CN1243322A - Metal film high-resistance resistor and mfg. technology thereof - Google Patents
Metal film high-resistance resistor and mfg. technology thereof Download PDFInfo
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- CN1243322A CN1243322A CN 99113963 CN99113963A CN1243322A CN 1243322 A CN1243322 A CN 1243322A CN 99113963 CN99113963 CN 99113963 CN 99113963 A CN99113963 A CN 99113963A CN 1243322 A CN1243322 A CN 1243322A
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Abstract
The production process of metal-film high-resistance resistor is characterized by that it adopts the Si-Cr-Ni-Re four-component alloy system high-resistance sputtering target materials containing lanthanum series and actinium series rare earth elements as raw material, and its concrete components are Si (35%-72%), Cr (25%-50%), Ni (2%-20%) and the rare earth element content is 0.1%-3.0% of total weight of three elements. It adopts the D. C. sputtering plus radio-frequency sputtering process to obtain the unique double-film structure resistive body, its .D. C. sputtering gas is argon, and the radio-frequency sputtering gas is the mixture of argon and oxygen. Said invented resistor is stable in performance, high in precision and low in resistance temp. coefficient.
Description
The present invention relates to a kind of manufacturing process of metal film high-resistance resistor, relate in particular to that a kind of usefulness is novel to contain the manufacturing process that the mixed rare-earth elements high sputtering-resistant target material prepares metal film resistor, belong to electronic technology or technical field of semiconductors.
Owing to raising and the miniaturization of devices and the microminiaturization of device integrated level, the accuracy of components and parts, stability, reliability and long-life just become most important performance index in electronics industry and semi-conductor industry.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.Preparation metal film resistor sputter target material commonly used is Cr-Ni-Si (chromium-nickel-silicon), Cr-Ni (chromium-nickel), Cr-Si (chromium-silicon) and Cr-SiO in electronics industry
x(x=1,2) (chromium-silica) is alloy and compound.The resistor temperature coefficient prepared big (usually ± 100ppm/ ℃) with this alloy system and compound, the finished product resistor was by 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 rate of 56 days Steadydamp-heat performance tests is low, accuracy and stability are not good enough, the high resistance measurement device from tens of kilohms to tens of megohms particularly for resistance value, particularly loom large the requirement of the accurate resistance element of incompatibility.Discussed in the United States Patent (USP) (patent No. 4569742) and prepare target with Cr and Si element and feed the metal film resistor that Ni obtained when the sputter, resistor after heat treatment TCR in-200--400ppm/ ℃ scope.The prepared resistor stability of this technology, accurate unsatisfactory can not satisfy low TCR requirement.
The objective of the invention is to adopt a kind of new target, cooperate and improve sputtering technology, make a kind of metal film resistor, meeting the market requirement with high reliability, high stability, high-accuracy property.
For realizing such goal of the invention, it is raw material that metal film high-resistance resistor of the present invention has adopted a kind of Si-Cr-Ni-Re (Re is a rare earth element) high sputtering-resistant target material that the quaternary alloy system is new, adopt direct current sputtering to add radio frequency sputtering technology, obtain a kind of resistive element of double membrane structure of uniqueness, obtain resistor through heat treatment and other later process again.
The prescription of target is to add group of the lanthanides and the actinium series lucium is an alloy in alloy system, make high sputtering-resistant target material become a Si-Cr-Ni-Re (Re is a rare earth element) quaternary alloy system, reach the purpose of regulating and improving preparation-obtained resistor performance with this.Its concrete composition is Si (35%-72%), Cr (25%-50%), Ni (2%-20%), more than is all percentage by weight (wt%), and Si, Cr and Ni element percent of total are 100%.Content of rare earth is the 0.1%-3.0% (percentage by weight) of Si, Cr and Ni element total weight, and rare earth element is group of the lanthanides and actinium series lucium.
The present invention adopts this novel target to make the metal high resistance resistor, and its production technology is:
1, direct current sputtering: the preceding operating room of sputter forevacuum should be more than 5 * 10-3pa, when forevacuum reaches
Just feed sputter gas after this vacuum degree.Sputter gas is an argon gas in the direct current sputtering, and flow is
50sccm。Sputtering pressure is 1.0-3.0 * 10-1Pa during direct current sputtering, and sputtering power is 200-
450W, the time is 20-100 minute.The direct current sputtering operation finishes the laggard radio frequency sputtering of going into.
2, radio frequency sputtering: working gas is argon gas and oxygen mixture in radio frequency sputtering, Ar and O
2
Ratio is 9: 1 (percent by volume), and sputtering pressure is 1.0-3.0 * 10
-1Pa, power is
500W, the time is 10-20 minute.Obtain the blank of resistor, i.e. resistive element.
3, heat treatment: temperature is 300-500 ℃, and the time is depended on the scope of actual needs and TCR.
4, later process: comprise japanning, pressure cap, solder taul, cutting and be coated with operation such as outer lacquer, obtain
Whole finished product resistor.
By the resistive element structure that direct current sputtering and radio frequency sputtering face obtain, be a kind of double membrane structure of uniqueness, one deck inner layer film is arranged outside the resistive element core body, inner layer film also covers one deck outer membrane outward.
The characteristics of this double membrane structure maximum are can be played by the formed outer membrane of radio frequency sputtering the double action of protection and adjusting electric property.Inner layer film is mainly by Si, and Cr and Ni element are formed, and shows the electric behavioral trait of metal species, has positive temperature coefficient of resistance, is conductive layer, and outer membrane is except Si, and Cr and Ni element also have the O element outward, and oxygen element and Si and Cr react in sputter procedure and generate SiO
xAnd Cr
yO
x, have the electric behavioral trait of semi-conducting material, negative temperature coefficient of resistance feature is arranged, be protective layer and electrical property regulating course.Resistive element after the sputter this outer membrane in heat treatment can be protected inner layer film, stops the diffusion of the O in the heat treatment atmosphere, reduces the oxidation of inner layer film, makes the resistor stable performance.Oxide in the outer membrane has semiconductor electric conductivity and negative temperature coefficient of resistance simultaneously, in use the positive temperature coefficient of resistance of the negative temperature coefficient of resistance of outer membrane and inner layer film acts on mutually, the temperature coefficient of resistance of energy regulating resistor makes the temperature coefficient of resistance of resistor littler.Simultaneously, outer membrane and inner layer film become parallel resistor device on the microcosmic together, and its conductive characteristic can make the performance of whole resistor more stable.
The present invention has utilized the special electronic structure of rare earth element, be added to it in the prescription of target as trace element, make to contain physical property and the chemical property that rare-earth compound shows uniqueness, reduced temperature coefficient of resistance, improved the comprehensive electric conductivity of material.The present invention adopts direct current sputtering to add radio frequency sputtering in production technology, obtains the resistive element of the double membrane structure of this uniqueness, reaches stable performance, effect that precision is high.
The present invention is a high sputtering-resistant target material by the quaternary alloy that use contains rare earth element, the mean temperature coefficient of resistance of resistor can reach-10.19ppm/ ℃ (55 ± 3 ℃) and-2.47ppm/ ℃ (=125 ± 2 ℃), the 56 days average change in resistance Δ of Steadydamp-heat R=0.032%R, 1000 hours upper category temperature durability average change in resistance Δ 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).
Embodiment 1:
Target alloy composition: Si=65%, Cr=30%, Ni=5%, (percentage by weight, three kinds of elements are combined into
100％)。Re=0.75% (Si, Cr and Ni element total weight 0.75%).
Resistor types: metal film resistor.
Resistor model specification: RJ14-0.25W-10M Ω.
Resistor Standard resistance range: 10M Ω.
Sputtering technology:
Direct current sputtering: power=300W, time=40min, sputter gas=Ar
Radio frequency sputtering: power=500W, time=15, min, sputter gas=Ar+O
2. ratio: Ar: O
2=9: 1.
Heat treatment temperature: 475 ℃, 4 hours.
Testing standard: GB5873-86
Finished product resistor The performance test results is listed in table 1.
Table 1 embodiment 1 finished product resistor The performance test results
Embodiment 2: target alloy composition: Si=50%, Cr=42%, Ni=8%, (percentage by weight, three kinds of elements are combined into 100%).Re=0.5% (Si, Cr and Ni element total weight 0.5%).Resistor types: metal film resistor.Resistor model specification: RJ14-0.25W-56K Ω.Resistor Standard resistance range: 56K Ω.Sputtering technology: direct current sputtering: power=400W, time=70min, sputter gas=Ar radio frequency sputtering: power=500w, time=15, min, sputter gas=Ar+O
2, ratio: Ar: O
2=9: 1.Heat treatment temperature: 450 ℃, 90 minutes.Testing standard: GB 5873-86.Finished product resistor The performance test results is listed in table 2.
| Sequence number | Pilot project | Experimental condition | Technical standard | Test result (20 samples) | ||
| Average | Standard deviation | |||||
| 1 | Temperature changes fast | -55 ± 3 ℃, 30min 125+2 ℃, 30min is for once, totally 5 times, interval 2-3min | Δ R≤± (0.5%R+0.05 Ω) | 0.017 | 0.0014 | |
| 2 | Vibration | 10-500Hz, amplitude 0.75 mm, or acceleration 98m/s 2, 6h | Δ R≤± (0.5%R+0.05 Ω) | 0.0019 | 0.00093 | |
| 3 | The weather order | Xeothermic: 125 ± 2 ℃, 16h circulate damp and hot first the circulation: 55 ℃, 24h.Cold :-55 ± 3 ℃, 2h low pressure: 8.5KPa, 1h damp and hot all the other circulations that circulate: 55 ℃, 24h, 5 times.DC load: 250V, 1min | Δ R≤± (2%R+0.1 Ω) | 0.034 | 0.00062 | |
| 4 | 70 ℃ of durability | 70 ± 2 ℃, 1.5h energising 250V-0.5h outage.1000h | Δ R≤± (2 R+0.1 Ω) | 48h | 0.0041 | 0.0011 |
| 500h | 0.030 | 0.0025 | ||||
| 1000h | 0.04 | 0.0025 | ||||
| 5 | Resistance varies with temperature | -55 ± 3 ℃, 10min | α: ± 100 * 10 -6/ ℃ | 20.64 | 9.80 | |
| 125 ± 2 ℃, 10min | α: ± 100 * 10 -6/ ℃ | -45.40 | 15.04 | |||
| 6 | Steadydamp-heat | 40 ± 2 ℃, 93+2 (3) %, 10 making alives not, 10 add 25V, add 250V-1min after 56 days | Δ R≤± (2%R+0.1 Ω) | 0.054 | 0.007 | |
| 7 | The upper category temperature durability | 125 ℃ of 1000h | Δ R≤± (2% R+0.1 Ω) | 48h | 0.027 | 0.0023 |
| 500h | 0.087 | 0.0048 | ||||
| 1000h | 0.11 | 0.0079 | ||||
Table 2 embodiment 2 finished product resistor The performance test results
| Sequence number | Pilot project | Experimental condition | Technical standard | Test result (20 samples) | ||
| Average | Standard deviation | |||||
| ??1 | Temperature changes fast | -55 ± 3 ℃, 125 ± 2 ℃ of 30min, 30min, for once, totally 5 times, 2-3min at interval | ?????ΔR≤±(0.5％R ?????????+0.05Ω) | ???0.01 | ??0.00 | |
| ??2 | Vibration | 10-500Hz, amplitude 0.75mm, or acceleration 98m/s 2，6h | ????ΔR≤±(0.5％R ????????+0.05Ω) | ???0.00 | ??0.00 | |
| ??3 | The weather order | Xeothermic: 125 ± 2 ℃, 16h circulate damp and hot first the circulation: 55 ℃, 24h. it is cold :-55 ± 3 ℃, 2h low pressure: 8.5KPa, 1h damp and hot all the other circulations that circulate: 55 ℃, 24h.5 it is inferior. DC load: 250V, 1min | ??ΔR≤±(2％R+0.1Ω) | ???0.049 | ??0.0049 | |
| ??4 | 70 ℃ of durability | 70 ± 2 ℃, 1.5h energising 250V-0.5h outage .1000h | ΔR≤±(2％ ???R+0.1Ω) | ??48h | ???0.0035 | ??0.0049 |
| ??500h | ???0.060 | ??0.013 | ||||
| ??1000h | ???0.10 | ??0.0085 | ||||
| ????5 | Resistance varies with temperature | -55±3℃，10min | ??α：±100×10 -6/℃ | ????-15.19 | ????9.87 | ||
| 125±2℃，10min | ??α：±100×10 -6/℃ | ????-2.47 | ????3.64 | ||||
| ????6 | Steadydamp-heat | 40 ± 2 ℃, 93+2 (3) %, 10 making alives not, 10 add 25V, add 250V-1min after 56 days | ??ΔR≤±(2％R ??+0.1Ω) | ????0.032 | ????0.0067 | ||
| ????7 | The upper category temperature durability | 125℃?1000h | ΔR≤±(2％ R+0.1Ω) | ??48h | ??0.033 | ????0.0044 | |
| ??500h | ??0.18 | ????0.014 | |||||
| ??1000h | ??0.24 | ????0.020 | |||||
Listed the performance index that this resistor is mainly examined in the 2nd row in the table 1 and 2, temperature changes fast, vibration, weather order, 70 ℃ of durability, resistances vary with temperature, Steadydamp-heat and upper category temperature durability.The 3rd classifies the test condition that each test event must reach in when test institute as, and the 4th classifies the index of test event GB defined as, and the 5th row then are resistor measured actual value in this test event among the present invention.Can see that its performance index of resistor among the present invention are much better than national standard from table, average index is better than a GB 1-2 order of magnitude.
Claims (2)
1, a kind of metal film high-resistance resistor, it is characterized in that adopting the Si-Cr-Ni-Re quaternary alloy system high sputtering-resistant target material that contains rare earth element to make, the concrete composition of target is Si (35%-72%), Cr (25%-50%), Ni (2%-20%), Si, Cr and Ni element percent of total are 100%, rare earth element is group of the lanthanides and actinium series lucium, and content is the 0.1%-3.0% of Si, Cr and Ni element total weight.
2, a kind of manufacturing process of metal film high-resistance resistor is characterized in that adopting in the technology direct current sputtering to add radio frequency sputtering, obtains the resistive element of double membrane structure; The preceding operating room of direct current sputtering forevacuum is 5 * 10
-3More than the pa, direct current sputtering gas is argon gas, and sputtering pressure is 1.0-3.0 * 10
-1Pa, sputtering power are 200-450W, and the time is 20-100 minute; The radio frequency sputtering working gas is argon gas and oxygen mixture, Ar and O
2Percent by volume be 9: 1, sputtering pressure is 1.0-3.0 * 10
-1Pa, power are 500W, and the time is 10-20 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99113963 CN1093310C (en) | 1999-08-06 | 1999-08-06 | Metal film high-resistance resistor and mfg. technology thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99113963 CN1093310C (en) | 1999-08-06 | 1999-08-06 | Metal film high-resistance resistor and mfg. technology thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1243322A true CN1243322A (en) | 2000-02-02 |
| CN1093310C CN1093310C (en) | 2002-10-23 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 99113963 Expired - Fee Related CN1093310C (en) | 1999-08-06 | 1999-08-06 | Metal film high-resistance resistor and mfg. technology thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102013294A (en) * | 2010-09-10 | 2011-04-13 | 东莞市福德电子有限公司 | High-resistance value metal oxide film resistor and manufacture method thereof |
| CN103429788A (en) * | 2011-03-28 | 2013-12-04 | 吉坤日矿日石金属株式会社 | Metal foil provided with electrically resistive film, and method for producing same |
| CN104485190A (en) * | 2014-11-27 | 2015-04-01 | 天津大学 | Method for improving moisture and heat resistance of Cr-Si high resistance film resistor based on electro-catalytic property |
| CN107686909A (en) * | 2016-08-03 | 2018-02-13 | 国立屏东科技大学 | Thin film resistance alloy |
| CN114360824A (en) * | 2021-12-29 | 2022-04-15 | 西安交通大学 | NiCr CuNi double-layer film resistor with near-zero resistance temperature coefficient and preparation method thereof |
-
1999
- 1999-08-06 CN CN 99113963 patent/CN1093310C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102013294A (en) * | 2010-09-10 | 2011-04-13 | 东莞市福德电子有限公司 | High-resistance value metal oxide film resistor and manufacture method thereof |
| CN103429788A (en) * | 2011-03-28 | 2013-12-04 | 吉坤日矿日石金属株式会社 | Metal foil provided with electrically resistive film, and method for producing same |
| CN104485190A (en) * | 2014-11-27 | 2015-04-01 | 天津大学 | Method for improving moisture and heat resistance of Cr-Si high resistance film resistor based on electro-catalytic property |
| CN104485190B (en) * | 2014-11-27 | 2017-05-03 | 天津大学 | Method for improving moisture and heat resistance of Cr-Si high resistance film resistor based on electro-catalytic property |
| CN107686909A (en) * | 2016-08-03 | 2018-02-13 | 国立屏东科技大学 | Thin film resistance alloy |
| CN114360824A (en) * | 2021-12-29 | 2022-04-15 | 西安交通大学 | NiCr CuNi double-layer film resistor with near-zero resistance temperature coefficient and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1093310C (en) | 2002-10-23 |
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