CN1148722A - Inorganic thick-film resistance coating - Google Patents
Inorganic thick-film resistance coating Download PDFInfo
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- CN1148722A CN1148722A CN 96106321 CN96106321A CN1148722A CN 1148722 A CN1148722 A CN 1148722A CN 96106321 CN96106321 CN 96106321 CN 96106321 A CN96106321 A CN 96106321A CN 1148722 A CN1148722 A CN 1148722A
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Abstract
The present invention relates to an inorganic thick-film resistor coating, the weight ratio of its ingredients is graphite powder 41.7-55.6, lead oxide 36.8-48.4 and boric oxide 7.6-9.9. Said two oxides are melted, pulverized and ground, mixed with graphite powder, the powdered mixture is made into slurry material by using liquid organic carrier, said slurry materal is applied onto the insulating base material to make film, and then said film is dried and sintered to obtain the invented product. It possesses the advantages of low cost, long service life, heat-resisting, moisture-proof nd good thermal stability, etc..
Description
The present invention relates to resistance material, or rather, relate to inorganic thick-film resistance coating and preparation method thereof.
The resistive coating used always of people has following three major types so far: (1) admixing type resistive coating; (2) Intrinsical resistive coating; (3) inorganic thick-film resistance coating.It is binding agent that the admixing type resistive coating generally adopts organic polymer resin, and binding agent itself is non-conductive, by mixing the resistance dusty material with certain conductivity, relies on the mutual overlap joint between these powder particles and forms the network type conductive channel.Its major defect is: binding agent is an organic polymer resin, the hydroscopicity height, and coating resistance instability, heat resistance be poor, be subject to heat ageing, therefore limited the commercial applications of admixing type organic polymer resistive coating greatly.The Intrinsical resistive coating does not need to mix the resistance dusty material, but regulates the resistance value of coating by the conductivity that macromolecule resin itself is had.Yet the synthesis technique of this conductive polymer resin is very complicated, and cost is too high, and the film resistance of its coating is not suitable for using as resistive coating generally more than megaohm.In addition, also there is serious problem in this type coating at heatproof, moisture-proof, aspect such as ageing-resistant, causes the application of Intrinsical resistive coating still to be difficult to reach commercialization.The exploitation of inorganic thick-film resistance coating is later relatively, it be with resistant to elevated temperatures electric conducting materials such as graphite as the resistance powder,, its system film and sintering are made after adding organic carrier as binding agent with the powder of glass-like materials.With respect to preceding two type coatings, inorganic thick-film resistance coating can anti-higher temperature, yet when this type coating of preparation on glass, ceramic-like ground, bursts easily, thereby make the rate of finished products reduction, thereby increased cost.And the disbonding phenomenon in use takes place easily, shortened useful life greatly.In addition, the recipe ingredient of frit binding agent is generally all complicated, except that lead oxide, silica, boron oxide and the basic glass ingredient of zinc oxide conduct, also increase bismuth oxide, thallium oxide, lithia etc. are arranged, the recipe ingredient that has is more complicated, increasing has (addition of above three class components are 1%～8%) such as (addition of above six kinds of oxides are 1%～5%) such as cobalt oxide, aluminium oxide, cupric oxide, iron oxide, tin oxide, selenium oxide, alkali metal oxide, alkaline earth oxide and rare earth oxides.So complicated component has increased considerably manufacturing cost, and manufacturing process is difficult to stable.
Therefore, the objective of the invention is to provide a kind of shortcoming that can overcome above-mentioned a few quasi-resistance coatings, its recipe ingredient is simpler, and manufacturability is better, inorganic thick-film resistance coating that performance is more superior and preparation method thereof.
The inventor finds through after the further investigation of long period, making the prescription of frit binding agent can greatly simplify, only get final product with lead oxide and two kinds of components of boron oxide, just tighter to ratio requirement, as long as proportioning is proper, its performance is better than the frit binding agent of complicated prescription, because this discovery, thereby finished the present invention.
Technical scheme of the present invention is as follows:
The proportioning of inorganic thick-film resistance coating (weight portion):
The composition weight portion
Graphite powder (C)≤149um (100 order) 41.7～55.6
Lead oxide (PbO) 36.8～48.4
Boron oxide (B
2O
3) 7.6～9.9
The preparation method of inorganic thick-film resistance coating:
According to the proportioning weight portion with lead oxide, boron oxide mixes, 750～900 ℃ heat to fusion, treat after its cooling the frit block that is obtained to be pulverized and ball milling, sieve is got the following particle of 74um (200 order), adding granularity by the proportioning weight portion then is the following graphite powder of 149um (100 order), and add the nothing fixedly boiling point and the commercially available liquid organic carrier that under follow-up bake out temperature, can all volatilize be equivalent to mixture total weight amount 10～25%, be modulated into the slurry that is suitable for making film, adopt conventional thick film filming technology on the pretreated high temperature insulation surface of bottom material that insulate, making film then, 100～200 ℃ of down oven dry 7～13 minutes, at last 350～550 ℃ of following sintering 10～15 minutes.
In inorganic thick-film resistance coating of the present invention, graphite powder is as the resistance dusty material that plays electric action, and its granularity is defined as≤149um.The frit that lead oxide and boron oxide are made through high-temperature fusion plays the binding agent effect.
Compare with the resistive coating of prior art, outstanding advantage of the present invention is: component is simpler, cost is lower, the life-span is long, (long-term heatproof can reach 280 ℃ to heatproof, the short-term heatproof can reach 450 ℃), moisture-proof (hydroscopicity≤0.1%), wear-resisting, corrosion-resistant, ageing-resistant and storage stability and thermal stability be all good, and manufacturing process is simple, process repeatability is fabulous, the rate of finished products height, coating combines firmly with ground.What deserves to be mentioned is that the inventor finds in experiment, after in the glass dust binding agent, adding silica and zinc oxide, the softening temperature of glass binder is increased by 60～100 ℃ at least, but also can increase the viscosity of glass binder, this is extremely harmful to the sintering film forming.As for adding other multiple oxides also is unnecessary, because the inventor has found the best ratio range of lead oxide and boron oxide, it is unnecessary that this just makes that the above-mentioned multiple oxide of increase becomes.
What be worth paying special attention to is the present invention to the ratio requirement strictness: the weight portion of boron oxide surpass the upper limit then inorganic thick-film resistance coating be prone to unsettled slow hydrolysis, surpass lower limit the coating be full of cracks easily take place; The weight portion of lead oxide surpass the upper limit then inorganic thick-film resistance coating be prone to the layering peeling, surpass lower limit and be prone to the not yet done situation of sintering; The weight portion of graphite powder surpass the upper limit then coating combine not firmly with ground, be easy to chap above lower limit.Therefore should be specifically noted that the weight portion scope of proportioning.
Further explain the present invention below in conjunction with preferred embodiment and accompanying drawing thereof.Wherein:
Fig. 1, inorganic thick-film resistance coating element front view;
The sectional view of Fig. 2, element shown in Figure 1.
In Fig. 2: 1) base plate; 2) inorganic thick-film resistance coating; 3) electrode.
Embodiment 1
The rectangular ceramic sheet of preparing a block length 100mm, wide 80mm, thick 5mm is as base plate.Respectively coat a long 80mm, the electrode of wide 10mm with two minor faces of commercially available conductive silver slurry on the same side of this base plate.With this base plate together with the electrode dry for standby.
In addition, the resistive coating material of preparation 1000g is also made inorganic resistive coating, and used prescription is as follows:
Composition weight (g)
Graphite powder (C) (≤74um) 500
Lead oxide (PbO) 415
Boron oxide (B
2O
3) 85
With two kinds of composition mixings except that graphite powder in the above-mentioned prescription, with this mixture in 800 ℃ of following fusions 60 minutes.With its fragmentation, used the ball mill ball milling then 48 hours after the frit block cooling of waiting to be obtained, sieve the Powdered inorganic binder of acquisition≤74um with the standard screen of 74um (200 order).Toward wherein adding graphite powder, add the liquid organic carrier that 170g is made up of 95%a terpinol and 5% ethyl cellulose then, be modulated into uniform slurry.Adopting silk-screen printing technique that a small amount of slurry is printed on ceramic bottom board has on the side surface of thin layer electrode 3.It 150 ℃ of down oven dry 10 minutes, 460 ℃ of following sintering 12 minutes, has promptly been made inorganic thick-film resistance coating of the present invention (2 among Fig. 2) again, and the thickness of coating is about 0.2mm.Thereby having formed an area is 10 * 8=80cm
2The tabular resistive element.Get two interelectrode resistance with the resistance instrumentation and be about 55 Ω.
In embodiment 2, except replacing the ceramic bottom board with metal sheet surface enamel and through the base plate that insulation is handled, other all experimentize by the condition of embodiment 1, have obtained the substantially the same result of embodiment 1.
Stability test (storage stability)
Each 10 of 2 kinds of resistive elements that the foregoing description 1-2 is obtained store 1 year under China's south wet weather, the result does not find any one resistive element moisture absorption or goes mouldy.The resistance value testing result shows that the variable quantity of its square resistance all＜0.8%.
Should illustrate that inorganic thick-film resistance coating of the present invention is not limited to tabular, and it can also make tubulose, and is cylindric waits different shape.Be particularly suitable for making various large power, electrically resistance elements to using in high resistive element of stability requirement and the main equipment.Also can be used as heating element and use, for example make various types of heating appliances.Those skilled in the art can make many variations to the foregoing description in design of the present invention and claim institute restricted portion, yet all these variations all considered to be in the scope of the present invention.
Claims (5)
1, a kind of inorganic thick-film resistance coating is characterized in that, it contains following ingredients (weight portion):
The composition weight portion
Graphite powder (C)≤149um (100 order) 41.7～55.6
Lead oxide (PbO) 36.8～48.4
Boron oxide (B
2O
3) 7.6～9.9
2, the method for preparing the described inorganic resistive coating of claim 1, it is characterized in that, according to the described weight portion of claim 1 with lead oxide, boron oxide, mix, be heated to and dissolve, treat after its cooling the frit block that is obtained to be pulverized and ball milling, sieve is got the following particle of 74um (200 order), add the following graphite powder of granularity≤149um (100 order) by the described weight portion of claim 1, and add the nothing fixedly boiling point and the commercially available liquid organic carrier that under follow-up bake out temperature, can all volatilize be equivalent to mixture total weight amount 10～25%, mixture is modulated into the slurry that is suitable for making film, adopt conventional thick film filming technology through the pretreated high temperature insulation surface of bottom material system film that insulate then, 100～200 ℃ of oven dry down, at last at 350～550 ℃ of following sintering.
3, method as claimed in claim 2 is characterized in that, wherein said heating and melting temperature is 750～900 ℃.
4, method as claimed in claim 2 is characterized in that, wherein said drying time under 100～200 ℃ is 7～13 minutes.
5, method as claimed in claim 2 is characterized in that, the sintering time under wherein said 350～550 ℃ is 10～15 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96106321 CN1148722A (en) | 1996-06-13 | 1996-06-13 | Inorganic thick-film resistance coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96106321 CN1148722A (en) | 1996-06-13 | 1996-06-13 | Inorganic thick-film resistance coating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1148722A true CN1148722A (en) | 1997-04-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96106321 Pending CN1148722A (en) | 1996-06-13 | 1996-06-13 | Inorganic thick-film resistance coating |
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|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105993052A (en) * | 2013-12-04 | 2016-10-05 | 奥斯兰姆奥普托半导体有限责任公司 | Varistor paste, optoelectronic component, method for producing a varistor paste and method for producing a varistor element |
| CN113766681A (en) * | 2021-09-10 | 2021-12-07 | 厦门海洋芯科技有限公司 | Electric heating film electrode and electric heating body with same |
| CN113800889A (en) * | 2021-09-10 | 2021-12-17 | 厦门海洋芯科技有限公司 | Carbon Hertz film and application thereof |
-
1996
- 1996-06-13 CN CN 96106321 patent/CN1148722A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105993052A (en) * | 2013-12-04 | 2016-10-05 | 奥斯兰姆奥普托半导体有限责任公司 | Varistor paste, optoelectronic component, method for producing a varistor paste and method for producing a varistor element |
| CN105993052B (en) * | 2013-12-04 | 2018-09-11 | 奥斯兰姆奥普托半导体有限责任公司 | Varistor paste, photoelectric subassembly, the method for manufacturing varistor paste and the method for manufacturing piezoresistive element |
| CN113766681A (en) * | 2021-09-10 | 2021-12-07 | 厦门海洋芯科技有限公司 | Electric heating film electrode and electric heating body with same |
| CN113800889A (en) * | 2021-09-10 | 2021-12-17 | 厦门海洋芯科技有限公司 | Carbon Hertz film and application thereof |
| CN113800889B (en) * | 2021-09-10 | 2022-10-28 | 厦门海洋芯科技有限公司 | Carbon Hertz film and application thereof |
| CN113766681B (en) * | 2021-09-10 | 2023-08-18 | 厦门海洋芯科技有限公司 | Electrothermal film electrode and electric heating body with same |
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