CN103643085B - Embed type film resistor material and preparation method thereof - Google Patents
Embed type film resistor material and preparation method thereof Download PDFInfo
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- CN103643085B CN103643085B CN201310566007.5A CN201310566007A CN103643085B CN 103643085 B CN103643085 B CN 103643085B CN 201310566007 A CN201310566007 A CN 201310566007A CN 103643085 B CN103643085 B CN 103643085B
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Abstract
The present invention relates to a kind of embed type film resistor material and preparation method thereof.This embed type film resistor material presses atomic percentage, comprises nickel 50 ~ 76%, chromium 10 ~ 18%, carbon 10 ~ 30% and tungsten 0.5 ~ 5%.By magnetron sputtering technique nickel, chromium, carbon and tungsten atom be deposited on Copper Foil substrate and obtain nickel chromium triangle carbon W film, our experiments show that, use the electrical property of the embed type thin film resistor device of this nickel chromium triangle carbon W film more stable, sheet resistance value is higher.
Description
Technical field
The present invention relates to electronic material and technical field of electronic components, particularly relate to a kind of embed type film resistor material and preparation method thereof.
Background technology
The development trend of electronic devices and components high-performance, miniaturization, the electronic devices and components quantity requiring printed circuit board (PCB) unit surface to mount constantly increases, and causes printed circuit board surface to amass over-saturation.Compared with traditional discrete formula resistance, embed type thin film resistor device (burying resistance) can save wiring distance, reduces attachment component number, reduces circuit board size and weight; The induction reactance produced in parasitic inductance in signals transmission and surface mount or plug-in unit processing can be reduced; The impedance matching capability of circuit can be improved; Signal cross-talk, noise and electromagnetic interference can be reduced.Embed type thin film resistor device reliability is high, and resistance value is stablized, and loss is little.Embed type thin film resistor device is that film resistor material is overlayed on special semicure resin board, forms sheet resistance, be then laminated into printed wiring intralamellar part after etching.
The embed type film resistor material of Foreign Modern table has: the NiP that Ohmega Ply company adopts electrochemical plating to produce buries resistance material, the NiCr that GOULD electronics, inc. adopts magnetron sputtering method to produce, these material sheet resistance value tolerances are little, electric performance stablity, but sheet resistance value is less than normal, use range is limited, and various aspects of performance also also has the space promoted.Domestic, embed type film resistor material many places, in development, also do not enter industrialization completely.
Summary of the invention
Based on this, be necessary that providing a kind of can improve the electric performance stablity of embed type thin film resistor device and improve the embed type film resistor material of sheet resistance value.
A kind of embed type film resistor material, by atomic percentage, comprising:
Nickel 50 ~ 76%, chromium 10 ~ 18%, carbon 10 ~ 30% and tungsten 0.5 ~ 5%.
A kind of embed type film resistor material, comprise nickel chromium triangle carbon W film, the element of described nickel chromium triangle carbon W film presses atomic percentage, comprises nickel 50 ~ 76%, chromium 10 ~ 18%, carbon 10 ~ 30% and tungsten 0.5 ~ 5%.
Wherein in an embodiment, also comprise substrate, described nickel chromium triangle carbon W film is deposited on described substrate.
Wherein in an embodiment, described substrate is low profile flexible copper clad.
Wherein in an embodiment, the thickness of described nickel chromium triangle carbon W film is 85 nanometer ~ 200 nanometers.
A preparation method for embed type film resistor material, comprises the steps:
Substrate is provided; And
Adopt sputtering method to form nickel chromium triangle carbon W film over the substrate, obtain embed type film resistor material, wherein, the element of described nickel chromium triangle carbon W film presses atomic percentage, comprises nickel 50 ~ 76%, chromium 10 ~ 18%, carbon 10 ~ 30% and tungsten 0.5 ~ 5%.
Wherein in an embodiment, after described employing sputtering method forms the step of nickel chromium triangle carbon W film over the substrate, also comprise the step of described nickel chromium triangle carbon W film being carried out high temperature annealing.
Wherein in an embodiment, the step of described high temperature annealing is in shielding gas atmosphere, anneals 480 seconds ~ 720 seconds at 250 DEG C ~ 400 DEG C.
Wherein in an embodiment, the step that described employing sputtering method forms nickel chromium triangle carbon W film over the substrate adopts nichrome target, carbon target and tungsten target material, nickel chromium triangle, carbon and tungsten are sputtered onto on described substrate, deposit nickel chromium triangle carbon W film over the substrate.
Wherein in an embodiment, described employing sputtering method is formed in the step of nickel chromium triangle carbon W film over the substrate, the electric current of described nichrome target is 2 ~ 5 peaces, and the electric current of described carbon target is that 1 peace ~ 1.5 are pacified, and the electric current of described tungsten target material is that 0.1 peace ~ 0.3 is pacified.
Wherein in an embodiment, described employing sputtering method is formed in the step of nickel chromium triangle carbon W film over the substrate, applies the bias voltage of 30 volts ~ 120 volts over the substrate.
Wherein in an embodiment, described employing sputtering method is formed in the step of nickel chromium triangle carbon W film over the substrate, and described substrate rotates, and the speed of described rotation is 4 revs/min.
Above-mentioned embed type film resistor material, by atomic percentage, comprises nickel 50 ~ 76%, chromium 10 ~ 18%, carbon 10 ~ 30% and tungsten 0.5 ~ 5%.By magnetron sputtering technique nickel, chromium, carbon and tungsten atom be deposited on Copper Foil substrate and obtain nickel chromium triangle carbon W film, our experiments show that, use the electrical property of the embed type thin film resistor device of this nickel chromium triangle carbon W film more stable, sheet resistance value is higher.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of the embed type film resistor material of an embodiment;
Fig. 2 is temperature coefficient of resistance (TCR) the variation with temperature curve of the embed type film resistor material of embodiment 1 and the embed type film resistor material of comparative example 1;
Fig. 3 is temperature coefficient of resistance (TCR) the variation with temperature curve of the embed type film resistor material of embodiment 2 and the embed type film resistor material of comparative example 2;
Fig. 4 is temperature coefficient of resistance (TCR) the variation with temperature curve of the embed type film resistor material of embodiment 3 and the embed type film resistor material of comparative example 1;
Fig. 5 is temperature coefficient of resistance (TCR) the variation with temperature curve of the embed type film resistor material of embodiment 4 and the embed type film resistor material of comparative example 2;
Fig. 6 is the polarization curve of the embed type film resistor material of embodiment 1 and the embed type film resistor material of comparative example 1;
Fig. 7 is the polarization curve of the embed type film resistor material of embodiment 2 and the embed type film resistor material of comparative example 2;
Fig. 8 is nickel chromium triangle carbon tungsten (NiCrCW) film prepared by embodiment 1 is soak SEM shape appearance figure after 85 hours in the H2SO4 of 60% at mass percent concentration;
Fig. 9 is nickel chromium triangle (NiCr) film of preparation in comparative example 1 is soak SEM shape appearance figure after 85 hours in the H2SO4 of 60% at mass percent concentration.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
The embed type film resistor material of one embodiment, by atomic percentage, comprises nickel 50 ~ 76%, chromium 10 ~ 18%, carbon 10 ~ 30% and tungsten 0.5 ~ 5%.
Use above-mentioned alloy material to prepare nickel chromium triangle carbon W film, this nickel chromium triangle carbon W film can be used in preparing that electrical property is comparatively stable, the higher embed type thin film resistor device of sheet resistance value.
The embed type film resistor material of another embodiment, comprises nickel chromium triangle carbon W film.
The material of nickel chromium triangle carbon W film using nickel (Ni) and chromium (Cr) as material of main part, the carbon (C) adulterating appropriate and tungsten (W).Wherein, by atomic percentage, nickel accounts for 50 ~ 76%, and chromium accounts for 10 ~ 18%, and carbon accounts for 10 ~ 30%, and tungsten accounts for 0.5% ~ 5%.
Preferably, the thickness of nickel chromium triangle carbon W film is 85 nanometer ~ 200 nanometers.
This nickel chromium triangle carbon W film is using Ni and Cr as material of main part, the W element of appropriate C element of adulterating and trace, this nickel chromium triangle carbon W film is made to have stable electrical property, large sheet resistance value, high hardness, good erosion resistance and wear resistance, have better properties than existing Of NiCr Alloy Films Resistance material.
Carbon mainly exists with amorphous and nanocrystalline mixed structure form at nickel chromium triangle carbon W film; their mixed interface can promote the diffusion of chromium element in nichrome; thus make the easier chromium sesquioxide protective membrane forming densification on surface of chromium, make the corrosion resistance nature of nickel chromium triangle carbon W film higher.
The stable chemical nature of W elements, even if in case of heating, also can not with the effect of the strong acid such as hydrochloric acid, sulfuric acid, even can not be dissolved in chloroazotic acid, be only corrosive extremely strong hydrofluoric acid and the mixture of nitric acid, could dissolve tungsten.W elements further increases the corrosion resistance nature of nickel chromium triangle carbon W film.
Preferably, embed type film resistor material also comprises substrate, and nickel chromium triangle carbon W film is deposited on substrate.
Substrate is ceramic substrate or metal substrate, is preferably low profile (VLP) flexible copper clad.Two relative surfaces of low profile flexible copper clad are respectively light face and hair side, and the roughness of hair side is comparatively even.
Preferably, nickel chromium triangle carbon W film is deposited on the hair side of low profile flexible copper clad, not only can increase the sheet resistance value of nickel chromium triangle carbon W film, the bonding force of nickel chromium triangle carbon W film and substrate can also be improved, be conducive to preparing that sheet resistance value is high, the embed type thin film resistor device of good stability.
Our experiments show that, above-mentioned embed type film resistor material has higher electric performance stablity and higher sheet resistance value, and, there is higher hardness, higher corrosion resistance nature and comparatively high-wearing feature, make this embed type film resistor material have higher using value, range of application is wider.
When applying this embed type film resistor material, this embed type film resistor material is carried out etching obtain need bury resistance device, be then laminated to printed wiring intralamellar part.
Nickel chromium triangle carbon W film is etched into after burying resistance device, buries the low profile flexible copper clad that retains of resistance two ends and as the electrode burying resistance, the step preparing electrode in addition can be eliminated, be conducive to reducing costs.
Further, adopt low profile (VLP) flexible copper clad to be substrate, when preparing nickel chromium triangle carbon W film, circle can be realized around formula plated film, being applicable to suitability for industrialized production.
Refer to Fig. 1, the preparation method of the embed type film resistor material of an embodiment, comprises the steps:
Step S110: substrate is provided.
Substrate is preferably low profile flexible copper clad.
By substrate each ultrasonic cleaning 10 minutes in anhydrous propanone, dehydrated alcohol and deionized water successively, then dry up by nitrogen gun, then flatten stand-by with clean glass plate.
Step S120: adopt sputtering method to form nickel chromium triangle carbon W film on substrate, obtain embed type film resistor material, wherein, the element of nickel chromium triangle carbon W film presses atomic percentage, comprises nickel 50 ~ 76%, chromium 10 ~ 18%, carbon 10 ~ 30% and tungsten 0.5 ~ 5%.
Nichrome target (NiCr) is placed in the negative electrode target position 1 of vacuum sputtering room, carbon target (C) is placed in negative electrode target position 2, and tungsten target material (W) is placed in negative electrode target position 3, and substrate is fixed on rotational workpieces frame.
Wherein, the nickel of nichrome target and the atomic ratio of chromium are 4:1.The purity of nichrome target, carbon target and tungsten target material is 99.99%.
Vacuum sputtering room is sealed, makes the vacuum tightness of vacuum sputtering room reach 3.0 × 10 by pumped vacuum systems
-5~ 4.5 × 10
-5tuo Sila.Pass into argon gas, gas flow is 25 ~ 30sccm, when vacuum sputtering chamber pressure reaches 1.1 × 10
-3~ 1.5 × 10
-3during Tuo Sila, start ionization power supply, carry out ionization cleaning to substrate surface, scavenging period is 5 ~ 10 minutes, then at room temperature opens the shielding power supply of nichrome target, carbon target and tungsten target material three target simultaneously, pre-sputtering is after 5 ~ 10 minutes, open the turn switch of rotational workpieces frame, rotational workpieces frame rotated and drives substrate to rotate, sputtering 4 ~ 16 minutes, nickel chromium triangle carbon tungsten is deposited on substrate, thus on substrate, form nickel chromium triangle carbon W film.
First pre-sputtering sputters after 5 ~ 10 minutes again, removes the dust of each target material surface, is conducive to obtaining matter measured nickel chromium triangle carbon W film.
Preferably, in sputter procedure, the electric current of nichrome target is 2 ~ 5 peaces, and the electric current of carbon target is 1 ~ 1.5 peace, and the electric current of tungsten target material is 0.1 ~ 0.3 peace.
Preferably, in sputter procedure, substrate applies the bias voltage of 30 volts ~ 120 volts.
Preferably, in sputter procedure, the speed of rotation of substrate is 4 revs/min.
The electric current of nichrome target is 2 ~ 5 peaces, the electric current of carbon target is 1 ~ 1.5 peace, the electric current of tungsten target material is 0.1 ~ 0.3 peace, on substrate, apply the bias voltage of 30 volts ~ 120 volts and the speed of rotation of substrate is sputter nickel chromium triangle, carbon and tungsten under the sputtering condition of 4 revs/min, is conducive to forming the nickel chromium triangle carbon W film that compactness is higher, defect is few.
Preferably, closed field unbalanced magnetron sputtering technology is adopted to sputter.Relative to the sputtering of traditional unbalanced magnetron, the nickel chromium triangle carbon W film that closed field unbalanced magnetron sputtering is formed is finer and close, defect is few, and quality is high.Further, adopt closed field unbalanced magnetron sputtering technology to sputter, be conducive to the bonding force improving nickel chromium triangle carbon W film and substrate.
Preferably, after adopting sputtering method to form nickel chromium triangle carbon W film on substrate, the step of nickel chromium triangle carbon W film being carried out high temperature annealing is also comprised.
The step of high temperature annealing is preferably in shielding gas atmosphere, anneals 480 seconds ~ 720 seconds at 250 DEG C ~ 400 DEG C.
Sputter complete, after circulating water, take out the nickel chromium triangle carbon W film be deposited on substrate from vacuum sputtering room, and put into RTP-500 type fast heat treatment device and carry out anneal.Annealing conditions is under shielding gas atmosphere, short annealing 480 seconds ~ 720 seconds at 250 DEG C ~ 400 DEG C, takes out the embed type film resistor material after annealing after cooling.
Wherein, the element of nickel chromium triangle carbon W film presses atomic percentage, comprises nickel 50 ~ 76%, chromium 10 ~ 18%, carbon 10 ~ 30% and tungsten 0.5 ~ 5%.
Shielding gas is the rare gas elementes such as nitrogen, argon gas, helium, is preferably nitrogen.
Anneal 480 seconds ~ 720 seconds at 250 DEG C ~ 400 DEG C, the stress of the nickel chromium triangle carbon W film obtained is little, defect is few, electric performance stablity.
Preparation method's technique of above-mentioned embed type film resistor material is simple, prepared by obtain that the compactness of the nickel chromium triangle carbon W film of embed type film resistor material is high, good uniformity, and higher with the bonding force of substrate.Further, this preparation method is suitable for large-area coating film and produces, and is conducive to suitability for industrialized production.
Set forth further below by way of specific embodiment.
Embodiment 1
Prepare embed type film resistor material
(1) be each ultrasonic cleaning 10 minutes in anhydrous propanone, raw spirit and deionized water successively of 9cm × 9cm low profile flexible copper clad area, then dry up by nitrogen gun, then flatten stand-by with clean sheet glass;
(2) the low profile flexible copper clad of pressing is placed on the rotational workpieces frame of vacuum sputtering room, and closes vacuum sputtering room.Open pumped vacuum systems, when the vacuum tightness of vacuum sputtering chamber reaches 4.0 × 10
-5during Tuo Sila, pass into argon gas, gas flow is 25sccm, start ionization power supply, to substrate surface ionization cleaning 10 minutes, open the shielding power supply of nichrome target, carbon target and tungsten target material three target immediately, sputter 4 minutes, form the nickel chromium triangle carbon W film be deposited on substrate.Wherein, the target current of nichrome target, carbon target and tungsten target material is set to 3 peaces, 1 peace and 0.1 peace respectively, and the bias voltage be applied on substrate is 90 volts, and underlayer temperature is room temperature, and the rotating speed of rotational workpieces frame is set to 4 revs/min;
(3) after having sputtered, after circulating water, take out the nickel chromium triangle carbon W film be deposited on substrate from vacuum sputtering room, the thickness of nickel chromium triangle carbon W film is about 91 nanometers.The element of nickel chromium triangle carbon W film comprises nickel 65.0at.%, chromium 16.5at.%, carbon 17.6at.%, tungsten 0.9at.% by atomic percent.
Embodiment 2
Prepare embed type film resistor material
(1) be each ultrasonic cleaning 10 minutes in anhydrous propanone, raw spirit and deionized water successively of 9cm × 9cm low profile flexible copper clad area, then dry up by nitrogen gun, then flatten stand-by with clean sheet glass;
(2) the low profile flexible copper clad of pressing is placed on the rotational workpieces frame of vacuum sputtering room, and closes vacuum sputtering room.Open pumped vacuum systems, when the vacuum tightness of vacuum sputtering chamber reaches 4.0 × 10
-5during Tuo Sila, pass into argon gas, gas flow is 25sccm, start ionization power supply, to substrate surface ionization cleaning 10 minutes, open the shielding power supply of nichrome target, carbon target and tungsten target material three target immediately, sputter 4 minutes, form the deposited nickel chromium triangle carbon W film be deposited on substrate.Wherein, the target current of nichrome target, carbon target and tungsten target material is set to 3 peaces, 1 peace and 0.1 peace respectively, and the bias voltage be applied on substrate is 90 volts, and underlayer temperature is room temperature, and the rotating speed of rotational workpieces frame is set to 4 revs/min;
(3) after having sputtered, after circulating water, the nickel chromium triangle carbon W film being deposited on substrate is taken out from vacuum sputtering room.The nickel chromium triangle carbon W film this being deposited on substrate is put into RTP-500 type fast heat treatment device and is carried out anneal, and annealing conditions is: under nitrogen protection, anneals 540 seconds at 300 DEG C, the nickel chromium triangle carbon W film resistive material after the annealing obtained.Wherein, the thickness of nickel chromium triangle carbon W film is 88.9 nanometers.The element of nickel chromium triangle carbon W film comprises nickel 62.7at.%, chromium 17.1at.%, carbon 19.4at.%, tungsten 0.8at.% by atomic percent.
Embodiment 3
Prepare embed type film resistor material
(1) be each ultrasonic cleaning 10 minutes in anhydrous propanone, raw spirit and deionized water successively of 9cm × 9cm low profile flexible copper clad area, then dry up by nitrogen gun, then flatten stand-by with clean sheet glass;
(2) the low profile flexible copper clad of pressing is placed on the rotational workpieces frame of vacuum sputtering room, and closes vacuum sputtering room.Open pumped vacuum systems, when the vacuum tightness of vacuum sputtering chamber reaches 4.0 × 10
-5during Tuo Sila, pass into argon gas, gas flow is 25sccm, start ionization power supply, to substrate surface ionization cleaning 10 minutes, open the shielding power supply of nichrome target, carbon target and tungsten target material three target immediately, sputter 4 minutes, form the deposited nickel chromium triangle carbon W film be deposited on substrate, obtain embed type film resistor material.Wherein, the target current of nichrome target, carbon target and tungsten target material is set to 3 peaces, 1.5 peaces and 0.1 peace respectively, and the bias voltage be applied on substrate is 90 volts, and underlayer temperature is room temperature, and the rotating speed of rotational workpieces frame is set to 4 revs/min.Wherein, the thickness of nickel chromium triangle carbon W film is 93.7 nanometers.The element of nickel chromium triangle carbon W film comprises nickel 60.4at.%, chromium 14.6at.%, carbon 24.1at.%, tungsten 0.9at.% by atomic percent.
Embodiment 4
Prepare embed type film resistor material
(1) be each ultrasonic cleaning 10 minutes in anhydrous propanone, raw spirit and deionized water successively of 9cm × 9cm low profile flexible copper clad area, then dry up by nitrogen gun, then flatten stand-by with clean sheet glass;
(2) the low profile flexible copper clad of pressing is placed on the rotational workpieces frame of vacuum sputtering room, and closes vacuum sputtering room.Open pumped vacuum systems, when the vacuum tightness of vacuum sputtering chamber reaches 4.0 × 10
-5during Tuo Sila, pass into argon gas, gas flow is 25sccm, start ionization power supply, to substrate surface ionization cleaning 10 minutes, open the shielding power supply of nichrome target, carbon target and tungsten target material three target immediately, sputter 4 minutes, form the deposited nickel chromium triangle carbon W film be deposited on substrate, obtain embed type film resistor material.Wherein, the target current of nichrome target, carbon target and tungsten target material is set to 3 peaces, 1.5 peaces and 0.1 peace respectively, and the bias voltage be applied on substrate is 90 volts, and underlayer temperature is room temperature, and the rotating speed of rotational workpieces frame is set to 4 revs/min.The nickel chromium triangle carbon W film this being deposited on substrate is put into RTP-500 type fast heat treatment device and is carried out anneal, and annealing conditions is: under nitrogen protection, anneals 540 seconds at 300 DEG C, the nickel chromium triangle carbon W film resistive material after the annealing obtained.Wherein, the thickness of nickel chromium triangle carbon W film is 91.5 nanometers.The element of nickel chromium triangle carbon W film comprises nickel 60.1at.%, chromium 13.8at.%, carbon 25.3at.%, tungsten 0.8at.% by atomic percent.
Comparative example 1
Prepare embed type film resistor material
(1) be each ultrasonic cleaning 10 minutes in anhydrous propanone, raw spirit and deionized water successively of 9cm × 9cm low profile flexible copper clad area, then dry up by nitrogen gun, then flatten stand-by with clean sheet glass;
(2) the low profile flexible copper clad of pressing is placed on the rotational workpieces frame of vacuum sputtering room, and closes vacuum sputtering room.Open pumped vacuum systems, when the vacuum tightness of vacuum sputtering chamber reaches 4.0 × 10
-5during Tuo Sila, pass into argon gas, gas flow is 25sccm, starts ionization power supply, to substrate surface ionization cleaning 10 minutes, opens nichrome target as sputter power supply immediately, sputters 4 minutes, form the deposited nickel-chromium thin film be deposited on substrate.The target current of nichrome target is set to 3 peaces, and the bias voltage be applied on substrate is 90 volts, and underlayer temperature is room temperature, and the rotating speed of rotational workpieces frame is set to 4 revs/min;
(3) after having sputtered, after circulating water, the nickel-chromium thin film being deposited on substrate is taken out from vacuum sputtering room.The thickness of nickel-chromium thin film is about 94.8 nanometers.The element of nickel-chromium thin film comprises nickel 78.9at.% and chromium 21.1at.% by atomic percent.
Comparative example 2
Prepare embed type film resistor material
(1) be each ultrasonic cleaning 10 minutes in anhydrous propanone, raw spirit and deionized water successively of 9cm × 9cm low profile flexible copper clad area, then dry up by nitrogen gun, then flatten stand-by with clean sheet glass;
(2) the low profile flexible copper clad of pressing is placed on the rotational workpieces frame of vacuum sputtering room, and closes vacuum sputtering room.Open pumped vacuum systems, when the vacuum tightness of vacuum sputtering chamber reaches 4.0 × 10
-5during Tuo Sila, pass into argon gas, gas flow is 25sccm, starts ionization power supply, to substrate surface ionization cleaning 10 minutes, opens nichrome target as sputter power supply immediately, sputters 4 minutes, form the deposited nickel-chromium thin film be deposited on substrate.The target current of nichrome target is set to 3 peaces, and the bias voltage be applied on substrate is 90 volts, and underlayer temperature is room temperature, and the rotating speed of rotational workpieces frame is set to 4 revs/min;
(3) after having sputtered, after circulating water, the nickel-chromium thin film being deposited on substrate is taken out from vacuum sputtering room.RTP-500 type of the putting into fast heat treatment device this being deposited on the nickel chromium triangle carbon W film of substrate carries out anneal, and annealing conditions is: under nitrogen protection, anneals 540 seconds at 300 DEG C, the Of NiCr Alloy Films Resistance material after the annealing obtained.Wherein, the thickness of nickel-chromium thin film is 92.6 nanometers.The element of nickel-chromium thin film comprises nickel 77.3at.% and chromium 22.7at.% by atomic percent.
The nickel chromium triangle carbon W film of embodiment 1 ~ embodiment 4 and comparative example 1 ~ comparative example 2 and nickel-chromium thin film are etched into after burying resistance device, 250 DEG C are heated rapidly to respectively with HFSE-PB4 type detection probes platform, and then be cooled to 10 DEG C equably gradually, its resistance value in process of cooling is surveyed, according to formula with Keithley2410 type digital sourcemeter
calculate the temperature coefficient of resistance burying resistance, make the relation curve (Fig. 2) of temperature coefficient of resistance about temperature of embodiment 1 and comparative example 1, the temperature coefficient of resistance of embodiment 2 and comparative example 2 is about the relation curve (Fig. 3) of temperature, the temperature coefficient of resistance of embodiment 3 and comparative example 1 is about the relation curve (Fig. 4) of temperature, and the temperature coefficient of resistance of embodiment 4 and comparative example 2 is about the relation curve (Fig. 5) of temperature.
As seen from Figure 2, the temperature coefficient of resistance variation with temperature curve of the NiCrCW film (example 1) of deposited is more steady than NiCr film (comparative example 1) curve of deposited, and the two temperature coefficient of resistance variation range is respectively 3.39≤| TCR
niCrCW|≤219.62ppm/K, 165.72≤TCR
niCr≤ 378.97ppm/K, illustrates that the NiCrCW film of deposited is stablized than the electrical property of corresponding NiCr film.
As seen from Figure 3, the NiCrCW Thin film resistive temperature coefficient variation with temperature curve after 300 DEG C of annealing is more steady than the curve of the NiCr film after annealing under the same terms.The temperature coefficient of resistance variation range of the two is respectively 2.86≤TCR
niCrCW≤ 199.97ppm/K, 35.26≤TCR
niCr≤ 327.31ppm/K, after 300 DEG C of annealing are described, NiCrCW film is stablized than the NiCr thin-film electro performance after the same terms annealing.
As seen from Figure 4, the temperature coefficient of resistance variation with temperature curve of the NiCrCW film (example 3) of deposited is more steady than NiCr film (comparative example 1) curve of deposited, and the two temperature coefficient of resistance variation range is respectively 5.69≤| TCR
niCrCW≤ 101.15ppm/K, 165.72≤TCR
niCr≤ 378.97ppm/K, illustrates that the NiCr thin-film electro performance of the ratio deposited of the NiCrCW film of deposited is stablized.
As seen from Figure 5, NiCrCW film (embodiment 4) the temperature coefficient of resistance variation with temperature curve after 300 DEG C of annealing is more steady than the curve of the NiCr film (embodiment 2) after annealing under the same terms.The temperature coefficient of resistance variation range of the two is respectively 3.87≤TCR
niCrCW≤ 98.15ppm/K, 35.26≤TCR
niCr≤ 327.31ppm/K, after 300 DEG C of annealing are described, NiCrCW film is stablized than the NiCr thin-film electro performance after the same terms annealing.
Bury resistance material at NiCr adulterate appropriate C element and W element from above four groups of data declarations, contribute to the temperature coefficient of resistance reducing embed type film resistor material, have promoter action to the electrical property improving embed type film resistor material.
After measured, the sheet resistance value of embodiment 1 nickel chromium triangle carbon W film is 76.95 Ω/Sq, the sheet resistance value of embodiment 2 nickel chromium triangle carbon W film is 59.87 Ω/Sq, the sheet resistance value of embodiment 3 nickel chromium triangle carbon W film is 85.26 Ω/Sq, the sheet resistance value of embodiment 4 nickel chromium triangle carbon W film is 73.48 Ω/Sq, and the sheet resistance value of comparative example 1 is the sheet resistance value of 62.84 Ω/Sq comparative examples 2 is 50.05 Ω/Sq.These data declarations bury in resistance material at NiCr adulterate appropriate C element and W element can improve the sheet resistance value of burying resistance material.
Mass percent concentration is adopted to be the H of 60%
2sO
4as corrosive fluid, platinized platinum is supporting electrode, and the saturated calomel of standard is reference electrode, under room temperature, by the passivation anodic polarization curves of the embed type film resistor material of electrochemical workstation testing example 1, embodiment 2, comparative example 1, comparative example 2, test result is shown in Fig. 6 and Fig. 7.
In Fig. 6, the NiCr film of the deposited of the corresponding comparative example 1 of NiCr, the NiCrCW film of the deposited of the corresponding embodiment 1 of NiCrCW.In Fig. 7, the corresponding comparative example 2 of NiCr annealed after NiCr film, the annealed NiCrCW film of the corresponding embodiment 2 of NiCrCW.
From Fig. 6 and Fig. 7, no matter in deposited or after annealing, little all than NiCr film of the corrosion current of NiCrCW film, and NiCrCW film transpassivation current potential is to the right, these phenomenons all illustrate that to adulterate in NiCr film C element and W element are conducive to improving the erosion resistance of film.Exist with amorphous and nanocrystalline mixed structure form because C is main in the film, their mixed interface can promote the diffusion of Cr element in alloy, thus makes the easier Cr forming densification on surface of Cr
2o
3protective membrane.The chemical property of W is very stable, even if in case of heating, also can not with hydrochloric acid, effect of sulfuric acid, even can not be dissolved in chloroazotic acid, be only corrosive extremely strong hydrofluoric acid and the mixture of nitric acid, could dissolve tungsten.This illustrates, embodiment 1 and embodiment 2 are higher than the erosion resistance of the embed type sheet resistance of comparative example 1 and comparative example 2 respectively.
Mass percent concentration is adopted to be the H of 60%
2sO
4as corrosive fluid, the embed type film resistor material of embodiment 1 and comparative example 1 is soaked 85 hours in corrosive fluid, then uses scanning electron microscopic observation, respectively as shown in Figure 8 and Figure 9.Comparison diagram 8 and Fig. 9 can find out, from the size be corroded, NiCrCW film is obviously little, show that the corrosion resistance nature of NiCrCW film is stronger than NiCr film.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (7)
1. an embed type film resistor material, is characterized in that, comprises nickel chromium triangle carbon W film, and the element of described nickel chromium triangle carbon W film presses atomic percentage, by following elementary composition: nickel 50 ~ 76%, chromium 10 ~ 18%, carbon 10 ~ 30% and tungsten 0.5 ~ 5%.
2. embed type film resistor material according to claim 1, is characterized in that, also comprise substrate, and described nickel chromium triangle carbon W film is deposited on described substrate.
3. embed type film resistor material according to claim 2, is characterized in that, described substrate is low profile flexible copper clad.
4. embed type film resistor material according to claim 1, is characterized in that, the thickness of described nickel chromium triangle carbon W film is 85 nanometer ~ 200 nanometers.
5. a preparation method for embed type film resistor material, comprises the steps:
Substrate is provided; And
Sputtering method is adopted to form nickel chromium triangle carbon W film over the substrate, obtain embed type film resistor material, wherein, the element of described nickel chromium triangle carbon W film presses atomic percentage, by following elementary composition: nickel 50 ~ 76%, chromium 10 ~ 18%, carbon 10 ~ 30% and tungsten 0.5 ~ 5%;
After described employing sputtering method forms the step of nickel chromium triangle carbon W film over the substrate, also comprise the step of described nickel chromium triangle carbon W film being carried out high temperature annealing;
The step of described high temperature annealing is in shielding gas atmosphere, anneals 480 seconds ~ 720 seconds at 250 DEG C ~ 400 DEG C;
The step that described employing sputtering method forms nickel chromium triangle carbon W film over the substrate adopts nichrome target, carbon target and tungsten target material, nickel chromium triangle, carbon and tungsten is sputtered onto on described substrate, deposits nickel chromium triangle carbon W film over the substrate;
Described employing sputtering method is formed in the step of nickel chromium triangle carbon W film over the substrate, and the electric current of described nichrome target is 2 ~ 5 peaces, and the electric current of described carbon target is that 1 peace ~ 1.5 are pacified, and the electric current of described tungsten target material is that 0.1 peace ~ 0.3 is pacified.
6. the preparation method of embed type film resistor material according to claim 5, is characterized in that, described employing sputtering method is formed in the step of nickel chromium triangle carbon W film over the substrate, applies the bias voltage of 30 volts ~ 120 volts over the substrate.
7. the preparation method of embed type film resistor material according to claim 5, is characterized in that, described employing sputtering method is formed in the step of nickel chromium triangle carbon W film over the substrate, and described substrate rotates, and the speed of described rotation is 4 revs/min.
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| CN104988358A (en) * | 2015-07-22 | 2015-10-21 | 宁波工程学院 | Thin film resistance material and preparation method thereof |
| CN106435478A (en) * | 2016-07-01 | 2017-02-22 | 中国计量大学 | Preparation method of nickel-chromium-silicon film low in resistance temperature coefficient |
| CN116137197A (en) * | 2023-04-20 | 2023-05-19 | 广州方邦电子股份有限公司 | Composite substrate and circuit board |
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