CN108911722A - A kind of high dielectric stable type ceramic medium material and preparation method thereof - Google Patents
A kind of high dielectric stable type ceramic medium material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to ceramic medium material technical field, there are sintering temperatures to solve current ceramic material it is high, dielectric constant is low, loss is higher and warm area is narrow the problems such as, a kind of high dielectric stable type ceramic medium material and preparation method thereof is provided, by glass powder and xBaSiO3‑Y2O3- 0.5ZnO is made by a certain percentage, and wherein x is 4-7;The glass powder is Na2CO3、MnO2, LiF and H3BO3It is made by a certain percentage.Select BaSiO3‑Y2O3- 0.5ZnO system, taking addition glass powder is the method for sintering aid, makes its sintering temperature lower than 1000 DEG C, and dielectric constant is high, dielectric loss is low, and the capacitance temperature factor in -55~200 DEG C of temperature ranges is no more than ± 15%.
Description
Technical field
The invention belongs to ceramic medium material technical fields, and in particular to a kind of high dielectric stable type ceramic medium material and
Preparation method.
Background technique
Capacitor is a kind of important passive electronic, is device indispensable in electronics, communication and information industry
Part can play storage charge, partition direct current, ac filter, provide tuning and concussion etc..According to material is constituted, pottery can be divided into
Porcelain capacitor, alminium electrolytic condenser, tantalum capacitor, plastic film capacitor etc..Chip multilayer ceramic capacitor (MLCC) belongs to ceramic condenser class,
With small in size, capacitance is big, cheap, stability is high and the characteristics such as suitable mass production, pursued in electronics and IT products
Under the promotion of miniaturization, the development trend of lightness and surface mounting technology, development prospect is very wide.
In recent years, as electronic information equipment in the universal of all trades and professions and is widely applied, especially in some particular rows
The application of industry and extreme environment, to the dielectric temperature change rate performance of MLCC, more stringent requirements are proposed.It controls and leads in automobile
In domain, such as start the engine electronic control unit (ECU) installed in cabin, anti-lock braking system (ABS), air/fuel ratio control
Molding block etc., it is desirable that the hot operation temperature range of MLCC reaches 150 DEG C or so.Meanwhile in avionics, autoelectrinic
During, environment measuring etc. are multi-field, require that electronic system can work normally under extreme exacting terms, this requires
The hot operation temperature of MLCC extends to 150 DEG C or more or even 200 DEG C or more.Dielectric temperature of the large value capacitor in high temperature section
Degree characteristic has become one of the key factor that can electronic equipment under hot environment work normally.It studies in more wide temperature range
Temperature-stable dielectric material become it is current there is an urgent need to.
In addition, in order to reduce the difficulty and cost that commercially produced product emerges, under the premise of guaranteeing suitable dielectric properties, also
Need to reduce the sintering temperature of MLCC material, so that silver, the gold electrode with excellence conductor being capable of cofirings.More porcelain is reported at present
Material has BaTiO3System, BiScO3System and Bi0.5Na0.5TiO3The medium ceramic materials such as system, but there is sintering in these ceramic materials
The problems such as temperature is high, dielectric constant is low, loss is higher and warm area is narrow.
Summary of the invention
That there are sintering temperatures in order to solve current ceramic material is high by the present invention, dielectric constant is low, loss is higher and warm area is narrow
The problems such as, a kind of high dielectric stable type ceramic medium material and preparation method thereof is provided, prepared ceramic medium material is burnt
Junction temperature is low(970 DEG C~990 DEG C), dielectric constant is high, dielectric loss is low, the capacitor temperature in -55 DEG C~200 DEG C temperature ranges
It spends coefficient and is no more than ± 15%.
The present invention is realized by following technical solution:A kind of high dielectric stable type ceramic medium material is by weight percent
The glass powder and weight percent of 5-13% is the xBaSiO of 87-95%3-Y2O3- 0.5ZnO composition, wherein x is 4-7;By prepared
Glass powder quality be 100% meter, the glass powder by 15-30% Na2CO3, 5-20% MnO2, 10-25% LiF and 25-
40% H3BO3Composition.
A kind of method and step of preparation high medium stable type ceramic medium material is as follows:
(1)By raw material BaSiO3、Y2O3General formula xBaSiO is pressed with ZnO3-Y2O3- 0.5ZnO, wherein x=4-7, carries out ingredient ball milling,
Cross the hole 120-250/cm2Sub-sieve is warming up to 950 DEG C -1000 DEG C, keeps the temperature 2-4 hours, and frit is made;
(2)According to mass percent by Na2CO3、MnO2, LiF and H3BO3Water cooling is melted, obtained glass powder is ground up, sieved;
(3)Glass powder and frit A are subjected to second batch according to mass percent, obtain ingredient;
(4)Ingredient ball milling is crossed into the hole 120-250/cm2Sub-sieve, the binder that ingredient mass percent 5-8% is added are granulated, pressure
Green compact are made, are heated to 400-500 DEG C by the heating rate of 2 DEG C/min, then be warming up to 970 by the heating rate of 10 DEG C/min
DEG C -990 DEG C keep the temperature 1 hour, and ceramic dielectric is made after cooling.
The step(1)Middle Ball-milling Time is 4-6 hours;The step(1)Middle heating rate is 5-10 DEG C/min.It is described
Step(1)Middle heating rate is preferably 7 DEG C/min.
The step(4)Middle heating rate is 450 DEG C to be heated to by the heating rate of 2 DEG C/min, then press 10 DEG C/min's
Heating rate is heated to 970 DEG C -990 DEG C.The step(4)In binder be polyvinyl alcohol or paraffin.
BaSiO3-Y2O3- 0.5ZnO system media ceramic have moderate sintering temperature, generally 1200 DEG C or so, have compared with
High dielectric constant, adjustable temperature coefficient of capacity and lower loss is a kind of medium ceramic material haveing excellent performance.This hair
Bright selection BaSiO3-Y2O3- 0.5ZnO system, taking addition glass powder is the method for sintering aid, makes its sintering temperature lower than 1000
DEG C and dielectric constant is high, dielectric loss is low, capacitance temperature factor is small in -55 DEG C~200 DEG C temperature ranges.
High dielectric stable type ceramic medium material prepared by the present invention meets EIA X9R standard, at -55 DEG C~200 DEG C
Capacitance temperature factor in temperature range is no more than ± 15%.With good dielectric properties, dielectric constant be can reach at 25 DEG C
2252 or so, being lost is 0.0162.Sintering temperature is low(970 DEG C~990 DEG C), silver-bearing copper can be used as interior electrode, carry out low
Warm cofiring.Sintering range is wider, and performance is adjustable, and stability and reproducibility are good, high reliablity.Without nocuousness such as heavy metals
Substance, it is environmentally protective.
Detailed description of the invention
Fig. 1 is the electromicroscopic photograph of high dielectric stable type ceramic medium material prepared by the present invention.
Specific embodiment
Technical solution of the present invention is further illustrated combined with specific embodiments below.
Embodiment 1:By raw material BaSiO3、Y2O3With ZnO by formula xBaSiO3-Y2O3- 0.5ZnO, wherein x=4, are matched
Material, in 100 DEG C of dryings in a conventional oven of 3.3kw, crosses 250 ball milling 6 hours on the ball mill that revolving speed is 400r/min
Hole/cm2Sub-sieve is warming up to 990 DEG C with 5 DEG C/min, and keeps the temperature 3 hours at 990 DEG C, obtains frit.Compare according to described in table 1
Example ingredient, melts water cooling, and grinding is sieved and glass powder is made.
Table 1:Glass powder ingredient
Second batch is carried out, is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill in revolving speed2Point
Sample sieve is added 8wt% paraffin and is granulated, be pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then press 10 DEG C/
The heating rate of min is heated to 980 DEG C of firings, keeps the temperature 1 hour, and ceramic dielectric is made after cooling.When second batch, frit and glass
See Table 2 for details for the relationship between quality of glass powder.
Table 2:Frit and glass powder relationship between quality
The test result of above-described embodiment dielectric properties(Test frequency is 1KHz)See Table 3 for details.
Table 3:Dielectric properties testing result
Embodiment 2:By raw material BaSiO3、Y2O3With ZnO by formula xBaSiO3-Y2O3- 0.5ZnO, wherein x=5, carry out ingredient,
Revolving speed is, in 100 DEG C of dryings in a conventional oven of 3.3kw, to cross 250 holes/cm ball milling 6 hours on the ball mill of 400r/min2
Sub-sieve is warming up to 990 DEG C with 5 DEG C/min, and keeps the temperature 3 hours at 990 DEG C, obtains frit.Match according to ratio described in table 4
Material, melts water cooling, and grinding is sieved and glass powder is made.
Table 4:Glass powder ingredient
Second batch is carried out, is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill in revolving speed2Point
Sample sieve is added 8wt% paraffin and is granulated, be pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then press 10 DEG C/
The heating rate of min is heated to 970 DEG C of firings, keeps the temperature 1 hour, and ceramic dielectric is made after cooling.When second batch, frit and glass
See Table 5 for details for the relationship between quality of glass powder.
Table 5:Frit and glass powder relationship between quality
The dielectric properties test result of prepared material after ingredient(Test frequency is 1KHz)See Table 6 for details.
Table 6:The test result of dielectric properties
Embodiment 3:By raw material BaSiO3、Y2O3With ZnO by formula xBaSiO3-Y2O3- 0.5ZnO, wherein x=7, carry out ingredient,
Revolving speed is, in 100 DEG C of dryings in a conventional oven of 3.3kw, to cross 250 holes/cm ball milling 6 hours on the ball mill of 400r/min2
Sub-sieve is warming up to 990 DEG C with 5 DEG C/min, and keeps the temperature 3 hours at 990 DEG C, obtains frit.Match according to ratio described in table 7
Material, melts water cooling, and grinding is sieved and glass powder is made.
Table 7
Second batch is carried out, is, in 120 DEG C of dryings, to cross 250 holes/cm ball milling 8 hours on 400r/min ball mill in revolving speed2Point
Sample sieve is added 8wt% paraffin and is granulated, be pressed into green compact, is first heated to 450 DEG C by the heating rate of 2 DEG C/min, then press 10 DEG C/
The heating rate of min is heated to 990 DEG C of firings, keeps the temperature 1 hour, and ceramic dielectric is made after cooling.When second batch, frit and glass
See Table 8 for details for the relationship between quality of glass powder.
Table 8
The test result of above-described embodiment dielectric properties(Test frequency is 1KHz)See Table 9 for details.
Table 9
Test method and detection device used in the present invention are as follows:
1. the test of permittivity ε and loss tan δ:Using HEWLETT PACKARD 4278A capacitance measuring tester, the electricity of test capacitors
Capacity C and dielectric loss tan δ(Test frequency is 1KHz), and permittivity ε is calculated by following formula:;Its
In:C-print capacitance, unit pF;D-print thickness, unit cm;The sintered diameter of D-print, unit cm 2, temperature
The test (- 55 DEG C~200 DEG C) of coefficient T CC:Using 6425 type WAYKERR electric bridges, GZ-ESPEC MC -710F high-low temperature chamber and
HM27002 type capacitor C-T/V characteristic dedicated tester measures the capacitance variation with temperature situation of sample, so as to find out capacitor
The capacitance temperature factor of device(Test frequency is 1KHz), calculation formula is as follows:;
Wherein:We choose 25 DEG C to fiducial temperature, C0For 25 DEG C of capacity of temperature, C1For temperature t1Capacity.
High dielectric stable type ceramic medium material prepared by the present invention meets EIA X9R standard, at -55 DEG C~200 DEG C
Capacitance temperature factor in temperature range is no more than ± 15%.With good dielectric properties, dielectric constant be can reach at 25 DEG C
2252 or so, being lost is 0.0162.Sintering temperature is low(970 DEG C~990 DEG C), silver-bearing copper can be used as interior electrode, carry out low
Warm cofiring.Sintering range is wider, and performance is adjustable, and stability and reproducibility are good, high reliablity.Without nocuousness such as heavy metals
Substance, it is environmentally protective.
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Fall into protection scope of the present invention.
Claims (6)
1. a kind of high dielectric stable type ceramic medium material, it is characterised in that:The glass powder and again for being 5-13% by weight percent
Measure the xBaSiO that percentage is 87-95%3-Y2O3- 0.5ZnO composition, wherein x is 4-7;It is by prepared glass powder quality
100% meter, the glass powder by 15-30% Na2CO3, 5-20% MnO2, 10-25% LiF and 25-40% H3BO3Composition.
2. the method for preparing a kind of high medium stable type ceramic medium material described in claim 1, it is characterised in that:Step is such as
Under:
(1)By raw material BaSiO3、Y2O3General formula xBaSiO is pressed with ZnO3-Y2O3- 0.5ZnO, wherein x=4-7, carries out ingredient ball milling,
Cross the hole 120-250/cm2Sub-sieve is warming up to 950 DEG C -1000 DEG C, keeps the temperature 2-4 hours, and frit is made;
(2)According to mass percent by Na2CO3、MnO2, LiF and H3BO3Water cooling is melted, obtained glass powder is ground up, sieved;
(3)Glass powder and frit A are subjected to second batch according to mass percent, obtain ingredient;
(4)Ingredient ball milling is crossed into the hole 120-250/cm2Sub-sieve, the binder that ingredient mass percent 5-8% is added are granulated, pressure
Green compact are made, are heated to 400-500 DEG C by the heating rate of 2 DEG C/min, then be warming up to 970 by the heating rate of 10 DEG C/min
DEG C -990 DEG C keep the temperature 1 hour, and ceramic dielectric is made after cooling.
3. the method according to claim 2 for preparing high medium stable type ceramic medium material, it is characterised in that:The step
Suddenly(1)Middle Ball-milling Time is 4-6 hours;The step(1)Middle heating rate is 5-10 DEG C/min.
4. the method according to claim 3 for preparing high medium stable type ceramic medium material, it is characterised in that:The step
Suddenly(1)Middle heating rate is 7 DEG C/min.
5. the method according to claim 2 for preparing high medium stable type ceramic medium material, it is characterised in that:The step
Suddenly(4)Middle heating rate is to be heated to 450 DEG C by the heating rate of 2 DEG C/min, then be heated to by the heating rate of 10 DEG C/min
970℃-990℃。
6. the method according to claim 2 for preparing high medium stable type ceramic medium material, it is characterised in that:The step
Suddenly(4)In binder be polyvinyl alcohol or paraffin.
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CN116718585A (en) * | 2023-05-05 | 2023-09-08 | 北京先通国际医药科技股份有限公司 | Method for determining oxide content in yttrium-containing glass microspheres and application of melting agent in determination of oxide content in yttrium-containing glass microspheres |
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Application publication date: 20181130 |