CN115662719A - Lead-free thick film resistor paste and preparation method thereof - Google Patents
Lead-free thick film resistor paste and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a lead-free thick film resistor paste, which comprises: a conductive phase, glass frit, an additive and an organic vehicle; the conductive phase is micron-sized carbon,Sodium carboxymethylcellulose and La 0.5 Sr 0.5 Co 1‑ y Nb y O 3 A mixture of (a); the glass powder is a mixture obtained by mixing glass powder A and glass powder B; the additive comprises ZrSiO 4 、CuO、MnO 2 、TiO 2 、Ta 2 O 5 And Ni 2 O 3 At least two of; the invention also provides a preparation method of the lead-free thick film resistor paste. The invention has the beneficial effects that: the resistance paste is extremely low in cost, does not contain lead, does not cause environmental pollution, is adjustable in resistance value and temperature coefficient, is large in resistance value regulation range, is small in difference value between HTCR and CTCR, is kept within 200ppm, and can be used for preparing piezoresistive films and piezoresistive sensors; the encapsulation change rate and the electrostatic discharge performance of the resistance paste meet the requirements.
Description
Technical Field
The invention belongs to the technical field of resistor paste, and particularly relates to lead-free thick film resistor paste and a preparation method thereof.
Background
The resistor is used as an important functional component in the circuit, plays an important role in shunting and dividing voltage, and is the key for normal operation of the whole circuit. The resistor is fired from a resistance paste, which is typically composed of a conductive phase, a glass phase, and an organic vehicle.
The traditional resistance paste contains a large amount of lead in a glass phase and a conductive phase, the content of the lead is usually between 20 and 60 percent, the lead belongs to one of three heavy metal pollutants, the lead is a heavy metal element seriously harming human health, and the ideal lead content in a human body is zero.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides lead-free thick film resistor paste and a preparation method thereof.
The lead-free thick film resistor paste comprises the following components in percentage by mass: 5 to 10 percent of conductive phase, 50 to 70 percent of glass powder, 1 to 3 percent of additive and 20 to 45 percent of organic carrier;
the conductive phases are micron-sized carbon, sodium carboxymethylcellulose (NaCMC for short) and La 0.5 Sr 0.5 Co 1-y Nb y O 3 (abbreviated as LSCNb), wherein y is 0.02 to 0.08; wherein the proportion of micron-sized carbon to sodium carboxymethylcellulose is (1 0.5 Sr 0.5 Co 1-y Nb y O 3 The mixture ratio of (1;
the glass powder is glass powderA and glass powder B are mixed according to the proportion of (2-3) to 1, and the mixing proportion is calculated according to the mass ratio; the glass powder A is made of SiO 2 、H 3 BO 3 、Al 2 O 3 、CaCO 3 ZnO, mgO and BaCO 3 Composition is carried out; the glass powder B is composed of Bi 2 O 3 、H 3 BO 3 、SiO 2 、Al 2 O 3 And IrO 2 Composition is carried out;
the additive comprises ZrSiO 4 、CuO、MnO 2 、TiO 2 、Ta 2 O 5 And Ni 2 O 3 At least two of;
the organic carrier comprises 5-30% of resin and 70-95% of solvent by mass percent, wherein the resin is at least one of polymethacrylic resin, epoxy thermosetting resin, lauric acid, polyethylene wax and polyanionic cellulose; the solvent is at least one of terpineol, ethylene carbonate, lecithin and mixed dibasic acid ester.
Preferably, the content of the glass powder A is 50 to 55% SiO in terms of mole percentage 2 、6%～10%H 3 BO 3 、4%～7%Al 2 O 3 、3～6%CaCO 3 20 to 40% of ZnO, 1 to 5% of MgO and 10 to 15% of BaCO 3 And (4) forming.
Preferably, the content of the glass powder B is 50 to 65% by mole of Bi 2 O 3 、15%～25%H 3 BO 3 、5%～15%SiO 2 、2.5%～7.5%Al 2 O 3 And 5% to 15% of IrO 2 And (4) forming.
The preparation method of the lead-free thick film resistor paste comprises the following steps:
preparing a conductive phase: preheating the carbon micron powder to obtain micron-sized carbon; taking La by mol percent 2 O 3 、SrCO 3 、Co 2 O 3 And Nb 2 O 5 Then pre-ground with deionized water and heated in air, re-ground and dried, and the ground product was bonded with a PVA binder to give La 0.5 Sr 0.5 Co 1-y Nb y O 3 (ii) a Preparing sodium carboxymethylcellulose aqueous solution;mixing micron-sized carbon, sodium carboxymethyl cellulose and La 0.5 Sr 0.5 Co 1-y Nb y O 3 Mixing according to a set proportion to obtain a conductive phase;
preparing glass powder: 50-55% of SiO in mol% 2 、6%～10%H 3 BO 3 、4%～7%Al 2 O 3 、3%～6%CaCO 3 20 to 40% of ZnO, 1 to 5% of MgO and 10 to 15% of BaCO 3 Then uniformly mixing, smelting at a set temperature value for a set time, then water quenching for a set time, and sieving through dry grinding and wet grinding until the average particle size after sieving is smaller than a set value to obtain glass powder A; 50-65% of Bi by mol percentage 2 O 3 、15%～25%H 3 BO 3 、5%～15%SiO 2 、2.5%～7.5%Al 2 O 3 And 5% to 15% of IrO 2 Then uniformly mixing, smelting at a set temperature value for a set time, then water quenching for a set time, and sieving through dry grinding and wet grinding until the average particle size after sieving is smaller than a set value to obtain glass powder B; mixing the obtained glass powder A and glass powder B in a ratio of (2-3) to 1 to obtain glass powder;
preparing an organic carrier;
mixing the prepared conductive phase, the glass powder and the organic carrier with the additive, uniformly stirring by using a glass rod, and standing for a set time to finish infiltration; and then rolling the mixture by a three-roller mill until the fineness of the mixture is less than a set value to obtain the resistance paste.
Preferably, the preparation method of the conductive phase specifically comprises the following steps: preheating commercially available carbon micron powder with the transverse size of 3 microns to obtain micron-sized carbon; la 4.7% by mol 2 O 3 、4.7%SrCO 3 、90%Co 2 O 3 And 0.6% of Nb 2 O 5 Then pre-grinding with deionized water for 24 hours, heating at 1000 ℃ for 12 hours in the air, re-grinding for 24 hours and drying, and binding the ground product with PVA binder to obtain La with average particle size of 2.5 μm or less 0.5 Sr 0.5 Co 1- y Nb y O 3 (ii) a Preparing sodium carboxymethylcellulose (NaCMC) aqueous solution; mixing micron-sized carbonSodium carboxymethylcellulose (abbreviated as NaCMC) and La 0.5 Sr 0.5 Co 1-y Nb y O 3 Mixing the materials according to a set proportion to obtain the conductive phase.
Preferably, the preparation method of the organic carrier is as follows: mixing 83g of terpineol, 15g of polyanionic cellulose and 2g of lecithin, heating to 65-75 ℃ in a water bath, continuously stirring until the mixture is completely dissolved and homogenized, stopping heating, and cooling for 24 hours at room temperature to obtain a mixture; uniformly mixing 35g of the mixture, 60g of terpineol, 4g of epoxy thermosetting resin, 0.5g of polyethylene wax and 0.5g of lauric acid to obtain an organic carrier; the mass percent of the solvent in the organic carrier is 89.05 percent, and the mass percent of the resin is 10.95 percent.
Preferably, the mass percent of the prepared sodium carboxymethyl cellulose aqueous solution is 1.83%, and the mass percent of the obtained sodium carboxymethyl cellulose aqueous solution and the organic carrier is 20:1.
preferably, when the glass powder A is prepared, the melting temperature is 1300 ℃, and the average grain diameter of the sieved glass powder is less than 2.5 mu m; when the glass powder B is prepared, the melting temperature is 1100 ℃, and the average grain diameter of the sieved glass powder is less than 2.5 mu m.
Preferably, the fineness of the resulting resistor paste is less than 3 μm.
Preferably, the additives selected for preparing the resistance paste are CuO and ZrSiO 4 The mass ratio of the mixture is 1.
The beneficial effects of the invention are: the resistance paste has the outstanding advantages of extremely low cost, no lead, no environmental pollution, adjustable resistance value and temperature coefficient, large resistance value regulation range and capability of being used for preparing piezoresistive films and piezoresistive sensors; the encapsulation change rate and the electrostatic discharge performance of the resistance paste meet the requirements.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are set forth merely to aid in the understanding of the invention. It should be noted that, for a person skilled in the art, several modifications can be made to the invention without departing from the principle of the invention, and these modifications and modifications also fall within the protection scope of the claims of the present invention.
Example 1
Step 1, preparing a conductive phase:
(1) Preheating commercially available carbon micron powder with a transverse dimension of 3 microns to obtain micron-sized carbon (marked as C);
(2) La 4.7% by mol 2 O 3 、 4.7%SrCO 3 、90%Co 2 O 3 And 0.5% of Nb 2 O 5 Then pre-ground with deionized water for 24 hours, heated at 1000 ℃ for 12 hours in air, re-ground for 24 hours and dried, and the ground product is bonded with a PVA binder to obtain La with an average particle size of 2.5 μm or less 0.5 Sr 0.5 Co 1-y Nb y O 3 (labeled as D); preparing sodium carboxymethylcellulose (NaCMC) aqueous solution;
(3) Micron-sized carbon (labeled C), sodium carboxymethyl cellulose and La 0.5 Sr 0.5 Co 1-y Nb y O 3 (marked as D) mixing according to a set proportion to obtain a conductive phase;
step 2, preparing glass powder: taking 50 to 55 percent of SiO according to the mol percentage 2 、6%～10%H 3 BO 3 、4%～7%Al 2 O 3 、3～6%CaCO 3 20 to 40% of ZnO, 1 to 5% of MgO and 10 to 15% of BaCO 3 Then evenly mixing, smelting at 1300 ℃ for a set time, quenching with water, and sieving through dry grinding and wet grinding until the average particle size after sieving is less than 2.5 mu m to obtain glass powder A; 50-65% of Bi by mol percentage 2 O 3 、15%～25%H 3 BO 3 、5%～15%SiO 2 、2.5%～7.5%Al 2 O 3 And 5% to 15% of IrO 2 Then evenly mixing, smelting at 1100 ℃ for a set time, quenching with water, and sieving through dry grinding and wet grinding until the average particle size after sieving is less than 2.5 mu m to obtain glass powder B; mixing the obtained glass powder A and glass powder B according to the proportion of 3;
step 3, preparing an organic carrier: mixing 83g of terpineol, 15g of polyanionic cellulose and 2g of lecithin, heating to 65-75 ℃ in a water bath, continuously stirring until the mixture is completely dissolved and homogenized, stopping heating, and cooling for 24 hours at room temperature to obtain a mixture; uniformly mixing 35g of the mixture, 60g of terpineol, 4g of epoxy thermosetting resin, 0.5g of polyethylene wax and 0.5g of lauric acid to obtain an organic carrier; the mass percent of the solvent in the organic carrier is 89.05 percent, and the mass percent of the resin is 10.95 percent;
step 4, finally, independently preparing 1.83 mass percent sodium carboxymethylcellulose (NaCMC) aqueous solution;
step 5, taking 2g of micron-sized carbon (marked as C) with the grain diameter of less than 3 mu m and 8g of La 0.5 Sr 0.5 Co 1-y Nb y O 3 (marked as D), 40g of glass powder, 2.5g of additive and 47.5g of organic carrier, stirring uniformly by using a glass rod, standing for more than 1h to complete infiltration, and then rolling by using a three-roller mill to ensure that the fineness is less than or equal to 3 mu m to obtain the resistance paste.
Example 2
On the basis of embodiment 1, this embodiment adopts the same steps 1 to 4 as embodiment 1, and step 5 of this embodiment is: taking 3g micrometer carbon (labeled C) with particle diameter less than 3 μm, and 7g La 0.5 Sr 0.5 Co 1-y Nb y O 3 (marked as D), 40g of glass powder, 2.5g of additive and 47.5g of organic carrier, stirring uniformly by a glass rod, standing for more than 1h to complete soaking, and rolling by a three-roll mill to ensure that the fineness is less than or equal to 3 mu m to obtain the resistance paste.
Example 3
On the basis of embodiment 1, this embodiment adopts steps 1 to 4 the same as those of embodiment 1, and step 5 of this embodiment is: taking 4g micrometer carbon (labeled C) with particle diameter less than 3 μm, and 6g La 0.5 Sr 0.5 Co 1-y NbyO 3 (marked as D), 2.5g of additive and 47.5g of organic carrier, stirring uniformly by using a glass rod, standing for more than 1h to complete infiltration, and then rolling by using a three-roll mill to ensure that the fineness is less than or equal to 5 mu m to obtain the resistance paste.
Example 4
On the basis of example 1, the present example employs the same steps 1 to 1 as in example 1Step 5 of this embodiment is: 5g micron-sized carbon (marked as C) with a particle size of less than 3 μm and 5g La are taken 0.5 Sr 0.5 Co 1-y Nb y O 3 (marked as D), 40g of glass powder, 2.5g of additive and 47.5g of organic carrier, stirring uniformly by using a glass rod, standing for more than 1h to complete infiltration, and rolling by using a three-roller mill to ensure that the fineness is less than or equal to 3 mu m to obtain the resistance paste.
Example 5
On the basis of embodiment 1, this embodiment adopts steps 1 to 4 the same as those of embodiment 1, and step 5 of this embodiment is: taking 6g micrometer carbon (labeled C) with particle diameter less than 3 μm, and 4g La 0.5 Sr 0.5 Co 1-y Nb y O 3 (marked as D), 40g of glass powder, 2.5g of additive and 47.5g of organic carrier, stirring uniformly by a glass rod, standing for more than 1h to complete soaking, and rolling by a three-roll mill to ensure that the fineness is less than or equal to 3 mu m to obtain the resistance paste.
Example 6
On the basis of embodiment 1, this embodiment adopts the same steps 1 to 4 as embodiment 1, and step 5 of this embodiment is: taking 7g micrometer carbon (labeled C) with particle diameter less than 3 μm, and 3g La 0.5 Sr 0.5 Co 1-y Nb y O 3 (marked as D), 40g of glass powder, 2.5g of additive and 47.5g of organic carrier, stirring uniformly by using a glass rod, standing for more than 1h to complete infiltration, and rolling by using a three-roller mill to ensure that the fineness is less than or equal to 3 mu m to obtain the resistance paste.
Example 7
On the basis of embodiment 1, this embodiment adopts the same steps 1 to 4 as embodiment 1, and step 5 of this embodiment is: taking 8g micron-sized carbon (marked as C) with the particle diameter of less than 3 μm and 2g La 0.5 Sr 0.5 Co 1-y Nb y O 3 (marked as D), 40g of glass powder, 2.5g of additive and 47.5g of organic carrier, stirring uniformly by a glass rod, standing for more than 1h to complete soaking, and rolling by a three-roll mill to ensure that the fineness is less than or equal to 3 mu m to obtain the resistance paste.
Example 8
In the base of example 1In the above embodiment, steps 1 to 4 are the same as those in embodiment 1, and step 5 in this embodiment is: taking 9g micrometer carbon (labeled C) with particle diameter less than 3 μm, and 1g La 0.5 Sr 0.5 Co 1-y Nb y O 3 (marked as D), 40g of glass powder, 2.5g of additive and 47.5g of organic carrier, stirring uniformly by using a glass rod, standing for more than 1h to complete infiltration, and rolling by using a three-roller mill to ensure that the fineness is less than or equal to 3 mu m to obtain the resistance paste.
The resistance pastes of examples 1 to 8 were tested for their performance (test results are shown in table 1 below):
the resistance pastes of the above examples 1 to 8 were respectively screen-printed, leveled, and dried at 150 ℃ for 10min, and sintered by a tunnel furnace according to resistance sintering curves of peak temperature 800 ℃, duration 10min, temperature rise time 25min, and temperature fall time 35min, to obtain a plurality of sets of chip resistance sample wafers.
The method comprises the following steps of testing all sample wafers by film thickness, resistance, electrostatic discharge (ESD), temperature Coefficient (TCR) and the like, and averaging the three sample wafers tested in each group, wherein the specific testing method comprises the following steps:
1. resistance (R) test method: selecting a resistance meter with a proper measuring range, respectively lapping two test meter pens of the resistance meter on electrodes at two ends of a resistance to be tested, and recording a numerical value and a unit displayed on the resistance meter;
2. positive temperature coefficient (HTCR) testing was performed: and setting the temperature of the test equipment to be 25 ℃, measuring and recording the resistance value of the resistor to be tested to be R1 after the temperature is stable. And setting the temperature of the test equipment to 125 ℃, measuring and recording the resistance value of the resistor to be tested to be R2 after the temperature is stable. The positive temperature coefficient of resistance is calculated according to the following formula:
in the above formula, the first and second carbon atoms are,
representing the positive temperature coefficient of the resistance to be measured, R1 beingThe resistance value of the resistor to be tested is measured when the temperature of the test equipment is 25 ℃; r2 is the resistance value of the resistor to be tested measured when the temperature of the test equipment is 125 ℃;
3. negative temperature coefficient (CTCR) testing was performed: the temperature of the test equipment was set to 25 ℃, and after the temperature stabilized, the resistance was measured as R3 and recorded. The temperature of the test equipment was set to-55 deg.C, and after the temperature stabilized, the resistance was measured as R4 and recorded. The positive temperature coefficient of resistance is calculated according to the following formula:
in the above-mentioned formula, the compound has the following structure,
representing the positive temperature coefficient of the resistor to be tested, wherein R3 is the resistance value of the resistor to be tested measured when the temperature of the test equipment is 25 ℃, and R4 is the resistance value of the resistor to be tested measured when the temperature of the test equipment is-55 ℃;
table 1 resistance paste performance test data table
As shown in Table 1 above, examples 1 to 8 used micron-sized carbon (denoted by C) and La 0.5 Sr 0.5 Co 1-y Nb y O 3 The mixture of (LSCNb, y = 0.02-0.08) (marked as D) is used as a conductive phase, and the resistance and the temperature coefficient of the resistance paste prepared by the glass powder A and the glass powder B are adjustable, the difference between HTCR and CTCR is small and is kept within 200 ppm; the invention has the outstanding advantages of low cost, no lead, no environmental pollution, adjustable resistance value and temperature coefficient, and wide resistance value regulation range, and can be used for piezoresistive sensors.
Claims (10)
1. A lead-free thick-film resistor paste comprising, in mass percent: 5 to 10 percent of conductive phase, 50 to 70 percent of glass powder, 1 to 3 percent of additive and 20 to 45 percent of organic carrier;
the conductive phases are micron-sized carbon, sodium carboxymethyl cellulose and La 0.5 Sr 0.5 Co 1-y Nb y O 3 Wherein y is 0.02 to 0.08; wherein the proportion of micron-sized carbon to sodium carboxymethylcellulose is (1 0.5 Sr 0.5 Co 1-y NbyO 3 The mixture ratio of (1;
the glass powder is a mixture obtained by mixing the glass powder A and the glass powder B in a ratio of (2-3) to 1, and the mixing ratio is calculated by mass ratio; the glass powder A is made of SiO 2 、H 3 BO 3 、Al 2 O 3 、CaCO 3 ZnO, mgO and BaCO 3 Forming; the glass powder B is composed of Bi 2 O 3 、H 3 BO 3 、SiO 2 、Al 2 O 3 And IrO 2 Composition is carried out;
the additive comprises ZrSiO 4 、CuO、MnO 2 、TiO 2 、Ta 2 O 5 And Ni 2 O 3 At least two of;
the organic carrier comprises 5-30% of resin and 70-95% of solvent by mass percent, wherein the resin is at least one of polymethacrylic resin, epoxy thermosetting resin, lauric acid, polyethylene wax and polyanionic cellulose; the solvent is at least one of terpineol, ethylene carbonate, lecithin and mixed dibasic acid ester.
2. The lead-free thick-film resistor paste of claim 1, wherein: the content of the glass powder A is 50 to 55 percent of SiO in terms of mole percentage 2 、6%～10%H 3 BO 3 、4%～7%Al 2 O 3 、3%～6%CaCO 3 20 to 40% of ZnO, 1 to 5% of MgO and 10 to 15% of BaCO 3 And (4) forming.
3. The lead-free thick-film resistor paste of claim 1, wherein: the glass powder B is composed of, in mole percent, 50% -65% 2 O 3 、15%～25%H 3 BO 3 、5%～15%SiO 2 、2.5%～7.5%Al 2 O 3 And 5% to 15% of IrO 2 And (4) forming.
4. A method of preparing the lead-free thick-film resistor paste of any one of claims 1 to 3, comprising the steps of:
preparing a conductive phase: preheating the carbon micron powder to obtain micron-sized carbon; taking La by mol percent 2 O 3 、SrCO 3 、Co 2 O 3 And Nb 2 O 5 Then pre-ground with deionized water and heated in air, re-ground and dried, and the ground product was bonded with a PVA binder to give La 0.5 Sr 0.5 Co 1-y Nb y O 3 (ii) a Preparing sodium carboxymethylcellulose aqueous solution; mixing micron-sized carbon, sodium carboxymethyl cellulose and La 0.5 Sr 0.5 Co 1-y Nb y O 3 Mixing according to a set proportion to obtain a conductive phase;
preparing glass powder: 50-55% of SiO in mol percent 2 、6%～10%H 3 BO 3 、4%～7%Al 2 O 3 、3～6%CaCO 3 20-40% of ZnO, 1-5% of MgO and 10-15% of BaCO 3 Then uniformly mixing, smelting at a set temperature value for a set time, then water quenching for a set time, and sieving through dry grinding and wet grinding until the average particle size after sieving is smaller than a set value to obtain glass powder A; 50-65% of Bi by mol percentage 2 O 3 、15%～25%H 3 BO 3 、5%～15%SiO 2 、2.5%～7.5%Al 2 O 3 And 5% to 15% of IrO 2 Then uniformly mixing, smelting at a set temperature value for a set time, then water quenching for a set time, and sieving through dry grinding and wet grinding until the average particle size after sieving is smaller than a set value to obtain glass powder B; mixing the obtained glass powder A and glass powder B in a ratio of (2-3) to 1 to obtain glass powder;
preparing an organic carrier;
mixing the prepared conductive phase, the glass powder and the organic carrier with an additive, uniformly stirring, and standing for a set time to finish infiltration; and then rolling the mixture by a three-roller mill until the fineness of the mixture is less than a set value to obtain the resistance paste.
5. The method of preparing the lead-free thick film resistor paste of claim 4, wherein the conductive phase is prepared by: preheating commercially available carbon micron powder with the transverse size of 3 microns to obtain micron-sized carbon; la 4.7% by mol 2 O 3 、4.7%SrCO 3 、90%Co 2 O 3 And 0.6% of Nb 2 O 5 Then pre-grinding with deionized water for 24 hours, heating at 1000 ℃ for 12 hours in the air, re-grinding for 24 hours and drying, and binding the ground product with PVA binder to obtain La with average particle size of 2.5 μm or less 0.5 Sr 0.5 Co 1-y Nb y O 3 (ii) a Preparing sodium carboxymethylcellulose aqueous solution; mixing micron-sized carbon, sodium carboxymethyl cellulose and La 0.5 Sr 0.5 Co 1-y Nb y O 3 Mixing the materials according to a set proportion to obtain the conductive phase.
6. The method of preparing the lead-free thick-film resistor paste of claim 4, wherein the organic vehicle is prepared by: mixing 83g of terpineol, 15g of polyanionic cellulose and 2g of lecithin, heating to 65-75 ℃ in a water bath, continuously stirring until the mixture is completely dissolved and homogenized, stopping heating, and cooling for 24 hours at room temperature to obtain a mixture; uniformly mixing 35g of the mixture, 60g of terpineol, 4g of epoxy thermosetting resin, 0.5g of polyethylene wax and 0.5g of lauric acid to obtain an organic carrier; the mass percent of the solvent in the organic carrier is 89.05 percent, and the mass percent of the resin is 10.95 percent.
7. The method of making a lead-free thick film resistor paste of claim 6, wherein: the mass percent of the prepared sodium carboxymethyl cellulose aqueous solution is 1.83%, and the mass percent of the obtained sodium carboxymethyl cellulose aqueous solution to the organic carrier is 20:1.
8. the method of preparing a lead-free thick-film resistor paste of claim 4, wherein: when the glass powder A is prepared, the smelting temperature is 1300 ℃, and the average grain diameter of the sieved glass powder is less than 2.5 mu m; when the glass powder B is prepared, the melting temperature is 1100 ℃, and the average grain diameter of the sieved glass powder is less than 2.5 mu m.
9. The method of preparing a lead-free thick-film resistor paste of claim 4, wherein: the fineness of the obtained resistance paste is less than 3 mu m.
10. The method of making the lead-free thick film resistor paste of claim 4, wherein: the additives selected for preparing the resistance slurry are CuO and ZrSiO 4 The mass ratio of the mixture is 1.
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