CN107572824A - A kind of high thermal stability medium powder, its precursor, preparation method and application - Google Patents
A kind of high thermal stability medium powder, its precursor, preparation method and application Download PDFInfo
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- CN107572824A CN107572824A CN201710875592.5A CN201710875592A CN107572824A CN 107572824 A CN107572824 A CN 107572824A CN 201710875592 A CN201710875592 A CN 201710875592A CN 107572824 A CN107572824 A CN 107572824A
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- high thermal
- thermal stability
- medium powder
- stability medium
- thick film
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Abstract
The invention discloses a kind of high thermal stability medium powder, its precursor, preparation method and application.The precursor of the high thermal stability medium powder is made up of four kinds of montmorillonitic clay, Concave-convex clay rod, agstone, diatomite mineral materials.The preparation method of the high thermal stability medium powder includes：The high thermal stability medium powder precursor by high temperature melting, water quenching and is ground into processing successively, the high thermal stability medium powder is made.The present invention prepares high thermal stability medium powder using montmorillonitic clay, Concave-convex clay rod, agstone, diatomite as main raw material, not only raw material sources enrich for it, it is cheap, and the preparation method has the features such as technique is simple, and high temperature melting temperature is low, the time is short, energy consumption is low, and cost is cheap, it is easy to industrialization, it is very high that thick film dielectric coating thermal shock resistance is obtained simultaneously, can fully be met the needs of current thick film dielectric paste product, is particularly suitable for the application in high thermal shock field.
Description
Technical field
The present invention relates to a kind of thick film dielectric powder and its preparation technology, more particularly to one kind using montmorillonitic clay,
High insulation resistance thick film dielectric powder that Concave-convex clay rod, agstone and diatomite are formed for raw material and preparation method thereof
And application.
Background technology
Thick-film heating is a kind of Novel heating technology occurred with the development of thick film circuit technique, each in recent years
Kind family expenses and industrial electroheat device field possess the market demand of many trillion member.Thick film heating device is from inside to outside mainly by matrix, interior
Insulating medium layer, resistant heat generating layer and external insulation dielectric layer composition.Carrier and workbench of the matrix as thick-film heating, it is thick
The critical component of film heater.
Stainless steel is printing due to having the advantages that high mechanical strength, shock resistance are good, flatness is high, thermal conductivity is high
The most popular supporting base material of thick film circuit.But stainless steel is conductive in itself, and thermal coefficient of expansion is larger, therefore conductive in printing
There must be the matched use of the preferable deielectric-coating of matched coefficients of thermal expansion, insulating properties therewith during heating thick film.Dielectric
The thick film layers of high bond strength, heat conduction and good insulation preformance can be formed in metal surface, are the crucial core of thick-film heating technology
The heart.
Aluminous Silicate Glass-Ceramics powder is the thick film dielectric powder being most widely used at present, but existing aluminosilicate crystallite
Glass dust is because adhesive force and heat shock resistance intensity are relatively low, and its coating formed on stainless steel substrate easily comes off, and device makes
It is relatively low with the life-span.
The content of the invention
For deficiency of the prior art, an object of the present invention is before providing a kind of high thermal stability medium powder
Body, it includes the following component calculated by weight：50~100 parts of montmorillonitic clay, 40~80 parts of Concave-convex clay rod, lime
10~25 parts of 25~50 parts of stone flour and diatomite.
The second object of the present invention is to provide a kind of preparation method of high thermal stability medium powder, and it includes following step
Suddenly：
High thermal stability medium powder precursor is provided, includes following component：50~100 parts of montmorillonitic clay, attapulgite
10~25 parts of 40~80 parts of clay, 25~50 parts of agstone and diatomite；
Each component in the high thermal stability medium powder precursor is uniformly mixed, and melting is formed more than 1200 DEG C
Glass precursor solution；
The glass precursor solution is subjected to water quenching, forms devitrified glass slag；
And the devitrified glass sizing system is formed into high thermal stability medium powder of the particle diameter at 0.1~10 μm.
Further, the preparation method of the high thermal stability medium powder can include：The high thermal stability is situated between
Matter powder precursor is at 1200~1350 DEG C, particularly preferably in 1250~1300 DEG C of more than melting 15min, particularly preferably 15~
120min, form the glass precursor solution.
Further, the preparation method of the high thermal stability medium powder can include：By the devitrified glass slag according to
Secondary ground, ball milling forms the high thermal stability medium powder.
Further, among the preparation method of the high thermal stability medium powder, the process conditions of the ball milling are excellent
Elect as：Ball milling speed is 500~650r/min, and Ball-milling Time is 4~24h.
The third object of the present invention is to provide a kind of high thermal stability medium powder, and it is mainly by foregoing any
Method prepares to be formed.
The fourth object of the present invention is that providing foregoing any high thermal stability medium powder is preparing thick film dielectric painting
Application in layer.
The fifth object of the present invention is to provide a kind of thick film dielectric paste, including：Foregoing any high thermal stability
Medium powder, and, to disperse the high thermal stability medium powder and form the organic solvent of pulpous state system.
The sixth object of the present invention is to provide a kind of preparation method of thick film dielectric coating, including：
Foregoing any high thermal stability medium powder is taken to be uniformly mixed to form thick film dielectric paste with organic solvent；
The thick film dielectric paste is coated on substrate surface, after 350~450 DEG C of dumpings, then at 800 DEG C~850 DEG C
More than 12min is heat-treated, forms the thick film dielectric coating.
Among one more preferred embodiment, the preparation method of the thick film dielectric coating can include：To foregoing
Any high thermal stability medium powder in add organic solvent, through rolling form the thick film dielectric paste.
Compared with prior art, advantages of the present invention includes：
(1) present invention makes full use of four kinds of montmorillonitic clay, Concave-convex clay rod, agstone, diatomite materials in member
The medium powder that prepared by complementary on element composition and microstructure and stainless steel hot dilatancy is close, and by its with it is organic molten
Liquid compounds to form thick film dielectric paste, and the slurry obtains thick film dielectric coating thermal shock resistance after printing, dry film, heat cure
It is very high, can fully meet the needs of current thick film dielectric paste product, be particularly suitable for the application in high thermal shock field.
(2) present invention uses four kinds of montmorillonitic clay, Concave-convex clay rod, agstone, diatomite mineral materials as original
Material prepares high thermal stability medium powder, and not only raw material sources enrich for it, cheap, and the high thermal stability medium powder
The preparation method of body has the features such as technique is simple, and high temperature melting temperature is low, the time is short, energy consumption is low, and cost is cheap, is easy to industry
Change.
Embodiment
In view of the defects of existing insulating thick film medium powder product, inventor obtains through studying for a long period of time and largely putting into practice
To propose technical scheme, the technical scheme, its implementation process and principle etc. will be further explained as follows
It is bright.
Present invention firstly provides a kind of high thermal stability medium powder precursor, and it includes following component：Montmorillonitic clay
10~25 parts of 50~100 parts, 40~80 parts of Concave-convex clay rod, 25~50 parts of agstone and diatomite.
Further, invention broadly provides a kind of preparation method of high thermal stability medium powder, montmorillonite is glued
Soil, Concave-convex clay rod, agstone, diatomite uniformly after mixing, by high temperature melting, water quenching and grind processing successively, system
Obtain the high thermal stability medium powder.
Wherein, " high temperature " in " high temperature melting ", refer to the high thermal stability medium powder precursor melting can be formed
The temperature of glass precursor solution, particularly relates to more than 1200 DEG C of temperature, preferably 1200~1350 DEG C, especially preferably 1250~
1300℃。
Among one more preferred embodiment, the preparation method of the high thermal stability medium powder may include：
Foregoing high thermal stability medium powder precursor is provided, and makes each group in the high thermal stability medium powder precursor
Divide uniformly mixing；
By the high thermal stability medium powder precursor at 1200~1350 DEG C, particularly preferably in 1250~1300 DEG C of meltings
Glass precursor solution is formed, wherein, the time of melting, particularly preferably control was in 15~120min preferably in more than 15min；
The glass precursor solution is inserted in water, water quenching is particularly carried out in deionized water, forms devitrified glass slag；
And by the devitrified glass slag is ground and/or the technique such as ball milling, it is preferred to use what is carried out successively grinds, be high
Fast ball-milling technology grinds to form high thermal stability medium powder, preferably high thermal stability medium powder of the particle diameter at 0.1~10 μm
Body, to be assembled with organic solvent.
To make each component in the high thermal stability medium powder precursor uniformly mix, can use a variety of known to industry
Mode.
And one of more preferable scheme is used as, can be by the high thermal stability medium powder precursor dispersion in water decile
In dispersion media, decentralized medium is removed after ball-milling treatment, then from modes such as heating evaporations, and then reaches and makes the high heat stability
Property medium powder precursor in each component uniformly mixing purpose.
Postscript, the process conditions of foregoing high speed ball milling are preferably：500~650r/min of ball milling speed, Ball-milling Time be 4~
24h。
Secondly, present invention also offers the application of foregoing high thermal stability medium powder, for example, being applied preparing thick film dielectric
Purposes in layer.
As one of typical application scheme, thick film dielectric slurry can be prepared using the high thermal stability medium powder
Material.
For example, a kind of thick film dielectric paste therein can include：The high thermal stability medium powder, and, to
Disperse the high thermal stability medium powder and form the solvent of pulpous state system, particularly organic solvent, such as terpinol, butyl
Mixed solvent more than one or both of carbitol acetate, GBL, polyethylene glycol etc., but not limited to this.
And the preparation method of one of which thick film dielectric coating can include：
The high thermal stability medium powder is taken to be uniformly mixed to form thick film dielectric paste with organic solvent,
The thick film dielectric paste is coated on substrate surface, after 350~450 DEG C of dumpings, then at 800 DEG C~850 DEG C
More than 12min is heat-treated, forms the thick film dielectric coating.
Among one more preferred embodiment, it can be added into the high thermal stability medium powder organic molten
Agent, the thick film dielectric paste is formed through rolling.
The present invention is using four kinds of montmorillonitic clay, Concave-convex clay rod, agstone and diatomite mineral materials as raw material, warp
Cross mixing, high temperature melting, water quenching and grinding step, you can the high thermal stability medium powder that can be used for preparing thick devices is made
Body, technique is simple, can not only reduce energy consumption, it is cost-effective, be easy to industrialization, and can show the thermal shock resistance of coating
Write and improve.
In order that the narration of disclosure of the present invention is more detailed with complete, below for the present invention embodiment aspect with
Specific embodiment proposes illustrative description；But this not implements or the unique forms with the specific embodiment of the invention.With
Lower disclosed each embodiment, beneficial in the case of can be mutually combined or substitute, can also add others in one embodiment
Embodiment, and without further record or explanation.
Embodiment 1
Weigh following material：80 parts of (if not following special instruction, then be parts by weight) montmorillonitic clays, 60 parts of concave convex rods
Stone clay, 45 parts of agstones, 25 parts of diatomite are as raw material, using deionized water as decentralized medium ball milling 10 hours, its Central Plains
Material and the mass ratio of deionized water are 1：1, dried 6 hours at 120 DEG C, in 1250 DEG C of melting 60min, then water quenching obtains glass
Slag, for ball milling into the high thermal stability medium powder (following abbreviation " medium powder ") that average grain diameter is 2 μm or so, addition is organic molten
Agent is (for example, any one or more mixing among terpinol, butyl carbitol acetate, GBL, polyethylene glycol
Thing) after be rolled into thick film dielectric paste, then by the slurry using screen-printing deposition on 304 stainless steel substrate surfaces, through 400 DEG C
After dumping, it is heat-treated 12min at 820 DEG C and obtains product a.
Embodiment 2
Weigh following material：100 parts of (if not following special instruction, then be parts by weight) montmorillonitic clays, 80 parts it is (as follows
If not special instruction, then be parts by weight) Concave-convex clay rod, 30 parts of agstones, 10 parts of diatomite as raw material, with go from
Sub- water is decentralized medium ball milling 2 hours, and batch mixing is uniform, and wherein the mass ratio of raw material and deionized water is 1：1,150 after drying
DEG C dry 4 hours, in 1350 DEG C of melting 15min, then water quenching obtains glass dregs, and ball milling is into the high fever that average grain diameter is 10 μm or so
Stability medium powder (following abbreviation " medium powder "), (same as Example 1 or similar is organic molten for addition organic solvent
Agent) after be rolled into thick film dielectric paste, then by the slurry using screen-printing deposition on 430 stainless steel substrate surfaces, through 350 DEG C
After dumping, it is heat-treated 15min at 850 DEG C and obtains product b.
Embodiment 3
Weigh following material：60 parts of (if not following special instruction, then be parts by weight) montmorillonitic clays, 40 parts of concave convex rods
Stone clay, 50 agstones, 15 parts of diatomite are raw material, and using deionized water as decentralized medium ball milling 4 hours, wherein raw material is with going
The mass ratio of ionized water is 1：1, dried 10 hours at 100 DEG C, in 1300 DEG C of melting 120min, then water quenching obtains glass dregs, ball
The high thermal stability medium powder (following abbreviation " medium powder ") of 5 μm of average grain diameter is worn into, addition organic solvent is (with embodiment
1 same or similar organic solvent) after be rolled into thick film dielectric paste, it is then the slurry is stainless using screen-printing deposition 316
Base steel plate surface, after 450 DEG C of dumpings, it is heat-treated 15min at 830 DEG C and obtains product c.
Reference examples
Commercially available high thermal stability medium powder (XiAn Hongxing Electronic Paste Co., Ltd.) is taken according to embodiment 1
In mode thick film dielectric paste (" slurrying "), printing coating, sintering is made, obtain product d.
Obtain product a, b, c in 1-3 of the embodiment of the present invention and reference examples obtain product d thermal shock resistance properties contrast and can be found in
Shown in table 1-1, the thermal shock resistance of thick film dielectric coating of the invention is obviously improved as seen from the table.
Product a, b, c are obtained in table 1-1 embodiments 1-3 and reference examples obtain product d thermal shock resistance contrast
In summary, the present invention is using four kinds of montmorillonitic clay, Concave-convex clay rod, agstone and diatomite mineral materials
Expect to prepare high thermal stability medium powder for raw material, not only raw material sources enrich for it, cheap, and the preparation method has
The features such as technique is simple, and high temperature melting temperature is low, the time is short, energy consumption is low, and cost is cheap, it is easy to industrialization, while obtained thick film
Dielectric coated thermal shock resistance is very high, can fully meet the needs of current thick film dielectric paste product, be particularly suitable for height
The application in thermal shock field.
In addition, mode of the inventor referring also to embodiment 1~3, with the other raw materials and bar listed in this specification
Part etc. is tested, and the very high thick film dielectric of high thermal stability medium powder and thermal shock resistance has equally been made
Coating.
It should be understood that the foregoing is only the preferred embodiments of the present invention, it is not intended to limit the invention, for
For those skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles of the invention, institute
Any modification, equivalent substitution and improvements of work etc., should be included in the scope of the protection.
Claims (10)
1. a kind of high thermal stability medium powder precursor, it is characterised in that include the following component calculated by weight：Montmorillonite
10~25 parts of 50~100 parts of clay, 40~80 parts of Concave-convex clay rod, 25~50 parts of agstone and diatomite.
2. a kind of preparation method of high thermal stability medium powder, it is characterised in that comprise the following steps：
High thermal stability medium powder precursor is provided, includes following component：50~100 parts of montmorillonitic clay, Concave-convex clay rod
10~25 parts of 40~80 parts, 25~50 parts of agstone and diatomite；
Each component in the high thermal stability medium powder precursor is uniformly mixed, and melting forms glass more than 1200 DEG C
Liquid；
The glass precursor solution is subjected to water quenching, forms devitrified glass slag；
And the devitrified glass sizing system is formed into high thermal stability medium powder of the particle diameter at 0.1~10 μm.
3. the preparation method of high thermal stability medium powder according to claim 2, it is characterised in that including：By the height
Heat endurance medium powder precursor is at 1200~1350 DEG C, preferably 1250~1300 DEG C of more than melting 15min, preferably 15~
120min, form the glass precursor solution.
4. the preparation method of high thermal stability medium powder according to claim 2, it is characterised in that including：By the crystallite
Glass dregs are ground successively, ball milling forms the high thermal stability medium powder.
5. the preparation method of high thermal stability medium powder according to claim 4, it is characterised in that the technique of the ball milling
Condition is：Ball milling speed is 500~650r/min, and Ball-milling Time is 4~24h.
6. a kind of high thermal stability medium powder, it is characterised in that it is mainly as the method any one of claim 2-5
Prepare and formed.
7. application of the high thermal stability medium powder in thick film dielectric coating is prepared described in claim 6.
A kind of 8. thick film dielectric paste, it is characterised in that including：High thermal stability medium powder described in claim 6, and,
To disperse the high thermal stability medium powder and form the organic solvent of pulpous state system；Preferably, the organic solvent bag
Include any one in terpinol, butyl carbitol acetate, GBL and polyethylene glycol or two or more combinations.
A kind of 9. preparation method of thick film dielectric coating, it is characterised in that including：
The high thermal stability medium powder described in claim 6 is taken to be uniformly mixed to form thick film dielectric paste with organic solvent；
The thick film dielectric paste is coated on substrate surface, after 350 DEG C~450 DEG C dumpings, then in 800 DEG C~850 DEG C heat
More than 12min is handled, forms the thick film dielectric coating.
10. the preparation method of thick film dielectric coating according to claim 9, it is characterised in that including：To described in claim 6
High thermal stability medium powder in add organic solvent, through rolling form the thick film dielectric paste.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104071985A (en) * | 2014-07-14 | 2014-10-01 | 中国科学院宁波材料技术与工程研究所 | Microcrystal glass powder precursor, microcrystal glass powder as well as preparation method and application of microcrystal glass powder precursor and microcrystal glass powder |
| US20160185609A1 (en) * | 2013-06-03 | 2016-06-30 | China University Of Petroleum-Beijing | 4a-type molecular sieve synthesis method |
-
2017
- 2017-09-25 CN CN201710875592.5A patent/CN107572824A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160185609A1 (en) * | 2013-06-03 | 2016-06-30 | China University Of Petroleum-Beijing | 4a-type molecular sieve synthesis method |
| CN104071985A (en) * | 2014-07-14 | 2014-10-01 | 中国科学院宁波材料技术与工程研究所 | Microcrystal glass powder precursor, microcrystal glass powder as well as preparation method and application of microcrystal glass powder precursor and microcrystal glass powder |
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