[go: up one dir, main page]

CN109456038A - A kind of domestic ceramics and its preparation process - Google Patents

A kind of domestic ceramics and its preparation process Download PDF

Info

Publication number
CN109456038A
CN109456038A CN201811616532.2A CN201811616532A CN109456038A CN 109456038 A CN109456038 A CN 109456038A CN 201811616532 A CN201811616532 A CN 201811616532A CN 109456038 A CN109456038 A CN 109456038A
Authority
CN
China
Prior art keywords
preparation process
ceramics
hours
crude
domestic ceramics
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201811616532.2A
Other languages
Chinese (zh)
Inventor
卢蝶
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201811616532.2A priority Critical patent/CN109456038A/en
Publication of CN109456038A publication Critical patent/CN109456038A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/06—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on oxide mixtures derived from dolomite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
    • C04B41/5062—Borides, Nitrides or Silicides
    • C04B41/5068—Titanium nitride
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/87—Ceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427—Silicates other than clay, e.g. water glass
    • C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6565—Cooling rate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Physical Vapour Deposition (AREA)
  • Ceramic Products (AREA)

Abstract

The present invention provides a kind of domestic ceramics and its preparation processes, beautiful, high mechanical strength crude ceramics are made with raw materials such as dolomite, spinelle, mullite, pyrophyllite, lepidolite, vermiculite power and aerating aluminium powders in the present invention, then in exposure depositing titanium nitride-nitridation zirconium compound film of crude ceramics, finally undergo heating-slow cooling-fast cooling process, composite membrane sufficiently extends chimeric into the micro-pore of crude ceramic surface, further increase the mechanical strength and scratch-resistant of product, and not affecting the appearance property.

Description

A kind of domestic ceramics and its preparation process
Technical field
The present invention relates to ceramic technology fields, more particularly to a kind of domestic ceramics and its preparation process.
Background technique
Domestic ceramics is the demand with people to daily life and generates, as tableware, tea set, coffee tool, drinking utensils, very Vase container used into life etc. belongs to the scope of domestic ceramics.Domestic ceramics not only has preferable aesthetics, and And relatively cleaner bright and clean easy to clean.The chemical property of domestic ceramics is stablized, durable, there is acid and alkali resistance, salt and carbon in atmosphere acid The ability of gas cut erosion, is not susceptible to chemically react, will not get rusty aging.
With the improvement of living standards, people also have higher requirement the appearance and quality of domestic ceramics.City at present There are many high-grade ceramics, such as china, steatite ceramic etc. on, they have good whiteness and transparency, but mechanical strength It is poor, be not suitable for frequent routine and use, moreover, easily causing scratch when routine use or scrub, influences beauty, user experience It is very poor.
In order to improve the scratch-resistant of ceramic, have tried to still thus will affect in surface formation coating The indexs such as the whiteness of ceramics, aesthetics are deteriorated.
Summary of the invention
Present invention aim to provide a kind of domestic ceramics and its preparation process, aesthetics is good, and high mechanical strength is resistance to Scratch.
To achieve the above object, the present invention is achieved by the following scheme:
A kind of preparation process of domestic ceramics, comprising steps of
(1) dolomite, spinelle, mullite, pyrophyllite and lepidolite crushed respectively and with mass ratio 1:0.6~0.8:0.3 ~0.4:0.2~0.3:0.1~0.2 is mixed, and obtains mixed powder；
(2) mixed powder is calcined, and is ground, and sieving obtains calcining powder；
(3) after calcining powder and vermiculite power, the mixing of aerating aluminium powder, using dehydrated alcohol as decentralized medium, ultrasonic disperse, ball milling, drying, Obtain raw material；
(4) raw material is put into extrusion forming in mold, is cooled to room temperature (25 DEG C) in 20~30 minutes rapidly after sintering, obtains crude Ceramics；
(5) in exposure depositing titanium nitride-nitridation zirconium compound film of crude ceramics, deposition thickness is 20~30 μm；
(6) 1300~1400 DEG C are warming up to 25~30 DEG C/min of heating rate, 30~40 minutes are kept the temperature, then with 2~3 DEG C/min rate of temperature fall be cooled to 1000~1200 DEG C, room temperature is then cooled to 18~22 DEG C/min of rate of temperature fall, To obtain the final product.
Preferably, in step (1), diameter is crushed to less than 10mm.It is too small to improve production cost, it is excessive to be unfavorable for each group Divide and be sufficiently mixed, influences the final mechanical performance of product.
Preferably, in step (2), calcination condition are as follows: 500~600 DEG C are calcined 12~15 hours.The excessively high possibility of calcination temperature Cause decomposed, influences microcosmic reconstruct；It is too low also to will affect microcosmic reconstruct, and then influence product mechanical performance and whiteness etc..
Preferably, in step (2), 80~100 meshes are crossed after grinding.
Preferably, in step (3), the mass volume ratio for calcining powder, vermiculite power, aerating aluminium powder and dehydrated alcohol is 1g:0.5 ~0.6g:0.1~0.2g:30~40mL.
Preferably, in step (3), the ultrasonic disperse time is 30~40 minutes, and Ball-milling Time is 2~3 hours, 60~70 DEG C Drying 3~4 hours.
Preferably, in step (4), the process conditions of sintering are as follows: 1300~1400 DEG C are sintered 5~6 hours.
Preferably, exposure cvd nitride aluminium and nitridation in step (5), using magnetron sputtering technique in crude ceramics Zirconium.
It is further preferred that the process conditions of magnetron sputtering technique are as follows: multi-ion source coating machine, magnetron sputtering target diameter The single-stage medium-frequency pulse power supply of 10cm, pulse frequency 40kHz, pulse voltage maximum value 1000V, the one of single-stage medium-frequency pulse power supply Terminate vacuum chamber, the titanium-zirconium alloy sputtering target of another termination mass ratio 1:1, circular vacuum room connection molecule pump, ultimate vacuum 3 ×10-3Pa, titanium-zirconium alloy sputtering target purity are 99.99%, and discharge gas is Ar and N2Mixed gas, the purity of the two all exists 99.99% or more, after being filled with reaction gas, the pressure of vacuum chamber is maintained at 0.4Pa, the exposure face sputtering target of crude ceramics And the distance of the two is 20cm, power 800W, sedimentation time is 2~3 hours, N2Flow rate ratio (N2Flow/(N2Flow+ Ar flow), flux unit is mL/min) it is 2.5%.
A kind of domestic ceramics obtained using above-mentioned preparation process.
The beneficial effects of the present invention are:
Beauty is made with raw materials such as dolomite, spinelle, mullite, pyrophyllite, lepidolite, vermiculite power and aerating aluminium powders in the present invention It sees, the crude ceramics of high mechanical strength most pass through afterwards then in exposure depositing titanium nitride-nitridation zirconium compound film of crude ceramics Heating-slow cooling-fast cooling process is gone through, composite membrane sufficiently extends into the micro-pore of crude ceramic surface to be fitted into, into One step improves the mechanical strength and scratch-resistant of product, and not affecting the appearance property.
Dolomite, spinelle, mullite, pyrophyllite, lepidolite are calcined after crushing, and microcosmic reconstruct improves ceramic product Whiteness cooperates vermiculite power and aerating aluminium powder, has good mechanical strength after sintering.
The leading calcination processing of dolomite, spinelle, mullite, pyrophyllite, lepidolite there are one reason, directly heat to Higher sintering temperature, (such as dolomite decomposes and generates carbon dioxide and calcium oxide, magnesia partial material fast decoupled Mixture), it is unfavorable for carrying out structural remodeling with unclassified stores, synergistic effect can not be played, influence the aesthetics and machinery of product Intensity.
The present invention crude ceramics exposure depositing titanium nitride-nitridation zirconium compound film, titanium zirconium composite deposition with single group Divide sedimentary facies ratio, it is synergistic, the better scratch-resistant of product is assigned, and guarantee that product whiteness is unaffected.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
Titanium-zirconium alloy sputtering target of the present invention is purchased from Baoji Kai Ze metal material Co., Ltd.
Embodiment 1
A kind of preparation process of domestic ceramics, comprising steps of
(1) dolomite, spinelle, mullite, pyrophyllite and lepidolite crushed respectively and with mass ratio 1:0.6:0.3:0.2: 0.1 mixing, obtains mixed powder；
(2) mixed powder is calcined, and is ground, and sieving obtains calcining powder；
(3) after calcining powder and vermiculite power, the mixing of aerating aluminium powder, using dehydrated alcohol as decentralized medium, ultrasonic disperse, ball milling, drying, Obtain raw material；
(4) raw material is put into extrusion forming in mold, is cooled to room temperature (25 DEG C) in 20 minutes rapidly after sintering, obtains crude pottery Porcelain；
(5) in exposure depositing titanium nitride-nitridation zirconium compound film of crude ceramics, deposition thickness is 20 μm；
(6) 1300 DEG C are warming up to 25 DEG C/min of heating rate, 30 minutes are kept the temperature, then with 2 DEG C/min of rate of temperature fall Be cooled to 1000 DEG C, then with 18 DEG C/min of rate of temperature fall be cooled to room temperature to get.
Wherein, in step (1), diameter is crushed to less than 10mm.
In step (2), calcination condition are as follows: 500 DEG C are calcined 12 hours.
In step (2), 80 meshes are crossed after grinding.
In step (3), the mass volume ratio for calcining powder, vermiculite power, aerating aluminium powder and dehydrated alcohol is 1g:0.5g:0.1g: 30mL。
In step (3), the ultrasonic disperse time is 30 minutes, and Ball-milling Time is 2 hours, and 60 DEG C dry 3 hours.
In step (4), the process conditions of sintering are as follows: 1300 DEG C are sintered 5 hours.
In step (5), using magnetron sputtering technique crude ceramics exposure cvd nitride aluminium and zirconium nitride.Magnetic control splashes Penetrate the process conditions of technology are as follows: multi-ion source coating machine, the single-stage intermediate frequency of magnetron sputtering target diameter 10cm, pulse frequency 40kHz The pulse power, pulse voltage maximum value 1000V, a termination vacuum chamber of single-stage medium-frequency pulse power supply, another termination mass ratio 1:1 Titanium-zirconium alloy sputtering target, circular vacuum room connection molecule pump, ultimate vacuum be 3 × 10-3Pa, titanium-zirconium alloy sputtering target purity are 99.99%, discharge gas is Ar and N2Mixed gas, the purity of the two is all 99.99% or more, after being filled with reaction gas, very The pressure of empty room is maintained at 0.4Pa, the exposure face sputtering target of the crude ceramics and distance of the two is 20cm, and power is 800W, sedimentation time are 2 hours, N2Flow rate ratio (N2Flow/(N2Flow+Ar flow), flux unit is mL/min) be 2.5%。
A kind of domestic ceramics obtained using above-mentioned preparation process.
Embodiment 2
A kind of preparation process of domestic ceramics, comprising steps of
(1) dolomite, spinelle, mullite, pyrophyllite and lepidolite crushed respectively and with mass ratio 1:0.8:0.4: 0.3:0.2 mixing, obtains mixed powder；
(2) mixed powder is calcined, and is ground, and sieving obtains calcining powder；
(3) after calcining powder and vermiculite power, the mixing of aerating aluminium powder, using dehydrated alcohol as decentralized medium, ultrasonic disperse, ball milling, drying, Obtain raw material；
(4) raw material is put into extrusion forming in mold, is cooled to room temperature (25 DEG C) in 30 minutes rapidly after sintering, obtains crude pottery Porcelain；
(5) in exposure depositing titanium nitride-nitridation zirconium compound film of crude ceramics, deposition thickness is 30 μm；
(6) 1400 DEG C are warming up to 30 DEG C/min of heating rate, 40 minutes are kept the temperature, then with 3 DEG C/min of rate of temperature fall Be cooled to 1200 DEG C, then with 22 DEG C/min of rate of temperature fall be cooled to room temperature to get.
Wherein, in step (1), diameter is crushed to less than 10mm.
In step (2), calcination condition are as follows: calcination condition are as follows: 600 DEG C are calcined 15 hours.
In step (2), sieved with 100 mesh sieve after grinding.
In step (3), the mass volume ratio for calcining powder, vermiculite power, aerating aluminium powder and dehydrated alcohol is 1g:0.6g: 0.2g:40mL.
In step (3), the ultrasonic disperse time is 40 minutes, and Ball-milling Time is 3 hours, and 70 DEG C dry 4 hours.
In step (4), the process conditions of sintering are as follows: 1400 DEG C are sintered 6 hours.
In step (5), using magnetron sputtering technique crude ceramics exposure cvd nitride aluminium and zirconium nitride.Magnetic control splashes Penetrate the process conditions of technology are as follows: multi-ion source coating machine, the single-stage intermediate frequency of magnetron sputtering target diameter 10cm, pulse frequency 40kHz The pulse power, pulse voltage maximum value 1000V, a termination vacuum chamber of single-stage medium-frequency pulse power supply, another termination mass ratio 1:1 Titanium-zirconium alloy sputtering target, circular vacuum room connection molecule pump, ultimate vacuum be 3 × 10-3Pa, titanium-zirconium alloy sputtering target purity are 99.99%, discharge gas is Ar and N2Mixed gas, the purity of the two is all 99.99% or more, after being filled with reaction gas, very The pressure of empty room is maintained at 0.4Pa, the exposure face sputtering target of the crude ceramics and distance of the two is 20cm, and power is 800W, sedimentation time are 3 hours, N2Flow rate ratio (N2Flow/(N2Flow+Ar flow), flux unit is mL/min) be 2.5%。
A kind of domestic ceramics obtained using above-mentioned preparation process.
Embodiment 3
A kind of preparation process of domestic ceramics, comprising steps of
(1) dolomite, spinelle, mullite, pyrophyllite and lepidolite crushed respectively and with mass ratio 1:0.6:0.4:0.2: 0.2 mixing, obtains mixed powder；
(2) mixed powder is calcined, and is ground, and sieving obtains calcining powder；
(3) after calcining powder and vermiculite power, the mixing of aerating aluminium powder, using dehydrated alcohol as decentralized medium, ultrasonic disperse, ball milling, drying, Obtain raw material；
(4) raw material is put into extrusion forming in mold, is cooled to room temperature (25 DEG C) in 20 minutes rapidly after sintering, obtains crude pottery Porcelain；
(5) in exposure depositing titanium nitride-nitridation zirconium compound film of crude ceramics, deposition thickness is 30 μm；
(6) 1400 DEG C are warming up to 25 DEG C/min of heating rate, 30 minutes are kept the temperature, then with 3 DEG C/min of rate of temperature fall Be cooled to 1000 DEG C, then with 22 DEG C/min of rate of temperature fall be cooled to room temperature to get.
Wherein, in step (1), diameter is crushed to less than 10mm.
In step (2), calcination condition are as follows: 600 DEG C are calcined 12 hours.
In step (2), 80 meshes are crossed after grinding.
In step (3), the mass volume ratio for calcining powder, vermiculite power, aerating aluminium powder and dehydrated alcohol is 1g:0.6g: 0.1g:40mL.
In step (3), the ultrasonic disperse time is 30 minutes, and Ball-milling Time is 3 hours, and 60 DEG C dry 4 hours.
In step (4), the process conditions of sintering are as follows: 1300 DEG C are sintered 6 hours.
In step (5), using magnetron sputtering technique crude ceramics exposure cvd nitride aluminium and zirconium nitride.Magnetic control splashes Penetrate the process conditions of technology are as follows: multi-ion source coating machine, the single-stage intermediate frequency of magnetron sputtering target diameter 10cm, pulse frequency 40kHz The pulse power, pulse voltage maximum value 1000V, a termination vacuum chamber of single-stage medium-frequency pulse power supply, another termination mass ratio 1:1 Titanium-zirconium alloy sputtering target, circular vacuum room connection molecule pump, ultimate vacuum be 3 × 10-3Pa, titanium-zirconium alloy sputtering target purity are 99.99%, discharge gas is Ar and N2Mixed gas, the purity of the two is all 99.99% or more, after being filled with reaction gas, very The pressure of empty room is maintained at 0.4Pa, the exposure face sputtering target of the crude ceramics and distance of the two is 20cm, and power is 800W, sedimentation time are 2 hours, N2Flow rate ratio (N2Flow/(N2Flow+Ar flow), flux unit is mL/min) be 2.5%。
A kind of domestic ceramics obtained using above-mentioned preparation process.
Embodiment 4
A kind of preparation process of domestic ceramics, comprising steps of
(1) dolomite, spinelle, mullite, pyrophyllite and lepidolite crushed respectively and with mass ratio 1:0.8:0.3: 0.3:0.1 mixing, obtains mixed powder；
(2) mixed powder is calcined, and is ground, and sieving obtains calcining powder；
(3) after calcining powder and vermiculite power, the mixing of aerating aluminium powder, using dehydrated alcohol as decentralized medium, ultrasonic disperse, ball milling, drying, Obtain raw material；
(4) raw material is put into extrusion forming in mold, is cooled to room temperature (25 DEG C) in 30 minutes rapidly after sintering, obtains crude pottery Porcelain；
(5) in exposure depositing titanium nitride-nitridation zirconium compound film of crude ceramics, deposition thickness is 20 μm；
(6) 1300 DEG C are warming up to 30 DEG C/min of heating rate, 40 minutes are kept the temperature, then with 2 DEG C/min of rate of temperature fall Be cooled to 1200 DEG C, then with 18 DEG C/min of rate of temperature fall be cooled to room temperature to get.
Wherein, in step (1), diameter is crushed to less than 10mm.
In step (2), calcination condition are as follows: 500 DEG C are calcined 15 hours.
In step (2), sieved with 100 mesh sieve after grinding.
In step (3), the mass volume ratio for calcining powder, vermiculite power, aerating aluminium powder and dehydrated alcohol is 1g:0.5g: 0.2g:30mL.
In step (3), the ultrasonic disperse time is 40 minutes, and Ball-milling Time is 2 hours, and 70 DEG C dry 3 hours.
In step (4), the process conditions of sintering are as follows: 1400 DEG C are sintered 5 hours.
In step (5), using magnetron sputtering technique crude ceramics exposure cvd nitride aluminium and zirconium nitride.Magnetic control splashes Penetrate the process conditions of technology are as follows: multi-ion source coating machine, the single-stage intermediate frequency of magnetron sputtering target diameter 10cm, pulse frequency 40kHz The pulse power, pulse voltage maximum value 1000V, a termination vacuum chamber of single-stage medium-frequency pulse power supply, another termination mass ratio 1:1 Titanium-zirconium alloy sputtering target, circular vacuum room connection molecule pump, ultimate vacuum be 3 × 10-3Pa, titanium-zirconium alloy sputtering target purity are 99.99%, discharge gas is Ar and N2Mixed gas, the purity of the two is all 99.99% or more, after being filled with reaction gas, very The pressure of empty room is maintained at 0.4Pa, the exposure face sputtering target of the crude ceramics and distance of the two is 20cm, and power is 800W, sedimentation time are 3 hours, N2Flow rate ratio (N2Flow/(N2Flow+Ar flow), flux unit is mL/min) be 2.5%。
A kind of domestic ceramics obtained using above-mentioned preparation process.
Embodiment 5
A kind of preparation process of domestic ceramics, comprising steps of
(1) dolomite, spinelle, mullite, pyrophyllite and lepidolite crushed respectively and with mass ratio 1:0.7:0.35: 0.25:0.15 mixing, obtains mixed powder；
(2) mixed powder is calcined, and is ground, and sieving obtains calcining powder；
(3) after calcining powder and vermiculite power, the mixing of aerating aluminium powder, using dehydrated alcohol as decentralized medium, ultrasonic disperse, ball milling, drying, Obtain raw material；
(4) raw material is put into extrusion forming in mold, is cooled to room temperature (25 DEG C) in 25 minutes rapidly after sintering, obtains crude pottery Porcelain；
(5) in exposure depositing titanium nitride-nitridation zirconium compound film of crude ceramics, deposition thickness is 25 μm；
(6) 1350 DEG C are warming up to 28 DEG C/min of heating rate, 35 minutes are kept the temperature, then with 3 DEG C/min of rate of temperature fall Be cooled to 1100 DEG C, then with 20 DEG C/min of rate of temperature fall be cooled to room temperature to get.
Wherein, in step (1), diameter is crushed to less than 10mm.
In step (2), calcination condition are as follows: 550 DEG C are calcined 13 hours.
In step (2), sieved with 100 mesh sieve after grinding.
In step (3), the mass volume ratio for calcining powder, vermiculite power, aerating aluminium powder and dehydrated alcohol is 1g:0.55g: 0.15g:35mL.
In step (3), the ultrasonic disperse time is 35 minutes, and Ball-milling Time is 2 hours, and 65 DEG C dry 3 hours.
In step (4), the process conditions of sintering are as follows: 1350 DEG C are sintered 5 hours.
In step (5), using magnetron sputtering technique crude ceramics exposure cvd nitride aluminium and zirconium nitride.Magnetic control splashes Penetrate the process conditions of technology are as follows: multi-ion source coating machine, the single-stage intermediate frequency of magnetron sputtering target diameter 10cm, pulse frequency 40kHz The pulse power, pulse voltage maximum value 1000V, a termination vacuum chamber of single-stage medium-frequency pulse power supply, another termination mass ratio 1:1 Titanium-zirconium alloy sputtering target, circular vacuum room connection molecule pump, ultimate vacuum be 3 × 10-3Pa, titanium-zirconium alloy sputtering target purity are 99.99%, discharge gas is Ar and N2Mixed gas, the purity of the two is all 99.99% or more, after being filled with reaction gas, very The pressure of empty room is maintained at 0.4Pa, the exposure face sputtering target of the crude ceramics and distance of the two is 20cm, and power is 800W, sedimentation time are 2 hours, N2Flow rate ratio (N2Flow/(N2Flow+Ar flow), flux unit is mL/min) be 2.5%。
A kind of domestic ceramics obtained using above-mentioned preparation process.
Comparative example 1
A kind of preparation process of domestic ceramics, comprising steps of
(1) dolomite, spinelle, mullite and lepidolite are crushed respectively and is mixed with mass ratio 1:0.7:0.35:0.15, obtained Mixed powder；
(2) mixed powder is calcined, and is ground, and sieving obtains calcining powder；
(3) after calcining powder and vermiculite power, the mixing of aerating aluminium powder, using dehydrated alcohol as decentralized medium, ultrasonic disperse, ball milling, drying, Obtain raw material；
(4) raw material is put into extrusion forming in mold, is cooled to room temperature (25 DEG C) in 25 minutes rapidly after sintering, obtains crude pottery Porcelain；
(5) in exposure depositing titanium nitride-nitridation zirconium compound film of crude ceramics, deposition thickness is 25 μm；
(6) 1350 DEG C are warming up to 28 DEG C/min of heating rate, 35 minutes are kept the temperature, then with 3 DEG C/min of rate of temperature fall Be cooled to 1100 DEG C, then with 20 DEG C/min of rate of temperature fall be cooled to room temperature to get.
Wherein, in step (1), diameter is crushed to less than 10mm.
In step (2), calcination condition are as follows: 550 DEG C are calcined 13 hours.
In step (2), sieved with 100 mesh sieve after grinding.
In step (3), the mass volume ratio for calcining powder, vermiculite power, aerating aluminium powder and dehydrated alcohol is 1g:0.55g: 0.15g:35mL.
In step (3), the ultrasonic disperse time is 35 minutes, and Ball-milling Time is 2 hours, and 65 DEG C dry 3 hours.
In step (4), the process conditions of sintering are as follows: 1350 DEG C are sintered 5 hours.
In step (5), using magnetron sputtering technique crude ceramics exposure cvd nitride aluminium and zirconium nitride.Magnetic control splashes Penetrate the process conditions of technology are as follows: multi-ion source coating machine, the single-stage intermediate frequency of magnetron sputtering target diameter 10cm, pulse frequency 40kHz The pulse power, pulse voltage maximum value 1000V, a termination vacuum chamber of single-stage medium-frequency pulse power supply, another termination mass ratio 1:1 Titanium-zirconium alloy sputtering target, circular vacuum room connection molecule pump, ultimate vacuum be 3 × 10-3Pa, titanium-zirconium alloy sputtering target purity are 99.99%, discharge gas is Ar and N2Mixed gas, the purity of the two is all 99.99% or more, after being filled with reaction gas, very The pressure of empty room is maintained at 0.4Pa, the exposure face sputtering target of the crude ceramics and distance of the two is 20cm, and power is 800W, sedimentation time are 2 hours, N2Flow rate ratio (N2Flow/(N2Flow+Ar flow), flux unit is mL/min) be 2.5%。
A kind of domestic ceramics obtained using above-mentioned preparation process.
Comparative example 2
A kind of preparation process of domestic ceramics, comprising steps of
(1) dolomite, spinelle, mullite, pyrophyllite and lepidolite crushed respectively and with mass ratio 1:0.7:0.35: 0.25:0.15 mixing, obtains mixed powder；
(2) it omits；
(3) after mixed powder and vermiculite power, aerating aluminium powder mix, using dehydrated alcohol as decentralized medium, ultrasonic disperse, ball milling, drying, Obtain raw material；
(4) raw material is put into extrusion forming in mold, is cooled to room temperature (25 DEG C) in 25 minutes rapidly after sintering, obtains crude pottery Porcelain；
(5) in exposure depositing titanium nitride-nitridation zirconium compound film of crude ceramics, deposition thickness is 25 μm；
(6) 1350 DEG C are warming up to 28 DEG C/min of heating rate, 35 minutes are kept the temperature, then with 3 DEG C/min of rate of temperature fall Be cooled to 1100 DEG C, then with 20 DEG C/min of rate of temperature fall be cooled to room temperature to get.
Wherein, in step (1), diameter is crushed to less than 10mm.
In step (3), the mass volume ratio for calcining powder, vermiculite power, aerating aluminium powder and dehydrated alcohol is 1g:0.55g: 0.15g:35mL.
In step (3), the ultrasonic disperse time is 35 minutes, and Ball-milling Time is 2 hours, and 65 DEG C dry 3 hours.
In step (4), the process conditions of sintering are as follows: 1350 DEG C are sintered 5 hours.
In step (5), using magnetron sputtering technique crude ceramics exposure cvd nitride aluminium and zirconium nitride.Magnetic control splashes Penetrate the process conditions of technology are as follows: multi-ion source coating machine, the single-stage intermediate frequency of magnetron sputtering target diameter 10cm, pulse frequency 40kHz The pulse power, pulse voltage maximum value 1000V, a termination vacuum chamber of single-stage medium-frequency pulse power supply, another termination mass ratio 1:1 Titanium-zirconium alloy sputtering target, circular vacuum room connection molecule pump, ultimate vacuum be 3 × 10-3Pa, titanium-zirconium alloy sputtering target purity are 99.99%, discharge gas is Ar and N2Mixed gas, the purity of the two is all 99.99% or more, after being filled with reaction gas, very The pressure of empty room is maintained at 0.4Pa, the exposure face sputtering target of the crude ceramics and distance of the two is 20cm, and power is 800W, sedimentation time are 2 hours, N2Flow rate ratio (N2Flow/(N2Flow+Ar flow), flux unit is mL/min) be 2.5%。
A kind of domestic ceramics obtained using above-mentioned preparation process.
Comparative example 3
A kind of preparation process of domestic ceramics, comprising steps of
(1) dolomite, spinelle, mullite, pyrophyllite and lepidolite crushed respectively and with mass ratio 1:0.7:0.35: 0.25:0.15 mixing, obtains mixed powder；
(2) mixed powder is calcined, and is ground, and sieving obtains calcining powder；
(3) after calcining powder and vermiculite power, the mixing of aerating aluminium powder, using dehydrated alcohol as decentralized medium, ultrasonic disperse, ball milling, drying, Obtain raw material；
(4) raw material is put into extrusion forming in mold, is cooled to room temperature (25 DEG C) in 25 minutes rapidly after sintering, obtains crude pottery Porcelain；
(5) in the exposure cvd nitride zirconium film of crude ceramics, deposition thickness is 25 μm；
(6) 1350 DEG C are warming up to 28 DEG C/min of heating rate, 35 minutes are kept the temperature, then with 3 DEG C/min of rate of temperature fall Be cooled to 1100 DEG C, then with 20 DEG C/min of rate of temperature fall be cooled to room temperature to get.
Wherein, in step (1), diameter is crushed to less than 10mm.
In step (2), calcination condition are as follows: 550 DEG C are calcined 13 hours.
In step (2), sieved with 100 mesh sieve after grinding.
In step (3), the mass volume ratio for calcining powder, vermiculite power, aerating aluminium powder and dehydrated alcohol is 1g:0.55g: 0.15g:35mL.
In step (3), the ultrasonic disperse time is 35 minutes, and Ball-milling Time is 2 hours, and 65 DEG C dry 3 hours.
In step (4), the process conditions of sintering are as follows: 1350 DEG C are sintered 5 hours.
In step (5), using magnetron sputtering technique crude ceramics exposure cvd nitride aluminium and zirconium nitride.Magnetic control splashes Penetrate the process conditions of technology are as follows: multi-ion source coating machine, the single-stage intermediate frequency of magnetron sputtering target diameter 10cm, pulse frequency 40kHz The pulse power, pulse voltage maximum value 1000V, a termination vacuum chamber of single-stage medium-frequency pulse power supply, another termination mass ratio 1:1 Zirconium sputtering target, circular vacuum room connection molecule pump, ultimate vacuum be 3 × 10-3Pa, zirconium sputtering target purity are 99.99%, electric discharge Gas is Ar and N2Mixed gas, the purity of the two is all 99.99% or more, and after being filled with reaction gas, the pressure of vacuum chamber is protected It holds in 0.4Pa, the distance of the exposure face sputtering targets of crude ceramics and the two is 20cm, power 800W, sedimentation time 2 Hour, N2Flow rate ratio (N2Flow/(N2Flow+Ar flow), flux unit is mL/min) it is 2.5%.
A kind of domestic ceramics obtained using above-mentioned preparation process.
Comparative example 4
A kind of preparation process of domestic ceramics, comprising steps of
(1) dolomite, spinelle, mullite, pyrophyllite and lepidolite crushed respectively and with mass ratio 1:0.7:0.35: 0.25:0.15 mixing, obtains mixed powder；
(2) mixed powder is calcined, and is ground, and sieving obtains calcining powder；
(3) after calcining powder and vermiculite power, the mixing of aerating aluminium powder, using dehydrated alcohol as decentralized medium, ultrasonic disperse, ball milling, drying, Obtain raw material；
(4) raw material is put into extrusion forming in mold, is cooled to room temperature (25 DEG C) in 25 minutes rapidly after sintering, obtains crude pottery Porcelain；
(5) in exposure depositing titanium nitride-nitridation zirconium compound film of crude ceramics, deposition thickness is 25 μm；
(6) 1350 DEG C are warming up to 28 DEG C/min of heating rate, 35 minutes are kept the temperature, then with 20 DEG C/min of rate of temperature fall Be cooled to room temperature to get.
Wherein, in step (1), diameter is crushed to less than 10mm.
In step (2), calcination condition are as follows: 550 DEG C are calcined 13 hours.
In step (2), sieved with 100 mesh sieve after grinding.
In step (3), the mass volume ratio for calcining powder, vermiculite power, aerating aluminium powder and dehydrated alcohol is 1g:0.55g: 0.15g:35mL.
In step (3), the ultrasonic disperse time is 35 minutes, and Ball-milling Time is 2 hours, and 65 DEG C dry 3 hours.
In step (4), the process conditions of sintering are as follows: 1350 DEG C are sintered 5 hours.
In step (5), using magnetron sputtering technique crude ceramics exposure cvd nitride aluminium and zirconium nitride.Magnetic control splashes Penetrate the process conditions of technology are as follows: multi-ion source coating machine, the single-stage intermediate frequency of magnetron sputtering target diameter 10cm, pulse frequency 40kHz The pulse power, pulse voltage maximum value 1000V, a termination vacuum chamber of single-stage medium-frequency pulse power supply, another termination mass ratio 1:1 Titanium-zirconium alloy sputtering target, circular vacuum room connection molecule pump, ultimate vacuum be 3 × 10-3Pa, titanium-zirconium alloy sputtering target purity are 99.99%, discharge gas is Ar and N2Mixed gas, the purity of the two is all 99.99% or more, after being filled with reaction gas, very The pressure of empty room is maintained at 0.4Pa, the exposure face sputtering target of the crude ceramics and distance of the two is 20cm, and power is 800W, sedimentation time are 2 hours, N2Flow rate ratio (N2Flow/(N2Flow+Ar flow), flux unit is mL/min) be 2.5%。
A kind of domestic ceramics obtained using above-mentioned preparation process.
Test example
Whiteness, mechanical strength, thermal stability, the scratch-resistant etc. for detecting 1~4 gained ceramics of Examples 1 to 5 and comparative example refer to Mark, the results are shown in Table 1.
Wherein, scratch-resistant uses hardness number of the tip diamond Bu Shi by nanoindentation, uses Agilent G2000 nano impress meter executes continuous stiffness method and is superimposed small sine on it when tip loads in crystallizing layer It replaces signal (1mm amplitude, 45Hz)
1. performance of table compares
Whiteness (°) Compression strength (MPa) Thermal stability (is put into heat exchange in 20 DEG C of water) Hardness (GPa)
Embodiment 1 86 830 240 DEG C do not burst for 3 times into the water 35
Embodiment 2 86 830 240 DEG C do not burst for 3 times into the water 35
Embodiment 3 88 835 240 DEG C do not burst for 3 times into the water 38
Embodiment 4 88 834 240 DEG C do not burst for 3 times into the water 37
Embodiment 5 88 840 240 DEG C do not burst for 3 times into the water 40
Comparative example 1 71 635 140 DEG C do not burst for 3 times into the water 35
Comparative example 2 64 611 140 DEG C do not burst for 3 times into the water 33
Comparative example 3 72 800 190 DEG C do not burst for 3 times into the water 19
Comparative example 4 76 725 140 DEG C do not burst for 3 times into the water 22
As shown in Table 1, the ceramics of Examples 1 to 5 have good compression strength and thermal stability, and whiteness is high, and scratch-resistant is good. Comparative example 1 omits pyrophyllite, and comparative example 2 omits mixed powder calcining step, and comparative example 3 is nitrogenized with cvd nitride zirconium replacement deposit Titanium-zirconium nitride, comparative example 4 change last heat treatment step, and indices have different degrees of variation, are nothing like implementing Example 1~5.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art The other embodiments being understood that.

Claims (10)

1. a kind of preparation process of domestic ceramics, which is characterized in that comprising steps of
(1) dolomite, spinelle, mullite, pyrophyllite and lepidolite crushed respectively and with mass ratio 1:0.6~0.8:0.3 ~0.4:0.2~0.3:0.1~0.2 is mixed, and obtains mixed powder；
(2) mixed powder is calcined, and is ground, and sieving obtains calcining powder；
(3) after calcining powder and vermiculite power, the mixing of aerating aluminium powder, using dehydrated alcohol as decentralized medium, ultrasonic disperse, ball milling, drying, Obtain raw material；
(4) raw material is put into extrusion forming in mold, is cooled to room temperature rapidly in 20~30 minutes after sintering, obtain crude ceramics；
(5) in exposure depositing titanium nitride-nitridation zirconium compound film of crude ceramics, deposition thickness is 20~30 μm；
(6) 1300~1400 DEG C are warming up to 25~30 DEG C/min of heating rate, 30~40 minutes are kept the temperature, then with 2~3 DEG C/min rate of temperature fall be cooled to 1000~1200 DEG C, room temperature is then cooled to 18~22 DEG C/min of rate of temperature fall, To obtain the final product.
2. a kind of preparation process of domestic ceramics according to claim 1, which is characterized in that in step (1), be crushed to straight Diameter is less than 10mm.
3. a kind of preparation process of domestic ceramics according to claim 1, which is characterized in that it is preferred, in step (2), Calcination condition are as follows: 500~600 DEG C are calcined 12~15 hours.
4. a kind of preparation process of domestic ceramics according to claim 1, which is characterized in that in step (2), mistake after grinding 80~100 meshes.
5. a kind of preparation process of domestic ceramics according to claim 1, which is characterized in that in step (3), calcining powder, The mass volume ratio of vermiculite power, aerating aluminium powder and dehydrated alcohol is about 1g:0.5~0.6g:0.1~0.2g:30~40mL.
6. a kind of preparation process of domestic ceramics according to claim 1, which is characterized in that in step (3), ultrasonic disperse Time is 30~40 minutes, and Ball-milling Time is 2~3 hours, and 60~70 DEG C dry 3~4 hours.
7. a kind of preparation process of domestic ceramics according to claim 1, which is characterized in that in step (4), the work of sintering Skill condition are as follows: 1300~1400 DEG C are sintered 5~6 hours.
8. a kind of preparation process of domestic ceramics according to claim 1, which is characterized in that in step (5), using magnetic control Exposure cvd nitride aluminium and zirconium nitride of the sputtering technology in crude ceramics.
9. a kind of preparation process of domestic ceramics according to claim 8, which is characterized in that the technique of magnetron sputtering technique Condition are as follows: multi-ion source coating machine, the single-stage medium-frequency pulse power supply of magnetron sputtering target diameter 10cm, pulse frequency 40kHz, pulse Voltage max 1000V, a termination vacuum chamber of single-stage medium-frequency pulse power supply, the titanium-zirconium alloy of another termination mass ratio 1:1 splash It shoots at the target, circular vacuum room connection molecule pump, ultimate vacuum is 3 × 10-3Pa, titanium-zirconium alloy sputtering target purity are 99.99%, electric discharge Gas is Ar and N2Mixed gas, the purity of the two is all 99.99% or more, and after being filled with reaction gas, the pressure of vacuum chamber is protected It holds in 0.4Pa, the distance of the exposure face sputtering targets of crude ceramics and the two is 20cm, power 800W, sedimentation time 2 ~3 hours, N2Flow rate ratio be 2.5%.
10. a kind of domestic ceramics obtained using preparation process described in any one of claim 1~9.
CN201811616532.2A 2018-12-28 2018-12-28 A kind of domestic ceramics and its preparation process Withdrawn CN109456038A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811616532.2A CN109456038A (en) 2018-12-28 2018-12-28 A kind of domestic ceramics and its preparation process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811616532.2A CN109456038A (en) 2018-12-28 2018-12-28 A kind of domestic ceramics and its preparation process

Publications (1)

Publication Number Publication Date
CN109456038A true CN109456038A (en) 2019-03-12

Family

ID=65615223

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811616532.2A Withdrawn CN109456038A (en) 2018-12-28 2018-12-28 A kind of domestic ceramics and its preparation process

Country Status (1)

Country Link
CN (1) CN109456038A (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001253760A (en) * 2000-03-08 2001-09-18 Toto Ltd China and porcelain
CN101337831A (en) * 2008-08-08 2009-01-07 朱元义 Method for metalizing surface of ceramic
CN106518018A (en) * 2016-09-20 2017-03-22 崔松伟 Ceramic product and production method thereof
CN106699202A (en) * 2016-12-19 2017-05-24 马鞍山豹龙新型建材有限公司 Anti-oxidative refractory brick and preparation method thereof
CN107793128A (en) * 2017-11-07 2018-03-13 湖南嘉盛电陶新材料股份有限公司 Low expansion ceramic blank and its preparation method and application
CN108516795A (en) * 2018-06-13 2018-09-11 福建省德化县中国白陶瓷有限责任公司 A kind of lightening fire resistant ceramic and preparation method thereof
CN108698395A (en) * 2016-02-23 2018-10-23 法国圣戈班玻璃厂 Include the product on the protection upper layer of the mixed oxide based on zirconium and aluminium

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001253760A (en) * 2000-03-08 2001-09-18 Toto Ltd China and porcelain
CN101337831A (en) * 2008-08-08 2009-01-07 朱元义 Method for metalizing surface of ceramic
CN108698395A (en) * 2016-02-23 2018-10-23 法国圣戈班玻璃厂 Include the product on the protection upper layer of the mixed oxide based on zirconium and aluminium
CN106518018A (en) * 2016-09-20 2017-03-22 崔松伟 Ceramic product and production method thereof
CN106699202A (en) * 2016-12-19 2017-05-24 马鞍山豹龙新型建材有限公司 Anti-oxidative refractory brick and preparation method thereof
CN107793128A (en) * 2017-11-07 2018-03-13 湖南嘉盛电陶新材料股份有限公司 Low expansion ceramic blank and its preparation method and application
CN108516795A (en) * 2018-06-13 2018-09-11 福建省德化县中国白陶瓷有限责任公司 A kind of lightening fire resistant ceramic and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
本书编委会编: "《最新保温隔热材料及其制品实用配方创新设计、相关质量检验技术标准实用手册 第2卷》", 31 August 2004, 广州音像出版社 *

Similar Documents

Publication Publication Date Title
CN100560143C (en) A Composite Process for Preparing Porous Titanium Coatings by Cold Spraying and Vacuum Sintering
CN109896839B (en) Antibacterial and mildewproof ceramic tile and preparation method thereof
CN105152683A (en) Method for manufacturing nanometer antibacterial ceramic glaze layers
CN105837198B (en) Composite boilogical ceramic
CN111548122B (en) Antibacterial carved stone ceramic tile and preparation method thereof
CN101468538B (en) Coating material and preparation method thereof
CN1486955A (en) Tourmaline-purple sand product
WO2012022113A1 (en) Food/drink container for health preservation
CN103263302A (en) Orthodontic highly-transparent ceramic bracket and making method thereof
CN102268661A (en) Method for preparing Al2O3/TiC composite coating hard alloy
US20120171472A1 (en) Coated article and method for making same
CN109456038A (en) A kind of domestic ceramics and its preparation process
CN100417617C (en) In-situ growth of titanium carbonitride whisker toughened alumina-based ceramic tool material powder and its preparation process
CN104388874A (en) Silver doped alumina ceramic coating and its making method
CN107713708B (en) Anti-corrosion pot and preparation method thereof
CN107675134A (en) A kind of sintered Nd-Fe-B permanent magnet surface nitride composite deposite and preparation method
CN103923570A (en) Preparation method of rare earth-doped silicon carbide composite polishing powder
CN103422048A (en) High abrasion resistant boron carbide coating layer and preparation method thereof
CN116586610A (en) A kind of diamond-reinforced copper-based material and its preparation method and application
CN102181858A (en) Method for preparing SiC layer on surface of diamond particles
Lim et al. The effect of deposition parameters on the phase of TiO 2 films grown by RF magnetron sputtering
CN106913905A (en) A kind of anti-degraded and the good ceria doping calcium silicates coating of anti-microbial property and its preparation method and application
CN100417618C (en) In-situ growth of titanium carbide whisker toughened alumina-based ceramic tool material powder and its preparation process
CN110436890A (en) Super hydrophilic easily cleaning function ceramic material and its preparation process
CN110240491B (en) High-toughness zirconia ceramic block

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication
WW01 Invention patent application withdrawn after publication

Application publication date: 20190312