lucium.
The entire production process of target can be divided into get the raw materials ready, melting, thermal treatment and machining and cover and add liner plate.
1, gets the raw materials ready in getting the raw materials ready selected Cr, Ni element purity greater than 99.5%; Si element purity is greater than 99.9%; Lucium purity is greater than 98%.
2, melting is for the material of this class of Si, can run into a difficulty during with common vacuum induction melting molten alloy, i.e. this class material infusibilityization of Si, and therefore in the present invention, the accurate casting of special vacuum induction melting dewax fusible pattern is adopted in the melting of target.Because Si is a refractory material, therefore the master alloy of preparation melting earlier before melting promptly is smelted into master alloy with electric arc furnace with Ni, Cr and a spot of Si, and the power of electric arc furnace is voltage 20V during melting, electric current 500-600A, and the time is 2-5 minute.Carry out the vacuum induction melting of entire target material after the master alloy melting.The master alloy that will prepare in vacuum induction melting is placed on the bottom of feeder, and refractory material makes master alloy melt earlier in vacuum induction melting, and then infusibility Si material is added on top.Vacuum tightness during vacuum induction melting is 2 * 10
-2Torr, power 35KW, the time is 1 hour.Enter refining stage behind this end of processing.Power is 20KW during refining, and the time is 30 minutes.For guaranteeing the adding of rare earth element, do not add rare earth element in the melting material phase, just rare earth element is added up to refining stage.Add back application electromagnetic induction liquation is stirred, inject fusible pattern.The fusible pattern cooling is after stripping process obtains the cast member of target.
3, thermal treatment and machining are heat-treated and machining the casting blank.Thermal treatment process is 800 ℃, is incubated 2 hours.Blank after the thermal treatment can carry out machining, and blank is processed into required shape and size.High resistant target commonly used is shaped as rectangle, is of a size of 380 * 127 * 10mm or 300 * 127 * 10mm.
4, cover the target that adds after the liner plate machining in order to improve its intensity, also must cover it and add liner plate and promptly weld a copper coin overleaf, copper plate thickness is between 1-3mm, and shape and size are identical with target.With target and copper coin firm welding, welding temperature is 250-270 ℃ with the method for soldering of indium tin or adhering with epoxy resin, and the time is 4 hours.
Target after above-mentioned operation is finished promptly can be used for actual production to be used.
The quad alloy that contains rare earth element of the application of the invention is a high sputtering-resistant target material, the mean temperature coefficient of resistance of resistor can reach-15.19ppm/ ℃ (55 ± 3 ℃) and-2.47ppm/ ℃ (+125 ± 2 ℃) 56 days average change in resistance Δs of Steadydamp-heat R=0.032%R, the 1000 hours average change in resistance Δ of upper category temperature weather resistance R=0.24%R, 70 ℃, the 1000 hours average change in resistance Δ of weather resistance R=0.10%R, and-55 ℃ of average change in resistance Δ R=0.049%R of-125 ± 2 ℃ of weathers order, these performance index are much better than national standard (GB5873-86).As long as select different sputtering technologies and parameter on the other hand for use, the prepared high sputtering-resistant target material of the present invention can be applicable to preparation metalster and metal-oxide film resistor simultaneously, has expanded the scope of application of target and has reduced production cost.The present invention also can be applicable to prepare unicircuit, transmitter etc.
Embodiment:
Embodiment 1:
Target alloy ingredient: Si=72%, Cr=25%, Ni=3% (weight percent, three kinds of elements are combined into 100%), Re=2.50%.
Target performance: phase composite: Si (principal phase)+CrSi
2+ NiSi
2(trace); Bending strength: 32.23MPa; Average microhardness: H
M1084-1145: target resistivity: 35780.0 μ m.cm; Film resiativity: 186560.0 μ m.cm; Film initial resistance temperature factor :-412.5ppm/ ℃; Temperature coefficient of resistance after the film thermal treatment :-22.6ppm/ ℃.
Embodiment 2:
Target alloy ingredient: Si=60%, Cr=30%, Ni=10% (weight percent, three kinds of elements are combined into 100%), Re=1.55%.
Target performance: phase composite: Si (principal phase)+CrSi
2+ NiSi
2(on a small quantity); Bending strength: 33.21MPa; Average microhardness: H
M1027-1088: target resistivity: 12411.6 μ m.cm; Film resiativity: 116843.7 μ m.cm; Film initial resistance temperature factor :-302.8ppm/ ℃; Temperature coefficient of resistance after the film thermal treatment :-12.2ppm/ ℃.Embodiment 3:
Target alloy ingredient: Si=35%, Cr=45%, Ni=20% (weight percent, three kinds of elements are combined into 100%), Re=0.75%.
Target performance: phase composite: CrSi+CrSi
2+ Ni
2Si; Bending strength: 24.20MPa; Average microhardness: H
M975-1084: target resistivity: 7376.0 μ m.cm; Film resiativity: 86521.5 μ m.cm; Film initial resistance temperature factor :-265.3ppm/ ℃; Temperature coefficient of resistance after the film thermal treatment :-9.2ppm/ ℃.
The target electrical property shows high specific conductivity and low temperature coefficient of resistance among the present invention, the difference of each alloying element content will make each composition of alloy change mutually simultaneously, each forms the difference that phase electrical property difference is reflected at the target electrical property again, can be used for different fields when the alloy of different proportionings is prepared into film.
Claims (4)
1, a kind of high sputtering-resistant target material that contains mixed rare-earth elements, it is characterized in that in alloy system, adding group of the lanthanides and actinium series rare earth element, make high sputtering-resistant target material become a Si-Cr-Ni-Re quad alloy system, wherein Re is a rare earth element, concrete composition is Si 35%-72%, Cr 25%-50%, Ni 2%-20%, Si, Cr and Ni element summation per-cent are 100%, and content of rare earth is the 0.1%-3.0% of Si, Cr and Ni element gross weight.
2, a kind of as the said production technique that contains the high sputtering-resistant target material of mixed rare-earth elements of claim 1, it is characterized in that adopting in the technology the accurate casting of special vacuum induction melting dewax fusible pattern, earlier Ni, Cr and a spot of Si are smelted into master alloy, carry out the vacuum induction melting of whole target then; The power of electric arc furnace is voltage 20V during the melting master alloy, electric current 500-600A, and the time is 2-5 minute; Vacuum tightness during vacuum induction melting is 2 * 10
-2Torr, power 35KW, the time is 1 hour; Rare earth element adds at refining stage, and power is 20KW during refining, and the time is 30 minutes; The cast member of target covers after thermal treatment and machining and adds liner plate.
3, as the said production technique that contains the high sputtering-resistant target material of mixed rare-earth elements of claim 2, it is characterized in that thermal treatment temp is 800 ℃, be incubated 2 hours.
4, as the said production technique that contains the high sputtering-resistant target material of mixed rare-earth elements of claim 2, it is characterized in that covering when adding liner plate, the copper plate thickness that welds at the target back side is between 1-3mm, shape and size are identical with target, with the method for soldering of indium tin or adhering with epoxy resin with target and copper coin firm welding, welding temperature is 250-270 ℃, and the time is 4 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99113965 CN1121507C (en) | 1999-08-06 | 1999-08-06 | High sputtering-resistant target material containing mixed rare-earth elements |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99113965 CN1121507C (en) | 1999-08-06 | 1999-08-06 | High sputtering-resistant target material containing mixed rare-earth elements |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1243171A CN1243171A (en) | 2000-02-02 |
| CN1121507C true CN1121507C (en) | 2003-09-17 |
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ID=5277097
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 99113965 Expired - Fee Related CN1121507C (en) | 1999-08-06 | 1999-08-06 | High sputtering-resistant target material containing mixed rare-earth elements |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5547094B2 (en) * | 2009-01-29 | 2014-07-09 | Ｊｘ日鉱日石金属株式会社 | Manufacturing method of high purity erbium sputtering target |
| US9347130B2 (en) | 2009-03-27 | 2016-05-24 | Jx Nippon Mining & Metals Corporation | Lanthanum target for sputtering |
| CN102378825B (en) | 2009-03-31 | 2013-10-23 | 吉坤日矿日石金属株式会社 | Lanthanum target for sputtering |
| CN106244988B (en) * | 2016-07-31 | 2019-01-29 | 包头稀土研究院 | A kind of high resistant target manufacturing method |
| CN106756836A (en) * | 2017-01-06 | 2017-05-31 | 广州市祺虹电子科技有限公司 | A kind of transparent circuit board group of the lanthanides target and its manufacture method |
| CN111748783A (en) * | 2019-03-29 | 2020-10-09 | 浙江云度新材料科技有限公司 | Multi-element heavy rare earth metal target for magnetic material coating |
| CN110484886B (en) * | 2019-09-12 | 2021-09-17 | 南京达迈科技实业有限公司 | Nickel-rhenium alloy rotary tubular target containing trace rare earth elements and preparation method |
| US20230121940A1 (en) * | 2020-03-26 | 2023-04-20 | Tosoh Corporation | Cr-si sintered body, sputtering target, and method for producing thin film |
| CN114015921A (en) * | 2021-11-04 | 2022-02-08 | 温州市铜仁新材料研究院 | High-resistance magnetron sputtering target material and preparation method thereof |
-
1999
- 1999-08-06 CN CN 99113965 patent/CN1121507C/en not_active Expired - Fee Related
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