CN105924152A - Microwave dielectric ceramic material for multi-layer ceramic capacitor and preparing method of microwave dielectric ceramic material - Google Patents

Microwave dielectric ceramic material for multi-layer ceramic capacitor and preparing method of microwave dielectric ceramic material Download PDF

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CN105924152A
CN105924152A CN201610298269.1A CN201610298269A CN105924152A CN 105924152 A CN105924152 A CN 105924152A CN 201610298269 A CN201610298269 A CN 201610298269A CN 105924152 A CN105924152 A CN 105924152A
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ball milling
microwave dielectric
sintering
ceramic capacitor
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钟朝位
陶煜
刘稷
陈松
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University of Electronic Science and Technology of China
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Abstract

The invention discloses a microwave dielectric ceramic material for a multi-layer ceramic capacitor and a preparing method of the microwave dielectric ceramic material, and belongs to the technical field of electronic ceramic. The ceramic material is prepared from calcium-doped (MgZn)TiO3 system ceramic and a composite burning improver through ball milling mixing, granulating, forming, glue discharging and sintering, wherein the main crystal phase of the calcium-doped (MgZn)TiO3 system ceramic is MgTiO3, and the composite burning improver is prepared from BaCO3, B2O3, SiO2 and one or more of Li2CO3, Nb2O5 and Nd2O3. The prepared ceramic material has the advantages that a medium dielectric constant is achieved, sintering can be carried out at the medium temperature, a high Qf value is achieved, and the frequency temperature coefficient is stable. The preparing process is environmentally friendly and free of pollution, and the ceramic material can be used at the microwave frequency band of 300 M-300 GHz, can be widely applied to filters, oscillators and other microwave devices, and is especially suitable for the multi-layer ceramic capacitor.

Description

A kind of multilayer ceramic capacitor microwave dielectric ceramic materials and preparation method thereof
Technical field
The invention belongs to electronic ceramic fields, particularly relate to a kind of multilayer ceramic capacitor microwave dielectric ceramic materials and preparation thereof Method.
Background technology
Multilayer ceramic capacitor (Multilayer Ceramic Capacitors, be called for short MLCC), is main passive in complete electronic set One of surface mount elements, play in electronic circuit filtering, coupling, every straight effect, be widely used in smart mobile phone, flat board The product for civilian use and the consumer electronics such as computer, radio and television, mobile communication；Aero-Space, tank electronics, weapon bullet control etc. Military Electronic Equipment；And energy industry.MLCC mainly sends out to miniaturization, high frequency, Large Copacity, low cost direction at present Exhibition.
Low frequency (1kHz) BaTiO3Base MLCC dielectric material and high frequency CaTiO3The MLCC dielectric material of system is reported for work more, as The BaTiO announced in Chinese patent CN102718477A in 20123The MLCC material of base at 1270 DEG C～1310 DEG C sintering, Dielectric constant is between 2600～3100, and loss is less than 0.02, temperature stabilization sexual satisfaction X8R standard.Chinese patent in 2013 The BaTiO announced in CN103482975B3The MLCC material of base sinters more than 1100 DEG C, and it is left that dielectric constant is about 1800 The right side, loss is about about 0.01, and temperature stabilization sexual satisfaction meets X8R standard for ± 15%.Chinese patent in 2015 The wide temperature of one announced in CN105272220A is stable, Gao Jie, low-loss MLCC dielectric material be at 1175 DEG C～1250 DEG C Sintering, dielectric constant is about 800, and under low frequency, loss is less than 0.02.The article delivered in electronic component in 2005 and material " adds Add agent to CaTiO3The impact of ceramic performance ", in literary composition, the addition of surface additive makes CaTiO3Pottery is at 1260～1300 DEG C Sintering, in high frequency dielectric constant be 175, dielectric loss about 10-4, it is more satisfactory high frequency (1MHz) capacitor dielectric material. But, the report ratio for microwave M LCC material is sparser at present.
In the last few years, along with developing rapidly of microwave communication industry, microwave circuit has to MLCC following performance requirement:
(1) suitable dielectric constant is beneficial to the miniaturization of device；
(2) raising of dielectric constant can not victim's prime factor Qf value (whereinF is resonant frequency)；
(3) temperature coefficient of resonance frequency of stable nearly zero；
Traditional MLCC dielectric ceramic composition mentioned above cannot meet the requirement in microwave circuit to MLCC, major embodiment At Qf value and frequency-temperature coefficient, and sintering temperature higher (> 1100 DEG C), this just has higher requirement to electrode, thus carries The high cost of MLCC.
Summary of the invention
The deficiency that the present invention exists to overcome prior art, it is provided that one can have Medium dielectric constant, high Qf by intermediate sintering temperature Value and the stable multilayer ceramic capacitor (MLCC) of frequency-temperature coefficient use microwave dielectric ceramic materials.The medium pottery of the present invention Ceramic material stable performance, it is possible to use at the microwave frequency band of 300M～300GHz, and preparation technology is simple, it is easy to industry metaplasia Produce.
A kind of multilayer ceramic capacitor microwave dielectric ceramic materials, by (MgZn) TiO of calcium analysis3System pottery and compound fall Burning agent to mix through ball milling, pelletize, molding, binder removal and sintering are made；
(MgZn) TiO of described calcium analysis3The molecular formula of ceramic systems is (MgxZn1-x)TiO3·aCaTiO3, its principal crystalline phase is MgTiO3, described (MgxZn1-x)TiO3·aCaTiO3In 0.5 < x < 0.9,0.05 < a < 0.2, its quality accounts for gross mass percentage ratio and is 91%～99.5%；
Described compound fall is burnt agent raw material and is included BaCO3、B2O3And SiO2And more than one Li2CO3、Nb2O5And Nd2O3, It is 0.5%～9% that its quality accounts for gross mass percentage ratio.
In multilayer ceramic capacitor microwave dielectric ceramic materials of the present invention, its described (MgxZn1-x)TiO3·aCaTiO3In 0.5 < x < 0.9,0.05 < a < 0.2, can be by Mg (OH)2、ZnO、TiO2、CaTiO3Composition, the mol ratio of its component is Mg(OH)2∶ZnO∶TiO2∶CaTiO3=(5～9): (1～5): 10: (0.05～0.2).
The preparation method of multilayer ceramic capacitor microwave dielectric ceramic materials of the present invention is accomplished by, specifically include with Lower step:
Step 1: dispensing；By Mg (OH)2Powder, ZnO powder, TiO2Powder, CaTiO3Powder according to mol ratio be (5～ 9): (1～5): 10: it is (Mg that the component dispensing of (0.05～0.2) forms molecular formulaxZn1-x)TiO3·aCaTiO3Mixing Thing, described (MgxZn1-x)TiO3·aCaTiO3In 0.5 < x < 0.9,0.05 < a < 0.2；Porcelain ball milling is mixed to get ceramic size；
Step 2: after ceramic size step 1 prepared is dried, pre-burning synthesis principal crystalline phase obtains porcelain；
Step 3: ball milling mixes；The compound fall burning accounting for gross mass percentage ratio 0.5%～9% is added in the porcelain that step 2 obtains Agent, obtains ball milling material by described compound ball milling mix homogeneously；
Step 4: pelletize, molding；Ball milling material step 3 obtained adds binding agent pelletize after drying, and then molding is given birth to Base；
Step 5: binder removal, sintering；Step 4 gained green compact sintering after binder removal processes is prepared multilayer ceramic capacitor with micro- Ripple medium ceramic material.
Dispensing is that according to formula preparation, raw material is formed after ball milling slurry, and this operation is the of multilayer ceramic capacitor production technology One procedure.The present invention can use any suitable feedstock to form (MgxZn1-x)TiO3·aCaTiO3Porcelain, wherein 0.5 < x < 0.9, 0.05<a<0.2.Additive, described additive can be used mainly to have defoamer, increasing for raising ceramic material quality in blending process Mould agent, dispersant etc..
Pre-burning is in advance porcelain to be carried out process of thermal treatment, less than at a temperature of final sintering temperature to porcelain heat treated, Make porcelain produce series of physical chemical reaction thus improve composition and the microstructure of porcelain.In step 2 of the present invention Temperature is under the air atmosphere of 800～1000 DEG C, pre-burning 2～within 6 hours, obtain formed principal crystalline phase be MgTiO3Porcelain.
The compound fall of the multilayer ceramic capacitor microwave dielectric ceramic materials of the present invention is burnt agent and is used compound eutectic point oxide (BaCO3、B2O3、SiO2、Li2CO3) and trace mineral supplement (Nb2O5、Nd2O3).Described composition is carried out suitably Combining and mix through ball milling, melted, water is pure, and pulverizing is made compound fall and burnt agent, invention further improves conventional sintering aids Shortcoming, such as: the low melting point oxide that cannot mate with casting technique is (such as V2O5)。
The principle of ball milling is to utilize tank body to rotate, under gravity, between ball milling body mutually collision or phase mutual friction thus provide and hit Hitting and shear action so that granule depolymerization, the slurry between ball is in high turbulence state simultaneously, makes powder be disperseed；Ball Grinding process parameter mainly has rotating speed and the Ball-milling Time of ball grinder.Ball-milling technology, described step is all used in step 1 and step 3 In rapid 1, concrete mechanical milling process is: with deionized water as solvent, and ball milling mixes 3～7 hours.Concrete ball milling mistake in described step 3 Cheng Wei: with deionized water as solvent, ball milling mixes 3～8 hours.
Pelletize is so that product structure is finer and close and fine and smooth, and its technique is that through dried, levigate powder is handed over binding agent system Becoming the granule of good fluidity, general binding agent to have enough stickiness to ensure good mouldability and the mechanical strength of base substrate；Warp After high-temperature calcination can all performances etc., selecting acrylic acid solution in step 4 of the present invention is binding agent, and its mass fraction accounts for gross mass 2～5%.
Binder removal is to be placed on load bearing board by green compact according to certain temperature curve, and through high-temperature baking, removing binding agent therein etc. has Machine material, thus when avoiding sintering, the quickly volatilization of organic substance causes ceramic material layering or cracking and elimination binding agent to exist Chemical reaction effect in sintering process.Sintering is that the green compact completed by binder removal carry out high-temperature process and prepare functional ceramic material, In step 5 of the present invention, under conditions of temperature is 1000～1100 DEG C, sintering becomes multilayer ceramic capacitor use for 2～4 hours Microwave dielectric ceramic materials.
Due to magnesium titanate (MgTiO3) there is negative temperature coefficient of resonance frequency, in order to make the frequency temperature of ceramic material of the present invention Coefficient is actually needed close to zero to meet, and the calcium titanate adding positive frequency temperature coefficient is adjusted, and also improves the present invention simultaneously The dielectric constant of ceramic material；In addition the addition of zinc oxide can effectively reduce the sintering temperature of ceramic material, improves ceramic material and causes Degree of densification.
Compared to prior art, the method have the advantages that
1, the dielectric constant of the multilayer ceramic capacitor microwave dielectric ceramic materials of the present invention is adjustable from 20～25, quality factor Qf is high, and temperature coefficient of resonance frequency is little；The composite can be widely applied to high frequency, microwave M LCC, wave filter, agitator etc. micro- In wave device, the present invention is low temperature high-permittivity microwave medium core material, has essential industry using value.
2, without heavy metal component in the multilayer ceramic capacitor microwave dielectric ceramic materials of the present invention, can be at high frequency field product Middle application, environmental protection is pollution-free, and the RHOS meeting the up-to-date appearance of the European Community (" electrically, limits in electronic equipment and uses some Hazardous Substances Directive ") and the strict standard requirement of recycling management rules (WEEE).
3, the compound fall of the multilayer ceramic capacitor microwave dielectric ceramic materials of the present invention burns the compound eutectic point oxide of agent use And trace mineral supplement, the shortcoming further improving conventional sintering aids, such as: the low melting point oxidation cannot mated with casting technique Thing is (such as V2O5)。
Accompanying drawing explanation
Fig. 1 is the embodiment 1 X-ray diffractogram at 1100 degree of sintering；
Fig. 2 is the embodiment 4 X-ray diffractogram at 1050 degree of sintering；
Fig. 3 is the embodiment 1 scanning electron microscope (SEM) photograph at 1050 degree of sintering；
Fig. 4 is the embodiment 3 scanning electron microscope (SEM) photograph at 1050 degree of sintering.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further elaborated:
Embodiment:
The present invention is by by (MgZn) TiO of calcium analysis3System pottery and compound fall burn agent through ball milling mixing, pelletize, molding, row Glue and sintering are made.Wherein, (MgZn) TiO of calcium analysis3The molecular formula of system ceramic material is (MgxZn1-x)TiO3·aCaTiO3 Wherein: x=0.75, a=0.1.The manufacture raw material that described compound fall burns agent includes BaCO3、B2O3And SiO2And more than one Li2CO3、Nb2O5And Nd2O3, described compound fall is burnt each component of agent and is mixed through ball milling, melted, and water essence, pulverizing is made.
Table 1 is each component content data form of (MgZn) TiO3 system ceramic material specific embodiment:
Table 1
Wherein, embodiment 1 is (MgZn) TiO of common calcium analysis3System ceramic material component content data, embodiment 2～ The multilayer ceramic capacitor microwave dielectric ceramic materials that 8 is the present invention；The preparation method of each embodiment is as follows:
Embodiment 1:
A kind of (MgZn) TiO of common calcium analysis3The preparation method of system pottery, specifically comprises the following steps that
Step 1: dispensing；By Mg (OH)2Powder, ZnO powder, TiO2Powder, CaTiO3Powder according to mol ratio is The component dispensing of 75: 25: 100: 10 forms the (Mg of 100 gramsxZn1-x)TiO3·aCaTiO3Mixture, described (MgxZn1-x)TiO3·aCaTiO3Middle x=0.75, a=0.1；By described mixture with deionized water as solvent, ball milling mixes 5 hours Obtain ceramic size；
Step 2: after ceramic size step 1 prepared is dried, pre-burning obtains porcelain, and described calcined temperature is 880 DEG C, described pre- The burning time is 5 hours；
Step 3: ball milling mixes；In the porcelain that step 2 obtains, it is not added with any compound fall burns agent, with deionized water as solvent, Ball milling 6 hours mix homogeneously of mixing obtain ball milling material；
Step 4: pelletize, molding；After ball milling material step 3 obtained is dried, addition accounts for the acrylic acid that gross mass percentage ratio is 3% Solution pelletize, then molding obtains green compact；
Step 5: binder removal, sintering；Step 4 gained green compact sintering after binder removal processes is prepared common (MgZn) TiO3Body Series ceramic material, described sintering temperature is 1100 DEG C, and sintering time is 3 hours.
Embodiment 2:
The preparation method of a kind of multilayer ceramic capacitor microwave dielectric ceramic materials, specifically comprises the following steps that
Step 1: dispensing；By Mg (OH)2Powder, ZnO powder, TiO2Powder, CaTiO3Powder according to mol ratio is The component dispensing of 75: 25: 100: 10 forms the (Mg of 100 gramsxZn1-x)TiO3·aCaTiO3Mixture, described (MgxZn1-x)TiO3·aCaTiO3Middle x=0.75, a=0.1；By described mixture with deionized water as solvent, ball milling mixes 5 hours Obtain ceramic size；
Step 2: after ceramic size step 1 prepared is dried, pre-burning obtains porcelain, and described calcined temperature is 880 DEG C, described pre- The burning time is 5 hours；
Step 3: ball milling mixes；Adding compound fall in the porcelain that step 2 obtains and burn agent, described compound fall burns agent by 0.25 gram BaCO3, the B of 0.225 gram2O3, the SiO of 0.075 gram2, the Nb of 0.1 gram2O5With the Nd of 0.07 gram2O3Mix through ball milling Closing, melted, water is pure, and pulverizing is made, and then porcelain and compound fall burns agent composition with deionized water as solvent, and ball milling mixes Within 6 hours, mix homogeneously obtains ball milling material；
Step 4: pelletize, molding；After ball milling material step 3 obtained is dried, addition accounts for the acrylic acid that gross mass percentage ratio is 3% Solution pelletize, then molding obtains green compact；
Step 5: binder removal, sintering；Step 4 gained green compact sintering after binder removal processes is prepared multilayer ceramic capacitor with micro- Ripple medium ceramic material, described sintering temperature is 1100 DEG C, and sintering time is 3 hours.
Embodiment 3:
The preparation method of a kind of multilayer ceramic capacitor microwave dielectric ceramic materials, specifically comprises the following steps that
Step 1: dispensing；By Mg (OH)2Powder, ZnO powder, TiO2Powder, CaTiO3Powder according to mol ratio is The component dispensing of 75: 25: 100: 10 forms the (Mg of 100 gramsxZn1-x)TiO3·aCaTiO3Mixture, described (MgxZn1-x)TiO3·aCaTiO3Middle x=0.75, a=0.1；By described mixture with deionized water as solvent, ball milling mixes 4 hours Obtain ceramic size；
Step 2: after ceramic size step 1 prepared is dried, pre-burning obtains porcelain, and described calcined temperature is 900 DEG C, described pre- The burning time is 4 hours；
Step 3: ball milling mixes；Adding compound fall in the porcelain that step 2 obtains and burn agent, described compound fall burns agent by 0.30 gram BaCO3, the B of 0.25 gram2O3, the SiO of 0.08 gram2, the Nb of 0.08 gram2O5With the Nd of 0.05 gram2O3Mix through ball milling Closing, melt, water is pure, and pulverizing is made, and by porcelain with compound fall burning agent composition with deionized water as solvent, it is little that ball milling mixes 5 Time mix homogeneously obtain ball milling material；
Step 4: pelletize, molding；After ball milling material step 3 obtained is dried, addition accounts for the acrylic acid that gross mass percentage ratio is 4% Solution pelletize, then molding obtains green compact；
Step 5: binder removal, sintering；Step 4 gained green compact sintering after binder removal processes is prepared multilayer ceramic capacitor with micro- Ripple medium ceramic material, described sintering temperature is 1075 DEG C, and sintering time is 4 hours.
Embodiment 4:
The preparation method of a kind of multilayer ceramic capacitor microwave dielectric ceramic materials, specifically comprises the following steps that
Step 1: dispensing；By Mg (OH)2Powder, ZnO powder, TiO2Powder, CaTiO3Powder according to mol ratio is The component dispensing of 75: 25: 100: 10 forms the (Mg of 100 gramsxZn1-x)TiO3·aCaTiO3Mixture, described (MgxZn1-x)TiO3·aCaTiO3Middle x=0.75, a=0.1；By described mixture with deionized water as solvent, ball milling mixes 4 hours Obtain ceramic size；
Step 2: after ceramic size step 1 prepared is dried, pre-burning obtains porcelain, and described calcined temperature is 900 DEG C, described pre- The burning time is 4 hours；
Step 3: ball milling mixes；Adding compound fall in the porcelain that step 2 obtains and burn agent, described compound fall burns agent by 0.25 gram BaCO3, the B of 0.225 gram2O3, the LiCO of 0.25 gram3, the SiO of 0.15 gram2, the Nb of 0.1 gram2O5With 0.07 gram Nd2O3Mixing through ball milling, melted, water is pure, and pulverizing is made, and with compound fall, porcelain is burnt agent composition is molten with deionized water Agent, ball milling 5 hours mix homogeneously of mixing obtain ball milling material；
Step 4: pelletize, molding；After ball milling material step 3 obtained is dried, addition accounts for the acrylic acid that gross mass percentage ratio is 4% Solution pelletize, then molding obtains green compact；
Step 5: binder removal, sintering；Step 4 gained green compact sintering after binder removal processes is prepared multilayer ceramic capacitor with micro- Ripple medium ceramic material, described sintering temperature is 1075 DEG C, and sintering time is 4 hours.
Embodiment 5:
The preparation method of a kind of multilayer ceramic capacitor microwave dielectric ceramic materials, specifically comprises the following steps that
Step 1: dispensing；By Mg (OH)2Powder, ZnO powder, TiO2Powder, CaTiO3Powder according to mol ratio is The component dispensing of 75: 25: 100: 10 forms the (Mg of 100 gramsxZn1-x)TiO3·aCaTiO3Mixture, described (MgxZn1-x)TiO3·aCaTiO3Middle x=0.75, a=0.1；By described mixture with deionized water as solvent, ball milling mixes 4 hours Obtain ceramic size；
Step 2: after ceramic size step 1 prepared is dried, pre-burning obtains porcelain, and described calcined temperature is 900 DEG C, described pre- The burning time is 4 hours；
Step 3: ball milling mixes；Adding compound fall in the porcelain that step 2 obtains and burn agent, described compound fall burns agent by 0.5 gram BaCO3, the B of 0.75 gram2O3, the LiCO of 0.25 gram3, the SiO of 0.3 gram2, the Nb of 0.1 gram2O5With the Nd of 0.07 gram2O3 Mixing through ball milling, melt, water is pure, and pulverizing is made, by porcelain with compound fall burning agent composition with deionized water as solvent, and ball Mill 5 hours mix homogeneously of mixing obtain ball milling material；
Step 4: pelletize, molding；After ball milling material step 3 obtained is dried, addition accounts for the acrylic acid that gross mass percentage ratio is 4% Solution pelletize, then molding obtains green compact；
Step 5: binder removal, sintering；Step 4 gained green compact sintering after binder removal processes is prepared multilayer ceramic capacitor with micro- Ripple medium ceramic material, described sintering temperature is 1025 DEG C, and sintering time is 4 hours.
Embodiment 6:
The preparation method of a kind of multilayer ceramic capacitor microwave dielectric ceramic materials, specifically comprises the following steps that
Step 1: dispensing；By Mg (OH)2Powder, ZnO powder, TiO2Powder, CaTiO3Powder according to mol ratio is The component dispensing of 75: 25: 100: 10 forms the (Mg of 100 gramsxZn1-x)TiO3·aCaTiO3Mixture, described (MgxZn1-x)TiO3·aCaTiO3Middle x=0.75, a=0.1；By described mixture with deionized water as solvent, ball milling mixes 4 hours Obtain ceramic size；
Step 2: after ceramic size step 1 prepared is dried, pre-burning obtains porcelain, and described calcined temperature is 900 DEG C, described pre- The burning time is 4 hours；
Step 3: ball milling mixes；Adding compound fall in the porcelain that step 2 obtains and burn agent, described compound fall burns agent by 0.3 gram BaCO3, the B of 0.5 gram2O3, the LiCO of 0.3 gram3, the SiO of 0.2 gram2, the Nb of 0.1 gram2O5With the Nd of 0.07 gram2O3 Mixing through ball milling, melt, water is pure, and pulverizing is made, by porcelain with compound fall burning agent composition with deionized water as solvent, and ball Mill 5 hours mix homogeneously of mixing obtain ball milling material；
Step 4: pelletize, molding；After ball milling material step 3 obtained is dried, addition accounts for the acrylic acid that gross mass percentage ratio is 4% Solution pelletize, then molding obtains green compact；
Step 5: binder removal, sintering；Step 4 gained green compact sintering after binder removal processes is prepared multilayer ceramic capacitor with micro- Ripple medium ceramic material, described sintering temperature is 1000 DEG C, and sintering time is 4 hours.
Embodiment 7:
The operation of the present embodiment is substantially the same manner as Example 2, simply the sintering temperature of step 5 in example 2 is replaced with 1050 DEG C, Sintering temperature replaces with 4 hours.
Embodiment 8:
The operation of the present embodiment is substantially the same manner as Example 7, simply the compound fall of step 3 in example 7 is burnt agent component and replaces with The BaCO of 0.25 gram3, the B of 0.225 gram2O3, the LiCO of 0.3 gram3, the SiO of 0.2 gram2。
Table 2 is the microwave dielectric property of each embodiment corresponding in table 1, by embodiment 1～8 gained ceramic material cylindrical dielectric Resonator method carries out the evaluation of microwave dielectric property, and detection method is that (test frequency exists GB/T 7265.2-1987 open type cell method About 7GHz), its result is as shown in table 2 below:
Table 2
Below in conjunction with drawings and Examples, the present invention is further described:
Being illustrated in figure 1 the comparative examples 1 X-ray diffractogram at 1100 DEG C of sintering, Fig. 2 is that the embodiment of the present invention 5 exists The X-ray diffractogram of 1100 DEG C of sintering, can be seen that the ceramic material of the present invention generates (described fall burning agent without dephasign by contrast Do not react with material of main part, more easy to control little to performance impact)；Fig. 3 illustrates the embodiment 1 scanning at 1100 DEG C of sintering Electronic Speculum figure, Fig. 4 illustrates the embodiment 3 scanning electron microscope (SEM) photograph at 1075 DEG C of sintering, as seen from the figure, the pottery prepared of the present invention Material has been greatly facilitated sintered density, thus improves the microwave property of multilayer ceramic capacitor microwave dielectric ceramic materials.
The principle of above-described embodiment only illustrative present invention and effect thereof, not for limiting the present invention.The present invention can expand The new feature or any new combination what discloses in this manual is taken office in exhibition, and the arbitrary new method that discloses or the step of process Rapid or any new combination.Any person skilled in the art all can be under the spirit and the scope of the present invention, to above-mentioned reality Execute example modify or change.Therefore, art has usually intellectual such as without departing from disclosed All equivalences completed under spirit and technological thought are modified or change, and must be contained by the claim of the present invention.

Claims (9)

1. a multilayer ceramic capacitor microwave dielectric ceramic materials, it is characterised in that include (MgZn) TiO of calcium analysis3Ceramic systems and compound fall are burnt agent and are made through ball milling mixing, pelletize, molding, binder removal and sintering；
(MgZn) TiO of described calcium analysis3The molecular formula of ceramic systems is (MgxZn1-x)TiO3·aCaTiO3, its principal crystalline phase is MgTiO3, described (MgxZn1-x)TiO3·aCaTiO3In 0.5 < x < 0.9,0.05 < a < 0.2, it is 91%～99.5% that its quality accounts for gross mass percentage ratio；
Described compound fall is burnt agent raw material and is included BaCO3、B2O3And SiO2And more than one Li2CO3、Nb2O5And Nd2O3, it is 0.5%～9% that its quality accounts for gross mass percentage ratio.
A kind of multilayer ceramic capacitor microwave dielectric ceramic materials the most according to claim 1, it is characterised in that described (MgxZn1-x)TiO3·aCaTiO3, wherein 0.5 < x < 0.9,0.05 < a < 0.2, by Mg (OH)2、ZnO、TiO2And CaTiO3Composition, the mol ratio of its component is Mg (OH)2∶ZnO∶TiO2∶CaTiO3=(5～9): (1～5): 10: (0.05～0.2).
3. the preparation method of a multilayer ceramic capacitor microwave dielectric ceramic materials, it is characterised in that comprise the following steps:
Step 1: dispensing；By Mg (OH)2Powder, ZnO powder, TiO2Powder and CaTiO3Powder is (5～9) according to mol ratio: (1～5): 10: it is (Mg that the component dispensing of (0.05～0.2) forms molecular formulaxZn1-x)TiO3·aCaTiO3Mixture, described (MgxZn1-x)TiO3·aCaTiO3In 0.5 < x < 0.9,0.05 < a < 0.2；Described mixture ball milling is mixed to get ceramic size；
Step 2: ceramic size step 1 prepared is dried, pre-burning synthesis principal crystalline phase MgTiO3, prepare porcelain；
Step 3: ball milling mixes；In the porcelain that step 2 obtains, add the compound fall burning agent accounting for gross mass percentage ratio 0.5%～9%, described compound ball milling mix homogeneously is obtained ball milling material；
Step 4: pelletize, molding；Ball milling material step 3 obtained adds binding agent pelletize after drying, and then molding obtains green compact；
Step 5: binder removal, sintering；Step 4 gained green compact sintering after binder removal processes is prepared multilayer ceramic capacitor microwave dielectric ceramic materials.
The preparation method of a kind of multilayer ceramic capacitor microwave dielectric ceramic materials the most according to claim 3, it is characterised in that in described step 1, concrete mechanical milling process is: with deionized water as solvent, ball milling mixes 3～7 hours.
The preparation method of a kind of multilayer ceramic capacitor microwave dielectric ceramic materials the most according to claim 3, it is characterised in that in described step 2, calcined temperature is 800～1000 DEG C, burn-in time is 2～6 hours.
The preparation method of a kind of multilayer ceramic capacitor microwave dielectric ceramic materials the most according to claim 3, it is characterised in that in described step 3, compound fall burning agent raw material mixes through ball milling, and melted, water is pure, and pulverizing is made.
The preparation method of a kind of multilayer ceramic capacitor microwave dielectric ceramic materials the most according to claim 3, it is characterised in that in described step 3, concrete mechanical milling process is: with deionized water as solvent, ball milling mixes 3～8 hours.
The preparation method of a kind of multilayer ceramic capacitor microwave dielectric ceramic materials the most according to claim 3, it is characterised in that in described step 4, binding agent is acrylic acid solution, it is 2～5% that its quality accounts for gross mass percentage ratio.
The preparation method of a kind of multilayer ceramic capacitor microwave dielectric ceramic materials the most according to claim 3, it is characterised in that in described step 5, high temperature sintering temperature is 1000～1100 DEG C, sintering time is 2～4 hours.
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CN106631002A (en) * 2017-01-11 2017-05-10 电子科技大学 Dielectric material for Mg-Zn-Ti-based radio-frequency MLCC (multi-layer ceramic capacitor) and preparation method of dielectric material
CN110436917A (en) * 2018-05-04 2019-11-12 中国科学院上海硅酸盐研究所 A kind of intermediary's microwave dielectric ceramic materials and preparation method thereof
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CN110581273B (en) * 2019-09-18 2021-04-13 东北大学秦皇岛分校 Zinc-position sodium-copper co-doped synergetic nitrogen-sulfur doped carbon-coated modified zinc titanate negative electrode material and preparation method and application thereof
CN110581273A (en) * 2019-09-18 2019-12-17 东北大学秦皇岛分校 Zinc-position sodium-copper co-doped synergetic nitrogen-sulfur doped carbon-coated modified zinc titanate negative electrode material and preparation method and application thereof
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CN112159222A (en) * 2020-08-18 2021-01-01 湖南艾迪奥电子科技有限公司 High-dielectric-constant capacitor material and preparation method thereof
CN112624754A (en) * 2020-12-08 2021-04-09 赣州中瓷科技有限公司 LTCC ceramic powder for high-frequency capacitor and preparation process thereof
CN112624754B (en) * 2020-12-08 2022-11-29 赣州中傲新瓷科技有限公司 LTCC ceramic powder for high-frequency capacitor and preparation process thereof
CN112521129A (en) * 2020-12-25 2021-03-19 无锡鑫圣慧龙纳米陶瓷技术有限公司 Low-dielectric-constant ceramic dielectric material for low-temperature sintered MLCC and preparation method thereof
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